Department of Materials and Metallurgical Engineering

Bangladesh University of Engineering and Technology, Dhaka

MME 296 Engineering Materials Sessional (1.50 Credits)

Laboratory 1:
Introduction to Metallography

INTRODUCTION
The properties of a material are a direct consequence of the microstructural features of that material. These
structural patterns vary both with the materials themselves and with their manufacturing processes. The
identification of the microstructural features of a material is therefore of paramount importance.
The general microstructural features of most of the common materials can be evaluated with relatively simple and
inexpensive apparatus, known as the metallurgical microscope. To reveal other special features with intricate
details, we require more sophisticated and very expensive microscopes, such as scanning electron microscope,
transmission electron microscope etc. A representative area from the material to be investigated is cut and
specially prepared to reveal its structural features and to be observed under these microscopes. The science of
preparation of samples for investigation under microscope is commonly known as metallography,
Metallography is the study of the physical structure and components of metals, typically using microscopy.
Ceramic and polymeric materials may also be prepared using metallographic techniques, hence the
terms ceramography, plastography and, collectively, materiallography.
The ideal specimen for metallographic examination is a representative block of handy size, having a plane mirror-
like surface with good edge retention, on which the structure of the material can be easily seen and evaluated and
which is practically free from any changes due to the preparation. These changes include deformation, loss of
inclusions, scratches, reaction products or smearing of the individual phases. The preparation of specimens for
observation under a microscope, often regarded as a tedious and frustrating process, is of great importance,
since the true microstructure may be partially or fully obscured by poor technique or execution.

SAMPLE PREPARATION

To produce a distortion-free, polished surface capable of revealing the true microstructure.

Sample preparation consists of a number of rather simple-appearing operations. However, these operations
require great care, precise techniques, extreme cleanliness and much practice before a professional level of
results can be obtained. While the microscope is one of the most sophisticated equipment items used in materials
technology, its value is entirely dependent on the quality of the job done in preparing the specimen for
observation.
Preparation of samples for microstructural examination involves a process consisting of a number of steps. These
steps are as follows (briefly):

1. Selection of sample or specimen

2. Sectioning or cutting: to produce a manageable size sample
3. Rough Grinding: to remove surface deposits or level irregular surfaces.
4. Mounting: to provide a safe means of holding the specimen and protect its edges from rounding.
5. Fine Grinding: to systematically abrade the specimen with a series of grits of decreasing coarseness.
6. Polishing: to remove the remaining scratches and produce the smooth lustrous surface required for
microscopic examination i.e; polishing the specimen to make it flat and mirror-smooth.

7. Etching: to create relief on the surface to be observed and hence to develop the microstructure not normally
visible in the as-polished condition. Inclusions and certain types of defect identification should be
performed prior to application of the etchant.

8. Microscopy:
-Manipulating the microscope to see the structures
-The ‘reading’ or interpretation of the structures observed: to observe, analyze, and record the true
microstructure of the material.

Other tests, such as micro-hardness, provide additional information as required by the authority requesting the
services.

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Selection of sample
Only a small piece of material can be placed on the platform of a metallurgical microscope and only a plane or flat
section of it can be observed under it. The intent of metallographic examination usually dictates the location of the
specimens to be studied. A large body of metal may not be homogeneous either in composition or in structure.
Specimens from locations that are most likely to reveal the maximum variations within the material under study
should be chosen.
Sometimes more than one specimen may be necessary to adequately represent the material. For example, for
the examination of the structure of a casting, specimens should be taken from the zones wherein maximum
segregation might be expected to occur as well from the zones where segregation should be at a minimum. To
examine the structure of fibrous materials or other similar materials having anisotropic properties, both
longitudinal and transverse sections of material are necessary. For the identification of the causes of premature
failures, the test specimens should be taken as closely as possible to the fracture or to the initiation of the failure.
In many cases, specimens should also be taken from a sound area for a comparison of structure and properties.
The nature of the research study dictates the location of test specimens, orientation etc. Sampling for research
studies is usually more extensive than for routine examinations.

