METALLOGRAPHY

LABORATORY EXPERIMENT
MANUAL
International Program
Metallurgy and Material Department
2
nd
Sementer
2008/2009

Department of Metallurgy and Materials
Engineering Faculty
University of Indonesia
INTRODUCTION
Metallography can be defined as the visual study of the constitution and
structure of materials. Metallographic examinations can be broadly
classified into two types namely, macroscopic examinations and
microscopic examinations. Macroscopic examinations refer to the
observations carried out at a magnification of X10 of less. Microscopic
examinations, on the other hand, refer to the examination of the structure
at a magnification greater than X10. Microscopic examinations, depending
on the nature of information to be extracted, can be accomplished using an
Optical Microscope (up to X2000) or Scanning Electron Microscope (up to X
50000) or a Transmission Electron Microscope (up to X500000). For most of
the routine purposes in optical microscope is used to obtain first hand
information on the geometric arrangement of the grains and phases in a
material. In order to retain the information visualized using the microscope,
microstructural details are often recorded on a 35 mm film or a Polaroid
film. The photograph thus obtained, revealing the microstructural details,
taken at a magnification of greater than X10 is known as a
photomicrograph. Maintaining a record of the microstructural studies in the
form of photomicrographs is a common practice employed by research
scholars and leading laboratories all over the world.
The study of microstructaral details is important due to its correlation with
the ensuing mechanical properties of the material. As an example, if
material A exhibits a more homogeneous and refined microstructure than
material B, it may very well be anticipated that material A will exhibit better
room temperature properties when compared to material B.
In order to metallographically examine a specimen, it is essential to learn
about the various steps that are required to prepare it. The following
section briefly describe the various steps involved in the metallographic
preparation of the samples.
METALLOGRAPHIC PREPARATION OF THE SPECIMENS
The basic operation outlining the metallographic preparation of the
specimens is as follows:
Selection of the Size of the Specimen : The selection of the size of the
specimen is dependent on the nature of material and the information to be
gathered. Normally, the linear dimensions may vary from 5 mm to 30 mm
while the thickness is kept lower than the linear dimensions.
Mounting the Specimen : Mounting of the specimen is normally carried
out, if the specimen does not permit convenient handling . Plastic mounting
is normally carried out by placing the specimen in a plastic or rubber mold
face down, filling the mold with mounting grade of plastic and allowing it to
dry for a few hours. The plastic mounting is carried out such that the
surface to be examined is exposed on one side of the plastic mount.
Rough Grinding : Rough grinding is carried out on the emery belt surfacer
in order to round off the corners, if necessary and to remove deep scratches
from the surface.
Fine Grinding : Fine grinding involves rubbing of the specimen surface
against the silicon carbide powders bonded onto specially prepared papers.
There are various grit sizes of silicon carbide papers and. the ones normally
used are 400 grit, 600 grit and 1000 grit papers. These papers are
normally mounted on a flat surface. Grinding involves holding the
specimens face downwards on the abrasive paper followed by rubbing in
forward and backward directions until the surface is covered with an even
pattern of fine scratches. The process is repeated with successively finer
grade papers (increase in grit number). With each change of paper, the
specimen should be turned through 90 to facilitate the observation of the
disappearance of the previous scratch marks. In addition, at every new
stage the specimen and equipment should be washed of grit and dirt from
the preceding grinding.
Rough Polishing: This stage involves the polishing of the specimen
surface on a rotating wheel using alumina or diamond abrasive with a
particle size of about 5 microns. Polishing aids include diamond particle
suspension or alumina powder suspension. In the polishing stage, the
specimen is moved around the wheel in the direction opposite to the wheel
itself.
This ensures a uniform polishing action.
Fine Polishing: This stage involves the removal of very fine scratches
and the thin distorted layer remaining from the rough polishing stages.
Fine polishing is usually carried on a polishing wheel using fine alumina
particles with an average size of less than 1 micron (normally 0.5 micron
size is used). Fine polishing, if properly carried out, yields a scratch free
surface ready for etching.
Etching: Etching is carried out on the properly dried specimen obtained
from fine polishing step. Etching involves chemically treating the specimen
surface using a mild acidic or alkaline solution. The etchant differentially
