Metallography History and Development

Background
The name metallography was initially used in the early 1700s to signify the description
of metals and their properties. It was first used in its modern sense in 1892, that is, to
define the study of the internal structure of metals and alloys in relation to their
physical, chemical and mechanical properties. Thus it can be seen that its procedures
permeate all aspects of the understanding and development of metals and their alloys.
Moreover, these techniques are widely used, or at least readily adapted to the study of
engineering materials, although full use of this commonality has only been achieved
comparatively recently with the replacement of courses in metallurgy by courses in
materials science and engineering.
This article is written from the personal viewpoint of one who became employed as a
metallurgist in 1937 and has thus lived through an era of rapid and widespread
developments in metallography. It so happens that 1937 marks a significant divide in
this story, for metallographic methods remained fairly static for the first third of the 20th
century and a very detailed description of that period was published in the 4th Edition
(1937) of C.M. Deschs text Metallography; the 1st Edition was published in 1910. It
is especially significant that as well as descriptions of the basic techniques of preparing
and examining micro-specimens and of obtaining data to produce phase diagrams,
Desch had two chapters written by G.D. Preston (of Guinier-Preston Zones fame).
These chapters described X-ray metallography, by which the specific crystallographic
structures of metals and alloys were elucidated. This was the first time this topic had
been included in a text, at least an English one, and moreover, this text was used almost
universally in teaching metallurgy in the English Speaking World.
1901-1938
Desch was the Superintendent of the Metallurgy Department of the National Physical
Laboratory of DSIR in the UK. My viewpoint is oriented by the fact that Desch
recruited me to his Department in 1937 and made me his personal assistant in 1938.
Deschs predecessor as Superintendent had been W Rosenhain who was appointed to
that post in 1905. Rosenhain was trained in the University of Melbourne as a civil
engineer and had emigrated to England on graduating some years before 1905.
Standard Specimen Preparation
Rosenhain was a strong leader and an innovator in the theory and practice of physical
metallurgy and by the time he resigned from NPL in the 1930s, he had made the
department pre-eminent in metallographic practice. Moreover, these metallographic
procedures and instruments had remained much the same for all these years. For
example, during the period from the late 1930s to at least 1948, most of the polishing
of microspecimens was done at NPL by the same two members of staff, who did
nothing else all day. Preliminary rough polishing was done on abrasive papers and final
polishing on rotating laps.
These were covered with cloth and loaded with polishing powder made into a paste with
distilled water. On the final lap, the abrasive was chromic oxide, made by the
Departments chemists to a consistent degree of fineness. This stage usually took up to
half an hour and even then after etching, had to be repeated often several times. It was a

procedure requiring skill, born of experience and backed up with a great amount of
patience.
Metallurgical Microscopes and Phase Diagrams
Early on, Rosenhain designed and had built a metallurgical microscope, which was
mechanically easier to use, but optically unchanged. This microscope was still in use
when I worked at NPL. He also automated the collection of the data from cooling
curves of alloys to build up phase diagrams.
Major Innovations of the 1930s
The major innovations of the early-to-mid 1930s were the use of X-rays and electron
beams to derive crystallographic structures; this was made possible by the enunciation
of Braggs Law of diffraction. Also in 1938, a pioneering systematic study of the
polishing and etching of steels for optical examination was published by Vilella. This
book was to be a factor in one of the major metallographic developments, that is Len
Samuels work on mechanical polishing-which we will come to later. Mechanical
polishing was very labour intensive, preparing a specimen took 5 weeks of polishing in
Sorbys pioneering work in the 1860s and still took several hours in the 1940s. Etching
of microsamples was a matter of using empirically developed etchants looked up in a
handbook. It is still much the same nowadays.
Mechanical Polishing
Mechanical polishing in 1937 and, indeed for the next 20 years was to remain very
much an art, neither studied nor understood. This statement requires some qualification.
A layer of anomalous structure was found on polished (unetched) surfaces and identified
by Beilby as a smeared layer of amorphous structure, the so-called Beilby layer. The
presence of amorphous metal was widely accepted in the 1930s, mainly as a result of
work by Rosenhain, and his powerful support of it using his great skill in debate. This
did not lead to any significant advances in polishing techniques and was eventually fully
discredited.
Alternatives to Mechanical Polishing
Alternative methods of polishing by purely chemical treatment with or without an
electrical driving force emerged in the late 1930s and were developed further in the
1940-1950s. An Australian book on electropolishing was published by Tegart in 1959.
Electropolishing proved a valuable method for preparing test specimens for the study of
mechanisms of deformation such as slip bands, creep and fatigue. It was less successful
with complex alloys, despite special equipment designed by Jaquet to polish small areas
by dabbing them with electrolyte using a sheathed cathode.
Post 1940
Mechanical Polishing
Improved equipment and polishing material emerged gradually in the 1940s and 1950s
which also saw the first and most comprehensive research into mechanical polishing, by
Samuels and his colleagues. The unique nature of this work was that it placed emphasis
on measurement to evaluate stages of mechanical polishing, rather than using subject
viewing. It also included elegant experiments to elucidate details of the basic
microscopic processes involved. Besides a large number of papers published and
lectures given, the field was comprehensively reviewed by Samuels in a book first
published in 1959, revised twice with the latest in 1982.

