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STP 1165

Metallography:
Past, Present, and Future
(75th Anniversary Volume)
George F. Vander Voort, Francis J. Warmuth,
Samuel M. Purdy, and Albert Szirmae, editors

ASTM Pubhcation Code No. (PCN)


04-011650-23

AsTM
1916 Race Street
Philadelphia, PA 19103

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Library of Congress Cataloging-in-Publication Data
Metallography--past, present, and future 75th anniversary volume/
George F Vander Voort [et al ], editors
(STP 1165)
"ASTM publication code no (PCN) 04-011650-23 "
Includes bibliograph=cal references and indexes
ISBN 0-8031-1484-2
1 Metallography--Congresses I Vander Voort, George F
II Amencan Soc=ety for Testing and Materials III Senes ASTM
speo=altechnical pubhcation 1165
TN689 2 M445 1993
669' 95--dc20 93-14998
CIP

Copyright 9 1993 AMERICAN SOCIETY FOR TESTING AND MATERIALS, Philadelphia, PA All
nghts reserved This material may not be reproduced or cop=ed,=nwhole or in part, in any pnnted,
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Peer Review Policy

Each paper pubhshed in th=s volume was evaluated by three peer reviewers The authors addressed
all of the reviewers' comments to the satisfaction of both the technical ed0tor(s)and the ASTM
Committee on Pubhcatlons
The quality of the papers m this pubhcatlon reflects not only the obvious efforts of the authors and the
technical editor(s), but also the work of these peer rev=ewers The ASTM Committee on Publications
acknowledges w=th appreciation their ded~cat=onand contribution to t~meand effort on behalf of ASTM

Pnnted In Baltimore,MD
June 1993

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Foreword

The papers m this pubhcatlon, Metallography Past, Present, and Future, were presented at
the symposmm on Metallography" 75 Years Later held 8-10 May 1991 m Atlantic C~ty, New
Jersey The symposmm was sponsored by ASTM Committee E4 on Metallography. George
F Vander Voort, Carpenter Technology Corporation, Franc~s J. Warmuth, Cameron Forge
Company, Samuel M Purdy, National Steel Company, and Albert Szlrmae, U S Steel Cor-
poration, served as symposmm cochmrmen and are coe&tors of th~s pubhcatlon

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Contents

Overview

The History of ASTM Committee E4 on Metallography--


GEORGE F VANDER VOORT

LIGHT MICROSCOPY

Some Incidental History of Metallography and ASTM Committee E 4 - -


THEODORE G. ROCHOW 83

Research Under the Microscope--WILLIAM G. FRICKE,JR 88

METALLOGRAPHIC PREPARATION TECHNIQUES

Automotive Materials and Their Characterization: 1916 to 1 9 9 1 -


GERALD S COLE, LESLIE BARTOSIEWICZ, AND FLOYD E ALBERTS 109

New Diamond Grinding Disks for Specimen Surface l>reparation--


ROBERT L. BENNER 139

Advancements in Ultrathin Section Techniques for the Characterization of Brittle


m a t e r i a l s - - N A T A L I O T SAENZ 155

The Early Metallographic Studies of Chih-Hung Chon on the Formation and


Morphology of Widmanstatten Structure and Martensite--
MICHAEL R. NOTIS, ARNOLD R. MARDER, AND YE T. CHOU 167

X - R A Y AND ELECTRON METALLOGRAPHY

Those Magnificent Men on Their Scanning Machines--KURT F. J HEINRICH 177

Seventy-Five Years of Activity in X-Ray Methods by ASTM Committee E4.06--


SAMUEL M. PURDY AND LEO ZWELL 184

Microstrnetural Studies of an Oxide-Dispersion-Stabilized Niobium Composite


Using Transmission Electron Microscopy--ATUL S RAMANI
AND PAUL R HOWELL 189

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The Application of Transmission Electron Microscopy to the Study of a Low-
Carbon Steel: H S L A - 1 0 0 - - R A J A N VARUGHESE AND PAUL R HOWELL 199

Transmission Electron Microscopy of the lnterdiffusion Regions of Iron-Zinc


C o u p I e s - - L U C I L L E A. GIANNUZZI, PAUL R HOWELL,
HOWARD W PICKERING, AND WILLIAM R. BITLER 212

Some Reflections on the Early Development of Electron Microscopy and


Microanalysis--JAMES HILLIER 224

QUANTITATIVE METALLOGRAPHY

Quantitative Metallography in Test Method Standards and Product


SpecificationS--DANIEL B FOWLER 235

Artificial Intelligence for Twin Identification--JOHN J. FRIEL


AND EDDIE B PRESTRIDGE 243

The Use of Quantitative Image Analysis for the Characterization of Corrosion-


Resistant Coatings--SCOTT T. BLUNI, KATHERINE M. GOGGINS,
BRIAN J. SMITH, AND ARNOLD R MARDER 254

Examination of Some Grain Size Measurement Problems--


G E O R G E F. VANDER VOORT 266

Measurement and Interpretation of Fracture Surface Fractal Dimension--


WILLIAM DRURY AND ARUN M GOKHALE 295

APPLICATIONS I

In Search of Mierostructure--JAMES A NELSON 313

The Microstructure of Laser-Welded Aluminum BronzeS--DAVID E BELL,


TERRI A. MARSICO, KATHLEEN PETROLONIS, PAUL E DENNEY,
AND PAUL R HOWELL 327

Metallography of Mechanically Alloyed Aluminum--WILLIAM J. D SHAW 344

Microstructural Investigations of Rapidly Solidified Copper-Niobium (Cu-Nb)


Alloy Powders Produced by Inert Gas Atomization--gEVXN L ZEIK,
IVER E ANDERSON, DONALD A KOOS, AND PAUL R. HOWELL 363

Metallography Applied to the Structure of Electrorheoiogical (ER) Fluids--


M A R K D. FISHER, ARNOLD F. SPRECHER, AND HANS CONRAD 372

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APPLICATIONS II

Interpreting Solidification Phenomena and Microstructural Evolution in Metals


Through the Use of Transparent Model Alloy Systems--
R I C H A R D N. GRUGEL AND ROHIT TRIVEDI 393

Some Failure Analysis Case Histories in Galvanized Steel Products--


E D W A R D LARKIN AND MEHROOZ ZAMANZADEH 414

Characterization of Reaction Between Cast Titanium and Silica-Containing


Investment M o l d - - H E R B E R T J. MUELLER 429

Author Index 447

Subject Index 449

VII

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STP1165-EB/Jun. 1993

Overview
The ongm o f metallography is traced generally to the ploneenng efforts of Henry Chfton
Sorby, gifted British amateur soentlst, who m 1863 made the first observation of the micro-
structure of a pohshed and etched metal speomen. However, the mdustnal and soentlfic
world greeted this development with indifference and nearly 25 years passed before others
began to budd upon Sorby's work.
The growth of the steel industry after the Cwd War, spurred by developments such as the
Bessemer converter and the open hearth furnace, transformed technology and sooety. But this
growth could not be accomphshed without development of the soence of metals. Techniques
such as metallography made th~s possible
ASTM Committee E4 on Metallography was founded m 1916, 53 years after Sorby's lmtlal
observatmn of m~crostructure. Prior to that, ASTM had one committee, E 1, that covered all
methods of testing of metals and alloys and only one standard, E 1, containing two pages
devoted to metallography. It was recogmzed that more work needed to be done and a new
committee, E4, was formed for this purpose.
This symposmm, held on 8-10 May 1991, commemorates the 75th anmversary of com-
mittee E4 F~ttmgly, ~t was held m Atlantic C~ty, where ASTM met annually for many years,
up to about 1970
Committee E4 has been a leader m developing metallographlc test methods. Th,s has been
accomphshed by the combined efforts of hundreds of volunteer members over the past 75
years The enclosed historical rewew of E4 hlghhghts the techmcal achievements and the hves
of many of the responsible E4 members Putting together this history was difficult and it prob-
ably is imperfect. However, it does show the importance of drawing talented metallographers
into E4 actwmes
Many of the papers m th~s book discuss the historical developments of specific areas m met-
allography Knowledge of the past ~s important, not s~mply to maintain our perspectwe, but
as a foundation for growth. Too often, we ~gnore the past and find that we are merely rede-
velopmg what others have done before and, perhaps not as well

George F. Vander Voort Samuel M. Purdy


Carpenter Technology Corporatmn, Reading, PA Nattonal Steel Company, Trenton, MI 48183,
19612, symposmm cochmrman and coed,tor symposmm cochalrman and coedltor

Francis J. Warmuth Albert Szirmae


Cameron Forge Company, Houston, TX 77251, U S Steel Corporation, Monroevllle, PA 15146,
symposium cochmrman and coed~tor symposmm cochalrman and coedltor

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George F. Vander Voorf

The History of ASTM Committee E4 on


Metallography
R E F E R E N C E : Vander Voort, G F, "The History of ASTM Committee E4 on Metallography,"
Metallography Past, Present, and Future (75th Anmversary Volume), ASTM STP 1165, G F
Vander Voort, F J Warmuth, S M Purdy, and A Szlrmae, Eds, American Society for Testing
and Materials, Phdadelphla, 1993 pp 3-79

ABSTRACT. Organized on 10 October 1916 to estabhshed standard magnifications for micro-


graphs, Committee E4 has branched out into many different areas, far beyond its mlhal scope,
m the process producing forty-two standards, twenty-five STPs (this is the twenty-fifth), five
ASTM presidents, two other ASTM Committees, and the Joint Committee on Powder Dlffrac-
tmn Standards The committee has met 138 times, not counting separate task group meetings
ASTM E4 standards are used by many other countries, ezther m full, or m part As with all ASTM
committees, E4's members are volunteers Whatever success E4 has had is due to these volun-
teers and the support of their orgamzatmns

KEY WORDS: metallography, history, standards, testing

ASTM E4 on Metallography, organized on 10 October 1916, grew out of Committee E 1 on


Methods of Testing (as is true of many other E committees) At that time, standard E 1-16
(Standard Methods of Testing, originally adopted in 1910) consisted of five parts, the last enti-
tled "Methods for Metallographlc Tests of Metals" requlnng somewhat less than three pages.
The organizational efforts were chaired by Edgar Marburg, ASTM's Secretary-Treasurer, who
died m 1918
At that time, it was perceived that there was a need to estabhsh standard magmficatmns for
mlcrographs and that this work would be best performed by a new standing committee This
new group was called Committee E4 on Magnification Scales for Mlcrographs Actually, there
had been an earher committee called E4 on Methods of Samphng and Analysis of Coal, which
was disbanded m 1915 and there also was a &sbanded E3 at the time Hence, we could have
been known as E3 on Metallographyjust as easily as E4. At any rate, the original E4 name did
not last long because the members reahzed that the estabhshment of standard magnifications
was a simple task and many more complex problems needed to be solved. Subsequently, m
1920, the members decided to change their name to Committee E4 on Metallography, and
this name has been used since 1921 E4's original fifteen members, not counting Marburg,
hsted two ASTM presidents, Dr Henry Marion Howe, the dean of American metallurgmts at
that time, and George Kamball Burgess, famed director of the National Bureau of Standards
Howe was a founder of ASTM, his name is the first hsted on the charter, and he was the first
(and third) ASTM president serving a total of four years Burgess was ASTM's fourteenth
president
E4, as with all volunteer groups, has had its share of successes and failures History walljudge
E4 based mainly on its tangible accomphshments These can be viewed in several ways. Issu-

Supervisor, Materials Characterization, Carpenter Technology Corporation, Reading, PA 19612

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4 METALLOGRAPHYPAST, PRESENT, AND FUTURE

ance of standards is an obvious yardstick. E4 has published forty-two standards Of these,


seven were discontinued (six of these were replaced by newer documents), five were transferred
to other standing committees, and thirty are now active Another good yardstick is symposia,
particularly those subsequently published E4 has sponsored or cosponsored numerous sym-
posia since 1936 and these have generated twenty-five special technical pubhcatlons (see list).
Two other E committees, E7 on Nondestructive Testing and E37 on Thermal Measurements,
were spun offE4, and they have been highly successful E4 members started the highly sigmf-
icant work of the Joint Committee on Powder Diffraction Standards, JCPDS, in Swarthmore,
Pennsylvania, and four E4 members have been officers of this organization Four E4 members
have served as vice president and five as president of ASTM and eight others have served as
directors or as members of the executive committee Thirteen E4 members were made hon-
orary ASTM members and thirty-four have received the Award o f Merit (five were made Fel-
lows prior to creation of the Award of Merit) Naturally, some of these men were also active
on other committees. The accompanying tables list E4 award winners E4 members have been
active in other societies, for example, nine E4 members have been presidents of the American
Society for Metals
It is more difficult, however, to gage how well E4 has served the metallographlc needs of
industry. Has E4 met the needs of the metallographic community in a timely fashion9 Have
other groups done a better job9 Has E4 led the way in standards development compared to
other technical societies, here or abroad, or industrial companies9 These are tough questions
to answer, but a little soul searching is necessary at times In general, we would conclude that
E4 has done a very good j o b overall as ASTM metallographic standards are the most widely
used in the United States, and many other countries have followed our lead No doubt we
could have been faster in many of our tasks. O f course, this is a totally unbiased, highly precise
evaluation, based upon a massive survey (of one) vBut, as Paul Harvey says, let's hear"the rest
o f the storyV"
E4 has met at least 138 times since its formation. This May's meeting was the thirty-first in
Atlantic City, New Jersey, the last being in June o f 1971 Philadelphia, New York, Pittsburgh,
and Chicago were the next most frequent meeting sites with 16, l 0, 9, and 8 visits, respectively
E4 membership (Fig 1) grew steadily over the years reaching Its peak in 1979 with 161 mem-
ben's. Since then, membership has been declining steadily These numbers are somewhat
deceptive as some of the members were consultants (nondues paying) and for the past ten years
we have been purging the roster of members who do not return ballots. Membership is
rebounding, however, due to recruiting efforts and new E4 activities However, compared to
the peak years, E4 has had a reduction in active meeting participants, although we have again
rebounded in this area
Despite a general drop In membership since 1979, Fig 2 shows that E4's standards devel-
opment effort has not decreased, but increased In 1979, E4 had 15 active standards In the
last eleven years, this number has doubled to 30 (see E4 Standards at a Glance) Prior to 1979,
E4 had developed twenty-four standards but nine were either transferred to other committees,
discontinued, merged with another, or replaced Since 1979, seventeen new standards have
been developed, one was transferred and one was replaced by a new standard Either way, the
past eleven years have been highly productive despite the loss of E4 membership

E4 Officers
Only thirteen people have chaired E4 (see officers list), largely because LeRoy L Wyman,
Sr. held the chairmanship for 28 years (1938-1966), an ASTM record E4 was not the only
committee W y m a n chaired W y m a n certainly qualified as a full-time, unpaid ASTM

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VANDER VOORTON HISTORYOF COMMITTEEE4 5

200

150

~100

50

0 I I I I I I I I
1910 1920 1930 1940 1950 1960 1970 1980 1990 2000
Year
FIG. I --Graph of Committee E4 membership.

35
30

ii i i i i i.i!i.i.i.ii.i..i.i.i..i.i..i..i.i.i..i.i
25
.a 20
E
Z
15

10

.............. j ......... ~ ...............................................................................................................................................................

I I I I I I I I
0
1910 1920 1930 1940 1950 1960 1970 1980 1990 2000
Year
FIG. 2--Committee E4 active standards.

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6 METALLOGRAPHYPAST, PRESENT,AND FUTURE

employee v More recently, E4 chairmen have been restricted to no more than two consecutive
two-year terms.
There have been thirteen E4 secretaries, the first elected in 1921 Three people held this
position for long p e r i o d s - - M a r y R. Norton (20 years), John J Bowman (ten years), and
George F. Comstock (nine years) In 1936, E4 appointed its first vice chairman, Dr Marcus
A Grossman, who held the position for eight years Grossman was internationally recognized
for his work on hardenabdlty He was followed by R Earl Penrod who held the position for
twenty years Wyman, Penrod, and Norton ran E4 for about a third of its existenceV E4 also
has the unique distinction o f having father and son chairmen, William D Forgeng, Sr and
J r , serving with only a two year interval between them
E4 appointed its first second vice-chairman in 1972 and eight people have held this position
for either two- or four-year terms Our first membership chairman was appointed in 1964 and
eight people have served in this capacity The accompanying table lists all of the past E4 officers
and their terms of office

E4 Subcommittees
E4 created fifteen techmcal subcommittees with the first started m 1920. Roman numerals
were used to number subs up until 1970, since then Arabic numbers have been used. 2 Only
eight subcommittees are now active, mainly due to mergers
Sub 1 on Sample Selection and Preparation and Photography was formed in 1920 as Sub I
on Preparation of Metallographic Specimens Its name was changed twice, in 1921 and 1988,
the latter due to the merging of Sub 4 on Photography into Sub 1 When many people think
of metallography, they think of Sub l's domain first Indeed, Sub l's activities have been
always a focal point of E4 concentration Sub 1 has prepared the greatest number of standards
and hasjunsdictlon over eight active standards, the most of any E4 subcommittee Sub 1 has
had ten chairmen with one person, Sam Purdy, serving during two different time periods for
a total o f 23 years (and still going strong!) The list of Sub 1 chairmen (see list of all subchalr-
men) is very impressive.
For many years, standard E 2 (Preparation of Mlcrographs of Metals and Alloys) guided
metallographers but it was discontinued In 1983 at the age of 66 The original version, intro-
duced in 1917 (they were offto a good start), was written largely by William H Bassett (Ana-
conda Wire and Cable). E 2 contained grain size measurement information, which really was
inconsistent with the specification title, until 1949, when this information was removed and
incorporated into new standard E 79 E 2 also had the first grain size chart for copper, added
in the 1930 revision This chart was developed by Edgar H Dlx, J r , Francis F Lucas, Henry
S. Rawdon, and Charles H Davis The actual mlcrographs were prepared by Davis and his
staffofthe American Brass Co in Waterbury, Connecticut
Standard E 3, Preparation o f Metallographic Specimens, has been one of the most Impor-
tant E4 documents In the early days of this century, there were few, if any, compilations of
preparation procedures and etchants. E 3, prepared largely by Henry Marion Howe, pulled
much of the existing information together, and this has been continually updated William
Campbell and George F. Comstock also contributed to E 3 (and also E 5, which was merged
into E 3 in 1935) as did E. C. Groesbeck of the then U.S. Bureau of Standards and a developer
of selective etchants [ 1]
In 1928, Sub l introduced metailographers to the use of Bakehte (phenolic plastic) for
mounting specimens. Later, in 1938, LeRoy L. W y m a n presented a detailed report on the use

2 In this text, 1 wdl used Roman numerals when referring to a sub and its actwltles before 1970 and
Arabic numbers for subsequent events

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VANDER VOORT ON HISTORYOF COMMITTEEE4 7

of plastics for mounting [2] In 1932, W y m a n had replaced Wllham E. Ruder as General Elec-
tric Research Laboratories representatwe, thus beganmng a long, productive assocmt~on
Throughout the 1920s and 1930s, Sub 1 was constantly searching for sources of good cloths
for pohshmg W y m a n reported [3] that due to fashion changes m the 1920s, "kitten-ear"
broadcloth, a very popular pohshmg cloth, had become unavailable W y m a n canvassed the
garment district of New York City for possible subsUtutes E4 members tried these but without
success Eventually, they persuaded the Horne Co of Pittsburgh to produce k~tten ear for met-
allographers ASTM was conwnced to order huge rolls ofth~s cloth which was sold to metal-
Iographers at cost. After several years m the pohshmg cloth business, a newly formed metal-
lographlc supply house took over th~s function. Kitten-ear cloth is stdl commonly used for
final pohshmg, particularly for soft metals where scratch removal is particularly difficult
W~th each rews~on, standard E 3 grew and grew, from the mmal thirteen page 1921 version
to a s~xty-s~x page document m 1958. At this time, it was felt that E 3 was becoming cumber-
some Information on macroetch and m~croetch composmons and uses was removed from E
3 and used as the basis for new standards E 340 and E 407, respectwely In 1980, E 3 was
reduced to coverage of mechamcal pohshmg alone. Subsequently, E 1180 was written expand-
mg upon the brief description of sulfur printing found m E 3 up to 1980. The electropohshmg
mformahon m E 3 up to 1980 has not yet emerged as a new standard, but thas work is again
mowng forward
Sub l developed standard E 381, building upon ASTM A 317 (Macroetch Testing and
Inspection of Forgmgs), to describe classaficatlon and interpretation of macroetched sectaons
cut from wrought ingot-cast material (blooms, billets, and bars, for example) This is a general
purpose standard that complements other special purpose standards, for example, A561 and
A 604 Continuous casting has become increasingly popular due primarily to cost sawngs
Steels made by th~s process may be evaluated for macrostructure m the as-cast condmon,
unhke ingot cast material, or after hot reduction. The existing E 381 macroetch classification
charts are not really useful for continuously cast steels, particularly fftested m the as-cast con-
dmon An extenswe effort has been underway for several years now to expand E 38 l's
coverage
Another recent effort of Sub 1 has been the development o f E 1351 which describes how to
make and evaluate rephcas made m the field to estimate the remaining hfe of steam p~pmg m
power plants This standard began hfe as an emergency standard, ES 12, E4's only emergency
standard Thas approach was taken as a result of a serious accadent due to fadure of a mare
steam lane Many power plants are now at or beyond thear original design hfe Assessment of
the remnant hfe of components subjected to many years of h~gh temperatures and pressures
has rehed upon examination of mlcrostructural evolution and the formation and growth of
creep cawt~es under these operating condmons. Almost overnight, numerous people were
revolved m such evaluations, and there was an obvious need to standar&ze the procedures.
Sub 1 was approached by members o f the power generation industry to tackle thas problem
and they responded swiftly wath a h~ghly useful document
Sub 1 as now workmg on preparataon methods for thermally sprayed coatmgs These coat-
rags are used on a variety of products, for example, mrcraft engine components The m~cro-
structures tend to be rather heterogeneous and porosity is generally present Specimen prep-
aratlon can bade the porosity, or exaggerate ~t, depending upon the parameters chosen
Standard procedures are needed to insure that the true m~crostructure ~s revealed, otherwise
any evaluataon or measurement will be incorrect.
Sub 2 on Metallographlc Terminology and Nomenclature of Phase Diagrams was formed
m 1920 Originally, defimtlons were to be incorporated into standard E 2 and s~xteen terms
were first defined and balloted. However, only eleven of these made ~t through the ballot pro-
cess and a separate standard, E 7, was issued m 1924. It was soon noted that E4 on Metallog-

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8 METALLOGRAPHYPAST, PRESENT,AND FUTURE

raphy had forgotten to define metallography so this term was added in 1926, but the definmon
was revised m 1927.
Henry C Boynton was Sub II's first chairman and Professor Arthur Phdhps (see biography)
of Yale Umverslty was the second Inmally called Sub II on Nomenclature and Definmons, it
was mactwe through most of the 1930s. Reactivated under Dr. Robert S Wdhams of Mas-
sachusetts Institute of Technology m 1939, it stayed active only two years as he recommended
against revis~ons to E 7
In 1946, efforts were made to revise Sub II, but nothing happened until 1948 when Dr Paul
A Beck ofthe Umversity of Notre Dame (later the Unwerslty ofllhnois) was appointed Chair-
m a n The sub was renamed Sub II on Definitions and Beck started a massive effort to turn E
7 into a comprehensive terminology standard Beck created a long list of potential terms and
turned this work over to Dr. Robert S Busk o f Dow Chemical Co. Nearly a thousand terms
were considered. In 1955, E 7 j u m p e d from twelve definitions to a forty-five page document
with 750 defimtlons.
After this massive effort, Sub II became inactive m the late 1950s until 1966 when Mary R.
Norton of Watertown Arsenal became chairman. She worked with then Committee E8 (on
Nomenclature and Definmons) to add metallography terms to the new ASTM glossary and
also with members of new Committee E25 (on Microscopy) to compare definmons for the
same terms in E 7 and in their terminology standard, E 175. This revealed twenty-three defi-
rations with &fferences to be reconciled, which was done Since 1955, there have been at least
thirteen additional revisions of E 7 revolving refinements to definmons, deletions of obsolete
terms, and addmons of new terms, for example, on electron metallography and ~mage analysis.
More recently, Sub 2 has been working on adding symbol and acronym secuons Beth Knuep-
pel is the current chairman of Sub 2.
Sub 3, formed m 1920 as Sub l l l o n ThermalAnalysis, has had an interesting history In
1920, E4 recommended to A S T M that a standard committee be formed on pyrometry as this
was too far outside the scope of E4 While temperature measurement per se was considered
too far afield, the interpretation of cooling curves and thermal arrests were not In the early
days of metaliography, one of the chief act~vmes was the construction of eqmhbnum phase
dtagrams and thermal analyses (both heating and cooling) was a major tool for such work
The first chmrman o f Sub III was George Kimball Burgess, director o f the U S Bureau o f
Standards who was replaced, after a few years o f mactwlty, by W d h a m E Ruder of General
Electric Co. Ruder and his subcommittee produced standard E 14 m 1925. This standard was
revised five times and then transferred to new Committee E37 (on Thermal Measurements)
m 1978 Howard Scott took over Sub III m 1928 but actwlty stopped by 1933.
In 1949, this committee was reactivated as Sub I I I on Nomenclature under Dr. Paul A
Beck Its goal was to establish a system of nomenclature for alloy phases in binary and more
complex systems The development and construction of eqmhbrlum phase dmgrams was not
standar&zed and the naming of phases was performed erraUcaUy. Beck pulled together a sub-
committee consisting of the major American and British experts on phase diagrams (not all
were ASTM members, h o w e v e r ) - - K W. Andrews, Max Hansen, W d h a m Hume-Rothery, F.
Laves, Taylor Lyman, John S. Marsh, G. V Raynor, Frederick N. Rhlnes, Cyril Stanley
Smith, and Arthur J. C. Wdson, besides knowledgeable E4 members such as Robert S Busk
and W d h a m L. Flnk. The latter became the subchmrman in 1960 and held this poslUon until
1978
This work, started by Beck and continued by Flnk, resulted m a new system [4,5] of alloy
phase nomenclature described in standard E 157, introduced in 1961 The SUbcommittee then
began work on rules for drawing phase diagrams suitable for publication This resulted m stan-
dard E 391 in 1969 Since then, aside from revisions to E 157 and E 391, which have been
minor, there has been no activity in this area and Sub 3 was merged into Sub 2 in 1988

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VANDER VOORT ON HISTORY OF COMMITTEE E4 9

S u b IVon Pkotograpky was also estabhshed m 1920 V H Blhlman was the first chmrman,
followed by Henry S Rawdon and Leon V. Foster, each of whom served for long periods (12
and 17 years, respectively) Foster developed the well-known, very popular calcite prism polar-
lzer used on Bausch and Lomb metallographs Sub IV developed photomlcroscopy reforma-
tion that was Incorporated into standard E 2. The mtroducUon of E 883 m 1983, which was a
massive updating of the photographic reformation formerly m E 2, led by Fran Warmuth,
resulted in the withdrawal o f E 2
One of Sub IV's most slgmficant achievements was the sponsorship of the annual ASTM
photographic contest which started m 1936 but ended with the 1980 contest The decision to
stop the society-wide annual meeting made it very difficult to run the contest. Sub IV also held
a symposmm m 1948 on the use of color m photomlcroscopy (STP 86) At that time, such use
of color was m its infancy, and the symposium demonstrated the value of color After the issu-
ance of E 883, and the demise of the annual photographic contest, Sub 4 activity waned In
1988, Sub 4 duties were taken over by Sub 1
S u b 5 on Microindentation Hardness Testingwas created m 1923 as Sub V on Micro-Hard-
ness to evaluate the scratch hardness instrument developed by C H Blerbaum, an E4 mem-
ber Henry S Rawdon chaired the committee The method was found to be useful only m a
comparative manner to show &fferences m hardness between &fferent constituents [6] As no
other m~crolndentat~on eqmpment existed at that time, the sub was disbanded m 1927
Instrumentation, using both Knoop and Vlckers type indenters, was developed starting m
the late 1930s prompting E4 to reactivate the committee, now Sub V on Mlcrohardness, m
1948 under Alexander Gobus A round robin (the first of many) was lmtlated m 1950 to eval-
uate instruments At the request of Sub V, Bausch and Lomb developed a new stage m~crom-
eter m 1950 w~th 0 02 u m accuracy
Walter A. Shebest of the Frankford Arsenal took over Sub V m 1955 and the round robin
continued After a period ofmactwlty, Larry Toman, Jr. took over Sub V in 1965. One of his
first tasks was to define m~crohardness. Today, E4 tries to &scourage use of this term although
its use ~s thoroughly ingrained. Mlcrohardness, at face value, suggests a very small hardness,
which is not the retention. These tests produce a very small indentation due to application of
a rather low load, to determine the same hardness number (hopefully) as obtained using a bulk
test w~th a much h~gher load and much larger indent Consequently, the preferred term ~s
m~cromdentat~on hardness testing.
T o m a n and Sub V issued standard E 384 m 1969 to cover Knoop and Vlckers micromden-
tat~on hardness testing In 1975, the symbols HV and H K were adopted m preference to the
original VHN (or DPN) and KHN. Another round robin was begun m the late 1970s, but it
was dropped after only four laboratories completed the tests It was apparent that the approach
used was too complex The results appeared to show that most of the vanabd~ty of test results
occurred m the measurement of the indents, rather than m making the rodents
Yet another round robin was begun m the early 1980s Seven test blocks, three ferrous and
four nonferrous, were indented by one person using five rodents at each of six loads, with both
Knoop and Vlckers indenters The ferrous and nonferrous test specimens were separated and
sent to d~fferent compames Twelve people measured the rodents on the nonferrous specimens
and fourteen people (twenty-four &fferent people m all) measured rodents on the ferrous spec-
imens Tony DeBeihs tabulated all of the test results, but analys~s work was slow m coming
This writer agreed to evaluate the ferrous data After this was done, and the nonferrous data
were stdl untouched, I again volunteered. The results [ 7,8] of this round robin 0ts origins can
be traced back at least to 1972) were used to prepare a detailed precision and bins section for
E 384 Frank Toye is the current chairman of Sub 5
S u b 111 on X-Ray Crystal Analysis was started m 1924 The eminent metallurg)st Zay Jef-
fries was its first chmrman. Jeffnes [9] became interested m the new field of X-ray &ffractlon

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10 METALLOGRAPHYPAST,PRESENT,AND FUTURE

after World War I when acting as a consultant to the Cleveland Wire Co. of General Electric
Co He hired a young metallurgist, Edgar Colhns Barn [ 10] (who later gained fame and fortune
with the United States Steel Corp ), to evaluate these new techniques
The mmal work of Sub VI consisted of introduction of standard E 15 (Radiographic Testing
of Metal Casting) written by Horace H Lester of the Watertown Arsenal in 1926, pubhcatlon
of a glossary of X-ray metallography terms [11] prepared by Louis W McKeehan of Bell Tele-
phone Laboratory (later at Yale University), and issuance of a superb review paper [12] on the
current status of X-ray metallography (prepared by Jeffries, Lester, McKeehan, and Bain).
In 1931, the name was changed to Sub VI on X-Ray Methods and in 1933 Dr Robert F.
Mehi of the Carnegie Institute of Technology (now Carnegie Mellon University) became chair-
man Mehl played a dominant role in the founding of the science of physical metallurgy His
mare contribution as an E4 member was the organization of E4's first symposium, held on 2
July 1936, on Ra&ography and X-Ray Diffraction Methods which became E4's first STP (STP
28) At that time, X-ray diffraction was unlocking the secrets of metal crystals It was the first
really powerful tool for studying the internal structure ofcrystalhne materials
In 1937, E4 recommended that a separate standing committee be formed to cover the
inspection aspects of X-ray methods, that ~s, ra&ography. Subsequently, E7 on Radiographic
Testing (now E7 on Nondestructive Testing) was founded [13] in 1938 under the chairman-
ship of Horace Hardy Lester Standard E 15 was transferred to E7 in 1939
Wllham L. Fink of Alcoa took over Sub VI in 1938 and continued as subchalrman until
1960 Under Flnk, standards E 43, E 81, and E 82 were developed. In 1940, Sub VI began
perhaps their greatest task, the estabhshment of a center for information on diffraction meth-
ods for chemical analysis In 194 l, they began work with an X-ray diffraction group of the
National Research Council providing the technical expertise and personnel to start a file cat-
alog of materials already Identified by X-ray diffraction Within a year, 250 sets of X-ray file
cards with 3936 entries had been prepared
This effort spawned the Joint Committee on Powder Diffraction Standards (JCPDS), in
Swarthmore, Pennsylvania, now jointly cosponsored by a number of organizations worldwide
[14] Their function has been to collect, edit, publish, and &stnbute powder diffraction data.
Solids were first studied by X-ray diffraction m 1912 and A W Hull (General Electric Co )
reported the need for a database of diffraction patterns in 1919 Hull demonstrated the unique
nature of each crystalhne substances diffraction pattern, which did not change, even when sev-
eral substances were mixed together Development of a diffraction pattern file was hampered
by the fact that they were recorded on a photographic negative A classification scheme for the
films was developed in 1936 and pubhshed [15] in 1939 by Joseph D. Hanawalt, Harold W
Rinn, and L K Frevel of Dow Chemical Co This paper began the cataloging effort as dif-
fraction patterns for a thousand substances were tabulated
Sub V I and the National Research Council (NRC) formed a joint committee, joined shortly
by the Institute of Physics of Britain who supplied a number of diffraction patterns NRC was
replaced by the American Society of X-Ray and Electron Diffraction (now the American Crys-
tallographic Society) and other groups have since joined JCPDS was housed initially at the
Pennsylvania State Umverslty m the office of E4 member and first JCPDS chairman, Dr
Wheeler P Davey It has been located m Swarthmore since 1970
The original method for searching the database has changed somewhat as the files have
grown Hanawalt revised his original method to one based on the three strongest peaks This
was later modified by William L Fink to a system of ordenng and reordering of the eight
strongest peaks. As the files continued to grow, hand searching became te&ous and other
methods [16-18] have been tried, for example, visual comparative search systems Despite the
magnitude of the file now, the information can be obtained in pnnted form and on microfiche
X-ray diffractomers can be equipped with the entire powder &ffraction file on a CD-ROM for

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VANDER VOORT ON HISTORY OF COMMITTEE E4 11

rapid computer searching. Besides JCPDS's massive effort to collect diffraction data published
worldwide, it also evaluates the quality of the d a t a - - a challenging task) E4 members Wheeler
P Davey, William L Fmk, LeRoy L Wyman, and Andrew W Danko have served as chair-
men and/or general manager of the JCPDS
Not all of Sub VI's efforts have been this successful In 1942, standard E 43 covering the
Hanawalt method for identifying substances by X-ray diffraction was issued It was intended
to be a companion to the newjoint committee powder diffraction database E 43 was revised
twice, In 1946 and 1949. Thereafter it was under a constant state of revision, even up to seven
years after it was withdrawn (in 1961) The subject was considered to be too complex for a
standard, and a book was started but never completed
More recent years have seen the development of an X-ray diffraction standard for measunng
the retained austenlte content of steels, written mainly by Robert W Hinton of Bethlehem
Steel Corp, and issued in 1984 Since then, activity has decreased and Sub 6 became Inactive
m 1987, then merged into Sub 11
S u b V I I on R e c o m m e n d e d Practice for Dilatometric Analysis was formed in 1938 with
LeRoy Wyman, Chairman of E4, as subehalrman as well Laurence H Carr (Edward Valves,
Inc ) took over from Wyman m 1940 and ran Sub VII for the next eleven years during which
E 80 (Dllatometrlc Analysis of Metalhc Materials) was developed and issued in 1949 E 80 was
reapproved but not revised through 1978 when jurisdiction was tranferred to new committee
E37
Donald I Finch of Leeds & Northrup Co took over Sub VII in 1951 and ran it for the next
nineteen years During his tenure, E 189 (Determining Temperature-Electrical Resistance
Characteristics of Metalhc Materials) was developed and issued in 1961 As with E 80, it was
transferred to E37 in 1978
S u b V I I I on Grain Size was a long time in formation as grmn size measurement procedures
were part of E4's first standard in 1917. Although E4 always has been active in the area of grain
size measurement, it was 1931 when a separate committee was estabhshed. This work was
assigned to a Special Committee on Grain Characteristics, rather than a subeommlttee, and
Clarence J Tobin of General Motors Research Laboratory was its chairman Their first effort
was to develop a procedure for assessing the grain growth characteristics of a given heat of steel
The method chosen was the McQuaid-Ehn carbunzlng test originally developed to assess the
smtablhty of a low-carbon steel for carburlzlng Harry McQuaid of Repubhc Steel Corporation
was a consulting member A chart was developed depicting the hypereutectold and hypoeu-
tectold regions of the carbunzed case of specimens with different grain sizes, and the method
and chart were issued as E 19 in 1933
In 1937, Dr Marcus A. Grossman took over the Special Subcommittee which became S u b
VllIon Grain Size m 1938 Although E 19 was an important development, and the orlgmal
chart was claimed to be a result often years effort, the chart was widely criticized as inaccurate
and was under constant revision up to 1961 when it was withdrawn Grossman formed three
separate groups under Sub VIII Group A was to revise E 19 and he headed it Group B was
to develop a ferrlte grain size rating method and was headed by R Earl Penrod Group C was
to develop methods for nonferrous alloys other than copper and was headed by Carl H.
Samans of Standard Oil Company of Indmna H P George (Dept. of the Army, Frankford
Arsenal) took over Group C in 1951 and Penrod replaced Grossman after he died in 1952
Their work resulted m three new standards, E 79 issued in 1949, E 89 issued in 1950, and E
91 issued m 1951. E 79, however, was for copper-based alloys and was largely the grain size
reformation stripped out ofE 2 This work revealed and confirmed comments from members
that gram size analysis was basically a problem of geometry and a single standard could be
developed [19,20] for all alloys. For comparison ratings, it would be necessary to have charts
developed that were realistic depictions of true structures. E 112 grew from these ideas and

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12 METALLOGRAPHYPAST, PRESENT, AND FUTURE

replaced E 19, E 79, E 89, and E 91, the latter three having rather short lives The only grain
size chart that survived was the copper chart orE 79, but it too was modified Today, E 112 is
one of the most widely cited ASTM test methods. Nothing, of course, is sacred E I 12 has been
revised eleven times in its thirty-six year history, with a twelfth underway. The most significant
revision to E 112 occurred in 1974 when the three-circle intercept procedure, developed by
Dr Halle Abrams [21] of Bethlehem Steel Corp, was added along with a statistical evaluation
procedure to assess the quality of the measurement
While E 112 contains extensive reformation about grain size measurement procedures, the
most commonly used method is the chart comparison procedure Numerous approaches have
been suggested For example, the appropriate chart can be placed on the wall and the operator
examines the structure through the microscope eyepieces and then looks up at the chart. Ret-
icles can be also prepared depicting portions of the grain size pictures, and these can be super-
imposed over the image viewed through the eyepieces Clear plastic templates of the gram size
photographs can be placed over a projection screen Charles H Davis described [22] a projec-
tion box device produced for the Bausch and Lomb Euscope for grain size rating Frederick
C Hull of the Westinghouse Research Laboratories improved the comparison rating approach
revealing factors that affect its precision and developing correction factors for using alternate
magnifications [23]
E 112 is used for rating the grain size of equlaxed grain structures It has some guidance,
currently being improved, for measunng deformed grain structures However, other situations
exist that are not covered. In certain metals and alloys, we sometimes observe a few grains,
generally widely scattered, that are far larger in size than the rest of the grains. E 930, on the
ALA (as large as) method, describes how to measure these "rogue" grains E 930 was written
by Robert Sleplan and Fran Warmuth It is also possible to have larger amounts of these
mixtures, and a number of such patterns can be observed. Such specimens exhibit a non-Gaus-
sian distribution of gram sizes and are referred to as blmodel or duplex. E I 18 l, written by
Jeremy P Morse [24] covers these situations Fran Warmuth is the present chairman of Sub
8
Sub I X on Inclusions was formed in 1940 and was chaired for twenty-five years by Samuel
Epstein of Bethlehem Steel's Research Department until he retired. His six successors have
served for the following twenty-six years Al Brandemarte is the current Sub 9 chairman.
Epstein had developed an Inclusion measurement method m his previous job at Battelle
[25] Standard E 45 was issued in 1942 containing a chart rating method based on Swedish
work and the nonchart method developed by Epstein. In 1960, a second chart method was
added based on work by Walker [26] and two years later, the third chart was added, the mod-
ified J-K chart for steels with low inclusion contents. E 45 is also a widely referenced standard
and it has been revised nine times
Sub IX also developed a standard practice for detecting large inclusions in beanng steels by
ultrasonics [27], E 588 It was transferred to E7'sjunsdlCtlOn m 1984 Sub 9 is presently eval-
uating the electron beam melt button test for rating the inclusion content of superalloys
Sub X was not one of E4's big successes, either time it existed Formed first in 1949 as Sub
X on Decarburization, the sub members worked with the Society of Automotive Engineers
(SAE) and the American Iron and Steel Institute (AISI) to develop a measurement method,
but no E4 standard resulted, activity stopped m 1952, and Sub X was disbanded m 1956 In
1968, it was reborn as Sub X on Research. Whatever the original purpose was, nothing of sig-
nificance apparently resulted, and Sub X was again disbanded Sub X has two strikes against
it, but it has not yet gotten to bat for a third time
Sub X I on Electron Microstructure o f Steels was formed m 1949, and its name was changed
seven times m the next thirty-nine years, an E4 record Sub I 1 has had also the most chawmen,
eighteen since 1950, another E4 record Sub I l has also taken over the work of three other E4

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VANDER VOORT ON HISTORY OF COMMITTEE E4 13

subs, Subs 6, 15, and 16 Sub 11 has also sponsored more symposia and published more STPs
than any other E4 sub It has not been as prolific in developing standards, however, as it has
only developed two (E 766 and E 986, both written by Dave Ballard of the National Bureau
of Standards).
Sub I l had its origins at the 1947 annual meeting of the Electron Microscope Society of
America (EMSA) where discussions were held among transmission electron microscope
enthusiasts working with metals. They formally organized a group on 13 February 1948 and
then merged their group into E4 in 1949 Their first subchalrman, George E Pelhssier of U S
Steel C o r p , was appointed in 1950 They were a fairly large, very active group and published
seven detailed annual subcommittee reports in the 1950s before concentrating mainly on sym-
posia for this purpose
Electron microscopy was a hot topic in 1950 as the TEM provided at least an order of mag-
nitude increase in resolution over the light microscope at that time At that time, metal struc-
tures were only examined using replica methods, and Sub XI did outstanding work in devel-
oping these procedures Later, when thin foil methods were developed, Sub XI again played a
major role in developing this method Sub XI also produced a very popular manual on TEM
techniques, STP 547
While their initial work centered on ferrous alloys, Sub XI started a B group on nonferrous
alloys in 1954, the same year they published their first symposium as STP 155 A C group on
super strength alloys followed in 1956, and so did the STPs, STP 245 and STP 262 In 1960,
the C group topic was Electron Mlcrostructure of PH (precipitation hardened) AustenItic and
Ni-Based Alloys, a very active group A group on Electron Diffraction followed in 196 l, and
another STP, number 317. The electron microprobe analyzer was introduced and Sub XI got
interested A round robin was conducted on 316 stainless steel with Committee A l 0 .
In October of 1966, Sub XI formed a task group (number 6, numbers being used now) on
the Analysis of Extracted Phases in Superalloys under Matthew T Donachle, J r , of Pratt &
Whitney Aircraft. This group became a special task group, TG 001, in 1968, then in 1975 a
special subcommittee, E04 91, then in 1977 it became the only task group of a new subcom-
mittee as E04 16 0 l, then Sub 16 was merged back into Sub I l in 1983 and it was again a Sub
I l task group, completing a grand swing through E4V On the way, they did issue (in 1983) a
very fine standard, E 963, which describes a method for extracting second phases from NI-
based superalloys This T G was exceptionally active over the seventeen years, some of the
results of their round robins are described in Refs 28 and 29
Another very active task group was T G 1115 on fiber analysis, chaired by Kuldip Chopra of
ELKEM Metals Co. In the mid-1970s, there was a great deal of interest in contamination of
water and air by asbestos fibers However, there were no accepted methods estabhshed for sam-
piing water, or air, and then for identification There were Individuals performing such work,
for example, using polarized light examination, but the federal laws being passed would
require much greater testing, and many new laboratories would be doing such work New
approaches were being examined, for example, energy-dispersive spectroscopy (EDS) using
the relatively new scanning electron microscope (SEM) or electron diffraction (ED) using the
transmission electron microscope (TEM). Clearly, there was a need to establish standards. The
task group labored long and hard, but, alas, no ASTM standard was developed although a great
deal of insight was developed [30].
Sub 1 l's only standards (E 963 was written before Sub 16 was merged back into Sub 11)
have been in the area of scanning electron microscopy The SEM was commercially intro-
duced in 1965 and became an instant winner Dave Ballard of the National Bureau of Stan-
dards (now a consultant) wrote two standards, E 766 for SEM calibration [31] and E 986 for
SEM performance evaluation [32] In more recent times, Sub 11 has been conducting EDS
round robins, and a draft for a guide to energy-dispersive X-ray analysis (EDXA) has been

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14 METALLOGRAPHY PAST, PRESENT, AND FUTURE

wntten by Dr John J Friel o f P n n c e t o n Gamma-Tech, current Sub 11 chairman Frank Vel-


try of Inco Alloys International organized the round robin
E4 never had a Sub 12, no one seems to know why, and, Sub 13 has been always the name
of our evening dinner activities at meetings, so we wliljump to Sub X I V o n Quantitative Met-
allography formed in 1960 As with Sub XI, George E Pelhssier of U S Steel Corp was its
first chairman One of their first activities was to work with Committee A3 on the graphite
rating charts in A 247 Work in 1963 was successful in adding the nodular graphite senes chart
to A 247 George A Moore of the National Bureau of Standards (NBS) made some very early
quantitative measurements of these chart pictures using a computenzed system developed at
NBS Dr Moore was an interesting person, and Sub XIV meetings were never complacent
events when he was present Legally blind, Moore could see more with his limited vision than
many people with 20-20 visionI
Sub 14 has sponsored four symposia and published each, the last being held in May 1990
and dedicated to Dr Halle Abrams, long time member and former Sub XIV chairman who
died of a heart attack in October 1989 Halle had been involved in all four of E4's MiCon
(Mtcrostructural Control) conferences, and this was the fourth when he died Sub XIV's initial
efforts in quantitative metallography were in the domain of manual methods. Its first standard
was E 562 on the point counting method Manual methods have not been forgotten as auto-
mated methods have become popular [33,34] Sub 14 wrote a standard practice for measunng
decarburlzatlon, the original goal of Sub X when it first formed in 1949, and has a manual
approach (which can be automated) for assessing banded or elongated mIcrostructures
George Moore's efforts in the 1960s and 1970s to develop image analysis procedures for mea-
sunng structures, like inclusions, have been achieved in the last several years with three image
analysis standards, E I 122, E 1245, and E 1382 E 1122 describes an Image analysis approach
for obtaining J-K inclusion ratings according to methods A and D of E 45, a manual chart
method It is presently being pursued aggressively by image analysis manufacturers and steel-
makers E 1245 descnbes a stereological approach for measuring second-phase particles, such
as inclusions, and it too IS gaining interest in the market place E 1382 descnbes approaches
for measuring grain size using semiautomatic and automatic image analyzers and hasjust been
issued With these three standards, E4 has been leading the way, pushing the development and
use of image analyzers Hence, they have been better than timely)
Sub 14 has several projects underway A new task group was formed to explore evaluation
procedures for thermally sprayed coatings. Sub 14 is also trying to develop an image analysis
procedure for assessing the shape of graphite in cast iron and is working on an approach to
classify grain boundary carbide films in sensitized austenltic stainless steels In the equipment
area, Sub 14 is trying to develop a calibration test slide that could be used also to test out newly
written computer measurement programs for precision and accuracy George Vander Voort
is chairman of Sub 14
Sub X V on Emission Microscopy was formed in December 1968 with Dr Erwin Eichen of
Ford Motor Co as chairman This sub was to cover scanning microscopy while Sub XI would
cover transmission microscopy. The work on the SEM resolution standard, E 766, actually
began under Sub XV, but was completed under Sub 11 Sub XV did hold a symposium, pub-
hshed as STP 485 In 1977, Sub XV was merged back into Sub XI Sub 16on Phase Identi-
fication in Metal Alloys was established in November 1977 with Rick Anderson-Decina as
chairman The work on E 963, reported above, was moved under Sub 16 In 1983, when E
963 was issued, Sub 16 was merged into Sub l 1
Sub 17 on Laboratory Evaluation and Safety began as special subcommittee E04.94 on
Standard Recommended Practice for Evaluation of Metallographlc Laboratories on 14
November 1977 under chairman Fran Warmuth of Special Metals Corp (now with Cameron
Forge Co ) At that Ume ASTM was recommending the E committees to create standards gov-

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VANDER VOORTON HISTORY OF COMMITTEE E4 15

erning the evaluation of laboratones In 1981, this group became Sub 17, the same year that
they issued standard E 807 Sub 17 is now rewsmg E 807 and is working on a guide to labo-
ratory safety under Bob Nester.

Conclusion
Committee E4 has accomplished a great deal in its 75 years of voluntary service to the tech-
nical community Those accomphshments have come from the dedicated efforts o f m a n y indi-
wduals, both well known and not so well known, but all working together We need to remind
ourselves regularly of our goals so that we can continue to build upon the shoulders of these
grants of the past. There are still many worthwhde areas of endeavor for E4 activity despite
our past accomphshments

References
[1] Groesbeck, E C, "Solutions for Carbides, Etc, in Alloy Steels," Proceedings, American Society for
Testing and Matenals, Philadelphia, Vol 26, Part I, 1926, pp 569-571 and Vol 27, Part I, 1927,
pp 601-607
[2] Wyman, L L, "The Plastics for Mounting of Metallographlc Samples," Proceedings, Amencan
Sooety for Testing and Materials, Philadelphia, Vol 38, Part I, 1938, pp 511-5 t 5
[3] Wyman, L L, "A Mid-Century of Metallography--Retrospect and Aspect," Fifty Years o f Progress
in Metallographic Techniques, ASTM STP 430, American Sooety for Testing and Materials, Phd-
adelphia, 1968, pp 1-16
[4] "What Can Be Done to Improve Alloy Phase Nomenclatureg," Bulletin, American Sooety for Test-
mg and Materials, Philadelphia, December 1957, pp 27-30
[5] Fmk, W L and Wyman, L L, "The New ASTM System of Alloy Phase Nomenclature," Materials
Research & Standards, Vol 1, Apnl 1961, pp 289-290
[6] Rawdon, H S, "Report of Sub-Committee V on Micro-Hardness," Proceedings, Amencan Society
for Testing and Materials, Philadelphia, Vol 26, Part I, 1926, pp 572-580
[7] Vander Voort, G F, "Results of an ASTM E4 Round-Robin on the Preosion and Bias of Mea-
surements of MlcromdentaUon Hardness Impressions," Factors That Affect the Precision o f
Mechanical Tests, A S T M STP 1025, American Society for Testing and Materials, Philadelphia,
1989, pp 3-39
[8] VanderVoort, G F,"OperatorErrorslntheMeasurementofMlcromdentationHardness,"Accred-
itation Practices for Inspections, Tests, and Laboratories, ASTM STP 1057, American Society for
Testing and Materials, Philadelphia, 1989, pp 47-77
[9] Mogerman, W D, Zay Jeffries, American Sooety for Metals, Metals Park, OH 1973
[10] Barn, E C, Pioneering in Steel Resarch, Amencan Sooety for Metals, Metals Park, OH, 1975
[ 11] McKeehan, L W, "Glossary of Terms Relating to X-Ray Metatlography," Proceedings, Amencan
Sooety for Testing and Materials, Phdadelphta, Vol 26, Part I, 1926, pp 582-589
[12] "Report of Sub-Committee VI on X-Ray Metallography," Proceedings, American Society for Test-
mg and Materials, Philadelphia, Vol 25, Part I, 1925, pp 444-485
[13] Moyer, R B, Committee E-7 on Nondestructive Testing An Overview," Standardization News,
Vol 10, Nov 1982, pp 12-13
[14] "The Joint Committee on Powder Diffraction Standards--an InternationalData Resource," Stan-
dardization News, Vol 2, July 1974, pp 26-27
[15] Hanawalt, J D, et al, "Chemical Analysis by X-Ray Diffraction," Industrial and Engineering
Chemistry, Analytical Ed, Vol 10, No 9, 15 Sept 1938, pp 457-512
[16] Matthews, F W, "A Coordinate Index to X-Ray Powder Diffraction Data Using Punched Cards,"
Materials Research & Standards, Vol 1, August 1962, pp 643-645
[ 17] "New Retrieval System Developed for X-Ray Powder Data," Materials Research & Standards, Vol
1, October 1962, pp 842-843
[18] McMur&e, H F, "Progress in X-Ray Diffraction Data Compilations," Fifty Years of Progrcss in
Metallographic Techniques, ASTM STP 430, American Sooety for Testing and Materials, Phda-
delphm, 1968, pp 192-200
[19] Wyman, L L, "The NewASTM Grain-Size Methods," Bulletin, Amencan Sooety for Testmgand
Materials, Phdadelphm, July 1956, pp 59-61

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16 METALLOGRAPHY PAST, PRESENT, AND FUTURE

[20] Wyman, L L and Penrod, R E, "For a Unified Gram-Size Standard," Materials Research & Stan-
dards, Vol 1, August 1961, pp 638-639
[21] Abrams, H, "Grain Size Measurement by the Intercept Method," Metallography, Vol 4, February
1971,pp 59-78
[22] Davis, C H, "Gram Size Comparator," Bulletin, American Society for Testing and Materials, Phil-
adelphia, August 1941, p 45
[23] Hull, F C, "A New Method for Making Rapid and Accurate Estimates of Gram Size," Transactions,
Amencan Institute of Mining, Metallurgical, and Petroleum Engineers, Vol 172, 1947, pp 439-
451
[24] Morse, J P, "Standard Methods for Characterizing Duplex Grain Sizes," Standardization News,
Vol 15, December 1987, pp 44-46
[25] Epstein, S, "A Suggested Method of Determining the Cleanness of a Heat of Steel," Metals and
Alloys, Vol 2, October 1931, pp 186-191
[26] Walker, G W, "Rating of Inclusions ("Dirt Chart")," Metal Progress, Vol 35, February 1939, pp
169, 170 and 167
[27] "Detection of Inclusions in Beanng Quahty Steel by the Ultrasonic Method," Materials Research &
Standards, Vol 9, September !969, pp 21-24, 72
[28] Donachle, Jr, M J , and Knege, O H , "Phase Extraction and Analysis in Superalloys--Summary
of Investigations by ASTM Committee E4 Task Group 1," Journal of Materials, Vol 7, September
1972, pp 269-278
[29] Donachle, Jr, M J , "Phase Extraction and Analysis of Superalloys--Second Summary of Investi-
gations by ASTM Subcommittee E04 91," Journal of Testing and Evaluation, Vol 6, May 1978, pp
189-195
[30] Chopra, K S, "Interlaboratory Measurements of Amphibole and Chrysotfle Fiber Concentration
m Water," Journal of Testing and Evaluation, Vol 6, July 1978, pp 241-247
[31] "E4 to Rewew Cahbratlon Pracuce for Scanning Electron Microscopes," Standardization News,
Vol 8, July 1980, p 19
[32] "SEM Performance Characterized," Standardization News, Vol 13, February 1985, p 18
[33] Abrams, H, "Quantitative Metallography," Standardization News, Vol 5, December 1977, pp 16-
18
[34] Vander Voort, G F, "Advances in Microstructural Imaging--Directions m Metallography," Stan-
dardization News, Vol 16, November 1988, pp 50-57, and, Vol 17, February 1989, p 12

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VANDER VOORT ON HISTORY OF COMMITTEE E4 17

OIficers Committee E4 on Metallography

Chairmen
1916-1917 Edgar Marburg
1917-1924 Wdham Hastings Bassett
1924-1930 Henry C Boynton
1930-1936 Charles H Davis
1936-1938 John Torrey Norton
1938-1966 LeRoy L Wyman
1966-1972 Wdham D Forgeng, Sr.
1972-1974 Andrew W Danko
1974-1978 William D. Forgeng, Jr
1978-1982 Gunvant N Manmr
1982-1986 Halle Abrams
1986-1990 Francis J Warmuth
1990- George F Vander Voort

Secretaries
1916-1921 none
1921-1930 George F Comstock
1930-1936 Oscar E Harder
1936-1946 John J Bowman
1946-1966 Mary R Norton
1966-1970 Edward F O'Mara
1970-1973 John C Russ
1973-1974 Wdham D Forgeng, Jr
1974-1979 Robert M Sleplan
1979-1982 Francis J Warmuth
1982-1984 Albert Szlrmae
1984-1988 Donald R Green
1988-1990 Robert S Graham
1990- Richard K Wilson

First Vice Chairmen


1916-1936 none
1936-1944 Marcus A Grossman
1944-1964 R Earl Penrod
1964-1966 Wdham D Forgeng, Sr
1966-1972 Andrew W Danko
1972-1974 Larry Toman, Jr
1974-1978 Gunvant N. Mamar
1978-1982 Halle Abrams
1982-1986 Francis J Warmuth
1986-1988 Matthew J A Nousak
1988-1990 George F Vander Voort
1990 Donald R. Green
1990- Samuel M. Purdy
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18 METALLOGRAPHY PAST, PRESENT, AND FUTURE

2nd Vice Chairmen


1916-1972 none
1972-1974 John C Russ
1974-1978 Halle Abrams
1978-1982 John A Hendnckson
1982-1984 Rick Anderson-Decma
1984-1986 Matthew J A Nousak
1986-1988 George F. Vander Voort
1988-1990 Donald R Green
1990-1991 Robert S Graham
1991- Albert V Brandemarte

Membership Secretary
1916-1964 none
1964-1965 Barn R Baner lee
1965-1974 Robert M Sleplan
1974-1976 Conme B Craver
1976-1979 Donald A Nail
1979-1981 TheresaV Brassard
1981-1986 GallV Bennett
1986-1990 Albert Szlrmae
1990- Thomas N Rouns

Honorary Officers
1964 (Vice Chairman) R Earl Penrod
1967 (Chairman) LeRoy L Wyman
1968 (Secretary) Mary R Norton

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VANDER VOORT ON HISTORY OF COMMITTEE E4 19

Subcommittee Chairmen

Sub I on Sample Selection and Preparation and Photography


1920-1927 Wdham Campbell
1927-1928 George F Comstock
1928-1941 Edgar H Dlx, Jr
1941-1947 George F Comstock
1947-1951 Joseph R Vdella
1951-1959 Frederick C Hull
1959-1966 Wdham D Forgeng, Sr
1966-1982 Samuel M Purdy
1982-1986 Roger Koch
1986- Samuel M Purdy

Sub 2 on Metallographic Terminology and Nomenclature of Phase Diagrams


1920-1925 HenryC Boynton
1925-1938 Arthur Phxlllps
1938-1940 Robert S. Wdhams
1948-1950 Paul A. Beck
1951-1955 Robert S Busk
1966-1974 Mary R Norton
1974-1978 Wdham D Forgeng, Jr.
1978-1985 Roger Koch
1985-1986 Gary Hamman
1986-1992 RobertS Graham
1992- Beth Knueppel

Sub III on Thermal Analysis/Sub 3 on Nomenclature


1920-1921 George K Burgess
1924-1928 Wdham E Ruder
1928-1933 Howard Scott
1949-1960 Paul A Beck
1960-1978 W d h a m L Flnk
1978-1979 Wdham L Mankms
1979-1985 MatthewJ A Nousak

Sub 4 on Photography
1920-1922 V H Blhlman
1922-1934 Henry S. Rawdon
1934-1951 Leon V Foster
1951-1957 Sidney Poole
1957-1968 George A Elhnger
1968-1971 Conme B Craver
1971-1975 Charles H. Brown
1975-1983 Rick J Anderson (later Anderson-Decma)
1983-1985 Gary Hamman
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20 METALLOGRAPHYPAST, PRESENT, AND FUTURE

Sub 5 on Microindentation Hardness Testing


1923-1926 Henry S Rawdon
1948-1955 Alexander Gobus
1955-1958 WalterA Shebest
1965-1978 Larry Toman, Jr
1978-1980 William D Forgeng, Jr
1980-1982 Robert M. Slepian
1982-1983 Anthony DeBelhs
1983-1988 Samuel M Purdy
1988-1989 Robert S Graham
1989- Francis J Toye, Jr

Sub 6 on X-Ray Methods


1924-1930 Zay Jeffnes
1930-1933 Lores W. McKeehan
1933-1937 Robert Franklin Mehl
1937-1938 Horace Hardy Lester
1938-1960 Wdham L. Fmk
1960-1971 Robert K Scott
1971-1973 AndrewW Danko
1973-1986 Leo Zwell

Sub VII on Methods of Thermal Analysis


1938-1940 LeRoy L Wyman, Sr
1940-1951 Laurence H Carr
1951-1970 Donald I Finch
1971-1972 Wllham D Forgeng, Jr
1972-1977 CharlesH Brown

Sub 8 on Grain Size


1931-1937 Clarence J Tobm
1937-1952 Marcus A Grossman
1952-1964 R Earl Penrod
1964-1968 Harold S Link
1968-1972 Edward F O'Mara
1972-1975 Wdham D. Forgeng, Jr
1975-1977 Donald E Van Inwegen
1977-1978 Robert Mdlsop
1978-1982 Robert M Sleplan
1982-1983 Ernest C. Pearson
1983-1985 Matthew J A Nousak
1985-1989 Halle Abrams
1989- Franos J Warmuth

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VANDER VOORT ON HISTORY OF COMMITTEE E4 21

Sub 9 on Inclusions
1940-1965 Samuel Epstein
1965-1968 Gordon Meldrum
1968-1969 George H Baile
1969-1972 Gordon Meldrum
1972-1975 Gunvant N. Manlar
1975-1984 John A Hendrlckson
1984-1988 SherryA. Majoy
1988- Albert V Brandemarte

Sub X on Decarburization/Sub X on Research


1949-1953 John J B. Rutherford
1968-1974 Donald I Finch

Sub 11 on X-Ray and Electron Metallography


1950-1951 George E. Pellissler
1951-1953 D MaxwelITeague
1953-1955 William L Grube
1955-1956 Robert M Fisher
1956-1959 S T. Ross
1959-1961 Norman A Nielsen
196 l- 1963 Charles M. Schwartz
1963-1965 John R Mihahsln
1965-1967 Banl R. Banerjee
1967-1969 Thomas P Turnbull
1969-1973 George E. Pelhssler
1973-1975 GunvantN Manlar
1975-1977 Albert Szlrmae
1977-1980 KuldipS Chopra
1980-1985 Donald R Green
1985-1986 Chuck Bnckner
1986-1989 Donald R. Green
1989-1991 Albert Szirmae
1991- John J Frlel

Sub 14 on Quantitative Metailography


1961-1964 George E Pelhssler
1964-1966 SamuelM Purdy
1966-1967 Wllham D. Forgeng, Jr
1968-1972 Samuel M Purdy
1972-1978 Halle Abrams
1979-1981 James Hider Steele, Jr.
1981-1982 EdwardJ Korda
1982- George F Vander Voort

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22 METALLOGRAPHY PAST, PRESENT, AND FUTURE

Sub XV on Emission Microscopy


1969-1976 Erwm Elchen
1976-1977 Kuldlp S Chopra

Sub 16 on Phase Identification in Metal Alloys


1977-1980 Rick J Anderson-Declna
1980-1983 Donald R Green

Sub 17 on Laboratory Evaluation and Safety


1977-1982 FranclsJ Warmuth
1982-1983 GunvantN Mamar
1983-1988 JeremyP Morse
1988-1989 Raymond M Mlddleton
1989-1991 Lmda K Kern
1991- Robert C Nester

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VANDER VOORT ON HISTORY OF COMMITTEE E4 23

Committee FA Award Winners

Award of Merit
Halle Abrams- 1983
Wdlard Bablngton- 1962
Andrew W Danko-1970
Wheeler P Davey-1952
George A Elhnger-1967
Samuel Epstein- 1966
Donald I. Finch-1963
Wdham L Fmk-1956
Alexander Gobus- 1964
Joseph D Hanawalt-1965
John A, Hendnckson-1986
George O Hlers-1959
Fritz V. Lenel-1958
Horace H Lester-1951
Roger P Loveland- 1966
Gunvant N Manlar- 1984
Fred W Matthews-1968
Warren H Mayo-1965
George A Moore-1977
Mary R Norton-1959
Leander F Pease, III-1989
R Earl Penrod-1957
Samuel M Purdy-1989
Frederick N. Rhmes- 1962
Harold W Rmn-1971
Theodore G Rochow-1968
Robert M. Sleplan-1980
Albert Szlrmae- 1990
Ernest E Thum-1954
George F Vander Voort-1987
Andrew Van Echo-1973
Francis J Warmuth- 1985
Vmcent P Weaver-1958
LeRoy L Wyman, Sr -1950