attacks various microstructural features as a result of their different
chemical affinities. This differential attack leads to a non-similar reflection
of light into the objective lens leading to the generation of contrast between
the various microstructural features. After etching is successfully carried
out, the specimen can be taken to the optical microscope for
microstructural examination.
I. THEORY OF WELD STRUCTURE
In the present laboratory session, we will be examining the microstructure
of fusion welded steel. In order to gain better understanding of the various
features we will see in the welded area, it is essential to know about Fe -
Fe
3
C metastable phase diagram and the various microstructural zones that
are normally formed following welding operation. Figure 1 shows a typical
Fe - Fe
3
C metastable phase diagram. The various phases in this phase
diagram which may be of interest to us can be defined as follows:
Ferrite ( -iron):a solid solution of carbon in iron having a
maximum carbon content of about 0.022%.
Austenite ( -iron):a solid solution of carbon in iron formed at
high temperatures containing a maximum carbon content of about
2.11 %.
Cementite (Fe
3
C): a compound of carbon and iron, having a
chemical formula o Fe
3
Cand a carbon content 6.7%.
Pearlite ( + Fe
3
C): a two phase mixture that exists with an
average carbon content of 0.77%. Pearlite has a lamellar structure.
Figure 1. The Fe - Fe
3
C phase diagram. (adapted from Metals
Handbook:
Metallography, Structures and Phase Diagrams, Vol.8, 8th edition,
ASM Handbook Committee, T. Lyman, Editor, ASM, 1973, p.275).
After gaining a basic insight into the Fe - Fe
3
C phase diagram, we will in the
following section try to gain knowledge regarding fusion welding and the
microstructural zones that are formed as a result of fusion welding process.
A fusion weld is normally produced by the electric arc welding process.
There are basically six zones that can be discerned in the welded area and
the parent metal adjacent to it. These zones are created since the various
regions of the parent metal and the weld itself are subjected to different
degrees of heat treatment during the welding process. The six basic zones
are:
a) Deposited Metal Zone Weld Metal Zone
b) Fusion Zone -
c) Grain Growth Zone
d) Grain Refinement Zone The Heat Affected Zone
e) Transition Zone
f) Unaffected Zone
Figure2. Schematic diagram showing six microstructural zones in the
welded steel.
These six zones are distributed in the welded specimen as shown in Figure
2 for hot rolled metal.
The Deposited Metal Zone is the portion where the filler metal was
deposited. In the Fusion Zone, the parent metal was heated to the melting
point and subsequently cooled. These two zones are generally
indistinguishable from each other and make for the Weld Metal Zone.
The Weld metal zone is generally characterized by the presence of two
important microstructural features i.e. Columnar grains and Widmanstatten
structures. As steel is a good conductor of heat, the weld is subjected to
very rapid cooling from its molten state and the result is essentially a
chilled casting having the associated columnar grains. On the other hand, a
Widmanstatten structure appears as a result of large austenite grains being
put through a moderately fast cooling rate.
The Grain Growth Zone exhibits the effect of high temperature treatment at
temperatures somewhat less than its melting point. The high temperature
exposure leads to a significant growth of austenite grains. On cooling to
room temperature, this effect is retained as a region of coarse ferrite grains
and Widmanstatten ferrite and pearlite. The demarcation between grain
growth zone and weld metal zone is generally more distinct than between
the other zones.
In the Grain Refinement Zone , the parent metal is heated into the
temperature range corresponding to the austenite phase in the Fe - Fe
3
C
phase diagram. Because of the relatively lower temperatures, the austenite
grains began to nucleate at many points to form smaller austenite grains
which on cooling will result in fine ferrite and pearlite grains.
In the Transition Zone, the parent metal during welding is heated to the
region where ferrite and austenite coexist. In other words, mostly only
pearlite grains have transformed to small austenite grains. On cooling very
fine pearlite grains with ragged looking boundaries are formed among the
mostly untransformed original ferrite grains.
The Unaffected Zone represents the region of the parent metal that was not
heated beyond the eutectoid temperature (727 C) and there is therefore no
observable structural change.
II. FERROUS AND NON FERROUS
MICROSTRUCTURES
The property of materials totally depends on their microstrectures which
consists of many phases. We have studied about their characteristics in our
last Subjects of Microstructure Analysis Technics of Materials. Each
phases has their own properties and their mechanism to obtain. The
following is some examples of ferrous and non ferrous microstructures:
Fig. 3 Aluminum-killed 1008 steel, normalized after 60% cold reduction to a
final thickness of 0.8 mm (0.03 in.). The ferritic structure contains fine pearlite
(dark areas) at the grain boundaries. 4% nital. 1000
Fig. 4 High-strength low-alloy steel (0.2% C), hot rolled. The structure is ferrite
and pearlite. 4% picral, then 2% nital. 200
Fig. 5 0.20% C steel, water quenched. The structure is lath martensite. 8%
Na2S2O5. 500. (R.L. Perry)
Fig. 6 10B35 steel, austenitized 1 h at 850 C (1560 F), quenched in still water,
and tempered 1 h at 175 C (350 F). Structure is ferrite (small white areas) and
lower bainite
III. THEORY OF HARDENABILITY OF STEEL.
What is hardenability? The primary objective of austenitizing, quenching
and tempering a steel part is to produce a hard martensitic microstructure
in the material. The ease of accomplishing this task is a measure of the
steel alloys hardenability. The higher the hardenability the easier it is to
produce a martensitic microstructure throughout the part. Alloying
elements are added to iron to influence the hardenability of steel. The most
significant being: C, Mn, Si, Ni, Cr and Mo. Additions of V, W and Ti are also
useful depending on the application. If the steel alloy has a very high
hardenability it is possible the produce nearly 100% martensite in large
parts.
Measurement of hardenability is accomplished experimentally through the
use of an end-quench apparatus, illustrated in Figures 1 and 2, that
produces a severe quench at one end of an austenitized steel bar. The
linear heat transfer through the length of the bar provides an infinite
number of continuous cooling paths that can be correlated to the kinetics of
the decomposition of austenite. The quenched end is nearly 100%
martensite. At some distance from the quenched-end, for HSLA steels, the
microstructure becomes pearlite and ferrite. In between, mixtures of
martensite, bainite, ferrite and pearlite
1
are possible depending on the
distance from the quenched end and the specific alloy being evaluated.
SCOPE
In accordance with the subject matter covered in the present manual, the
scope of this laboratory exercise will be two fold:
1. To obtain experience in the metallographic preparation of metallic
specimens;
1
Pearlite is not a phase. It is a mixture of ferrite and cementite (Fe3C).
2. To observe the various microstructures of various metal ferrous,
non ferros , and of welded mild steel joint;
3. To observe the effects of cooling rate to the amount of martensite
and to the hardness of a steel bar.
PROCEDURE
Experiment 1
In this experiment, students will assigned to do a sample preparation, start
from cutting and mounting the sample. Each student will have one specific
microstructure sample of their own, and the other 3 sample ferrous and
nonferrous which have been prepared by the instructure for a whole group
member.. Besides the 3 samples, each student have one sample to be heat
treating to be prepared and observed, and one macrostructure sample. All
the samples have to be obreved with optical microscope, and to be
analyzed the microstructure. Sample Preparation have the steps as
follows;
1. Grind the specimen using the coarser grade silicon carbide paper laid
on the hand grinder. Hold the specimen face downwards on the
silicon carbide paper and rub forwards and backwards with as even a
pressure as possible to obtain an even pattern of finer scratches.
2. Wash the specimen and repeat step 1 using the finer grade silicon
carbide paper. The specimen should be turned through 90 to
facilitate removal of the previous scratch marks.
3 Wash the specimen when only fine parallel scratch marks are
obtained.
4. Polish the specimen using a cloth-covered rotating disc with Alumina
(fine abrasive aluminum oxide powder, suspended in water ) as the
polishing agent until a flat and scratch-free mirror -like finish is
obtained.
5. Wash and dry.
6. Etch the surface of the specimen with 2% Nital (2 parts of
concentrated nitric acid and 98 parts of ethyl alcohol by volume ) for
15 to 25 seconds.
7. Wash and dry the specimen using a specimen drier.
8. The specimen is now ready for observation.
9. Observe the specimen under a optical microscope.
10. Ask the experiment supervisor to have a look and if he is satisfied
that your preparation has produced clearly observable
microstructures then proceed to step I 1. If not, repolish and re-etch
the specimen until the microstructures are observable.
11. Sketch the general microstructural arrangement of the various
distinguishable zones stating the magnification used. Your sketches
are to be of high quality. Label all important features neatly.
The photograph of the sample have to be made in micro( more than 100X)
magnification and macro scale(less than 100X) magnification .
Experiment 2
In this laboratory experiment will consist of Photomicrograph making and
a discussion of some of the microstructures features present in steeel and
nonferrous alloys. How the microstructure is modified by thermal