Steps to Evaluate Mechanical Polishing

The critical experiments in this wide-reaching series and which might well qualify to be
the turning point are the following. Firstly the depths of scratches made by the various
stages of mechanical polishing were measured, employing taper sectioning where the
scratches became small. Secondly the depth of damage beneath these scratches was
determined using polished sections normal to the surface and etchants which revealed
the regions of cold work; these could be matched with etched patterns of specimens
worked to known degrees of compression. This then yielded the depth of material that
had to be removed at each stage of polishing to leave no distortion. The third set of
experiments was to elucidate how these various stages were effected by the abrasive
particles. The scanning electron microscope was an important tool here.
The upshot was that in all cases the removal of materials was by chip formation, which
Samuels group was also studying in the engineering machining of metals. Particle
shape and particle orientation were involved in ascertaining optimum performance
through control of the rake angle. Thus, quantitative standards were set and could be
used in selecting grades of abrasives, their shape and how they were held on paper
backing, polishing laps or cloths. By the time this body of work was completed, graded
powders of diamond were available and have subsequently become universally used in
the later stages of polishing. Here again, Samuels was at the forefront, evolving recipes
for making diamond pastes before they were available commercially and characterising
the efficiency of various sources of diamond.
Optical Microscopy
Optical microscopy also underwent a steady development in design and quality of
lenses, in mechanical robustness and stability and probably most importantly, in the
brightness and stability of illuminating sources. This was particularly the case for those
used for photography of microstructures where unreliable carbon arcs depending on
carbon rods moved by clockwork mechanisms were replaced by much brighter and
stable xenon arc lamps. Given a satisfactory polish, resolution of micro detail was not
usually a problem, even in 1937, provided one was content to be limited by the
wavelength of light. It was contrast between features which was often limiting, despite
ingenuity of etching and use of special high-contrast photographic plates. Plates
approximately 8 cm x 6 cm were universally used until the 1960s, 35 mm roll film
became widely used after the 1960s.
Advances in Imaging
A number of different ways of forming optical images were exploited to obtain either
improved contrast or information about relative heights of features. Contrast was
improved by methods which involved the use of information carried by the phase of
light from features, as distinct from the amplitude of the light waves. This was in the
technique of phase contrast which has had several modified versions. Polarisation, long
established in mineralogy, was also developed for metals but it proved to have only
limited utility, although it was able to produce beautiful coloured photographs.
Interference fringes, produced by splitting the incident illuminating beam and reflecting
part of it to a flat reference reflector, proved of use in studies involving changes in the
level of a polished metal surface induced by mechanical deformation or by
transformations such as the formation of martensite. These interference patterns were in
effect contour maps of the surfaces examined, the vertical distance between the contour