Fellows Prior to the Award of Merit


Wllham H Bassett
Henry Marion Howe
James G Morrow

Honorary Officers
LeRoy L Wyman-Honorary E4 Chalrman-1967
Mary R Norton-Honorary E4 Secretary- 1967
Wdham Campbell-Honorary B2 Chmrman- 1934
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24 METALLOGRAPHYPAST, PRESENT, AND FUTURE

Honorary ASTM Members


Donald I Finch (Leeds & Northrup)- 1976
Wdham L Flnk (Alcoa Res Labs.)-1966
Wdham D Forgeng, Sr (Umon Carblde)-1974
Henry Marion Howe (Columbia Umversity)- 1919
Horace Hardy Lester (Watertown Arsenal)-1953
Warren H Mayo (US Steel)-1978
James G Morrow (Steel Co of Canada)- 1958
Henry S Rawdon (National Bureau of Standards)-1950
Andrew Van Echo (ERDA)-1975
Joseph F Woodruff (Armco Steel)- 1975
LeRoy L Wyman, Sr (National Bureau of Standards)-1967

Past ASTM Officers


William H Bassett-Member of Executive Committee 1916-1918, VP 1932-1934, P 1934-
1935 (he died only a few weeks after taking office on 7/21/34)
William Campbell-Member of Executwe Committee 1924-1926
Donald I Finch-Director 1971-1974
William L Fmk-Dlrector 1958-1961
Henry Marion Howe-VP 1898-1900, P 1900-1902 and 1910-1912 (Howe's name is the first
hsted on the ASTM Charter)
Zay Jeffnes-Member of Executive Committee 1930-1932
Warren H Mayo-Director 1967-1970
James G Morrow-Member of Executwe Committee 1944-1947, VP 1947-1949, P 1949-
1950
Albert Sauveur-Member of Executive Committee 1913-1915
(Edgar Marburg-Secretary-Treasurer 1902-1918, Marburg suggested the original ASTM
name and was the founding chairman of E4, he died m 1918)

L. L. Wyman Award
Halle Abrams- 1977
Wlllard W Bayre-1977
Francis J Warmuth- 1980
Wdham D, Forgeng, Sr -1982
John A Hendrlckson-1982
Erme Pearson- 1984
Roger W Koch- 1986
Matthew J A Nousak-1988
Jeremy P Morse-1988

Joseph R. Vilella Award


1974--Bruce L Bramfitt, Arian O Benscoter, James L Kllpatnck and Arnold R Marder
"The Use of Hot-Stage Microscopy in the Study of Phase Transformations," Metal-
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VANDER VOORT ON HISTORY OF COMMITTEE E4 25

lography--A Practical Toolfor Correlating the Structure and Properties of Materials,


A S T M STP 557, 1974, pp 43-70

1979--Morris Cohen and Steven S Hansen


"Mlcrostructural Control m Mlcroalloyed Steels," MiCon 78: Optimization of Pro-
cessing, Properties, and Service Performance Through Microstructural Control,
A S T M S T P 672, 1979, pp 34-52
1979--Harvey D Solomon and Thomas M Devine, Jr
"Influence of M~crostructure on the Mechanical Properties and Locahzed Corrosion
of a Duplex Stainless Steel," MiCon 78: Optimization of Processing, Properties, and
Service Performance Through Microstructural Control, A STM STP 672, 1979, pp
430-461
1986--Ervm E Underwood
"Practical Solutions to Stereologlcal Problems," Practical Applications of Quantita-
~.tveMetallography, A STM STP 839, 1984, pp 160-179

Other Awards
Charles B. Dudley Metal (for a paper of outstanding merit in the field of materials research)
Samuel Epstein, 1933, "Embnttlement of Hot-Galvanized Structural Steel," Proceedings,
ASTM, Vol 32, Part II, 1932, pp 293-379
Frederick C Hull, 1962, "Effects of Alloying Ad&tlons on Hot Cracking ofAustenmc Chro-
mmm-Nlckel Stainless Steels," Proceedings, ASTM, Vol 60, 1960, pp 667-690
Wilbur C Blgelow, 1964, "The Development of Electron Microscopic Methods for the
Study of Metals," STP 317, Symposium on Advances in Electron Metallography and Elec-
tron Probe Microanalysis, 1962, pp 58-139
Edgar Marburg Lecture (promote knowledge of outstanding developments in englneenng
materials)
George L Clark, 1927, "The X-Ray Examination of Materials in Industry," Proceedings,
ASTM, Vol 27, Part II, 1927, pp 5-51
Albert Sauveur, 1938, "The Torsion Test," Proceedings, ASTM, Vol 38, Part II, 1938, pp
3-20
Gillett Memorial Lecture
Norman A Nielsen, 1970, "Observations and Thoughts on Stress Corrosion Mechanisms,"
Journal of Materials, Vol 5, No 4, December 1970, pp 794-829
Richard L. Templin Award (for an outstanding paper describing new and useful testing pro-
cedures and mechanical apparatus)
Theodore G Rochow, 1973, "A Microscopical Automated Mlcrodynamometer Mlcroten-
slon Tester," Materials Research and Standards, Vol. 12, April 1972, pp 27-30, 53-54 (R
J Bates coauthor)
H. V. ChurchillAwards (given by Committee E2 on Emission Spectroscopy)
Joseph F Woodruff, 1974
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26 METALLOGRAPHYPAST, PRESENT,AND FUTURE

Robert D. Thompson Award (given by Committee E20 on Temperature Measurement)


Donald I Finch, 1976
Anthony DeBellis Memorial A ward (given by Committee E28 on Mechamcal Testing for slg-
mficant contrlbuUons in the field on hardness testing)
George F Vander Voort, 1990

Mary R. Norton Memorial Scholarship Recipients


Elane C Sanderson, Colorado School of Mines, 1975
Margaret D Weeks, Carnegie-Mellon University, 1976
Elma B Stapes, North Carohna State University, 1977
Loranne M Brydges, Ilhnols Institute of Technology, 1979
Knstme M Stanecki, Umverslty of Michigan, 1980
Phylhs Anne Klein, University of Illinois at Champalgn-Urbana, 1981
M~chelle W Gabriel, Massachusetts Institute of Technology, 1982
Judith Glazer, Umversity of California at Berkeley, 1984
Amta J HIll, Duke University, 1985
Carol-Ann Baer, California Polytechnic State Umversity, 1986-1987
Leshe S Steele, Umversity of Dayton, 1987-1988
Chrysanthe Demetry, Massachusetts Institute of Technology, 1988-1989,
Yvonne Field, State Umverslty of New York at Stony Brook, 1989-1990,
Ann M Redsen, Umverslty of Wisconsin at Madison, 1990-1991
Jennifer S Wheeler, Purdue University, 1991-1992
W Elan McGee, Cahfornla Polytechmc Umverslty, 1992-1993

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a

Committee E4 Standards at a Glance

E 2--Preparation of Micrographs of Metals and Alloys


Issued m 1917, E 2 was revised twelve times, and the title changed twice before being dis-
continued and replaced by E 883 m 1983 Grain size measurement methods were described
in E 2 from 1917 The first comparative grain size chart, for copper, was added in the 1930
revision but was deleted in the 1949 revision when E 79 was issued Standard definmons were
balloted m the 1923 revision but transferred to E 7, instead Ironically, photomlcroscopy
guidelines were first ballotted as E 7-23, but then incorporated into the 1924 revision o f E 2

E 3--Preparation of Metallographic Specimens


Issued in 1921, E 3 has been revised ten times, and its title was changed twice The initial
13 page document swelled to 33 pages when m 1935 it was revised and combined with E 5
With further revisions, it grew to 36 pages (1939), 43 pages (1944), 46 pages (1946), and 66
pages in 1958, then shrank as new standards were formed based largely upon it, for example,
E 340 and E 407 Later, E 1180 was developed to cover the sulfur pnnt method, described
briefly in E 3 up to 1980 Also m 1980, the electropohshmg information was deleted but a new
standard has not yet emerged

E 5--Metallographic Testing of Non-Ferrous Metals and Alloys


Issued in 1923, it was revised twice before being merged into E 3 in 1935

E 7--Definitions of Terms Relating to Metallography


Terms were first defined in a 1921 proposed revision of E 2 Sixteen were proposed but this
dropped to 13 In she 1923 revision, still under E 2 In 1924, this document was renumbered
as E 7, with 11 terms, and Issued as standard Metallography was added as a term m 1926, but
this defimhon was changed in 1927 (and has remained unchanged since) After four revisions,
E 7 remained at 12 definitions until 1955 when it zoomed up to a 45 page standard with 750
definitions Since 1955, it has been revised twelve times, mainly editorially through the addi-
tion of terms approved in other standards

E 14--Thermal Analysis of Steel


Issued m 1925, it was revised five times before new Committee E37 on Thermal Measure-
ments took over its jurisdiction in 1978 (it was discontinued in 1983)

E 15--Radiographic Testing of Metal Castings


Issued m 1926, it was revised twice before new Committee E7 on Radiographic Testing (now
in Nondestructive Testing) took over jurisdiction in 1939 (It was discontinued in 1949 )

E 19--Grain Size Chart for Classification of Steels


Issued m 1933, E 19 estabhshed the McQuald-Ehn carbunzmg method as the standard pro-
cedure for evaluating the austemte grain s~ze and the gram-coarsening tendency of steels.
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28 METALLOGRAPHYPAST, PRESENT, AND FUTURE

Revised three times, it was discontinued in 1961 when E 112 was issued The 1933 version
contained a single chart showing the hypoeutectoid and hypereutectold regions of carburlzed
steels with grain sizes from l to 8 The 1939 revision added a second chart, stylized grain struc-
tures (black boundaries on a white matrix and white boundaries against a black matrix) Nei-
ther chart was incorporated into E 112

E 43--Identification of Crystalline Materials by the Hanawalt X-Ray Diffraction Method


Issued in 1942, it enjoyed a brief but stormy life Revised in 1946 and 1949, it was under
constant revision from 1951 on, reportedly completed in 1960, but wxthdrawn in 1961 How-
ever, revision work continued at least up to 1968 The method was considered too extensive
for a standard and a text was started but never published

E 45--Determining the Inclusion Content of Steel


Issued in 1942 and revised nine times, E 45 is presently undergoing a major overhaul The
mmal standard contained only one chart, the J-K chart, used for Method A and a nonchart
method (B) developed by Sam Epstein Method C and Plate lI were added in 1960 and Method
D and Plate Ill were added in 1962

E 79--Estimating the Average Grain Size of Wrought Copper and Copper-Base Alloys
Issued in 1949, E 79 was based on the chart and methods formerly in E 2 Two micrographs
were added to the chart in 1949 This chart, and the method, were merged into E 112 when it
was written (the chart was again expanded by two mlcrographs) and E 79-49T was discontin-
ued in 1963

E 80--Dilatometric Analysis of Metallic Materials


Issued m 1949, it remained as written until new committee E37 on Thermal Measurements
assumedjurls&CtlOn in 1978 (E 80 was discontinued in 1986 and replaced by E 228 )

E 8 l--Preparing Quantitative Pole Figures of Metals


Issued in 1949, it has been revised three times E 81 is an X-ray diffraction method for detect-
mg and describing crystallographic texture.

E 82--Determining the Orientation of a Metal Crystal


Issued m 1949, adopted without change and revised editorially twice, E 82 describes the
back-reflection Laue method The technique is used to determine the crystallographic orien-
tation of single crystals (or large crystals in a polycrystalline material)

E 89--Estimating the Average Ferrite Grain Size of Low-Carbon Steels


Issued in 1950 and approved m 1952, E 89 introduced the first correlation between the aver-
age intercept length and the ASTM grain size It contained a ferrite gram size chart for ASTM
gram sizes 1-8 E 89 was discontinued in 1961 after E 112 was developed and its chart was
dropped

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VANDER VOORT ON HISTORY OF COMMITTEE E4 29

E 9 ! - - E s t i m a t i n g the Average Grain Size of Non-Ferrous Metals, Other than Copper, and
Their Alloys
Issued m 1951, E 91 contained two charts for rating gram size, one with a fiat etch and the
other with a contrast etch Both charts were for twinned austemte grams and each contained
17 mlcrographs for ASTM 2 to 10 E 91 was discontinued m 1961 after E 112 was adopted
and both charts were dropped

E l 12--Determining the Average Grain Size of Metals


Issued m 1955, E 112 was the culmination of 37 years work replacing E 19, E 79 (developed
from E 2), E 89, and E 91 Four charts for rating gram size are included, three were new m
1955 Plate I for rating nontwmned grams with a fiat etch underwent extensive minor correc-
tions through the 1980s to enhance the precision of the mlcrographs E 112 has been revised
eleven times in its 36 year hxstory, its name has been changed twice, and it is one of the most
widely cited ASTM standards Nevertheless, it is under rewslon now

E 157--Assigning Crystallographic Phase Designations in Metallic Systems


Issued In 1961, E 157 has been revised four hmes It defines nomenclature for alloy phases
based on composmon and crystal structure

E 189--Determining Temperature--Electrical Resistance Characteristics (EMF) of


Metallic Materials
Issued m 1961, E 189 was revised once, and ~ts name was changed, before new Committee
E37 on Thermal Measurements took over jurisdiction m 1978 (It was discontinued in 1987 )

E 340--Macroetching Metals and Alloys


Issued m 1968, E 340 was based on macroetch mformaUon formerly m E 3 It has been
revised twice and ~ts name was changed once

E 381--Macroetch Testing, Inspection, and Rating Steel Products, Comprising Bars,


Billets, Blooms, and Forgings
Issued m 1968, E 381 was revised twice and its name was changed m 1979 Two plates are
used to rate the macrostructure A task group has been working on a major revision of E 381
to extend coverage to the rating of continuously cast steels

E 384--Microhardness of Materials
Issued m 1969, E 384 has been rewsed five t~mes and Its name was changed m 1976 It is
currently being revised extensively, including another name change

E 391--Presentation of Phase Diagrams


Issued m 1969, E 391 has been rewsed three times E 391 provides rules for drawing binary
and ternary e q m h b r m m phase diagrams for pubhcatlon
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30 METALLOGRAPHYPAST, PRESENT, AND FUTURE

E 407--Microetching Metals and Alloys


Issued in 1970, E 407 was based on etchant information formerly in E 3 Its organization
approach is ideal for pubhcatlon (each etchant is described and given a number while a table
lists the suitable etchant numbers for different metals anti alloys) as redundancy is avoided but
this makes it extremely difficult to revise The original document contained 209 etchants and
has not been revised However, a task group has begun a revision and plans to create a com-
puter database program which would enhance its use and simplify future revisions

E 562~Determining Volume Fraction by Systematic Manual Point Count


Issued in 1976, E 562 was revised three times E 562 describes the manual point counting
approach for determining the volume fraction of phases or constituents in mlcrostructures

E 588~Detection of Large Inclusions in Bearing Quality Steel by the Ultrasonic Method


Issued in 1976, E 588 covered ultrasonic inspection procedures for detecting the infrequent,
irregularly distributed larger Inclusions that the microscopic methods will rarely detect It was
transferred to E 7'sjunsdictlon in 1984 and was revised in 1988

E 766--Calibrating the Magnification of SEM Using NBS-SRM-484


Issued in 1980, it was revised in 1986 E 766 describes how to calibrate a scanning electron
microscope A second revision IS in ballot now

E 768--Preparing and Evaluating Specimens for Automatic Inclusion Assessment of Steel


Issued in 1980, but not revised since, E 768 contains a color plate illustrating correct and
incorrect specimen preparation as evaluated by differential interference contrast (DIC)
illumination

E 807--Metallographic Laboratory Evaluation


Issued in 1981, a revision of E 807 is now in progress

E 883--Metallographic Photomicrography
Issued in 1982 and revised twice, E 883 replaced the venerable E 2 standard

E 930--Estimating the Largest Grain Observed in a Metallographic Section (ALA Grain


Size)
Issued in 1983, edltonal changes were made in 1989 and a revision is now in progress E 930
is used to rate the size of one or a few very large grains m an otherwise fine-grained matrix, a
problem not covered in E 112

E 963--Electrolytic Extraction of Phases from Ni and Ni-Fe Base Superalloys Using a


Hydrochloric-Methanol Electrolyte
Issued in 1983 after an extensive seventeen year effort, E 963 has not been revised since E
963 describes a techmque for bulk extraction of second-phase constituents from superalloys
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VANDER VOORT ON HISTORY OF COMMITTEE E4 31

E 975--X-ray Determination of Retained Austenite in Steel with Near Random


Crystallographic Orientation
Issued m 1984, E 975 has not been revised to date E 975 describes how to determine the
amount of retained austemte in steels using an X-ray dlffracUon procedure

E 986--Scanning Electron Microscopy Performance Characterization


Issued m 1984, and rewsed in 1986, E 986 describes an approach for assessing the imaging
performance of a scanning electron microscope. A revision is being ballotted now

E 1077--Estimating the Depth of Decarburization of Steel Specimens


Issued m 1985, an editorial change was made in 1986 and it was revised m 1991

E 1122--Obtaining JK Inclusion Ratings Using Automatic Image Analysis


Issued in 1986, E 1122 is an automated approach for obtaining E 45 method A or D ratings
It is becoming widely used as Image analyzer capabdlty has improved The first revmion is
being balloted now

E 1180--Preparing Sulfur Prints for Macrostructural Examination


Issued in 1987, this standard greatly expands on the simple instructions given in E 3 but
deleted in its 1980 revision Sulfur printing has become a popular method for evaluating the
macrostructure of continuously cast steels.

E 1181--Characterizing Duplex Grain Sizes


Issued in 1987, E 1181 addresses characterization of non-Gausslan grain size distnbuUons,
a problem not addressed by E 112

E 1182--Measurement of Surface Layer Thickness by Radial Sectioning


Issued in 1987, E 1182 describes a simple, elegant, approach for measunng the thickness of
surface layers or coatings

E 1245--Determining Inclusion Content of Steel and Other Metals by Automatic Image


Analysis
Issued in 1988 and revised in 1989, E 1245 provides an approach for characterizing discrete
second-phase particles, such as inclusions, carbides, or nltrldes, using automated quantitative
microscopy It incorporates an automated E 562 approach to determine volume fractions with
other basic measurements

E 1268--Assessing the Degree of Banding or Orientation of Microstructures


Issued m 1988, E 1268 describes a quantitative method for characterizing banded or ori-
ented mlcrostructures
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32 METALLOGRAPHYPAST, PRESENT, AND FUTURE

E 1351--Production and Evaluation of Field Metallographic Replicas


Issued initially as emergency standard ES 12 in 1987, it became a standard in 1990 The
standard was w n t t e n due to the need to assess creep damage in steam pipes

E 1382--Determining the Average Grain Size Using Semiautomatic and Automatic Image
Analysis
Issued m 1990, but revised in 1991, E 1382 describes a n u m b e r of approaches for determin-
ing gram size using either s e m i a u t o m a t i c or automatic image analyzers

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VANDER VOORT ON HISTORY OF COMMITTEE E4 33

Symposia Special Technical Publications by Committee


E4

STP Year Title


28 1936 Symposium on Radiography and X-Ray Diffraction Methods
28A 1942 Symposium on Radiography
86 1948 Symposium on Metallography in Color
155 1953 Symposium on Techniques for Electron Metallography
245 1958 Advances in Electron Metallography
262 1959 Symposmm on Electron Metallography
285 1960 Symposium on Methods of Metallographic Specimen Preparation
317 1962 Symposium on Advances in Electron Metallography and Electron
Probe Mlcroanalysls
339 1962 Symposium on Advances in Techniques in Electron Metallography
349 1963 Symposium on X-Ray and Electron Probe Analysis (with E2)
372 1963 Techniques of Electron Microscopy, Diffraction, and Microprobe
Analysis
396 1965 Advances in Electron Metallography
430 1966 Fifty Years of Progress in Metallographlc Techniques
480 1969 Applications of Modern Metallographlc Techniques
485 1970 Energy Dispersive X-ray Analysis X-ray and Electron Probe
Analysis
504 1971 Stereology and Quantitative Metallography
547 1973 Manual on Electron Metallography Techniques
557 1973 Metallography--A Practical Tool for Correlating the Structure and
Properties of Materials
672 1979 MiCon 78--Optimization of Processing, Properties, and Service
Performance Through Mlcrostructural Control
792 1983 MiCon 82--Optimization of Processing, Properties, and Service
Performance through Mlcrostructural Control
839 1984 Practical Applications of Quantitative Metallography (with IMS)
889 1986 MlCrOlndentatlon Techniques in Materials Science and Englneenng
(with IMS)
979 1988 MiCon 86--Optimization of Processing, Properties, and Service
Performance through Microstructural Control
1094 1990 M1Con 90 Advances in Video Technology for Mlcrostructural
Control
1165 1992 Metallography Past, Present, and Future (75th Anniversary
Volume)

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34 METALLOGRAPHYPAST, PRESENT,AND FUTURE

Committee E4 Chairmen

William Hastings Bassett

(born 7 March 1868 m New Bedford, Massachusetts, died 21 July 1934 just a few weeks after
becoming president of ASTM)
Bassett, the first chairman of E4 (the founding chairman, Edgar Marburg, was the Secretary-
Treasurer of ASTM, an employee and neither a metallurgist nor a metallographer) graduated
from Massachusetts Institute of Technology m 1891 with a bachelor's degree in chemistry He
began his career as a chemist, first with Pope's Island Manufactunng Co ( 1891 ), then teaching
chemistry for the Swain Free School (1895), then with New Jersey Zinc Co, Newark, New
Jersey (1900) In 1902, he joined the American Brass Co at its Coe branch m Torrlngton,
Connecticut, advancing to chief chemist and metallurgist m 1903 and techmcal supennten-
dent and metallurgist m 1912 at their Waterbury, Connecticut headquarters He joined ASTM
in 1903.
Bassett was a leading expert m nonferrous metallurgy and has been credited w~th mtroduc-
Uon of metailographlc and spectrographic techniques to the copper industry For his efforts m
implovmg the quahty of copper alloys, he recewed the James Douglas Gold Medal of the
American Institute of Mining, Metallurgical, and Petroleum Engineers (AIME) in 1925 In
1930, he was president of AIME He also helped to bring Cyril Stanley Smith to the United
States from the Umverslty of B~rmmgham

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VANDER VOORT ON HISTORY OF COMMITTEE E4 35

Henry Cook Boynton

(born 16'Apnl 1874 in Wlllsborough, New York, died 28 March 1970)


Henry, a founding m e m b e r of E4, was its second chairman (1924-1930) and was the first
chairman of Sub II (I 920-1925) He attended Harvard University receiving A B (1900), S M
( 1901) and Sc.D (1904) degrees While his A B was in geology, the graduate degrees were m
metallurgy Boynton was the first to receive a doctorate from the Department of Metallurgy
and was Albert Sauveur's first doctoral student He remained at Harvard until 1906 teaching
metallurgy and metallography and assisting Professor Sauveur
In 1906 he joined John A Roebling's Sons Co (Trenton, New Jersey) as a metallurgist and
stayed with them until retirement on 1 January 1947 He worked on the manufacture of high
strength wire for suspension bndge cables, for example, for the Manhattan, Bear Mountain,
George Washington, and Golden Gate bridges For most of his career, he was chief metallur-
gist at Roebhng's After retirement, he joined Temple Umversity (on 1 September 1947) as
head of their new department of metallurgy and consulting metallurgist in their Research
Institute. He continued this work until 1955, remaining as a consultant until 1960 when he
again retired
Henry was also very active m the A m e n c a n Society for Metals with the Philadelphia Chap-
ter, serving as chairman m 1931 The Philadelphia Chapter ran an adult course m metallurgy
at Temple Umversity for many years and Boynton was a lecturer in th~s program from 1935
to 1939 Henry was a strong believer m tolerance and moderation m all aspects ofhfe, personal
and professional

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36 METALLOGRAPHY PAST, PRESENT, AND FUTURE

Charles Hollister Davis

(born 5 November 1886 in Manchester, Connecticut, died 22 May 1945)


Davis chaired E4 from 1930 to 1936 and prepared the mlcrographs for E4's first grain size
chart, for copper and brass, added to E 2 m 1930 After graduating from South Manchester
HlghSchool, he entered Yale Umverslty, recelvlngaB A ln geology in 1909 He pursued grad-
uate education at Yale in 1909-1910, then moved west in July of 1910 The balance of 1910
was spent mining in Idaho, surveying in Washington, and tounng through the Pacific North-
west He was a teacher and vice-principal at Manzanlta Hall (Palo Alto, California) while
studying geology at the Leland Stanford University. He recewed an M A in geology in 1912
He assisted Professor James P e m n Smith m a study of the paleontology of the area south of
Mt Shasta
Next, he took a job, m 1912, with the American Brass Co in Waterbury, Connecticut The
geologist was now a metallographer) During World War I, he was in charge of most of the
laboratory inspection work as brass was an important m u n m o n material By 1925, he was in
charge of the chemical and metallurgical laboratory and worked closely with Wdham H Bas-
sett Later, he was assistant technical manager

John Torrey Norton

(born 13 November 1898 in Medford, Massachusetts, died 18 July 1989)


John Norton, chairman of E4 from 1936 to 1938, recewed an S B degree in physics from
the Massachusetts Institute of Technology (MIT) in 1918, then joined the MIT staff as a
research associate m 1920 He was made an assistant professor of physics m 1926 His father,
Charles L Norton was head of the department of physics at MIT and his brother, Frederick
H Norton was an expert m ceramics and a member of the MIT department of metallurgy
John became very interested m the use of X-rays and gradually concentrated h~s interests in
this field In 1930, he was promoted to assooate professor of metallurgy, and in 1932, he

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VANDER VOORT ON HISTORY OF COMMITTEE E4 37

received his Sc D from M I T m metallurgy In 1941, he was promoted to full professor m the
physics of metals During World War II, he was head of the Radiographic Laboratory at MIT
and used X-ray inspection methods to solve a number of defense related problems, including
the assessment of residual stresses He also did fundamental studies on the bonding of pressed
powder metals For his contributions to the new field of powder metallurgy, he was awarded
the Plansee Plaque at the Fourth International Plansee Seminar (1961) in Austria, the first
American so honored
John Norton was chmrman of the faculty of MIT (1956-1958) and acting dean of the grad-
uate school (1961) He played an active role in developing the graduate curricula in metallurgy
at MIT In 1964, he retired becoming professor emeritus, ending nearly 75 years of service to
MIT by the three Nortons
Before retirement, he launched a business career as one of the founders (1957) of the
Advanced Metals Research C o r p , now AMRAY, I n c , the largest U S manufacturer of scan-
ning electron microscopes John acted as president from 1961 to 1973, then as board chairman
from 1973 until his death at age 90

LeRoy Linwood Wyman, Sr.

(born 20 September 1899 in Kenosha, Wisconsin, died 12 May 1975)


Roy Wyman, chairman of E4 from 1938-1966 and chairman of Sub VII on dIlatometnc
analysis ( 1938-1940), was also chairman of Committee A 10 on Iron-Chrommm, Iron-Chro-
mium-Nickel and Related Alloys from 1958-1966 He was named an honorary chairman of
both committees. He also was a founding member and chairman (1945-1957) of the Com-
mittee on Simulated Service Testing, a founding member of Committee F4 on Surgical
Implant Materials, a member of the Committee B9 on Metal Powders, a member of the exec-
utwe committee of Committee A 1 on steel, and a member o f several other ASTM committees
He was also one of the founders and a chairman of the Joint Committee on Powder Diffraction
Standards (JCPDS) He was a member of five U S National Committees involved with inter-
national standards
Roy attended the University of Minnesota, receiving a B Sc in chemical engineering m
1923 He spent h~s first year after graduation as assistant professor of metallurgy at the Okla-
homa School of Mines, then joined the Edison Lamp Works of the General Electric Co as a
metallographer He made some of the earliest cemented carbides in the United States in this
Job In 1929, he transferred to the General Electric Research Laboratory m Schenectady, in
charge of metallography In 1931, he was also put m charge of the X-ray diffraction laboratory
He headed the department of metallography and X-ray diffraction for the next 13 years
In 1942, he was given a year's leave from General Electric to serve as research supervisor,
War Metallurgy Committee, Office of Scientific Research and Development, National Acad-

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38 METALLOGRAPHYPAST, PRESENT,AND FUTURE

emy of Science In this posmon, he supervised research projects vital to the war effort He
returned to the General Electric Research Laboratory m 1944 as halson officer, metallurgy
From 1947 to 1953, he was in charge of alloy research at the Knolls Atomic Power Laboratory
of the Atomic Energy Comm~sslon
In 1953, W y m a n switched careers, joining the National Bureau of Standards as chief of
chemical metallurgy in their metallurgy dwlslon From 1961 to 1965 he was a consultant for
the National Bureau of Standards Following retirement, he took an active roll m the operahon
of the Joint Committee on Powder Dlffract~on Standards and was its chmrman at the time of
his death
W y m a n received numerous awards for h~s work He received the ASTM Award of Merit in
1950 and was made an honorary ASTM member in 1967 He received a Certificate of Merit
from the Office of Scientific Research and Development in 1945 and the Sdver Medal of the
U S Department of Commerce m 1958

William Daniel Forgeng, Sr.

(born 31 May 1909 m Scranton, Pennsylvama, died 4 June 1986)


Committee E4 has the unique distraction of father and son c h a i r m e n - - a n d with terms only
two years apart Bill Forgeng, Sr followed LeRoy W y m a n as chairman, his term was 1966-
1972 He also served as vice-chairman and chairman of Sub I on Selection and Preparation of
Samples
Ball senior received a bachelors degree m chemistry from Cornell University in 1930, then
did his Ph D. under Clyde W Mason (famed chemical microscopist) at Cornell in 1934 In
that year, he joined the Union Carbide Research Laboratories in Long Island City, New York
(moved m 1935 to Niagara Falls where Ball junior was born) Bill senior replaced Joseph R
Vdella who did not want to move away from New York City Vllella's wife, Eve, was a well-
known high fashion model in New York City Vdella joined U S. Steel's research laboratory
in Kearny, New Jersey, and also had an outstanding career
Bdl semor stayed with Union Carbide his enUre career, retiring in 1973 as semor research
fellow He pubhshed over thirty papers and had a half dozen patents He was recognized as an
expert m the metallography of stainless steels (he helped develop the 200 series), refractory
metals and other heat- and corrosion-resistant alloys He was also noted for his work on inclu-
sion identification, phase identification by X-ray diffraction, and color metallography During
World War II, he studied uranium production and fabrication under the Manhattan ProJect
He was made an honorary ASTM member m 1974.

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VANDER VOORT ON HISTORY OF COMMITTEE E4 39

Andrew William Danko

(born 11 December 1917 in Coraopohs, Pennsylvania, died 9 November 1987)


Andy Danko served as chairman of E4 ( 1972-1974), vice chairman (1966-1972) and chair-
man of Sub VI on X-ray methods (1971-1973) He joined E4 in 1952 After receiving his B S.
in chemical engineenng in 1940 from the University of Pittsburgh, he joined Westinghouse
Electric Corp in their Materials Engineering Department (became the Materials Research
Laboratory in 1960) as a chemist He progressed to supervisor of Optical, Electron and X-ray
Metallography, Materials D e p t , Astronuclear Laboratory at their Large, Pennsylvania site in
1962
In 1944, he introduced use of X-ray diffraction as an analytical tool at Westinghouse He
designed and built a number of X-ray instruments, for example, mlcroradlography cameras,
both film and dlffractometer pole figure gonlometers, and devices for measuring residual
stresses In 1956, he set up their first transmission electron microscope for service work In
1960, he recommended addition of an electron microprobe to the service group and devoted
subsequent efforts to standardization efforts for compositional work
Andy joined the Joint Committee on Powder Diffraction in 1956 and served as vice chair-
man from 1970-1973 and Secretary/General Manager from 1973 to 1979 He was also active
in ASTM Committees E2 and E3 and received the Award of Merit in 1970

William Daniel Forgeng, Jr.

(born 26 July 1935 in Niagara Falls, New York)


Bill Forgeng, Jr served as chairman of E4 only two years after his father, from 1974-1978
He also served as secretary and was chairman of five different subcommittees (an E4 record)"
Subs 2, 5, 7, 8, and 14 Bill j u m o r also received his bachelors degree (in metallurgical engi-
neering) from Cornell University (1958), then received a Ph D from Purdue University in
1962. Following graduation, he joined the Rochester Products Division of General Motors
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40 METALLOGRAPHYPAST, PRESENT,AND FUTURE

C o r p , then in 1964joined U S Steel Corp In 1980, he joined the staffofthe Cahfornia Poly-
technic State University in San Luls Oblspo where he ~s presently a professor in the Depart-
ment of Materials Englneenng
Bill states that his career has been influenced by two great metallographers--hls teaching
was influenced by Dr Clyde Walter Mason, the chemical microscopist from Cornell Univer-
sity, and his hands-on skills were influenced by his father Bdl did not begin his career as a
metailographer His work with General Motors and his first assignments at U S Steel were in
the area of products and process development In 1966, Jim Alger of the apphed research lab
at U S. Steel was looking for a supervisor of a metallographlc service section Since he knew
of Bdl's educational background, and heritage, he offered the j o b to Bill, which he took and
held for the next thirteen years Bill got revolved in some ploneenng work in image analysis,
with the Quantimet B, in scanning electron microscopy, with a Cambridge Stereoscan, and in
automated polishing, with the Struers Abrapol Bill even made presentations on these subjects
at E4 symposia)
Bdl always enjoyed his A S T M actwmes. He parhculady enjoyed coming to meetings, partly
because his Dad would always buy droner) By 1979, Bdl had gotten disillusioned w~th the steel
industry and had grown t~red of coping w~th winters m P~ttsburgh Because he most enjoyed
the instructional side o f his j o b at U S Steel, Bill decided to go into academm He wanted a
posmon where teaching came first and found a position at Cahfornm Polytechnic, where it
never snows) Bdl has a heavy teaching load, usually averagang four lectures and four labs per
week. He has his students reading and using A S T M standards m their labs Bdl ~s still acUve
wRh E4 but generally cannot attend meetings now

Gunvant Nandlal Maniar

(born 27 May 1932 in Karachi, Pakistan)


Gunny, an E4 member since 1962, was chairman of E4 from 1978 to 1982 after serving
previously as First Vzce Chairman from 1974 to 1978. He also served as Chairman of Sub 9
(1972-1975),Sub 11 (1973-1975), and Sub 17(1982-1983) G u n n y w a s c o e d l t o r o f S T P 547,
Manual on Electron Metallography Techniques, and of STP 557, Metallography--A Practi-
cal Toolfor Correlating the Structure and Properties of Materials, and was editor of the first
MiCon conference proceedings, STP 672. G u n n y has also been active with the American Soci-
ety for Metals, (ASM) serving as chairman of the Lehigh Valley Chapter (1973-1974) and with
the national organization as a member of the Handbook Committee (1975-1980) and as
chairman of this committee (1978-1980) He was a member of the Long Range Planning
Committee ( 1981-1984) and an ASM Trustee ( 1988-1989) He received the Bradley Stough-
ton Award of the Lehigh Valley ASM Chapter m 1979
He received a B Sc. m chemistry and physics from Gujarat University of India (1953), and
M S in metallurgy from Stevens InsUtute of Technology (1958) and an M S E m metallur-

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VANDER VOORT ON HISTORY OF COMMITTEE E4 41

glcal engineenng from the Umverslty of Michigan (1960) He was employed by the Auditor
General's Office, Government of India, from 1953-1956 He acted as a teaching assistant
while at Stevens and as a research assistant while at Michigan In 1960, he joined Crucible Steel
Co m Pittsburgh as a staff metallurgist
After two years with Crucible Steel, G u n n y came to Carpenter Technology Corp as a super-
visor m their R&D Center in 1962 In 1973, he was promoted to manager of physical metal-
lurgy and m 1977 was made general manager of the R&D laboratories He is presently man-
ager of New Products Development, a posmon he has held since 1983 Gunny is a Fellow of
ASTM and ASM He holds three patents and has published about thirty papers

Halle Abrams

(born 16 January 1938 in New York, New York, died 15 October 1989)
Halle joined ASTM and E4 in 1970 and was extremely acnve with E4 over the next nineteen
years He was chairman from 1982 to 1986 following four years as first vice chairman (1978-
1982) and four years as second vice chairman (1974-1978) Halle was also chairman o f Sub 8
( 1985-1989) when he died and had earher been chairman of Sub 14 (1972-1978) Halle was
active with all four MlCon symposia and was an editor for two of the resulting STPs He also
co-edited STP 557, Metallography--.4 Practical Toolfor Correlating the Structure and Prop-
erties of Materials. Halle's work on the intercept method for measunng grain size was Incor-
porated into the 1974 revision of E 112 He was also heavily involved with the development
of E 562, our manual point counting standard Halle also served as E4's representative to the
International Standards Organizauon
Halle studied chemical englneenng at the Polytechnic University of New York graduating
cum laude m 1959 He obtained M S degrees m chemical engineering from the New Jersey
Institute of Technology (1965) and in metallurgy from Lehigh University (1964) In 1968, he
obtained a Ph D in metallurgy and materials science from Lehigh University
He began his industrial career m 1959 at the former Western Electric Allentown (Pennsyl-
vama) plant D u n n g his etght years there, he pubhshed seven papers, two of which concerned
electrolytic polishing While working on his Ph D thesis, Halle taught at Lehigh from 1967 to
1968 In 1968, he joined Bethlehem Steel's Homer Research Laboratory, where he worked
until his death His research centered on alloy development, chiefly with hneplpe and plate
steels, strengthening mechanisms, structure-property-processing correlations, and quantita-
tive metallography He developed Beth Star 80, Bethlehem's 80 ksi yield strength plate grade
He was heavily involved with hneplpe orders and headed HRL's involvement with the North-
ern Border and Trailblazer projects His work earned him the D J Bhckwede Research Rec-
ognmon Award in 1982 He held four patents and authored or coauthored thirty papers He
was a senior research engineer at the time of his death

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42 METALLOGRAPHYPAST, PRESENT, AND FUTURE

In 1983, Halle received ASTM's Award of Merit and in 1977, he was named (along with W
W Bayre) coreclplent of the first L L W y m a n Memorial Award from E4 He received the
Michael Tenenbaum Award in 1986 for the best paper at the 1985 Mechanical Working and
Steel Processing Conference of the Iron and Steel Society of the American Institute of Mining,
Metallurgical, and Petroleum Engineers, "Statistical Analysis of the Trailblazer Plate Chem-
istry, Processing and Property Data Base to Optimize X-70 Llneplpe Requirements" Halle
believed in living life to its fullest--he worked hard, he played hard He was enthusiastic, even
to excess, he was brash but lovable

Francis Joseph Warmuth

(born 31 May 1937 in Utica, New York)


Fran was chairman of E4 from 1986 to 1990 following service as First Vice Chairman from
1982 to 1986 and secretary from 1979 to 1982 He is currently Chairman of Sub 8 since 1989,
and was the founding chairman of Sub 17, serving from 1977 to 1983 Fran received a B.A
degree in Chemistry from Utica College of Syracuse University in 1958 He joined Special
Metals Corporation m 1958 and served in a number of positions, particularly as supervisor of
the Metallography Department from 1963 to 1984 Fran took an early retirement offer from
Special Metals in 1986 a n d j o i n e d Leco Corp in 1987 In 1988, hejolned the Cameron Forged
Products Division of Cooper Industries in Houston, Texas as supervisor of metallography
Fran has had a hfelong interest in photography and he led the work on Guide E 883 He has
one patent and has pubhshed a dozen papers He is a fellow of ASTM and received the L L
W y m a n Memorial Award

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VANDER VOORT ON HISTORY OF COMMITTEE E4 43

George Frederic Vander Voort

(born 1 September 1944 in Philadelphia, Pennsylvama)


George is the current ASTM chairman having served as first vice chmrman and second vice
chairman previously He has been chairman of Sub 14 on quantitative metallography since
1982 He was a coorgamzer of MiCon 86 and chairman of the MiCon 90 conferences, and
cochalrman of the Metallography Past, Present, and Future (75th Anmversary Volume) sym-
posium. He ~s the primary author of seven ASTM standards and is the current E4 represen-
tative to the International Standardization Orgamzatlon
George received a B S in metallurgical engineering from Drexel University m 1967 and an
M S in metallurgy and materials science from Lehigh Umverslty m 1974 In 1967, he joined
the metallurgical department of the Bethlehem Plant of Bethlehem Steel Corp. where he held
various positions In 1972, he transferred to Bethlehem's Homer Research Laboratory where
he was a research engineer m the metallurgical services and investigations group In 1983, he
joined Carpenter Technology Corp. as supervisor of their metal physics research group
George is well known for his work in light microscopy, particularly for color etching tech-
niques, and for his work in linage analysis He is the author of over eighty pubhcatlons includ-
ing Metallography: Principles and Practice (McGraw-Hill, 1984) He has been active with the
American Society for Metals (ASM) as an instructor in their Metals Engineering Institute and
for their video course, Principles of Metallography. He is a fellow of ASM as well as ASTM
He has also been active with the International Metallographic Society and was their president
from 1981 to 1983 George is an avid photographer and hiker and enjoys reading mystery
stones

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44 METALLOGRAPHYPAST, PRESENT, AND FUTURE

Committee E4 Notables

Paul Adams Beck

(born 5 February 1908 m Budapest, Hungary)


Paul Beck chaired Sub II on terminology (1948-1950), starting the work that led to the vast
expansion o f E 7, and Sub III on nomenclature (1949-1960) He set up the prestzg~ous rater-
national committee of phase diagram experts that produced E 157
Beck studied mechanical engineering at the Royal Hunganan Technological InsUtute m
Budapest and then recewed an M S m metallurgy at the M~ch~gan Technological Institute in
1929 Next, he performed post-graduate work w~th M~chael Polanyl at the Kaiser Wilhelm
InsUtute of Metallurgy in Berhn and with Pierre Auger at the University of Paris His Industrial
career began m 1931 as a research engineer with the Vatea Electric Company m Hungary In
1933, he joined the Institute of Chemistry and Physics in Pans, followed by work as a patent
engineer m Budapest m 1935 Returning to the Umted States m 1937, he was a research met-
allurglst with the American Smelting and Refining Co in New Jersey In 1941, he joined the
Berylhum Corp (Reading, Pennsylvania) as chief metallurgist Then, in 1942, he became
superintendent of the metallurgical laboratory o f the Cleveland Graphite Bronze Company
In 1945, he entered academia as an associate professor of metallurgy at Notre Dame Pro-
moted to professor m 1949, he moved to the Umverslty of Illinois in 1951 as a research pro-
fessor In 1976, he officially retired, although he has continued active research on spmglass
alloys
Professor Beck has recewed numerous awards for research He is a fellow of the American
Physical Society, The Metallurgical Society of the American Institute of Mining, Metallurgi-
cal, and Petroleum Engineers (AIME) and the American Society for Metals (ASM) Interna-
tional and a member of the National Academy of Engmeenng He recewed the Mathewson
Gold Medal Award of AIME, the Albert Sauveur Achievement Award of ASM, the Alexander
Humboldt Award, the Heyn Memorial Award of the German Metallurgical Society, and he is
an honorary member of the Hungarian Physical Society He received an honorary doctorate
from the Montanumvers~tat m Leoben, Austria in 1976

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VANDER VOORT ON HISTORY OF COMMITTEE E4 45

John James Bowman

(born 29 May 1907 m Mlllersburg, Pennsylvanm, died 10 October 1950)


John Bowman was E4's third secretary, holding that office from 1936 to 1946 He became
secretary of Committee B7 on Light Metals and Alloys m 1944 and held that posmon until his
death from a heart attack at age 43 m 1950 He was also a sub chairman for Committee B6 on
Die-Cast Metals and Alloys and was acUve with the ASTM Pittsburgh D~stnct, serving two
terms as its chairman
Bowman graduated with honors from Pennsylvania State College (now University) in June
1929 with a bachelors degree in electrochemical engtneenng After graduation, he joined the
A l u m i n u m Research Laboratories of ALCOA Dunng the WWII, he served on the War Pro-
ductlon Board in Washington in the Conservation Dwlslon From 1943 to his death, he was
executive assistant to the chief metallurgist

Robert Schoiley Busk

(born 13 December 1915 in Brooklyn, New York)


Robert Busk chaired Sub II on terminology from 1951 to 1955 continuing the work started
by Paul Beck, the masswe enlargement o f E 7 He received a B.A in chemistry from Colgate
University (1937) and a D Eng in metallurgy from Yale University (1940) Joining Dow
Chemical Co. in 1940, he became director of the metallurgical laboratory (1956-1966), busi-
ness manager of wrought products (1963-1966), R&D manager of the Metal Products Depart-
ment (1966-1972), and assistant &rector of research (1968-1972) He retired from Dow in
1972 and opened his own business, International Magnesium Consultants, Inc
Busk is a fellow of the American Society for Metals International In ASTM, he was also a
m e m b e r of B6 and B7 and served as chmrman of subcommittees B06 07 and B07.04 He has
also been very active in the International Magnesmm Association serving as a member of their
board from 1978 to 1987 He was named an honorary lifetime member in 1988 He ~s the
author of Magnesium Product Design (Marcel Dekker, 1986) and holds 15 patents
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46 METALLOGRAPHYPAST, PRESENT,AND FUTURE

Theresa Mary (Vandecar) Brassard

(born 3 January 1929 in Cohoes, New York)


Theresa served as E4 membership secretary from 1979 to 1981, worked with the ASTM
photographic contest and was a major contributor to E 768, particularly with regards to the
DIC photographic adjunct She served as secretary for Subs 1 and 17 and was a participant in
several task groups She will be remembered always for her innovative use of available mate-
rials in specimen preparation (for example, yellow tablet paper or brown paper towels rather
than cloths for pohshmg, "Never-Dull--the Original Magic Wadding Polish" for field polish-
mg ship propellers, etching BI-50 Sn with "Fresca," and so on)
Theresa gained her knowledge of metallography through selected courses at local colleges,
the American Sooety for Metals (ASM) Metals Engineering Institute courses and U S Army
correspondence courses, plus on-the-jobtrial-and-errorexpenmentatlon Shebegan hercareer
m 1953 as a metallographlc technician with Allegheny Ludlurn's research laboratory in Water-
vllet, New York In 1959, she joined the corporate R&D Center of the General Electnc Co in
Schenectady as a metallographer m the metals and ceramics laboratory In 1967, she became
a metallographer at the Benet Weapons Laboratory, ARRADCOM, of the Watervhet Arsenal,
Watervhet, New York. In 1983, she moved west, becoming a metallographer m the quahty
assurance laboratory at Long Beach Naval Shipyard, Long Beach, Cahforma. She retired in
1988
Theresa has also been acUve m ASM, with the Eastern New York chapter, and with the
International Metallographlc Sooety (IMS) She received several awards for her work with the
Eastern New York ASM chapter (President's Award in 1974 and 1977) and received the ASM
Metallurgical Engineering Assistants Award In 1975 Between 1959 and 1987, she received 37
awards in metallographic and ceramographlc contests sponsored by ASM, 1MS, ASTM, and
ACS.

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VANDER VOORT ON HISTORY OF COMMITTEE E4 47

William Campbell

(born 24 June 1876 m Gateshead-on-Tyne, England, died 16 December 1936)


Campbell, first chairman of Sub I and main author of standard E 2-17T, graduated from
Kang's College, London, m 1892, then studied at St. Kenelm's College, Oxford, from 1892-
1894 He recewed an assocfate in science degree from Durham University College of Science
in 1896, a B S degree m 1898, an M S. m 1903 and a D Sc in 1905 He came to Columbia
Umverslty m 1902 as University Fellow and was a Barnard Fellow the following year He
became an instructor m Metallurgy m 1904, adjunct professor m 1907, associate professor in
1912, and full professor m 1914 In 1924, he became the first Howe professor of metallurgy at
Columbia Aside from his academic experience, Campbell worked as a metallographer for the
U S Geological Survey (1907-1911) and the Bureau of Mines (1911-1921) Dunng World
W a r I, he was a metallurgist at the Brooklyn Navy Yard. In 1918, he was a lieutenant com-
mander m the Naval reserve, and he maintained this activity for many years
Campbell joined ASTM in 1903 and was Chairman of Committee B2 from its organization
m 1909 untd his retirement from Columbia in 1934 He was made honorary chairman of B2
He collected corns, both modern and ancient. He was often requested to clean and restore
ancient corns for various museums and collectors He published about fifty papers mclud-
lng"A List of Alloys" (ASTM Proceedings, 1992, revised m 1930), one of the earliest collec-
tions of alloy designations and compositions

George Frederick Comstock

(born April 1886 m New York, New York, died 2 August 1982)
George Comstock was E4's first secretary (1921 to 1930) and chaired Sub I twice, 1927-
1928 and from 1941 to 1947 As a chdd, his health was poor; hence, his schoohng began at
home by tutor Later, he recewed manual training at the Horace Mann School which spawned
a hfelong interest m woodworking His health improved with time and summers in the A&-
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48 METALLOGRAPHY PAST, PRESENT, AND FUTURE

rondacks By 1908, he had made 53 ascents of fourteen mountains in the Adirondacks, includ-
ing cutting of a trail up Giant Mountain
Comstock entered Columbia University and received A B and Met E degrees in 1907 and
1909 Chess dominated his spare time, playing fourth board on Columbia's Championship
team (his exploits were recorded in the New York Sun n e w s p a p e r - - a far cry from today v)
He began his professional career in 1909 with the Vanadium Alloy Company's smelter in
Newmlre, Colorado A dam burst during a flood which closed down the railroad line and shut
down the smelter He then joined the Maryland Steel Company at Sparrows Point, Maryland
(now part of Bethlehem Steel Corp,) and then with Crucible Steel Co of America in Pittsburgh
as assistant to the chief metallurgist In 1912, he joined the Titanium Alloy Manufacturing
Co (TAMCO) in Niagara Falls, being placed In charge of their new physical testing laboratory
(built at a cost of $10 0001) He progressed to chief metallurgist and was assistant director of
research from 1946 to 1951 when T A M C O became a division of National Lead Co He retired
in 1951, but remained active as a consultant until 1954
Comstock published numerous papers on the use of titanium in irons and steels and two
books--Titanium in Steel (with Stephen F Urban and Morns Cohen, published by Pitman
in 1949) and Titanium in Iron and Steel (pubhshed by John Wiley & Sons and by Chapman
& Hall for the Engineering Foundation in 1955) He was an abstractor for ChemicalAbstracts
for many years
Besides devoting his professional career to the development of titanium alloys and titanium
additions to iron and steels, Comstock was literally "branded" with titanium, as he liked to
tell people In 1930, an experiment went awry causing an explosion which sprayed him with
molten titanium, "the titanium brand," and several mflhgrams embedded in his body ever
afted

Constance Lovell (Beams) (Brodie) Craver

(born 14 May 1911 in Newark. New Jersey)


Connie was the E4 membership secretary from 1974 to 1976 and chairman of Sub 1 from
1968 to 1971 She was a member of most of the E4 subcommittees and was quite active with
the ASTM photographic contest, which she chaired in 1966 for E4's 50th anniversary meeting
Connie began her professional career as a dietitian after graduating from Pratt Institute in
Brooklyn In 1930, Edgar Baln of the U S. Steel Research Laboratory in Kearny, New Jersey
decided that metallography would be a good field for women He contacted Pratt Institute in
his search for a woman to tram Connie expressed an interest in trying laboratory work in this
newly emerging, but unknown, field She worked for Baln for a year but moved to Schenectady
after her m a m a g e finding employment at the General Electric Research laboratory as an assls-
t a n t m e t a l l o g r a p h e r w o r k l n g f o r L e R o y L W y m a n Eventually she became head ofthe metal-

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VANDER VOORT ON HISTORY OF COMMITTEE E4 49

lographlc section. She learned her trade the hard way by good, old fashioned on-the-job
tramlng.
Conme left General Electric in 1950 to work for Allegheny Ludlum at their Watervllet
research facility Again, she worked with another eminent pioneer, Dr Gunther Mohhng,
inventor of A-286 In 1955, she was a coreclplent of the Lounsberry Award for her study of
precipitation hardening of alloy A-286. Connie trained Theresa Brassard when Theresa began
her career at Allegheny Ludlum In 1959, the laboratory was transferred to their Brackenndge
facility
In 1970, Connie retired from Allegheny Ludlum Steel Corp However, Conme was not
ready to rest and play shuffleboard No, she joined Rensselaer Polytechnic Institute and was
gwen responslblhty for the graduate school metallographic laboratory Finally, in 1980, after
fifty years of metallography, she retired for good Conme o n c e said, "I feel like a pioneer since
I have been privileged to see metallography grow from more or less an art to a science. It has
been an excmng experience"

Edgar Hutton Dix, Jr.

(born 11 August 1892 m BalUmore, Maryland, died 26 January 1963)


"Dixie" graduated from Cornell University in 1914 with a bachelors degree in mechanical
englneenng He dld some postgraduate studles and taught matenals testmg at Cornell Hethen
entered industry at the Morse Chain C o , then the Baltimore Copper Smelting and Rolling
C o , then as chief of the testing department of the Bureau of Aircraft Production, next as assis-
tant engineer of tests of the Aluminum Castings C o , then as chief of the metals branch, eng~-
neenng division, U S Air Service In 1923, he joined the Aluminum Co of America and
became chief metallurgist of the New Kensington and Cleveland laboratories in 1930 He was
appointed assistant director of research m 1942 and stayed with them until retirement
Dlx joined ASTM in 1919 and was a member of six committees, serving as chairman of our
Sub I from 1928 to 1941 He is best known as the inventor of Alclad sheet, the first major
development of an aircraft structural material since Wllm's duralumin in 1910 Alclad revo-
lutiomzed mrcraft construction He also developed AI-SI alloys as a new class of alloys and
developed a theory for stress corrosion cracking (24th Edward de Mille Campbell Memorial
Lecture of the American Society for Metals in 1949) He also served as chairman of the Insti-
tute of Metals division of the American Institute of Mining, Metallurgical, and Petroleum
Engineers. Dix received numerous awards, for example, the FrancisJ Clamer Medal fromthe
Franklin InsUtute in 1947, the Frank Newman Speller Award from the National Assocmtaon
of Corrosion Engineers m 1954, the Distinguished Public Service Award from the U S Navy
m 1958, and an honorary doctorate from the Carnegie InsUtute of Technology in 1958

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50 METALLOGRAPHYPAST, PRESENT,AND FUTURE

George Austin Ellinger

(born 31 October 1900 in Lewlstown, Pennsylvania, died 27 Apnl 1985)


George Elhnger chaired Sub IV on photography from 1957 to 1968 and was active with the
ASTM photographic contest He was also active in Committees A5, B3, E25, and G1 He
received a B.S degree in mining and metallurgy in 1922 from Pennsylvania State College
Later, he took additional courses at the National Bureau of Standards (NBS) graduate school
George began h~s career in 1922 with the Standard Steel Works Co in Pennsylvania, as a
laboratory metallurgist In 1923, he joined the Atchison, Topeka & Santa Fe Railroad Co in
Kansas, as a metallurgist Two years later, he joined the Page Steel & Wire Co in Pennsylva-
nia, as chief chemist In 1927, he became a research metallurgist with Page In July, 1929, he
joined the metallurgy division of the National Bureau of Standards as an assistant physicist
In 1936, he became an associate metallurgist, then metallurgist in 1940, senior metallurgist in
1944, chief of the optical metallography section in 1946, chief of the corrosion section in 1950,
and in 1962, he was named chief of the Metal Reactions section and Assistant Chief of the
Metallurgy Division He retired on 1 January 1968 but remained active as a consultant
One of his first major efforts at NBS was the study of broken bridge wire from the failed Mt
Hope bridge This work was followed by studies of the weldablhty of armor plate, high tensile
strength steels, and some nonferrous alloys This knowledge was applied subsequently to the
construction of tanks and other armored vehicles where welding replaced riveting. Later, he
was deeply involved with the study of failures o f Liberty ships and T-2 tankers that occurred
during World War II.
Elhnger received the A S T M award of merit in 1967 His welding stu&es were honored by
the Lincoln Gold Medal of the American Welding Society in 1942 and the Meritorious Service
Award of the Department of Commerce in 1949.