processing (heat treatment) is part of this experience. An optical Olympus
microscope will be used to present alloy microstructures. The alloys
selected are presented in Table I.
Table I. Summary of specimens prepared for viewing from the Metallurgy
Departments metallography sample collection. The listing is in the order of
presentation. Composition is weight percent unless otherwise specified.
Sample Description
1
2
3
4
Heat Treatment Sample
Macrostructure
Macrostructure
A photomicrograph of each alloy listed in Table I have to be made by
students and they have to make note of phases and microstructure
features identified during the lecture. This document with student notations
is the laboratory report. Turn this document in at the end of the laboratory
class.
As the instructor projects each specimen, (1) sketch the basic
microstructural features and label these features as they are identified, or
(2) identify features on the photomicrographs supplied.
Experiment 3
The recommended austenitizing temperature for medium steel is between
845-950C.
2
The student is expected to research other aspects of the heat
treatment process such as: quenching, tempering and the role of alloying
elements on hardenability. A standard Jominy end-quench specimen will be
heated to the suggested temperature and placed in the Jominy end-quench
test apparatus. After the quenching and cooling process is completed, a
flat is ground on the longitudinal axis of the Jominy bar. A series of HRC
hardness measurement will be made at approximately 1/16-inch intervals
along the length of the bar. This data can be compared to published and
computed data.
2
ASM Metals Handbook, 8
th
edition, Volume 4, Heat Treating, American Society for Metals, Metals
park, Ohio 44073, p.29.
Figure 7. Schematic of Jominy end-quench facility. After Smith.
3
Formal Pre experiment Reports
Write the report for readers with a broader background then what is
expected for memorandum reports, including:
Team Information
Team Information transmittal will contain details of team member.
Who in the team was in charge to some kinds of materials
observed.
Summary
Be concise, 100 words or less, present primary objectives, how
objectives were accomplished and the most important
conclusions.
Introduction
Background information developed, usually from the literature
research, to acquaint reader with the problem and the purpose
for carrying out the work (objective of the experiment work).
Experimental Procedure
Discuss the equipment used and any relevant details. For
example, calibration of the equipment.
Final Report
Pre experiment Report will be attached together with Final Report. Final
report is consist of:
Experimental Results
Present the results in the appropriate from. For example, present
the data as computations, as tabulated data or in figures
(photographs or graphs).
Discussion of Results
The main point of the discussion is to determine if your
experimental measurements have any correlation to
3
William F. Smith: Foundation of Materials Science and Engineering, second edition, McGraw-
Hill, New Your, 1993, p. 457.
measurements made by others. Are the results valid? Why?
Were any problems encountered with the experiment design?
Conclusions
Prepare very concise statements about the experiment.
Possibilities are; what was learned, quality of the engineering
data, problems with the experimental study and what
improvements could be made if the experiment were repeated.
References
List reference in the order they are used in to report. Identify in
the report where references are used.
Appendices (Attachements)
Use an appendix for any computations or lengthy discussions that
is important to the knowledge base, but would detract from the
main flow of ideas in the report.
Tables
Tabulated Data
Figures
Photographs, graphs or other artwork
A set of question have to be answered in the Final report
Reference Examples
Place the references at the end of the written report. There are three types
of references. There are several accepted formats. The goal is to assure
the reader can find the reference in the library.
Technical Journals
Author: Journal, year, ser., vol., pp.
Cahn, J.W.: Trans TMS-AIME, 1968, vol. 242, p. 166.
Books
Author: Book, edition, vol., page, Publisher, Place, Date.
Barrett, C.S.: Structure of Metals, p.25, McGraw-Hill, New York,
1954.
Private Communications
Name: Date, Place, Address.
Kellar, J.: January, 2002, South Dakota School of Mines and
Technology, 501 E. St. Joseph St., Rapid City, SD, 57701-3995.
Standard Numbering Conventions for Appendices, Tables and
Figures
Appendix A, B, C, D --- (Capital letters)
Table I, II, III, IV --- (Roman numerals)
Figures 1, 2, 3,4 --- (Numbers)
Appendix Example
The appendix title must stand-alone. This means reference to the main
report is not needed to understand what the author is demonstrating.
Consider the following.
Appendix A: Derivation of the equation for the theoretical shear strength of
a crystalline solid. This model assumes deformation involves entire planes
of atoms sliding over each other.