lines being half the wavelength of light. Local changes in specific fringes allowed
estimation of even smaller heights.
Electron Microscopy
By the time these various techniques were understood and in many cases incorporated
into standard microscopes, they were becoming obsolete because of the outstanding
performance of electron microscopes and the multitude of instruments of the electronic
kind. Electron microscopes were first used in metallography in the mid 1940s when
their increased resolution was seen to be their advantage. The fact that electrons only
penetrate metals to very little depth meant that polished specimens had to have their
surfaces replicated by softened films of cellulose acetate, or later by coating with a
carbon layer. Contrast then often had to be enhanced by oblique coatings of a metal. It
was in all a rather difficult procedure and the gain in resolution often yielded little new
information. Early microscopes also suffered from problems of sustaining an adequate
degree of evacuation and sufficient stability of the power supply.
Within a surprisingly few years, these problems had been mastered and great flexibility
introduced in the mechanics of specimen changing, tilting and rotating of the sample.
The big advantage came with the development of thinning techniques which made
areas, albeit small ones, transparent to the electron beam. This led to imaging not only
very small precipitates and particles of various kinds but also of crystalline defects such
as dislocations and even images of the crystal lattice itself. Development was
increasingly rapid and too diverse to catalogue in this article but it is important to
include reference to it because of the unprecedented power of these instruments in so
many ways. It is also relevant to remark that by the 1970s, it came close to
extinguishing training in optical microscopy and thus detaching what was seen in the
electron microscope from the larger relationships of structure optically revealed.
Quantitative Metallography
It was recognised that it was important to preserve the optical expertise, not only as a
reference base but also in day-to-day characterisation and control of microstructure in
industry. Another line of development in metallography also had a notable growth and
reinforced the importance of the optical microscope. This was the technique of
quantitative metallography or quantitative stereometry.
Grain Size
The starting point in quantitative metallography was the apparently simple one of
measuring grain size. The usual method for many years was to compare (by eye) the
sample microstructure with a series of idealised charts and thus pick out a particular
numbered chart as the grain size number. Grains, even in a fully annealed single-phase
alloy take up a complex shape of which the two-dimensional polygon on a polished
surface is not obviously related.
Grain size became increasingly measured by taking the average of the intercepts made
by the grain-boundary traces along specified lengths traversed. In the 1950s, several
investigations led the way to understanding the connections between various estimates
of grain size and became, in fact, part of a broad attack on measurements of structural
features in general. C.S. Smith began this movement in metallography in 1952 and by
1970 it was fully documented in papers and by texts, particularly the books by DeHoff
and Rhines and by Underwood. Serial sectioning was used in some cases to build up an

accurate three-dimensional picture. Typical features given accurate parameters to

characterise them were volume fractions of second phases, separation distances between
phases and the dimensional parameters of various shapes of particles such as spheres,
discs or rods. Increasingly too, these measurements were produced with statistical limits
assigned to them.
Electronic Advances
This was also a period in which automatic instruments were made possible by the
advances in electronics and the introduction of computers. Thus data were collected
with specified sensitivity, collated and eventually plotted graphically if desired. This all
meant that it was possible to make experiments which could be completed in durations
of time reckoned in minutes in contrast to previous manual operation of many hours or
even days of work. This was also an area which metallography shared with the study of
other engineering materials such as ceramics and polymers, and even with biological
and botanical materials.
Concluding Remarks
The foregoing has shown, it is hoped, that metallography has developed by the
accumulation of advances, often small ones, in techniques, instrumentation and basic
understanding of metals and alloys. These have usually been driven by industrial
innovation and needs. This has resulted in gradual turning points, not sudden
revolutions.
Looking back over the 20th century, it is evident that the first third of it was relatively
static, the middle third one of significant development of existing procedures followed
in the final third by the explosive proliferation of instruments utilising all aspects of the
wave-like properties of matter and the power of electronic computing.
Several, indeed many, important areas of metallography have been neglected in this
article. Examples would be measurement of distributions of crystallographic orientation
of grains, analyses of chemical composition of alloys, inclusions and precipitates, nondestructive testing and fractography.
As to the future, this very wide ambit of metallography assures its continued importance
and it is at least certain that existing techniques will be increasingly automated and data
ever more speedily collected and collated. Beyond that it is prudent to remember that it
has been said. Prophecy is difficult, especially about the future.

Primary author: R.C. Gifkins

Source: Materials Australia, Vol. 33 no. 1, pp. 11-13, January/February 2001

For more information on this source please visit the Institute of Materials Engineering
Australia