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VANDER VOORT ON HISTORY OF COMMITTEE E4 51

Samuel Epstein

(born 27 November 1896 in Russia, died 15 Apnl 1972)


Sam Epstein, the first chairman of Sub IX on inclusions (1940-1965), was the pnnclpal
author of E 45 (one of the most widely cited ASTM standards) and its two major revisions in
1960 and 1962 His parents emigrated to Amenca and settled m Brooklyn when Sam was a
child Epstein graduated from the College of the City of New York (CCNY) in 1918 with a
B S in chemistry He took an Army Ordnance course in metallurgy at Carnegie and then was
stationed by the Chemical Warfare Service in the metallurgy &vision of the Bureau of Stan-
dards, Washington, D C He stayed at the Bureau until 1929 While at the Bureau, he was a
special student at George Washington University receiving an M.S m 1929 He developed an
automatlcpollshlngdevlcewhlleattheBureau Hejolned the Carnegle-Illinols Steel Co (later
part of U S Steel Corp ) in 1929 and in 1930, joined the recently formed Battelle Memorial
Institute in Columbus, Ohio
At Battelle, he authored volume 1 of Alloys of Iron and Carbon (McGraw-Hill, 1937) Also,
while at Battelle, he discovered that steels could be made fine grained by additions of small
amounts of aluminum and later determined that aluminum nitnde was responsible for grain
size control, not aluminum oxide as widely believed In 1932, he received ASTM's Dudley
Metal for his paper on embnttlement of structural steel by the galvanized zinc coating He
joined Bethlehem Steel's research department on 8 June 1936 and remained there until his
retirement on 31 January 1964 From 1950 to 1958, he was division head of the Steel Products
section of the research department. He developed the first nonagmg rimmed steel, developed
mtrlded ferrromanganese (for adding nitrogen to steel), did ploneenng work on leaded steels
(for improved machlnablhty), and developed a high-strength nvet steel He also did research
on the Fe-N phase diagram During World War II, he worked on beanng alloys for rolling mills
with a reduced tm content, tin being in short supply For this work, the Assocmtlon of Iron
and Steel Engineers gave him (and coauthor Richard C Hess) the John Frederick Kelly Award
in 1944 He developed a weathenng type structural steel, Mayarl R He received the Bradley
Stoughton Award of the Lehigh Valley Chapter of the Amencan Society for Metals in 1950
He received the ASTM Award of Ment in 1966. After retirement, he (and Robert E Somers)
rewsed the Welding Research Council book Weldability of Steels (2nd edmon, 1971)

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52 METALLOGRAPHYPAST, PRESENT, AND FUTURE

Donald Ira Finch

(born 20 July 1907 in Grand Rapids, Michigan, died 28 September 1981)


Don Finch was chairman of Sub VII on Thermal Analysis from 1951 to 1970 and chairman
of Sub X on Research from 1968 to 1974 Don was also involved with the ASTM photographic
contest Finch received a B S in chemical engineering from the University of Michigan in
1929 Don pursued graduate studies, but left in 1930 to join Leeds and Northrup Co and
worked for them until 1972 He was a research metallurgist from 1930 to 1933 and 1935 to
1945, chief of the R&D metallurgical division from 1945 to 1955, head of the R&D metallur-
gical section from 1955 to 1968, then principal scientist from 1968 until retirement in 1972
Flnch's work centered on metals and alloys used with or within furnaces and furnace instru-
mentation He was also involved with temperature measurement systems for nuclear reactors
Don joined ASTM in 1945 Besides his E4 activity, he was a founding member and chair-
man of E20 on Temperature Measurements Don also served as a member of the ASTM board
of directors from 1971 to 1974 He chaired the Advisory Committee on Thermocouples to the
National Bureau of Standards and served as vice president and president of the Philadelphia
Chapter of the American Institute of Mining, Metallurgical, and Petroleum Engineers
Finch received numerous awards He was an honorary member of ASTM and a fellow. He
received the E20 Robert D Thompson award for 1976

William LaVilla Fink

(born 14 September 1896 in Falrmount, Indiana, died 2 April 1992)


Bill Fink studied at the University of Michigan receiving his B S E (1921), M S E (1923),
and Ph D in Chemistry (1926) Fink's thesis work at Michigan, under Edward DeMille Camp-
bell, utilized X-ray diffraction and showed that the strengthening phase in steels, martenslte,
was a solid solution of carbon in iron with a body-centered tetragonal crystal structure Prior
to this work, martenslte was believed to consist of extremely fine fernte grains Flnk measured
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VANDER VOORT ON HISTORY OF COMMITTEE E4 53

the lattice parameters and was the first to define the c/a ratio He also showed that tempenng
ehmlnated the bct structure producing a bcc structure. After this important contribution to
the understanding of the strengthening of ferrous alloys, Fink joined the Aluminum Co of
America in 1925 and never worked on Fe-based alloys again v He was chief of the physical
metallurgy division ( 1943-1958), then science coordinator until he retired in 1961 He taught
physical metallurgy at the Carnegie Institute of Technology (1936-1937) He was one of the
founders of the Joint Committee on Powder Diffraction Standards (JCPDS), later served as its
chairman He joined E4 m 1930
Flnk, an expert in X-ray techniques, served as chairman of Sub VI on X-Ray Methods from
1938-1960 and of Sub III on Nomenclature from 1960-1978 He is known as the "father" of
E 157 and played a major role in the development of E 391 The "Fink Method" for identi-
fying unknowns using the JCPDS Search Manual was named in his honor He served on the
ASTM Board of Directors (1958-1961), received the Award of Merit m 1956 and was made
an honorary member in 1966 He was also a member of E7 He received the C H Mathewson
Award of the American Institute of Mining, Metallurgical, and Petroleum Engineers for his
publication (with D W Smith) on the theory of precipitation hardening. Fink published over
forty papers and held twelve patents He was a fellow of the American Association for the
Advancement of Science

Leon Victor Foster

(born 11 August 1895 in Fulton, New York, died 26 July 1971)


Leon Foster was chairman of Sub 4 on Photography from 1934 to 1951 and was actwe with
the ASTM photographic contest He received a B S m liberal arts from Syracuse University
m 1917 He joined Bausch & Lomb Optical Co in 1917 and spent his entire career with them
From 1917 to 1920, he was a "computer," from 1920 to 1926, a lens designer, then group
leader (1926-1932), and section head (1932-1945) of the lens design group From 1945 to
1950, he was acting head of the science bureau of the microscope design section In 1950, he
became director of the defense engmeenng department, and, in 1960 he was liaison engineer
until he retired at the end of 1960
Foster developed the legendary Foster calcite pnsm used with B&L metallographs to pro-
duce polarized light This prism was apparently rather challenging to construct but did pro-
duce superb polarized light and was highly regarded by users who depended on it to study
metals and alloys, such as beryllium, uranium and its alloys, niobium, and zirconium and Its
alloys
Foster joined ASTM In 1932 and was also active with D20 (Plastics), A3 (Cast Iron), El2
(Appearance), and D 13 (Textile Matenals) He was a member of the Optical Society of Amer-
ica, the American Microscopical Society, the Society of Motion Picture and TV Engineers,
and the Electron Microscopy Sooety of America
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54 METALLOGRAPHYPAST, PRESENT, AND FUTURE

Marcus Aurelius Grossmann

(born 15 September 1890 in Youngstown, Ohio, died 21 May 1952)


Grossmann, E4's first vice chairman (1936-1944) and chairman of Sub VIII on grain size
from 1937 until his death in 1952, played a major role in developing E4's gram size standards
that led to E 112 (three years after his death) Grossmann, famous for his work on hardena-
blhty, recewed a B S from the Massachusetts Institute of Technology (MIT) in 1911, later
recewed a D Sc from Harvard m 1930
After a year as an assistant at MIT, Marc joined Pittsburgh Testing Laboratories (1912-
1915), then Vanadium Corp of America ( 1915-1917), the Bureau of Standards ( 1917-1919),
again at Vanadium Corp (1919-1920), then the Electric Alloy Steel Co which became the
Atlas Steel Corp (1920-1924), next the Umted Alloy Steel Corp which became the Central
Alloy Steel Corp and later the Republic Steel Corp (i 924-1931), and, finally, the Illinois Steel
Co which became the Carnegie-llhnols Steel Corp and later part of the U S Steel Corp (1931
until his death in 1952) He became director of research at Carnegie-Illinois in 1935
Grossmann was noted for his wit, his wide range of knowledge, his skills m writing and
speaking A series of his lectures became the well known book, Principlesof Heat Treatment,
published by the American Sooety for Metals (ASM) in 1935 The fifth edition (1964) was
revmed by Edgar Bain after Grossmann's death He also translated Emil Heyn's book, Physical
Metaliography, pubhshed m 1925 by John Wiley Together with Baln, they pubhshed High
Speed Steel with John Wiley m 1931
Grossmann received numerous major awards for his work His doctoral thesis ("Oxygen in
Steel"), under Albert Sauveur, was the subject of his Campbell Memorial Lecture in 1930 His
paper on "Hardenabihty and Quenching, and Some Quantitative Data" (Transactions, ASM,
194 l, co-authored with M Asimow and S F. Urban) received the Henry Marion Howe Medal
while his paper "Hardenablllty Calculated from Chemical Composition " (Transactions,
AIME, 1943) received the Robert W Hunt Gold Medal He was a chairman of three different
ASM chapters, national trustee ( 1939-1941), vice president (1942) and president (1943) of the
American Society for Metals

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VANDER VOORT ON HISTORY OF COMMITTEE E4 55

Joseph Donald Hanawalt

(born 6 July 1902 in Royersford, Pennsylvama, died 26 June 1987)


Don Hanawalt was a long time member of Sub VI of E4, beginning in 1935, a member of
E7 since 1941, and was a founder and chairman of the Joint Committee on Powder Diffraction
Standards (JCPDS) Don studied at Akron University and Jumata College He received an
A B from Oberhn College m 1924, an M A from the University of Wisconsin m 1926, and a
Ph D in physics from the University of Michigan m 1929 He was a National Research Coun-
cd Fellow, Rockefeller Foundation from 1929 to 1931 and an International Research Fellow
at the University of Gronmger (the Netherlands) in 1931 He joined Dow Chemical Co as a
physicist m 1931, advancing to director of the spectroscopy laboratory m 1934, director of
metallurgical research m 1940, head of the magnesium department in 1946, vice president m
1953 and vice president of Dow Metal Products m 1959 He retired m Apnl of 1964 and joined
the University of Michigan as professor of chemical and metallurgical engxneenng where he
taught and continued his interests m magnesium technology until 1972
The publlcanon of his landmark paper on chemical analysis by X-ray dlffracnon m 1938
opened the way for the implementation of a powerful new tool The data pubhshed m this
paper became the foundation for the ASTM card file for compound ldennficatlon, now under
control of JCPDS In his magnesium research, his 1941 paper estabhshed the influence of
heavy metal impurities, for example, iron, mckel and copper, on the corrosion rate of mag-
nesium and magnesmm alloys From this work evolved a number of alloys with vastly
improved corrosion resistance He also developed a fluxless melting procedure for melting
magnesium, for which he received the Directors Award from the Magnesium Association m
1972 He held 30 patents and received a number of awards, for example, the Mathewson Gold
Medal of the Insntute of Metals of the American Insntute of Mining, Metallurgical, and Petro-
leum Engineers (1943), and the Gold Medal of the American Sooety for Metals (1965) He
was a Fellow of ASM and ASTM

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56 METALLOGRAPHYPAST, PRESENT, AND FUTURE

Oscar Edward Harder

(born m 1883 m Frankhn County, Arkansas, died 10 July 1956)


Oscar was the second secretary of E4, serving from 1930 to 1936 His parents were pioneers,
traveling by covered wagon from Tennessee to Arkansas where he was born m a log cabin
While a boy, they moved to Texas and later to Oklahoma in a prairie schooner Although he
never graduated from either grade school or high school, he was admitted as a special student
to the University of Oklahoma m 1905 He received a B A m chemistry in 1910 and an M S
m 1911 After a brief period of employment as a food chemist, he enrolled at the Umverslty
of Illinois m Urbana and received a doctorate m chemistry in 1915
His first contact with ASTM came at the Lewis Institute in Chicago where he stu&ed cement
and concrete for an ASTM research committee and the Portland Cement Assoclatmn Next,
he held an alloy scholarship ( 1918-1919) at the Mellon Institute of Pittsburgh studying ura-
nium In September 1919, he succeeded Samuel L Hoyt as professor of metallography at the
Umverslty of Minnesota In his eleven years there, he taught a unique course m dental met-
allography and &d work on gold alloys, drill rod, bearing alloys, rail steel, and steel castings
In 1930, Oscar came to the Battelle Memorial Institute (founded in 1929) as assistant direc-
tor He retained this posmon until his retirement in 1949 and continued as a technical advisor
and consultant until his death m 1956 at age 73 He held more than 100 patents in twenty
counmes for his developments He is best known for two developments, leaded steels known
as "ledloy" and a corrosion-resistant, nonmagnetic alloy for watch spnngs called "elglloy"
(40Co-20Cr- 15N1-7Mo-2Mn- 15Fe-0 15C-0 05Be heat treated to 380 ks1 tensile strength, 702
HB)
Harder was active with several technical societies He was a trustee ( 1930-1932), vice-pres-
ident (1940), and president ( 1941 ) of the American Society for Metals (ASM) He was presi-
dent of the Minnesota Section of the American Chemical Society and was a section editor of
ChemicalAbstracts (1930-1953) He received the Henry Marion Howe Medal in 1928 for his
paper "Studies on Normal and Abnormal Carbunzing Steels" (Transactions, ASM, 1928)

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VANDER VOORT ON HISTORY OF COMMITTEE E4 57

Henry Marion Howe

(born 2 March 1848 m Boston, Massachusetts, died 14 May 1922)


Howe, first president of ASTM, a founding member of E4 and main author of standard E
3, was the nation's outstanding metallurgast of his day His father, Dr Samuel Gndley Howe
left for Greece shortly after recewmg his medical degree and parUclpated for six years m their
war for independence He pubhshed a History of the Greek Revolution m 1828 Returning to
America m 1831, he began working w~th the blind and headed the Perkins Institute for the
Bhnd His mother, Juha Ward Howe, author and reformer, began pubhshmg poems at age 16
She wdl be forever remembered for her "Battle H y m n of the Repubhc" written to the tune of
"John Brown's Body" whde she was at the front during the Cwd War (1861).
Howe attended the Boston Latin School, then entered Harvard graduating m 1869 with an
A B degree He recewed a B S from the Massachusetts Institute of Technology (MIT) m 1871,
and an A M degree m 1872, m metallurgy, from Harvard He then spent a year m Troy, New
York studying the production of iron and steel and in 1872 became superintendent of the
Bessemer Steel Works m Johet, Illinois followed by the Blmr Iron & Steel Co (1873-1874)
Next, he spent five years on the metallurgy of copper m Chde and designing plants m Quebec
prownce and Bergen Point, New Jersey for the Orford Copper & Nickel C o , followed by man-
aging the Plma Copper & Smelting Co of Arizona This work was the nucleus of his first book,
Copper Smelting, pubhshed m 1885
At age 35, he changed his career path and became a consultant m Boston whde also teaching
at MIT untd 1897 when he was offered the chmr of metallurgy at Columbm Umverslty He
remained their untd retirement in 1913, as professor emeritus He continued to perform
research at his laboratory at h~s home "Green Peace" m Bedford Hdls, New York, untd his
death in 1922 at age 74 He also acted as a consultant to the Bureau of Standards from 1918
untd h~s death
In 1891, Howe pubhshed The Metallurgy of Steel, which collected all of the knowledge at
that u m e on steeimakmg, be ~t m Enghsh, French, or German Th~s book &d much to change
steelmakmg from an art to a science In 1903, he pubhshed Iron, Steel, and Other Alloys, and
in 1916, The Metallography of Steel and Cast Iron (m two parts). This later book was an mtro-
ducUon to the new science of metallography In 1910, Howe chmred an international com-
mittee on nomenclature under the International Assocmt~on for the Testing of Materials The
other U S delegates were W d h a m Campbell and Albert Sauveur whde the foreign delegates
were Flons Osmond and Leon Gudlet (France), H C H Carpenter, John E Stead and Walter
Rosenham (England), Carl Benedlcks (Sweden), F Wust and Emd Heyn (Germany), and A
Stansfield (Canada) Howe named the constituents femte, cemenute, and pearllte (the latter
based on Henry Clifton Sorby's "pearly" constituent) and the term eutecto~d
Howe was very active m professional orgamzat~ons, besides serwng twice as president of
ASTM In 1893 he was president of the American Institute of Mining, Metallurgical, and

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58 METALLOGRAPHYPAST, PRESENT,AND FUTURE

Petroleum Engineers which he joined m 1871 He was acting president of the International
Assocmtlon for Testing Materials (1902-19 t 2) He recewed a host of honors, including three
honorary doctorates and medals from many countries, including Russia, France, England,
Germany, and Sweden He was a prohfic author with over 300 publlcaUons to his credit

Frederick Charles Hull

(born 9 November 1915 in Alliance, Ohio)


Fred Hull was chairman of Sub I from 1951 to 1959 and was an active contributor to E4's
grain size standards He developed improved approaches for performing companson grain size
ratings and the approach used when working at magnifications other than that of the chart
Fred received a B S in metallurgy from the University of Michigan in 1937 and a D Sc in
metallurgy from Carnegie Institute of Technology in 1941
Fred spent his entire professional career w~th Westinghouse at their research laboratories In
Pzttsburgh He started in 1941 as a research engineer In 1951, he was made manager of the
metallurgical sectton, in 1954 he became assistant manager of the metallurgy department, and,
m 1957, he was named advisory metallurgist He retwed in 1981 but worked as a part t~me
consultant unnl 1985
Besides his life long interest an grain size work, Fred has been active m alloy development
He is the inventor of Dtscaloy, a h~gh temperature alloy, and Kromarc, a stainless steel He
has eleven patents and twenty-s~x pubhcauons
In 1962, Fred received ASTM's Charles B Dudley medal for his paper "Effects of Alloying
Elements on Hot Cracking of Austenmc Stainless Steels" In 1974, he received the James F
Lincoln medal of the Amencan Welding Society (AWS) for his paper"Effects of Composmon
on Embnttlement of Austenmc Stainless Steels." The Institute of Metals (London) gave Fred
an "Elegant Work" award in 1989 for his paper"Plane and Spatml Charactenstlcs of Equmxed
Beta Brass G r a m s " Fred is a Fellow of the Amencan Society for Metals

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VANDER VOORT ON HISTORY OF COMMITTEE E4 59

Zay Jeffries

(born 22 April 1888 m Wdlow Lake, South Dakota, died 21 May 1965)
Zay Jeffnes, one of the outstanding metallurgists of this century, recommended that E4
establish a subcommittee on the new field of X-ray diffraction and was Sub VI's first chmrman
(1924-1930) Jeffnes developed the plammetnc method of grain s~ze measurement that was
incorporated into E4's first standard, E 2, and is now m E 112 He was a graduate of the South
Dakota School of Mines (mechamcal englneenng, 1910) and became an instructor at the Case
School of Applied Science m 1911 His first major paper was gwen at the February 1916 meet-
lng of the American Institute of Mining, Metallurgical, and Petroleum Engineers, on "The
Determination of Grain S~ze m M e t a l s " Zay stu&ed w~th Albert Sauveur at Harvard and
received his Ph.D. m 1918 for his study of secondary recrystalhzatlon
Jeffnes must have been an mcre&bly busy person as he led two careers s~multaneously. He
was a consultant to the lamp &ViSIOn of the Cleveland Wire Works ( 1914-1925) of the General
Electric Co (GE) and to the Cleveland &vision (1920-1936) of the Alcoa Research Laboratory
(he was &rector of research (1916-1920) of the Lymte Laboratory of the Aluminum Casting
C o , taken over by Alcoa m 1920). After six years of teaching at Case, he dwlded his t~me
between Alcoa and GE W~th R. S Archer, Zay developed aluminum alloys 2025, 5051, and
2014 and they wrote the popular book, The Science of Metals, m 1924 Jeffnes headed Alcoa's
research laboratory m Cleveland and Edgar Dlx headed the one m New Kensington, Penn-
syivanm With GE, he worked on problems with tungsten filaments, for example, the sag prob-
lem He installed the first X-ray spectrometer used by industry and hired a young graduate by
the name of Edgar Colhns Barn to operate it Barn later became a pioneer m the use of X-rays
and had an outstanding career with U S Steel (he was also an E4 member) W~th GE, he was
a consultant to the incandescent lamp department ( 1925-1936), techmcal &rector of the lamp
department (1936-1945), and vice president of the chemistry department (1945-1949). He
was Chairman of the Board of their subsldmry, The Carboloy C o , which produced smtered
carbide cuttmg tools He retired m 1950
Jeffrles suceeded Henry Marion Howe and Albert Sauveur as metallurgy's representaUve to
the National Academy of Science D u n n g World War II, he was chmrman of the Office of
Production Management on Strategic Metals He was president of the American Society for
Metals in 1941 As m~ght be expected, Zay recewed nearly every major award, several hon-
orary degrees, and was on the board of several restitutions

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60 METALLOGRAPHYPAST, PRESENT,AND FUTURE

Horace Hardy Lester

(born 30 December 1883 in Shelburn, Indiana (see below), died on 11 November 1955)
Horace Lester ("Doc") was chairman of Sub VI on X-ray Methods from 1937 to 1938 His
pioneenng 1926 Sub VI report became the first ASTM standard on radiographic testing, E 15-
26T He was the founding chairman o f Committee E7, from 1938 to 1948 He was also active
with the Joint Committee on Powder Diffraction Standards He received the ASTM Award of
Merit in 1951 and was made an honorary member in 1953
Lester was the son of Mark and Sarah Jane (Rigley) Lester who were m a m e d in England in
1878 and emigrated to the United States in 1879 They settled in Shelburn, Indiana and began
naturalization proceedings However, in 1883, they rented their house for an indefinite penod
and returned to England Horace was born in the home of his maternal grandmother in Aws-
worth, Nottinghamshire, England He was about nine months old when the Lesters returned
to Shelburn, which he used as his legal birthplace When he was three, they moved to Carhsle,
Indiana where he grew up He graduated from Carlisle High School in a class of two students)
The high school program was for only three years Lester graduated from Vincennes Univer-
sity preparatory department m 1902 He worked his way through school at Vincennes Um-
vers~ty Jumor College graduating m 1904 He was a bus boy at the Grand Hotel m Vincennes
and tended the coal furnace m the home where he was staying Dr Eugene Manchester, pres-
ident of Vincennes Umverslty, took an interest m Lester's mathematical and scientific skills
and progress Manchester took a job with the Umverslty of Minnesota and Lester went with
him After recexvlng his bachelor's degree at Minnesota m 1906, Horace moved to the Um-
verslty of Washington where he obtained a master's degree in 1912 Again, he worked to cover
his hving expenses, this nine as a high school teacher m Anacortes (1906-1908) and m Bel-
lingham (1908-1910) where he taught botany and astronomy He became a night watchman
for fishing traps and began smoking a pipe (forever after!) He moved back east to Pnnceton
University where he received a Ph D in physics in 1915 He returned to the University of
Washington as an instructor (1915-1917) This was interrupted by World War I when he was
enlisted to install radio eqmpment on naval vessels m the Puget Sound Navy Yard (1917-
1920)
Lester again returned east and worked briefly for Westinghouse Lamp Co (Bloomfield, New
York) from 1920-1921, then took a teaching posmon at the Case School of Apphed Science
in Cleveland He had barely settled m at Case when he recewed an offer to work at the Water-
town Arsenal Laboratory General Tracy C Dickson had obtained X-ray eqmpment for radm-
graphic testing and X-ray dlffracnon, both areas were new at that time Dr F C Langenberg,
head of the laboratory, recruited Lester for the new posmon created by Dickson He started as
a research physicist m July, 1922 and, within a year, published "Radmgraphy of Metals," and
" X - R a y Examination of Steel Castings" The following year, 1924, he pubhshed (with the
A m e n c a n Society for Steel Tesnng (ASST), later the Amencan Society for Metals (ASM)) "X-
Ray Tests Apphed to Problems of the Steel Foundry" for which he received the Henry M a n o n
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VANDER VOORT ON HISTORY OF COMMITTEE E4 61

Howe medal in 1925 Lester quickly recogmzed the need to standardize radiographic tests
which led to his hfelong involvement with ASTM E4 and E7
Mary Norton reported that when Doc was doing desk work, he generally put on his lab coat
(rarely used when he did experimental work)), and an old peaked cap and then fired up his
pipe On a Saturday afternoon one summer, Arsenal personnel had left for home and their
month long vacation About an hour later all of the Building 73 employees who could be
reached by telephone were summoned back to work On the front lawn, General Dlckson was
conducting an mveshgatlon of a small fire that was discovered m Building 73 just after noon
The fire was caused by a nail that was d n v e n through a section of BX cable The fire had broken
out above a door on which Doc's lab coat was hanging The general was lambasting Lester's
p~pe for causing the fire since he knew that Doc often tucked it into his lab coat pocket, stdl
ht Naturally, the lab coat contained numerous burn holes)
Lester became a close friend of Albert Sauveur, the father of metallography in the United
States Sauveur invited Lester to teach an X-ray metallography course at Harvard for his grad-
uate students He did this from 1931 to 1936
Besides being a founder and first chairman of E7 (then called "on Radiographic Testing")
from 1938 to 1948, he was a founder and first president of the Society for Nondestructive Test-
mg In 1943, the Society for Nondestructive Testing established the Lester Honor Lecture in
recognmon of his accomplishments Their first handbook, published in 1960, was dedicated
m his memory and he was their first honorary member In 1944, he received the Civilian Ser-
vice Award from the War Department He received the ASTM Award of Merit (! 951) and was
named an honorary member (1953) ASM honored Lester with the Albert Sauveur Achieve-
ment Award m 1953 He was also a fellow of the American Physical Society and the American
Society for the Advancement of Science On May 17, 1960, the Army's first nuclear reactor
was dedicated as the Horace Hardy Lester Reactor Lester began the research project that ulti-
mately led to the mstallahon of the reactor at the Watertown Arsenal Research conducted
with this reactor demonstrated the phenomenon of radiation hardening He pubhshed twenty-
five papers, nearly all on radiography or nondestructive testing He retired in 1953, at age 70,
but continued as a consultant to Ordnance Matermls Research until his death

Francis Ferdinand Lueas

(born 7 August 1884 m Glens Falls, New York, died 20 June 1951)
Franczs Lucas was never an officer or subchmrman of E4 but he was a long time member
who contributed actively, for example, in the construction of the first grain size charts He was
widely regarded as one of the premier metallographers of his time and his advice was sought
Lucas was a self-educated man with no formal technical education At age 16 in 1902, he began
his career with the Bell System as a groundman with the Hudson Rwer Telephone Co He rose
to the posmon of district wire chief Next, he joined the Engineering Department of the
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62 METALLOGRAPHYPAST, PRESENT,AND FUTURE

Southern Bell Telephone Company, and, m 1910 he joined the Western Electric Englneenng
Department, the predecessor orgamzatlon of the famed Bell Telephone Laboratories
H~s interest m m~croscopy began when he was placed in charge of respecting t~mber prod-
ucts As part of h~s inspection, Lucas purchased a microscope to study the wood In the early
1920s, hght microscopes were hmlted to about 1000, or 1500 with immersion objectwes
Lucas devoted considerable efforts, with the help of the Zelss works m Jena, Germany, to rais-
ing these hm~ts--first to 3500, then to 5000 and ulUmately, to nearly 7000 These very
h~gh magmficat~ons were chiefly obtained by refinement oftechmques to permit utd~zaUon of
ultraviolet hght with its shorter wavelength and improved resolution The ultrawolet micro-
scope was not a new tool Biologists had attempted to utlhze them nearly twenty-five years
earher However, there are a great many problems revolved with the use of ultraviolet (UV)
hght, which ~s outside the v~s~ble spectrum How do you focus a hght that cannot be observed9
This and other problems, caused biologists to give up the UV m~croscope and ~t fell into
obscurity
Lucas was frequently revolved with consulting work In World War II, he examined the
mlcrostructure of paint films on sh~p hulls For the Pubhc Health Service, he made a motion
picture o f the hfe cycle of the syphflhs spirochaete Lucas was probably the first person to
observe the very fine m~crocracks that act as lnmat~on s~tes for fatigue fractures These cracks
were found to be assocmted with coarse, plate martens~te, the first recognmon of such cracks
Lucas published forty papers, about ten of whxch were devoted to the UV microscope, p e r
s e Others demonstrated the value of "the most powerful microscope m the world" for the
study of m~crostructures One paper studied austemte, two were on martens~te, one was on
fatigue lnltmtlon sites at martenslte m~crocracks, and two were on troost~te In the 1930s there
was considerable debate about the "lamellar famfly"--pearhte, troost~te, and sorblte Lucas's
ultrahigh magmficatmn work helped to show that troost~te was simply very fine pearhte where
the mterlamellar spacing was too fine to resolve with standard hght microscopes Lucas studied
other materials as well, for example, the surface of phonograph records, tumor cells in mice,
hvmg sperm cells m grasshoppers, and latex rubber He developed an "optical sectioning" pro-
cedure to produce complete plan wews oforgamc cells or metal crystals He had at least three
patents, one for an Insulating material, another for a steel alloy for submanne cable armor,
and the third for a method to detect fingerpnnts
In 1924, the American Society for Steel Testing (ASST) (later the American Society for Met-
als (ASM)) awarded him the Henry Marion Howe Medal for his paper on "High Power Pho-
tomlcrography of Metallurgical Specxmens." In 1931, he dehvered the American Institute of
Mining, Metallurgical, and Petroleum Engineers, Henry Marion Howe Lecture "On the Art
ofMetallography " A l s o m 1931, Professor Bradley Stoughton and Lehigh University awarded
Lucas an honorary D Sc He retired from Bell Labs on 31 August 1949 In 1957, ASM estab-
hshed the Francis F Lucas Award for excellence m metallography whxch was endowed by the
late Adolph E Buehler, founder and Presxdent ofBuehler, Ltd Lucas was ASM's delegate to
the World Engmeenng Congress in Tokyo m 1929 He was a fellow of the American Assoc~-
atxon for the Advancement of Science The Royal Photographic Society of Great Britain
awarded him medals for his work in 1926 and 1929 The Frankhn Institute conferred upon
Lucas the John Price Wethenll medal m 1935

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VANDER VOORT ON HISTORY OF COMMITTEE E4 63

Taylor Lyman

(born 13 September 1917 m Lemon, South Dakota, died 8 February 1973)


For many years, E4 had a close relat~onshlp with the American Society for Metals (ASM)
as Taylor Lyman and Ernle T h u m were both long time E4 and ASTM members, as well as
ASM employees Taylor Lyman's main E4 activity was as a member of Subs II and III He was
one of the experts on phase diagrams on Paul Beck's subcommittee that eventually developed
E 157 and, later, E 391 Lyman also enhsted a number of E4 members to prepare articles for
the American Society for Metals (ASM) Metals Handbooks.
Taylor was born m a private home next to the home of the doctor who delivered him, w~thm
sight of the plains of North Dakota Several days later, he and his parents returned to the log
cabin built by his father on their homestead claim m Thunder Hawk, South Dakota Later, he
regretted missing th~s opportumty to have been born, Lincoln-style, m a true American log
cabin H~s first ancestor m the New World, Richard Lyman, emigrated from England m 1631
and, w~th Thomas Hooker and Samuel Stone, founded the town of Hartford, Connecticut
(Hartford was originally called Newton) m 1636
Lyman a n d h l s famdy m o v e d t o Mt Vernon, South Dakota just before he entered grammar
school He was an excellent student and a hard w o r k e r - - d e h v e n n g the Sioux City Journal,
the Saturday Evening Post, the Ladies' Home Journal and the Country Gentlemen whde keep-
mg up with the routine chores of a country boy, such as chopping and stacking cords of wood
Besides academics, Taylor excelled in athletics Baseball was h~s favorite sport In high school,
he was captain of the basketball team and second m the discus throw in the state At Stanford
University, he played varsity baseball--the coach was Lefty O'Doul (he won National League
batting champlonsh~ps m 1929 and 1932 w~th Phdadelphm and Brooklyn)
Taylor began his college career in 1935 at Yanktown College hopmg to become a mmmg
engineer After a year, he took a job in Fort Peck, Montana He saved his money and subse-
quently entered Stanford University Ray Lyman Wilbur, h~s father's cousin, was president of
Stanford after servmg as Herbert Hoover's Secretary of the Interior At Stanford, Taylor dis-
covered metallurgy which was taught along with mining courses He recewed an A B m engl-
neenng in 1940 and was awarded a Gordon McKay Fellowship m metallurgy and metallog-
raphy at Harvard At Harvard, he learned of a recent graduate, Alexander R Tromno, who
had left to teach at Notre Dame
In 1941, he recewed an S M at Harvard and he moved to Notre Dame to study under
Tromno He recewed his Ph D m 1944, his thes~s toplc was "The Isothermal Transformation
of Austemte " He stayed on as an Instructor and worked part time w~th Bendix Aviation
The sixth edmon of the ASM Metals Handbook was pubhshed m 1939 and repnnted in
1942 and 1944 Although m need of revision, thxs task was deferred dunng the war ASM
began a search for a staffedltor to lead this rewsmn and Trolano recommended Taylor Lyman,
after convincing Taylor that his lack of edltonal experience was overshadowed by his other
quallUes H e j o m e d ASM m the summer of 1945
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64 METALLOGRAPHYPAST, PRESENT, AND FUTURE

In 1948, the 7th edition of the Metals Handbook (and perhaps the most popular edition)
was published using a larger page format than p n o r edmons and containing far more infor-
mation (1332 pages. 40% larger than the 6th edition). The 7th edition also contained the first
extensive collecUon of phase d~agrams published in the United States
The 8th edmon of the Metals Handbook was a major change as the single volume work
increased to eleven volumes w~th more than 4600 author-contnbutors Taylor, however, was
stncken w~th illness m the summer of 1972 near the completion of Vol 7 of the 8th edition.
Robert F Mehl, chairman of the volume 7 committees, was also senously ill from dmbetes
F r o m his hospital bed, Taylor rewewed pages and planned Volume 8 He died at Umversity
Hospital m Cleveland on 8 February 1973

Louis Williams McKeehan

(born 31 March 1887 m Mmneapohs, Minnesota, died 31 March 1975)


Louis McKeehan was the second chairman of Sub VI from 1930 to 1933 Originally titled
Sub VI on X-Ray Crystal Analysis, it was changed to Sub VI on X-Ray Methods m 1931 In
1926, McKeehan published m the A S T M Proceedings an extensive glossary of terms relating
to X-ray metallography
McKeehan began his academic career at the U S Naval Academy (1903-1905), then
returned home to the Umverslty of Minnesota receiving a B.S m Engmeenng m 1908, an M S
m 1909 and a Ph.D in physics m 1911. He was a member o f t b e faculty from 1906 to 1919
In 1927, he received an honorary M A from Yale University
He was a physicist with Western Electnc C o , Bell Telephone Laboratones, from 1921 to
1927 where he began his interest in X-ray techniques He then joined Yale Umverslty in 1927
as professor of physics (1927-1955) He was the director of the Sloan Physics Laboratory at
Yale from 1927 to 1941 and from 1946 to 1954 In 1955, he was named professor emeritus
McKeehan received the Legion of Ment and a Mentonous Pubhc Service Award of the U S.
Navy m 1965

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VANDER VOORT ON HISTORY OF COMMITTEE E4 65

Robert Franklin Mehl

(born 30 March 1898 m Lancaster, Pennsylvama, died 29 January 1976)


Bob Mehl orgamzed E4's first symposium m 1936 which became its first specml techmcal
pubhcaUon (STP 28) and was chairman of Sub VI on X-ray methods from 1933 to 1937 He
was a pioneer m the development of gamma-ray radiography for the study o f steel castings. He
received a B.S from Frankhn and Marshall College m 1919 and a Ph D m physical chemistry
from Pnnceton m 1924. He taught chemistry at Jumata College (1923-1925), became a
naUonal research fellow at Harvard Umverstty ( 1925-1927), then supenntendent of the Divi-
sion of Physical Metallurgy, Naval Research Laboratory ( 1927-1931), then assistant director,
Research Laboratories of the American Rolhng Mill Company (Armco, 1931-1932) In 1932,
he joined the Carnegie Institute of Technology as director of the Metals Research Laboratory
and professor of metallurgy
Mehl's interest m chemistry began as a boy when he built a chemical laboratory m the base-
ment of his home He once said "'I scared the daylights out of my m o t h e r - - t o say nothing of
myself" In 1914, when Bob was m high school, he and another student placed uranyl acetate
on top of a key, then placed the key over photographic film, thus producing a radiograph of
the key X-ray radiographs were already well known at that time. Soon after Rontgen discov-
ered X-rays m 1896, Albert Sauveur (a young man in Belgmm at that time) made an X-ray
radiograph of a weldment When Mehi went to the Naval Research Laboratory (NRL), he was
shmulated by a brief Russmn note about the use of gamma rays. Mehl knew that the absorp-
tion coefficient of gamma rays was lower than for X-rays which suggested greater penetrating
power. Also, g a m m a ray sources could be portable whde X-ray generators were not Mehl con-
vmced the Navy m 1928 that thts work was worthwhde and actwe work began in 1929 The
Howard Kelly Hospital m Baltimore had 5 g of radium and regularly pumped offradloactwe
radmm emanation, radon The first gamma-ray radiograph was made m the hospital base-
ment. In this work, Mehl was joined in 1929 by Drs Charles S Barrett and Gdbert Doan In
1930, Roy A. Gezehus, Herman F Kmser, and Charles W. Bnggs joined Radiographs were
made of sections up to 12 5 m thtck, while X-rays were limited to 3 in at that time. The first
"commercial" test of gamma-ray radiography was made later m 1930 on the sternpost casting
on the cruiser "Chester." The radiograph found large hot tears that d~d not come out to the
surface. Naturally, tt was kept m service and the tears propagated to the surface
Mehl was head of the department of metallurgy from 1935 to 1959 and dean of graduate
studLes from 1953 to 1960 From 1960-1966, he was on leave from Carnegie as a consultant
to U S Steel Corp Next, he acted as vtsmng professor at the Umverslty of Delaware and at
Syracuse University. D u n n g World War II, he and his colleagues performed research for the
U.S Army. In 1945, he was an attache with the U S Embassy m London working with the
Techmcal Intelligence Investigating Committee m Germany evaluating their iron and steel
industry He subsequently served on a number of government committees Ship Steel Com-

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66 METALLOGRAPHY PAST, PRESENT, AND FUTURE

mmttee, National Research Council (chairman, 1948), the Metallurgy Committee, Research
and Development Board (chairman, 1950), and, the Metallurgical Advisory Board, National
Research Council (chairman, 1951) He also chaired the Commission of Technical Coopera-
tive Administration under President Truman's Point Four Program and was an advisor to the
Atomic Energy Commission Dr Mehl was interested in developing metallurgy outside of the
United States He made a number of trips to Brazil, for example, to stimulate work there In
1944, at the request of Nelson Rockefeller (coordinator o f inter-American affairs at that time),
he organized a lecturing and technical liaison mission to Brazil and helped orgamze Brazil's
first metallurgical society H e a l s o s t u d l e d B r a z i l ' s m e t a l s i n d u s t r y u n d e r t h e U S State Depart-
ment's Point Four program
Meht put together an illustrious staff at the Metals Research Laboratory of the Carnegie
Instmtute of Technology consisting initially of Charles S Barrett, Maxwell Gensamer, Cyril
Wells, Frederick N Rhlnes, and Gerhard Derge Mehl and these five colleagues had a major
influence on the establishment and development of the field of physical metallurgy He pub-
lished over 200 papers He enjoyed oil painting and tennis as hobbles Mehl mentioned that
on one ofhms traps to Brazil, "the reporters asked me what I liked to do mnmy spare time I told
them I paint and used to play tennis So they wrote 'Dr Mehl is the best known amateur artmst
in the United States, and he msa tennis champion He would like very much to meet some of
the Brazihan c h a m p i o n s ' "
Mehl presented fifteen honorary lectures and received thirteen medals and numerous
awards, for example, election to the National Academy of Sciences ( 1958), fellow of the Amer-
ican Institute of Mining, Metallurgical, and Petroleum Engineers (AIME) (1964), honorary
member of the Iron and Steel Institute (UK) in 1969, the John Scott Medal, certificate and
prize from the Dmrectors of the Board of City Trustees, City of Philadelphia, for development
of gamma-ray radiography (1934), the Henry Marion Howe Medal of the American Society
for Metals (ASM) (1939), the James Douglas Gold Medal o f A I M E (1945), the Gold Medal of
ASM (1952), the LeChateher Medal of the Soci&6 Franqalse de M&allurgle (1956), the Plat-
m u m Medal of the Institute of Metals (1962), and six honorary degrees Two awards have been
named after him The Society of Nondestructive Testing established the Mehl Honor Lecture
at its first meeting, 17 October 194 l, with Charles W Briggs as recipient Mehl was the recip-
ient of this award on 18 October 1971 but gave his lecture by tape, "in absentia," due to ampu-
tation of both of his legs, as a result o f diabetes

George Andrew Moore

(born 14 February 1913 in New York, New York)


George Moore, although never an officer or subcommittee chairman, was an active E4
member for about 30 years He was a tireless worker on Sub 14, particularly in the areas of
volume fractmon, grain size, and inclusion measurement In 1960, at the suggestion of LeRoy
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VANDER VOORT ON HISTORY OF COMMITTEE E4 67

Wyman, he started work on the storing, manipulating, and measuring of microstructural


images with a digital computer His subsequent report on the potential for computerized quan-
titative microscopy stimulated creation of Sub 14 George was also quite active in the devel-
opment of improved A247 graphite charts and wrote several classic papers in STPs
George was trained as a chemist and metallurgast receiving a B.S degree in chemistry from
Union College in 1934, an M S in metallurgy from Harvard in 1935, and a Ph D from Prince-
ton in 1939 in chemistry and metallurgy While at Princeton, he was an assistant instructor
from 1935-1939, then an instructor until 1940 At that time, he joined the Battelle Memorial
Institute as a research engineer where he was involved with work on hydrogen in steel and in
fractography, using the light microscope, with Carl Zappfe In 1948, he joined the University
of Pennsylvania as an associate professor of metallurgy In 195 l, he joined the National
Bureau of Standards where he performed his work in quantitative metallography He retired
in 1979 He was a lecturer at the University of Maryland from 1954 to 1962. He was also a
long-time member of the International Society for Stereology and chaired its Fourth Inter-
national Congress for Stereology in 1975. Thoroughness was a hallmark of George Moore's
work He was a total purist in all his endeavors

Mary Rose Norton

(born in June 1905 in Cambridge, Massachusetts, died 30 January 1974)


Mary Norton served as secretary of E4 from 1946 to 1966 and as chairman of Sub II on
Definitions from 1966 until her death in 1974 Mary attended Emmanuel College in Boston
and received an A.B in chemistry and mathematics in 1926 Next, she enrolled in Columbia
University and received an A M in chemistry in 1928 Before, during and after her graduate
studies, she worked in the research laboratory of the Merrlmac Chemical C o , North Woburn,
Massachusetts Mary's entrance into the ordnance field and metallography is an interesting
story
General T C Dlckson, commanding officer of the Watertown Arsenal in 1928 was
intrigued by the work of Francis F Lucas of the Bell Telephone Laboratories, a consultant to
the Arsenal General Dlckson wanted to establish a similar high-resolution light microscopy
laboratory at the Arsenal to investigate ordnance steels He ordered that the new facility should
duplicate that of Dr Lucas, even to having a woman assistant whose background was soence)
Arsenal personnel called local colleges and recruited Mary as the woman assistant Mary
enrolled in metallurgy courses at both Harvard and Massachusetts Institute of Technology
(MIT), particularly with professors Robert Wllhams and Arthur Homerberg at MIT
Mary learned her craft well receiving numerous commendations for her work Other orga-
nizations requested her help, for example, the U S. Geological Survey, the U S Navy Bureau
of Ships, Harvard Observatory, independent test laboratories, and industrial companies such
as Republic Steel The Arsenal purchased a Zelss Neophot metallograph in 1935 Mary loved
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68 METALLOGRAPHY PAST, PRESENT, AND FUTURE

to use its 1 60 NA (numerical aperture) oil-immersion objective for high magnification stud-
les Mary quickly discovered that even the best microscope was useless if the specimens were
not polished properly and she devoted her energies toward mastering this necessary skill This
interest led her to study surface finishing techniques During World W a r II, she developed,
prepared and cahbrated standards for ordnance finishes used for quality control In 1942, she
was assigned leadership of the Metallurgical Structures Section in the Physical Metallurgy
branch In this position, she contributed to the knowledge of how to best utlhze high strength
steels and did notable work on temper embrittlement
Mary received the War Department's Meritorious Civilian Service Award in 1945 The
ASTM Award of Merit was bestowed in 1959, and she was named honorary secretary in 1966
In 1974, Committee E4 established, with the help of many of her friends, the Mary R Norton
Memorial Scholarship Fund for women studying metallurgy

Robert Earl Penrod

(born 22 July 1887 in Johnstown, Pennsylvania, died 11 September 1971)


Earl Penrod served as vice chairman o f E4 (1944 to 1964) and as chairman of Sub VIII on
Gram Size (1952-1964), replacing Marc Grossmann after his death. He took over the work of
unifying E4 grain size methods into one standard, E 112, issued in 1955
Penrod joined the Cambria Iron Works on 1 September 1902 at age fifteen This plant was
acqmred by Bethlehem Steel and became their Johnstown Plant Penrod did not attend col-
lege, he did attend summer courses on metallography with Albert Sauveur He worked his way
up to chief metallurgist in 1927 and held that position until his retirement on 31 August 1955
after 53 years
Penrod was active in the Johnstown community, as a member of the industrial council of
the Greater Johnstown Chamber of Commerce and as the chief fund raiser for the Johnstown
Symphony Orchestra He received the ASTM Award of Merit in 1957 and was named hon-
orary vice chairman of E4 m 1964

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VANDER VOORT ON HISTORY OF COMMITTEE E4 69

George Edward Pellissier

(born 15 March 1915 m Spnngfield, Massachusetts, died 24 June 1982)


George Pelhssler was the first chairman of Sub XI ( 1950-1951 ) and Sub XIV ( 1961-1964)
He chaired Sub 11 again from 1969 to 1973 George was also achve with E24 on Fracture
Testing of Metals, where he chaired Sub 1 (on High-Strength Metals) from 1965 to 1969 and
was the founder and first chmrman of Sub 2 (on Fractography) from 1963 to 1965 George
recewed B.A and M A degrees m chemistry from Cornell Umverslty m 1936 and 1938,
respecUvely, He started doctoral work at Carnegie InsUtute of Technology m Metallurgy m
1938, but this work was interrupted in 1941 by World War II
From 1942 to 1945, he was group leader for Manhattan Project work performed at Colum-
bm Umversity He apphed transm~ssion electron microscopy to the determination of
extremely fine pore sizes m gaseous isotope diffusion separation barriers under development
and to the study o f " d u s t " plugging problems This work was performed using one of the first
commercially available electron microscopes m the United States
After the war, George joined the Apphed Research Laboratory of the U S Steel Corp as a
research associate. In 1947, he was named section head, physics and analytical chemistry, then
division chief m 1955 In 1959, he was manager, advanced applied research In 1966, he
became senior consultant m physical metallurgy until he retired m 1968
George continued his interests m electron m~croscopy when he joined U S Steel developing
rephcat~on methods, the only approach for studying fine structure at that time He also worked
on developing the extraction replica techmque as an offshoot of the X-ray reflecUon-dlffrac-
tion concentration technique He uUhzed these methods m h~s efforts to develop tougher, high-
and ultrahigh-strength steels
Pelhssier became interested m electron fractography in 1962 when he began to study frac-
ture modes and mechamsms of h~gh-strength alloys He used one of the first prototype scan-
nmg electron microscopes for fractographlc work
After retirement, George became laboratory manager for Ernest F Fullam, I n c , Schenec-
tady, New York, a major supplier of electron metallograph~c eqmpment He continued m this
role until 1971 when he joined RRC International, Inc as department manager He main-
tamed this association until shortly before his death m 1982
George pubhshed over twenty-five papers, including his classic work on "The Interlamellar
Spacing of Pearhte" (Transactions, ASM, December 1942) He held four patents Three are
on methods of measunng coating thicknesses He was a fellow of the American InsUtute of
Chemists and a fellow of the American Society for Metals (ASM) He was a charter member
of the Electron Microscope Society of America and of the International Metallographic Soci-
ety In 1961, he was a member of an inspection tour of metallurgical research msututes in the
Soviet Union, sponsored by the Electrochemical Society and the U S State Department In
1970, he gave the Albert Sauveur memorial lecture for the Philadelphia Chapter of ASM

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a

Arthur Phillips

(born 3 February 1892 in Troy, New York, died 25 December 1977)


Arthur Phillips was chairman of Sub II on Terminology from 1925 to 1938 Phillips
attended public school in New Haven, Connecticut and graduated from Hlllhouse High
School Phillips received a bachelor of phdosophy degree from the Sheffield Scientific School
o f Yale University, graduating summa cum laude. Continuing at Yale, he received his M S
in metallurgy in 1915--he was the first person to receive an M.S in metallurgy from Yale
Phllhps joined the Bridgeport Brass C o , but four years later returned to Yale as an assistant
professor (1919-1928) He advanced to assooate professor (1928-1934), then professor
(1934-1959) and emeritus professor in 1959 F r o m 1950 to 1959, he was head of the depart-
ment of metallurgy.
He was a student of Champion H Mathewson Their paper "The Recrystalhzation of Cold-
Worked Alpha Brass on Annealing" (Transactions, AIME, Vol. 54, 1917) had a major impact
on the understanding ofrecrystalhzatlon In 1942, with Robert M Brick, he published the well
known text Structure and Properties of Alloys (McGraw-Hall Book Co ) This book was built
upon lectures by Mathewson, instructor o f both Phillips and Brick.
When Phllhps was working on the recrystalhzatlon of brass m the 1920s, there were few
sources of graded abrasives for pohshlng. The metallurgy department was located m the Ham-
m o n d Laboratory at that time. This was a large, open building on the inside, several stones
high and equipped with gnnding equipment The dust from grinding would settle on the walls
as there was no exhaust or dust collection system at that time. Phillips would climb up a ladder
to different levels and brush the dust into coin envelopes. The higher he went, the finer the
dust. Much of the dust was iron oxide. Hence, he utilized gravity to grade the iron oxide by
s~ze, that is, height above the floor!
In 1944, Phdhps gave a series of lectures at the University of Sap Paulo, Brazil and received
an honorary Ph D from them, and also from the Stevens Institute of Technology in the same
year He was an active consultant, particularly for the Henry D Thompson C o , manufacturer
of saw blades At the time o f his death, he was a director ofth~s company

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VANDER VOORT ON HISTORY OF COMMITTEE E4 71

Samuel Moreau Purdy

(born 27 May 1926 in Bethlehem, Pennsylvania)


Sam, current First Vice Chairman of E4, has had a long association with Sub 1 as its chair-
man from 1966 to 1982 and from 1986 to the present From 1983 to 1988, he was chairman
of Sub 5 on MlCrOlndentation Hardness and from 1968 to 1972, he chaired Sub 14 on Quan-
titative Metallography Sam has left his l m p n n t on many ASM standards, such as E 3, E 340,
and E 381 The most recent is E 1351 on the production and evaluation of replicas made in
the field to evaluate creep damage in electric power plant components, which began life as an
emergency standard, ES 12-87, E4's only emergency standard He also was our representative
to the International Standardization Organization from 1977-1981
Sam, a descendant of early English colonial settlers around Manhattan, received a B S in
metallurgical englneenng from Lehigh University in 1948 Following graduation, he joined
Carpenter Steel Company, starting as a hot mill observer He transferred to their research
department and became supervisor of stainless steel development, then supervisor of physical
metallurgy In 1962, he joined Youngstown Sheet and Tube as supervisor of the metallo-
graphic laboratories, a position he held until their demise in 1979 He then joined Jones and
Laughlin Steel as a senior research engineer and in June 1980, joined National Steel Corp as
senior research engineer, later senior research associate, his current position He is an avid
reader (British history and French revolution) and gardener--he usually grows twelve varieties
of Mexican and Oriental peppers!

Henry S. Rawdon

(born 7 June 1880 in Derby, England, died 14 May 1954)


Henry Rawdon was the first chairman of Sub V (on "Micro-Hardness") and was chairman
of Sub IV on Photography from 1922 to 1934 Sub V was established in 1923 to evaluate the
Blerbaum micro-character tester, a scratch indentation tester performed with the aid of an

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72 METALLOGRAPHYPAST,PRESENT,AND FUTURE

upright microscope with a scratch indenter The work concluded that it was of comparative
use only and the Sub was disbanded in 1926
Henry came to America when he was four years old His family settled in Michigan with
relatives on a farm in a small village Educated in the ungraded district schools, he studied at
home and passed the examination for country teacher when he was 17, the m l m m u m age for
such lobs However, it was difficult to get a position, so he entered the Michigan State Normal
College in Ypsllantl He worked his way through school and graduated in 1903 with a life
certificate in teaching For the next six years, he taught high school at Marlette, M i c h i g a n - -
for the first three years, he taught soence and for the last three years, he was superintendent
He decided to make chemistry his career and, in 1909, entered the englneenng college of
the University of Michigan Metallurgy courses were being introduced into the chemical engl-
neenng program and Henry's interest in metals was fostered by these courses and by Professor
Edward DeMflle Campbell, the famous blind metallurgist Rawdon acted as his personal assis-
tant dunng his senior year. In 1912, he received a B Ch E and started to do graduate studies
when he was recruited by the new division of metallurgy at the U S Bureau of Standards to
work in metallography as an assistant physicist
Rawdon spent his entire career at the Bureau becoming Chief of the division of metallurgy
m 1929, a position he held until he retired in 1945 Henry attributed his interest in metallog-
raphy and the structure of metals to his earlier training in biology with the transmitted light
microscope He had an abiding interest m studying structure-property relationships He was
also fascinated by corrosion mechanisms, problems, and solutions His book, Protective
Metallic Coatings, published in 1928 by the American Chemical Society, was a pioneering
effort m this field He had 88 publications He served on the Metallurgy Advisory Board of the
Ordnance Department for the National Advisory Committee for Aeronautics and for the
National Academy of Sciences During World War II, he was on advisory committees to the
Army and Navy Munitions Board, Office of Production Management, War Production Board

Frederick Nims Rhines

(born 25 July 1907 in Toledo, Ohio, died 10 Apnl 1986)


Fred Rhlnes was one of the phase diagram experts recruited by Paul Beck to help develop
standard nomenclature and presentation procedures leading to E 157 and E 391 He mare-
tamed this interest with E4 for more than thirty years Fred was more active on B9 on Metal
Powders and Metal Powder Products, than on E4 He,loined B9 in 1944 and E4 in 1949 He
chaired B09 01 on Nomenclature and Technical Data from 1944 to 1965 He also contributed
substantially to the development of a "Glossary of Terms for Powder Metallurgy" and to many
other projects He received the Award of Ment in 1962 He was also a member of the former
E8 committee

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VANDER VOORT ON HISTORY OF COMMITTEE E4 73

Fred received a B S.E. from the University of Michigan in 1929 He worked as a metallurgist
m the Research Laboratories of Alcoa from 1929 to 1931 In the summer of 1932, he studied
at the University of Berlin and received a language certificate In 1933, he received a Ph D
from Yale University He was a laboratory instructor at Yale from 1933-1934, then joined
Robert F Mehl at Carnegie Institute of Technology as a member of the staff of the metals
research laboratory and the metallurgical engineering faculty From 1946 to 1959, he was
Alcoa professor of light metals at Carnegie Institute of Technology
In 1959, Rhines left Carnegie and headed south where he established the department of
materials soence and materials engineering at the Umverslty of Florida (Gainesville). Fred was
professor of metallurgy and materials engineering and head of the metals research laboratory
engineering industrial experiment station from 1959 to 1973 He was chairman of this depart-
ment from 1963 to 1973, then became distinguished service professor He retired in 1978.
Fred received the C H Mathewson American Institute of Mining, Metallurgical, and Petro-
leum Engineers best paper awards in 1939 and 1942 He received the Henry Marion Howe
Medal of American Society for Metals (ASM) in 1947 and 1960 and the Albert Easton White
Dlstmgmshed Teacher Award of ASM m 1970 In 1970, he received the Willis R Whitney
Award from the National AssocmUon of Corrosion Engineers He was a fellow of ASM,
ASTM, and AIME He also conducted excellent pioneering studies m quantitative microscopy
and was coeditor with Robert T. DeHoff, of the book Quantitative Microscopy (McGraw-Hill,
1968) His classic 1956 text, Phase Diagrams in Metallurgy (McGraw-Hill Book Co ), was
used by colleges for many years

William Ernst Ruder

(born 22 December 1886 in Stockdale, Pennsylvania, died 10 February 1963)


Bill Ruder was chairman of Sub III on Thermal Analysis from 1924 to 1928 After gradu-
ation from the Pennsylvania State College in 1907 with a B S. in electrical engineering, he
joined the General Electric Research Laboratory (10 July 1907) He had earlier received a
teacher's certificate after studying at the state teacher's college in California, Pennsylvania, He
spent his entire career with General Electric, retlnng in 1952 as manager of the metallurgy
department of their Research Laboratory He was well known for his research on magnetic
alloys, both soft and hard
His first patent, issued in 1914, covered the manufacture and processing ofslhcon electrical
sheet steel This work led to improved efficiency and lower electric costs His work on the rate
of grain growth, with Zay Jeffrles, helped to demonstrate the importance of a large grain size
for high temperature applications He helped develop methods for obtaining large grain sizes
and was one of the first to demonstrate the importance of crystal orientation in reducing mag-
netic hysteresis losses Later, he devoted attention to work on permanent magnets In 1934,

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74 METALLOGRAPHYPAST, PRESENT, AND FUTURE

he received his first patent for Alnico-type permanent magnet materials In the United States
Ruder was known as the father of the Alnico magnet His initial research on these materials
occurred at the same time as Mlshima of Japan
In 1938, he was named head of the Metallurgy Department For seventeen years, beginning
in 1933, he was a director of the Allegheny Ludlum Steel Corporation, a manufacturer of mag-
netic materials He served as a member of their executive committee and their research advi-
sory council He held 19 patents by the end of his career

John James Brown Rutherford

(born 26 August 1908 m Hamilton, Scotland, died 19 March 1967)


Rutherford was the primary author of an important early paper (Metals andAlloys, Vol 8,
Dec 1937, pp 345-348) on the correlation between planar and spatial gram size Conse-
quently, he was a long-term participant in E4's grain size standards work, although he never
chawed Sub VIII He did organize Sub X on Decarbunzation and was its first, and only, chair-
man ( 1949 to 1953) This sub worked with the Society of Automotive Engineers and the Amer-
ican Iron and Steel Institute on decarburlzatlon measurement Rutherford was actually more
active on other ASTM committees than on E4 He was a member of A l, A 10, E7, E9, and
several other ASTM activities
John began his academic training at Her~ot-Watt College in Edinburgh, Scotland He came
to the United States in 1928 as an exchange student before fimshlng his degree Instead of
returning and finishing his studies, he joined the American Chain and Cable Co in Bridgeport,
Connecticut working as a research metallurgist under A V deForest He pursued further stud-
les at New York University and at Columbia University but never did complete his degree
requirements In 1929, he joined U S Steel's Research Laboratory in Kearney, New Jersey
He helped E S Davenport with his isothermal transformation studies of steel He also did
some pioneering work on the lntergranular corrosion of austenltlC stainless steels w~th R H
Aborn On 20 June 1938, he joined the Babcock and Wilcox Company an Beaver Falls, Penn-
sylvania, as a research metallurgist At the time of his death, he was chief metallurgist He held
a number of patents on the processing of stainless steels In 1957, he gave the 24th Annual
Sauveur Lecture of the Phdadelphla Chapter of the American Society tbr Metals
John was a descendant of Jean Armour who married the Scottish poet Robert Burns ("Auld
Lang Syne") in 1788 John spoke Gaelic and was a frequent speaker at Bobby Burns Clubs on
the anniversaries of the poet's birth He was an avid golfer and gardener

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VANDER VOORT ON HISTORY OF COMMITTEE E4 75

Carl Hubert Samans

(born 27 January 1909 in Greenville, Pennsylvania, died 22 March 1981)


Carl Samans was not an officer or subcommittee chairman of E4 In 1937, when Marcus
Grossman took over the Special Subcommittee on Grain Characteristics (which became Sub
VIII on Grain Size in 1938), Grossman established three groups (now called task groups) to
work on specific aspects of gram size analysis Group C was set up to develop methods for
nonferrous alloys other than copper Group C was headed by Carl until 1951 when H P
George took over Standard E 9 l, issued in 195 l, resulted from this work
Samans received a bachelor's in chemical engineering from Rensselaer Polytechnic Institute
in 1929 He then joined the research laboratory of Chase Brass and Copper Co and obtained
his M S (1932) and Ph D (1934) in metallurgy from Yale University while with Chase He
then joined Lehigh University as an instructor in metallurgy (1934-1935), then taught at
Rensselaer Polytechnic Institute (1935-1937) while acting as a consulting physicist for the
International Nickel Co In 1937 he joined the metallurgy faculty at Penn State.
Samans returned to industry In 1941 joining the American Optical C o , moving up to chief
of the metallurgical section of their Research Department In 1949 he joined Standard Oll Co
(Indiana) as associate director, engineering research In 1960, he became director of this
department
Samans was president of the American Society for Metals (1968-1969) after previous terms
as a trustee ( 1959-196 l) and as secretary ( 1964-1966) Samans authored two books Engi-
neering Metals and their Alloys and Metallic Materials in Engineering.

Ernest Edgar Thum

(born 20 November 1884 at Hamsonvllle, Missouri, died 10 April 1961)


Ernle was never an officer or subcommittee chairman o r E 4 but he was active with E4 and
ASTM from 1924 until his death in 1961 He was also a member of Committees A 1 on Steel,

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76 METALLOGRAPHYPAST, PRESENT, AND FUTURE

B2 on Non-Ferrous Metals and Alloys, E5 on F~re Tests of Material and Construction, B6 on


Die-Cast Metals and Alloys, B9 on Metal Powders and Metal Powder Products, and was E4's
representative to E 1 on Methods of Testing (at that t~me) He was most active with B2 where
he served as secretary (1928-1939), chawman (1939-1948), and honorary vice chairman
( 1948 until death m 1961) He recewed the Award of Merit m 1954, mainly for his B2 work
Erme recewed a bachelor's degree in m m m g engineering from the Colorado School of Mines
m 1906 He joined the Anaconda Copper Mmmg Co as a field engineer after graduation.
From 1908-1910, he was chief clwl engineer for the constructmn of the Tooele Smelter of the
International Smelting and Refining Co. m Utah In 1910 he became engineer in charge of
construction of The Great Falls (Montana) Smelter of the Anaconda Copper Mining Co. He
switched career paths at this ume, 1915, when he joined the University of Cincinnati as pro-
fessor of metallurgy
In 1917, Erme again changed his career path becoming associate editor of Metallurgicaland
Chemical Engineering, a popular monthly trade journal published by McGraw-Hill From
1924-1927 he managed the technical pubhclty department of the Union Carbide and Carbon
Corporation He returned to pubhshmg m 1928 as pnnclpal associate editor of The Iron Age.
In 1930, he joined the American Society for Metals (ASM) as the founding editor of Metal
Progress. In 1947, he took on the task of superwsing book pubhshmg for ASM During his
tenure as editor m chief of Metal Progress, ~t was widely recogmzed as one of the premier
metallurgical journals He also pubhshed a number of books, such as The Book of Stainless
Steels and Modern Steels.
Erme recewed numerous awards for his work He received a Dlstmgmshed Service Award
from ASM m 1948 and was made an Honorary Member m 1958 His alma mater gave him
their Silver Medal m 1951

Clarence Jory Tobin

(born 29 May 1896 m Calumet, Michigan, died 4 March 1978)


Clarence "Tobe" Tobin, a long time E4 member, was the chairman of the Special Com-
mittee on Grain Characteristics from its formation in 1931 until 1937 This committee's first
goal was to develop a procedure for evaluating the grain growth tendency of steels The
McQuald-Ehn carburlzing test was subsequently adopted and standard E 19 incorporated the
method A grain size chart depicting the hypoeutecto~d and hypereutectold regions for grain
sizes 1 to 8 was Included in the lmtlal version orE 19 (a second chart was added in 1939) Tobe
was also an active member of Committee B2 on Non-Ferrous Metals and Alloys
Tobe received a B S in chemical engmeenng from the University of Michigan in February
of 1920 He then joined the Dodge Brothers, Inc as a metallurgical troubleman and metal-
Iographer In March of 1925, he joined the General Motors Central Laboratories (now the G M

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VANDER VOORT ON HISTORY OF COMMITTEE E4 77

Research Laboratones) as a metallurgist In 1933 he became assistant department head of the


metallurgy department, a position he held until his retirement on 1 June 1961 He was noted
for his contributions in the field of gear metallurgy, automotive component failure analysis,
and metallographlc methods His 1938 paper (Transactions, ASM, Vol 26), co-author with
A. L. Boegehold, on "Factors Governing Selection of Type of Carbunzed Case" was consid-
ered a classic paper on this subject He had two U S patents on brake drums
Tobe was also quite active with the A m e n c a n Society for Metals (ASM), particularly in the
Detroit Chapter where he was its chairman In 1932 He was elected a Fellow of ASM in 1974
and was a fifty-year member

Jose ("Joseph") Ramon Vilella

(born 11 August 1897 in Lares, Puerto Rico, died 27 November 1971)


Joe Vllella, perhaps the best-known metaliographer in his day, was chairman of Sub I from
1947 to 1951 An active E4 member for many years, he also was involved with the ASTM
photographic exhibit He was also a member of Committee El
Vilella's studies at Pennsylvania State College (now Pennsylvania State University) were
interrupted by service dunng W W I with the U S Army as a second lieutenant ( 1917-1918)
He returned and graduated from Penn State in June 1921 with a B.S in chemistry He then
worked as a physiological chemist for two years at the Psychiatnc Institute in Mornstown,
New Jersey In 1923, he joined the Union Carbide Research Laboratory as a microscopist/
metallographer
Vilella married Eve Edwards, a noted fashion model in 1930 Several years later, Union
Carbide decided they wanted to move their research laboratory (in Long Island City) away
from the New York City area to Nmgara Falls Because of Eve's career (Joe was a modern
man), Joe decided to change career paths On 1 May, 1934, hejolned the U S Steel Research
Lab, then in Kearny, New Jersey, as a senior scientist In 1956, when U S Steel moved this
lab (Fundamental Research Lab) to Monroeville, Pennsylvania, Eve had "retired" and the
Vilellas moved to Pittsburgh Bill Forging, Sr replaced Vilella at Union Carbide
Joe retired from U S Steel on 31 August 1962 a n d j o m e d the metallurgy facility of the Uni-
versity of Pittsburgh on the following day as an adjunct professor Vllelta had taught at Rutgers
Umversity during his last year with Union Carbide, 1933-1934 Joe taught at the University
of Pittsburgh for six years between September 1962 and his second retirement m July 1971
Joe is best known, especially today, as a ferrous metallographer and for his development of
"Vilella's reagent," an alcoholic mixture of picnc acid and hydrochloric acid However, Joe
began his career as a nonferrous man, he even coauthored a book on aluminum Aside from
the well known Vilella's microetch for steels, there are at least five other reagents also known
as "Vilella's reagent" used for microetchlng aluminum and alloys, copper-lead alloys, lead and
alloys, tin and dilute tin-lead alloys, and for macroetchlng high alloy steels)

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78 METALLOGRAPHYPAST, PRESENT,AND FUTURE

Joe had one U S patent (for a levlgated alumina for polishing) and thirty-four pubhcatlons
In 1937, he gave a series of education lectures for the American Sooety for Metals which were
pubhshed in 1938 in book form as Metallographie Technique for Steel. In 1951, he gave the
Henry Marion Howe Memorial Lecture for the American Institute of Mining, Metallurgical,
and Petroleum Engineers
In September 1972, the ASTM board approved the creatmn of the Vdella award of E4.
This award recognizes papers published by ASTM that are of outstanding significance to
metallography

Robert Seaton Williams

(born 11 July 1880 in Hartford, Connecticut, died 11 December 1961)


Robert Wllhams was chairman of Sub II from 1938 to 1940 and a long time ASTM member
He received an S B degree in 1902 from the Massachusetts Institute of Technology (MIT) and
was an assistant m analytical chemistry at MIT beginning in the fall of 1902 until he began
graduate school in 1905 at the University of Gottlngen where he studied under Gustav Tam-
man and received his Ph D in 1907 He returned to MIT in 1907 as an instructor in the chem-
istry department He was named assistant professor in 1911 and associate professor in 1917
In 1921 he was named associate professor of chemistry and metallography, and, in 1926, pro-
fessor of physical metallurgy He was head of the metallurgy department at MIT from 1937 to
1946 and dean ofenglneenng from 1942-1945 He retired in 1946 but continued as a lecturer
untd 1951
During W W I, Dr Williams worked on problems with shell cases and conducted research
with Alcoa on bearing metals for aircraft and tanks At MIT, he was a mare force m developing
courses in metallography, heat treatment, spectroscopic analys~s, and X-rays Dunng W W II,
he was revolved with studies on berylhum and its use in aluminum alloys He also served as
technical advisor to the Division of Research and Development m the Quartermaster Gener-
al's Department where he worked on problems with mdltary equipment
With V O Homerberg, he authored Principles ofMetallography m 1919 The fifth edmon
of this very popular book was issued in 1948 He also coauthored The Examination of Iron,
Steel and Brass m 1924 and translated two books pubhshed originally in German

Acknowledgments
Arthur Phdhps--Courtesy o f the Yale Picture Collection, Manuscripts and Archives, Yale
University Library
Charles H Davis--Courtesy of Manuscripts and Archives, Yale University Library
L W M c K e e h a n - - C o u r t e s y of Manuscripts and Archives, Yale University Library
Leon V Foster--Courtesy of Syracuse University Library

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VANDER VOORT ON HISTORY OF COMMITTEE E4 79

F F Lucas--Courtesy of AT & T Archives


Henry M Howe--Courtesy of Columbia University
W Campbell--Courtesy of Columbia Umverslty
George A Elhnger--Courtesy of The National Institute of Standards and Technology
Henry S Rawdon--Courtesy of The National Institute of Standards and Technology
LeRoy L Wyman, Sr --Courtesy of The National Institute of Standards and Technology
R S Williams--Courtesy of the MIT Museum
Edgar H Dlx--Courtesy of the Cornell Umverslty Library
H C Boynton--Courtesy of the Harvard University Archives

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Light Microscopy

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Theodore G. R o c h o w I

Some Incidental History of Metallography and


ASTM Committee E4
REFERENCE: Rochow, T G , "Some Incidental History of Metailography and ASTM Com-
mittee E4," Metallography Past, Present, and Future (75th Anmversary Volume), ASTM STP
1165, G F Vander Voort, F J Warmuth, S M Purdy, and A Szirmae, Eds, American Society
for Testing and Matenals, Philadelphia, 1993, pp 83-87

ABSTRACT: Pioneenng investigations were by Sorby (1826-1908) at Sheffield, England, fol-


lowed by other European metallurgists at the turn of the century "Dean" of Amencan metal-
lurg~stswas Professor Sauveur at Harvard He designed the Sauveur metallograph~cmicroscope
and named the investigated area, "metallography "As Professor of Metallurgy at Sheffield Um-
verslty and F~sher lecturer at Cornell, 1931-1932, Cecd H Desch called attentmn to the coop-
eratmn of umversmes, lndustnes, and governments m research and development m soence and
engineering ASTM, m general, and Committee E4, m pamcular, added consensus of standards
of nomenclature, testing, instruments, procedures and evaluatmns
The modental wews m this paper s~mplysupplement the up-to-date scholarly h~stoncalreview
by the present chmrman of ASTM Committee E4 on Metallography, George F Vander Voort

KEY WORDS. metallography, metallurgical specimens, mlcrostructure, metallographlc tech-


niques, history, standards, testing, nomenclature, instruments

Origin of Metallography
When ASTM Committee E4 was estabhshed m 1916 (see the complete historical review in
Ref 1), the principles of metallography were based on the pioneering microscopical investi-
gations of Henry Clifton Sorby ( 1826-1908) He was the son of the owners of the famous Shef-
field iron and steel works in England He could afford to spend his long hfe as a truly amateur
microscopist, purposely looking through up-to-date microscopes by current techniques,
answering his own questions, such as What makes a good or a bad iron ore, limestone, smelter,
or heat treatment? He saw variations in both structure and morphology Above all, he thought
about the "mechanism" that brought about the resultant physzcal and chemical changes He
taught himself to prepare specimens, vary modes of illumination, and think through to con-
cluslons [2] He published effectively [3] and taught others He was not an ordained scientist,
but was a close associate of the University of Sheffield, where his portrait (Fig l) and some of
his preparations of metalhc speomens are now on display [4]
Professor A Martens added much (1892) [5] to Sorby's methods as did F Osmond (1892)
[6], C T Heycock and F. H Neville (1904) [7], and many others at the turn of the century
Albert Sauveur (1863-1939), who coined the terms "metallography" and its denvauves,
was an ordained scientist At Harvard University, he investigated, taught, and wrote about
"The Mlcrostructure of Steel and the Current Theories of Hardening" in 1895 [8, 9] He used
the term "metallographlst" in 1898 While instructor in Metallurgy at Harvard, he designed

Associate Professor, Ementus, N C State University at Raleigh, home address 740 Smallwood Dnve,
#33, Ralogh, NC 27605

83
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84 METALLOGRAPHY PAST, PRESENT, AND FUTURE