Sectioning or cutting
The object of sectioning is to extract specimen of suitable size from the parent material. Sectioning is not a
prerequisite of subsequent preparation, but if done wrongly, the original structure of the material can be changed.
Hence, it can have a drastic effect on subsequent preparation techniques. This is usually associated with heat
and can be readily demonstrated on a hardened steel component where the heat generated during sectioning can
temper the hardened structure. Therefore, in cutting metallographic specimens from the main body of the
material, care must be exercised to ensure proper heat dissipation so that the structure of the metal is not
changed. Hacksaw or abrasive cut-off wheel are ideally suitable for removing a sample from an object. Flame
cutting completely alters the structure of the metal at the flame cut edge and therefore, should not be used for
sectioning.
Polishing of Specimen
Abrasive particles are used in successively finer steps to remove material from the surface of the specimen in
order to produce in it a surface that is perfectly flat and scratch-free when viewed under a microscope. The first
step towards obtaining a perfectly flat and scratch-free surface is often required to rough grind the face of the
specimen on a grinding wheel, a fairly coarse file or a belt sander. The sample is then ground manually by
grinding on a series of emery papers of progressively finer grade. Emery is a natural abrasive containing 55-75%
Al2O3 (corundum) the balance is iron oxide (magnetite) and has Mohs hardness of 8.0. The emery papers are
made by attaching hard abrasive particles onto papers by suitable glue. These must be of the very best quality,
particularly in respect of uniformity of the particle size. Various nomenclatures are used to indicate the fineness of
the hard particles glued on to the emery papers. In some cases, the paper containing the coarsest paper is
designated as No. 3 and the subsequent papers are designated as No. 2, 1, 1/0, 2/0, 3/0 and 4/0. [120/180,
320,600,800,1200,1500]
Before polishing, the specimen may often require mounting for the following reasons:
1. The specimen is too small or of awkward shape for ease of handling in subsequent stages of preparation.
2. To support the outermost edge of the specimen surface to prevent damage or rounding during the
subsequent grinding/polishing operations.
3. The specimen is of delicate or of friable nature.
Specimens may be either mechanically mounted by binding or clamping, mounted in plastics by using a
thermosetting material such as bakelite or phenolic or a combination of the two to obtain optimum results.
To polish at each station, the paper should be held taut with one hand while the specimen is rubbed, with
moderate pressure, back and forth across the abrasive surface in one direction only. This creates a series of
parallel scratches or grind marks on the specimen. Of course the specimen itself must remain in the same
position and must not be turned while working on one particular paper.
When all the marks on the surface being polished are running in one direction and all others have been removed,
the operator should clean the specimen and his hands and then proceed to the next finer paper. During grinding
on the next finer paper, the operator should hold the specimen in such a way that the new, finer set of scratches
will be approximately perpendicular to the existing set of scratches (Fig. 1). Rubbing is continued again in a single
direction until the previous set of coarser scratches is gone and a new fresh set of scratches along the new
direction is produced.

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 FIGURE 1: Appearance of specimen surface at successive stages of grinding.

The process is continued until grinding on the finest paper (the 4/0 grade) is completed. During grinding, the
specimen should not be pressed too hard against the abrasive paper, because the heat generated due to friction
may change the original structure of the specimen. Moreover, the specimen should be held flat against the
abrasive paper throughout the polishing action.
Although considerable time and energy may have been spent during grinding and polishing the specimen, the
failure to observe simple precautions will result in complete obscurity when the specimen is placed on the
microscope stage. This is due to the crisscross lines that will show up under the microscope, signifying the
presence of un-removed scratches (Fig. 2.). Should this be the case, it will be necessary to go back to the coarser
grades of emery paper and start all over again.
After fine grinding the sample using emery papers, final polishing is done. Polishing makes the surface of the
specimen smooth than grinding. As opposed to grinding, several techniques of polishing are used, which can be
divided into chemical, mechanical or electrolytic methods.
The mechanical polishing process is the most commonly used methods of polishing where the sample is pressed
on to a rotating wheel, covered with a cloth such as billiard felt, and a slurry of a finely divided polishing powder. A
number of abrasives have been used in metallography. Silicon carbide (SiC), iron oxide (Fe2O3), chromium oxide
(Cr2O3), cerium oxide (CeO), silica (SiO2), alumina (Al2O3), magnesia (MgO) and diamond powders are most
common abrasives in polishing.

FIGURE 2: Criss-cross lines due to improper grinding.