1
]
1

,
_

,
_

1
]
1

,
_

1
]
1

,
_

'

1
]
1

,
_

'

,
_

2
G
d 2
Gr
.
r
x 2
sin
d 2
Gr
is result final The
.
d 2
Gr
k or
r
x 2
k
d
Gx
Therefore,
.
d
x
where , G stress shear the
and , ) sin( ion apporximat angle small the using by k constant the Evaluate
.
r
x 2
sin k
r
x 2
sin
A r
C 2
A
F
is stress shear applied the therefor and
,
r
x 2
sin
r
2
C
dx
dV
F
as defined is force the
,
r
x 2
cos C V V PE
is stress shear applied an under plane, lower the over
glide to forced is plane top the as crystal, the in change energy potential The
o
max
o
o
o
o
o o o
o o
o
ref
The above is excessively complicated and therefore could distract from the
flow of ideas. This appendix could be addressed from the main report as
follows.
The theoretical strength of a crystal, assuming the deformation process
involves the sliding of entire planes of atoms over one another, is shown to
be .
2
G
d 2
Gr
o
max

This result is developed in Appendix A.

Table Example
Like the appendix title, the table caption must also stand-alone. Table
captions are always located above the table body.
Table 1. Summary of ASTM E112 grain size measurement obtain
from a hot-rolled steel rod. Results from ten independent
measurements.
Longitudinal Specimen Transverse Specimen
n Grain Size n Grain Size

ASTM
E112 Micron-metersASTM E112 Micron-meters
Average 9.93 10.2 10.14 9.5
StdDev 0.15 0.5 0.09 0.3
Max 10.11 10.8 10.29 9.8
Min 9.78 9.6 10.07 9
Figure Example
Figure captions must also stand-alone. Figure captions are always located
below the figure.

Figure 1. Hot rolled steel rod. The left figure is from the round (longitudinal
cross-section) and the right figure is from the transverse cross-
section. The arrow in the transverse specimen designates the
longitudinal axis of the rod. The dark regions in the
photomicrograph are pearlite. The white magnification bars are
50 micron-meters long on the photomicrograph.
Each group (consist of at least 2 Student) will grind,mounting, polish and
etching
List of Materials;
1. Carburized Steel; Medium Carbon Steel, Mild Steel
2. Welded Steel
3. Plating Steel
4. Aluminium Alloy;AC4B (Al-Si)
5. Cu-Zn (Brass Alloy)
6. Al-Mg-Si