FIG 1--Henry Chflon Sorby (1826-1908) Photograph of the portratt that ts hangmg m Ftrth Hall at
the Umverstty of SheJfield (taken by the author, July 1965)

the Sauveur metallographlc microscope in 1899 He was made a full professor m 1924 and
professor ementus in 1939 [8] His book, The Metallography and Heat Treatment of Steel,
was published by the Harvard Umverslty Press m 1935 [10] (see Fig 2 [8]
Cambridge, Massachusetts, m the 1930s, was also a busy center for the mechamcal pohshmg
and microscopical examination of ore minerals and such, by means of the Graton-Vanderwllt
type of"mechanical" grinding and pohshmg machine It was developed ongmally for Profes-
sor L C Graton of the Laboratory of Economic Geology at Harvard Umvers~ty by Vanderwilt
and produced by the Mann Instrument Company (MICO) in Cambndge [11] This type of
pohshmg machine was designed to keep hard and soft mineral constituents In the same pol-
ished plane by using successive metal (lead) laps embedded with abrasive grains or pohshing
powder [ 12] An example may be tiny particles of gold in a quartz matrix By the same token,
a larger boundary is maintained between two large parts, such as galena contacting pynte
Starting m 1935 at the Experimental Laboratory of the American Cyanamid C o , the present
author and associates used the Graton-Vanderwilt type of mechamcal pohshIng machine to
pohsh thin layers of steel on soft ~ron cores that had been case hardened with calcmm cyamde
made from calcmm cyanamlde The Graton-Vanderwxlt automatic pohshmg machines have
been proven valuable to maintain such hard and soft constituents within a reasonable level
The same ~s true for composites containing metal, resin or rubber, or both (such as automobile
Ures), or adhesives for aluminum sheets [13]
Metallography came to Cornell via Emil M o n n m Chamot (1868-1950) (Fig 3), who, dur-
ing the first quarter of this century, developed the course in Chemical Microscopy that became
one of those reqmred for the Bachelor of Chemistry degree Among Chamot's graduate stu-
dents was Clyde Walter Mason (1893-1983) (Fig 4) He later collaborated with Chamot in

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ROCHOW ON HISTORY OF ASTM COMMITTEE E4 ON METALLOGRAPHY 85

FIG 2--Albert Sauveur (1863-1939) The dean o[ Amertcan metallurgists named his textbook, Met-
allography Heat Treatment of Iron and Steel, and developed the Sauveur mwroscope for opaque
speumens

FIG 3--Emtl Monnm Chamot (1868-1950) Duphcates of this" photograph were autographed by Pro-
/es sor Chamot and ~ent to/ormer students and other frlend~

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86 METALLOGRAPHYPAST, PRESENT,AND FUTURE

FIG 4--Clyde Walter MaJon (1893-1983). on the occaston of one ofhls lectures to the New York Mtcro-
~optcal So~tety. 3 Aprtl 1964

their famous Handbook o f Chemtcal Microscopy [14] Mason introduced the chapter on
"Metallographlc Microscopes."
In 1934, Professor Mason's two laboratory assistants were the present author and Wflham
D Forgeng (1909-1986) who majored in metallography for his Ph D His thesis was "The
Effect of Bxsmuth on the Mlcrostructure of Tin " H e joined the U m o n Carbide Research Lab-
oratones as a metallographer, became Senior Research Fellow in 1968, and retired in 1973
He joined ASTM and Committee E4 in 1940 and was chairman between 1968 and 1972
Metallography at Cornell Umverslty received a b~g boost from the Professor of Metallurgy,
Cecil H Desch of Sheffield University, as nonresident Lecturer (1931-1932) at Cornell, under
the George Fisher Baker Foundation In his lectures, Dr Desch frequently referred to Sorby's
use of the microscope m the study of the structure of iron and steel, pursued purely as science
But Dr Desch also pointed up that this information was quickly applied by industry to
improve products and to invent new ones He also referred to some large mdustnal research
laboratories in the Umted States where both pure and apphed sciences were researched [15]
In February, 1932, Professor Desch became Supenntendent of the Metallurgical Department
of the National Physical Laboratory in England [16]
ASTM Committee E4 on Metallography is a key example of the cooperation among indus-
trial corporations, universities, scientists, engineers, and specmhsts One such industry is the
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ROCHOW ON HISTORY OF ASTM COMMITTEE E4 ON METALLOGRAPHY 87

General Electric Company, and the metallographer around 1938 was Leroy L Wyman, Sr,
who later transferred to the U S Bureau of Standards He was chmrman of Committee E4
from 1938 to 1966, 28 yearsl By 1950 he already had won the ASTM Award of Ment for &s-
tmgulshed serwce "to the cause of voluntary standar&zat~on" H~s serwce to ASTM contin-
ued to grow, and m 1967 he was elected an Honorary Member for h~s "specmlly meritorious
service to the Society [17] " N o t that he did not have expert help The secretary of Committee
E4 for 20 years was Mary R Norton, for whom the Memorial Scholarship Award for Women
is named And there was Joseph R Vdella, of the U n i o n Carbide Corporation and Umted
States Steel Corporation, leader m the preparaUon of specimens for metallograph~c exam~-
nation, for whom the Vflella Award was named for outstanding "merit m the field of metal-
lography [1 7] " T h e r e were, of course, many others who contnbuted to the size, actwlty, pro-
ductwlty, and health of Committee E4 during those 75 yearsV

References
[1] Vander Voort, G F, "75 Years of Metallography The ASTM Committee E4 Perspective," Stan-
dardtzatton News, Vol 19, May 1991, pp 58-77
[2] Sorby, H C, "On Microscopical Photographs of Various Kinds of Iron and Steel," BnUsh Associ-
ation Report, Part II, 1864, p 198
[3] Sorby, H C, "Microscopical Structure of Iron and Steel," Journal oflron and Steel Instttute, 1887,
p 225
[4] Rochow, T G, review of MICRO-65, InternationalSymposium on Applied Microscopy, University
of Shetfield, England, 6-9 July 1965, Apphed Opttcs, Vol 5, 1966, pp 420, 461,462
[5] Martens, A, "Die Mlkroskopiche Untersuchungder Metalle," Glaser's Annalen, 1892, p 201
[6] Osmond, F, "Sur la metallographlc mlcroscoplque," Rapport presente' b,la commission des meth-
odes d6ssal des materlaux de construction le 10 f&ner, 1892
[ 7] Heycock, C T and Neville, F H, "On the ConstltuUon of the Copper-Tin Series of Alloys," Phdo-
sophwal Transacttons', Vol 202, Senes A 1, 1904
[8] "Our Front Cover, Albert Sauveur ( 1863-1939)," Cenco News Chats, No 63, p 3
[9] Sauveur, A, "The Mlcrostructure of Steel and the Current Theories of Hardening," Transac'ttons,
American Institute of Mining, Metallurgical, and Petroleum Engineers, 1896, p 867
[ 10] Sauveur, A, The Metallography and Heat Treatment o! Iron and Steel, The Umverslty Press, Cam-
bridge, MA, 1935
[11] "The Role of the Microscope m Ore Dressing," Ore Dressing Notes, No 5, American Cyanamid
Co, Oct 1935
[12] Vanderwllt, "Improvements in the Pohshmg of Ores," Economzc Geology, Vol 23, 1928, p 292
[13] Rochow, T G and Rochow, E G, Resmography, Plenum Press, New York, 1976
[14] Chamot, E M and Mason, C W, Handbook ofChemlcalMtcroscopy, Vol 1, Wiley, New York,
1930
[15] Desch, C E, "Pure and Applied Science," Sctence, Vol 74, No 1925, 20 Nov 1931, pp 495-502
[16] Vander Voort, G F (note, Dec 1990) notice m Metals andAlloys, Vol 2, No 3, Sept 1931
[17] ASTM 1985 Directory, American Society for Testing and Matenals, Phdadelphm, 1985

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Wilham G. Frlcke, Jr. 1

Research Under the Microscope


REFERENCE: Frlcke, W G , Jr, "Research Under the Microscope," Metallography Past,
Present, and Future (75th Anniversary Volume), ASTM STP 1165, G F Vander Voort, F J
Warmuth, S M Purdy, and A Szlrmae, Eds, American Society for Testing and Materials, Phll-
adelphm, 1993, pp 88-106

ABSTRACT. Microscopes help man to see All microscopes and ,maglng devices have an inher-
ent resolution that limits the maximum magmficatmn at wh,ch they can be used The pnnclple
of scanning greatly simplifies an ~magmg instrument and sometimes is the only way a picture
can be made Any s~gnal that varies in various areas of a sample can, m pnnople, be used to
make an image

KEY WORDS. m~croscopes, scanning, transm~ssmn electron microscope, electron m~croprobe,


auger, image analysis, local orientation, metallography, metallurgical speomens, mlcrostruc-
ture, metallographlc techmques

Come, let us ramble in the world of microscopes that I have known in my 37 years at Alcoa
and along the way look at research--research, first of all, as we use a microscope to do it, but
then let us put research itself under the m,croscope and wax philosophical You might call this
talk, "Microscopes I Have Known "
We sometimes say a p~cture is worth a thousand words I suggest that pictures are more
~mportant than that When you look into a microscope, you not only see an image, but with
your mind you interpret what you see and get an overall impression, capture the very essence
of the specimen You appreciate what the Germans call its "Gestalt " Y o u become part of the
material when looking through a microscope and, through emotion, know what to do about
thmgs
I deplore the kind of engineer who sends samples to a microscopist and says, "Send me back
a p i c t u r e " He then looks at the picture and does not bother discussing it with anybody, all he
wants ~s a pretty picture to suck m a report to say, "This is my material " Instead, you really
must get familiar with the samples you're working with You have to understand, become one
with the material
Everyone who was around 48 years ago remembers what he was doing on 7 December,
1941, Pearl Harbor Day, when the United States got into World War II Actually, the Euro-
pean war had started two years earlier than that, in September 1939 It was about that time
that something happened when I was walking to school I was in seventh grade, 13 years old
It was a foggy morning and I heard an airplane flying overhead. With my thoughts being on
the war, which had just started, I imagined that someday I might be up there in a plane hke
that, I might want to look through clouds and see what I wanted to bomb So I invented some-
thing I called the cloud-piercing telescope (Fig l) I knew that infrared radiation could go
through clouds a lot easier than visible light could, and so I Imagined a device where infrared
hght coming from the ground went through a lens and was focussed onto an array of photo-
cells--hundreds of them in each direction The individual photocells each put a tiny electrical

Fellow, Alloy Technology Division, Alcoa Laboratories, Alcoa Center, PA 15069

88

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FRICKE ON RESEARCH UNDER THE MICROSCOPE 89

FIG. 1--The cloud-piercing telescope invention.

current into individual wires that went up to a viewing screen in front of the pilot. There each
of these wires had a little light bulb; and the light would get bright if a lot of radiation was
hitting the corresponding place in the detector array, or dark if only a little bit of light was
hitting it. The overall effect would reproduce an image of the ground.
I was so proud of the concept that I submitted that idea to the War Department, and they
even acknowledged my letter. They were kind to me, but even as a seventh grader, I knew there
were a couple of things wrong with that idea. For example, it was too complicated. Look at all
those wires and cells. There are too many things to go wrong and it was too heavy. But worse
than that, with those light bulbs in there, even in the little shadow boxes I visualized, the points
of light were just too big. All you would really see would be a bunch of light bulbs, some lit,
some not lit. In order to get a true impression of the scene below, you would have to back up
quite a bit so the lights would blend into each other, and even then you could never hope to
see objects in the image smaller than the individual photocells. The resolution was not good.
Two things were wrong: the instrument was too complex and the resolution--the ability to
distinguish fine detail--was poor. I could have made the whole apparatus a lot simpler if I had
realized that I did not have to have all of those detectors connected to all of those output
devices simultaneously. In fact, it could be done by one set moving row by row, point by point,
to build up the picture. I would not have a simultaneous picture, but I could have a picture
accumulated over time. Our television sets do that.
This limitation called resolution is a problem that's always with us in any kind of imaging
device. The situation is that of Fig. 2. Here two fellows are looking at two very different instru-
ments, one a microscope and one a telescope. Both see somewhat similar things and they both
are saying (probably under their breath), "If I only had a little bit more resolution! This is great,

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90 METALLOGRAPHY:PAST,PRESENT,AND FUTURE

FIG. 2-- The dilemma of resolution.

but I know there's something in there that I just can not see. If I could only improve things
just a little bit, it would be wonderful." Of course, if they did get an improvement then they
would say, "Just a little bit more." We always want more than we can get.
From now on, we will be looking at various kinds of microscopes, seeing what limits their
resolution in each case, and looking at the principle of scanning to see what a powerful concept
it is in giving us information.

l.ight Microscope
Someone asked me one time, "If you could only have one microscope, which one would it
be?" I said, "'Give me a low-magnification stereographic microscope." Many problems are
solved completely at low magnification, but more importantly, to appreciate a material you
must start with a magnification just a little bit more than what the human eye can see. Only
after you appreciate what you arc seeing at low magnification can you go on to higher and
higher magnifications and use the more sophisticated microscopes.
The h u m a n eye, without any lens, can see detail of 0.11 mm, 110 ram. You can not see
anything finer than that because the spacing of the rods and cones in your eye do not allow it.
So, if there is something out there in the world that you want to look at that is smaller, you
need the aid of some sort of a microscope. To see a 1-urn particle, you have to magnify it in
order to get up to the 100-um size that your eye can see. And you have to do it faithfully,
without blurring. A light microscope does that for you by sending light waves to the sample,
and after the light interacts with the sample, say the particle of Fig. 3, you have a lens that
collects the diffracted rays that make up the image that the eye sees. Obviously, that particle
has to change that incoming ray somehow or the eye on the other end will not know it is there.
There are rules of optics that allow you to estimate the fineness of detail, the resolution, that
you can get with a particular lens (Fig. 4). The equation says, among other things, the resolu-
tion depends on the wavelength of the illumination. We commonly use wavelengths about
that of green light where the eye is most sensitive. Resolution also depends greatly on the angle

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FRICKE ON RESEARCH UNDER THE MICROSCOPE 91

FIG. 3--Electromagnetic radiation illuminating a sample. Since a microscope collects diffracted rays
to make an image, the particle will not be seen unless it is larger than half of a wavelength.

over which the bottom lens of the microscope collects light, the so-called numerical aperture.
It also depends, to a slight degree, on the medium between the lens and the sample, the index
of refraction.
When you put typical numbers in the equation, you find that the best light microscope can
resolve detail of a quarter of a micron or larger. How far can you magnify that detail to the
size where the human eye can see it (make it 110 um across)? If you magnify only X400, you
can see that quarter-micron object in the image. It does not do any good to magnify more than
X 400, because the detail is not in the original image. Actually, though, the human eye appre-
ciates having a little bit of fuzziness, so you can conveniently go up to magnifications of about
X 1000 in the light microscope.
So much for resolution; what about the subject of scanning? Even light microscopes some-
times do scanning. Here is one that I like in concept (Fig. 5). One problem with light micro-
scopes is that they focus only on one plane. Anything higher than that or lower than that is out
of focus. So if you have a material that extends into the third dimension, all you can see is a
ring around objects at the plane of focus. Anything about that plane or below it would be out
of focus and makes blurry areas in the image. Well, this microscope shown says if certain areas

FIG. 4--Equation for resolution when electromagnetic radiation is used.


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92 METALLOGRAPHY PAST, PRESENT, AND FUTURE

FIG 5--A hght mlcro~6ope that scans

are going to be out of focus anyway, let us not illuminate them Let usjust illuminate the parts
that are in focus The illuminator projects a plane of light intercepting that specimen along
that line that is in focus Let us take a picture of that and then scan the illumination and the
microscope together so successively new areas will be illuminated and in focus Ultimately, we
will have a whole picture with the whole specimen in focus and well lit and we've done it a step
at a time The confocal light microscopes that are appearing on the market work similarly
They scan points ofhght not only up and down, but sideways as well Once you begin thinking
of scanning as a potential fix to your problems, you get all sorts of Ideas

Transmission Electron Microscope


Before we look further at scanning-type instruments, let us look at another that, like the light
microscope, has the picture present all over at one time, the transmission electron microscope
(TEM) When I came to work 37 years ago, we had two kinds of microscopes the light micro-
scope and the TEM The TEM at that time was a little thing, a desk with a short microscope
column about a foot high It took pictures at two magnifications 600 and 6000 In order
to change from one magnification to the other, you had to take out the entire lining tube, put
it aside, and get the one for the other magnification I took a few mlcrographs in that instru-
ment personally, but the experts tried to keep me away from it The electron microscope was
too complex, too sophisticated, for a young engineer like me
How does the TEM solve the problem of resolution9 Why are we able to go to the very high
magnifications known today, over ten times higher than that early electron microscope9 The
primary advantage is the wavelength of the illumination used Electrons typically have wave-
lengths on the order of four hundredths of an angstrom (Fig 6) This is many orders of mag-
nitude finer than the radiation used In a light microscope and so the resolution IS much better
Unfortunately, a typical TEM also has poor numerical aperture, the angle through which the
illumination comes from the sample is small Fortunately, the favorable wavelength effect

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FRICKE ON RESEARCH UNDER THE MICROSCOPE 93

Transmission Electron Microscope

At 100 KV, ~. = 0.037 ~,

Typically:
cz = 0 o 3 0 '
sin ct = 0.01

Resolution = 0.2 nm
FIG 6--Resolution m the transmission electron microscope determined by the equauon o f Fig 4

overpowers this negative aperture effect, and so we get resolutions typically two-tenths of a
nanometer With care, we can do better than that these days, all because we have changed the
illumination from light to electrons
Nowadays, many TEMs even do scanning (making them STEMs), they measure crystallo-
graphic orientation and do chemical analysis. But the classical TEM and the light microscope
are alike in that they have the image present all over, all at once If we start exposing a picture
in this kind of microscope and stop the exposure halfway through, what we have is the picture
that is half exposed--but it is a full picture If we did that with a scanning microscope--stop
halfway through--we would have half a picture, but that half of a picture would be fully
exposed

Electron Microprobe
The next instrument I was associated with ( 1961) was the electron microprobe Notice, I did
not say the scanning electron microscope (SEM) The SEM came later, it is a modified micro-
probe As a matter of fact, our first microprobe, when we got it, did not do scanning Some-
where around 1965, we added ordinary oscilloscopes that provided the ramping voltages to
both scan the beam m the instrument and the beam in the cathode-ray tube used for viewing
An ordinary oscilloscope camera photographed the screen and that was the micrograph In
those days, charged pairs of plates were used to steer the beam over the specimen
What happens when an electron beam hits a material9 Every one of the signals shown in
Fig 7 has been used to make pictures Figure 10, for example, will show a micrograph made
with the electrons captured in the sample (shown schematically at the bottom of Fig 7) We
also have backscattered electrons coming from the impacted areas, electrons that bounce out
of the sample They too can be used to make a picture Secondary electrons, low energy elec-
trons that get jostled out, can make a picture and are the most common source for SEM micro-
graphs Some of these electrons (auger electrons) have particular energies that give us lnfor-
matLon about the kind of atoms in the sample and these can make a composition image X-
rays also give us compositional information Some samples will give off visible light, and you
can get a light mlcrograph out of a microprobe or a scanning electron microscope Anything
else that happens in the material when it is prodded with an electron beam or some other
energy source can, m principle, be used to make pictures if we have a detector for it
Figure 8 shows, m more detail, the paths that individual electrons make as they go down
through a material Most of these electrons follow tortuous paths as they bounce offofatoms
Some even come back out of the sample These are the backscattered electrons Along the way,
secondary electrons are generated throughout that entire bulk However, since secondary elec-
trons have low energies, it 1s only the ones near the surface that can emerge from the material

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94 METALLOGRAPHY PAST, PRESENT, AND FUTURE

FIG 7--StgnaA artsmg [rom a sohd sample when struck by an electron beam

and get detected and appear in the picture It is only that area right around the incoming beam
that is seen by a SEM in the secondary electron mode That is why resolution ~s much better
for secondary electrons than backscattered electrons or X-rays
In the lower part of Fig 7 are circled points where its calculated X-rays emerge A quantum
of X-ray comes o f f o f e a c h point indicated It can be seen that the X-rays are generated from
a large volume and they also escape from the specimen easily The resolution for X-rays and
for backscattered electrons IS consequently rather poor, several microns for aluminum
Figure 9 is a light mlcrograph of a casting alloy and Fig 10 shows images of this same area
taken o f f o f o u r original microprobe, the one with electrostatm deflection The first mlcrograph
of this area was made using the electrons conducted through the sample, the ones captured by
the sample Because different areas of the sample captured more or less electrons from the
beam, contrast was built up Most people are used to seeing backscattered electron pictures,
this is the opposite phenomenon, the electrons that are not backscattered The remaining pho-
tos are X-ray maps If we had a light microscope and used it to look down at the sample and
could see particular X-rays coming off, these images are what we would see If we could see
iron X-rays, we would see them coming from those outer particles that contain iron, and we
would also see some silicon X-rays coming from the same ones, even a little bit of copper The
inner particles there contain magnesium and slhcon, as seen in those pictures
We have here an analytical tool, but it is awfully qualitative We would get more quantitative
results from a stationary beam sitting on a particle However, human beings so like pictures,
so hke to think with images, that they often prefer this kind of information Therefore, we end
up giving them both the quahtatlve image and the quantitative analyses

Scanning Electron Microscope


Let us move on to the variation of the microprobe that is intended primarily to make elec-
tron pictures of bulk samples the scanning electron microscope We have an electron beam
that moves over the specimen in a series of parallel lines, while simultaneously, a point ofhght
on a cathode-ray tube (CRT) (a television-hke screen) is moving In the same pattern (Fig 11)
They are doing this scanning in synchronization with each other Now, all we must do to make
up a picture is to measure some signal from the specimen and ask, " H o w many electrons are

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FRICKE ON RESEARCH UNDER THE MICROSCOPE 95

~c

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96 METALLOGRAPHY: PAST, PRESENT, AND FUTURE

FIG. 9--A photomicrograph of an aluminum casting alloy (light microscope).

coming off of each of those points as I go over them?" Feed that information into the CRT
and make the spot on the screen bright or dark, as the signal changes, and we build up a picture
like this (Fig. 12). As we went over one area of the sample and there were a lot of electrons
coming off, we would paint the picture bright. When we went over another area and there was
a medium number of electrons coming off, we would put a medium brightness light on the
screen, and so forth. Notice that, in principle, the image is divided up into a bunch of little
squares, like my original cloud-piercing telescope, and the finest of the detail (the resolution)
has to do with how tiny an area on the specimen is emitting that signal. For X-rays, those
squares are relatively big; for secondary electrons, the squares are small. In other words, the
effective size of the squares (pixels) making up the pictures is the resolution itself.
Before we leave the SEM, let us look at just one scanning micrograph to illustrate a point as
well as to pique your curiosity. Figure 13 (left) is a SEM shot of a sample etched in caustic. See
the little craters on the surface in the left photograph? It so happens that we can ordinarily
believe our eyes when we look at a SEM micrograph, even though the picture was made with
electrons and our eyes are not used to seeing electrons. Fortunately, the impression we get is
the same as if we were looking with light, and since we are educated to interpret things with
light, we can quickly appreciate what we are looking at there. (Incidentally, that is not true
with TEM; we have to sit down and consciously think what is causing contrast in the TEM.)
On the fight of Fig. 13 there is another micrograph that looks completely different, but in real-
ity, is the same picture turned upside down. The reason it looks different is that our mind is
interpreting changes of illumination as ups and downs. SEM micrographs usually appear to
have oblique illumination. As long as we keep the apparent source of illumination coming

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FRICKE ON RESEARCH UNDER THE MICROSCOPE 97

FIG 10-- lJhcropmbepi~tmes o/ H~e same area as big 9 The hrsl photo used spec tmen emrenl and the
others used X-ra~ s o/ parttL ular ~ ave/en,~lhs lhal ~ould be tdenldted ~ ith lhe elemenls mdtcated

from the t o p ( l d t p h o t o ) , o u r m i n d interprets surface c o n t o u r s correctly If we turn the picture


upside d o w n ( r l g h t p h o l o ) , the a p p a r e n t source o f i l l u m i n a t i o n ~s c o m i n g from the b o t t o m , but
o u r m i n d rejects t h a t W e n e v e r h a v e a s~tuatlon zn real hfe where s u n h g h t zs c o m i n g out o f
the g r o u n d A n d so we say, " N o t h a t c a n n o t be n g h t , the light has to be o u t there, the s u n is
o u t t h e r e s o m e p l a c e a n d so I a m going to interpret those features as hills r a t h e r t h a n
depressions "

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98 METALLOGRAPHY PAST, PRESENT, AND FUTURE

FIG 1l - - T h e ra ~terpattern u~ed In scanning The dashed hne Is the retrace path

Auger Spectroscopy
We said a while back that s o m e o f the secondary electrons c o m i n g off the sample have par-
ticular energies that are characteristic o f the elements in the sample These are auger electrons
Although an auger instrument usually works with a stationary electron beam, if we can scan
the b e a m and m a k e the auger electron detector accept electrons from only one kind of atom,
we get element distribution maps similar to Fig 10 However, since auger electrons c o m e from
only the outer 20 A or so of the surface, these element maps show what kinds of atoms are
sitting right on the surface and how they are distributed
A look at the energy levels o f electrons inside an a t o m will Illustrate where auger electrons
c o m e from and give us a review of other signals that can be used in microscopes (F~g 14) The
energy levels represented by horizontal lines are at particular locations for each kind of atom
T h e y are occupied by those little fellows shown m the figure that are electrons When we shoot
an external electron at such an atom, we are occasionally going to hit one of those electrons
sitting in the a t o m and knock him away Measure the energy of that fellow who used to be in
the a t o m and we have a t e c h m q u e called ESCA, electron spectroscopy for chemical analysis,
because measuring the energy of that level tells us what kind of element that was That electron
that caused the d a m a g e and bounces off~s one of those baekscattered electrons that we can use
to m a k e a picture
The atom, of course, does not like to have an electron missing, especmlly if, as in the picture,
~t is one of the m o r e t~ghtly b o u n d ones O n e way to get an electron back into the lower energy
level is to capture s o m e other electron sitting on an upper level W h e n one of ItS own electrons
(that electron pictured with the parachute) m o v e s down, the atom loses some energy H o w
does that a t o m get rid of that energy9 O n e thing it can do, and all atoms can do it, is emit an

FIG 12--Sketeh o! the ~trength of the signal coming from various areas of the sample and the corre-
sponding brightness on the vlewmg screen

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FRICKE ON RESEARCH UNDER THE MICROSCOPE 99

FIG 13-- Two S E M mtcrographs of an etched ~urface The right photo ts the same a ~the left, but turned
up~tde down

X-ray quantum The X-ray has an energy equal to the energy difference between where the
parachuting electron was and where it ended up If we used an electron microprobe, for exam-
ple, to look at the energy of that X-ray, we could make an analys~s or store the information as
part of a picture Another way for that particular excited atom to decrease its energy, however,
is to put that energy into another electron, get nd of another one of its other electrons and put
all that energy into kinetic energy That ejected electron is the auger electron represented by
the fellow m the balloon
When we have a material with lots of atoms being bombarded by an electron beam, some
of them will be ejecting auger electrons and some of them will be e m m l n g X-rays Both signals
will be coming from the sample And some of the energy of the probing beam will bejosthng
low energy electrons out of the upper energy levels (hghtmg a match under them in Fig 14)
and producing secondary electrons Remember that any of these events can be used to make
a p~cture
Let us pause for a summary here Resolution--the finest of detail in an ~mage--depends on
where the sxgnal ~s coming from In instruments hke the auger, SEM, and m~croprobe, ~t is the
area from around the incident beam that emits those electrons or X-rays that determines the
fineness ofdetad that we can image (Table 1) So with X-rays, we have resolution of about 2
um, with auger electrons, considerably better than that Modern auger instruments use a
focused electron beam and they can get resolutions on the order o f h a l f a micron In a SEM,

TABLE l--Rewlutton of various mtcroscopes

Maximum
Finest Detad,/~m Magmlication

Microprobe (X-rays) 20 100


Auger
m depth 0 002 100 000
laterally 05 400
Scanning electron microscope 0 006 30 000
Light microscope 0 27 1 000
Transmission electron microscope 0 0002 1 000 000

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100 METALLOGRAPHY:PAST, PRESENT,AND FUTURE

FIG. 14--Energy levels in an atom showing the source of backscattered, secondary, auger, and ESCA
electrons as well as the transition that produces X-rays.

about 60 A is typical resolution these days. The two instruments that use overall illumination
by electromagnetic radiation depend on wavelength for their resolution. The light microscope
gives us about a quarter of a micron resolution, and TEM gives us four ten-thousandths of a
micron resolution. When we take advantage of these resolutions by magnifying the detail to
the size that the h u m a n eye can see, the m a x i m u m useful magnifications that we can get are
indicated in the last column of Table 1.

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FRICKE ON RESEARCH UNDER THE MICROSCOPE 101

ScanningTunnelingMicroscope
There are other kinds o f microscopes, o f course, s o m e of t h e m just being developed O n e o f
t h e m is the scanning t u n n e h n g microscope. It is a very simple microscope in principle There
is a pair o f translating devices to physically m o v e a needle m the X a n d Ydlrectlons The point
o f that needle, hopefully sharp to a t o m i c dimensions, is maintained at a constant distance
above the surface o f the sample by maintaining a constant tunneling electrical current or
a t o m i c force Meanwhile, the data collection system is recording the input needed to maintain
the separation In other words, we have a surface roughness m e a s u n n g device of atomic
dimensions where we get pictures reconstructed through a c o m p u t e r Distances are measured
in n a n o m e t e r s In ideal cases, we can detect the ups and downs as the needle moves over indi-
vidual a t o m s

Image Analysis
As soon as s o m e o n e gives a scientist a picture, the first thing he or she wants to know Is, how
big is that thing there or how m a n y of these things do I have here Getting quantitative infor-
mation from a microscope or mlcrograph is called image analysis Along the way, we often
c o m p u t e i m p r o v e m e n t s to the image as well That is called image e n h a n c e m e n t
The secret to getting an image into a form that a c o m p u t e r can deal with it is to dlgmze it,
break it up into picture points (plxels) T h i n k back to m y cloud-piercing telescope I had light
bulbs arranged m a grid pattern, the picture was broken up in a series o f points close enough
together so that the h u m a n eye could not see that they were not continuous A digitizing T V
c a m e r a on a hght microscope or a similar device on a SEM can break the image into a series
o f picture points each o f which has an associated n u m b e r that represents the brightness at that
particular point (Fig 15) O n c e the data are m a form that a c o m p u t e r can read, all sorts of
c o m p u t a t i o n s are possible

004 025 036 121 163 226 178 152 102 089

124 078 023 133 187 204 172 144 085

255 174 033 167 199 210 189 132

231 189 042 196 174 186 145 172

203 187 078 098 127 173 131

196 163 064 045 103 147 122

154 112 038 053 089 093

128 130 042 028 064

085 086 044 027 057

062 075 038 026


FIG 15--Data representmg a dtgtttzed ptcture The numbers are brtghtness levels These are the num-
bers producmg ~ontrast as m Ftg 12

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102 METALLOGRAPHY PAST, PRESENT, AND FUTURE

For example, the top left photo in Fig 16 is an original picture presented to a c o m p u t e r We
can see that the illumination was not uniform The left side area is darker than the right side
Since we are dealing with numbers, it is easy for a c o m p u t e r to i m p r o v e the p~cture It just
measures the average brightness in one locaUon and adjusts it to s o m e standard level that has
been set, and measures the average brightness m another area and brings everything to the
same average to wipe out that illumination difference (top rtght o f Fig 16)
A n d the c o m p u t e r can do things like fill In little gaps m the grain boundaries, change the
overall contrast, and so forth It can emphasize some things, de-emphasize some other things,
and completely get rid o f features that it does not hke because of size considerations or other
criteria Eventually, we end up m a r k i n g the things that we want to measure by creating a
binary picture where everything is either white or black, leaving bright the things that we want
to measure (lower left, Fig 16)
Since the whole picture IS broken up into an array o f picture points, measuring these is now
fairly simple T o measure the area o f a particle, we just c o u n t the n u m b e r of picture points in

FIG 16--Dtgltlzed mlcr(~Traphs The upper le[t is the orlgmal tmage The uppet rtght Is aper shading
corre~tton, and the lower left ts a binary (black-)4har tmage ready[or measurement

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FRICKE ON RESEARCH UNDER THE MICROSCOPE 103

the particle To measure a chord, we just count the number of picture points along the chord
To measure the perimeter, we measure the number of picture points all the way around the
outside of a feature

Local Orientation Measurement


Crystallographic oraentatlon Is not something that makes an image, but xt is something that
can be measured in a m~croscope Since gram orientation is important, we have attachments
on our SEM and T EM to make rapid evaluation ofbackscattered electron diffraction patterns
(KJkuchl lines) The patterns have always been there if we wanted to look at them What is
new is that a computer assists us m rapidly reconstructing the crystallographic radices for the
orientation of that particle crystal

Stereo Micrographs
The third dimension, the height dimension, is often important We can get a qualitative
impression of height on almost any of these microscopes by taking two pictures at an angle to
each other, one for each eye These can be put into a stereo viewer to visualize the third dimen-
sion or even measure the elevation of a few points But we are still tookmg for easy ways to
characterize the ups and downs of a rough surface quant~tatwely and m detail, not just a few
points, but all over so we can, for example, analyze fracture surfaces to estabhsh failure
mechanisms

The Future
Now we are beginning to estabhsh a wish list for the future What do we want9 Back in 1976,
I good-humoredly perpetrated a hoax about supposed late-breaking developments around two
new microscopes, the flashdark microscope and the temporal scanning microscope When I
sent the article in for publication, I intended it for a column called "Light Metallurgy," light
in the sense of not heavy, even frivolous But even back there in 1976, microscopes were com-
plex enough that nobody could really keep up-to-date, nobody could quite dare to say, "There
ain't no such t h i n g " Today things are so complex that people are almost sure to believe if we
tell them it is so
The supposed flashdark microscope worked on the premise that if there is something called
a flashlight, it is reasonable that there is a flashdark as well Now, we can not see the particles
inside a piece of aluminum, for example, because the light bounces off of the surface--and it
is left dark down in there But If we use a collimated beam of darkness, the dark can penetrate
down inside the metal and we can see those particles
An even more important concept is the temporal scanning microscope (Notice my empha-
sis back then on the concept of scanning ) A time machine on a microscope would be useful
for things like failure analysis, allowing us to see what conditions were dunng the actual failure
Although the Instrument Itself IS a hoax, temporal scanning has been done and I have done
it Figure 17, for example, out of one of my early papers, shows a fatigue crack at increasing
numbers of cycles You might ask the question, " H o w did I know that something interesting
was going to happen to the tip of this crack so that I took this series of mlcrographsg" And the
answer is, I did not know that something interesting was going to happen I waited until I saw
that something did happen and then scanned backwards in time I took the last micrograph
first and then the next-to-the-last, etc That was possible because I had replicas of what the
material looked like at those previous stages I had frozen time

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104 METALLOGRAPHY:PAST,PRESENT,AND FUTURE

FIG. 17--The same fatigue crack seen at successive times in its Ire. The numbers are millions o f cycles
(light microscope).

Another example of time scanning, this one in the transmission microscope, shows a frac-
ture surface made by a stress-corrosion crack (Fig. 18). I managed to mark where it was at one
time before I was able to look at the sample at a later time when the crack had grown further.
Again this was through replicas, but there is no question about how the crack had looked in
the past.
Now we are starting to get serious about what is going to happen in the future of microscopy.
Although it is always dangerous to make predictions, some directions seem evident.
New objective lenses for the light microscope are coming on the market that allow us to back
the microscope away from the specimen. We can get 1-#m resolution, for example, at a work-
ing distance of 152.4 m m (6 in.). This allows us to put windows, environment, furnaces, etc.,
in the gap. It also allows us to look at rougher surfaces without much loss of resolution.
I think we are going to see a lot more of computers. I think there will be a lot of image storage,
the digitized pictures going into rather permanent files, so that microscopists can call up an
image of what typical material looks like, to compare to their present specimens. They will not
have to go digging through the files and trying to find a micrograph of something they have
done before. The images will be accessed by other people in other groups and other buildings.
I think we will be seeing scanning pictures using novel signals. After all, any signal that
comes offthe sample that makes changes in a detector can, in principle, be put into a picture.
Ultrasound--we are already into ultrasonic microscopes--infrared, sonic emission, or per-
haps, a microscope built on, say, smell. If we had a detector for smell, and the smell varied
across the specimen, we could get a smell picture. Who knows?
Let us get philosophical. Who does microscopy? Who should do microscopy?

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FRICKE ON RESEARCH UNDER THE MICROSCOPE 105

FIG 18--A s'tre~s-corroston crack m a r k e d / o r where tt was at one ttme /or vtewmg at a later ttme

Microscopes are powerful instruments and I think microscopy has to be done on two levels
The ordinary researcher, somebody whose main interest is in precipitation or recrystallizatlon
or some metallurgical phenomenon, should not be afraid to use a microscope In fact, he or
she has to use a microscope to see in his head what is happening That does not mean just
looking at mlcrographs that somebody else takes He has to be there looking at the sample,
moving around and seeing the overall process He has to get the mental picture
But we also need experts, those whose profession is microscopy, those trained, those who
will guide the other fellow and do some of the work for him or her
And that raises the question of where the microscopes should be It is not an easy question
to answer There is something to be said for the microscopes being where the research is being
done The individual investigators are more likely to use the microscopes if they are close by
The microscopes become more involved in the projects The response time for work tends to
be short

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106 METALLOGRAPHY PAST, PRESENT, AND FUTURE

But we can also make a good case for having all the microscopes and all of the microscopists
in one central location and require that the investigators and samples come to the central
microscopy laboratory That way, because of proximity, there is communication between
microscopists They stimulate each other, profit from past experience They share reczpes,
avoid blind alleys Equipment is better utilized and expensive duplication avoided The
approach is more professional ! tend to favor this approach
But I suggest that there is a test for determining if the microscopist m your area is justified
It is through the word "exult " I f your microscopist is good and knows he or she is good, if you
have challenged him or her with Interesting work, if he or she contributes to projects and prob-
lem solving, if he or she is eager to come to work each day, m short, if he or she "exults" m his
or her work, you have a valuable and necessary individual
I've exulted m my work for 37 years

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Metallographic PreparationTechniques

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Gerald S. Cole, ~Leslie Bartosiewlcz, ~a n d F l o y d E. Alberts ~

Automotive Materials and Their


Characterization: 1916 to 1991
REFERENCE" Cole, G S, Bartoslewlcz, L, and Alberts, F E, "Automotive Materials and
Their Characterization. 1916 to 1991," Metallography Past, Present, and Future (75th Anmver-
sary Volume), ASTMSTP 1165, G F Vander Voort, F J Warmuth, S M Purdy, and A Szir-
mae, Eds, American Society for Testing and Materials, Philadelphia, 1993, pp 109-138

ABSTRACT" The automotive industry has been altered enormously since the era of the Model
T This paper describes some of the reasons for the changes in terms of technological drivers,
especmlly in terms of how new materials and processes ~mprovecomponent functmnahty Sev-
eral materials used in the Model T, such as cast iron, steel, glass, and ceramics wdl be compared
to modern materials used in a vanety ofautomotwe components The key systems of the vehicle
represented include electncal, exhaust, powertraln, chmate control, and body

KEY WORDS. automotive materials, metallography, metallurgacalspectmens, mlcrostructure,


metallographlc techniques

Automobiles have changed enormously since the early 1900s in almost every detail of mate-
rials and manufacturing With respect to material changes, vehicle bo&es were based on con-
ventlonal cold-rolled steel and have evolved into new high-strength, galvanized, bake harden-
able, dent, crash, and corrosion resistant steels, aluminum, magnesium, polymeric, and metal
matrix composites make up a growing list of lightweight materials, cast irons now include
spheroidal and compacted graphites along with the more common flake form, new ceramic
materials have been developed for catalysts and turbine blades whde semiconductors are now
used m electronic devices, complex glass/polymer laminates have replaced the dangerous sin-
gle panes of glass, high-strength steels have been developed for lighter weight, high-tempera-
ture materials, such as titanium alloys, have been developed for exhaust valves, and so on
With regard to components powertrams are low-polluting, lower weight, lower friction, and
more responsive, new sealed-beam halogen designs have changed our hghtmg concepts, com-
puterized slhcon-based digital controls have replaced analog circuitry, seat belts and air bags,
coupled with anti-lock brakes provide considerable more safety to the driver, and so forth
New design, fabrication, and assembly techniques have had to be developed to produce the
new components from these new materials
Material analysis in the Model T era used classic metallography, based only on light micros-
copy The matenals and components m modern vehicles require materials characterization
methodology based on a much broader range of sophisticated instrumentation scanning and
transmission electron microscopy (SEM and TEM), electron microprobe analysis (EMPA),
and electron and X-ray spectroscopies
Since the authors collectively have worked over 75 years in the automotive industry, we
dec~ded to commemorate thin seventy-fifth anmversary of the ASTM Committee E4 on Met-
allography by reflecting on the auto lndustry's 75 years of metallography and materials expe-

SoentlfiC research staff, Ford Motor Company, Dearborn, M148121

109

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110 METALLOGRAPHYPAST, PRESENT,AND FUTURE

hence Because of our association with Ford Motor Company, we will &rect our presentation
to comparing differences between some of the materials used in the Model T and in present
Ford vehicles
The Ford Model T was introduced a httle more than 75 years ago (in 1908 to be exact) but
really reached its stride by 1916 when over 500 000 umts were produced Figures 1 through 5
show sections of this vehicle that revolutionized the personal transportation industry of the
world Figures 1 and 2 show right and left sides of a conventional four-passenger Model T,
Figs 3 and 4 show the components of a "Touring Model T," and Fig 5 depicts the powertraxn.
It is interesting to note that by 1916 the overall functlonahty of the automobile had been fairly
well defined with the major components--powertraln, dnvetraln, body, chassis, exhaust, inte-
rior, electncal, and fuel systems--not &ffenng much from modern vehicles (see Appendix I)
Upon examining the literature of circa 1916, we realized that there was not too much dif-
ference between the metallographlC techmques used then and those used today Metallo-
graphic samples were cut, mounted (albeit with Canada balsam rather than with polymeric
materials), ground, polished (using many of the presently used materials except diamond), and
etched (with nitric, pacrlc, hydrochloric, and sulphunc acids) as today Microscopy was begin-
nmg to be developed and there were even metallographs to take photomicrographs, see Fig 6
[ 1] Other authors in this conference will discuss these developments m more detail Our paper
will focus more on the applications of microscopy for materials characterization, particularly
with respect to the materials and components used m the automotive industry
Because of space constraints, it is Impossible to examine all the components, and their con-
stltuent materials, used in the Ford Model T Rather, we wdl analyze the material makeup of
some e~ght components that we were fortunate to obtain from a local Model T restorer The
Model T used many materials that are still employed to this day (see Appendix II) examples

FIG l--Ford Model T, right sld~

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COLE ET AL. ON AUTOMOTIVE MATERIALS 111

FIG. 2--k~)rd Model T, left side.

have been selected (and are starred*) from cast iron, steel, aluminum, copper, glass, ceramics,
and paint.
Modern vehicles are very different in design (compare Figs. 7 through 9 with Figs. I through
5). The overall view of a 1990 Ford Probe is seen in Fig. 7, the body and chassis in Fig. 8, and
the powerplant in Fig. 9. However, the major materials used in today's cars are not altogether
different from those used in the Model T (see, for example, Table 1).
Materials trends from 1975 to 1985 (Table 2) demonstrate continuing reduction in total
vehicle weight achieved by a marked reduction in the amount of steel.

The Evolution of New Materials and Components


On examining the changes between the Model T and the present generation of vehicles, it
is interesting to surmise how and why the materials and components have evolved. The many
driving forces for technological change are exceedingly complex. They can be cataloged in

TABLE 1--Materials" used in Model T and modern cars.


Material Model T, % Modern, %
Rubber 3 4
Wood 14 9 (polymers)
Glass 4 3
Aluminum 6 5
Iron 10 13
Steel 47 60

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112 METALLOGRAPHY PAST, PRESENT,AND FUTURE

TABLE 2--Materials m the automobtle (rounded weights and percentages) a


1975 Car 1985 Car

Matenal Weight, lb % Dry Weight, lb % Dry

Steel
Cold Rolled 530 20
Other 2300 850 30
HSS 100 270 10
2400 65 1650 60
Grey ~ron 600 15 370 13
Aluminum
Wrought 40 1
Cast 110 4
100 3 150 5
Magnesium
Copper/brass 40 25 1
Lead 30 3 30 1
Zinc die castings 30 10
Glass 90 2 75 3
Plastics 160 4 235 9
Rubber 180 5 125 4
Sound deadener 90 2 60 2
Miscellaneous (paint, adheswes, 50 2
textiles, etc )
Average dry weight 3800 2800
a 1 lb = 0 029 kg

terms of technological change pushed by product (that ~s, vehicle) considerations, changes in
manufactunng technology, and governmental pressures (acting as a catalyst) A bnefdescnp-
Uon of the pressures for change are included m Appendix III(a) and (b) for the reader who
wishes to understand the pressures that drive evolutionary change in the automotive industry
The selection of materials and components that have been selected for analys~s include a
cross-sectmn of ~mportant components used m the automobile.

1 electrical system (spark plug),


2 exhaust system (catalyst and muffler),
3 powertram (valve, from gray cast iron and steel),
4 dnvetram (transmission axle and gear from alloy heat-treated steel),
5 chmate control (radiator from brass and aluminum),
6 body structures (stamped box from painted cold-rolled steel), and
7 windshield (glass)

A short description of each component wtll be presented including mlcrographs companng


the Model T and modern component, where possible The authors will try to consider some
of the crmcal product and materials features that differentiate component, materials, and pro-
cess development over the last 75 years

Electrical System
The spark plug lgmtes the fuel charge by taking the electrical impulse from the ignition sys-
tem and discharging it across the gap between the plug electrode to produce a spark to ignite

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COLE ET AL ON AUTOMOTIVE MATERIALS 113

FIG 3--Ford Model T, schemattc of body structure

the gasohne/alr mixture The cnUcal ~ssue ~s that there ,s no eas~er path for the electrical dis-
charge than across the gap to form a combusUon-promotmg spark Historically, ceramic insu-
lating materials have predominated, but at various t~mes, glass, quartz, mica, and even wood
have been employed The Model T used a porcelain, clay-based ceramic These materials were
excellent electrically at room temperature when unstressed, but of poor strength when sub-
jected to mechanical pressure and thermal shock Figure 10 shows the design of the modern
and Model T plugs Figure 11 shows the structure of a modern plug m more detail

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114 METALLOGRAPHY PAST, PRESENT, AND FUTURE

I
L~

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COLE ET AL ON AUTOMOTIVE MATERIALS 1 15

I
L~

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116 METALLOGRAPHY:PAST, PRESENT, AND FUTURE

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COLE ET AL ON AUTOMOTIVE MATERIALS 117

FIG 7--1 otd Probe

Charactert s'ltcs o/ the ( eramlc


The heart of the spark plug is the insulator The demands on this ceramic component are
very. severe, and according to Owens et al [2], has the following properties

1 High strength to withstand the severe mechanical stresses of the assembly and installa-
tion and the large thermomechanlcal stresses associated with operating for most of its life
at a red heat with one end under high pressure and the other at atmospheric (and may
even at times be sprayed with water)
2 High hardness to resist abrasion

FIG 8--Ford Tempo, body structure

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118 METALLOGRAPHY:PAST, PRESENT, AND FUTURE

FIG. 9--Cutaway view ~?/t')~rd 12 valve 2.2 L, turhocharged I-4.

3. Electrical resistance: to prevent power loss by electrical leakage over a broad range of
operating temperatures (a resistance of 105 mcgohms or greater is typical).
4. Dielectric strength: to prevent electrical breakdown at potentials that can reach 20 kV or
greater.
5. Thermal conductivity: as the temperature is raised, thermal conductivity increases (as
with most ceramics). When the temperature is <350~ excessive combustion deposits
occur leading to engine misfiring. At temperatures between 500 and 600~ combustion
deposits burn away, but at temperatures >950~ too high a conductivity can lead to
preignition problems. Note that too low a conductivity can reduce thermal shock
resistance.
6. Thermal shock resistance: since spark plugs have to operate at temperatures between
cold incoming fuel air mixtures at subzero temperatures, greater than 800"C temperature
of the exhaust gases, and in approximately 1 min.
7. Chemical inertness: to fuel mixtures and lubricating oil additives.
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COLE ET AL. ON AUTOMOTIVE MATERIALS 119

FIG. 10--(a)Model T sparkplug, and (b)modern spark plug (original magnification, X 1.5).

Electrode Materials
The metals selected for the electrode are important because of the extreme environmental
and chemical conditions operating at the spark plug gap. Electrodes tend to erode in the com-
plex environment of the electrical volatization, high temperatures, and the corrosive nature of
the oxygen and sulfur present in the gasoline. The earliest electrodes were platinum or copper;
later, nickel was used, but was further alloyed with manganese and silicon to increase resist-
ance to sulfur and oxygen attack. The classic manganese-silicon-nickel alloy plug material now
contains titanium, zirconium, barium, thorium, cobalt, and chromium. Some alloy additions
improve the corrosion resistance, either directly or by grain refining; others reduce the work
function in an attempt to influence breakdown voltage. Modern materials use high chromium-
content alloys, but chromium's low electrical and thermal conductivity affects functioning.
Higher heat transfer is desirable, and copper cores are present in the electrodes so that heat can
be more easily removed from the central firing system and back to the engine cooling system
via the plug insulator, body shell, thread, and gasket.

Seal Between Plug and Head


Early components used copper-containing asbestos string; gaskets of rolled copper and steel
were also used. Since smooth gaskets fall offwhen the plug is removed, a locking design is now
used.
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120 METALLOGRAPHY PAST, PRESENT, AND FUTURE

FIG 1l--Schematl~ o/ modern spark plug ( l ) flash over rzbs, (2) termmal post, (3) ceramtc m~ulator,
(4) ~teel shell, (5) hm pre~s groow,, (6) mckel/glars seal, (7) carbon suppresor, (8) shell teat, (9) lower seal,
( 1O) ~hell thread~, ( 11 ) ~opper core center ~lectrode, (12) msulator ttp,(13) ground electrode, and (14) pro-
le~tton mto ~ombu~ton chamber

M o d e l T versus M o d e r n Destgn
As shown m Figs 10 and 11, modern plug materials are composed of an Inconel (trademark
o f INCO Alloys International) sheathed copper electrode, a cold-rolled steel terminal post, a
90% A1203 plus clay porcelain ceramic, and a copper glass seal The Model T materials
included a brass-threaded connector onto the steel base electrode and a carbon-conducting
path between the two electrodes
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COLE ET AL. ON AUTOMOTIVE MATERIALS 121

Exhaust System
The exhaust system for the Model T used a gray cast iron exhaust manifold coupled to a
steel muffler, to reduce the sound of the exhaust. Modern vehicles now require a very sophis-
ticated exhaust catalyst capability. Every car presently built in or imported into the United
States has a catalytic converter to reduce the unwanted pollutants from the combusted and
unburned gasoline vapors emitted from the tailpipe. The catalytic converter increases the con-
version of unwanted exhaust gases such as hydrocarbons water and carbon monoxide (CO)
into nitrogen (N,), carbon dioxide (CO,), and water (H20). The complete exhaust converter is
shown in Fig. 12. The ceramic monoliths, shown below the assembly, are hard ceramics, usu-
ally cordierite [Mg2 (Ai4SisO~0)], having thousands of axial channel openings (approximately
1 m m wide) running from end to end. Each channel is lined with a thin coating o f stabilized
gamma A1203 to promote a large specific area and thermally stable component. The catalyst
itself is either platinum, palladium, or rhodium; Fig. 13 shows the details of the washcoat that
contains the precious metal catalyst. The size and distribution of precious metal is critical,
since a uniformly large catalyst surface area is required to contact and react with the exhaust
gases. The large surface area is accomplished by having the catalyst distributed in small par-
ticles of typically 5 nm or so diameter.

Valvetrain (Valve)
Valves continue to undergo significant design and materials changes since the initial Model
T design was developed. The dual material seen in the Model T valve (Figs. 14 through 16)
results from a cast iron valve body that is friction-welded to the cold-rolled steel stem. The
overall view is shown in Fig. 14. Figure 15 shows the interesting structure of the weld zone
region. The structure of the cold-rolled steel stem is shown in Fig. 16(a) while the typical gray
cast iron structure of the valve head is seen in Fig. 16(b). Much of the materials' developments
in valves has been due to increasing demand for higher and higher engine operating temper-
atures over the past 75 years. This has necessitated more corrosion resistance and higher hot

FIG. 12--Cutaway view o['modern catalytic converter showing ceramic element.


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122 METALLOGRAPHY:PAST,PRESENT,AND FUTURE

FIG. 13--Detailed view o f ceramic monolith with wash coat.

strength. Coupled with the removal of leaded fuels, the requirements for higher power and
improved durability have necessitated that there be reduced wear between the valve, valve
stem, and the head. In the 25-hp Model T engines, both intake and exhaust valves were the
same design and material. This is not true in modern vehicles where both the design and mate-
rials parameters for the intake and exhaust are different. The modern intake valve is composed

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FIG 14--Model T ~@aust valve (X 3)

FIG 15--Structure at welded regton of valve s'tem and head ( 100)

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124 METALLOGRAPHY PAST, PRESENT, AND FUTURE

FIG 16--(a) Structure o! cold-rolled s'teel stem o f valve and (b) ~'tru~ture of grey ~ast m m head ~ectton
o! Model T valve (ortgmal magmfi~atlon, 100)

of a one-piece cold-rolled steel shaft, heat treated at the upper retainer end for wear resistance
Figure 17(a) shows the complexity of the modern valve Both the valve seat configuration and
the valve surface have changed considerably versus the Model T In addition, the steel used in
the modern intake valve is of much higher quality, and this is shown in Fig 17(b) Because of
the higher operating temperatures, the exhaust valve materials are even more comphcated, the

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COLE ET AL ON AUTOMOTIVE MATERIALS 125

FIG 17--(a) Overall shape o[ modern retake valve (X 3), and (b) structure of heat treated ~teel used m
modern retake valve body (X 500)

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126 METALLOGRAPHY PAST, PRESENT, AND FUTURE

valve body is comprised of a hollow (sometimes sodium-filled) high-temperature Inconel alloy


stem that in turn is welded to a heat-treatable steel tip

Transmission (Axle Shaft, Transmission Gear)


The transmission gear and shaft steels used in the Model T were fairly high quality Two
examples are shown in Figs 18 and 19, the axle shaft and a transmission gear The modern
and Model T axle shafts are shown in Figs. 18(a) and (b), at )< 100 While the austenlte grains
are almost identical in the two steels (the Model T has a slightly larger grain size), the carbide
proportion is quite different and the modern steels are correspondingly stronger The modern
and Model T transmission gears are shown at 10 in Figs 19(a) and (b), respectively. In addi-
tion to the different tooth design, the modern version has a case-hardened layer of about 400
#m thick The Model T structure, shown in Fig 19c, has approximately one-tenth as much
hardening depth (to 50 #m) The large difference in microstructure is associated with the dif-
ferent processing available with the Model T Seventy-five years ago, case hardening was either
a salt bath or flame treatment, this was slow, poorly controlled, and produced a shallow surface
treatment. Modern case hardening is performed by induction heating, this takes place in sec-
onds and has a greater effect on the structure The improved properties allow the modern com-
ponent to withstand much higher abrasion and compression loads

Climate Control (Radiator)


It was not until quite recently (the past ten years) that the copper-brass radiator began to be
replaced by other materials Ford Motor Company has been a leader in using lighter weight,
less costly processing in this area Figure 20 shows the vacuum brazed aluminum radiator that
has been the result of many years of metallurgical and process research and development [3]
The new process required that a braze be developed that (a) would not corrode during service
(that is, did not require a flux) and (b) could be applied in such a manner that it would flow at
the processing (brazing) temperature tOjOln the fins and headers without melting through and
destroying the assembly There are many issues that have to be controlled in a brazing oper-
ation the heat source and temperature, vacuum environment, fixturlng, alloy brazes used,
brazing application methodology, etc Figure 21 illustrates the kind of problems that had to
be overcome The photograph on the right shows a void resulting from incomplete brazing of
fins to a header When the temperature became too high (in this case, the control temperature
was only 2~ above the set point), the braze flowed away from the junction and left the
observed void failure The typical brass structure of a Model T radiator component is shown
m Fig 22, it is not different from modern brass microstructures

Body Structures (Stamped Box)


The demands on the steels that formed the body structures of the Model T were obviously
different from those required for the modern vehicle designs The typical mlcrostructure of
ingot-cast cold-rolled steel used in the Model T is shown in Fig 23, there are a sufficient num-
ber ofnonmetalhc inclusions that this matenal could not be used to form the skins of the pres-
ent vehicles Modern body steels are considerably more drawable and are produced by contin-
uously cast low-carbon, low-sulfur steels that often are mlcroalloyed to develop hardening
during paint baking operations There is insufficient space in this presentation to document
the considerable research and development efforts by the steel industry that have resulted m
highly drawable, reduced gage thickness (yet dent resistant), automotive steels developed over
the past 75 years

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COLE ET AL ON AUTOMOTIVE MATERIALS 127

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128 METALLOGRAPHY PAST, PRESENT, AND FUTURE

FIG 19--Transmls~ton gear ( 6) (a) M o d o n gear, and (b) Model T, and (c) Model T transmls ston
gear (ortgmal magmjl~atum, 100)

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COLE ET AL ON AUTOMOTIVE MATERIALS 129

FIG 20--Modern vacuum-brazed radiator

FIG 2 l--Structure oHm~header region (ortgmal magndl~atton, X 100)

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130 METALLOGRAPHY PAST, PRESENT, AND FUTURE

FIG 22--Structure o! conventional brass sectton of Model T radtator (X 100)

FIG 23--Structure of cold-rolled steel box (X250)


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COLE ET AL ON AUTOMOTIVE MATERIALS 131

FIG 24--Pamled surlace o/Mode/T body component (~<750)

Corrosion protechon is an ~mportant characterlsnc of body structures In the era of the


Model T, there was httle problem with rusting of car bodies, smce there was no salt used on
the roads Thus, the pamt system employed was simply several layers of enamel over the
primed steel component, as m Fig 24(a) Modern auto bodies are now exposed to an entire
range of corrosive med~a, which produces generahzed corrosion, as seen in the characteristic
scratch test of Fig 25 In order to reduce this corrosion, the steel and auto industries have
developed an entire range of protective coatings, m addition to paint (It should be noted that
paint systems have undergone considerable change over the past few years as a result of pres-
sures for reduced hydrocarbon emissions ) Zinc-based coatings (electrogalvanlzed and hot
dtpped) are the first protectwe layer This is followed by a phosphate electrocoat and a primer,
then by a base coat, a top coat, and finally by a clear outer coating

Body Structure (Windshield)


The original developments m glass technology have followed pressures for increased pas-
senger safety Whereas the Model T used plam plate glass, modern vehicles began using tem-
pered and laminated glass many decades ago Recent developments have focussed on ad&-
tional customer-desirable features The modern Ford "Instaclear" glass contains sophtsttcated
Z n O / A g / Z n O layers that, while maintaining perfect vlslbthty, can be heated by the apphcat~on
of a low voltage (Fig 26). Such products allow the wmdshleid to be deiced in several seconds

Conclusion
The Model T was an exciting revolution m motor transport But, over the past 75 years,
there has been a continual evolution to the modern automobile In contrast to 1916, when
Ford Motor Company sold 501 000 vehicles, the company now sells seven Umes or 3 5 mflhon

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132 METALLOGRAPHY PAST, PRESENT, AND FUTURE

FIG 25--Corrosion m modern steel panel

vehicles in the U S and Canada and over 5 8 million worldwide The automotive industry
has grown considerably over the past 75 years and now consumes some one-sixth of America's
Gross National Product
It is unfair to attempt to understand the Model T by examining only a small slice of seven
or so components and develop a complete description of how and why the materials, com-
ponents, and processes evolved from the Model T era The goal of the authors was to outline
some of the materials and processing changes that have led to the present vehicles For each
material and component, material structural analysis and characterization and physical/prop-
erty standards have been developed by the industry Without materials structure characteriza-
tion, automotive developments could not have proceeded as rapidly as they have, and It IS for
this reason that the seventy-fifth anniversary o f ASTM Committee E4 requires recognition
Modern materials characterization includes more than just light microscopy Since the
Model T era, new technologies have been invented for mlcrostructural examination, analysis,
and evaluation Electron microscopy (SEM, TEM, AEM) and spectroscoples (Auger, XPS,
SIMS), X-ray, and acoustical techniques, all coupled with computer methodologies, are now
being employed to analyze the performance and behavior of materials and their fabncatlon
As the automotive industry employs more complex materials and processing, and as safety
requirements increase, more sophisticated materials characterization techniques will continue
to be developed With the members of ASTM Committee E4 ensunng continual standardiza-
tion of these methods, the quality of the automotive industry will be able to advance in an
orderly fashion

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COLE ET AL ON AUTOMOTIVE MATERIALS 133

FIG 26--StJu6ture o/modern Ford "lnslaclear"glass wmds'hleld ( 100 000)

Acknowledgments
We would like to thank the staff of Greenfield Village/Henry Ford Museum for access to
their records and files, Mr Bill Barth of Troy, Michigan, a restorer of Model T cars, for all of
the Model T components described in this paper, Ms Darlene Flaherty for access to Ford
Motor Company Archives, and Dr W Wlnterbottom for supplying photographs of the alu-
minum radiator

APPENDIX I Major Components in the Automobile

Powertraln (dependent on design) Chassis


Head Frame
Valvetraln Suspension
Valves (Intake/exhaust) Arms
Retainers Springs
Springs Brackets/crossmembers
Camshaft Steering
Tappets Wheel
Rocker arms Kruckle
Intake mamfold Shaft, locks
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134 METALLOGRAPHYPAST, PRESENT,AND FUTURE

Block Air bag


Power conversion Brakes
Connecting rod Fraction matenals
Piston Rotors
Piston rings Drums
Wrist pin Calipers
Crankshaft Master cyhnder
Miscellaneous Wheels
Covers Rims, spiders
Brackets Tires
Pumps Exhaust System
Belts/chains Exhaust manifold
Hoses Emission control
Drivetraln Muffler, pipes
Transmlsslon Climate Control
Housing Heater, A/C
Torque converter Radiator
Clutch Fluids
Housing Fan
Rear axle Belts/hoses
Gears Fuel System
Drlveshaft Gas tank
Clutches Pumps
Housings Valves
Differential Fuel
Body Interior
Bumpers Seats
Fenders Belts
Trunk (deck lid) Instrument panel, switches
Hood (inner/outer) Electronics
Doors (inner/outer) Miscellaneous
Hinges Lubricants
Fasteners Bushings, insulation
Glass Adhesives
Moldings, grill Sealers and fillers
Rocker panel Corrosion protection
Floor pan
Paint

APPENDIX II Materials and Components in the Ford


Model T circa 1916

Powertraln
Head Gray iron (GI)
Valvetram
Tappets GI head, cold-rolled (CR) steel stem
Valves* Heat-treated steel
Push Rods
Camshaft Drop-forged, heat-treated steel
Gear Malleable iron
Beanngs GI bushing, babbit beanng
NOTE Starred components (*) are those experienced m this paper

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COLE ET AL ON AUTOMOTIVE MATERIALS 135

Intake mamfold GI (aluminum prior to 1915)


Block Steel frame, cast GI combustion, Welsh plug
Power Conversion GI (hardened steel pro/bronze bushing/beveled after 1914)
Piston Drop-forged steel
Connecting rod GI
P~ston nngs Machined seamless steel tubing
Wrist pm Drop-forged V-steela
Crankshaft Babbitt
Beanngs GI
Hywheel Bronze, (GI b in 1919)
Carburetor*
Dnvetraln
Transmission
Housing GI (aluminum prior to 1916)
Brakes Steel on steel (GI housing)
F/R Axle* Drop-forged V-steel, paper gasket, fiber thrust washer
Gears Drop-forged, heat-treated V-steel
Dnveshaft* Drop-forged, heat-treated V-steel
Clutches Steel d~sk in oll
Housings GI
Differential GI
Body Body structure (pressed sheet steel over wooden frame)
Bumpers None
Fenders* CR steel (form, roll, hammer, press)
Trunk, hood CR steel (hood was aluminum prior to 1915)
Hinges/fasteners CR steel
Glass* Untempered glass
Corrosion Protection Paint
Paint* Four coats 450~ baked enamel on primer
Flrewall Wood
Exhaust system
Mamfold GI, with flanged steel p~pes connected by brass nuts
Emission control None
Muffler/pipes GI ends, steel tubes (asbestos wrapped before 1916)
Chassis
Frame Wood
Suspension V-steel
Spnngs Steel (six leaf m front, eight m rear)
Steenng wheel Wood w~th GI spider
Shaft Steel
Gears Planetary
Knuckles/spindles V-steel
Hand brake Steel/asbestos on GI expanding with spnngs on rear wheels
Wheels Wood (ball beanngs m front)
Hub caps Brass
Tires Rubber (rear treaded m 1915)
Lubricants, sealers
Electrical
Commutator* Cast aluminum
Starting motor (1917)
Generator
Ignmon Magneto with 16 magnets
Spark plugs* Porcelain and steel
Battery
Wrong Copper
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136 METALLOGRAPHYPAST, PRESENT, AND FUTURE

Lighting Sealed beam (gas until 1915)


Horn Electrical (after 1915)
Climate Control
Heater None
A/C None
Radiator Brass fins soldered to copper tubes
Fluids Water
Fan blades Steel, GI hub, leather belt driven
Hoses
Fuel System
Gas tank Soldered terne plate, brass sediment bulb
Pumps None" gravity feed, brass tubing
Valves
Fuel Unleaded gasoline
Intenor
Seats Imitation leather and burlap
Belts None
Switches Light switch/ignition switch attached to dash (firewall)
Instrument panel None
Electronics None
Miscellaneous
Lubricants
Bushmgs GI, steel or babblt (69)
Insulation Paper products
Mats Rubber
Descnptlon Engine 14. 176.7 m 3, 22.5 hp, 4 0 compression raUo
Maximum speed 35 mph
aHeat, quench, anneal, forge, tumble, snag, straighten, machine, polish
b41 lbs as-cast, 35 lbs fimshed, in 16 operations

APPENDIX IIIA--Product-Based Technological Change


Most changes m the automobile have been customer-driven They occurred as a result of a
new material, component, or design that enhanced the vehicle's functlonahty or reduced its
cost or both. A list of the important attributes could include

1 enhanced drlveablllty and performance (in terms of power, pickup and feel),
2 enhanced vehicle dynamics (reduced noise, vibration and harshness, improved handling
and braking, and greater comfort),
3 improved duraNhty, quality, and reliability,
4 enhanced appearance (including corrosion);
5 reduced cost and effort for maintenance and repairability,
6 increased fuel economy,
7 safety considerations (improved passenger protection and reduced vehicle dam-
ageabihty),
8 product/component/materials interactions that reduced cost to manufacturer and to
customer and reduced timing of product to market;

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COLE ET AL ON AUTOMOTIVE MATERIALS 137

9 design considerations (interior and exterior styhng),


l0 enhanced instrumentation,
11 product/process interactions to reduce fixed and variable costs, and
12 because a competitor had introduced a similar feature

Each category may have many different subsets that helped "push" the particular improve-
ment to market For example, a product that improves a vehicle's appearance (4) will achieve
market acceptance if it is a paint or protecting layer that reduces surface damage from envi-
ronmental corrosion or impact or both with road dust and stones.
The attributes, enhanced vehicle dnveablhty/performance (1) and fuel economy (6), are
driven by reducing component weight, improving aerodynamics, and increasing powertram/
dnvetraln efficiency In turn, this latter attribute is affected by reducing friction, use of elec-
tromc controls, etc Additional subsets for weight reduction might include Increasing a com-
ponent's mechamcal properties, so that the component can have the same rigidity, fracture
toughness, creep, and be thinner and therefore hghter The additional improvement in prop-
ertles by materials that have higher temperature and humidity resistance can be additional
drivers for change in under-the-hood components
Government can influence product design by leglslatmn. For example, emission reductions,
better material recycleabfllty, use of alternate fuels, enhanced fuel economy, and improved
safety (say by increasing capaoty to absorb energy in a crash) will promote new materials
technology

APPENDIX IIIB Process-Based Technological Change

Advances m manufacturing technology have been major drivers for materials and compo-
nents changes m the automotive industry Several important attributes include

1 enhanced manufactureablllty (the material or component can be designed more readily


for lower-cost manufactunng),
2 the new material/component has higher quality (and quality that is more easily
verifiable),
3 the process is more rehable and reproducible,
4 the components are more machinable;
5 the component can be more easily joined (by adhesives, welding, etc.);
6 the c~176 are m~ c~ f~ van~ types ~ c~
7 the product can be produced to near net shape,
8 the product can be produced in comphcated one-piece components with thin walls/
close dlmens~onal tolerances and nonuniform wall thickness,
9 the design is more suitable for mass production,
10 the process has shorter cycle times,
11 the process can increase the speed of getting the products to market, and
12 the process has reduced variable and fixed manufacturing costs.