Etching
Ordinarily a polished metal surface reflects light so equally that the details of the structure cannot be
distinguished. Thus it is necessary to develop contrast in the structure. The most common method to give contrast
is etching, a chemical method where the surface of the sample is corroded by dipping it to a selected corrosive
media for a pre-determined time. Control of the etch time is important in obtaining a sharp, crisp image that
permits resolution of fine details.
The majority of etched specimens are prepared by dissolution of the specimen in selected solutions. This is
known as chemical etching and depends on electrochemical processes, namely oxidation-reduction processes.
The increase in contrast depends on differences in electrochemical potential. For pure metals and single phase
alloys, a potential difference exists between grains of different orientations, between grain boundaries and grain
interiors, between impurity phases and the matrix or at concentration gradients in single phase alloys. For
multiphase alloys, a potential difference also exists between the various phases present. These potential
differences alter the rate of attack, thus revealing the microstructure when chemical etchants are used. Common

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etching reagents used are 2% nital (2 ml nitric acid solution in 98 ml methyl alcohol) for steels, 4% picral (4 g
picric acid solution in 96 ml methyl alcohol) for cast irons, ammonia-hydrogen peroxide (50 ml ammonia, 20 ml
hydrogen peroxide and 50 ml water) for copper-base alloys and dilute hydrofluoric acid (0.5 ml hydrofluoric acid,
99.5 ml water) for aluminium-base alloys.
It must be remembered, however, that there are many features that are best examined on unetched specimens.
Indeed it is a good practice always to look at a specimen in the unetched condition in the first place, particularly
when the specimen has been taken from a component which has failed in service or when it is being used to
sample the quality of the material. Non-metallic inclusions, cracks and cavities are obvious cases of features that
should be viewed before etching.

METALLURGICAL MICROSCOPE
The metallurgical microscope, also known as optical microscope, is a major tool used for the identification of
common microstructural features of most of the common metals and alloys and non-metallic materials.
A metallurgical microscope is similar in optical principles to any other microscope, but it differs from some of them
in the method by which the specimen is illuminated. For example, most of the biological specimens can be
prepared as thin, transparent slices mounted between sheets of thin glass and illumination can be arranged
simply by having a source of light behind the specimen. Metals, on the other hand, are opaque substances and
visible radiation cannot penetrate even a very thin metallic object. Therefore, the study of structures of metals and
alloys with a metallurgical microscope is carried out by using reflected light.
In a metallurgical microscope (Fig. 3), the image produced by the objective lens system is further magnified by the
eye-piece. The total magnification is, therefore, the product of the magnification of the objective lens and the
magnification of the eye-piece. In a metallurgical microscope a magnification of 1000 (usually written as 1000X) is
the practical upper limit. Most work, however, is done at magnification of a few hundred.
To examine a specimen under the microscope, the specimen must first be mounted so that its surface becomes
normal to the axis of the instrument. In any study, one should always begin the examination by visual observation
followed by application of progressively higher magnification. The specimen is brought into focus by using first the
coarse adjustment and then the fine adjustment knobs. Accidental jamming against the specimen surface may
damage the objective. It is a good practice to bring the specimen slightly closer to the objective than necessary for
true focus, using the coarse focusing knob and observing this directly by eye. Then whilst viewing the image
through the eye-piece, true focus is approached by using the fine focusing knob to remove the specimen away
from the objective. This reduces the risk of damaging the objective lens by running it into the specimen. Slight
adjustment can then be made to suit the individual eye. Finally the iris in the illumination system should be closed
to a point where illumination just begins to decrease. This will limit the glare due to internal reflections in the tube.

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 Eye

Eye-piece

Draw Tube
Body Tube

Iris
Lamp
Coarse

Fine

Adjustment
knobs Glass Objective

Specimen
Limb Stage

Clip

Foot

FIGURE 3: Schematic Representation of a Metallurgical Microscope.

It is a mistake to assume that high magnifications, in the region of 500 or 1000, are always most useful. In fact,
they may give a completely meaningless impression of the structure, since the field of observation will be so
small. Directional properties in wrought structures or dendritic formation in cast structures are best seen using low
magnifications of 40X to 100X. Even at 40X a single crystal of say cast 70-30 brass may completely fill the field of
view and the dendritic pattern will be clearly apparent, where as at 500X only a small area between two dendrite
arms would fill the field of view and the nature of the dendritic structure will not be apparent. Thus as a matter of
routine, a low power objective should always be used first to gain a general impression of the structure before it is
examined at high magnification.

REFERENCE
1. ASTM Standard E 3 – 95: Standard Practice for Preparation of Metallographic Specimens.
2. ASW Kurny, A Beginners Guide to Metallographic Laboratory Practice, BUET, Dhaka, 2003.
3. GL Kehl, The Principles of Laboratory Metallographic Practice, 3rd Ed., 1949, Indian Reprint Eurasia, New
Delhi, 1965.

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