Government can influence manufacturing processing by mandating emission reductions


and safety Improvements at the workplace through the Occupational Safety and Health
Administration (OSHA) and the National Institute for Occupational Safety and Health
(NIOSH)

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138 METALLOGRAPHY PAST, PRESENT, AND FUTURE

References
[ 1] Pusch, R , "Hxstory of Metallography," Pracncal Metallography, Vol 16, 1979, p 294
[2] Owens, J S, Hmton, J W , Insley, R H, and Polan, M E, "Development of Ceramic Insulators for
Spark Plugs," Ceramtc Bulletm, Vol 56, No 4, 1977, p 437
[3] Wlnterbottom, W , Ford Motor Company, private commumcatlon

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Robert L. Benne?

New Diamond Grinding Disks for Specimen


Surface Preparation
REFERENCE" Benner, R L , "New Diamond Grinding Disks for Specimen Surface Prepara-
tion," Metallography Past, Present, and Future (75th Anniversary Volume), ASTM STP 1165,
G F Vander Voort, F J Warmuth, S M Purdy, and A Szirmae, Eds, Amencan Society for
Testing and Materials, Philadelphia, 1993, pp 139-154

ABSTRACT: A new multflayer abrasive gnndmg disk has been developed to overcome the
grinding and pohshmg problems associated with metallographlc speomen preparation These
problems are discussed in detail The dlscussmn focuses on the contnbutlng factors of poor spec-
imen preparation, how they affect the surface, and how they are allewated The difficulties of
surface deformation, edge rounding, soft-phase undercutting, pullout, and chipping of brittle
specimens are reviewed together w~th their root causes Th~s foundatmn was used to design a
supenor gnndlng system employing the benefits of dmmond
Micrographs of speomens prepared using conventmnal techniques are compared to that of
the new grinding system The mlcrographs illustrate that edge rounding and soft-phase under-
cutting can be Chmlnated with chipping and pullout greatly reduced Other examples show that
the new grinding system greatly improves the specimen surface fimsh and that three gnndmg
&sks of the new design can replace five or six conventmnal gnndmg and pohshmg steps

KEY WORDS: specimen gnndmg, specimen polishing, specimen undercutting, edge rounding,
surface deformation, chipping, diamond abrasives, cubic boron nitnde, metaUography, metal-
lurglcal specimens, mlcrostructure, metallographlc techniques

Surface damage of metallographlc specimens and its affect on interpretation has always
plagued metallographers T h e three m a r e contributors are

(a) dull or deteriorated abrasive particles,


(b) heat from gnndlng, which can be significant (calculations indicate temperatures of
2200~ are possible on a mlcroscale [1], and,
(c) swarf or debris that c o m e s off the specimen and the abrasive, eroding the softer phases
o f the specimen and the m o u n t i n g material This swarf ts also a prime cause of edge
rounding

With this as a background let us review s o m e typical procedures

Specimen Preparation Techniques


Conventional Preparatton
I f a typical steel specimen ~s considered, the procedure generally starts out w~th a small seg-
m e n t being cut out w~th an abraswe cut-offwheel This segment ts then m o u n t e d m a plastic
material If edge e x a m i n a t i o n is required, additmnal precauuons m a y be required such as plat-

President, TBW Industries, Inc, Furlong, PA 18925

139

Copyright
Copyright*by1993
ASTM
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140 METALLOGRAPHYPAST, PRESENT,AND FUTURE

mg the surface of the piece before mounting so that the surface edge of the specimen is encap-
sulated m another metal
Once the specimen is mounted, gnnding can begin If the abrasive cut-off saw was used for
sectioning, gnndlng generally starts with a 180 (70 ~zm) grit aluminum oxide (A1203) or silicon
carbide (SIC) paper then proceeds through the 240 (54 #m), 320 (35 #m), 400 (23 #m), and
600 (17 um) grits If the s p e o m e n was cut with a hacksaw or sheared, gnnding generally starts
with an 80 (190 ~m) or 120 (115 um) grit paper and then moves on to the gnnding steps
described earlier What these finishes look like microscopically is shown in Fig 1 It shows a
progressively finer scratch pattern through the five gnndlng steps prior to polishing Evidence
of particle deterioration can be noted on the figure by the random staggered scratch patterns
in the specimen, especially for the coarser grit sizes. Th~s random scratch pattern ~s more prev-
alent when the paper is new, It subsides as the paper becomes dull. On the other hand, dull
paper causes more heat and surface deformation than new paper
In th~s example, an epoxy mount material was used and no special precautions were taken
to preserve the edge Figure 2 illustrates how the edge was affected by the gnndlng process
Figure 2a shows a scanning electron microscope (SEM) mlcrograph of the edge of the speci-
men and the adjacent mounting material Considerable undercutting of the mounting mate-
rlal and extensive edge rounding of the steel can be observed This undercutting and edge
rounding IS promoted by the turbulence of swarf and loose particles collecting at the leading
edge of the specimen As the particles travel over the surface they leave deep gouges and
grooves m the rounded edge and top surface of the s p e o m e n These grooves extend for a con-
siderable distance Figure 2b shows a mlcrograph of this rounded edge area The staggered
random pattern of the loose abrasive particles can be observed.
S~mflar scratch patterns are observed with other materials, such as the bronze spray coating
on a steel plate shown in Fig 3 In general, the softer the material, the deeper the scratch pat-
tern for a given grit size
The coarser grit sizes have reduced considerable tearing and damage in the fragile bronze
coating. This gives the appearance of a larger pore size than really exists Not all of this damage
is removed m subsequent fine grinding steps as shown in the photomicrographs of Fig 3

New System
Fundamentals--In order to understand some of the problems with conventional abrasives,
~t would be well to understand some of the fundamentals of gnndlng As previously men-
tloned, there are three major contributors to poor specimen preparation, namely, particle
deterioration, heat flow, and swarf. The first two can be alleviated by using a particle that has
good thermal conductivity and does not dull easily. In this instance, diamond and cubic boron
nltrlde (CBN) are natural selections. Figure 4 shows that the hardness of diamond and CBN
are superior to those of other abrasives. They also have a much higher thermal conductivity
than other abrasives, even metals, so that the heat flows into the abrasive particle rather than
the specimen, see F~g 5
Fixed abraswes, diamond and CBN gnndlng disks, have another property that is not shared
by other fixed abrasives This property yields an added bonus in specimen preparation Recent
studtes have shown [2,3] that the more diamond or CBN particles m contact with the speomen
the better the surface fimsh This phenomenon was noted in grinding metals and nonmetals
over a wide range of grit sizes, from 300 ~m down to 45 #m, and using a wide range of bond
types including resin, metal, and wtreous bonds F~gure 6 shows that increasing the volume
percent of d m m o n d particles m an impregnated resin bond, improves the surface finish of
material. Part of this improvement is because the greater the number particles m contact w~th
the surface, the less pressure exerted by any one particle Naturally, as the volume of diamond

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BENNER ON DIAMOND GRINDING DISKS 141

i
rT

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142 METALLOGRAPHY PAST, PRESENT, AND FUTURE

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BENNER ON DIAMOND GRINDING DISKS 143

L~

4~

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144 METALLOGRAPHY:PAST, PRESENT, AND FUTURE

FIG. 4--Knoop hardness ~f diamond and CBN compared to that of other abrasives.

FIG. 5 - - l'hermal conductivity ~f varimts materials and the effect on heat[low in diamond as compared
to aluminum
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BENNER ON DIAMOND GRINDINGDISKS 145

cO
ill
2533
0.9 , l .......................................................................
0
r
o
0.8 . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . m.~ .....................................................................
-,,~.
"r
"4,666
z l.,
tL. 0.7 ................................................................ .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .
I.LJ ",,,.
L)
U.
ff '5269 6383
0.6 ..........................................................................................
"= . . . . . . . . . . . m ..............................

Z
ttl
0.5 ............................................................................................................................ ~ - ......................
ttl \
13.

! ! ! T I i~

0.4 5.0% 10.0% 12.5% 15.0% 20.0% 25.0%


VOLUME PERCENT DIAMOND IN DISK
FIG. 6--Surlktce.[inish versus volume percent diamond in a resin bond and calculated number of par-
ticles per unit area protruding from the bond Surface.

FIG. 7--Development of particle protrusion during grinding.

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146 METALLOGRAPHYPAST, PRESENT, AND FUTURE

increases m the bond, the number of dmmond parhcles m contact with the surface increases
As the particles get closer together, there is less chance for bond erosion m between the particles
and they do not protrude from the bond as much This is dlustrated schematically m Fzg 7
Consider a row of diamond particles m a metal or resin bond as shown m Fig 7a As the bond
~s worn away by the swarf coming off the specimen, a long support or "tall" develops in the
back, or trading edge, of the abrasive particle At the same time, the front and sides of the
particle protrude from the bond more as shown in Fig 7b This protrusion (E), the number
of particles, and the pressure apphed to the specimen, control the depth of the cut or scratch
pattern in the specimen The diamond particles that are far apart develop extensive protrusion
on the front and sides as shown m Fig 8 Here the sides and front are well protruded and with
httle effort the particle can pull out of the bond leaving a hole s~mdar to that shown in Fig 9
This pullout shortens the life of the grinding disk
If the number of particles is increased, as shown in F~g 7c, the undercutting and protrusion
(e) ~s decreased With the decreased protrusion and greater number of particles, the particles
do not cut as deep and the surface finish is better.
It would be very expensive to increase the volume of dmmond m a gnndmg &sk that has
slgmficant depth of diamond If however, the particles are consohdated into a three-&men-
s~onal honeycomb network, such as dlustrated in F~g 10, the effectiveness of the particles can
be maximized This type of structure offers a continuing supply of diamond for grinding As

FIG 8 - - S E M photo,graph o / d i a m o n d protru ston m metal bond

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BENNER ON DIAMOND GRINDING DISKS 147

F I G 9 - - S E M pholoy(raph o{ empt~ socket/e/t by dlamond pullout /rom a metal bond

FIG 1O--Method o[ ~on~ entratmg dtamond

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148 METALLOGRAPHYPAST, PRESENT, AND FUTURE

one layer is worn away other layers come to the surface to continue the grinding Unhke abra-
sive papers, the third dimension of diamond depth increases the hfe of the product slgmficantly
so that ~t can replace thousands of paper disks
This type of consohdatlon has other advantages The empty spaces within the honeycomb
offer a place for the s p e o m e n swarfto collect This addresses the last major source of specimen
preparation problems The holes also carry coolant across the entire surface of the s p e o m e n
at all times The absence of mterfenng swarfallows the hard d~amond parhcles to do all of the
gnndmg, thus reducing the undercutting of soft phases It also offers full-time cooling to the
speomen, reducing still further the potentml for thermal damage

Results
If the same steel specimen is prepared using the new technique, the sectioning procedure is
the same as for the abrasive paper technique At this point, the new system is simpler No
speoal edge preservatxon techniques are required because undercutting does not occur The
grinding begins with a 200-grit (68-urn) gnndlng disk of the new configuration This is then
followed by a 30-um disk and a 12-em disk, both of the new configuration This is illustrated
in the photomicrographs as shown in Fig 11 When Fig 11 is compared with Fig 1 at equiv-
alent abrasive particle size, a dramatic difference is noted It will be shown later that the final
step in the new system is equivalent to a polish step
Figure 12 shows a scanning electron microscope mlcrograph of the edge of the specimen
and the adjacent epoxy mounting material, using the new system and an equivalent grit size
to the SiC grit used m Fig 2a A dramatic difference is noted between the two fgures. With
the new method, virtually no undercutting is observed The scratch pattern is much finer and
the gouging has been virtually ehmlnated Figure 12b shows that the edge is fiat with virtually
no edge rounding
Figure 13 shows a comparison of scratch patterns produced by 17-um SIC papers, a 12-um
diamond disk o f the new system and a 3-~m diamond paste on a medium nap c o t t o n cloth
In this case, the steel specimens show marked differences in the depth and width of the
scratches produced by the different abrasives
Figure 13 illustrates that the surface fimsh from a 12-~m dmmond gnndmg disk of the new
system gives a finer scratch pattern than other S~C fixed abrasive disks of comparable particle
size as well as 3-urn pohshmg pastes on cotton cloth. The printed orcult (PC) board, shown in
Fig. 13, illustrates that the new diamond grinding disk yields excellent definmon of the glass
fibers encapsulated by the copper plate The 3-~m d m m o n d pohshmg cloth, on the other hand,
seemed to undercut the soft phases of the solder A comparison of the bronze spray-coated
specimens, pohshed with 3-#m diamond paste on cloth, shows areas where bronze particles
were removed in prior grinding steps, whereas, the new 12-um diamond disk shows almost
none of this
Figure 13 illustrates that the new system is apphcable to a wide range of materials from
bronze coatings to steel or PC boards In this instance, the specimens were not rotated so that
the scratch pattern would be unidirectional In each case, the observed pattern from the new
system is better than a 3-urn diamond pohsh paste on cotton cloth
When the results of Fig 1, 11, and 13 are compared, it is obvious that the three disks of the
new system can replace easily five S1C grinding disks and the rough pohshmg step of the stan-
dard procedure, as shown in Fig. 14 Speomens were flatter, with no edge rounding, as shown
in Fig 12 Comparing Figs 3 and t3 also shows that they do not cause pore distortion in
porous materials such as the spray-coated bronze

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BENNER ON DIAMOND GRINDING DISKS 149

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150 METALLOGRAPHYPAST, PRESENT, AND FUTURE

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BENNER ON DIAMOND GRINDING DISKS 1 51

FIG. 13--Comparison o f scratch patterns made with 17-#m SiC papers, 3-#m diamond paste on cotton
cloth, and 12-um new diamond disk on printed circuit board, low-carbon steel, and bronze spray coating
(um;tched).

Special Problems of Ceramics and Mixed-Phase Specimens


Preparation of ceramic specimens presents a special set of problems. Because of their brittle
nature, chipping and spalling is often encountered. The reasons for this are many and varied.
Most chipping is a result of compressive stresses induced on the surface of the specimen by the
abrasive particles. In many cases, the particles act like a moving indenter that causes a stressed
area on the surface creating cracks parallel to the stress direction. As the particle moves by,

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152 METALLOGRAPHY:PAST, PRESENT, AND FUTURE

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BENNER ON DIAMOND GRINDING DISKS 153

cracks perpendicular to the stress develop giving rise to a series of concoldal chips forming
behind the particle These chips leave a trench much wider than the abrasive particle From a
materials removal standpoint, this is good because the rate of removal is high From a surface
fimsh standpoint, however, it is detrimental because the surface becomes irregular and
chipped
If the n u m b e r of particles in contact with the specimen surface is increased, then the stress
induced by each particle Is reduced and chipping is reduced A good example of this is shown
in Fig 15 that compares a glass-to-metal seal, ground with a standard SIC paper disk and with
a honeycomb resin bond diamond disk with a comparable particle size Figure 15 shows the

FIG 15--SEMphotograph~ comparing a glass to rnetal seal ground wuh (a) StC papers and(b) a new
dtamond grmdmg dl~k o/ ~omparable grtt stze

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154 METALLOGRAPHY PAST, PRESENT, AND FUTURE

specimen after grinding to a 17-um SIC The figure shows a relatively deep scratch pattern in
the metal and some ch~ppmg m the glass section The glass/metal interface presents a special
problem because of the large difference in thermal coefficients of expansion Figure 15a shows
that a considerable a m o u n t of chipping has occurred at the interface This is probably brought
about by the heat generated d u n n g the gnndmg process The heat causes the surface of the
metal to expand quicker than the glass The sudden expansion of the metal m relation to the
glass causes considerable strain m the glass, which in turn, fractures the glass at the interface
Figure 15b shows the same specimen after grinding with the new resin-bonded diamond disks
A much finer scratch pattern is apparent on the metal and less chipping is present in the glass
More importantly, there is no chipping at the interface With the new method, there is less
heat generated, less d~fference in thermal expansion, and less mterfaclal chipping

Summary
By consolidating closely packed diamond particles into a three-dimensional honeycomb
structure, one obtains an abraswe d~sk that yields a superior finish to conventional abrasives
This reduces speomen preparation time considerably Its unique design allows one to g n n d
and polish speomens flatter with reduced mechamcal and thermal damage and edge rounding
In many cases, it will produce a surface eqmvalent to a 3-#m diamond paste and cloth polish
that is ready for a final pohshmg ff required by the application
A patent [4] has been recently granted on the concept, and the disks have been used suc-
cessfully in s p e o m e n preparation of a variety of materials Including metal coatings, barium
titanate capacitors, turbine engine parts, and carbides

References
[1] Snoeys, R, Leuven, K U, Maris, M, Wo, N F, and Peters, J, "Thermally Induced Damage m
Grinding," Grmdmg Theory, Techntques, and Trouble~hootmg, R P Llndsay and C P Bhateja, Eds,
Society of Manufacturing Engineers, Dearborn, MI, 1982, pp 206-216
[2] Wapler, H and Juchem, H O, "Diamond Abrasives for Machining Glass," Industrial Dtamond
Revtew, Vol 47, No 521, April 1987, pp 159-162
[3] Cooley, B A and Wapler, H, "Surface Finish when Gnndlng with CBN Abrasives," Industrial Dta-
mondRevtew, Vol 44, No 502, March 1984, pp 147-150
[4] U S Patent No 4,882,878 Gnndmg Wheel, 28 Nov 1989

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N a t a h o T. S a e n z ~

Advancements in Ultrathin Section


Techniques for the Characterization of Brittle
Materials
REFERENCE. Saenz, N T, "Advancements in Ultrathin Section Techniques for the Charac-
terization of Brittle Materials," Metallography Past, Present, and Future (75th Anmversary Vol-
ume),ASTMSTPlI65, G F VanderVoort, F J Warmuth, S M Purdy, andA Szlrmae, Eds,
American Society for Testing and Materials, Phdadelphla, 1993, pp 155-166

ABSTRACT The use of ultrathm sections, on the order of'/. to V.,the thickness ofconventmnal
30-um thin secUons, consmutes a slgmficant advancement m the charactenzanon of brittle
matermls At a t~mewhen greater emphas~s~sbeing placed on optimum resoluUonand mterfacml
characterization of brittle materials, this approach makes possible a whole new order of optical
access to m~crostructural detad W~ththe evolution of~mproved mounting medm and pohshlng
eqmpment, ultrathln sectmmng techmques have also improved to produce sectmns that reduce
preparation time and operator dependence Preparatmn methods and examples of matenals
exammatmn using th~stechmque will be discussed

KEY WORDS ultrathln sections, metallographlc techmques, ceramics, ceramic composites,


rock and minerals, transmitted light microscopy, metallurgical specimens, m~crostructure,
metallography

The geologist and the metallographer have long used dlffenng sample preparation methods
because of the differences between the materials they study The brittle, elastic nature of most
minerals has allowed the geologist to prepare secnons under conditions that would be unthink-
ably abusive to the metallographer However, as one goes substantially below the traditional
30-urn thin section or seeks artifact-free, highly polished surfaces for reflected light examlna-
non, the most careful methods of the metallographer are definitely required, and traditional
petrography techniques are no longer adequate
Since the entire technology of petrography has centered around the 30-urn thin section for
well over 100 years, basic thin secnon sample preparation techmques have changed little dur-
ing that time Basically, 30-um-thlck petrographic thin sections have been prepared by free
abrasive grinding on thick glass plates using mechanical or manual laps while the matenal is
secured to glass slides with transparent balsam Upon completion of the thin section, a cover
slip is placed on the upper surface of the section to reduce the scattenng of light during exam-
marion ofthe thin secUon [1] Mineral constituents are identifiable partly because ofthelr crys-
talhne morphology and by their behavior under transmitted polarized hght The characteristic
interference colors ofa gwen matenal in a standard 30-um thin secUon is an tmportant feature
m convennonal petrography These colors, and the way in which they shift with the insertion
of polarizing filters, constitute mineral identification for vanous materials The science of min-
eral identification with the use of conventional thin sections, including all training and all text
book resource materials, are budt on the 30-urn thin sectmn techmques

Senior techmcal speclahst, Pacific Northwest Laboratory, Rlchland, WA 99352

155

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156 METALLOGRAPHYPAST, PRESENT, AND FUTURE

Optical petrography, as traditionally practiced, has suffered from two basic deficiencies the
unpolished surfaces are not suitable for study by reflective light techniques, which limit optical
methods, and the relatively great specimen thickness of 30 ~m leads to opacity and poor res-
olution Earlier efforts were made to produce thicknesses below the standard norm, but those
efforts have generally proven unsuccessful because of poor adhesive performance, inadequate
surface preparation techniques, excessive stresses causing material pullout during the prepa-
ration steps, or a combination of all these factors Since the mid 1940s, refinements have
occurred in the preparation of thin sections G C Kennedy [2] produced and reported pol-
ished sections of conventional thickness roughly 100 years after the beginning of petrography
Refinements in microscopy and improvements in abrasives and preparation equipment have
also occurred Improvements in adhesive materials, premlxed and graded diamond abrasives,
lapping materials, and the evolution of the universal microscope have all combined to produce
an Increasing interest in polished thin sections
The use of the pohshed sections, mixed-mode illumination, and other minor refinements
to the 30-um standard thin section are of increasing interest The next natural step in the evo-
lution of the thin section was to produce sections below the standard 30-t~m limit Within the
past 20 years, R H Beauchamp [3] pioneered ultrathln section techniques for application to
brittle materials, such as lunar basalts and brecclas The sections, on the order of ~,, to V~the
thickness of standard 30-t~m thin sections, make possible essentially new levels of sophistica-
tion in the examination of brittle materials The intent of this paper IS to describe ultrathln
section techmques and to illustrate the wealth of information obtained through microscopic
analysis of brittle materials using this technique

First-Side Preparation Techniques


Sample material is sectioned and mounted with resin The first side is prepared by planar
grinding and vibratory polishing

Secttomng and Cast-Mounting


Sectioning is the first critical step in prepanng brittle materials for ultrathln section tech-
niques Its main function is to reduce the parent material to a smaller workable piece with
m i n i m u m deformation When prepanng ultrathln sections of brittle and fragile materials, it
is important that the pores in the material be impregnated with a low-viscosity thermosetting
resin before the material is sectioned This encapsulation step ensures that no sample degra-
dation, such as fracturing or plucking, occurs during the wafer sectioning process, it also
enhances the ability to produce thinner wafers The smaller section of material is then
mounted in the same type of epoxy resin and vacuum impregnated After the resin 1s hard-
ened, thin wafers of less than 0 6 cm thickness are sectioned from the resin-mounted material
Whenever possible, sectioning of the material should be done using a slow speed (300 to 500
rpm) cut-offsaw with a diamond wafering blade, using oll as the lubricant The sides of the cut
wafer are ground down with the use of a belt surfacer, placing the square wafer into a specimen
casting mold, as shown in Fig l The smaller section or wafer of material is then remounted
in epoxy resin and vacuum impregnated, partially filling the casting mold with the resin While
the specimens are being vacuum Impregnated, an alumina powder is added to the remaining
epoxy resin and stirred until a homogeneous mixture is achieved.
When the epoxy resin in the specimen casting mold has a minimal amount of outgasslng,
the alumina-loaded resin is used to finish filling the specimen casting mold The reason alu-
mina filler is added to the casting mold is that it serves as a guide for any specimen wedging
(nonparallel planes) and a thickness indicator d u n n g the thinning process An example of a
metallographlc m o u n t is shown m Fig 2
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SAENZ ON ULTRATHIN SECTION TECHNIQUES FOR BRITTLE MATERIALS 157

FIG. 1--Sectioned specimen wqfi,r in casting mount.

Planar Grinding
The mounted metallographic samples are rough ground on an oil-cooled 125-urn diamond
planar grinding disk until the surface of the material covered by resin is exposed. It is impor-
tant not to grind too deep into the specimen; the grinding should stay within the depth of the
resin impregnation zone of the material being polished. The thickness of the resin impregna-
tion zone is dependent on the amount of porosity present in the material being polished. Vac-
uum impregnation causes the resin to flow within the interconnecting pores of the material,

FIG. 2--Metallographic sample mounts with alumina filler.


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158 METALLOGRAPHY PAST, PRESENT, AND FUTURE

helping to reduce any pullout or plucking of the matenal during this aggressive gnndlng step
The decision to use either water or oil as the coolant depends on the water reactivity of the
mlcrostructural constituents of the specimen being polished The mounted samples are then
hand-lapped using an oil-based coolant on a 30-#m diamond planar grmdlng disk with wheel
speed of approximately 300 rpm, malntmnlng medium-to-heavy uniform pressure until all
gnnding scratches from the previous step have been removed. After each grinding step, the
mounted samples should be thoroughly cleaned to prevent contamination from the previous
step The mounted samples are then placed in a pohshlng weight assembly, shown in Fig 3

Vibratory Pohshmg
The mounted samples are polished with vibratory polishing equipment using a combination
of polishing slurries and polishing cloths that maintain surface flatness and artifact-free sam-
ples The use of diamond polishing abrasives IS indispensable for the preparation of ultrathln
sections The polishing rates using diamond abrasives are equal to, or better than, other pol-
ishing abrasives The type ofpohshlng cloth used has an extremely important beanng on the
finished s p e o m e n Napless polishing cloths should be used when rehefbetween the microcon-
stltuents of varying hardness and sample mount interfaces are to be held to a minimum Some
examples of napless pohshmg cloths are nylon, pellon, stainless steel mesh, and silk
Vibratory polishing is an effective polishing technique for thinning brittle, fragile materials
Resin-mounted samples are placed in weight assemblies, face down on the pohshing cloth
Inertia from the sample weight produces movement, which induces polishing Since the
removal rate of material is low, several hours ofpohshlng may be reqmred With the selection
of all these elements, the combination ofpohshmg cloth, abrasive slurry, and vibratory motion
gently pohshes the sample surface, slowly removing material, creating very little thermal or
mechanical shear loading of the material being studied
The first vibratory pohshmg step involves the use of 1-#m diamond abrasives using an oil-
based carrier slurry on a stainless steel mesh polishing cloth This combination of polishing
m e d m m and cloth produces samples with excellent interfaclal flatness between the mlcrocon-
stltuents as well as excellent edge retention The amount o f time involved m this rough pol-
ishing or flattening step depends on the hardness vanatlons within the specimen being pol-

FIG 3--Ftr~t-~tdepohshmg wetghtassemblyfor vtbratorypohshlng

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SAENZ ON ULTRATHIN SECTION TECHNIQUES FOR BRITTLE MATERIALS 159

lshed, 4 h is typical The fine pohshmg step consists of using 1-um diamond abrasives in an
off-based slurry on a synthetic napless pohshmg cloth Again, the time depends on the removal
rate of the material being studied, approximately 12 h of polishing time is required to remove
any artifacts
After the examination of the mounted specimen for any type of surface defects, the mounted
specimen can be prepared for transfer to a petrographic slide for preparation of the second side

Second-Side Preparation Techniques


The second side of the specimen is prepared by mounting a 2 to 3-mm-thick wafer on a glass
shde and mechanically thinning the exposed side

M o u n t i n g on Glass Shde
Upon completion of the first side of the specimen and m~croscopic examination of the sam-
ple, the polished m o u n t is placed in an abrasive cutter and a thin wafer IS sectioned from the
mount, parallel to the polished surface The thickness of the cut wafer is very important and
should be on the order of 2 to 3 m m in thickness to ensure satisfactory gluing to the petro-
graphic well slide The polished thin disk m o u n t is then belt-surfaced into a rectangular-shaped
wafer with an alumina ring around the outer edge of the wafer so that the resultant polished
wafer will fit within the well area on the petrographic well slide
The rectangular-shaped wafer is then placed, polished side up, into a casting mold The pol-
ished wafer is recast using the same type of epoxy resin as used in earlier steps, again partially
filhng the casting m o u n t After the resin-filled wafer is heated and vacuum impregnated, the
resin-filled wafer is removed from the casting mold and is placed with the polished side of the
wafer down on the glass slide, contacting the glass well surface of the petrographic well slide
The wafer ~sworked around to remove any mr bubbles trapped between the wafer and the glass
shde because air trapped m the section, or m the wafer/glass interface would cause a debond
area at the glue line, which could cause plucking or pullout of material in later steps of the
process The mounted slide is oven-cured to allow the resin to set The glass mounting pro-
cedure is shown in Fig 4

FIG 4--Step~ [or se~ond-stde thmnmg pohshed wafer, waJer mounted on gla.s s shde, and )~mshed ultra-
lhgn ~er
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160 METALLOGRAPHY PAST, PRESENT, AND FUTURE

Planar Grmdmg
Thin-section fixturing is not used by the author dunng the grinding process, the initial grind-
lng operation is done with the glass shde held d~rectly in the preparator's finger tips This tech-
tuque requires a good deal of dexterity to prevent grinding of the preparator's finger Ups along
with the section If more substantmi fixturing is desired, various metallographlc vendors pro-
vide different types of thin-section fixtures. Standard clamp-type slide holders should be
avoided because they impose undue stresses on the mounted glass shde
The first step m the grinding process is the use of a 125-urn diamond planar gnnding disk
using an od coolant, gnndmg until light can be seen through the alumina filler around the
sectnon Examination of the alumina filler can signal any wedging of the section The alumina
filler should have the same color thickness around the section (no hght or dark areas), so great
care must be taken d u n n g th~s aggresswe grinding step The thin section may be taken to a
thickness of 50 um on th~s first grinding step An additional 10 to 20 ~m can be removed with
the use of a thin-section grinder This step 1s optional, depending on the avadabihty of this
specmhzed piece o f e q m p m e n t Lapping continues by hand through 30-#m diamond wheels,
again with the use of an od coolant, until all scratches from the previous grinding step are
removed The alumina filler around the specimen is highly translucent at this point, again
looking at the color thickness of the alumina filler as an indicator for any wedging of the sam-
ple. After the grinding process is complete, and the thin section has been cleaned thoroughly,
the shde is placed into a pohshmg weight assembly for the vibratory pohshmg step, shown m
Fig 5

Vtbratory Pohshlng
The mechanical thinning process is continued with the use of vibratory polishing equip-
ment, again using an oil-dispersed diamond slurry of 1-urn particle size on a synthetic napless
polishing cloth The pohshmg time vanes, depending on the hardness of the material. During
this process, the ultrathin section must be respected periodically to ensure that the section

FIG 5--Second-~tdepohshlng wetghtassembly wtthmountedglassshdes

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SAENZ ON ULTRATHIN SECTION TECHNIQUES FOR BRITTLE MATERIALS 1 61

is pohshlng evenly and has not been pohshed through The difference between an ultrathm
section (under lO um) and no sectmn is slight. The use of the Michel-Levy Interference
Color Chart is a valuable aid when examining polished ultrathln sections with the micro-
scope because it graphically relates thickness, blrefrlngence, and retardatmn of trans-
parent materials

Results
Characterization of brittle materials using ultrathm section techniques presents a new level
of clarity and resolution to the optical microscopist Since a section is pohshed on both sides
or surfaces of the material, it can be examined using a full range of reflected and transmitted
light methods
Figures 6 through 9 show examples of ultrathm section techniques using a wide variety of
materials.
Figure 6 is a direct comparison of a standard thin sectmn (Fig 6a) with an ultrathm section
(Fig 6b) of tin oxide electrode material. The photomicrograph shown m Fig 6a illustrates the
unsuitability of the standard 30-#m thin section for resolving needed mlcrostructural refor-
mation Figure 6b illustrates the resolution of individual grains, their boundary relationships,
and twinning habits of this material.
Figure 7 illustrates very clearly the fine detail and complex microstructure ofchondrules m
stony meteorites. The photomicrographs are from the Dhajala meteorite showing loosely
bound chondrules with well-preserved, cleary-uneqmhbrated mlcrostructures
Figure 8 shows the complex range of minerals, textures, and the scale of m~crostructural
details In terrestrial mineralogical studies The photomicrographs of the minerals aphte and
graphic schist demonstrate clear dehneatlon of individual grains and their characteristics mak-
ing mineral ~dentlficaUon an easier task
Figure 9 shows the mlcrostructural detail of silicon-carbon/silicon-carbon (SIC/SIC) fiber
composites prepared by the chemical vapor induction (CVI) process Growth of the SIC matnx
from the black SIC fibers dunng infiltration reveals impingement interfaces of this material
that can be seen only by transmission light microscopy

Conclusions
The advantages of ultrathin sections are that much greater resolution is avadable to the
microscopist, and that regions of the material that may be opaque m thicker 30-#m sections
can be illuminated and examined The gain m clarity is illustrated m Fig. 6 It is apparent that
the standard thin section of tin oxide electrode material provides very little information while
the ultrathln section reveals grain relationships, twinning, and a small amount of porosity The
improvement m clanty results from thinning the section of matenal to a monolayer of grains
This eliminates the overlapping diffraction patterns of stacked, small grams, which obscure
structure m the standard 30-#m thin section Because the ultrathln secUon ehmmates the scat-
terlng ofhght that occurs in a standard thin section, it is well suited for the application of newer
microscopic techniques, such as Nomarskl differential interference contrast (DIC) Such
methods are most powerful m providing apparent rehefbecause small refractive index differ-
ences build contrast m some difficult objects.
The ultrathln section technique described here is one of many analytical tools for the char-
actenzation of brittle matenals The technique given m this paper should help overcome major
obstacles m the preparation of bnttle matenals for m~croscopIc examination.

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162 METALLOGRAPHY PAST, PRESENT, AND FUTURE

~3

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SAENZ ON ULTRATHIN SECTION TECHNIQUES FOR BRITTLE MATERIALS 163

I
L~

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164 METALLOGRAPHY PAST, PRESENT, AND FUTURE

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SAENZ ON ULTRATHIN SECTION TECHNIQUES FOR BRITTLE MATERIALS 165

t~

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166 METALLOGRAPHY PAST, PRESENT, AND FUTURE

Acknowledgment
The Pacific Northwest Laboratory ~soperated for the U S Department of Energy by Battelle
Memorial Institute under Contract DE-AC06-76RLO 1830

References
[1] Kerr, P F, OpttcalMmeralogy, McGraw-HallCo, New York, 1977
[2] Kennedy, G C, "The Preparation of Pohshed Thin Sections," Economw Geology and the Bulk,tin of
the Socwty ofEconontc Geologtsts, Vol 41, 1946, pp 353-360
[3] Beauchamp, R H and Wdhford, J F, "Metallograph~cMethods Apphed to Ultrathmnmgof Lunar
Rock, Meteorites, Fossds and Other Brittle Materials for Ophcal Microscopy," Metagographlc Spec-
Imen Preparation, Plenum Press, New York, 1974

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M i c h a e l R. Notis, ~A r n o l d R. Marder, ~ a n d Ye T Chou ~

The Early Metallographic Studies of Chih-


Hung Chou on the Formation and Morphology
of Widmanstatten Structure and Martensite
REFERENCE" Notls, M R, Marder, A R., and Chou, Y T , "The Early Metallographic Stud-
les of Chih-Hung Chou on the Formation and Morphology of Widmanstatten Structure and Mar-
tensite," Metallography Past, Present, and Future (75th Anntversary Volume), ASTM STP
1165, G F Vander Voort, F J Warmuth, S M Purdy, and A Szwmae, Eds, American Society
for Testing and Materials, Phdadelphm, 1993, pp 167-173

ABSTRACT: One of the early studies concerning the detaded mtcrostructural aspects of phase
transformatmns m ~ron-carbon alloys was performed by Ch~h-Hung Chou (Ph D, Harvard,
1928), a student of Professor Albert Sauveur The research describes the formatmn of W~dman-
statten structure and martenslte m ~ron-carbon alloys possessing a broad range of carbon con-
tents and heat treated using a broad range ofcoohng rates A umque mercury quench method ~s
descnbed This research work was never fully pubhshed
The present paper shows original photomicrographs and portmns of the written text from the
dlssertatmn, and seeks to clanfy and reinterpret these m terms of our present understanding of
ferrous phase transformatmns Also included zs the background h~story of the introduction of
modern industry and science In China, and Chou's personal reminiscences of Professor Sauveur

KEY WORDS: metallography, history, won-carbon alloys, martenslte, Wldmanstatten struc-


tures, surface rehef, metallurgical specimens, mlcrostructure, metallograph~ctechmques

In 1872, the first yearly group of 30 students was sent from China to study science m the
Umted States With the establishment of the Chinese Repubhc in 1911, the Chinese reahzed
the importance of modern science and technology m nation building In 1914, the Chinese
Society of Science (Zhong Guo Ke Xue Sh0 was founded, with its inaugural meeting held in
1915 at Cornell University, members came predominantly from Andover, Carnegie Institute
of Technology (now Carnegie-Mellon Umverslty), Columbia, Cornell, Harvard, Lehigh,
Princeton, Wflhston, and Yale Among these students was a semor m Chemical Engmeenng
from Lehigh, Chin Wong, who was soon to return to China to set up the first laboratory for
modern quantitative analytmal chemistry m China, at the Nanking H~gher Normal School,
now Nanking Umverstty Among his research interests was the analys~s of ~mpunt~es m cast
bronze alloys used for coinage In the early 1920s, he was a founder and &rectlng e&tor of the
journal, K e X u e (Sctence), and in 1928 he became the first &rector of the Natmnal Institute of
Chemistry (Academ~ca Smlca) Chin Wong, known as the father of modern chemistry m
China, was therefore an lnfluentml figure m the Intellectual circles that promoted the idea of
saving China through the development of modern industry and science
Among the young men that Chin Wong in turn influenced to study in the Umted States was
Chlh-Hung Chou, who graduated m 1923 from the Metallurgy Department of Belyang Unl-
vers,ty m Tianjen Chou strongly beheved that ff people m China could master the field of

' Department of Martenals Science and Engmeenng, Lehigh Umvers~ty,Bethlehem, PA 18015-3195

167

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168 METALLOGRAPHYPAST, PRESENT, AND FUTURE

metallurgical science, then China would give rise to a modern steel industry that would greatly
aid its industrial development As it turned out, Chou was the only member of his graduating
class of 16 (five in metallurgy, eleven in mining), who continued in his field He was helped by
Professor Edwin Sperry, an Amencan, who was his department head in Belyang University,
to obtain a two-year work-study position in the South Chicago Steel Works In 1925 he
enrolled in the Graduate School of Carnegie Institute of Technology where he received a mas-
ter's degree m metallurgy in 1926 His research thesis, on medium carbon manganese steel,
won h~m a dtploma "with distinction," and for which he received the attention of Albert Sau-
veur, a professor at Harvard who had come to Carnegie to give a seminar lecture Chou was
recrmted by Sauveur and was admitted to graduate school at Harvard In verbal reminiscence,
Chou remembers his advisor, Professor Sauveur, as a good teacher who was always cordial,
patient, and listened to his student's ideas. The graduate students in his group (R F Mehl, C
R. Wohman, R Luter, and D. C Lee) would meet each week and everyone would present
their work for discussion and suggestion He was also concerned with their personal life and
well being, especially of his foreign students.
After two years, by mid-1928, Chou had completed a two-volume dissertation [1]. In fact,
Sauveur had recommended him to receive his Ph.D. after one year (research on the effect of
different cooling rates on the formation of Widmanstatten structure in sub-eutectold steels),
but this was not granted, as no one had ever completed a Ph.D at Harvard in one year Chou
subsequently completed a second volume (research on Wldmanstatten-hke structure in rap-
idly quenched pure iron), which will be the focus of much of the remainder of this paper
J. Gordon Parr, in a paper entitled, "The Criterion of the Martenslte Transformation," pre-
sented at the Sorby Centennial Symposium on the History of Metallurgy [2], ascnbes the ear-
hest descnptlon of shape change in martensite to Dumas [3], who, in 1905, descnbed the sur-
face rehef that was observed when a polished sample of nickel steel was rapidly cooled The
portions that "have been transformed project above the onglnal surface, they are those which
have passed into the c o n d m o n of martensite." An earlier observation of such a surface effect
was recorded and illustrated by Osmund in a paper published in 1901 [4] Parr further points
out that, with the exception of the work of Sauveur and Chou [5] in 1929, the characteristic
of surface relief in martensite was apparently forgotten between its early mention up to more
recent studies near mid-century Parr also notes that although the observation of surface rum-
phng had been made by Sauveur and Chou, httle importance was attached to it We have had
the opportumty to examme Chou's onginal Ph D thesis, m addition to the pubhshed paper,
and would like to share some of the contents here
Dr C H Chou studied the allotropic transformation in pure Iron His objective was to
prove that his mentor and adviser at Harvard, Professor Albert Sauveur, was correct m describ-
ing that allotroplc transformation of iron as follows [6]

On coohng through the point A3, at about 900~ iron passes from the gamma condmon to a new
allotrop~c form generally desagnated as alpha Th~stransformation, however, ~s not instantaneous
There are good reasons for behewng that it begins at the gram boundanesalong the octahedral planes
of the crystals and that at progresses untd each gram of gamma iron ~schanged into a gram of alpha
aron, the resulting structure being s~mdar to that of gamma ~ron Were ~t possible to retam at room
temperature pure ~ron but partmlly transformed, at seems probable that a w~dmanstatten structure,
or rather, as later explained, a martensmc structure would be observed, consisting of alpha aron at
the gram boundaries and at the octahedral planes, and ofa groundmass of gamma iron

In order to confirm Sauveur's hypothesis, Chou developed several innovative experimental


techmques, combined with exceptional metallography, to document the transformation.
Using a vacuum etching technique, Chou placed polished samples of electrolytic iron in evac-

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NOTIS ET AL. ON EARLY METALLOGRAPHIC STUDIES 169

uated quartz tubes heated to 1000*C for 2 h and quenched. The results (Fig. 1) show the prior
austenite grain structure that was attributed "to iron volatizing at the grain boundary" [5].
Convinced that iced brine and liquid air were not efficient quench media, he developed an
elaborate method to quench the quartz capsules in mercury. As a result, the quench severity
was vastly improved and what was referred to as the allotropic transformation was clearly
revealed (Fig. 2).
Although Sauveur and Chou left no doubt that they were observing a martensitic/Widman-
statten transformation, they nevertheless mistakenly referred to this transformation as being
allotropic. It was not until 1964, some 36 years later, that Bilby and Parr [ 7] were able to show
the effect of cooling rate on the transformation mode in pure iron.
Chou clearly revealed the surface relief accompanying the martensitic transformation (Fig.
3). He went on to study the effect of carbon on the ability to form martensite and was able to
conclude that increased carbon content and faster quench rate more easily produced the mar-
tensitic structure. On polishing from the surface inward, he was able to show that as the quench
rate decreased the martensite gave way to Widmanstatten and eventually to equiaxed alpha.
Chou was one of the first investigators to recognize that martensite was similar to Widman-
statten in that it formed along octahedral planes (Fig. 4). In the next decade, these results led
to the important crystallographic martensite studies of Kurdjumov and Sachs [8], Nishiyama
[9], and Greninger and Troiano [10].
Finally, recognizing that this low-carbon martensitic structure was unique, Chou labeled it
"Sauveurite," in honor of his mentor. Although the name did not catch on, it became part of
the long list of names for low-carbon martensite including: schiebung, self-accommodating,
cell, massive martensite, needlelike, dislocation, lath, unidirectional, Type I, and packet mar-
tensite [11]. Clearly, the advances made by Chou in 1928 on the study of martensite were great

FIG. 1--Vacuum etching of electrolytic iron.

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170 METALLOGRAPHYPAST, PRESENT,AND FUTURE

FIG 2--Structure of ele6trolytlc iron alter mercury, quenching

and his efforts encouraged the numerous investigations on martenslte in the coming
generations
In the fall of 1929, at age 32, Dr Chlh-Hung Chou returned to the turmod of Kuomlntang,
China, to work at the Shanghal Steel Works where he rapidly moved up to become director.
Starting in 1949, he also simultaneously taught at both Datong Umverslty (where he became
professor and department head) and Shanghai Jlao Tong University (where he became pro-
fessor and vice president) He became associate chief advisor to the Baoshan Iron and Steel
Complex, a modern integrated basic oxygen furnace (BOF) steel plant that started operation
in 1985 In his teaching and research, Professor Chou always stressed the importance of the
study o f phase transformations and the use o f metallographlc techniques At Jiao Tong Uni-
versity, he organized a complete metallographlc laboratory using eqmpment bmlt almost
entirely by his students. For example, he had a graduate student, Longyuan Xu, and a young
teacher, Yongpel Xle, construct a h~gh-temperature metallographlc microscope In the very
late 1970s and early 1980s, when the first groups of American visitors were able to come to
Jlao Tong Umverslty, we all marveled at the mvenhveness demonstrated m this laboratory
Professor Chou realized that in the history of the development of science and technology, qmte
a number of critical invenUons and discoveries were made with the help of a specific experi-
mental instrument or apparatus It was because of this concept that Professor Chou had built
the first high-temperature metallographic microscope in China With it, he and subsequent
workers were able to study the growth rate of WIdmanstatten plates in hypoeutectold steels
and the kinetics of bainitic transformations This work led to the conclusion that the maxi-
m u m growth rate appears after austenltizmg at certain temperatures, and that there is a peak
growth rate corresponding to the incubation period These observations were among the ear-

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NOTIS ET AL ON EARLY METALLOGRAPHIC STUDIES 171

FIG 3--Rehel ~flect of the martenslttc structure (a)fi~cus on valleys and (b) locus on ridges

hest international studies that demonstrated that the Wldmanstatten structure, being coherent
with the matrix, proceeds by dlffusional transformation
In 1985, m Its inaugural issue, the Journal ofChmese Htstory of Sctence and Technology of
Academlca Slmca honored Professor Chou's 70 years as a metallurgist with a rewew article
concerning his professional contributions [ 12] Professor Chou was regarded as the founder of

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172 METALLOGRAPHY:PAST, PRESENT,AND FUTURE

FIG. 4--Octahedral traces in martensite.

modern metallurgy in China, just as his Ph.D. advisor, Albert Sauveur, is considered one of
the fathers of modern metallurgy in the United States.
Chih-Hung Chou was born on 28 December 1897 in Yangzhou, Jiansu Province. Professor
Chou passed away peacefully on 13 February 1991, in Shanghai, at the age of 94. He was loved
by all who knew him; relatives, friends, students, and colleagues all around the world. As a
young student, Chih-Hung Chou must surely have studied the photomicrographs of Henry
Clifton Sorby. As his legacy, Dr. Chou produced one of the most beautiful and thorough
metallographic studies to be found. If a picture is worth a thousand words, and if metallogra-
phy is the metallurgist's universal language, then Chou's thesis is truly encyclopedic and his
metallographic research represents an enduring gift to materials science throughout the world.
As a post script, the special relationships between Lehigh University (started through Chin
Wong) and Jiao Tong University (through Chih-Hung Chou) still continues. His son, Ye T.
Chou, is a professor in the Department of Materials Science and Engineering at Lehigh~ Many
of the faculty at Lehigh, including the present authors, have had the opportunity to visit Jiao
Tong, or to meet Professor Chih-Hung Chou when he visited at Lehigh. A number of under-
graduate students from Jiao Tong University have been graduate students or visitors at Lehigh,
and a few have returned to become faculty members at Jiao Tong University, among them Yi
Cheng Lu, Bing Chu Cai, Ming Gao, and Ming Yuan Gu.

References
[1] Chou, C. H., "The Crystallization of Iron-Carbon Alloys With Special Reference to the Widman-
statten Structure," Parts I & II, Ph.D. thesis, Harvard University, Cambridge, MA, 1928.
[2] Parr, J. G., "The Criterion of the Martensite Transformation," The Sorby Centennial SympoJium
on the History of Metallurgy, C. S. Smith, Ed., Gordon and Breach, New York, 1964, pp. 235-243.
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NOTIS ET AL ON EARLY METALLOGRAPHIC STUDIES 173

[3] Dumas, L, Journal oflron and Steel Instztute Vol 68, 1905, p 255
[4] Osmund, F, "Contribution ~ l'e'tude des alhages," Society d' Encouragement pour l'Industne
Natlonale, 1901, Pans
[5] Sauveur, A and Chou, C H, "The Gamma-alpha TransformaUon m Pure Iron," Transacttons,
American Institute of Mining, Metallurgical, and Petroleum Engineers, Vol 84, 1929, pp 350-369
[6] Sauveur, A, Proceedings, American Phdosophlcal Society, Vol 66, 1927, p 267
[ 7] Bdby, M J and Parr, J G , Journal of the Iron and Steel Instttute, Vol 202, 1964, p 100
[8] Kurdjumov, G V and Sachs, G , Zettschrtft~urPhyslk, Vol 64, 1934, p 325
[9] Nlshlyama, Z, Sctenufic Reports, Tohoku Umverslty, Vol 23, 1934, p 637
[10] Grenmger, B A and Trmano, A R, Transactions, Amertcan Institute ofMining, Metallurgwal, and
Petroleum Engineers, Vol 140, 1940, p 307
[11] Krauss, G and Marder, A R, Metallurgtcal Transactions, Vol 2, 1971, p 2343
[12] Chou, C-H, "Seventy Years A Metallur~st," Zhong Guo Yue Jm Sht Ltao (Journal ofChmese Hts-
tory ofSctence & Technology), Issue 1, 1985, pp 61-71, translated mto Enghsh by the Council of
Chou Chlh-Hung Foundation, 1988

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X-Ray and Electron Metallography

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K u r t F. J. H e m r l c h I

Those Magnificent Men on Their Scanning


Machines
REFERENCE: Heinnch, K F J, "Those Magnificent Men on Their Scanning Machines," Met-
allography Past, Present, and Future (75th Anmversary Volume), ASTM STP 1165, G F Van-
der Voort, F J Warmuth, S M Purdy, and A Szirmae, Eds, Amencan Society for Testing and
Materials, Philadelphia, 1993, pp 177-183

ABSTRACr: A handful of lngemous scientists and engineers, m developing scanning electron


beam instruments, have revolutmmzed the characterization of m~crostructures m material
research Like an adventure game, the development of the scanningelectron m~croscope(SEM),
the electron probe mlcroanalyzer, and the analyhcal transmlssmn m~croscope includes tales of
war and conquest, of genres and intrigue, of s~multaneous and (perhaps not so) independent
d~scovenes, and of strange and Nzarre failures The future perspectwes of this art would be wor-
thy of a science fictmn story

KEY WORDS: metallography, mlcrostructure, metallograph~ctechmques, electrons, ~magmg,


instrument manufacture, metallurgical specimens, m~croanalys~s, m~croscopy, quantitative
analysis, scanning, X-ray absorption, X-ray fluorescence, X-ray spectrometry

The electron was discovered by J J Thomson shortly before the end of the nineteenth cen-
tury [I]. In the decade of 1930, the science and technology of electron optics developed rap-
idly, particularly in Germany De Broghe, Busch, Ruska, and Knoll established the bases for
electron optics and electron microscopy, and a commercial transmission electron microscope
(TEM) built by Bomes and Ruska was available in 1939 (For reviews of the early history of
electron microscopy see Refs 2 and 3, for the development ofmlcroanalysls see Refs 4 through
6 ) Knoll demonstrated the feasibility of the scanning electron microscope (SEM) in 1935, and
scanning versions of the TEM were described by yon Ardenne in 1938 This budding tech-
nology was interrupted by the Second World War the German electron optical instruments
in part were 'liberated' by the victorious allies, and the rest divided between two antagonistic
regimes Where before the war much of the development had occurred, it would take years
until research in applied electron optics was restarted Von Ardenne, following his political
mchnaUons, established himself in Dresden, DDR, cooperating with colleagues in the USSR,
but his work performed there, surely under difficult circumstances, did not greatly influence
the further development of the SEM Smith and Oatley finally built a viable SEM in 1955, and
the first commercial model appeared in England as late as 1965 In the meantime, significant
breakthroughs in applied electron optics had been made in France, the United Kangdom, and
in the United States
In the United States, Radio Corporation of America (RCA) had developed a transmission
electron microscope that became commercially available in 1942, some of these instruments
went to Europe Several institutions in France, Canada, and the United Kingdom received
German instruments after the conclusmn of the war, and these sources of lnstrumentatmn

Retired, National Institute of Standards and Technology, Rockvdle, MD 20850

177

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178 METALLOGRAPHYPAST, PRESENT,AND FUTURE

stimulated further developments in electron microscopy and related areas The main focus of
innovations m England wasthe Cavendlsh Laboratory in Cambridge, where Dr V E Cosslett
directed activities that enriched the field through his work and that of of his colleagues and
students, and through the stimulus it provided to investigators in other places The British
group would lmtlate and further the study of b~ologlcal and geological specimens, high-voltage
spectroscopy (an instrument of this type was developed in Cambridge), the first scanning elec-
tron m~croscope, significant contributions to practical electron optics and development of
electron lenses (Dr Mulvey), and the first prototypes of the analytical transmission electron
microscope (P Duncumb)
Compared with th~s massive effort, the activity in France was, at the beginning, essentially
a one-man show, performed, to be sure, by an extraordinary man, Raymond Castalng He was
at that time working at the Office National d'Etudes et de Recherches Aeronautlques
(ONERA) Castamg became fascinated with the electron microscopes he saw at his institute
Professor Gulmer from the University o f Paris, a d,stmgu~shed sclentzst in the field o f X-ray
optics and diffraction, suggested that he investigate the poss~bdmes of identifying the com-
posmon of small precipitates In steel by exciting them with a focused beam of electrons and
obserwng the emitted X-ray spectra Castamg first underesUmated the difficulty and the mher-
ent limitations of the proposed method, in fact, he thought that the task was too trivial for a
doctoral thesis But after some hesitation he agreed to develop such a mlcroanalytlcal method
(an account by Castalng of these events wdl soon appear m the proceedings of a workshop held
at the National Bureau of Standards (NBS) in 1988) [6]
The precipitates Castamg was planning to characterize were much smaller than 1 um m
diameter--usually they could not be ldenUfied by X-ray diffraction The mmal calculations
indicated that the X-ray lntensmes observable with crystal spectrometers would be a few
counts per minute Castalng and Gulmer considered the posslblhty ofenergy-d,sperslve anal-
ysis (which many years later would be a very widely used techmque in electron microscopes),
but after attaching a focusing (curved-crystal) X-ray spectrometer such as Gmmer used to
monochromatlze X-rays to a modified TEM, Castamg found that h~s forecast had been too
pess,m~sUc, due to the metficlency of curved-crystals for large X-ray sources For a point source
such as that produced on the specimen in his instrument, the count rates were sufficiently high
O N E R A then budt for Castamg a well-constructed spectrometer of h~gh resolution that gave
him the means for the development of the electron probe m~croanalyzer
Another difficulty Castamg ran into was basic, and thus less tractable to impart to the elec-
trons the energy reqmred to excite X-rays emitted by the elements of interest and observable
with the X-ray spectrometers at his dlsposmon, he had to operate at several ten thousands of
volts (his initial work was done at an effective electron energy of 29 keV) But electrons so
energized would penetrate into a microscopically thick specimen to a depth of several microns
The resolution of the classical electron probe m~croanalyzer was therefore considerably poorer
than Castamg had originally expected, nevertheless it was better by several powers often than
the available alternatives (spark source spectroscopy), and Castamg had to accept this physical
hmltatlon
The instrument that Castalng modified was an electrostatic microscope built by Campagme
Francame de Telegraphle Sans Fd (CSF), and its first commercml versions were also provided
w~th electrostatic lenses Later, these were replaced by electromagnetic optics, and Mulvey as
well as Wlttry in the United States contributed to the development of asymmetrical lenses that
allowed the observation of X-rays at h~gh ( > 2 0 ~ emergence angles A static-beam electron
probe was independently developed by I B Borovsky and N P II'ln m the USSR Their work
was published m 1956 The interesting illustration o f their instrument shows the electron col-
umn as a mere attachment mounted on the mowng arm of a large curved-crystal X-ray
spectrometer

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HEINRICH ON SCANNING MACHINES 179

The thesis of Castalng is an admirable document that lays the foundations to the theory of
the instrument and its use for quantitative analysis It also contains examples of applications
in fields of importance, particularly in metallurgy Castalng's work, and the construction of
the first commercial microprobes by CAMECA (the first two Instruments were built at
ONERA), put the French in a leading posmon in microprobe analysis and provided the basis
for the development of a powerful group of investigators, including, among many others, Phi-
llbert, Descamps, Klnanenko, Tlxier, Henoc, Maurice, Galle (in biological applications), and
Pouchou
The development of quantitative analysis was also rapid, although the physics of electron-
target interaction was far from being known to a satisfactory degree X-ray physics and X-ray
generation had been explored by the physicists in the 1920s and 30s, and they had no need for
the quantitative accuracy later required for a microanalytlcal method However, Castamg
observed that many uncertainties in physical and instrument parameters canceled when the
compositional evaluation was based on companng the X-ray intensities from the unknown
s p e o m e n with that from a pure element, and that therefore some simple approximations
could be established We should recall that at that time the powerful computers that nowadays
dominate the processes of analysis and data evaluation did not as yet exist, hence, involved
calculations and particularly procedures for on-line data evaluation were not practical The
main limitation of accuracy was the absorption of X-rays produced within the specimen Its
estimation required the knowledge of the depth distribution of X-ray generation This prob-
lem was resolved by Castalng and his students with the aid of tracer experiments Phlhbert was
the first to provide a general algebraic model for calculating the absorption losses He and Tix-
ler then established the so-called Z A F method that contains three factors responding to atomic
number (Z), absorption (A), and X-ray fluorescence (F) effects
The developments in the United Kingdom covered a wide range of techniques With the
stimulus of the work across the Channel, contributions to electron probe mlcroanalysis came
quickly In Harwell, Poole and Thomas had demonstrated the existence of the atomic number
effect, Green performed important experiments on X-ray absorption by means of an instru-
ment with variable X-ray emergence angle, and introduced the use of Monte Carlo calcula-
tions for the determination of electron trajectories The Monte-Carlo technique was later used
and perfected by numerous scientists, particularly in Japan under the leadership of Professor
G Shlnoda D u n c u m b was the first to formulate algebraically the losses of X-ray production
due to backscatter, and Reed proposed a simple and effective correction for fluorescence But
perhaps the most important British contribution was the introduction of scanning techmques
Electron beam scanning was widely used at that time, for instance, in oscilloscopes The
French school did not, however, use such techniques for the construction of images of element
distributions in the microscopic domain Castaing, and later CAMECA, the French manufac-
turers of commercial instruments, used X-ray spectrometers of fairly high wavelength reso-
lution The X-ray intensities provided with these were too dependent on the position of the
X-ray source on the specimen to be of much use for obtaining X-ray images by electronic beam
scanning Scanning X-ray techniques were first developed at the Cavendlsh Laboratory in
Cambridge, United Kingdom, by Cosslett and Duncumb The latter was also the first to use
color images to simultaneously dlustrate the distribution of as many as three elements m one
image To allow the use of beam displacement necessary for scanning operations, the Cam-
bridge firm that produced the first commercial microprobe used a semifocusing spectrometer
Such devices did have unsatisfactory resolution for some wavelength regions, however, work
such as that performed by Melford clearly demonstrated the usefulness and importance of
scanning imaging for practical applications
Duncumb, who worked in ferrous metallurgy, was also concerned about the problem of
poor spatial resolution observed by Castalng To resolve this difficulty, he constructed the Elec-

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180 METALLOGRAPHYPAST, PRESENT,AND FUTURE

tron Microscope Micro Analyzer (EMMA), in which a thinned metallurgical specimen was
exposed to an electron beam of submlcron width, and the X-rays were observed with energy-
dispersing gas detectors or with conventional crystal spectrometers The fact that the electrons
emerged from the thinned specimen at a short distance from the point of impact minimized
the effects of electron diffusion. Therefore, high acceleration potentials could be used without
penalty in spatial resolution Yet, the intensities observed with the aid of crystal spectrometers
were low, and the energy-dispersive devices were often lacking in the required resolution Dun-
cumb was, unfortunately, ahead of the technical developments only when sohd-state energy
dispersive detectors (SILl detectors) were introduced In microprobe analysis could his instru-
ment (which is now called the Analytical Electron Transmission Microscope) be used to full
advantage Modern instruments of this type also have scanning faclhties, their use has greatly
extended the potential of X-ray mlcroanalysls In metallurgy and biological sciences.
The use o f energy-dispersive detectors was not new in the field At the Stanford International
Conference on X-Ray Optics and Mlcroanalysls, R. M Dolby, a Callforman who was a stu-
dent of the Cosslett group, caused sensation by showing scanning images of the distribution of
low-atomic number elements such as carbon, oxygen, and boron The ultrasoft X-rays emitted
by these elements were detected by a gas proportional counter and separated electronically by
a complicated network of single-channel analyzers That this bnlhant investigator should later
have switched from microanalysls to the construction of novel sound amphficatlon devices
was a loss for m~croanalysls as well as a gain for music lovers
James Hllher, at RCA in Princeton, having made various significant contributions to elec-
tron optics, also became interested in the possibihtles of mlcroanalysls with electron beams
In 1942, he obtained a patent for a device in which a focusing electron column was used for
elemental analysis in the microscopic domain by the energy analysis of the electrons that had
passed through a thin specimen. He later dwected his attention to other problems, and, due to
Castamg's work, X-ray analysis became the preferred tool for this purpose
Before commercial instruments became available, many investigators m the United States,
such as Bwks, Wittry, Adler, J Brown, Ziebold and Ogllvie, Macres, and others, built their
instruments themselves. Microprobe research in this country did not proceed as much as a
team effort as in Europe, rather it was performed by metallurgists and geologists who wished
to apply this instrument to their field It was at that time that I began to make personal contact
with the field Being a chemist, I felt a strong interest in learning the physics on which micro-
analysis is based, and I found my wish more than fulfilled with my participation in an electron
probe summer school at Massachusetts Institute of Technology (MIT), with the partlopation
of Castalng, professor Norton (MIT), Mulvey, and several other experts The abundant display
of "laws" of electron-target interaction, with which I had been unfamlhar, was to me quite
overwhelming. To make up for my ignorance, I collected bibliography in all pertinent fields,
and then proceeded, with the help of some of my colleagues, to prove wrong what I had not
understood m the first place I dare say that m this task we were qmte successful
Of the many instruments that were individually constructed, that of LaVerne Bwks at the
Naval Research Laboratory stands out in my mind It was quite compact, as in most Instru-
ments of that generation, the X-rays exited the vacuum enclosure through a window The col-
umn was standing on a table covered by heavy paper or cardboard, on which mysterious draw-
lngs were traced. A circular curve turned out to be the focal circle along which the bent crystal
and the window of the detector were aligned by hand The device was, from a didactical view-
point, of utmost clarity
Another remarkable instrument had been built by B W Schumacher at the Ontario
Research Foundation The electron beam in his device left the vacuum enclosure through a
d~fferentlally pumped gate, and produced cathodoluminescence in interaction w~th the air I
do not think that many persons have seen, as I did, an electron beam entering a small beaker

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HEINRICH ON SCANNINGMACHINES 1 81

filled with water And I do not believe that this Instrument would meet present safety criteria
any better than Birks'. Curiously, the idea of letting the electrons enter a gas (in this case at low
pressure) was recently revived for .use in a SEM for biological specimens because this technique
reduces at low beam energies the electrostatic charging of poor electrical conductors
The concept of an atmosphenc electron probe was of some interest to the students of mete-
orltes I recall a laboratory, m the area of Boston, where an investigator was building an instru-
ment that could analyze specimens weighing up to a ton To mlmmize vlbrat~ons, the entire
probe system was hung from the ceding on steel girders The design was based on the assump-
tion that meteontes are very precious and could not be cut into the small specimens that could
enter the ports leading to the vacuum enclosure of more conventional instruments Th~s
apprehension, fortunately for the meteorite analysts, turned out to be groundless. The con-
structor ofth~s unique instrument, who insisted m budding all sections of the instrument h~m-
self, apparently ran out of grant money shortly after having built the first spectrometer.
Another designer worked on an instrument to be built commercially m which space charges
w~thm the electron beam were to be avoided by the use of an optical system m which the beam
was gradually compressed without forming a crossover This design, to the chagnn of several
potential customers, never got offthe ground e~ther, although ~ts ongmator was able to pro-
duce the scanning p~cture of a dxme on which I could read the somewhat fuzzy lnscnpt~on:
"In God We Trust "
Although a few French microprobes were |mported into the Umted States, electron probe
microanalys~s only became w~despread with the introduction of a commercial instrument
built by Apphed Research Laboratories (ARL) in Santa Barbara, Cahfornia, designed by D
Wlttry This instrument was quite successful It had three curved-crystal spectrometers (each
with two exchangeable crystals) and efficient scanning facdmes An X-ray emergence angle of
52 5~ ensured an efficient and accurate measurement of X-rays of photon energy down to
about 1000 eV. This angle was obtained by means of a clever design in which the X-ray emis-
sion was observed through the center of the objectwe lens, the specimen had to be elevated
through the body of this lens to pass from the specimen chamber into the operating pos~t~on
The electron column and the spectrometers were inside a huge evacuated chamber that gave
this instrument its characteristic "pregnant" shape The readout electronics were rather simple
but could be upgraded w~thout difficulties This instrument was, I beheve, sold in greater num-
bers than any other electron probe Why this successful mltlal design was not upgraded or
replaced by the manufacturers to keep up with the developing technology ~s a sad story that
should be analyzed in more detad The competing American manufacturers of electron
probes, such as Macres, eventually stopped producing as well, at present, no electron probe is
manufactured in the United States
The motlvat~on for Castamg's work was to resolve a metallurgical problem, and it was m
metallurgy where the instrument was particularly helpful Many phase equdibnum dmgrams
were substantially improved w~th the md of electron probe analysis, and studies of mtergran-
ular diffusion and oxidation were of great practical usefulness The technique also became a
tool of ~mportance m mineralogy, where many new species were--and stall are--first docu-
mented w~th th~s instrument. But the most exciting aspect for many researchers was the study
of extraterrestrial objects In th~s respect, I should mention an interesting investigation, in
which huge hehum balloons were sent to stratospheric heights from a base in Australia, some
cwcled one or more times around the globe, and by means of a funnel-shaped feature at the
top of the balloon, they collected dust particles, presumably of extraterrestrial ongm Unfor-
tunately, ~t was not possible to ehmmate completely the dust contamination d u n n g the take-
off and landing, although a large number of particles were collected, characterized, and visu-
ahzed m scanning images, one could never be fully certain ofthew origin
The excitement reached its culmination with the arrival of the lunar specimens from the

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182 METALLOGRAPHYPAST, PRESENT, AND FUTURE

Apollo flights We had several specimens at NBS, searching for unusual phases by means of
backscattered electron scans that revealed the mean atomic number of the phases under the
beam, and providing qualitative and quantitative analyses of phases of interest The word of
the arrival of the " m o o n stones" in our laboratory spread quickly, and everybody wanted to
see them Unfortunately, several visitors also tned to touch our delicate polished specimens
To avoid such profanation, we prepared a mock "lunar specimen" from one of the pebbles
found in the gravel outside the building We gave our visitors ample opportunities to put their
fingerprints on this artifact, while the real specimens were spared the rough treatment
We soon appreciated the great advantages of the scanning procedure, and Harvey Yakowltz
and myself developed a technique of representing up to three elements, in primary colors, as
well as topographic information on the brightness scale, in color composite images (A similar
procedure had previously been demonstrated by D u n c u m b ) These pictures were not only
informative but also very attractive However, the technique was never widely used because
of the lack of electronic data storage facilities and signal manipulation techniques Blrks had
performed early expenments on storage of scan data in a multlchannel pulse height analyzer
(which had only 500 channels), but the lack of on-line computers hampered the effective use
of the instrument, both for scans and for quantitatlon We were forced to use instant devel-
opment films for the recording of scans, if the result of the color addition procedure was unsat-
isfactory, the entire operation had to be repeated The defocuslng properties of the spectrom-
eter further affected the value and appearance of area scans over more than a few microns
In 1968, at the occasion of an electron probe meeting in California, my family and I toured
the United States by car, and this trap included a visit to the Scnpps Institute of Oceanography
in La Jolla, California There, Ray Fitzgerald showed me a lithium-drifted silicon detector that
he had brought from Oak Ridge, Tennessee, to La Jolla in his car, and installed in his electron
probe Although the energy resolution of this device was four to five times worse than that
available at present, and the observation of low-energy X-rays was hindered by the excessive
thickness of the beryllium detector window, it was very exciting to see the lines of the X-ray
spectrum develop simultaneously on the oscilloscope screen, rather than being revealed
through a lengthy spectrometer scanning operation Ray kindly invited me to stay for a few
days, and, with the cooperation o f K Kell from the University of Anzona (who was not in La
Jolla during my visit), we obtained data that resulted In the first publication demonstrating the
use of such detectors in mlcroanalyzers [ 7] The new X-ray detection device was of very great
impact It was not only very useful in the traditional electron probe mlcroanalyzer, where it
sped up enormously the quahtauve identicatlon process, but it could also be installed in a con-
ventional scanning electron microscope (and also in a TEM), virtually transforming it into an
electron probe mlcroanalyzer, at a relatively low cost The diffusion of this technique in SEMs
may, in fact, have contributed to the slackening in the demands for the more expensive elec-
tron probe
The new technique has some disadvantages the resolution of energy spectra is lnferaor to
that of crystal spectrometers, so that overlap problems anse, and, for the same reason, the
background due to c o n t i n u u m emission IS more pronounced and particularly disturbing in
the conventional scanning images Such problems were resolved when It became possible to
connect the scanning instruments to powerful and fast computers for on-line data evaluation
Excellent scanning pictures can now be obtained, both with crystal and silicon detectors, due
to the calibration and background corrections performed at high speeds Large numbers of
scans can be stored permanently on magnetic tapes and disks At the same time, the data
reduction schemes for quantitative analysis can be made more accurate since there is no longer
the need for mathematical shortcuts as before Because more involved calculations can be per-
formed, it is also possible to extend quantltatlon to layered specimens, to thin films, and to
small (submlcron) particles

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HEINRICH ON SCANNING MACHINES 183

As to the SEM, investigations by many researchers such as Crewe, Wells, and Joy are push-
mg the limits of resolution into molecular dimensions, and this instrument is now a necessary
adjunct to research and quality control in many areas (such as semiconductor manufacture)
The remaining limitations of the X-ray mIcroanalyzer and the SEM have stimulated the
invention of other mlcroanalytlcal tools, such as the ion microprobe and microscope, the
Laser Raman probe, the atomic probe, and the energy loss spectroscope Instruments We now
possess an arsenal of microanalytlcal tools that has proven indispensable for modern science
and technology, thanks to those magnificent men on their scanning machines

References
[1] Thompson, J J, Phtlo~ophlcalMagazme, Vol 4, 1897, p 293
[2] Hall, C E, Introductton to Electron Mtcroscopy, 2nd ed, McGraw-Hall,New York, 1966
[3] Wells, O C, Scanmng Electron Mlcrogcopy, McGraw-Hill, New York, 1974
[4] Quantttatlve Electron Probe Mtcroanalysls, K F J Hemnch, Ed, National Bureau of Standards Spe-
cial PubhcaUon 298, 1968
[5] Helnnch, K F J, Electron Beam X-Ray Mlcroanalyszs, Van Nostrand Reinhold Co, New York,
1981
[6] Electron Probe Quantttatton, K F J Helnnch and D E Newbury, Eds, Plenum Pubhshmg Corp,
New York, in press
[7] Fitzgerald, R, Ked, K, and Helnnch, K F J, Sctence, Vol 159, 1968, p 528

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Samuel M. P u t ' d y I and Leo Zwell 2

Seventy-Five Years of Activity in X-Ray


Methods by ASTM Subcommittee E4.06
REFERENCE" Purdy, S M and Zwell, L, "Seventy-Five Years of Activity in X-Ray Methods
by ASTM Subcommittee E4.06," Metallography Past, Present, and Future (75th Anniversary
Volume), ASTMSTPl165, G F Vander Voort, F J Warmuth, S M Purdy, andA Szlrmae,
Eds, American Sooety for Testing and Matenals, Philadelphia, 1993, pp 184-188

ABSTRACT: ASTM Subcommittee E4 06 on X-ray Metallography was orgamzed m 1925, nine


years after Committee E4 ~tselfwasformed The first standard on radmgraphy was pubhshed the
next year, 30 years after the dmcoveryof X-rays In 1938, Hanawalt et al developed their method
of identifying compounds by X-ray diffraction that became the basis of ASTM Standard E 43,
pubhshed m 1942 In 194 l, the Natmnal Research Councd and ASTM orgamzed the Joint Com-
mittee on Powder Dlffrachon Standards (JCPDS) to administrate the pubhcahon of the data
used m th~s method Since then, the JCPDS has grown to include twelve Cooperating Organl-
zatmns and over 100 contributing sooet~es It became independent of ASTM m 1969 Other
additional activities of Subcommittee E4 06 Have included developing standards on determin-
ing the onentatmn of single crystals, the preferred onentatmn of polycrystals, and retained aus-
tenlte m heat-treated steels

KEY WORDS. X-rays, X-ray diffraction, dlffracUon, standards, metallography, metallurgical


specimens, mlcrostructure, metaUographlc techniques

Sixteen to seventeen years elapsed after the discovery of X-rays by Roentgen in 1895 before
their nature was disclosed by the work of Laue and Bragg F n e d n c h and Kmpplng, at Laue's
suggestion, produced X-ray diffraction patterns of single crystals, which Laue was able to show
reflected the symmetryofthe crystal Thlsdevelopedlnto the famlhar Laue method orpattern
used to determine the orientation of a single crystal and appears as ASTM Method for Deter-
mining the Orientation of a Metal Crystal (E 82-63); and, it is still going strong after 80 years
(the method, not the standard; that's only 42 years old) W. L Bragg, at the same time, 1912,
made the first crystal structure analysis of potassium chloride (KC1) and sodium chloride
(NaCl) by application of his famous law, nX = 2d sm 0 [1] Following close upon these devel-
opments, Debye and Scherrer in Germany in 1916 [2] and A W Hull in the United States m
1917 [3] came up with the powder diffraction camera Hull has been neglected in the history
of X-ray diffraction but he developed a powder camera independently from Debye and
Scherer This was d u n n g World War I and communications between Germany and the United
States were intermittent at best From these developments arose new sciences, X-ray crystal-
lography itself, and the materials sciences
ASTM Committee E4 on Metallography was orgamzed in | 916 Nine years later in 1925,
Subcommittee 6 on X-ray Metallography was organized Its first activity was to publish a long
report [4] prepared by Zay Jeffrles with a section on radiography by H H Lester and another

Semor research associate, Technical Research Center, Detroit, National Steel Corporation, Trenton,
M148183
2Consultant, Swarthmore, PA 19081

184

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PURDY AND ZWELL ON X-RAY METHODS 185

on diffraction by L W McKeehan and E C Baln Two well-known names in metallurgy,


Jeffnes and Baln, have shown up, and later on, other famous names m diffraction and met-
allurgy will appear In 1926, ASTM Tentative Recommended Practice for Radiographic Test-
ing of Metal Castings (E 15-26T) was published as well as defimtions of terms for both crys-
tallography and radiography Thirty years after the discovery of X-rays, ASTM had
standardized their practical use
In the custom of ASTM in those days, standards were published as Tentative for a few years
to obtain field experience in their application Communications were slow, mall traveled by
railroad, and people were reluctant to travel any distance because of the time involved Phil-
adelphia to New Orleans by train took two nights, New York to San Francisco nearly a week
A trip by airplane was an act of desperation, long distance telephoning was an exercise in frus-
tration To clarify a point in a standard required wntmg a letter and awaiting a reply, some-
thing that might take a few weeks, or if the reply was complicated, a few months Life was more
leisurely then You sent off your letter and went about your business until the reply came
In 1929, ASTM E 15 was advanced from a Tentative Practice to a Standard Practice and a
hst containing 20 establishments using radiography and 41 doing diffraction was prepared Of
these, 23 were universities, 12 were industrial laboratories, three were government laborato-
ries, and three were commencal laboratories Interestingly enough, ten of the industrial con-
cerns are still in business and still doing X-ray diffraction A glossary of terms was to be pub-
hshed jointly with the AIME (American Institute of Mining, Metallurgical, and Petroleum
Engineers) and ASST (American Society for Steel Treating, now ASM International) but
apparently was never finished
X-ray diffraction in the times between the World Wars was not easy First of all, you had to
build your own power supply, starting with a me&cal or radlologlcal power supply Second,
there was the problem of obtaining or building a tube A Coohdge tube required no cooling
but only tungsten or molybdenum targets could be used Water-cooled tubes were built but
maintaining the required vacuum was difficult Usually this Involved cracking open a valve
just enough to hold a vacuum low enough to keep the target clean without losing conductivity
through the vacuum Third, there was the matter of camera design and construction In the
second half of the 1930s these problems were alleviated General Electric X-ray Company and
Phflhps Metalhx both began manufactunng sealed-off, demountable X-ray tubes, allowing
production of commerlcal X-ray apparatus. In the same period of time, M J Burger devel-
oped the familiar cyhndncal camera using the Straumanis film mounting method [5] By using
camera diameters of 57 3 or 1 l 4 6 mm, the film could be read directly using a mllhmetre scale
General Electric came out with a 145.5 mm (5 73 in ) diameter camera that had the advantage
that the specimen was out in the open, however, you had to be careful not to stick your finger
through the a l u m i n u m foil shielding the film With these developments, X-ray diffraction
became relatively simple and uncomplicated
At the Annual Meeting of ASTM in 1935, a preliminary symposium was held with nine
talks on radiography and more than 20 on &ffractlon. Next year, 1936, these papers were sum-
marlzed m a formal symposium with six papers each on radiography and diffraction It
was published by ASTM m 1937 as the "Symposmm on Radiography and X-ray Diffrac-
tion" [6]
Back in 193 l, the name of the subcommittee had been changed to X-Ray Methods. Then,
in 1937, Committee E7 on Radiographic Testing (now titled Nondestructive Testing) spht off
from Committee E4 under the leadership of Horace Hardy Lester and Earnshaw Cook. The
remaining portion in Committee E4 took up X-ray diffraction as its main topic There were,
however, a few meetings with the American Society for Metals (ASM), AIME, and American
Physical Society (APS) devoted to considerations of the physical basis of metal properties, but
these went nowhere, as far as we know
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186 METALLOGRAPHY PAST, PRESENT, AND FUTURE

In 1938, J D Hanawalt and coworkers at the Dow Chemical Co published their historical
paper "Chemical Analysis by X-ray Diffraction" [ 7,8]. This paper, which contained the dif-
fraction patterns of 1000 compounds and a method of comparing the three strongest lines
(remember, this was all done on film) of the unknown with the three strongest lines of the
known compounds, was immediately recognized as presenting a workable method of deter-
mining the compounds present in a sample. This is an important point Ordinary chemical
analysis will tell you what elements are present but not how they are combined with one
another Sometimes, a good guess will allow you to make a prediction, but there is no certainty
X-ray diffraction, on the other hand, will tell you what crystal structures are present, and, if
you have been careful, you can infer what chemical compounds are present With both chem-
ical analysis and X-ray diffraction, the chemical compounds in a sample usually can be
identified.
In pnnciple, the procedure is quite simple In the original Index, the " d " spacings o f the
strongest lines of the diffraction patterns, ranging from 0 8 to 20 A, were divided into 77
groups Within each group, the patterns were listed in order of the second strongest line The
third strongest line was also listed Additionally, the intensities of the three lines were also
listed In making a search, you opened the Index to the section containing the strongest line
in your unknown and looked down the list until you came to the second strongest line, then
confirmed the identification with the third strongest line and comparison with the listed inten-
sities A complete diffraction pattern was hsted in a card file The prudent searcher checked
his, or her, identification from the Index with the pattern on the card file Of course, if your
unknown contained several compounds, hfe became complicated It took time, experience,
intuition, and, it is to be hoped, the chemical composition of the unknown, to sort out the
compounds present in a mixed unknown
Subcommittee 6, under W L Fmk, using this method, issued ASTM E 43-42T, Recom-
mended Practice for Identification of Crystalhne Materials by the Hanawalt X-ray Diffraction
Method. Later on, m 1952, there was an argument over the narrowness ofASTM E 43 A small
task force, C L Christ, F W Matthews, and W Parnsh, took up the question of either revising
ASTM E 43 or writing a new procedure After several meetings, a comprehensive text was
written, to be published as a Special Technical PubhcatIon (STP) It never was released
Finally, in 1962, ASTM E 43 was withdrawn Following protracted discussion, if not argu-
ment, agreement that a Methods and Procedures Manual ought to be written was realized
Karl Beu became chairman of the Task Group and was lust getting things going when he died
suddenly After that, calls to authors were ineffective
Returning to 1941, the U S National Research Council (NRC) and ASTM orgamzed the
Joint Committee on Chemical Analysis by X-Ray Diffraction Methods The Joint Committee
pubhshed the first set of X R D cards, comprising the Dow Chemical Co data Each card con-
talned the complete diffraction pattern, ~dentificaUon of the material, its source, and a litera-
ture citation along with the Index book containing the the three strongest hnes and their mten-
slues As menUoned earher, Subcommittee 6 had ,lust promulgated the tentative standard
ASTM E 43-42T, that used these data sets Later, having felt that they had completed their
mission, the N R C dropped out of the Joint Committee and was replaced by the American
Sooety for X-Ray and Electron Diffraction (AXRED), which later combined with the Crys-
tallographic Society of America to form The American Crystallographic Assocmt~on
Meanwhile, the British Institute of Physics had been collecting their own set of cards They
,lomed the Joint Committee in 1944 and thew cards formed the first Supplementary Set of the
Powder Diffraction File (PDF) This Supplementary Set, along with an appropriate Alpha-
betlcai and Formula Index, was pubhshed m 1945 as Set No 2 of the P D F In this set, organic
and lnorgamc compounds were separated, which was not the case in the first set Set No 3
appeared in 1950, Set No 4 in 1952, Set No 5 in 1953, and Set No 6 in 1955 Since 1957, a
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PURDY AND ZWELL ON X-RAY METHODS 187

new set, with about 2000 diffraction patterns, has come out every year Each contained mostly
new data, but some older cards were replaced as better data became available Each new Index
Book interleaved the old and new data, formulas, names, and strongest lines, so that the newest
Index could be used without having to go back to an older edition
Data from the National Association of Corrosion Englneenng (NACE) were incorporated
into the fifth set and NACE became the fourth cooperating society of the Joint Committee in
1953 In 1969, the Joint Committee was separated from ASTM and became an independent
organization--the Joint Committee on Powder Diffraction Standards (JCPDS) Other orga-
nizations from the United States, Canada, the United Kingdom, France, Germany, and Aus-
traha, twelve m all, now comprise the Cooperating Organizations of the JCPDS Finally, in
1977, the name was changed to JCPDS-International Centre for Diffraction Data (JCPDS-
ICDD) Some things, though, die hard, reference IS still made to the ASTM Card File
In the mid 1960s, with the development of modern electron microscopes, selected area elec-
tron diffraction became popular Observed intensities of electron diffraction patterns often dif-
fered from those found in X-ray diffraction of the same substance W C B~gelow and J V
Smnh developed a new index listing the patterns In order of decreasing " d " spacing but using
eight spacings for each pattern and leaving out intensity values The JCPDS called this the Flnk
Index, after Dr W L Flnk of ALCOA, then chairman of the JCPDS In recent times, when
space became available, intensities have been added and now there is so little difference
between the Hanawalt and Flnk Indices that the latter is pubhshed only occasionally
In more recent times, the card file and the index have been computenzed, making searching
easier New software allows better matching but still experience and intuition are required for
effioent searching
Since becoming independent, JCPDS-ICDD has grown m membership and activity
JCPDS-ICDD now publishes its data m several forms, book (three patterns to a page), micro-
fiche, tape, and CD-ROM Selected data sets are published for minerals, for metals and alloys,
for forensic materials, and for electron diffraction Returning to a project of Subcommittee 6,
they have published several sections of the Methods and Practices Manual m the quarterly
journal, Powder Dtffractton These include "Toward Improved Alignment of Powder Dlffrac-
tometers," "Methods of Producing Standard X-ray Diffraction Powder Patterns," "Sample
Preparation Methods in X-ray Powder Diffraction," and "Standard Reference Materials for
X-ray Diffraction," among others Round-robin tests have shown, as they always do, that
uncertainty or error is one to two orders o f magnitude greater than that claimed by individual
participants JCPDS-ICDD is also the publisher of Crystal Data, a compilation ordered on
lattice parameters, of references to structural articles
To be horticultural, the present JCPDS is the flowenng tree that grew from the seed planted
by Subcommittee 6
Other things occupied the subcommittee besides the Powder Diffraction File In 1967, a
Task Group was organized to work on quantitative measurement of retained austenlte in
steels After discussion with the Sooety of Automotive Engineers (SAE), the decision was
made not to duplicate their work However, when Leo Zwell, one of the authors of this paper,
became chairman of the Subcommittee, in 1973, dissatisfaction with the results obtained by
the SAE method was evident A round-robin test was conducted, w~th ten laboratories partic-
ipating As expected, without equipment to rotate and translate the s p e o m e n dunng the test,
the results in three directions were very different but the averages of the three directions were
surprisingly close Robert Hlnton of Bethlehem Steel (a determined man and he had to be)
started offa Task Group that prepared and validated by another round-robm test the ASTM
Practice for X-Ray Determination of Retained Austenlte in Steel with Near Random Crys-
tallographic Orientation (E 975), issued in 1984
Another determined man, Peter R Morns, then of Armco Steel, accepted the lob ofimprov-

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188 METALLOGRAPHYPAST, PRESENT,AND FUTURE

mg ASTM E 81-49, Method for Prepanng Quantitative Pole Figure Diagrams which dated
back to 1949 X-ray diffraction techniques had improved since then He wrote letters to many
people that he thought were qualified but recewed less than ten acceptances Nevertheless, in
two years, he rewsed ASTM E 8 l, producing the document, ASTM E 81-77, with the same
Utle, about the only thing left untouched m the revision
In more recent years, Subcommittee 6 has faltered and lost its way The major achievement
of Subcommittee 6, creation and n u r t u n n g JCPDS, was done JCPDS grew into a strong and
self-sufficient orgamzat~on The present procedures work, although some date back 40 years
and others are as recent as 1984 There seems to be httle demand for new procedures in X-ray
analysis of metal, however, one subject that may offer an opportumty for work ~s the Orien-
tation DlsmbuUon Function, but this is an enormously comphcated subject Subcommittee
6 on X-ray Methods has been folded into Subcommittee I 1 to form a subcommittee on X-ray
and Electron Metallography

References
[1] Bragg, W L, Proceedings, Royal Sooety, London, Vol 89A, 1913, p 248
[2] Debye, P and Scherrer, P, Zetts~hrdt[urPhyslk, Vol 17, 1916, p 277, Vol 18, 1917, p 291
[3] Hull, A W, Phystcal Revw~, Vol 10, 1916, p 661, Journal, American Chemical Sooety, Vol 41,
1919, p 1169
[4] Jeffrles, Z, Proceedings, American Sooety for Testing and Materials, Vol 25, Pt 1, 1925, p 444
[5] Buerger, M J, Amertcan Mlneralologlst, Vol 21, 1936, p 11
[6] Proceedings, Symposmm on Radiography and X-ray Diffraction, American Sooety for Testing and
Materials, 1937
[7] Hanawalt, J D and Rmn, H W, lndustrlalandEngmeermg Chermstry, AnalyttcalEdmon, Vol 8,
1936, p 244
[8] Hanawalt, J D, Rmn, H W, and Frevel, L K, Industrial and Engineering Chemtstry, Analytwal
Edltlon, Vol 10, 1938, p 457

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Atul S. Rarnanl ~and Paul R. H o w e l l I

Microstructural Studies of an Oxide-


Dispersion-Stabilized Niobium Composite
Using Transmission Electron Microscopy
REFERENCE: Ramani, A S and Howell, P R, "Microstructnral Studies of an Oxide-Disper-
sion-Stabilized Niobium Composite Using Transmission Electron Microscopy," Metallography
Past, Present, and Future (75th Anmversary Volume), ASTM STP 1165, G F Vander Voort, F
J Warmuth, S M Purdy, and A Szirmae, Eds, American Society for Testing and Matenals,
PhdadelphIa, 1993, pp 189-198

ABSTRACT: Transmission electron microscopy (TEM) has been employed to examine the
effect of mechanical alloying and subsequent hot isostatlc pressing (HIPmg) on the mlcrostruc-
lure of a mechanically alloyed nioblum-yttrlacomposite It ~sshown that the mechanical alloy-
ing process severely cold-works the niobium matrix and an elongated cell structure develops
Partially recrystalhzed regions form dunng the HIP cycle From the TEM data, it is argued that
recrystallization proceeds by repeated nucleation of new strain-free grains m contact with the
"old" recrystalhzation front This process is facilitated by the yttna-denved dispersoids that are
efl~ctwe m mhlbmng the motion of the "old" recrystallizatlon front Hence, partial recrystalh-
zation produces a necklace of small (~0 5 to 5 urn) grains that surround the still highly deformed
matr, x

KEY WORDS: niobium, yttna, oxide d~sperslonstrengthening, metal matnx composite, creep,
recrystalhzatlon behavior, necklace mlcrostructure, transmission electron microscopy, mechan-
ical alloying, hot isostatlc pressing, metallography, metallurgical specimens, mlcrostructure,
metallograph~ctechniques

In this paper, we report results of microstructural studies of an as-hot lSOStatically pressed


(HIPed) m o b m m - 2 % by volume yttna (Nb-2Y) composite using transmission electron
microscopy (TEM) The metallographic studies have permitted the formulation of a model
for recrystalhzation m this composite
The invention of mechanical alloying by Benjamin [1] made it possible to produce a whole
new class of oxlde-dlspersion-stablhzed alloys with good high-temperature strength The
promise that oxide-dispersion-staNhzed alloys offer is their exceptional creep resistance and
good mlcrostructural stabihty at high homologous temperatures The refractory metal, nio-
bium, has the potential for being used m applications that require high strength-to-weight
ratios at elevated temperatures However, at high temperatures, creep processes become a
major concern and these have been extensively studied in both pure niobium and nlobmm-
based alloys [2-4] Creep strengthening by second-phase particles has been shown to be fairly
effective [3], however, the thermal stability of the precipitate distribution is a major concern,
since coarsening of the precipitate d~stnbutlon d u n n g prolonged aging at high temperatures
significantly affects the creep strength We have employed mechanical alloying to d~sperse fine
(_<0 5 ~m) high purity yttna particles, homogeneously into a niobium matrix as a means of

hGraduate student and professor of Metallurgy, respectively, Department of Materials Science and
Engmeenng, The Pennsylvama State Umverslty, Umverslty Park, PA 16802

189

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190 METALLOGRAPHYPAST, PRESENT, AND FUTURE

obtaining a creep resistant moblum composite with a stable second-phase distnbutlon Due
to the high-energy nature of the mechamcal alloying process, where repeated welding, frac-
tunng, and reweldmg of dry powder particles produces the final alloy, the deformation pro-
cesslng aspect of the mechanical alloying process is very important The mechamcally alloyed
powder particles have a considerable amount of cold-work stored in them Hot isostatlc (HIP-
rag) of the mechanically alloyed powder particles that is used to consohdate them into a com-
posite, brings thermally achvated processes such as recovery and recrystallIzatlon into play

Composite Processing
Feedstock of overall composmon, m o b m m - 2 % by volume yttria, was prepared by blending
elemental (~< 100 #m) niobium powders and ( < 10/~m) yttna powders of high starting pumty
Mechamcal alloying of this feedstock was camed out by charging it into a laboratory-scale
high-energy ball mill, known as a Szegvan attntor, that was filled with steel balls During the
entire mechamcal alloying process, the attntor was water cooled and an inert argon atmo-
sphere was maintained to prevent any major contamination of the powders The process was
considered complete when the composite powder particles had a finely layered and umform
structure as determined by hght microscopy It was assumed that at this stage the yttna dls-
persolds were randomly distributed within the m o b m m matrix. The mechanically alloyed
powders were sealed m mild steel tubes under a vacuum of 10 2 Pa at 673 K The sealed tubes
were HIPed at 1573 K for 4 h under a pressure of 210 MPa to obtain the final composite A
schematic dmgram of the processing schedule is shown in Fig 1

Preparation of Niobium Composite Specimens for TEM


Two major steps were involved in preparation of specimens for TEM (1) preparation of
thin disks from bulk material, and (2) final thinning of the disks to electron transparency

Preparation of Thm Dtsks from Bulk Matertal


A diamond wafering saw was used to section a cylindrical rod of the bulk composite into
thin slices about 1 m m thick These slices were mechanically thinned to 200 #m using succes-
swely finer silicon carbide (SIC) grit papers. The final mechanical thinning step was done using
a mechanical thinning fixture and 600-grit SIC paper, where the specimen thickness was con-
stantly monitored with a micrometer gage Since the resulting thin sheets of the composite
speomen were not ductile enough to be punched using a conventional mechamcal punch,
d~sks that were 3 m m in diameter were cut from these sheets using an ultrasomc disk cutter
The disks were further throned down to 100 #m using the throning fixture and 600-grit SIC
paper Finally, the disks were dimpled to yield a 10-um-thick section m the center of the disk
speomen using a digital dimpling gnnder and (--<6 um) dmmond paste as the pohshing
medmm

Fmal Thmnlng of the Dtsks to Electron Transparency


The dimpled disks were mounted on an ion-millingspecimen stage and thinned to electron
transparency using an argon ion-mill operating at a gun voltage of 3 75 kV and a gun current
of I mA The initial ion-milling angle was set to 20* Ion milling was periodically interrupted
in order to check for formation of thin area on the dimpled speomen using a low-power micro-
scope Ion milling was stopped when the formation of a small hole was first noticed after which
the ion-milling angle was reduced to 7* and ion milling continued for an hour The ion-milled

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RAMANI AND HOWELL ON RECRYSTALLIZATION BEHAVIOR 191

START

[ Nb + Yttria : Blend ]

I Mechanical Alloying I
I Encapsulation of Alloyed Powders I

I Hot Isostatic Pressing I


1
FINISH : As - HIPed microcomposite
FIG l--Schematlc dlagram of composlteprocesslng schedule

speomens were then examined with a Phlhps EM420T TEM operating at 120 kV Figure 2 is
a schematic diagram of the specimen preparation procedure for TEM exammaUon

Results and Discussion


Mlcrostructure Due to Deformation Processing by Mechanical Alloyzng
In the as-HIPed condition, certam regions of the mlcrocomposlte show no evidence of
recovery and recrystalhzatlon Figure 3 is a bnght-field (BF) TEM mlcrograph from one such

[ Sectioning [

[ Mechanical Thinning[

] Ultrasonic Disk CuttingI

]Dimpling]

] lon'Milling I

ITEM Examination ]
FIG 2--Schematw diagram of specimen preparationprocedurefor TEM exammatlon
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192 METALLOGRAPHY PAST, PRESENT, AND FUTURE

region Characteristic of such regions are the severely elongated subgralns (aspect ratio
l0 1) The subgraln size is exceedingly fine along the thin dimension, typically 0.05 #m.
The figure clearly reveals the deformation processing aspect of the mechanical alloying pro-
cess This intense deformation of powder particles is due to the repeated high-energy cold
welding processes that occur within the attritor during collisions between the steel balls and
the concurrent entrapment of powder between the colhdlng balls It is evident from Fig 3 that
a large fraction of the input cold work from the mechanical alloying process is retained by the
niobium matrix In addmon to the preceding, certain regions of the specimen had partially
recrystalllzed These regions are discussed later

Nucleatton o f R e c r y s t a l h z a t l o n
Figure 4a is a BF Image of a partially recrystalhzed region The recrystalhzed grain (R) is
virtually strain free as can be gaged from both the BF image and the indexed selected area
diffraction pattern (SADP) of Fig 4b; the latter showing no evidence for arcing of the reflec-
tions Figure 4a also shows evidence of recovery in the deformed regions ahead of the advanc-
ing recrystalhzatlon front (the latter is marked F in Fig 4a) The presence of large subgralns
(S) suggests that recrystalhzatlon is o c c u m n g by a subgraln coalescence mechanism [5] How-
ever, the virtually ubiquitous observation of well-developed recrystalllzatlon fronts (for exam-
ple, see Figs 4 and 5) argues strongly for a mechanism involving pre-existing high-angle grain
boundaries rather than random nucleation in the deformed matrix Hence, it is likely that

FIG 3--BHght-/leld T L M linage o / a n tmretrvstalhzed regton m the ~ompostte 6hara~terlzed bl a


~eveteh ehmgated ~ell slrlt~lltre

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RAMANI AND HOWELL ON RECRYSTALLIZATION BEHAVIOR 193

FIG. 4 - - ( a ) Bri~,hl:/ield 7"EM imu~,e ~?/a partially cowtallizcd re,~,ion. N~le lhe ,~lram li'cc nalurc ~!/ lhc
rccry~la/lizcd L,raipl (R) and lhc pre~ence ~ f /ar~,(, .~ut~g,rains (S) in lhe vicmily O/'lh(' r~'o'.l'.~l~l//i:~llio/1 I/'O/ll
(F). (b) Selecl~'d urea df/lraclion l~allc>rn ot~lained //om the re~,ion (R) i/t b'i~,. 4a. 771ere i.~ m~ cvideHce #~r
arcin~, ~t l/tc rc/leclio/t.~. B = [ 1 lO]xj,.

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194 METALLOGRAPHYPAST, PRESENT,AND FUTURE

FIG 5--Brtght-BeM T E M trnage o[ a well-developed recrvsTa/hzatmn [ront (F) The re~ry~talhzed gt am


stze ts relattvelv smal[ (tvptcall)~ 0 5 to 5 urn) and eqmaxed

prior mobmm particle boundaries are the nucleation sites for recrystalllzatlon In ad&tlon,
the very infrequent observation of large subgralns, "in regions remote from the recrystalhza-
Uon front," (and see Fig 5) again argues against "random subgraln coalescence "
However, large subgrams were frequently observed "in contact with the recrystalhzatlon
front" and an example of this phenomenon is presented in Fig 6 Again, the coarsened
subgraln is labeled S and the recrystalllzaUon front is labeled F

T h e R o l e o f DIspersotd Parttcles in the D e v e l o p m e n t o f a " N e c k l a c e " Mtcrostructure


Figure 5 shows that the recrystalllzed grain size is relatively small (typically 0 5 to 5 um) and,
m general, the recrystalhzed grains are relatively equlaxed. To substantiate th~s claim, Fig 7
is included In this figure, the &spersold is labeled Y, and the band (or necklace) of recrystal-
hzed grains have dimensions that are similar to those in Fig. 5
It is considered that recrystalhzatlon in this composite ~s occurnng in a manner that is vir-
tually identical to that documented by Bee et al. [6] for the case of a powder-produced nickel-
base superalloy In c o m m o n with the present lnvestlgaUon, it was concluded m Ref 6 that
recrystalhzatlon was initiated at high-angle gram boundaries. Furthermore, the nickel-base
superalloy employed by Bee et al [6] contained relatively large ( ~ 0 5 um diameter) 3" parti-
cles and the present alloy also contains submlcrometer &spersold particles that derive from
the starting yttna powders. In the following, it is argued that repeated nucleation of recrystal-
hzed grains yields the so-called "necklace" structure
Figure 8 shows a recrystalhzatlon front In common with any second-phase particle, the
submlcrometer (--<0 5 #m) dispersold particle derived from yttrla is exerting a Zener-type [ 7]

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RAMANI AND HOWELL ON RECRYSTALLIZATION BEHAVIOR 195

FIG 6 - - B r t g h t - h e t d T E l 4 zmage sho~* m g a lars sub,g, ram (S) m conlacl atth the rer r~ slal/izallon
/ l o n t (F)

FIG 7-- Brl~hl-BeM T E ~1 t m a g e sho~ m g a l'ttrla-derl~ ed ch spot stud pat ire le ( Y ) art e s l m g t/~e ter t ~ s-
Copyright
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al~o lhe reserved); Wed pDec
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ol SltHllal
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196 METALLOGRAPHYPAST, PRESENT, AND FUTURE

FIG 8--Br;ghl-held T E M ;rnage dlustratmg lhe Zener drag [or~e on the recrystalhzatlon ]ront e.~erted
by a vHrta-der;ved d;spersotd partt~ h, (Y) Note the large subgram (S) m ~onta~l w;th the reervstalhzatmn
[ront

drag force on the boundary This drag force locally pros the boundary, which is then forced to
bow around the particle Figure 7 shows similar features (At this point, it should be noted that,
as yet, we have been unable to determine the crystal structure of the dispersolds Somewhat
surprisingly, they are not yttrlat) Figure 8 also shows that there is a large, strain-free subgraln
(S) in contact with the recrystalhzation front It is considered that this large subgraln forms by
the accelerated loss of dislocations to the high angle reaction front (this point will be returned
to later) The formation of this large subgrain (a further example of which has already been
presented in Fig 6) reduces the local strain energy differential, needed to propagate the "orig-
inal" recrystalhzatlon front through the heavily deformed regions that are immediately adja-
cent to the front Therefore, it is suggested that the formation of large subgralns, in contact
with the pinned reaction front, suppresses recrystalllzation from continuing from the original
position o f that front Rather, continued coarsening ofsubgrains such as (S) in Figs 6 and 8
will yield new recrystalhzation nuclei, and a necklace of small, equlaxed grams will result

The Model
The development of the necklace structure can be modeled with respect to Fig 9, which is
a schematic illustration of what we consider to be a sequence of events in the formation of the
"necklace" mlcrostructure. In Fig 9a, it is assumed that the recrystalhzation front has been
pinned by a dlspersoid particle (Y) (see also Figs 7 and 8) Because of the proximity of high
angle interfaces, subgraln coarsening (Areas C, D, and E in Fig 9a) will be accelerated m the
immediate vicinity of the recpystallized grains (see Figs 6 and 8) This will most probably occur

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RAMANI AND HOWELL ON RECRYSTALLIZATION BEHAVIOR 197

FIG. 9--Schematic illustration qf the sequence of events in the formation of the "'necklace" micro-
structure.

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198 METALLOGRAPHY PAST, PRESENT, AND FUTURE

by dislocation loss to the high-angle grain boundanes During the process, the driving force
that maintains migration for Grams A and B will continually decrease and, eventually, this
driving force will be less than the drag force Migration will then cease Further recrystalhza-
tion will occur when the coarsened subgralns will have attained a sufficient mlsonentatlon and
size advantage A new recrystalhzation front will then form as shown in Fig 9b The processes
descnbed here then simply repeat as new pinning dlspersold particles are encountered and new
coarsened subgralns (F and G in Fig 9b) are formed

Conclusions
An oxide-dispersion-strengthenedniobium composite with a nominal StOlChlometry of nio-
b i u m - 2 % by volume yttna has been fabricated using mechanical alloying and hot isostattc
pressing A fine dispersion of dispersolds In a highly deformed niobium matnx charactenzed
by severely elongated subgralns is obtained by the high-energy mechanical alloying process
Partial recrytalhzation of the niobium m a t n x occurs upon subsequent hot isostatic pressing
Evidence obtained by transmission electron microscope studies of the niobium composite
argues against random subgraln coalescence as a recrystallizatlon mechanism In this compos-
ite A model that explains the formation of the "necklace" mIcrostructure observed in the
composite hasbeen formulated It involves repeated nucleation ofrecrystalhzedgralnsat pnor
recrystalhzatlon fronts that have been pinned by the dlspersold particles This process yields
the "necklace" mlcrostructure

References
[1] Benjamin, J S, Metallurgwal Transactions, Vol 1, 1970. p 2943
[2] Begley,R T , Harrod, D L, and Gold, R E m Refractory Metals andAlloys, Metallurgy and Tech-
nology, I Machm, R T Begley,and E D Welsert, Eds, Plenum Press, New York, 1968, p 41
[3] McAdam, G D, Journal of the lnstuute of Metals, Vol 96, 1968, p 13
[4] Klein. M J and Metcalfe, A G , Metallurgical Transactions, Vol 4, 1973, p 2441
[5] Hu, H, Acta Metallurgtca, Vol 10, 1962, p 1112
[6] Bee, J V, Jones, A R, and Howell, P R, JournalofMaterlalsScwnce, Vol 15, 1980, p 337
[7] Zener, C, pnvate commumcanon to C S Smith, Transacnons of the Amerwan Institute of Mmmg
andMetallurgt~alEngmeers, Vol 175, 1949, p 15

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Rajan Varughese I and Paul R. H o w e l l I

The Application of Transmission Electron


Microscopy to the Study of a Low-Carbon
Steel: HSLA-100
REFERENCE: Varughese, R and Howell, P R , "The Application of Transmission Electron
Microscopy to the Study of a Low-Carbon Steel: HSLA-100," Metallography Past,Present, and
Future(75thAnmversary Volume),ASTMSTPI165, G F VanderVoort, F J Warmuth, S M
Purdy, and A Szlrmae, Eds, American Society for Testing and Matenals, Philadelphia, 1993,
pp 199-211

ABSTRACT: Transmission electron microscopy (TEM) together with scanning electron micros-
copy (SEM) and optical microscopy have been employed to analyze the microstructures that
develop in a copper-contalmng, low-carbon (0 04% by weight) HSLA- 100 alloy Specifically, the
martensmc mlcrostructures that develop in the simulated, coarse-grained heat-affected zones
(HAZs) have been examined and compared with those that develop in the base plate dunng con-
ventlonal quenching from the austemtlC phase field It has been shown that the lath martensltlC
packet size is increased dramatically in the HAZ as compared with the base plate In addition,
considerably more retamed austenite is found in the HAZ No ewdence for the so-called granular
balnite mlcroconstltuent has been found in either material However, for coohng rates somewhat
less than that experienced in the coarse-grained HAZ, a mlcroconstltuent that we term granular
fernte has been documented
Finally, the effect oftempenng on the martenslte in the base plate has been examined As soon
as they are observable, the copper (Cu) preopltates can be identified as face-centered cubic (fcc)
e-Cu

KEY WORDS: steels, martens~te, granular balnlte, granular ferrlte, copper precipitates, welding,
heat-affected zones, transmission electron microscopy, scanning electron microscopy, light
microscopy, metallography, metallurgmal specimens, microstructure, metallographlc
techniques

This paper is concerned with a metallographlc e x a m i n a t i o n of a new class o f steels that are
designated as H S L A - 1 0 0 Transmission electron microscopy (TEM), scanning electron
microscopy (SEM), and hght microscopy have been used to d o c u m e n t the p r e d o m i n a n t l y
martensltlC microstructures that develop in these alloys H S L A - 100 displays superior welda-
bihty and hence, as part o f an overall investigation o f the material, the coarse-grained heat-
affected zone ( H A Z ) has been simulated usmg a Gleeble and analyzed metallographlcally, pri-
marily by T E M In addition, the "base plate," which conventionally would be used in the
q u e n c h e d and t e m p e r e d condition, has been e x a m i n e d and c o m p a r e d with the H A Z
Previous studies [I,2] have indicated that "granular b a m l t e " might form In these steels
Smce the introduction of this terminology [3] to describe certain morphological features found
in hardenable steels, it has been often used in the literature, despite the lack o f a clear consensus
as to the strict nature of this transformation product In addition, there is no consensus con-
c e r n m g the phases, morphology, and the disposition of the phases that constitute granular

Research associate and professor of Metallurgy, respectively, Department of Materials Science and
Engmeenng, The Pennsylvania State University, University Park, PA 16802

199

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200 METALLOGRAPHYPAST, PRESENT,AND FUTURE

balnlte [4,5] Hence, one of the major goals of the study was to obtain unambiguous evidence
for the presence (or more likely, the absence) of this mlcrostructural entity To obtain this
"evidence," the present study has also employed cooling rates somewhat less than those expe-
rienced in either the HAZ or the quenched base plate

Experimental Approach
The composition of the expenmental material is given in Table 1 For the coarse-grained
HAZ studies, 6-mm-dlameter rods were machined and were weld s~mulated to a peak tem-
perature of 1320~ followed by cooling at a rate of 20~ through the 800 to 500~ temper-
ature range This simulation corresponds to a heat input of about 2 kJ/mm for the plate thick-
ness involved The simulation was performed on a Gleeble, courtesy of the David Taylor
Research Center, Annapolis, Maryland In addmon, continuous cooling transformation stud-
ies were performed on 5-mm-thlck samples by air cooling from 900~ at a rate of 7 5~ For
the present analysis on tempering of the HSLA-100 steel, 6-mm buttons (thickness = 6 mm)
were reaustenltlzed at 9000C for 15 m m and then water quenched at a rate of 40~ The
samples were then tempered at 600~ for times ranging from 30 rain to 48 h
Specimens for light microscopy and SEM were prepared through standard metallographlc
practices [6] and were etched in nltal or a mixture of nltal and plcral Thin foil specimens for
TEM analysis were prepared by first grinding 1-mm-thlck slices on a 400/600-grit silicon-car-
bide (SIC) paper to a thickness of 75 to 100 um Three-mllhmetre-dlameter disks were sub-
sequently punched, glued to a steel block, and further ground to a 35 to 50 #m thickness on
600-grit SIC paper After removing the disks from the block, they were then electropohshed to
electron transparency in a twin-jet electropohshlng unit using an electrolytic mixture consist-
ing of 95% acetic acid and 5% perchlorlc acid at room temperature TEM examinations were
carried out using a Phxhps EM420T at an accelerating voltage of 120 kV

Results and Discussion


The Mlcrostructure of the Coarse-Grained H A Z
The mlcrostructure of the simulated coarse-grained HAZ (peak temperature 1320~ and
coohng rate approximately 20~ consisted of very large packets ( ~ 50 um in diameter) of
lath martenslte as shown in F~gs 1a and b The laths are typically 0 2 to 0 4 um wide Reference
to Fig 1b shows that what might be termed "granular features" are present (arrowed)
TEM examination of the HAZ confirmed the presence of lath martenslte (for example, see
Fig. 2a) and it can also be seen that there are lnterlath films that appear dark in the bright field
(BF) image Centered dark field (CDF) images of the latter regions (for example, see Figs 2b
and c) show that these lnterlath films are retained austenlte (Figs 2b and c were imaged using
an 002 austemte reflection, see also Fig 8c) Reference to Figs 2b and c also shows that e-
copper (c-Cu) precipitation is absent m the CDF images (since both 7 and e-Cu are related to
the ferrlte by the Kurdjumov-Sachs OR [ 7,8], then a fraction of any e-Cu that might be present
should also be illuminated in the austenlte CDF image) This is not surprising, considering the
relatively rapid coohng rate However, the possibility of copper-rich Gurnler Preston (G P )

TABLE l--Chemtcal ~omposttton o/the HSLA-IO0 steel (percent by wetght)

C Mn P S SI Cu NI Cr Mo A1 Nb

004 082 0014 0002 032 1 59 345 058 051 003 003

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VARUGHESE AND HOWELL ON EXAMINATION OF STEEL ALLOYS 201

FIG 1--Ml~rostructure o/the coarse-gramed HA Z (stmulated /or a weld heat input of 2 kJ/mm) m the
ItSLA-IO0 alloy Coohng rate ~ 20~ (a) Ltght mt~rograph o/ the ba~l~ martemmc structure, and (b)
SEM mt~ rograph o/the lath ~tructure Narrow, elongated mterlath con~tttuent~ are also present

zones belng present cannot be discounted Finally, no evidence for granular bamlte was found,
and the occasional, large ferrltlC regions that were observed were found to be twinned as shown
In the BF-twln CDF image pair of Fig. 3 Hence, it can be concluded that the m~crostructure
in the HAZ is comprised of lath martenslte together with retained austenlte

The Ml~ro~tructure o f the Quenched Base Plate


Details of the material that has been reaustenltlzed at 900~ and quenched are to be pub-
llshed elsewhere However, for the sake of completeness and to facilitate a comparison with
the HAZ, a brief description follows Figures 4 and 5 are a hght mlcrograph and BF TEM
image, respectively, of the quenched material The quenched materml ~s fully martensltlC, con-
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202 METALLOGRAPHY PAST, PRESENT, AND FUTURE

FIG 2--(a) TE~I b~l#llt held (Bk) mlaL,e o/the lath mlcrosmr (b and c) ('Dk lma~,es o/retained
altsfclll{~" (002 atl~{eHll~, r~,/le~lion ~)

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VARUGHESE AND HOWELL ON EXAMINATION OF STEEL ALLOYS 203

FIG 3--(a) s Bk lmage of a lar,~e martensttlC ~t am that contam~ ~ne-s~ a/e t~ ms (b) r
twin CDb tmage

FIG 4 - - L i g h t mlcrograph o[ the quen6hed base plate

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204 METALLOGRAPHYPAST, PRESENT,AND FUTURE

FIG 5--BF tmage o[ the lath rnartenstte Free ntobmrn-~arbMeprectpttates are pre;ent

SlStlng prlmardy of fine laths with widths of the order of 0 1 to 0 2 ~m and several microns In
length Generally, th~s length ~s hmlted either by the block &menslon or the packet s~ze At
th~s point, it can be noted that the laths m the HAZ could be as long as 50 um that was the
approximate packet size Now, reference to Fig 4 reveals a number of regions that are hghtly
etched and again could be IdenUfied as granular bmmte However, TEM analysis provided no
ewdence for such a m~crostructure and the only other m~croconst~tuent found m the quenched
material was retained austemte, located primarily at the mterlath boundaries as also noted in
other low-carbon steels containing mckel and chrommm [9] In contrast to the HAZ, the vol-
ume fraction of retained austemte was very small In common w~th the HAZ, some large inter-
nally twinned regions were observed occasionally These large internally twinned martensmc
units are occasionally observed m low-carbon steels [10]

The Effect o f Tempering on the Quenched Base Plate


Figures 6 and 7 are hght mlcrographs of samples that had been tempered for 2 h and 48 h,
respectively, at 600"C At these magnifications, there seems to be httle &fference in the two
materials However, TEM examinations reveal that substantial m~crostructural changes occur
during extended tempering treatments
After 3 h aging (Figs 8a and b), the lath structure is stdl preserved and a fine dispersion
( ~ 25 nm m diameter) ofe-Cu has developed both on the lath boundaries and within the laths
The C D F image of copper precipitates seen m Fig 8b has been formed by the combined (002)
3,/e-Cu reflection as shown in Fig. 8c (austemte and e-Cu both being fcc and have slmdar lattice
parameters, the 002 diffraction spots coincide) The C D F image m F~g 8b also reveals the
presence of stabilized austemte in the m~crostructure after aging After 10 h of aging, the lath
structure is replaced partially by eqmaxed fernte (Fig. 9a) although certain regions still retain

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VARUGHESE AND HOWELL ON EXAMINATION OF STEEL ALLOYS 205

FIG 6--Light mlcrograph o/the ba~e plate after tempering/or 2 h at 600~

vestiges of the lath structure (Fig 10) C D F images of the precipitates formed by the (002)
copper reflection confirms their identity as e-Cu Comparison of Figs 9 and l0 with that of
Fig 8 shows that the copper precipitates have coarsened considerably after l0 h and many of
the larger lntragranular particles are assuming a rod-like morphology After 48 h aging, the
dominant femtlc morphology is equlaxed (Fig 1 l) although, in c o m m o n with the 10-h aged
material, certain regions still retain a lath-like morphology (Fig 12) Reference to Fig 11
shows a number of coarse e-Cu preopltates on the gram boundaries

FIG 7--Ltght mlcrograph o! the ba~e plate after tempering/or 48 h

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206 METALLOGRAPHY PAST, PRESENT, AND FUTURE

FIG 8--(a) T L M B F linage o/the lath structure and ( opper preclpttates, (b) austemte/e~-Cu CDF image,
and(c) s'elected area dl/]ractmn pattep n (SADP) o[ Ftg~ 8 a and b The 002 rejle~twn wa~ u~ed to /orm Fig
8b

The Mlcro~truc ture o / A i r - C o o l e d Sample~ o f the Base Plate

Specimens that were reaustenmzed at 900~ and cooled at 7 5~ were examined m order
to (hopefully) develop ferrlte/martenslUc mlcrostructures that could correspond to what has
been termed "granular balnlte "Reference to Fig 13 shows that a dual-phase, ferrlte plus mar-
tens~te, m~crostructure develops The martenslte was found at the equlaxed fernte grain

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VARUGHESE AND HOWELL ON EXAMINATION OF STEEL ALLOYS 207

FIG 9--(a) T I i ~1 B1~ m ~ a f e cd c oa~ ~ened coppcr prcc zptzazes a/let ] 0 h a~.n~~ (b a~ld c) ( ' D I ~ zrna~c
l o o m e d ~ zt h the 002 ~-( zl t e/lc,~11on

boundailes, and somewhat mtcrestlngb within the ferrlte grams (Figs 14a and b) This latter
mlcroconstltuent, fernte plus entrapped pools ot martenslte could be termed granular bamlte
However we would argue that granular fernte is a more appropriate designation since this
mlcroconsntuent, predominantly fernte plus martenslte, does not conform to either of the
current defimtlons of bamlte that are (for steels)

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208 METALLOGRAPHY PAST, PRESENT, AND FUTURE

FIG I O--BF tmage o/the lath-hke mtcrostructure after lO h o! agmg

FIG 11 --Coarse prectpttate~ o[ copper on the gram boundartes after 48 h agmg

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VARUGHESE AND HOWELL ON EXAMINATION OF STEEL ALLOYS 209

FIG 1 2 - - B F tmage oJ the 48-h aged material Remnants of a lath morphology are observed

FIG 13--(a) Ltght mlcrograph o/specimen ~ooled at 7 5~162 A granular morphology Is present (b)
T L M Bk linage the stru~lure is a dual phase, ~on.~Istmg o/equtaxed !errtle and marten site

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210 METALLOGRAPHYPAST, PRESENT, AND FUTURE

FIG 14--1nlragranularpools o! marlenstte m the aw-( ooled material (7 5~ (a) Bb and (b) ~orre-
spondmg marten stte C D F t mage

1 A nonlamellar aggregate of fernte plus cementlte [11]


2 A lath or plate-hke ferrltlc product that forms by shear [12]

At th~s point, ~t should be pointed out that, in the present investigation, mlcrostructures slm-
dar to that presented in Figs 13 and 14 have not been found in either the HAZ or the quenched
base plate This again reinforces our claim that these latter regions are predominantly lath mar-
tensltlc together wxth retained austenlte as the second phase constituent

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VARUGHESE AND HOWELL ON EXAMINATION OF STEEL ALLOYS 211

Conclusions
The major findings of the present investigations are as follows

1 The coarse-grained HAZ transforms to a coarse lath martenslte during coohng. Austen-
lte is retained as thin interlath films
2 The quenched base plate is also compnsed of lath martenslte, but on a finer scale L~ttle
retained austemte was observed
3 No granular balmte/fernte was found in either the HAZ or the quenched base plate
4 Tempering the quenched base plate led to the development of a dispersion ofe-Cu. The
lath structure was replaced generally by a more eqmaxed ferntlc structure.
5 Granular fernte was found m the air-cooled sample We suggest that the designation,
fernte, is far more appropriate than what has been used heretofore, bamlte

Acknowledgments
The authors gratefully acknowledge the support of The Office of Naval Research Grant
Number N00014-89-J 1958

References
[1] Wilson, A D, Hamburg, E G , Colvm, D J, Thompson, S W, and Krauss, G m Mlcroalloyed
HSLA Steels (Proceedmgs Mtcroalloymg "88), Amencan Society for Metals, Metals Park, OH, 1988,
p 259
[2] Thompson, S W, Colvm, D J, and Krauss, G , Scrlpta Metallurgtca, Vol 22, 1988, p 1069
[3] Habraken, L J and Economopoulos, M m Transformatton and Hardenablhty in Steels, Chmax
Molybdenum Company, Ann Arbor, MI, 1967, p 69
[4] Bramfitt, B L and Speer, J G , Metallurgtcal TransacttonsA, Vol 21A, 1990, p 817
[5] Ohtam, H, Okugach~, S, Fujlshlro, Y, and Ohmon, Y, Metallurgical TransacUons A, Vol 21A,
1990, p 877
[6] Vander Voort, G , Metallography-Prmctples and Pracltces, McGraw-HJll, New York, 1984
[7] Honeycombe, R W K in Phase Transformations m Ferrous Alloys, A R Marder and J I Gold-
stem, Eds, The Metallurgical Sooety of the American InsUtute of Mining, Metallurgical, and Petro-
leum Engineers, Warrendale, PA, 1984, p 259
[8] Howell, P R, Ricks, R A, and Honeycombe, R W K, Journal ofMaterlals Science, Vol 15, 1980,
p 376
[9] Thomas, G , Metallurgtcal TransacttonsA, Vol 9A, 1978, p 439
[10] Wayman, C M in Phase TransformaltonsmFerrousAlloys, A R MarderandJ I Goldsteln, Eds,
The Metallurgical Sooety of the Amencan Institute of Mining, Metallurgical, and Petroleum Engi-
neers, Warrendale, PA, 1984, p 49
[11] Aaronson, H I, Reynolds, W T, Jr, Shlflet, G J, and Spanos, G , Metallurgzcal TransacttonsA,
Vol, 21A, 1990, p 1343
[12] Olson, G B, Bhadeshla, H K D H, and Cohen, M, Metallurgwal Transacttons A, Vol 21A, 1990,
p 805

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Lucille A. Giannuzzi, ~Paul R. Howell, l H o w a r d W. Pwkerlng, 1 and
William R. Bltler ~

Transmission Electron Microscopy of the


Interdiffusion Regions of Iron-Zinc Couples
REFERENCE: Glannuzzl, L A , Howell, P R , Plckenng, H W , and Bltler, W R , "Trans-
mission Electron Microscopy of the Interdiffusion Regions of Iron-Zinc Couples," Metallogra-
phy Past, Present, and Future (75th Anmversary Volume), ASTM STP 1165, G F Vander
Voort, F J Warmuth, S M Purdy, and A Szlrmae, Eds, American Sooety for Testing and
Materials, Philadelphia, 1993, pp 212-223

ABSTRACT The iron-zinc system has been studied frequently due to the fact that zinc inhibits
corrosion of the ~ron by cathodic protection However, there are discrepancies in the literature
concerning both the nature of the mtermetalhc phases that can form in Iron-zinc (Fe-Zn) alloys
and the detads of the Fe-Zn phase diagram Many of the problems that are associated with this
system can be attributed to the difficulty of prepanng homogeneous alloys of known composi-
tions because of the high vapor pressure of zinc relative to iron For many of the same reasons,
it has proved difficult to produce thin foils for examination in the transmission electron micro-
scope (TEM) from blmetalhc Fe-Zn matenals Transmission electron microscopy of the blme-
talhc Fe-Zn couple in cross sectmn ~s desirable because m~crostructural reformation by ~maglng
techniques, phase identification by dlffractmn techmques, and chemical analysis by energy &s-
perslve spectroscopy can be achieved w~th one instrument
In the present investigation, a sample preparation techmque for the production of cross-sec-
tion TEM foils of Fe-Zn couples is described in detail In an attempt to obvmte the problem
associated with the thinness of commercial Fe-Zn couples, pure Fe-Zn couples have been pro-
duced that are in excess of 3 mm m thickness These samples can be cut directly to the required
dlmensmns for thin foil preparation Electron transparency has been achieved by liquid nitrogen
ion mdllng with specimen dlmphng Prehmlnary results from the zinc side of the Fe-Zn couple
are presented The zeta (~) phase has been identzfied, and It xsbeheved that these are the first TEM
m~crographs and electron diffraction patterns ofth~s phase observed from cross-sectioned Fe-Zn
couples The mlcrostructural evolution of the n (Zn) ~ ~ + ~"~ ~"phase transitions within the
&ffUSlOn zone is discussed

KEY WORDS" transmission electron microscopy, selected area dlffractlon pattern, rt phase, ~"
phase, mn mdhng, ~ron-zme couple, metallography, metallurgical specimens, mlcrostructure,
metallographlc techmques

Recently, m u c h a t t e n t i o n has been given to the analysis o f zinc-based steel coating systems
by t r a n s m i s s i o n electron m i c r o s c o p y ( T E M ) (see for example, Refs 1 t h r o u g h 8) O b s e r v a t i o n
o f the zinc-coated steel c o u p l e in cross section by T E M (or m o r e specifically analytical electron
m i c r o s c o p y ( A E M ) ) c o u l d be a d v a n t a g e o u s because the m o r p h o l o g y , chemistry, a n d structure
o f the lnterdlffUSlOn region m a y be d e t e r m i n e d In a d d i t i o n , t h e n a t u r e o f any i n t e r m e d i a t e
phases c o u l d be d e t e r m i n e d T o f a o h t a t e later discussion, T a b l e 1 lists the i n t e r m e d i a t e phases
t h a t h a v e b e e n f o u n d to o c c u r in the i r o n - z i n c ( F e - Z n ) system [9]

Post doctoral research associate, Center for Advanced Materials and professors of Metallurgy, respec-
tively, Department of Materials Science and Engineering, The Pennsylvania State Umverslty, University
Park, PA 16802

212

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GIANNUZZl ET AL ON IRON-ZINC COUPLES 213

TABLE 1--lntermedtate phase3 m the Fe-Zn system

Approximate Composition Range


Phase Crystal Structure at 450~ (atomic % Zn)

F cubxc (bcc) 68 5 to 73 5
F~ cubic (fcc) 78 0 to 81 0
hexagonal 86 5 to 92 0
~" monochnlc 92 5 to 94 0 (FeZnj3)

However, preparation of the lnterdiffUSlOn region of an Fe-Zn couple for TEM analysis is
nontrivlal For example, a c o m m o n techmque for prepanng conventional alloys for TEM IS
twin-jet electropohshlng. However, the role of zinc is to inhibit corrosion of the iron by cath-
odic protection and, therefore, the great difference in chemical reactivity between the zinc and
iron has thus far precluded jet polishing as a viable technique. As a result, TEM sample prep-
aration of Fe-Zn couples in cross section have concentrated on the techniques of ion beam
milling [ 1-4] and ultramicrotomy [5,6]. The physical properties of zinc (for example, the high
vapor pressure of zinc relative to iron) add to the uniqueness and difficulty in preparing TEM
foils m this system For example, it has been shown that zinc is extremely sensitive to damage
induced by ion bombardment d u n n g Ion beam mllhng [1,4] In addition, previous studies in
this laboratory have suggested that Fe-Zn intermediate phases may form during ion beam mill-
ing, even when a liquid nitrogen cooling stage IS being used, due to the redeposition of sput-
tered zinc onto the iron-based substrate [2, 7,8]
A recent study in this laboratory has shown that the steel-zinc interface may be imaged by
TEM using the technique of mechanically polishing to electron transparency, however, the
steel substrate is damaged and the zinc coating is recrystalllzed [1] Subsequent 1on milling
using a hqmd nitrogen coohng stage was shown to remove the mechanically damaged region
and revealed a mlcrostructure that was consistent with the starting material Unfortunately,
the interface could not be imaged due to the faster ion milling rate of zinc with respect to iron
Therefore, it was concluded that optimum sample preparation conditions for cross-section
analysis of Fe-Zn couples must minimize the degree of mechanical polishing in order to avoid
specimen damage, and shorten ion mill times to avoid preferential thinning and ion beam
damage In the present study, the lnterdlffusion region of an Fe-Zn couple has been observed
successfully by TEM utilizing the dimpling-liquid nitrogen ion milling technique of sample
preparation

Experimental
Fe-Zn Btmetalhc Couple Producuon
In an attempt to obviate the problem associated with the thinness of commercial Fe-Zn cou-
ples, pure Fe-Zn couples have been produced that are in excess of 3 m m in thickness A thick
zinc coating was electroplated onto the iron substrate so that a sample may be cut directly to
the required dimensions for thin foil preparation
A specially prepared "pure" lron-electrogalvamzed zinc couple was prepared courtesy of C
Cheng of Inland Steel A 50-mm iron ingot was hot rolled to 12 5 mm, then to 2 54 m m The
2 54-mm sheet was then cold rolled over several passes to a final thickness of 0 75 mm. The
composition of the iron sheet is listed in Table 2 Prior to electroplatlng, the iron sheet was
degreased in acetone, followed by an alkaline electrocleaner and was then activated by a 10%
sulfuric acid (H2SO4) solution Thereafter, it was plated in a conventional zinconium sulfate
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214 METALLOGRAPHY PAST, PRESENT,AND FUTURE

TABLE 2--1mpuray content of iron sheet (ppm)

C Mn P S SI Al As T~ Sn Cu

50 < 10 90 80 160 250 20 2000 100 20

(ZnSO4) bath at a current density of 4 8 A/dm 2 (the pH was controlled between 1 2 to l 8)


The plating process was carried out over a period of 24 h To avoid surface roughness due to
dendritic growth, the surface of the zinc coating and edge of the sample were mechanically
smoothed every 30 m m d u n n g electroplatmg The ZnSO4 was added to the bath every 30 rain
to maintain the bath composition The final thickness of the zinc-coating plated onto both
sides of the iron sheet was ~ I m m ( ~ 700 g/m 2 of zinc), thereby producing a couple thickness
of ~ 3 m m

Fe-Zn Heat Treatment


The as-received Fe-Zn sheet was sliced into strips of ~ 15 m m by 50 m m using a diamond
wafenng blade Each stnp was degreased in acetone and encapsulated in Vycor tubing Zinc
powder of 99 7% p u n t y was poured into the tubing until the Fe-Zn stnp was covered com-
pletely The assembly was topped with quartz wool that acted as a heat sink d u n n g necking of
the tubing. The assembly was then evacuated to 30/Lm Hg and sealed The encapsulated Fe-
Z n couple was annealed at 450 ~ _+ 2~ for l0 min and water quenched It should be appreci-
ated that the annealing temperature is above the melting point of pure zinc (419 58~ and
was chosen to reproduce the temperature in which hot-dip galvanizing of steels occur.

T E M Sample Preparation
A specimen for TEM analysis was prepared in the following manner The heat-treated Fe-
Z n couple was sliced m cross section to a thickness of ~ 1 m m using a diamond wafenng blade
The thickness was reduced further to ~ 100 um by grinding on sdicon-carbide (SIC) papers
with lapping od as a lubricant The specimen was dimpled in the vicinity of the interdiffuslon
region to < 5 ~m in thickness using 6-urn and 1-1zm diamond paste The specimen was
trimmed to a diameter suitable for TEM examination ( ~ 3 ram) Final TEM thinning was
achieved by ion milling with a liqmd nitrogen cooling stage until the Fe-Zn interface was per-
forated The couple was positioned inside the ion mill such that the argon beams were per-
pendicular to the interface for the majority of the milling time A light optical micrograph of
the perforated speomen is shown in Fig l Note that the thickness of the diffusion zone (DZ),
which is ~ 4 0 #m, is visible due to the ion milling procedure Note also that the perforation is
w~thm the diffusion zone on the zinc side of the couple, and, therefore, mlcrostructural infor-
mation by TEM on the iron side of the couple was not attainable The labels, a, b, c, and d,
around the perforation represent the approximate locations m which TEM analyses were per-
formed Position a is located in the zinc coating, and positions b, c, and d are points within the
diffusion zone that progress toward the iron-nch side Reference to these positions will be
made in the following section There is also evidence of pores (P) within the thick zinc coating
that may be due to the collapse of as-plated dendrites d u n n g the annealing operation. The
feature labeled T is a trench formed in the couple due to the direction of ion milling as
described earlier The specimen was examined in a Phlhps EM420T operating at 120 kV

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GIANNUZZl ET AL ON IRON-ZINC COUPLES 215

FIG 1--4 ~ro.~~-~ectmn hght optical rm~ rograph o/an Fe-Zn couple annealed at 450~ ]or 10 mm a[ter
dimpling and ton mllhng with a hqmd mtrogen cooling ~mge (see text/or the lull de~ rlptlon)

Results and Discussion


Fzgure 2a is a bright field (BF) mlcrograph of the zinc-rich eta phase (~), and Fig 2b is a
[0001] selected area diffraction pattern (SADP) from the region shown in Fig 2a Confirma-
tion of the indexing scheme is provided m the computer-generated pattern obtained in Fig 2c
Note the extended dislocations in Fig 2a that may have formed as a result of sample prepa-
ration The diffusion zone width and locations of the TEM analyses shown in Fig 1 are
approximate Nevertheless, the relative positions of the TEM images within the diffusion zone
will be mentioned to emphasize phase boundary transitions Figure 2a was imaged from Loca-
tion a in Fig 1
Figures 3 through 5 present micrographs dlustratlng vanous features of second-phase par-
tlcles (Figs 3a, 4a, and 5a), corresponding SADPs (Figs 3b, 4b, and 5b) and computer-gen-
erated patterns (F~gs 3c, 4c, and 5c) taken from each region The diffraction patterns index
consistently with the monochnIc Fe-Zn zeta (~-)phase The SADPs were indexed by companng
d-spacings and diffraction patterns obtained by computer simulation. The complexity of cal-
culating electron diffraction patterns from the ~"phase (as well as other complex crystal struc-
tures) is greatly diminished by employing computer calculations The computer simulations
m F~gs 3c, 4c, and 5c were generated using a = 1 086 nm, b = 0 761 nm, c = 0.506 nm, and
fl = 100 53 ~ [10] A base-centered monochnlc lattice was defined (that is, atom locations at
(0,0,0) and (0 5,0 5,0)) to yield matching extinctions of reflections present between the actual
and computed SADPs The indexing scheme reported in h g s 3c, 4c, and 5c are therefore con-
Slstent with the preceding crystallographic data Ftgure 3c indexes to [101], F~g 4c to [010],
and Fig 5c to [ 121 ] Figures 3a and 5a were imaged from Location d, and Fig 4a was imaged
from Location c m Fig 1 To our knowledge, these are the first published TEM ~mages and
electron dlffracUon patterns of the ~"phase obtained from cross-sectioned Fe-Zn couples
The ~"phase may appear as a d~screte particle within the )7 matrix ( ~ 0 . 5 to 1 ~m) as shown
by the example given m Fig 6 (Location b, Fig 1), as particles that have coalesced (F~g 4a),
or as larger single-crystal grains (Fig 5a), depending on the location within the diffusion zone
Thus far, it has been shown that, in general, as the distance into the diffusion zone from the
zinc side of the Fe-Zn couple increases, the number density of the ~'phase increases The pres-
ence o f twins m the f phase has been confirmed by electron d~ffraction lndwidual ~"particles

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216 METALLOGRAPHY PAST, PRESENT, AND FUTURE

FIG 2--(a) Brlght field (BF) T E M ml~rograph of the zm~-rtch ~ phas'e, (b) a [0001] selected area dtj-
fractwn pattern (SADP), and (c) computer generated pattern from the area m Ftg 2a

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GIANNUZZI ET AL ON IRON-ZINC COUPLES 217

FIG 3--(a) Centered dark ~eld (CDF) mlcrograph of the ~ phase, (b) a [ 101] SADP and (c) computer-
generated pattern fiom the area in Fig 3a

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218 METALLOGRAPHYPAST, PRESENT, AND FUTURE

FIG 4--(a) B F mlcrograph o f the ~ phase, (b) a [010] SADP, and (c) computer generatedpattern from
the area m Fig 4a

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GIANNUZZl ET AL ON IRON-ZINC COUPLES 219

FIG 5--(a) BF mzcrograph of the ~phase, (b) a [121] SADP, and (c) computer-generated pattern from
the area tn Ftg 5a

and the coalesced ~"region may contain twins, however, addmonal analyses are needed to
determme whether the various features m F~gs 3a and 5a are possible twins, stacking faults,
or antlphase boundaries Figures 7a and b are a BF and centered dark field (CDF) mlcrograph
of the same region Centered dark field imaging is useful for determining regions that have
s~mllar orlentaUons The usefulness of the C D F image is illustrated m Fig 7b where the large-
grained r/matrix appears bright due to virtually ~denucal orientation The particles are con-
tanned within a smgle zinc-rich ~ gram as illustrated by the contrast m Figs 7a and b, and the
single crystal [2110] SADP from the ~ region The computer-generated indexed SADP for Fig
7c is shown m Fig 7d The lower magmficatlon C D F image of Fig 8 again illustrates the single
crystal nature of the zinc-rich 7/matrix, individual ~"particles, and the onset of ~"parhcle coales-
cence Note again that in the C D F mlcrograph of Fig 8 the single crystal orientation of the 7/

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220 METALLOGRAPHYPAST, PRESENT, AND FUTURE

FIG 6 - - B P lrnage o/an isolated f phas'e parttde wtthm the o matrix

phase is emphasized by the relatively uniform image intensity Conversely, the particles m the
CDF mlcrographs appear dark Figures 7a, 7b, and 8 were imaged from Location b in Fig 1
A schematic diagram for the mlcrostructural evolution of the n ---"n + ~'~ ~'phase transition
Is illustrated in Fig 9 and described in the ensuing text Figure 9a begins with a large single
crystal zinc-rich n matrix (compare with Fig 2a) At the beginning of the diffusion zone (on
the zinc side of the Fe-Zn couple) isolated ~"particles probably nucleate within the liquid (L)
phase (which, upon coohng, transforms to the solid ~ phase see Fig 9b and Figs 6,7a,7b, and
8) As the distance into the diffusion zone increases, the volume fraction of the ~ phase in the
two-phase region (L + ~') increases by additional particle nucleation and pre-existing particle
growth Upon cooling, (L + ~') transforms to (n + ~) In addition, the onset of particle coales-
cence also takes place (compare Fig 9c with Figs 4a, 7a, 7b, and 8) Finally, complete particle
coalescence is attained (Fig 9 d a n d Fig 5a) and the single phase ~'reglon is produced contain-
ing defects that definitely include twins, and may contain stacking faults, and antlphase
boundaries Figures 9a through 9d can be correlated with positions within the diffusion zone
shown by Locations a through d m Fig 1

Conclusions
A successful TEM sample preparation techmque for the analysis of the mterdiffuslon region
of Fe-Zn couples, has been described. It is believed that the first TEM images and electron
diffraction patterns of the ~"phase from cross-sectioned Fe-Zn couples have been presented in
this paper Additional research is needed to fully characterize the defects present m the ~"phase
A schematic diagram for the mtcrostructural evolution of the reaction ~ ~ n + ~"~ ~"has been
provided

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GIANNUZZI ET AL ON IRON-ZINC COUPLES 221

<b

T~

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222 METALLOGRAPHYPAST, PRESENT, AND FUTURE

FIG 8--Lower magnlhca[mn BF tmage show'mgthe dlstrlbutmn of ~fparttdes wzthm the. matrix and
the on sel o/~ partl~le ~oale~scence

Acknowledgment
The Fe-Zn couple was prepared courtesy ofC Cheng, Inland Steel This research was sup-
ported by the American Electroplaters and Surface Finishers Society Research Project No 76
and Inland Steel Corporation

References
[1] Glannuzzl. L A, Howell, P R, Plckenng, H W, and B~tler, W R, Proceedings, SUR/FIN '91.
American Electroplaters and Surface Finishers Socwty, Toronto. 1991, to be pubhshed
[2] Glannuzzl. L A, Howell, P R, lhckermg, H W, and Bltler, W R m Zinc-Based Steel Coating
Systems Metallurgy and Performance, G Krauss and D K Matlock, Eds, The MetallurgacalSoci-
ety of the American InsUtute of Mining, Metallurgacal.and Petroleum Engineers, Warrendale. PA,
1990, p 121
[3] Chen. Y L and Snyder, D D m Zmc-Based Steel Coating Systems Metallurgy and Performance,
G Krauss and D K Matlock. Eds. The MetallurgacalSociety of the American Institute of Mining,
Metallurgical, and Petroleum Engineers, Warrendale, PA, 1990, p 95
[4] Lm, Y, Pak. S -W, and Meshn, M m Zmc-Based Steel Coating Systems Metallurgy and Perfor-
mance, G Krauss and D K Matlock, Eds. The Metallur~cal Society of the Amencan Institute of
Mining, Metallurgical. and Petroleum Engineers, Warrendale, PA, 1990, p 109
[5] Drewlen, C A, Ackland, D, and Marder, A R m Zinc-Based Steel Coatmg Systems Metallurgy
and Performance, G Krauss and D K Matlock, Eds. The Metallur~cal Society of the American
Institute of Mining, Metallurgical, and Petroleum Engineers, Warrendale. PA, 1990, p 31
[6] Takahashl, A, Mlyoshl, Y. and Hada. T m Zinc-Based Steel Coating Systems Metallurgy and
Performance, G Krauss and D K Matlock, Eds, The Metallurgical Society of the American Insti-
tute of Mining, Metallurgical, and Petroleum Engineers, Warrendale, PA, 1990, p 83

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GIANNUZZI ET AL. ON IRON-ZINC COUPLES 223

FIG. 9---A schematic diagram of the microstructural evolution of the n ~ n + ~ ~ ~phase transition
(see text for full description).

[7] Giannuzzi, L. A., Howell, P. R., Picketing, H. W., and Bitler, W. R., Proceedings, SUR/FIN '90,
American Electroplaters and Surface Finishers Society, Boston, 1990, p. 381.
[8] Giannuzzi, L. A., Howell, P. R., Pickering, H. W., and Bitler, W. R., Microstructural Science, Vol.
19, to be published.
[9] Kubaschewski, O., Iron-Binary Phase Diagrams, Springer-Verlag, Berlin, 1982, p. 173.
[10] Gellings, P. J., de Blee, E. W., and Gierman, G., ZeitschrifteJfirMetallkunde, Vol. 70, 1979, p. 315.

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James Hillier I

Some Reflections on the Early Development of


Electron Microscopy and Microanalysis
REFERENCE: Hllher, J, "Some Reflections on the Early Development of Electron Microscopy
and Microanalysis," Metallography Past, Present, and Future (75th Anntversary Volume),
ASTMSTP 1165, G F Vander Voort, F J Warmuth, S M Purdy, and A Szirmae, Eds, Amer-
ican Society for Testing and Matenals, Philadelphm, 1993, pp 224-232

ABSTRACT: Theoretical mathematscal physics estabhshed the posslblhty of an electron micro-


scope long before the discovery of the electron Much later, theoretical physics provided the
incentive for developing an electron microscope The reahzaUon of a working instrument had
to await the maturaUon ofa w~de spectrum of new technologies Recollections of the successes
and heartbreaks of the early days of this struggle, at the Umverslty of Toronto and then at RCA,
provide the background for some mterestmg thoughts on the importance of t~mmg and chance
in such developments In the middle 1930s, technologies were emerging that made the trans-
mission electron microscope possible By contrast, electron microprobe analys~s could not
become pracucal untd at least two decades later when the much more demanding technologies
reqmred had been developed

KEY WORDS" electron m~croscope, electron microprobe analysis, transmission, h~story, tech-
nological infrastructure, metallography, metallurgical speomens, mlcrostructure, metallo-
graphic techmques

In a s y m p o s m m celebrating the 75th Anniversary o f the formation o f the A S T M C o m m i t t e e


E4 on Metallography, it is very appropriate to have a discussion of the early days o f an instru-
m e n t as significant as the transmission electron microscope (TEM) It is also appropriate to
give s o m e thought as to the helpful impact our past experiences might have on the evolution
and d e v e l o p m e n t o f future instrumentation The period I shall be discussing will be the decade
from 1935 to 1945 T h a t is about two-thirds of the way back to the origin of C o m m i t t e e E4
and safely beyond the reach of most o f your m e m o r i e s
It was a most exciting, even spectacular, decade during which a remarkably small group of
researchers scattered around Europe and North America, took the magneuc T E M from a
rather quiescent, theorettcal concept to a reasonably rehable, practical instrument in senal
p r o d u c u o n . In the s a m e period, this group took the resolving power from a doubtful third of
a m~crometre to a routine resolving power o f ten n a n o m e t r e s and, in the hands of experts, to
an occasional one n a n o m e t r e In this decade, the fields of applicaUon o f the T E M were
expanded from essentially zero to almost the full range o f the hght microscope There was not
yet any way of cutting sufficiently thin sections o f biological specimens That occurred a year
or two later Color, as used so valuably in light microscopy, did not seem to have a counterpart
In electron microscopy
It ~s revealing to w o n d e r why the T E M c a m e into being in that particular decade The cor-
relaUon between the refraction o f hght rays and the action o f fields o f force on pamcles had

' Retired, RCA Corporation

224

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HtLLIER ON EARLY DEVELOPMENT OF ELECTRON MICROSCOPY 225

been elucidated by Hamilton m the middle of the nineteenth century, long before the forma-
tion of Committee E4 and long before the discovery of the electron The wave nature of the
electron and Its extremely small wavelength had been understood for more than the preceding
decade The theoretical posslbfi~ty that an electron microscope, that was the analog o f a hght
microscope could have much greater resolving power, had been qmte well accepted for several
years before the early 1930s when Knoll and Ruska attempted ~ts construcUon In my opimon,
the state of our technological infrastructure is a most sigmficant controlhng factor m the t~mmg
of the transition from a concept to a practical device. Certainly, with the TEM and m~croprobe
analys~s we have two contrasting examples of this point and, for which, my own expenences
prowde good support. (Incidentally, it IS interesting that none of the acUve workers m the field
ever claimed to have "invented" the electron microscope )

Our First Instrument


In early spnng, 1937, I was a senior about to graduate in mathematics and physics at the
University of Toronto In a discussion about my future with the assistant chairman of the
physics department, he happened to mention the electron microscope, m which, it appeared,
the chairman of the department had some interest. My curiosity was immediately aroused
That was the very first time I had encountered that particular combination of the words "elec-
tron" and "microscope." As a child, I had been very interested In microscopes and had even
made several crude light microscopes As a teenager, a high school geography teacher had
roused an interest in ham ra&o I was completely mystified as to how these two acUvltles could
be related I was intrigued and my career was launched I &d a lot of reading that summer. In
the fall, I was joined by A1 Prebus and we got some practical experience by rejuvenating a
couple of emission type microscopes that Cecd Hall had built before he left for Kodak By the
end of the year, we had reached the conclusion that the only way we could achieve resolving
powers better than a light microscope was to construct a h~gh-voltage, magnetic, transmisszon
instrument We spent the Christmas break designing our first instrument Looking back, I am
stdl amazed We designed the column and did all the critical drafting m a few eighteen-hour
days Although the general pattern of the design followed that of Knoll and Ruska, we were
on our own as far as any of the engmeenng details were concerned We made some mistakes,
but it is remarkable that the projection lens, the objecUve lens except for its polep~eces, the
specimen chamber, and the column support were never changed
Over the years, I have always been impressed by the wisdom of the chairman and the assis-
tant chmrman for allowing two very young, very brash, zealous graduates undertake such a
major project on their own Recall, at the beginning of 1938, the country was still m the throes
of the Great Depression and the physics department was seriously strapped for funds The
chairman and his assistant were faced with a Hobson's choice Should they try to support a
large project in an impossibly austere environment or should they risk deflating two enthusi-
asUc graduate students who just might make a breakthrough It is to their credit that they
approved the project even though it was rather clear that, for the most part, we were going to
have to shift for ourselves
The only assistance available to us was that of the part-time efforts of a glassblower and of
the most recent addition to the machine s h o p - - a fellow whose prior employment was In a
locomotive repair shop v That shook us up but, actually, became one of the more fortunate
things that happened to us Fred was a delight at precision machining of very large pieces, but
anything that needed more than one part per inch completely confounded him Prebus and I
quickly realized that If the more complicated, delicate parts of our instrument were going to
be made, we were going to have to learn to do the machining ourselves That we did In later

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226 METALLOGRAPHYPAST, PRESENT, AND FUTURE

years, for me at least, that experience was invaluable The many late hours I had spent m the
machine shop paid offhandsomely, primarily through the great advantage It gave me m com-
mumcatmg with instrument makers and machlmsts
So much for setting the scene Let us take a quick look at the technology we had avadable
then
By today's standards, the most laughable was the vacuum technology Except, to us, It was
very serious business The hagh-vacuum pump was a hand-blown glass mercury diffusion
pump, the largest that our glassblower could make We never really knew how fast ~t pumped
We estimated it to be somewhat under one htre per second The d~ffus~on pump was backed
by a small mechamcal pump Then, there was a maze of glass tubing and ground glass stop-
cocks that enabled us to bypass the mercury pump for the anatlal pumping of the instrument
Our vacuum gage was a monstrosity called a McLeod gage that gave us lots of physical exercise
but not more than one measurement per minute
That first instrument was a stack of lenses, tubes, a camera, an object chamber, and an elec-
tron gun Each piece was ahgned by shdmg it transversely relative to the group of segments
below it These junctaons were made vacuum taght by painstakingly hand lapping the shdmg
surfaces and seahng them with a special grease that we concocted ourselves. We spent many
hours surnng pure gum rubber very slowly into a pot of melted Vasehne In addmon to the
plane surfaces between segments, there were a number of lapped comcal plugs that provaded
access to the inside of our instrument
Our electrical components were equally primitive. The current supply to our lenses was sam-
ply a well-charged group of automobde batteries connected through large laboratory shdmg
variable resistors We d~d have a carcmt that prowded coarse, fine, and very fine adjustments
We also, very fortunately, had designed water-cooling into our lens coil structures to reduce
the thermal vanataons. However, they still took long periods to stabdlze Our hagh-voltage sup-
ply was an unbehevable concoction of parts that we scrounged from various nooks and cran-
rues around the physics department. It consisted of a very large 50 kV transformer, a mercury
vapor rectifier tube, and a filter capacitor made of glass plates and a l u m i n u m foal The only
place where one could possibly see anything comparable today would be m a very old Frank-
enstem mowe. Miraculously, ~t worked, although not very well. It turned out that the most
sophisticated ptece ofeqmpment, the mercury vapor rectafier tube, had a finng voltage with a
mind of ats own with vanataons that could not be smoothed out by our low-capacaty filter
system
In the design of our instrument, our most spectacular fadure was our camera. Recogmzmg
the slowness of our vacuum system and unaware of what problems we were going to encoun-
ter, we opted for a multiple exposure film camera Unfortunately, ~t took forever for the film
to outgas and when we d~d get adequate vacuum, any attempt to roll the film caused it to
fragment into a bunch of plastac shvers in the bottom of the camera

Applications Expand
In spite of these and many other problems, the instrument began to show promise and, as
~t d~d, some support began to dribble m from various Interested organizations.
It seems incomprehensible m today's world that, m the maddle th~rtaes, a few lndlwduais
were exerting enormous individual effort to develop a hlgh-resolutaon electron macroscope,
when the only type of specimen they were sure they could examine was no more exotic than
the cutting edge of a razor blade It was generally assumed that the contrast m an electron
image would be produced by the absorption of electrons m the specimen and, therefore, the
intensity reqmred to make a highly magmfied amage useful would immediately destroy any
but the most refractory specamen. Obviously, our dedlcataon had to be related to the challenge

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HILLIER ON EARLY DEVELOPMENT OF ELECTRON MICROSCOPY 227

of achieving increased resolving power, rather than the ultimate, general utdity of the instru-
ment In mid-1938, just as we were beginning to get some promising pictures, we became
aware of Marton's 1937 paper in which he demonstrated that a sufficiently thin, suspended
film of collodion was not destroyed by the electron beam and could be the counterpart o f the
hght microscope shde It became apparent that differential scattering of electrons without
absorpUon could provide adequate contrast for the formation of an image Immediately, the
entire field of very fine particles (paint pigments, colloids, bacteria, viruses, etc.) was opened
up and the future o f the TEM as a useful instrument was assured

On to Serial Production

As we refined the Toronto instrument and our useful pictures became more frequent, our
reputation began to spread and we had more and more requests for micrographs of materials
of interest to an ever-widening spectrum of organizations. It became obvious that a homemade
"stnng and sealing wax" instrument in a university laboratory could not possibly meet the
demand As a result, in February 1940, I found myself at RCA designing a commercial version
of the Toronto instrument I also became aware that the technological infrastructure m the
electromcs industry was coming together rapidly and was far ahead of the university
We now had 50-htre-per-second oil diffusion pumps and continuously reading vacuum
gages We could achieve rapid demountabihty with synthetic rubber gaskets and O-nngs
instead of ground grease joints We had vacuum-tight flexible metal bellows that gave us new
freedom in deslgmng a means of manipulating within a vacuum chamber I am sure some high
vacuum technologists are cringing as I list these developments I can appreciate your reaction
now, but please recognize that they were miracles to us in 1940
On the electrical side, we moved into the electronics age with the newly developed, preci-
sion, self-regulating, high-voltage supplies and regulated current supplies that completely elim-
inated the need for cooling the lens coils.
All these, and other developments, speeded our work by at least an order of magnitude,
possibly much more If you think about that for a moment, you begin to realize that such
numbers practically guarantee the historical coincidence of the development of enabling tech-
nology and the emergence of a major new development However, it is interesting to note some
other changes between 1940 and today
The group I had assisting me at RCA consisted of an electrical engineer, a mechanical engi-
neer, one electronic technician, and access to the development fabrication shop. In just four
months, we designed, built and debugged what became the RCA Model EMB instrument to
the point where we were getting a resolution of around ten nanometres The total cost to RCA
was slightly over l0 000 1940 dollars. That would be between one and two hundred thousand
1991 dollars. Given the bureaucratic, environmental, and safety requirements in today's
world, I suspect that today, it would take several times as long and at least an order of mag-
nitude more money
An interesting sidelight is that, when he hired me to do this job, Dr Zworykm did not tell
me that he did not have any budget to support my work He was gambling on my having the
Instrument built before the accountants caught up with him. He won They did catch up with
him, but not untd six months after I was hired and two months after the instrument was work-
mg quite well Typically, he balanced his budget by selling my developmental model to the
American Cyanamid laboratories. If this were happening today, I am sure that Dr. Zworykin
would find a way to bypass the llmltaUons of a computerized, short-term financial control
system One factor in Dr. Zworykln's greatness was his abdlty to remove irrelevant obstacles
from his workers' projects.

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228 METALLOGRAPHYPAST, PRESENT, AND FUTURE

The Pattern of Progress


In 1940, the technological mfrastructure that supported the design and constructmn of
TEMs was becoming avadable, but we were stdl almost two orders of magmtude from the
theorettcal hmlt of our spectfic design Unfortunately, the mstrumentatton needed to analyze
the limits of performance of the then current TEMs did not exist Before 1940, few of us appre-
crated how many external and internal factors were capable of disturbing the TEM image, or
the h~gh sensitivity of the images to those factors Ulttmately, the instruments themselves,
being the only devices with sufficient sensmvlty, had to become the means for detecting and
measunng the effects of the many techmcal problems that existed in those early instruments
The read-out was, of course, the nature and degree o f b l u m n g of the recorded image Because
of the low intensity of the visual images m those days, the necessary sensmwty was achievable
only m the recorded image and not m real time Not only was the read-out very ambtguous,
but ~t related only to those dtsturbances that happened to occur dunng the exposure interval
and, for which, we had no independent means of sensing. For example, the effect of a thermal
drift of the specimen, which represented a real physical movement of the specimen dunng the
exposure, was mdJstmgmshable from the motion of the image caused by an insulating parhcle
of material situated near the beam path As scattered electrons collect on such a particle, ~ts
potentml ts slowly rinsed causing the beam to be deflected slowly dunng the exposure Slmt-
iarly, the effect of a transient mechamcal vibrat~on that happened to occur dunng the exposure
could be lndlstlngmshable from the effect of a small transverse a-c magnetic field that was leak-
mg into the path of the beam In addition, it even took a very experienced eye to d~stmgmsh
between the effects of these two sets of examples
Thus, the development and refinement of the TEM became an unending repetmve series of
proposed hypotheses followed by the design of experimental tests and then, by the actual tests
Because of the erratic vanablhty of many of the defects, their large number, and of the absence
of real time observations, the successful ~dentlficatlon and removal of one defect rarely gave
an unequivocal signal that anything had happened However, there is another side to th~s coin
As it turned out, it was the same erratic vanabihty that prevented the process from becoming
completely discouraging As we were making thousands of exposures, m our struggle to
achieve consistent results at, say ten nanometres, there was always the unexpected exposure
that showed a resolving power several times better These were the mtcrographs that were pub-
hshed but, more ~mportantly, they were the teasers that kept telling us that it could be done
and gave us the incentive to continue
It is interesting to note that by 1943 the number of defects stdl present had been whittled
down to the point where identifying and removing the remaining ones became relattvely sim-
ple As a result, some spectacular improvements m resolving power were made qmckly and
easdy. It was this phenomenon that allowed the ~mphcit astigmatism of our magnetic objec-
tives to emerge from the masking effects of other problems and successfully be corrected by
the development of the shgmator
Using very small round holes m a collodion membrane as our test objects, it became clear
that we had some astigmatism m our objectives and that ~t was a relatively constant charac-
teristic of each set of objechve pole-pteces. Our first assumption was that the alignment of the
two poles was ~mpreclse We tried lapping the openings m the assembled pole-p~eces with
interesting results Sometimes, the pole-piece tmproved and sometimes, it got worse Because
none o f the best pole-p~eces was perfect, we tried contmmng the lapping We were surprised
to find that continued lapping, ultimately, always made a pole-piece worse We began to reahze
that the astigmattsm was due to the relative coarseness of the gram structure of the tron and,
frequently, due to mclustons of nonmagnettc ~mpuntles We then went through the exercise

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HILLIER ON EARLY DEVELOPMENT OF ELECTRON MICROSCOPY 229

of searching for better iron and better anneahng processes We had no success and became
quite frustrated
Then came the " e u r e k a " Late one night, I suddenly realized that if some very small defect
in the iron could pull the magnetic field askew, I should be able to find a way of introducing a
compensating defect that would pull it back This concept was exactly analogous to correcting
the astigmatism in an eye by adding a compensating amount of astigmatism m a spectacle lens
but the practical approach was equivalent to correcting the shape of the lens m our eye by
applying pressure or tension at evenly-spaced points around its periphery Early the next
morning, I had my machinst make some soft iron screws from (believe it or not) ordinary
welding rod He then threaded eight of them into the pole-p~ece spacer so that they pointed at
the axis of the lens and could be adjusted in or out It took a few hours to learn how to adjust
the screws to remove the astigmatism Nevertheless, w~thln 24 hours from conceiving the idea,
we were getting consistent results at about one nanometre that represented approximately an
order of magnitude improvement in average performance from the day before
IfI have a message In this part of my paper, it is to note that the great bulk of the work that
brought the TEM into being as a most useful tool for science and technology, had little if any-
thing to do with the basic theory o f the electron microscope. This leads to the observation that,
through some form of accepted scientific snobbery, of which I was as guilty as anyone, only
positive end results were ever published Reports of the tedious background work that led to
the achievement and details of the blind alleys that were encountered, remained buned m lab-
oratory notebooks There was much word-of-mouth exchange of such Information among the
early workers However, [ feel that our behavior condemned many newcomers, particularly
internationally, to repeating most of our research and many, if not all, of our mistakes.
In spite of the problems, the TEM did become useful and started providing essential infor-
mation to an expanding universe of research disclphnes, sometimes m spectacular and unex-
pected ways. Without question, some of the more interesting developments were attempts to
apply the electron microscope to metallography Theory clearly indicated that the fundamen-
tal interactions between electrons and solid surfaces would prevent the electronic analog of a
light metallograph~c microscope from providing any useful results In view of the fact that the
main stream of the research at RCA was the development of television, it was quite natural
for us to consider a scanning system for metallurgical specimens. When we &d, it became clear
that a scanning system would circumvent most of the difficulties we expected In the &rect
imaging approach Thus, in 1941, we embarked on building a scanning electron microscope
We did succeed in building such an instrument and in obtaining a few pictures However, it
became painfully clear that the technology of the early forties was far from adequate for our
objectives. Even so, we probably would have continued to pursue the scanning approach if we
had not learned of Mahl's success m applying the TEM to metallography by his brilliant use
ofrephca techniques We concluded, probably correctly, that we could achieve more of value
by devoting all our efforts to the development of the TEM and its applications

The Value of the TEM in Research


Let us examine, in a little more detail, what the TEM can do for research even when
restricted to revealing only the geometry of structures. There is an i n o d e n t that sticks in my
memory as a particularly significant demonstration of this role of the TEM and as one of the
building blocks of my own understanding In the late summer in 1940, we had the first devel-
opmental model of the RCA model EMB working in my laboratory in Camden We received
a call from Dr Wendell Stanley asking if it would be possible to take a look at one of his

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230 METALLOGRAPHYPAST, PRESENT,AND FUTURE

tobacco mosaic virus (TMV) preparations Dr Stanley had spent most of his professional
career, to that point, working on plant viruses at the Rockefeller Institute Laboratories that
were then located in Princeton, New Jersey Later, he received a Nobel Prize for his work on
the ~dentificatlon and characterization of plant viruses
We agreed to take a look and within an hour after he arrived we had a spectacular picture
of his wrus, clearly showing the characteristic rods with precisely the dimensions he had pre-
dicted In minutes we had "confirmed" what had taken Dr Stanley and his group many years
to determine by uhhzlng such indirect techniques as low-angle X-ray scattering, ultracentri-
fuglng, blrefrmgence optical studies, etc Please note that I used the word " c o n f i r m e d " This
spectacular confirmahon of Dr Stanley's work is only one indicator of the value of the TEM
It is more illuminating to consider what the scenario might have been if the TEM had been
available at the time Dr Stanley was just starting his work He had discovered that the infec-
tious agent that caused the tobacco mosaic disease could pass through an unbehevably fine
porcelain filter If he had had a TEM available, he undoubtedly would have examined speo-
mens of the filtered jmces from healthy and infected plants HIs attenUon would have been
attracted by the presence o f very uniform rods as the only ahen structures m the jmces from
the infected plants Note that the presence of the rods m only the infected speomens would
have been strongly suggestive but, by itself, would have proven nothing However, starting
with the TEM observation, showing that the rods were actually the infectious agent would have
been a rather straightforward and relatively simple procedure There is an important, but inad-
equately apprecmted aspect buried in this alternative scenario The enormous ~mprovement
that could have occurred in the effioency of Dr Stanley's research, if he had had a TEM at the
beginning, would have been the result of what the TEM did "not" show, as much as of what
it did show Without TEM lmages, all the possible slzes and shapes the virusmlght have, would
have to be investigated before the characterization of the virus could be narrowed
Th~s digression shows that the TEM had, and probably still has, two basic funcUons The
first is to make ws~ble "submicroscopic" geometrical structures that have significance in an
ongoing research project The second is to increase the efficiency of a research program greatly
by slgmficantly reducing the number of possible geometrical structures that might have rele-
vance to the research and for which appropriate hypotheses and tests would otherwise have to
be devised

On to Electron Microprobe Analysis


From the beginning of our understanding of the research role of the TEM, it was appreciated
that if we could, by some means, attach some point-by-point chemical information to the
geometries revealed, we would add a whole new dimension to the utility of the instrument
Staining with heavy metal compounds became useful for enhancing the contrast in images of
organic materials Unfortunately, these had very little of the specificity of the stares used m
light microscopy
There was a flurry ofachvlty in our laboratory to explore the potential of electron diffraction
as a means of ldenUfying the chemical composition of individual small particles and struc-
tures We built a probe-type electron diffraction camera that enabled us to obtain patterns
from selected particles in TEM specimens Although it was an Interesting project, it quickly
became clear that the approach had such limited application that it was not possible to justify
any development of the necessary instrumentation It was essentially worthless for very small
organic structures Very small inorganic particles tended to be single- or near single-crystal
structures with indeterminate orientation and rarely gave adequate information for identifi-
cation While the diffraction approach was not successful, the research did have a payoff" We

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HILLIER ON EARLY DEVELOPMENT OF ELECTRON MICROSCOPY 231

acquired invaluable experience in the design and operation of an electron probe type of
instrument
Some time around the beginning of 1943, I was browsing in the library and ran across an
article by G R u t h e m a n n in Naturwtssenschafien, the German counterpart of the British pub-
hcatlon, Nature R u t h e m a n n wanted to show experimentally that when an electron excited a
certain X-ray level in a target, it lost precisely the energy required for the excitation The exper-
iment required a target so thin that the transmitted electrons would experience not more than
one inelastic collision He chose a collodion film and showed that the discrete energy losses
caused by the excitation of the K-levels of carbon, nitrogen, and oxygen produced the pre-
dicted peaks in the velocity distribution of the electrons in the transmitted beam
Reading that article was an interesting experience in how the h u m a n mind works Even
though R u t h e m a n n was interested only In the basic physics, his article triggered recognition
that his experiment could be used for analysis and that, with the use of an electron microprobe,
might solve the chemical analysis problem in our TEM specimens Interestingly, the complete
design of our first instrument popped into my mind simultaneously with the recognition of
the possibdities I was also amused at my obvious stupidity when I realized that I had been
thoroughly familiar with all the physics involved since my undergraduate days
We quickly constructed a 180* magnetic electron spectrometer that we added to one of the
probe instruments used in our diffraction experiments We confirmed Ruthemann's results
using much higher voltage electrons and even extended them to some other light elements We
also did some work with a crystal X-ray spectrometer to detect the characteristic X-rays emit-
ted from a very small area of the specimen All of this was very good research that we pursued
very enthusiastically Unfortunately, our enthusiasm began to wane as we realized that, once
again, our concepts were running far ahead of the technologies needed for their routine
application
There were many problems, but three were particularly intractable The first and most
annoying was the very rapid build-up of contamination at the point where the probe was
focussed on the specimen As a result, when we tried to analyze a very minute particle, the
contamination caused the specimen to become opaque in less time than was required for an
adequate photographic exposure to record the spectrum The second was the cumbersome
nature of the state of the art of techniques for making quantitative measurements of X-ray or
electron intensities from photographic exposures If you have gone through the exercise of cal-
ibrating the exposure on a photographic emulsion, standardizing the development of the pho-
tographic material, and then running It through a recording mlcrophotometer, you will appre-
ciate what I am saying Moreover, all that technology was invalidated essentially by the rapidly
changing situation occurring during the exposure, as a result of the contamination problem
The third was the nature of our probe system, which could become very tedious in routine use
It was almost three decades before all the technologies required to make microprobe analysis
reasonably practical, came together These involved some major developments, such as very
high resolution scanning transmission electron microscopes, very small, fast, and Inexpensive
computers, a broad range of very sensitive sensors for direct detection and measurement of X-
ray or electron intensities, and, finally, the development of instruments with ultrahigh vacuum
systems The stories of those developments will have to be told by the individuals Involved
What we can say is that our dreams of the early forties are now being realized

Conclusion
In this very br~efblt of nostalgia, there are many pieces of information regarding the creative
process that lead to significant discoveries There is the important role of pure chance in the

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232 METALLOGRAPHYPAST, PRESENT,AND FUTURE

creative process and the need to have one's mind prepared to recognize and take advantage of
opportunities when they happen to emerge There is the relationship between the state of the
technological infrastructure and what is necessary to transform a theoretical concept into a
successful practical system Finally, there is the obvious desirability, if not necessity, of broad-
ening one's experience as widely as possible outside the limited requirements of one's imme-
diate projects

Bibliography
Rather than overload this somewhat philosophical article with a very long list of only slightly
relevant references, the author concluded that the interested reader would be better served if
he or she were directed to two monographs that cover the technical developments of the period
m much greater detail and provide all the significant references with a much better indication
of what each contains. These are:

1. Zworykm, V K , Morton, G A , Ramberg, E G , Hilher, J., and Vance, A W , Electron


Optics and the Electron Microscope, Wiley, New York, 1945, and
2. Hall, C. E., Introduction to Electron Microscopy, McGraw-Hall, New York, 1953

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Quantitative Metallography

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Daniel B. Fowler 1

Quantitative Metallography in Test Method


Standards and Product Specifications
REFERENCE" Fowler, D B, "Quantitative Metallography in Test Method Standards and
Product Specifications," Metallography Past, Present, and Future (75th Anmversary Volume),
ASTMSTPl165, G F Vander Voort, F J Warmuth, S M Purdy, and A Szirmae, Eds, Amer-
ican Society for Testing and Materials, Philadelphia, 1993, pp 235-242

ABSTRACT: Quantitative metallographlc and stereologlcal methods can be applied to micro-


structures observed with the light microscope These methods, however, are not presently
requested by product specifications, except in a few notable cases For the most part, manually
performed chart comparison methods, developed 50 to 60 years ago, are still specified
Most laboratories that rely upon chart methods utilize poorly controlled metallographlc pro-
cedures for specimen preparation Image analysis using specimens prepared by these processes
yield erratic, inaccurate and nonreproduclble test results Of course, this is attributed usually to
the measurement method and equipment rather than to the specimen preparation procedures
and their execution
Specimen preparation, however, can be performed in a controlled, efficient manner with
highly automated equipment Image analysis measurements using specimens prepared with such
equipment are accurate, precise, and reproducible However, product specifications have not
been updated to incorporate this new technology In our quest for greater product quality, these
methods are essential

KEY WORDS: quantitative metallography, stereologlcal methods, light microscope, testing,


product specifications, standards, metallography, metallurgmal specimens, microstructure,
metallographlc techniques

Although there are now a few test method standards that descnbe quantitative metallo-
graphic methods, performed manually or by automatic image analysis, few product standards
specify use of quantitative test methods These product standards still specify mlcrostructural
analysis, for the most part, according to s~mple comparison chart methods, performed man-
ually Many o f these methods have been used for 50 to 60 years.
Specification writers appear to be reluctant to adopt these new, more rigorous methods
Partly, this can be attnbuted to the natural resistance to change or to ignorance of these new
methods Some will state that the current methods are "good enough" and that these new
methods will be more costly The quality of image analysis results is influenced by the quality
of specimen preparation A c o m m o n misconception is that poorly controlled preparation pro-
cedures produce acceptable results using the existing chart methods However, if the same
poor preparation practices are applied to structures measured by image analysis, results are
imprecise and inconsistent O f course, this is incorrectly attributed to the measurement equip-
ment rather than the preparation methods
Substantial progress has been made over the past 20 years in gaining an understanding of
the specimen preparation process Moreover, this knowledge has been incorporated into
highly automated equipment This equipment consistently produces properly prepared spec-

J Analytical products manager, Struers, Inc, Westlake, OH 44145

235

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236 METALLOGRAPHYPAST, PRESENT,AND FUTURE

imens and at a lower unit cost Many laboratories have obtained such equipment With prop-
erly prepared specimens, good quantitative test method standards and a properly programmed
image analyzer, accurate, precise, reproducible microstructural measurements can be made.
However, product standards must speofy the use of these methods Otherwise, they will not
be used
ASTM Committee E4 on Metallography has been introducing quantitative analysis tech-
niques into their test methods Of course, the chart methods still exist, but efforts are being
made to improve them However, product specifications have not kept pace with this new
technology. They are still specifying 50 to 60 year old technology Comparison methods are
highly subjective The problems associated with developing chart methods has been well doc-
umented, for example, for assessing inclusion content [1], grain size [2], and graphite type,
size, and amount [3,4]. Regardless of the quality of the specimen preparation, comparison
methods yield less precise data than image analysis Moreover, chart method use may be
biased by the operator's desire to produce certain results
Precision instruments for sample preparation and evaluation make possible the develop-
ment of sophisticated quantitative metallographic standards. Recent developments in equip-
ment technology for mlcrostructural specimen preparation and measurement permit the
application of process control concepts to specimen preparation as well as evaluation Perhaps
more importantly, materials scientists have been working to change metallography from a
qualitative art to a quantitative science
Many existing product standards rely on visual companson test methods to determine
microstructural quality. As an industry, we can greatly improve upon these subjective stan-
dards The methods and tools needed to perform quantitative metallography efficiently are
now available What blocks the path to more scientific standards is a reluctance to accept new
ideas and methods
Consider the typical specifications and standards that exist tbr controlling the external
dimensions of a manufactured component To gage the acceptability of a part, certain meth-
ods and tools are employed Beginning w~th the design, the external dimensions of the part are
specified in a very precise way using engineering drawings The exact required dimensions
along with their corresponding allowable tolerances are given Dunng production of the part,
forming and finishing processes, such as casting, machining, and others are performed in a
highly controlled manner To determine the quality of the part, or its adherence to the speci-
fications, instruments are used to actually measure the dimensions. Whether it be a simple
caliper or more sophisticated electronic devices, the actual measurements are made and com-
pared with the dimensions given on the engineering drawings.
The demand for consistency in product quality, and the ability to measure part dimensions,
IS the basis for statistical quality control. It is difficult to imagine that the quality control of
dimensional specifications of a manufactured part could be based upon visually comparing It
to a picture in a specification book, and judging by eye whether or not the part meets the spec-
ificaUons. Yet the comparison methodology is exactly the basis for many specifications per-
taining to mlcrostructure.
The rigorous performance and environmental requirements placed upon engineered mate-
rials demand precise control of mlcrostructures Sophisticated metallographic tools and meth-
ods are readily available to meet these demands. Metallographlc preparation and evaluation
can be conducted as a manufactunng process Metallography, the controlled process, wdl yield
results that can be the basis for the product specifications and standards that are of the same
quantitative nature as those for any other manufactunng process. To do this requires the use
of tools for the precise development and measurement of mlcrostructure. All metallographic
standards should be quantitative standards. All metallographlc specifications should be based
on actual measurements o f microstructure with assessment of their statistical precision. Esti-

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FOWLER ON QUANTITATIVE METALLOGRAPHY 237

matlons and visual comparison methods are no longer needed because Instruments and meth-
ods exist that allow quantitative test methods and product specifications to be effectively
Implemented

Metallography
Metallography is based upon the long standing and continuously evolving body of evidence
that demonstrates that the internal structure of a material has a direct influence on the eng~-
neenng properties and behavior of that material In the more than 125 year history ofmetal-
lography, manual specimen preparation and visual observation techniques have been funda-
mental to the study of mlcrostrucutres of matenals In fact, one researcher has gone so far as
to state that, "optical examination of materials IS the foundation on which all of our present
understanding of the relationship between mlcrostructure and properties is based" [5] How-
ever, one of the problems in using mtcrostructure as an indicator of matenal properties is that
considerable effort is required to prepare specimens so that internal structures can be observed
Early practitioners of metallography invented and experimented with different techniques
to accomplish their goals of revealing mlcrostructure As In any new endeavor, there were no
established standard methods and the ploneenng individuals developed their own styles for
the solution of problems In tracing the history of technology, the early successes were based
upon the skills of individual artisans [6, 7] Similarly, the concept of metallographlc specimen
preparation as art can be traced to the association of individual talents with successful prepa-
ration methods [8] Today, there exists an enormous body of knowledge concerning applied
metallography There are many accomplished metallographers and several excellent text-
books covenng all aspects of specimen preparation [9,10] The concept of metallography as
only an art is no longer valid today Viewing metallography merely as an art is based on the
behefthat preparation of specimens requires an individual and qualitative approach that can-
not be described precisely or performed by the unskilled or by machines.
Traditional artisan preparation is based almost exclusively on manual methods. The hand
tools used for preparing specimens did not provide mechanisms for control The objective was
the creation o f a microstructural image that met subjective, visual criteria, established empir-
ically and, perhaps, arbitrarily Under the "metallography is art" philosophy, preparation pro-
cedures such as this result " the sample should be polished extensively on the silk cloth, by
hand, using the 0 3 Alumina/distilled water slurry mixture until the voids are filled in, or no
slgn~cant improvement is noticed" [11 ]
This procedure IS qualitative, relying upon the terms "polished extensively" and "no sig-
nificant improvement" that offer little hope ofreproduclblhty or agreement This sort of ambi-
guity inevitably leads to disagreements over the correct preparation method and the true
microstructure, making mIcrostructural specimen reproduction virtually impossible A major
problem m metallographlc preparation is the difficulty in achieving reproducibility
The limitations of art-based metallography are obvious The question of correctness is not
applicable to art and, as art, the possibility of measurement is illogical and impossible Qual-
ities attributable to good art, such as originality and unique individual style, are totally unde-
sirable m metallography Conducted merely as an art, metallography cannot possibly be the
basis for standards or specifications
Now, let us consider metallography as a controlled manufacturing process Seven basic
manufacturing processes have been defined [12] These are

casting or molding,
forming or sheanng,
machining (material removal),

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238 METALLOGRAPHY PAST, PRESENT, AND FUTURE

heat treating,
finishing,
assembly, and
inspection

With these operations in mind, consider the steps in a typical metallographic specimen prep-
aratlon procedure

l sectioning (sawing, a basic machining process);


2 mounting (an example of fixtunng in order to allow for subsequent machining
operations),
3. gnndlng (abrasive machining),
4. pohshlng (abrasive machining); and
5 etching, tinting, interference layering, etc. (finishing).

It is easy to define each step in the microstructural specimen preparation sequence as a basic
manufactunng process. By defining preparation as a series of manufactunng processes, com-
posed mainly o f abrasive machining and finishing steps, then the application of manufacturing
control concepts becomes feasible Metallographlc specimen preparation now becomes eligi-
ble for control
A wide variety of tools and methods are available to control specimen preparation.
Machines capable of precise preparation of specimens can control the rate and amount of
material removal, the pressure o f specimen on abrasive, and other variables associated with
specimen preparation Several controllable preparation variables have been identified, as listed
in Table l
The significance of controllable specimen preparation is enormous It yields a product of
reliable quality Specific tolerances may be achieved. Preparations can be performed equally
from laboratory to laboratory At last, the varlabihty in microstructure can be assigned to
causes other than specimen preparation Mlcrostructure revealed via controlled preparation
procedures provides a basis for reliable evaluation, quantitative standards, and specification
limits It also permits development of microstructural databases for quality control purposes.

Evaluation
The process of mlcrostructural analysis begins with specimen preparation The output of
preparation is the mIcrostructural image that becomes the input to evaluation Once specimen
preparation has been brought into a controlled state, it is necessary to provide for controlled
evaluation to complete the foundation for quantitative standards and specifications
What has microstructural evaluation meant in the past and what form must evaluation take

TABLE 1 Metallographlc preparation variables a

Abraswe type Material removal


Abraswe format Force
Abrasive dozing RPM
Lubricant type Rotatmn
Lubricant dosing Consumable degradation
Predoslng Cleaning
Time
a Table developed by S Glancy, Struers, Inc

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FOWLER ON QUANTITATIVE METALLOGRAPHY 239

m the process of quantitative metallography9 Historically, inspection of mlcrostructures was


made for the purpose of e n s u n n g the presence of features associated with desirable perfor-
mance (that is, long fatigue life, high strength, etc ) or, the absence of structures associated with
poor performance In the past, materials were not speofically engineered for certain applica-
tions and the need to monitor mlcrostructure very precisely was low In the age of"low tech-
nology" and nonenglneered materials, subjective evaluations were satisfactory since the
demands placed upon the materials were not closely matched with the material properties The
general evaluations produced by visual Inspection provided adequate information to verify
acceptability Many traditional evaluation methods rely upon the comparison of observed
mlcrostructures with charts or photomicrographs and are often referred to as microstructure
"interpretation" or mlcrostructure "characterization "
The problem with this approach is summarized by George Vander Voort in his book, Met-
allography Prmctples andPractwe, "Since the method depends heavily on the grading of the
pictures, errors m the grading influence rating accuracy and the ratings become highly depen-
dent on subjective opinion The result is that reproducibility suffers" [13] The development
of engineered materials, and the increasing recogmtlon of the need for more soentlfiC meth-
ods, has created a demand for a more precise definition of the objectives of mlcrostructural
evaluation. By replacing mlcrostructure mterpretatlon and characterization with microstruc-
ture measurement, it is possible to do more than supply subjective "pass/fall" Information on
the quality of a product
The grain size of metals and alloys, for example, is well known to influence many properties.
For many years, metals have been classed as fine or coarse, based upon the ASTM grain size
scale If the grain size was No 5 or finer (higher numbers), it was judged to be suitable for most
engmeenng applications. A comparison chart rating to simply show that the grain size was
clearly finer than No 5 was considered adequate Greater precision was not demanded as, in
most cases, the grain size rating was used for no other purpose
However, over the past 20 years, there has been a strong drive to improve the quality of
many metals and alloys, that is, to get much better properties and behavior from basically the
same alloy Llneplpe steels are a good example. Researchers [14,15] have discovered that
extreme refinement of the femte grain size is required for optimum properties The No 5 or
finer requirement does not work Grain size must be measured with a high degree of precision,
without bias, and with exceptional reproduclblhty Chart methods are inadequate
Through quantitative methods, metallography can be used to develop new or better infor-
mation on known materials or to develop new materials. It can also be employed to obtain
accurate measures of fundamental physical constants. What exactly is quantitative metallog-
raphy9 It is based upon a group of mathematical/geometric techniques for the actual mea-
surementofmlcrostructure It~stheeqmvalentofgaglngofmlcrostructure I t p r o w d e s a p r e -
clse way for mlcrostructural components to be measured that is exact and reproduoble
Although quantitative microstructural concepts can be traced to the mineralogical work of
Delesse in 1848, the first comprehensive publication of methods can be attributed to S A
Saltykov at the end of World War II However, it was not until a translation of the second
edition (1958) of his book [16], StereometncMetallography, became available m the West that
interest m this area began to grow. This stimulated ploneenng pubhcatlons by DeHoff and
Rhmes [17], Underwood [18] and many others.
Although the techniques are based on geometrical probability concepts, there is nothing
mysterious about the methods They involve the counting of points, intercepts, tangents or
features, measurements of line sections or areas based on the relationship of some sort of test
grid or pattern with respect to the mlcrostructure The test grid may be a group of systemati-
cally arranged points or lines, circles or areas, depending upon the desired measurement From
these data, numerical values for the amount, size, spacing, density, distribution or shape of

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240 METALLOGRAPHYPAST,PRESENT,AND FUTURE

mlcrostructural features can be calculated Further, because a n u m b e r of such measurements


are performed, the statistical quality of these data can be descnbed Depending upon the
nature of the mlcrostructure and the measurement conditions, these data taken from two-
dimensional cross sections through the structure can describe the three-dimensional charac-
tensUcs of the structure
The measurement ofmlcrostructual features can be performed manually, an approach that,
in many cases, can be quite tedious and time consuming However, tools and instruments are
now available that automatically acquire the necessary measurements Beginning m the early
1960s, video technology was introduced to the world of metallography Computer mathe-
matical power was also brought into the laboratory and the term "image analysis" infiltrated
the metallographer's vocabulary. There are a whole range of fully automatic and semmuto-
matlc instruments that have been designed to extract feature measurements from a digitized
video image These Instruments are relatively fast, and if we prepare the specimens consis-
tently, the results are preose and accurate
There is some confusion over the terms "image processing" and "image analysis "Process~
lng includes mathematical transformations of the video image that may be used to prepare the
image for analysis The result of image processing is another video image that attempts to dis-
play the microstructural features in a more distract way Metallographic specimen preparation
is designed to clearly reveal mlcrostructure Electromc video image processing cannot make
up for poor metallograph~c specimen preparation Image analysis describes the extraction of
measurement data from the wdeo image The output of image analysis ~sthe structural feature
data that quantitatively describes the mlcrostructure These measurements are the basis for
quantitatwe product specifications
Just as in specimen preparation, where automatic grinding and polishing tools provide con-
trol of the preparation process, automatic measurement tools can control the process of eval-
uation, ehmlnatlng the subjectwlty ofthe h u m a n eye It is no less important to consider micro-
structure measurement as a controllable process in establishing sound quantitative test
standards By consldenng the entire range of metallographlC functions, both preparation and
measurement, as part of the same process, and that each process is controllable, we can arrive
at an excellent basis for the formulation of quantitatwe metallographIc test standards and
product specifications

Specifications and Standards


Material mlcrostructure, with its proven correlation to engineering properties, is a suitable
measure for a product specification. If the strength of a material is influenced by the amount
of porosity in ItS structure, porosity can be measured in order to assess the quality of the mate-
hal The patterns of microstructure and performance correlation form the basis for material
standards Specifications are intended to be a statement of a standard of quality
Product specifications describe the chemical and mlcrostructural characteristics required to
produce a certain combination of mechanical properties deemed necessary for a particular
product Other product characteristics, such as product size and shape, are also important, but
are not related to mlcrostructural control or measurement The ideal product specification
would define uniquely the qualities necessary to serve most efficiently for a given use and they
can be approached if truly significant tests can be made to determine the presence of the
required qualities [19] Controlled preparation and measurement of mlcrostructure using
quantitative methods provide these significant tests There exist today many private and public
standards that incorporate metallographlc procedures Most manufacturing companies have
many volumes of raw material and component standards. There exist many other standards,
such as Military Specifications, and there are several standards writing organizations, such as

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FOWLER ON QUANTITATIVE METALLOGRAPHY 241

the American Society for Testing and Materials (ASTM) and the International Organization
for Standardization (ISO) [20]
Standards have evolved along with materials soence and metallographlc technology. Im-
tlally, the requirements of materials being rather general, the techmques of preparation and
evaluation being imprecise, the product standards themselves did not reqmre exactness. Many
metallographlc standards have made use of chart p~ctures or photographs for comparison to
the observed structures. The first appearance of chart rating methods for gram size and inclu-
sion content was m the 1930s These methods became popular and are still used today These
standards exist today and are used within all manufacturing industries These standards, how-
ever, are inadequate They are remnants of a time when neither the need for preose measure-
ment of materials, nor the abd~ty to make them, existed. Clearly that ttme has passed As Davis
[19] states m The Testmg of Matertals "The skdl and accuracy w~th which a thing can be
speofied depends on the state of knowledge concerning it and on the preoslon with which its
qualmes can be determined "W~th the increasing complexity of matenals, more adequate test
methods and product specifications have become necessary, w~th advances m soenhfic under-
standing of these materials, and the avadabd~ty of precision analytical instruments, more ade-
quate speoficat~ons have become possible.

Conclusions
Engineered materials designed for demanding apphcatlons reqmre a more soph~stlcated
approach to metallographlc speoficatlons Only a short time ago, the concept of automahc
specimen preparatton was rejected by many practmoners and there may still be those who
resist advanced methods However, that number is rapidly decreasing. There are now many
who understand the value and absolute necessity of controlled specimen preparaUon
The next step is controlled quantltatwe evaluation We must go beyond mere charactenza-
tlon to meaningful quantification This is possible through the use of soent~fic methods per-
formed by automatic measurmg instruments Mtcrostructure preparation and evaluation pro-
cedures can be developed using the same basic engmeenng p n n o p l e s apphed to any
manufactunng process These process speoficatlons become the basis for true quantitative
standards
Quanhtatlve test method standards are being developed. Within the Amencan Sooety for
Testing and Materials pubhcatlons, several mlcrostructural standards exist that incorporate
rigorous quanhtatlve methods. But, there are many poorly wntten quahtattve standards, par-
tlcularly those issued by industry as private standards It ~s the responslblhty of industry pro-
fesslonals, both suppliers and manufacturers, to provide the highest possible product quality
Th~s goal can only be achieved by employing the best methods and technology avadable m the
metallographlc process

References
[ 1] Vander Voort, G F, "Inclusion Measurement," Metallography as a Quahty Control Tool, Plenum
Press, New York, 1980, pp 1-88
[2] Vander Voort, G F "Gram Size Measurement," PractwalApphcattons of QuantltattveMetallog-
raphy, ASTM STP 839, J L McCall and J H Steele, Jr, Eds, American Society for Testing and
Materials, Phdadelphla, 1984, pp 85-131
[3] Wyman, L L and Moore, G A, "Quantaatwe Metallograph~c Evaluations of Graphmc M~cro-
structures," Transactions, AFS, Vol 71, 1963, pp 7-16
[4] Underwood, E E and Berry, J T, "Quantltatwe Measurements of Cast Iron M~crostructures,"
Transactions, AFS, Vol 89, 1981, pp 755-766
[5] Cochrane, R C, "Optxcal Microscopy," Charactenzatton of Htgh Temperature Materials 1, The
Institute of Metals, London, 1988, pp 43-93
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242 METALLOGRAPHY PAST, PRESENT, AND FUTURE

[6] Smith, C S, A Search for Structure Selected Essays on Science, Art, and History, The MIT Press,
Cambridge, MA, 1982
[7] Smith, C S, From Art to Science Seventy-Two Objects Illustrating the Nature of Discovery, The
MIT Press, Cambndge, MA, 1980
[8] Smith, C S, A History of Metallography, The University of Chicago Press, Chicago, 1965
[9] Vander Voort, G F, Metallography Principles andPracttce, McGraw-Hill, New York, 1984
[10] "Metallography and Mlcrostructures," Metals Handbook, 9th ed, Vol 9, American Society for
Metals, Metals Park, OH, 1985
[I 1] "Metco Polishing Procedure for all Ceramic Type Coatings," MLPP 5, Metco
[12] DeGarmo, E P, Materials and Processes in Manufacturmg, 5th ed, MacMllhan, New York, 1979
[13] Vander Voort, G F, Metallography Prmctples andPracttce, McGraw Hill, New York, 1984,p 410
[14] Abrams, H and Shmmon, P R, "Development and Properties of BethStar 80, A New 80 ksl Yield
Strength HSLA Plate," SAE Technical Paper Series, No 820486, Society of Automotive Engineers,
Warrendale, PA, 1982
[15] Abrams, H and Mueller, G E, "Development of Commercial HSLA Plate Steels Using the 160
Mill Process Control Computer Model," 1987 Mechamcal Working and Steel Processmg Proce-
dures, Iron and Steel Society, Warrendale, PA, 1988, pp 343-352
[16] Saltykov, S A, Stereometrw Metallography, 2nd ed, Metallurglzdat, Moscow, 1958, (3rd ed,
1970)
[17] QuantttatlveMwroscopy, R T DeHoffand F N Rhlnes, Eds, McGraw-Hill, New York, 1968
[18] Underwood, E E, Quantitative Stereology, Addison-Wesley Publishing Co, Reading, MA, 1970
[ 19] Davis, H E, et al, The Testing of Englneermg Materials, 4th ed, McGraw-Hill, New York, 1982
[20] Batik, A L, A Guide to Standards, Parker, CO, 1989, pp 77-128

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John J. F r i e l 1 and Eddle B. Prestridge 1

Artificial Intelligence for Twin Identification


REFERENCE: Fnel, J J and Prestndge, E B, "Artificial Intelligence for Twin Identification,"
Metallography Past, Present, and Future (75th Anmversary Volume), ASTM STP 1165, G F
Vander Voort, F J Warmuth, S M Purdy, and A Szlrmae, Eds, American Society for Testing
and Materials, Philadelphia, 1993, pp 243-253

ABSTRACT: The presence of twin bands in some alloys makes grain mzmg by automatic image
analysis difficult Twin bands appear mmilar to grain boundaries, therefore, the measured grain
size is too small Although an experienced metallographer can ignore twins while measunng
gram size manually, it is often desirable to use automatic image analysis to save time and increase
reproducibility Because twin bands are so similar to grain boundaries, traditional image pro-
cesslng techniques cannot distinguish them However, the techniques of artificial intelligence
(AI) can be used to impart knowledge to a computer that enables it to distinguish among micro-
structural features This method was tested on standard gram size charts and on real specimens
The results showed that the use of artificial intelligence for twin identification and removal works
sufficiently well to lead to an accurate measure of grain size

KEY WORDS: twin bands, artificial intelligence, image processing, image analysis, gram bound-
ary, mlcrostructure, metallography, metallurgacal specimens, metallograph~c techniques

W h e n annealing twins are present in a mlcrostructure, grain sizing by automatic image anal-
ysis is difficult T w i n boundaries appear similar to gram boundaries, and thus the measured
gram size is too small It is s o m e t i m e s possible to eliminate some o f the twins on the basis of
their gray level, but not all o f them. An entirely different approach is to attempt to identify
those characteristics o f twins that are different from grain boundaries and impart this lntelh-
gence into the image analyzer The first attempt to do this was reported previously, but
advances have now been m a d e that c o n v i n c e us that the artificial mtelhgence (AI) approach
succeeds [ I ]
A S T M M e t h o d s for D e t e r m i n i n g G r a i n Size (E 112-88 and E 1382) specify that a crystal
and its twin bands shall be considered as one gram Accordingly, if grain sizing by automatic
image analysis is contemplated, twin boundaries must be found and r e m o v e d This identifi-
c a h o n is not too difficult for an experienced metallographer, but quite difficult for a c o m p u t e r
However, if the c o m p u t e r can be taught to recognize most twins, removal is easy and auto-
matlC image analysts can proceed. It is not necessary for the c o m p u t e r to be perfect, accurate
analysis is still possible Even an operator is not perfect O n c e twins have been identified, it ts
possible to perform the analysis with and without twins as suggested for structure-property
correlations [2].

Image Processing
General Processmgfor Gram S l z m g
Before a mlcrostructure can be measured with a completely automatic image analyzer, some
preprocesslng or editing or both o f the digital image is often necessary. Image processing is

1Technical director and product manager, respectively, Pnnceton Gamma-Tech, Pnnceton, NJ 08540

243

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244 METALLOGRAPHYPAST, PRESENT, AND FUTURE

computer mampulat~on of an image that returns a d~fferent image Examples include contrast
transformation, digital filters for noise reduction or edge enhancement, illumination equah-
zatlon, etc Image editing means insertion or deletion of groups of pixels in a binary image.
For example, ffan image has been made binary by thresholdmg so that grains are bright and
gram boundaries are black, parts of the image can be edited to change them from boundary to
grain, or vice versa Image editing can be done by the operator and may be time consuming,
If there is much to be done Or it can be done by the computer as m erosion and dilation oper-
ations After appropriate image processing or editing steps or both are defined, the sequence
can be automated Image processing operations should have enough flexibility so that the
operator can determine the appropriate seventy of each process the first Ume and then apply
the same operation to other images.
Some of the preprocessmg steps that may be necessary are (l) uneven illumination correc-
tion, (2) gram boundary detection, (3) bmarizatlon, (4) inclusion removal, (5) gram boundary
completion, and (6) boundary throning. Not all of these processes are necessary on every spec-
,men, and one should never use image processing in place of proper s p e o m e n preparation and
microscope alignment
Whether or not a microstructure contains twins, the boundaries around each gram must be
complete, or the image analyzer wdl fuse them into one large gram Even one non-black plxel
on a gram boundary will cause the analyzer to measure these adjacent grains as one Achlewng
this condition might be done by careful etching or by setting a binary threshold that renders
all boundaries black If this condition is not met, all area-based measurements will be wrong
Measurements based on intercept counts are less affected by this problem [1] The methods
avadable to complete grain boundaries include manual editing, skeletomzation [3], watershed
segmentaUon [3], and modified convex segmentation [1 ]

Twin Finding
When twins are present, they must be removed or ~gnored by the measuring routine in order
to measure the correct gram size Ifa twin boundary ~s present across an entire grain, the grain
is measured as two. If the twin merely extends partially into a grain, it is irrelevant to area-
based measurement but not to intercept methods Such a twin may also cause a grain bound-
ary reconstruction program to close ~t offand create a false grain. This condmon can be coun-
tered by restricting the gram boundary routine to m l n l m u n seventy, so that it only completes
short lengths of m~ssmg boundary and does not attempt to reconstruct entire missing
boundaries
One way ofehmmatmg interferences from twins is manual measurement, wherein the oper-
ator ignores the twins In fact, mlcrostructures containing many twins have been considered
unsmtable for automatic image analyszs Another approach ~s use of specmhzed etchants that
do not attack twin boundaries [4] Other possibilities include image editing or semmutomatlc
analysis using a digitizing tablet Also, when setting the binary threshold, if only some twins
are filled in, there ~sless edmng to be done or less chance for even an lntelhgent image processor
to make a m~stake

A rtdictal Intelhgence
Because twins look so much like grain boundaries, it is difficult to develop an algorithm that
can distinguish them However, inasmuch as metallographers have little difficulty recognizing
most twins, an mtelhgent computer should be able to do the same One of the first steps was
to identify some of the common forms that twin bands take A compilation of these canonical
forms Is shown in Fig 1 The grain in the lower right portion of the figure is merely a comb1-

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FRIEL AND PRESTRIDGE ON ARTIFICIAL INTELLIGENCE 245

FIG 1--Comptlatton of some of the forms exhtbtted by twm bands

nation of types One can see that some of these forms divide the entire gram, yet others dis-
appear beneath the plane of the pohsh Some bend back on themselves, whereas others branch
in different d~rect~ons There are, of course, other forms, but if an mtelhgent processor can find
these, it may find others
The one thing that stands out most when looking at these forms is straightness In a first
attempt at twin finding, straightness was the main parameter that we considered. However, we
quickly found out that it was not enough, because gram boundaries may be strmght m parts
In the present approach, the computer examines the scale of the straightness Other factors are
considered such as whether ignoring the structure would make the gram more or less "grain-

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246 METALLOGRAPHYPAST, PRESENT, AND FUTURE

hke "Specifically, the computer measures the straightness all along a twin-candidate structure
and follows it even if it bends through angles such as those in Fig 1 It also examines the struc-
ture of the grain containing the candidate to ascertain if identifying a structure as a twin and
removing it would increase the overall convexity of the grain or, conversely, if leaving the
structure would produce two well-shaped grains. In the artificial intelligence approach to
metallographlc image processing, parts of the microstructures are taken as structures, not just
plxels In other words, the computer examines the entire microstructure and breaks it into
structures such as grains, grain boundaries, and twins By doing this, it is then possible to make
intelligent decisions among hypothetical images, that is, ones with different structures
included or excluded These decisions are made by computing a "twlnness score" that IS eval-
uated locally and lteratively, assuming that structures with higher scores have already been
eliminated If ehmlnatlng a twin candidate under consideration results in a higher score, then
that candidate is eliminated and the process repeated for all structures If the score IS lower,
the candidate is put back for reevaluation after other candidates have been examined It is
much faster for a computer to deal only with structures rather than more than a quarter of a
million individual pixels in a 512 by 512 digital image. Nevertheless, the AI approach still
requires the power and memory of a workstation class of computer
In order to ascertain how well this method works, we digitized an ASTM standard grain size
chart with twins (E 112 Plate II) for G = 6 0 Figure 2 shows the portion of the chart that we
digitized Some image processing was done to complete grain boundaries and to reduce the
thickness of boundaries and twins to two pixels A binary threshold was set producing the
image in Fig 2b Some twins were lost in this process. In particular, those that do not extend
across the entire grain may be eliminated in the boundary thinning operation [1], and a few
are eliminated just by carefully setting the binary threshold
Confidence Level--Once the binary image is formed, the twin finder goes to work Although
it is possible to identify twins and to eliminate them all in one step, it is more informative to
merely identify them at first The program classifies structures on the basis of"twinness," and
this measure is called confidence level Each structure is set to a gray level on the basis of the
computer's confidence that it is a twin Those about which it is most confident are set to a
brighter level or color than those at lesser confidence The lowest confidence level is zero or
black, implying that these structures are grain boundaries, not twins There are actually 40
individual levels from 0 to 100%. Figure 2c shows those structures above confidence level 75
as faint white, those below that level as black, and the grains themselves as gray Figure 2d
shows the mlcrostructure after the computer removed the structures it identified as twins
At this point it is necessary to assess how accurately the computer identified a structure and
the consequences of the mistakes it made. To do this, a one-gray-level density slice was passed
through the image This means that a pseudocolor was chosen one level wide (out of 256), and
as it was moved to each of the 40 confidence levels, the authors counted how many structures
were twins and how many were grain boundaries using our best judgment A plot of the results
is shown in Fig 3 We counted 496 total structures in this image and identified 241 of them
as twins and 255 of them as boundaries Figure 3 plots the cumulative number of twins cor-
rectly identified and also the total n u m b e r of grain boundaries minus those it incorrectly iden-
tified as twins, all against confidence level At confidence level 100, six twins were correctly
found, and no incorrect identifications were made As the confidence level was lowered, some
mistakes were made, and the n u m b e r of correct grain boundaries fell from 255 Below about
level 60, few additional twins were identified correctly, and more boundaries were incorrectly
picked up as twins At confidence level zero, all structures are called twins, and the number of
correct grain boundaries drops to zero by definition
We also performed this tedious structure counting on an image of brass with annealing twins
and found the same behavior Figure 4 shows the results This time we found a total of 526

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FRIEL AND PRESTRIDGE ON ARTIFICIAL INTELLIGENCE 247

FIG 2 - - D i g i t a l tmagesjpom A S T M ~tandard gram ~tze Plate H, G = 6 Ftgure 2a s'hows the original
tmage Figure 2b shows the resuh o / s e t t m g a binary threshold Figure 2c ~how~ m whlte the ~tructure
l d e n t ~ e d a ~ t~ zn s Ftgure 2d ts the mt6t ()structure alter twin removal

structures, of which we labeled 263 as twins and, comcldentally, 263 as boundanes After com-
paring Figs 3 and 4, it appears that the computer finds twins as a function of confidence level
similarly between a standard grain sxze chart and an image of brass This pattern suggests that
the operator's setting of the confidence hmlt need not be exact Consequently, at the outset of
an analysis, one could have the computer show the various structures with each at its confi-
dence level Then, after becoming satisfied with the setting, run subsequent fields or specimens
at the same level and have the computer both identify and eliminate twins all m one step It is
still possible to manually edit the image, but it is normally not necessary--the intelligent ana-
lyzer ~dentlfies enough twins correctly to measure the nght gram size automatically

Image Analysis
Image analysis is the process of extracting data from images, that is, turning images into
numbers In the case of the standard grain size chart, the relevant question is how senslhve is

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248 METALLOGRAPHY PAST, PRESENT, AND FUTURE

260
240 . .

200
180
i ii
160
~ 140
Q,) 120 "I'~ns

~) 100

Z 6o
40
20

0 I I I

100 90 80 70 60 50 40 30 20 10 0

Confidence Level
FIG 3--Plot o f twin confidence level m the A S T M standard gram stze chart versus (1) the number o f
structures correctly ldenttfed as twins and (2) the total number of gram boundary segments remus those
mlsMenttfied as twm~

the A S T M grain size n u m b e r to the confidence level setting A S T M G was measured auto-
matlcally after running the twin finder at three different confidence levels (75, 70, and 62) on
the standard gram size chart for G = 6 The P n n c e t o n G a m m a - T e c h (PGT) image analyzer
we used measures grain size by both the p l a n l m e t n c and intercept methods, so the results of
both are shown m Table 1
The data show that over this range o f confidence levels the A S T M G is no more than 0 5
umts off F r o m F~gs 3 and 4, one can see that most twins are ldenUfied somewhere m the range
o f 6 0 t o 75 Higher confidence levels do not identify enough twins, and lower levels do not find
m a n y m o r e The " n u m b e r of grams" c o l u m n m Table 1 shows how m a n y grams were found
by the ~mage analyzer In the case o f the original ~mage, m a n y grams were found because twin
bands split grains into two or m o r e Original ~mage here means the binary image w~th twins,
m o r e will be sa~d later on the effect o f setting the binary threshold
H a v i n g said that the choice of confidence level is not crucial, we can go on to make mea-
surements on various mlcrostructures both before and after twin removal The data for the

TABLE l--Effect o f confidence level settmg on A S T M G measurement

Confidence Level G (plammetnc) G (intercept) Number of Grains

Original image 72 73 403


75 63 64 218
70 60 62 174
62 55 58 117

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FRIEL AND PRESTRIDGE ON ARTIFICIAL INTELLIGENCE 249

280
260
240
Grain B o u n d a n e s ~
220
200
.+..a
r 180
160
O
(.) I40
120
100
80
Z 60
40
20
0
100 90 80 70 60 50 40 30 20 10 0

C o n f i d e n c e Level
FIG 4 Plot o f twin confidence level m a brass specimen contammg twins versus (1) the number o f
structures correctly tdenttfied as twms and (2) the total number o f gram boundary segments mmus those
mlsldenufied as twins

standard gram size chart example are compared with the results of manual analysis in Table
2. The authors each measured the image by the lineal intercept method In accordance with
A S T M (E 112-88) We did this by counting every intercept including twin bands and then
using our judgment to count only grain intercepts, ignoring twins The results in Table 2 show
a difference of a little more than one G unit owing to interferences from twins
The differences between the planlmetric and intercept measurements are interesting We
previously showed that the planlmetnc method is quite sensmve to incomplete grain bound-
aries [1] Just one nonblack pIxel on a boundary fuses two grains together and causes the ana-
lyzer to sum their area If this condition persists throughout the mlcrostructure, many discrete
grams are fused, and the measurement is meaningless Intercept methods are much less sen-

TABLE 2--Measurements o f A S T M G on standard gram size chart

Original Image Binary

Twins Yes No Yes No

ASTM G (manual) 72 60
ASTM G (intercept) 73 62
ASTM G (planlmetnc) 72 60
Number of grains 403 174

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250 METALLOGRAPHY PAST, PRESENT, AND FUTURE

sitive to this problem Not surprisingly, however, the intercept method is sensitive to the pres-
ence of twins Twin bands that do not extend completely across a grain are irrelevant to area-
based measurements, but they produce an intercept that does not correspond to a discrete
grain The best approach is probably to make both measurements and, if the results differ, then
look for the reason

Mtcrostructures wtth Few Twms


The grain size of a specimen of a beryllium-copper alloy containing twins was measured
both manually and by automatic image analysis before and after twin removal Although the
grain size of copper alloys is traditionally reported as average grain diameter, we will continue
to use ASTM G for consistency The authors individually measured four fields by the lineal
intercept method (ASTM E 112) and calculated ASTM G Again, we did this by counting
every intercept including twin bands and then using our judgment to count only grain inter-
cepts, ignonng twins These measurements were made on the original gray-scale images before
converting them to binary for automatic image analysis By using the gray-scale image, we had
all the contrast and shading information normally available to a metallographer using manual
methods The microstructure at various stages of processing is shown in Fig 5 The original
gray-scale image is shown in Fig 5a, and the other three images in the figure correspond to the
twin identification and removal process performed on the binary image In this mlcrostruc-
ture, there are not many twins, and setting the binary threshold eliminated some and caused
others to be incomplete This effect can be seen in the results given in Table 3
In this instance, setting the binary threshold clearly eliminated some twins The G = 8 7
that we measured by counting every twin band intercepted is not rephcated in the automatic
analysis It is also evident that the planimetrlc measurement was more accurate, whereas the
intercept measurement was probably fooled by remaining and Incomplete twins But it 1s still
within 0 4 G units of the manual results The total number of grains found by the image ana-
lyzer decreased only from 127 to 108 after twin removal, probably reflecting the few twins that
actually divided grains The total number of grains In the image were not counted manually

Mtcrostructures with Many Twins


An image showing the mlcrostructure of a brass specimen with many annealing twins is
shown in Fig 6 This mlcrostructure, taken from the work ofVander Voort [2], is made com-
plicated by the contrast between twins and grains Contrast within and between grains is useful
for grain sizing by companson with similarly prepared specimens and for identifying twins by
eye However, it makes automatic analysis difficult, because grams, grain boundanes, and
twins have an overlapping dlstnbutlon of gray levels Even an intelligent analyzer that distin-
guishes among structures must first find the structures. Accordingly, we selected this image to

TABLE 3--Measurements of ASTM G on berylhum-copper alloy with few twms

Original Image Binary

Twins Yes No Yes No

ASTM G (manual) 87 69
ASTM G (intercept) 74 73
ASTM G (plammetrlc) 74 71
Number of grams 127 108

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FRIEL AND PRESTRIDGE ON ARTIFICIAL INTELLIGENCE 251

FIG 5--Dtgltal lmages Jrom a berylhum-copper alloy contammg twtns Ftgure 5a shows the ortgmal
tmage Ftgure 5b shows the result of settmg a binary threshold Ftgure 5c shows m white the structures
zdenHfied as twins Figure 5d is the mtcrostructure after twm removal

see if there was any chance of identifying most of the twins and then accurately measunng
grain size
As one can see in Fig 6b, just setting a binary threshold eliminates many twins but certainly
not most of them The process of finding them by AI was largely successful but not perfect
Some twins remained, yet, lowering the confidence threshold would cause the mlsldentlfica-
tion of too many grain boundaries. Nevertheless, in an image with enough grains, the errors
in twin identification do not seem significant The results are given in Table 4
In like m a n n e r to the beryllium-copper alloy, manually counting every twin band produced
a grain size much too small The G = 6 9 that we measured was not replicated by the auto-
matxc image analyzer, it measured 6 4 and 6 3 before twin removal because twins were ehm-
mated by setting the binary threshold After twin removal, again at Confidence Level 70, the
analyzer found G = 5 3 by both methods, and this is in good agreement with G = 5 6 mea-
sured manually If we had selected Confidence Level 75 for twin removal by AI, the result
would be G = 5.5 by both intercept and planlmetnc methods, with a total of 212 grains

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252 METALLOGRAPHY PAST, PRESENT, AND FUTURE

FIG 6--Digital zmages from a brass speezmen containing many twlm Flgwe 6a shows the original
image Figure 6b shows the result of setting a binary threshold Figure 6c shows m white the structures
identified as twins Figure 6d is the mlcrostructure after twin removal

TABLE 4--Measurements of A S T M G on brass with many twms

Original Image Binary

Twins Yes No Yes No

ASTM G (manual) 69 56
ASTM G (intercept) 64 53
ASTM G (plammetnc) 63 53
Number of grams 418 181

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FRIEL AND PRESTRIDGE ON ARTIFICIAL INTELLIGENCE 253

remmnlng. The consequence of these results 1s that ASTM G is not a strong function of con-
fidence level, and it is possible to come within 0 5 G unit even on a d~fficult image In fact, it
is probably more important to set the binary threshold carefully than it is to select the exactly
right confidence level in the AI system

Summary and Conclusions


The presence of twin bands in a m~crostructure whose grain size is to be measured is at least
a complicating factor and an impediment to automatic image analysis The benefits of auto-
matic image analysis arise not from increased accuracy or speed over manual methods, but
from increased reproduclblhty both from specimen to specimen and from operator to opera-
tor Furthermore, skilled operators are free to perform other tasks while the analyzer measures
grain size Some image processing IS often necessary before image analysis, but it should never
be considered a substitute for proper specimen preparation and metallographic technique
Processing such as smoothing or crlspenlng can be accomplished by well-defined mathemat-
ical operations Grain boundary reconstruction and twin elimination, on the other hand, are
not easily accomplished by straightforward computer methods They are, however, amenable
to an artificial intelligence approach And the twin removal problem in particular requires a
computer with some of the knowledge ofa metallographer Another advantage of AI is that as
more knowledge becomes available it is easily taught to the computer
Once the images are suitable for analysis, measunng them is extremely rapid For example,
a field with several hundred grains can be analyzed in several seconds And in that time, 75
standard or user-defined measurements can be made on every grain Moreoever, not only are
field measurements such as ASTM G available, entire distributions of size and shape are also
available for structure/property correlations The accuracy of automatic Image analysis
depends on the quality of the image analyzed The measurements are virtually perfect if the
grains are delineated properly and the boundaries are in the right places Tests that we have
conducted previously [1], as well as those described in this paper, lead us to conclude that the
use of artificial intelligence for grain boundary reconstruction and twin identification works
sufficiently well to lead to an accurate measurement of grain size

Acknowledgment
The authors acknowledge discussions with Dr T Williams and his colleagues at Amennex
Artificial Intelligence, Inc Their collaboration in the basic area of knowledge englneenng
allowed us to develop the complex, competing strategies used in the AI method

References
[1] Fnel, J J, Prestndge, E B, and Glazer, F, "Gram Boundary Reconstruction for Gram Sizing,"
MtCon 90 Advances m Vtdeo Technologyfor Mwrostructural Control, ASTM STP 1094, G F Van-
der Voort, Ed, American Society for Testing and Materials, Philadelphia, 1990, pp 170-184
[2] Vander Voort, G F, "Grain Size Measurement," Practtcal Apphcatlons of Ouant~tattve Metallog-
raphy, ASTM STP 839, J L McCall and J H Steele, Jr, Eds, American Society for Testing and
Materials, Philadelphia, 1984, pp 85-131
[3] Serra, J, Image Analysts and Mathematlcal Morphology, Academic Press, London, 1982
[4] Vander Voort, G F, Metallography Prlnctples and Practwe, McGraw-Hill, New York, 1984

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Scott T. Bluni, 1 Katherine M. Goggins, 1 Brian J. Smith, ~and
ArnoM R. Marder I

The Use of Quantitative Image Analysis for


the Characterization of Corrosion-Resistant
Coatings
REFERENCE: Blunl, S T , Gogglns, K M , Smith, B J , and Marder, A R , "The Use of Quan-
titative Image Analysis for the Characterization of Corrosion-Resistant Coatings, Metallogra-
phy Past, Present, and Future (75th Anniversary Volume), ASTM STP 1165, G F Vander
Voort, F J Warmuth, S M Purdy, and A Szlrmae, Eds, Amencan Society for Testing and
Materials, Philadelphia, 1993, pp 254-265

ABSTRACT" Materials are subjected to corrosive environments in many engineering applica-


tions Among the most successful techniques employed to minimize matenal degradation in
such environments is the use of protective coatings, which may be non-reactive or serve as sac-
nficlal barriers to a particular corrosion process Coating deposition methods include hquld
sohdlfiCatlon deposition (hot-dip), vapor deposition (pack cementation), and hquld droplet con-
solldatlon (spray) processes Galvanneal, chromlzed, and electric arc spray are respective exam-
ples of these coating processes All of these coatings have been used extensively and have proven
successful at reducing substrate corrosion in various service environments
The coating structural charactenstlcs that may influence coating performance include coating
thickness and thickness vanatlon, volume percent porosity or voids or both, volume percent
flaking or cracking or both, and the presence and dlstnbutlon of different phases Such charac-
tenstlcs have been examined traditionally by direct inspection techniques that are not often accu-
rate, time-efficient, or reproducible The ability to gather more reliable measurements is neces-
sary to further enhance the understanding of these coatings and lead to the estabhshment of
structure-property relationships
The techniques of computer-automated image analysis permit materials scientists and engi-
neers to quickly evaluate a coating structure Relevant measurements that can be tailored to indi-
vidual coatings are readily obtained in an accurate and precise manner with the use of such quan-
titative systems This paper discusses critical mlcrostructural characteristics for galvanneal,
chromlze, and thermal spray coatings Measurement procedures for such charactenstlcs with the
use of an automated quantitative image analysis system are discussed

KEY WORDS: quantitative image analysis, hot-dip galvanneal, chromlze coatings, thermal
spray coatings, metallography, mlcrostructure, metallurgical specimens, metallographlc
techniques

C o r r o s i o n - r e s i s t a n t coatings are fast b e c o m i n g the preferred m e t h o d for e n g l n e e n n g c o m -


p o n e n t p r o t e c t i o n W h e r e a s s o m e c o a t i n g technologies h a v e existed for m a n y years, there h a v e
b e e n m a n y recent process modifications. A l t h o u g h the r a n g e o f corrosion-resistant coating
technologies a n d a p p h c a t l o n s is rapidly e x p a n d i n g , the research, quality control, a n d micro-
structural c h a r a c t e r i z a t i o n t e c h n i q u e s used to s u p p o r t this growth h a v e b e e n slow to c h a n g e
T h e n e e d for systematic, precise, a n d a c c u r a t e e v a l u a t i o n p r o c e d u r e s h a s forced b o t h research-

Research assistants and professor, respectively, Department of Materials Science and Englneenng,
Whltaker Lab No 5, Lehigh University, Bethlehem, PA 18015

254

Copyright
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ASTM
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BLUNI ET AL ON QUANTITATIVE IMAGE ANALYSIS 255

ers and manufacturers to consider many options Quantitative image analysis (QIA) is one
technique that has proven to be well-suited for coanng mlcrostructural evaluanon
Automated image analysis techniques are amenable to vanous quality control, processing,
and research applications In comparison to traditional measurement methods, quantitative
image analysis procedures are fast, accurate, reproducible, and allow for the immediate storage
and manipulation of large quantlnes of data The objective of this work IS to illustrate the
advantages of image analysis processes by describing the methods used to charactenze micro-
structural features that influence performance for a number of corrosion-resistant coatings

Hot-Dip Galvannealed Coatings


Purpose of Coating
Zinc coated steel sheet is used extensively m automobile apphcatlons due to the stringent
corrosion resistance requirements placed on car manufacturers [1-3] When coupled with
steel, zinc acts as the sacrificial anode offering protection to the steel substrate Being the more
reactive metal, zinc will preferentially corrode [4]
Hot-d~p galvanneal is a strong competitor as a corrosion resistance coating because it offers
enhanced performance properties over similar corrosion resistant coatings at low producnvlty
costs These properties include superior weldabdlty, scab corrosion resistance, and good pamt-
abflxty[2,3,5] However, due to the formanon ofbrlttle iron-zinc (Fe-Zn) mtermetalhcs dunng
processing, the coating tends to crack or powder during subsequent press-forming operations
Presently, the United States and Japan combined produce 5 2 mdhon tons per year & h o t - d i p
products for automotive applications [6]

Coating Charactertsncs
For automobile applications, hot-dip galvannealed coatings weights are between 45 and 100
g/m 2 [2,5] and the coating thickness is approximately 10 um Figure l a illustrates a fully
alloyed Fe-Zn coating containing several mtermetalhc layers Coating propertms are influ-
enced by the coanng morphology, thickness, and phase dlstrlbunon The use of QIA aids m
companng and determining the formabfllty of different coatings that contain vaned phase
morphologies due to vaned processing parameters

Measurement of Crmcal Coating Parameters


Some of the mlcrostructural features used to evaluate coating performance are coating
thickness and thickness variation and powdering The techniques used to evaluate these prop-
ertles with quantitative image analysis (QIA) techniques are described below
Coating Tkwkness--Coatmg thickness and thickness variation are crlncal properties in
coating processing. Varlanons of thickness cause uneven alloying rates that produce different
forming properties throughout the coating QIA offers an efficient method for measuring these
properties This fully automated method is qmck and more accurate than the conventmnal
method of measuring scanning electron or light optical mlcrographs
QIA sample preparation is identical to light optical metallography preparahon The sample
is pohshed to a 0 25 micron finish and etched with a modified Rowland's solution [7] The
etchant not only bungs out the true mlcrostructure of the coating but it also changes the grey
level of the coating from that of the substrate material
In using QIA techniques, the coating ~s first thresholded by grey level, from Fig. 1a to b In
this case the coating consists of two grey levels Since the resulting red binary image corre-

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256 METALLOGRAPHY PAST, PRESENT, AND FUTURE

FIG 1--Image analy~ l s procedures &r mea yurmg galvanneal coating t&ckness (a) typtcal galvanneal
coating, (b) thre~holded coatmg, (c) tmage appearance after feature hmtts, (d) superlmposed grtd used to
determine coating thickness', and (e,f) result display of typical measurement~

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BLUNI ET AL ON QUANTITATIVE IMAGE ANALYSIS 257

sponds to constituents also contained in the substrate, it is sized so that irrelevant substrate
matenals are discarded The two remaining binary images are combined, representing the
entire coating layer, Fig 2c A vertical grid IS superimposed on the coating and a new image is
created that marks the intersection of the coating with the grid lines Next, a feature limit is
set to ensure that any erroneous measurements due to damaged, cracked, or crushed coating
are not included in the measurement The length of the remaining lines shown in Fig 2d is
now measured to determine coating thickness From this particular image frame, 46 mea-
surements were taken and the average coating thickness was 11 6 ___ 1 5 ~m (note that where
data are written x _+ y, y denotes one standard deviation) The resulting histogram is illustrated
in Fig 2e With use of an automated stage, data from several fields are compiled into one his-
togram and better statistics can be obtained
P o w d e r l n g - - T y p I c a l l y , galvannealed coating performance is evaluated qualitatively Most
steel companies have individual test methods to evaluate the formation and adhesion prop-
erties of the galvannealed steel sheet These tests are quick, on-line methods for examining the

FIG 2--Slcp~ ~ e d to determine pe:~etTt p~,~tderm:~ m gal~annca/ ~oalmgs (a)/ormd u~almg, (b)
thre~holded zmage, (c) coalln,~., and background bmar) m~agc a/let ~ub~'irate ~cl)arafmn and (d) hacL-
ground and ~oaring la) er ~epat alzon

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258 METALLOGRAPHY PAST, PRESENT, AND FUTURE

FIG 2 (r onzmued)--(e) Lnttre coaling layer, (f) hortzontal grld ~uperlmpo~ed onto tmage, (g) [eature
hmlt~ ate ~et on the bmar) gpld/backL, round tmage to include only cracked or powdered tegmns, and (h)
odahedta[ dt/auon enables ~racked and powdered Jegtons to be fEh'd Percent crackmg or powdering t~
no~4 measured

quality of the coating One method 1s the peel-offtest Adhesive tape is apphed to a sample
either before or after forming The sample is formed by one of two methods, a bend test or a
cyhndrlcal cup draw-test The tape is then compared visually to a qualltatlve standard rating
system Th~s test is not quantitative nor particularly accurate A more quantitative method ~s
performed by QIA
A formed coating IS Illustrated in Fig 2a The coating layer and the background material
are first thresholded by different grey levels Because the substrate material is of the same grey
level as part of the coating and the background materials as shown by the binary image in Fig
2b, steps to distinguish these features are needed A size limit is set on the coating to exclude
the substrate material, Fig 2c The background material, coating, and cracks are next sepa-
rated A vertical grid as superimposed onto the background and coating layer, Fig 2d, that acts
to fragment the image into small segments By means of aspect ratio limitations, the segments
that correspond to coating phases are added to the coating layer, Fig 2e A horizontal grid is

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BLUNI ET AL ON QUANTITATIVE IMAGE ANALYSIS 259

superimposed onto the screen and combmed with the thresholded regions to form a new image
shown m Fig 2 f A feature size limit is then set so that the glad only lies within the spaces and
gaps o f the coating, Fig 2g Next, a vertical grid Is superimposed on the remaining horizontal
lines, and the points of intersection form another binary image. These points are ddated to fill
the spaces where the coating does not exist. The parts of the dilated binary image that over-
lapped onto the coating layer are deleted As shown m Fig 2h, the resulting image Is the com-
bination of two binary images, one corresponding to the coating area, and the other to the
powdered or cracked area in the coating F r o m this, a plane fraction o f powdered or damaged
coating can be determined Results indicate that 25 80% of this coating is cracked or has pow-
dered from the substrate

Chromize Coatings
Purpose of Coating
Chromlzmg, the process of coating a substrate metal/alloy with chromium, is a popular
choice for high-temperature surface protection. The chromlzlng process is inexpensive, appli-
cable to a w~de range o f metals and alloys, and is amenable to various part configurations
[8] The coating is formed by diffusing chromium atoms into a metal substrate that produces
an alloy layer that is an integral part of the substrate The high chromium alloy layer develops
a slow growing, t e n a o o u s surface oxide, that protects the substrate component from acceler-
ated corrosive attack The coating is also i m m u n e to the flaking and spallatlon problems that
afflict plating, overlay, and spray coatings Chrom~ze coatings are presently used extensively
in fossil-fired power generation plants and are being considered for certain aerospace
apphcatlons

Coatlng Charactertsttcs
An as-received chromlze coating mlcrostructure is shown m Figs 3a and b at magmficatlons
of 100 and respectively The coating mlcrostructure consists of an outer layer that
appears featureless at low magnification, columnar grains, grain boundary and lntragraln car-
bides, a black void layer beneath the outer layer, and a distinct coatlng/substrate interface The
Murakaml's reagent used for etching these samples has been shown to etch M6Cand M2C type
carbides Investigators have determined that the chromlze coating carbides consist of both
chromium and molybdenum carbides [ 9,10] The void layer and the columnar grain structure
are caused by the chromlzlng process itself [11-13]. The coatlng/substrate interface is very
abrupt and has been attacked aggressively by the pzcral etch, indicating the presence of car-
bides at the interface This interface is thought to act as an lnterdlffUSlOn barrier restricting
continuous chromium migration during service A direct consequence of the Interface for-
marion is a large decarburlzed substrate layer, immediately adjacent to the interface

Measurement of Crmcal Coating Parameters


Research into chromlze coatings indicates that the two critical mlcrostructural features that
influence coating performance are its thickness and porosity content Measurement of each
will influence repair and replacement decisions.
Coating Thtckness--Because the coating is designed to act as a protective barrier for the
substrate, maintaining a specified coating thickness is essential to extending the service life of
a component Traditionally, coating thickness measurement is performed in two ways (1) in
SltU measurement of component dimensions using a nondestructive evaluation technique, or

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260 METALLOGRAPHYPAST, PRESENT,ANDFUTURE

(2) removal of the component and metallographlcal analysis of coating thickness The latter
is the more accurate method Metallographlc thickness measurements are usually performed
manually or with an operator-interactive semiautomated image analysis system
In this example, the chromlze coating was ground and polished using tradmonal metallo-
graphic methods It was etched very deeply using Murakami's reagent, note the heavy attack
at the coating substrate interface, Fig 3a Measurement ofchromlze coating thickness by QIA
begins by removing the mount material and substrate material from the initial live image This
is done by first thresholdlng the image to highlight the darkest Image features, that is, m o u n t
material, porosity, and coatlng/substrate interface Image dilation of the thresholded regions
was required to enhance the lnterfaclal feature, Fig 3c The next step isolates the mount and
substrate from the coating by superimposing a horizontal grid upon the image and eliminating
all discontinuous lines, which correspond to the coating porosity The remaining grid lines are
combined with the previously thresholded regions resulting in a series of rectangular regions,
the largest being the coating, Fig 3d The m o u n t and substrate rectangles are then removed
by Imposing appropriate dimensional restrictions Since the coating region still possesses some
residual m o u n t and substrate material, an aspect ratio feature limit is introduced to eliminate
both The coating thickness is then measured by placing a vertical grid on the image, combin-
ing these lines with the coating Image, and measuring the length of the resulting lines, Fig 3e
The coating shown in Fig 3a was measured using this procedure and found to have a thickness
331 + 2 45 u m
Porosity Content--Porosity in chromlze coatings may act as initiation sites for coating fail-
ure This porosity is typically subsurface, but may also be in the outer coating layer depending
on the coating process parameters used These Internal free surfaces may act as crack initiation
sites or facilitate both thermal fatigue or corrosion fatigue crack growth The void content of
diffusion coatings is rarely quoted in the subject literature
Fully-automated image analysis is suited uniquely to measure porosity Porosity size, shape,
and area fraction can all be obtained quickly, accurately, and precisely The measurement
technique is similar to the one used m the coating thickness measurement, since the same step-
wise coating isolation is used for both First, the m o u n t material and the substrate matenal
features must be isolated and removed from the image (using the same thresholdmg and ehm-
inaUon techniques as described previously), Fig 3a In thresholdlng these two features, the
porosity is also included Therefore, a feature limit must be Imposed to exclude the porosity
and coating from the m o u n t material and substrate The coating and porosity are then placed
In another binary image, producing an image containing no m o u n t or substrate material The
image features (coating and porosity) are then thresholded again and placed on separate binary
images Residual m o u n t and substrate material are eliminated using an aspect ratio feature
limit leaving the true coating dimensions visible The coating and porosity are then brought
back together in the same binary image, Fig 3f The porosity area fraction, size, and shape can
now be measured The coating shown in Fig 3a was measured using this procedure and found
to possess 1 27 + 0 30% porosity

Thermal Spray Coatings


Purpose of Coatlng
Thermal spray coatings are used for a broad range of apphcatlons in which corrosion, wear,
or high-temperature protection is needed Such coatings provide a sacrificial bamer for a sub-
strate material, as they are either nonreactive or form a coherent, protective scale One advan-
tage of thermal spraying that makes it particularly attractive for some applications is the ability
to apply coatings in SltU Some of the industries that employ these coatings include aerospace,

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BLUNI ET AL ON QUANTITATIVE IMAGE ANALYSTS 261

FIG 3--Steps used to measure chromtzed coatmg thtcknes+ and porostty (a,b) as-received chromlzed
coating, (c) image thresholdmg and mterfacml dtlatlon reqmred to tsolate coating from other linage fea-
tures, (d) dtvtslon of the tmage into separate regtons, (e) grid superlmposed on the image that is used to
measure coating thwkness, and (f) f n a l tmage used to measure coatmg porosay content and morphology

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262 METALLOGRAPHYPAST, PRESENT, AND FUTURE

electronics, paper, automobile, utdlhes, matenal extracnon and manufacturing, and gas
turbine.

Coatmg Characteristics
A typical thermal spray-coating mlcrostructure is shown m Fig 4a, which is an electric-arc
spray coating Thickness is usually on the order of several hundred m~crons for an apphcanon
such as power plant boiler tubes Porosity can result from poor "splat" flow or from gas entrap-
ment between droplets. The total porosity volume frachon may be I to 15%, depending on the
deposition process Omdes, which appear as dark mlcrostructural constituents, can form as
droplets and travel from the gun to the substrate In addition, some oxides may be contained
within the feed material p n o r to spraying

Measurement of Crtttcal Coating Parameters


Poroslty--Poroslty has been noted generally to degrade the mechamcal properties of ther-
mal spray coatings [14] Both the volume percent and morphology of pores will dictate the
extent of property degradation For example, a pore with a large aspect ratio and correspond-
mg "tips" will provide a larger stress concentration than an equlaxed pore and may be more
likely to propagate as a crack upon the application of stress
Unfortunately, pores, oxides, and mounting material possess similar grey levels when
observed with a light optical microscope, as can be seen by inspection of Fig 4b For porosity
detection, thermal spray coatings should be vacuum mounted m fluorescent epoxy [ 15] Sam-
ples are ground with 320-grit slhcon carbide (SIC) paper just until the surface epoxy layer has
been removed By using fluorescent lighting microscopy and a color camera in conjunction
with an image analysis system, porosity is easily detected (Fig. 4c) and differentiated from all
other coating constituents. As shown m Fig 4d, the mount material will also be detected, but
can be ehmmated with a size hm~tanon The size, shape, and dlstnbunon of pores can now be
easily measured It ~s necessary to separate the coating from the substrate and mount materials
m order to determine porosity volume percent, and this can be performed under bnghtfieid
dlummatlon m the same manner as descnbed for coating thickness measurement A typical
thermal spray coating contains a porosity content of 5.15 + 0 99%
OxMes--hke porosity, oxides can degrade the mechanical properties of thermal spray coat-
rags as they are often bnttle and fractured easily with the apphcat~on of stress Oxides can be
thresholded readily with bnghtfield Illumination, and that contnbunon from porosity can be
subtracted using the porosity detection techniques described earher As an example of
acquired results, an oxide content of 25 97 + 0 52% was found for an electnc-arc spray
coating
Coatmg Thickness--Coating thickness is one cnncal mlcrostructural parameter that influ-
ences performance The effect of thickness is twofold as thickness increases, ( 1) substrate pro-
techon is enhanced as there is additional sacnficml matenal available, and (2) stresses that
develop upon heatlng/coohng of the coating system Increase due to thermal expansion m~s-
match. There should be an optimum coating thickness for each apphcahon and coating system
m particular
The task of thickness detection by fully-automated image analys~s procedures can be diffi-
cult because the substrate and mount matenals are often of the same grey level as many of the
coating components (refer to Fig 4a) and therefore cannot be easily dlfferennated The solu-
non to this problem lies within mlcroconsntuent contmmty; that is, the coating elements are
noncontmuous, while the substrate and mount materials are continuous m at least one dlmen-

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BLUNI ET AL ON QUANTITATIVE IMAGE ANALYSIS 263

FIG 4--[hermal ~pra) ~oalmgpo~osl[t measurcmen[ (a)as-apphedelectr~c-arc sp~al coalmg rmcro-


sltuclure (b) spa)' coating stlucture sho~mg slmEap grey leve]~ bet~een porosity, oxides and mount
rnaterml (c) obso ration o/poto~ttv and mount rnalertai wlth fluorescence hghtmg microscopy, and (d)
thresholdmg of por<)gll~ and mount materml, and converslon to binary zmage

slon When detected and thresholded by grey level, the coating components of a given grey
level range will therefore be observed as many particles, each of which is smaller in some
dimension than the mount or substrate material that has also been detected This is illustrated
in Fig 5a, where the mount material and coating porosity and oxides have been thresholded
together As shown m Fig 5b, the coating constituents are separated from the mount material
by placing sJze limitations on the binary image features The same concept is used to separate
the light coating background from the substrate material, as shown in Figs 5c and d By
manipulating the image such that the mount and substrate materials are all that remain, the
coating can be identified as the image portion that has not been detected As shown in Fig 5e,
the coating retains its charactensUc shape, but is now observed as a continuous entity Mea-
surement of coating thickness can now take place by superimposing a template of parallel lines
that are normal to the coatmg length, retaining that portion of the lines that Intersect the coat-
ing area, and measunng the length of these lines Figure 5fshows the resulting correspondence

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264 METALLOGRAPHY PAST, PRESENT, AND FUTURE

FIG 5 - - l hermal splay ~oalmg thuknes s measurement (a) deleclton o! mount material and coating
poro~lt~/o~ldes, (b) mount material removal from the "green" hmar~ tma,~e, (c) dete~tton o/substrale
materta/ a n d c ore el slon lo "blue" binary mTage, (d) e h m m a t m n o/ substrate [rom blue binary ~mage, (e)
tdentthcatzon o f t oaring matep ml, and (f) grtd supertmposed on image to m e a sure coatmg thteknes s"

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BLUNI ET AL ON QUANTITATIVE IMAGE ANALYSIS 265

between the coating mlcrostructure and the generated hnes that are used to measure coating
thickness As an example of obtained results, a thickness of 543.35 _+ 60.26 ~m was found for
an electric-arc spray coating

Summary
Quantitative image analysis procedures have proven to be fast, accurate, and reproducible
m the evaluation of various corrosion-resistant coatings The thickness and powdenng of hot-
dip galvannealed coatings, and the thickness and porosity of chromlzed and thermal spray
coatings are measured readily by QIA techniques The systematic evaluation of microstruc-
rural features with QIA may enhance the understanding of these coatings and lead to the estab-
lishment of valuable structure-property relationships

Acknowledgments
The authors would hke to thank Arian Benscoter for metallographlc consultation, and the
members of Pennsylvania Electric Research Council (PEERC) for their support

References
[1] Kalson, A M, "Coated Steel Sheets in North America--An Automotive Perspective," GALVA-
TECH, The Iron and Steel Institute of Japan, Tokyo, 1989, pp 271-272
[2] Denner, S G , "An Overview of the Manufacture and Apphcatlon of Zinc and Zinc Alloy Coated
Steel Sheet m North America," GALVATECH, The Iron and Steel InsUtute of Japan, Tokyo, 1989,
p 101
[3] Hada, T, "Present and Future Trends of Coated Steel Sheet," GALVATECH, The Iron and Steel
Institute of Japan, Tokyo, 1989, p 112
[4] Uhhg, H, Corroston and Corrosion Control, Wdey, New York, 1985, pp 234-235
[5] Hlsamatsu, Y, "Science and Technology of Zinc and Zinc Alloy Coated Steel Sheet," GALVA-
TECH, The Iron and Steel Institute of Japan, Tokyo, 1989, p 3
[6] Informatzon supphed by the International Lead and Zinc Research Orgamzatlon
[ 7] Rowland, D, Transactzons, American Sooety for Metals, Vol 40, 1948, p 983
[8] Rapp, R A, Wang, D, and Welsert, T, Htgh Temperature Coatmgs, M Khobalh and R C Kru-
tenant, Eds, The Metallurgical Sooety of the American InsUtute of Mining, Metallurgical, and
Petroleum Engineers, Warrendale, PA, 1986, pp 132-142
[9] Wada, T , et al, MetaOurgwal Transacttons, Vol 3A, No 11, 1972, p 2865
[10] Perry, A J and Horvath, E, Journal ofMatertal Sctence, Vol 13, 1978, p 1303
[11] Saunders, S J R, and Nlcholls, J R, Material Sctence& Engmeermg, Vol 5, 1989, p 780
[12] Sequelra, C A C and Nunes, C M G S, SurfaceEngmeermg, Vol 3, No 2, 1987, p 161
[13] Samuel, R L and Lockmgton, N A, Metal Treatment and Drop Forgmg, Oct 1951, p 440
[14] McPherson, R, Surface and Coatings Technology, Vols 39/40, pp 173-181
[15] Herrmann, E, PractlcalMetallography, Vol 20, 1983, pp 371-387

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George F. Vander V o o r t I

Examination of Some Grain Size


Measurement Problems
REFERENCE" Vander Voort, G F , "Examination of Some Grain Size Measurement Prob-
lems," Metallography Past, Present, and Future (75th Anmversary Volume), A S T M STP 1165,
G F Vander Voort, F J Warmuth, S M Purdy, and A Szlrmae, Eds, American Society for
Testing and Matenals, Philadelphia, 1993, pp 266-294

ABSTRACT: The measurement of grain size is performed nearly always on a metallographically


prepared cross section, suitably etched to reveal the gram structure, using methods that pertain
only to the grain cross sections These measurements are termed planar and some may be con-
verted mathematically into spatial estimates of the size of the three-dimensional grains How-
ever, the vast majority of such work is planar where no assumptions about grain shape are
required and grain size is described in one- or two-dimensional terms (intercept length, diameter,
or area) based on sections through the grams The most frequently used measurement methods
are described m this paper and compared using the same images These methods are the Jeffnes
planimetnc method, the tnple-polnt count method, and the Heyn intercept method These
methods base grain size on two-dimensional, zero-dlmensmnal, and one-&mensmnal features
of the mlcrostructure, respectively (that is, areas, points, and hnes)
Test lines can be utdized to count grain mterceptmns or grain boundary intersections, or,
actual intercept length measurements may be made Furthermore, the test hnes may be straight
or curved (circular test lines being commonly employed) Does the curvature of a circular test
line cause a bias in e~ther mtercept/intersectmn counts or intercept length measurements9 When
a digitizing tablet is used w~th a c~rcular test line, either chord lengths between sets of gram
boundary intersections, or arc lengths between the grain boundary intersecUons can be mea-
sured Does either practice cause bias, or are the results s~mdar? How do averages of intercept
lengths compare to the mean hneal intercept calculated from the reoprocal of the number of
intercepts (or intersections) per unit length9 Does the triple-point count method produce the
same results as the planimetnc results and how do these esUmates of the ASTM grain s~ze num-
ber compare to that from the intercept procedures9 These questions are addressed

KEY WORDS: metallography, grain size, quantitative metallography, Jeffnes plammetrlc


method, Heyn intercept method, dlgaUzlng tablet, statistical analys~s, metallurgical specimens,
mlcrostructure, metallographlc techniques

G r a i n size m e a s u r e m e n t s are p r o b a b l y the single m o s t i m p o r t a n t m l c r o s t r u c t u r a l m e a s u r e -


m e n t p e r f o r m e d , for either quality c o n t r o l or research p u r p o s e s G r a i n s are t h r e e - d i m e n s i o n a l
features; but, in the vast m a j o r i t y o f cases, they are viewed a n d m e a s u r e d o n a Nsectlng, two-
d i m e n s i o n a l p l a n e t h a t is p o l i s h e d a n d e t c h e d Because o f this, m o s t m e a s u r e m e n t s are o f a
p l a n a r r a t h e r t h a n a spatial n a t u r e . N u m e r o u s a p p r o a c h e s h a v e b e e n developed to m e a s u r e
grain size o n p o h s h e d a n d e t c h e d cross sections, a n d several a p p r o a c h e s are avmlable to trans-
late p l a n a r d a t a to spatial e s t i m a t e s o f g r a m size All o f these require s o m e simplifying a s s u m p -
t m n a b o u t grain s h a p e that, o f course, is n o t c o n s t a n t in a n y s p e o m e n D~rect m e a s u r e m e n t

Materials Characterization, Carpenter Technology Corporation, R & D Center, Reading, PA 19612-


4662

266

Copyright
Copyright*by1993
ASTM
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VANDER VOORT ON GRAIN SIZE 267

of spatial grain size is very difficult requmng either serial section analysis or mtergranular dis-
integration (liquid metal embnttlement) and direct measurement of the liberated grains
These methods are only applied m research studies
While there are a number of approaches for measuring planar grain size [ 1 ], some are more
efficient than others The chosen method should produce the most precise value for the least
amount of work For any method, the procedure must be well defined and clearly descnbed
This has been the goal of ASTM grain size standards, such as ASTM Methods for Determining
Average Grain Size (E 112-88), ASTM Methods of Estimating the Largest Gram Observed in
a Metallographlc Section (ALA Grain Size) (E 930-83), ASTM Test Methods for Character-
lzmg Duplex Grain Sizes (E 1181-87), and ASTM Test Methods for Determining the Average
Grain Size Using Semiautomatic and Automatic Image Analysis (E 1382-91). In this paper,
we will deal only with planar grain size measurement methods. These are free of any assump-
tions about grain shape

Definition of Grain Size


Dtfferent measurements have been used to assess the "size" ofgrmns Hlstoncally, the plan-
1metric method, suggested by Albert Sauveur [2] and refined by Zay Jeffnes [3,4], was the first
widely used techmque m the United States while the intercept method, developed by Emil
Heyn of G e r m a n y [5], was the first method widely used in Europe With the plammetnc
method, the grain size was described in terms of either the number o f grains per square md-
hmetre (mm 2) at 1, NA, or as the square root of the average grain area, A, which is called d.
With the intercept method, the grain size was defined as the mean hnear (or lineal) intercept
length, L3, which is the reciprocal of the number of intersections of grain boundanes per unit
length of test line, PL, or the number of grams Intercepted per unit length of test line, NL The
subscript, 3, means that the measurement is valid m three dimensions The use o f d t o describe
grain size by the Jeffnes method should be discouraged as it is calculated as the square root of
the average grain area that suggests that grains are square on the cross section, which they are
not Calculation of the diameter of a circle ofeqmvalent area ("equivalent circle diameter") is
a shght Improvement, but not much better Use of NA, a basic stereolog~cal parameter, to
define the planar grain size is recommended
The lack of a simple mterconverslon between the results of these two methods, that is,
between NA and NL or PL, has been a well-recognized weakness NA is a function of the total
length of grain edges per unit volume, Lv, while NL or PL (for a single-phase structure) is a
function of the grain boundary surface area per unit volume, Sv [6] Thus, these two measures
of grain size are based on different geometric characteristics of the grain structure To date,
there is no direct relationship between Lv and Sv and no experimental data linking the two for
the same specimens as a function of grain size
While the first (1930) comparison grain size chart (for copper and copper-based alloys)
scaled the grain size based on uniform linear increments of d, later charts used a power senes
and scaled the chart pictures based on NA increasingly exponentially The charts listed either
the NA value (number of grains per square Inch at 100) or the "ASTM grain size number,"
G, from the following equation

n = 2 G-I (1)

where n is the number of grams per square inch at 100 magnification To obtain NA as the
number of grains per m m 2 at 1, multiply n by 15 50031 Hence, NA lS related directly to G
and is measured readily by the Jeffnes method, or by the triple-point count method.

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268 METALLOGRAPHYPAST, PRESENT,AND FUTURE

Jeffries Planimetric Method


This method requires the counting of the number of grains m a known test area, usually
circular m shape. A orcle of 79 8-ram dmmeter (5000 m m 2) is drawn on a mlcrograph or a
template with such a circle ~s placed over a ground glass.projection screen or televlsmn mon-
itor The magnification is chosen so that at least 50 grams are within the test area Next, the
number of grains completely within the test area, n j, and the number of grams intersecting the
circle, n2, are counted. To obtain an accurate count, the grains must be checked offor n u m -
bered which slows down the analysis as either a new template must be used for each field count
or It must be cleaned between counts. Several fields must be counted in order to obtain a sat-
isfactory level of preoslon This number would depend upon the umformlty of the gram
structure.
The sum of n j and n2/2 is mulUphed by the Jeffnes factor,f, for the magmficatmn employed
with the 79 8-ram-diameter circle to obtain NA, the number of grains per m m 2 at 1 T h e f
value is obtained from

f = M2/5000 (2)

where M is the linear magnification Ifa circle of a different diameter is utilized, substitute its
area (m m m 2) for 5000 m Eq 2
The average grain area, A, is obtained from the reciprocal of N~

-A = 1/NA (3a)

where A is I n m m 2, or

= 106/NA (3b)

where A is m square mlcrometres (um 2) The Jeffnes grain diameter, d, is the square root of A,
but use of d should not be encouraged because grain cross sections are not square G can be
calculated from NA (number of grams per m m 2 at l) from

G = (3 222 log N~) - 2.954 (4)

or, from Table 2 ofASTM E 112-88

Triple-Point Count Method


This method, suggested by Cynl Stanley Smith [ 7], utlhzes Euler's law to obtain NA A orcle
of known size is placed over a mlcrograph, or a template with such a circle ~s placed over a
ground glass projection screen or television momtor. Although no statlsUcal studies of this
method have been made, the magnlficatmn should be chosen so that at least 40 to 50 tnple
points are present Too high a n u m b e r per test area may make counting imprecise and difficult
Again, a n u m b e r of such counts should be made and the triple points must be marked off as
they are counted to obtain an accurate count If a four-ray grain juncUon ~s observed, which
is rare, it is gwen a count of two NA ~Sdetermined from

N~ - (P/2) + 1 (5)
Ar
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VANDER VOORT ON GRAIN SIZE 269

where P is the n u m b e r of triple points 0unction point of three grains on the plane of polish)
counted, ATIS the test area in m m 2 at l, and NA is the number of grains per m m 2 at 1 G
is calculated from Eq 4 or from Table 2 ofASTM E 112-88.

Heyn Intercept Method


Unlike the Jeffnes method and the triple-point count method, the Heyn intercept method
does not require marking off of the intercepts or intersections to obtain an accurate count.
Hence, this method is faster than the other two, and the same degree of precision can be
obtained in less time The intercept method is useful for deformed grain structures, and a mea-
sure of their elongation can be obtained while G is determined Interest In the Heyn Intercept
method in the United States was stimulated by the work of John Hllliard [8] and Halle
Abrams [9].
Lines of known length are drawn on a template and placed at random over a micrograph,
projection screen, or TV monitor For a deformed (nonequiaxed) grain structure, one or more
parallel straight test lines are placed over the grain structure with orientations parallel and per-
pendicular to the deformation (longitudinal usually) direction For an equiaxed gram struc-
ture, ASTM E 112-88 recommends circular test lines (three concentric circles with a total cir-
cumference [line length] of 500 ram) Circular test lines are also used for amsotropic structures
to average out the anisotropy
For a single-phase grain structure, a count can be made of either the number of grains inter-
cepted by the test lines, N, or the n u m b e r of grain boundary intersections with the test lines,
P Both approaches produce equivalent results With straight test lines, it may be easier to
make N c o u n t s where the grains partly intercepted by the ends of the hnes (unless the end lies
exactly on a grain boundary, which happens seldomly) are counted as half values. For circular
test grids, there are no line ends to deal with and either P or N counts can be made. Many
raters prefer to make P counts (grain boundary intersections) The number of N o r P c o u n t s
is divided by the true test line length (mm at l) to obtain NL or PL. The true test line length
is found by dividing the total test line length by the magnification For a single-phase grain
structure, Sv is twice PL or NL
The mean lineal (or linear) intercept length, L3, is the reciprocal of NL or PL (for a single-
phase grain structure) For a deformed grain structure, NL or PL will be higher using test lines
perpendicular to the deformation axis than for test lines parallel to the deformation axis
Because L3 is the reciprocal Of NL or PL, the intercept lengths are inversely proportional Thus,
if straight test lines are placed parallel (ll) and perpendicular ( to the deformation axis, an
amsotropy index, AI, can be defined as

AI = NL = L3111L3 (6)

To obtain the gram size of a deformed grain structure, we can average the above L3Hand L3
values, use randomly placed straight test lines, or use circular test lines
The determination of the ASTM grain size number, G, from mean lineal intercept values
has been a weak part of this method. The first published relationship between L3 and G was in
ASTM Method for Estimating the Average Femte Gram Size of Low-Carbon Steels (E 89),
Introduced in 1950 but discontinued in 1961 after ASTM E 112 was adopted. This standard
suggested making intercept counts on two sets of mutually perpendicular test lines to obtain
NL and NLt, at magnification M The following equation was used to calculate the number of
grains per square inch at 100, n

n = 0 8(M/IOO)Z(NL (7)

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270 METALLOGRAPHY PAST, PRESENT, AND FUTURE

This equation was in ASTM E 112 when it was proposed Later, it was changed to a relation-
ship between L3 of a orcular gram and its area, A

L3 = (TrA/4) '/2 (8)

As grains are not circular in cross secnon, this value of L3 is underestimated and an a d d m o n
of 0 52% is made For any value of NA (or A), one can calculate L3 using Eq 8 and then Increase
it by 0 52% to develop the needed relationship between G and the measured L3 The differ-
ences in L3, calculated by these two methods, are very small From L3 in mllhmetres, the
ASTM grain size number, G, can be calculated from

G = ( - 6 6439 log Ls) - 3 288 (9)

Example of These Methods


Pieces of an experimental hot-work tool steel were heat treated using three different austen-
ltlzmg temperatures 1052, 1066, and 1080~ (1925, 1950, and 1975~ After soaking, they
were quenched to 704~ (1300~ and held long enough to permit a minor amount of precip-
itation at the pnor-austenIte gram boundaries, then air cooled to ambient Etching with Vilel-
la's reagent fully revealed the grain structure
Photographs were made oftypmal regions m each specimen (areas chosen bhndly) and 203
by 254 m m (8 by 10 in ) enlargements were made. One print for each austenInzIng treatment
was chosen for comparative measurements
First, the planimetnc method was employed ASTM grain sizes were 9 9, 9 5, and 8 7 for
the samples austemtlzed at 1052, 1066, and 1080~ (1925, 1950, and 1975~ respectively
Next, the three-circle test grid was used to measure the same photographs The ASTM gram
size numbers were 10, 9 5, and 8 9, respectively Finally, a digitizing tablet was used to measure
intercept lengths directly through use of a template with straight test lines applied randomly
over the grain structure The A S T M grain size numbers were 9 9, 9 6, and 8 7, respectively,
for the three specimens The data are given m Table 1
In the Heyn method, or the Abrams three-circle intercept method, actual intercept lengths
are not measured For each test grid placement, an average intercept length is determined
based upon Nintercepts or Plntersectlons These L3 averages for each placement (or field) are
then averaged and a standard deviaUon can be computed Using the average and standard
devmtlon, the 95% confidence interval and the percent relanve accuracy may be calculated
The Abrams three-circle intercept method recommends that the magnification be chosen so
that a relatwely high number of P or N counts per field is made, ideally 100, and five fields are
measured for a total of(Ideally) 500 counts I r a large number of fields were to be measured,
the distribution of the N or P counts would be observed to be Gaussian Thus, calculation of
the arithmetic standard deviation 1s valid and precision can be assessed F o r most speomens,
measurements on five fields gives acceptable precision and is highly efficient The magnitude
of the standard devianon gives some insight into the uniformity of the grain structure
However, to properly assess the uniformity of a gram size distribution, individual gram mea-
surements must be made Individual measurements of Intercept lengths of test hnes through
grains or individual grain areas may be measured With strictly manual techniques, individual
intercept lengths are easier to measure than grain areas Templates illustrating a graded series
of circles of varying diameter could be employed to classify individual grains, but precise area
measurements cannot be made in this way
Semlautomahc digitizing tablets can be utilized along with a template to measure mdlwdual
intercept lengths, and grains can be traced to measure grain areas, although this is tedious and

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VANDER VOORT ON GRAINSIZE 271

TABLE 1- - G r a m stze measurements o f hot-work tool steel spectmens

JEFFRIES PLANIMETRIC METHOD


Specimen Number Average, Average, Jeffnes, NA, ASTM
Code of Fields nl n2 f mm -2 G

1925~ 4 40 75 30 25 134 95 7540 1 99


1950"F 4 29 75 25 75 133 24 5679 1 95
1975~ 3 25 67 23 33 85 26 3183 2 87
ABRAMSTHREE-CIRCLEINTERCEPTMETHOD
Specimen Code Number of Fields Lr, ~ mm NL, mm-~ L3, tim ASTM G

1925"F 8 4 92 100 2 10 0 10 0
1950~ 10 6 19 83 0 12 1 95
1975~ 12 7 41 67 8 14 8 89
INDIVIDUALINTERCEPTLENGTHMEASUREMENTSb
Specimen Code Number of Intercepts L3, ~m ASTM G

1925"F 500 10 5 99
1950~ 432 11 6 96
1975~ 379 15 6 87
a L r 1Sthe total test hne length
b Straight test hnes used

requires a steady hand Automatic image analyzers could also be employed to make either type
measurement, so long as the grain structure can be properly delineated Once grain areas have
been measured, it is possible to compute the Jeffnes diameter, d, or the equivalent circle diam-
eter, ECD Furthermore, when the grains are detected, other statistical diameters may be mea-
sured, for example, a m a x i m u m caliper diameter (maximum Feret's diameter)
After a suitable number of measurements have been made, the data can be grouped into
classes usmg linear, logarithmic, or exponential class interval widths The amount in each class
can be computed as a simple numerical percent or as a weighted average, by length fraction
for intercept lengths or diameters, or by area fraction for grain area measurements
The digitizing tablet intercept length data for the three hot-work tool steel specimens were
grouped into 13 linear classes of equal width and eleven classes of uniform logarithmic spac-
Ing, producmg arithmetic and logarithmic intercept length groupings The frequency per class
was expressed as a simple number fraction or as a linear fraction, both as percentages The
percentage by length (sum of intercept lengths per class divided by the total intercept length,
times 100) puts greater emphasis on the data in the larger class intervals Figures 1 and 2 pre-
sent these data with the n u m b e r frequency at the top and the lineal fraction at the bottom
The hnearly scaled h~stograms, F~g 1, clearly demonstrate that the data are not Gausslan in
nature The lineal fraction percent, bottom of Fig 1, better reveals the emerging duplexity of
the grain size distribution than the n u m b e r fraction percent It is also apparent that the width
of the distribution increases with gram growth This has been observed in numerous prior stud-
ies of grain growth In contrast, the logarithmic histograms reveal slightly skewed, nearly uni-
formly shaped curves lndlcatmg a lognormal distribution of the data Many studies of such
data have also concluded that grain size distributions are essentially lognormal, although some
researchers have suggested that certain other more esoteric dlstnbutions may exhibit some-
what better fits to the data. In any case, grain size distribution data are not normal (Gausslan)
Hence, it is really not correct to compute an arithmetic standard deviation for lndwldual grain
size distributions, although this is done regularly due to the simplicity of such calculations

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272 METALLOGRAPHY: PAST, PRESENT, AND FUTURE

Percent

....... 9 ................................................................................. ........

0 20 40 60 80
Intercept Length,/z rn

0 1925F ~ 1950F o 1975F

Lineal Fraction, %

4~1 ~ 1925F L. 9 10.5 #m

3020I................................
.............................................................................................
~ .........................................................................................................................................................................................................................
~ ~ 1950F L = 11"6 ~l'm

1 0 ~ 0 .......................................

0 20 40 60 80
Intercept Length,/zm

0 1925F ~ 1950F o 1975F

FIG. 1--Intercept length distributions by number percent (top) and by linear fraction percent (bottom)
using linear size classes for heat-treated specimens of an experimental hot-work tool steel.

Intercept Counting Problems


A recent paper by Willis and Lake [10] discussed the measurement of grain size using cir-
cular test grids. When a circular test grid is employed, the number of grain boundary intersec-
tions (or grain intercepts) is divided by the circle circumference(s) to obtain P, (or Nt) and the
reciprocal of PL (or NL) gives the average intercept length, L3, which is an arc distance. On the
other hand, a digitizing tablet could be used with circular test patterns and the chord distance

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VANDERVOORTONGRAINSIZE 273

Percent
30
1925F [. 9 10.5 /~m
25- 1950F L" 11.6 /~m ~ i i
20 .......................................................................................................................................................................................................

5 . . . . . . . . . . . . . "........

0
0.5 5 50
Intercept Length, Nm

l o 1925F " 1950F ~ 1975F ~

Lineal Fraction, %
4O
1925F [. 9 10.5 /~m ~
30 .................................................................................................................................................................... .................. o ................................................................

. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . ............................................

1975F L 91 5 ~
10 .........................................................

0 ~r A~ L .L 9 I I I I I I I I I I I III"1"
0.6 5 60
Intercept Length,~ m
0
1925F 9 1950F o 1975F

FIG. 2--1ntercept length distributions by number percent (top) and by linear fraction percent (bottom)
using logarithmically scaled size classesfi)r heat-treated specimens o[an experimental hot- work tool steel.

between successive grain boundary intersections could be measured and averaged to obtain
L~. Alternatively, one can trace the circle circumference and measure the distance between
successive grain boundary intersections and the mean of these arc distances would be L3. Are
these two measurements equivalent, or is there a bias? Willis and Lake stated that for any
curved test line, the probability of intersecting grain boundaries depends on the test line length
but not on its curvature. They stated that the use of arcs rather than chords increases the overall

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274 METALLOGRAPHY PAST, PRESENT, AND FUTURE

test line length and the probability for intersecting grain boundaries They further concluded
that the test line length is arbitrary.
Willis and Lake [10] presented data to show that determination of L3 by Intersection counts
is not influenced by curvature, that is, test circle diameter An annealed low-carbon steel spec-
imen with a mean lineal intercept length of about 7 8 um (ASTM l0 7) was measured using
circles with true diameters, D, from 5 16 to 67 6 u m (D/L3 ratios from 0 66 to 8 7 l) and from
1274 to 482 intersection counts (fewer counts were made as the circle diameter increased)
Intersection counts were also made using straight test lines They concluded that multiple
application of small circles gives equivalent results to a reduced number of applications of a
larger circle if the number of intersection counts are similar Application of their two smallest
diameter circles did produce some placements without any Intersections Because the diame-
ters of these circles were less than L3, this is to be expected
While Willis and Lake concluded that intersection counts using circles of varying diameter
(that is, curvature) were not biased by the curvature, they stated that the measurement of indi-
vidual chord lengths, rather than arc lengths, using circular test grids did produce bias They
stated that such chord measurements did underestimate L3 and experimental data were shown
to substantiate these claims
Willis and Lake [10] stated that their observations were contrary to statements in ASTM E
112 where it is claimed that chord measurements of grain size using circular test lines are valid
Willis and Lake stated that arc lengths should be used, not chord lengths Further, they stated
that if L3 was the only desired measurement, measurements of Individual arc distances were
not required because the total arc distance (the circumference) would be known and the num-
ber of intersections could be counted easil