INTRODUCTION TO METALLOGRAPHY

Metallography:
Metallography or microscopy consists of the microscopic study of the structural
characteristics of a metal or an alloy. The microscope is by far the most important
tool of the metallurgist from both the scientific and technical stand points. It is
possible to determine grain size, shape, and distribution of various phases and
inclusions, which have a great effect on the mechanical properties of the metal. The
microstructure will reveal the mechanical and thermal treatment of metal and it may
be possible to predict its expected.

Experience has indicated that success in microscopic study depends largely upon
the care taken in the preparation of the specimen.

The steps required to prepare a metallographic specimen properly are:

1. Sampling:
The choice of a sample for microscopic study is very important. If a failure is to be
investigated, the sample should be chosen as close as possible to the area of failure
and should be compared with one taken from the normal section.

If the material is soft, such as non-ferrous metals or alloys and non-heat treated
steels, the section may be obtained by manual hacksawing. If the material is hard,
the section may be obtained by use of an abrasive cut off wheel or diamond cut off
wheel. The specimen should be kept cool during the cutting operation as the heat
generated during cutting may alter the microstructure of the material.

2. Rough grinding:
Whenever possible, the specimen should be of a size that is convenient to handle. A
soft sample may be made flat by slowly moving it up and back across the surface of
a flat smooth file. The soft or hard specimen may be rough ground on a belt sander,
with the specimen kept cool by frequent dropping in water during the grinding
operation. In all grinding and polishing operations the specimen should be moved
perpendicular to the existing scratches. This will facilitate recognition of the stage
when the deeper scratches have been replaced by shallower ones characteristics of
the finer abrasive. The rough grinding is continued until the surface is flat and free of
nicks, burrs, etc., and all scratches due to hacksaw or cutoff wheel are no longer
visible.

3. Mounting:
Specimens that are small or awkwardly shaped should be mounted to facilitate easy
handling in intermediate and final polishing operations.

Procedure:
1. Take an aluminium foil or a smooth surface and apply grease on it.
2. place the specimen on the smooth surface in such a way that the face on which
the metallographic observation has to be done is to face the smooth surface.

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3. Take a cold setting die and apply grease on its inside walls for easy ejection of the
mount.
4. Place the die on the smooth surface taking care that the sample is positioned at
the centre of the die.
5. Pour alternate layers of thermoplastic resin (cold setting powder) and bonding
liquid on and around the sample inside the die.
6. Pour approximately correct volumes of powder and liquid. Excess pouring of any
one of these two elements may damage the quality of the mount.
7. Pour the powder and liquid till the convenient size of the mount is achieved i.e.
approximately more than half of the height of the die.
8. Allow the mixture to get solidify. It may take few minutes.
9. Then the mount may be ejected from the die by tilting back the die. The mount at
this moment is in hot condition and will be cooled in air.
10. After cooling to room temperature, grind the back of the mount for flatness.
11. Now the mount is ready for further operations.

4. Intermediate polishing:

After mounting, the specimen is polished on a series of emery papers containing

successively finer abrasives; the first paper is usually 220,320,400,600 and then with
fine papers viz. 1/0, 2/0, 3/0 and finally 4/0.
The intermediate polishing operations using emery paper are usually done dry;
however, in certain cases, such as the preparation of soft materials, silicon carbide
abrasive may be used.

5. Fine polishing:

The time consumed and the success of the fine polishing depends largely upon the
care that was exercised during the previous polishing steps. The final approximation
to a flat scratch-free surface is obtained by use of a high speed rotating wheel
covered with a special cloth (Duro/Selvyt) that is charged with carefully sized
abrasive particles. Although a wide variety of abrasive powders are available the
preferred one is Gamma form of aluminium oxide (Alumina) for ferrous and copper-
based materials and their alloys.
A properly polished sample will show only the nonmetallic inclusions and will be
scratch free.

Single disc polisher Doubel disc polisher Cold setting powder &
resin
6. Etching:
The purpose of etching is to make visible the many structural characteristics of the
metal or ally. The process must be such that the various parts of the microstructure

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may be clearly differentiated. This is accomplished by use of an appropriate reagent,
which subjects the polished surface to chemical action.
If alloys composed of two or more phases, the components are revealed during
etching by a preference attack of one or more of these constituents by the reagent
because of difference in chemical composition of the phases. In uniform single-
phase or pure metals, contrast is obtained and grain boundaries are made visible
because of differences in the range at which various grains are attacked by the
reagent. Light from the microscope hitting the side of these valleys will be reflected
out of the microscope making the grain boundaries appears as dark lines.
The selection of the appropriate etching reagent is determined by the metal or alloy
and the specific structure desired for viewing.

The following table lists the most commonly used etchants

Etchant Composition Conc. Conditions Comments

33 ml
Distilled water For etching martensitic
1.5 Immersion etching
Kalling's No. CuCl2 stainless steels. Martensite
grams at 20 degrees
1 Hydrochloric acid will be dark and the ferrite
33 ml Celcius
Ethanol will be colored.
33 ml

CuCl2 5 grams Immersion etching For etching duplex stainless

Kalling's No.
Hydrochloric acid 100 ml at 20 degrees steels and Ni-Cu alloys and
2
Ethanol 100 ml Celcius superalloys.

Excellent for aluminum and

Distilled water 190 ml
10-30 second alloys - immersion for 10-20
Nitric acid 5 ml
Kellers Etch immersion. Use seconds ; titanium alloys
Hydrochloric acid 3 ml
only fresh etchant immersion for 10-20
Hydrofluoric acid 2 ml
seconds.

Distilled water 92 ml Excellent for titanium and

Krolls
Nitric acid 6 ml alloys. Swab specimen up to
Reagent 15 seconds
Hydrofluoric acid 2 ml 20 seconds.

Most common etchant for

Fe, carbon and alloys steels
and cast iron - Immerse
Ethanol 100 ml Seconds to sample up from seconds to
Nital
Nitric acid 1-10 ml minutes minutes; Mn-Fe, MnNi, Mn-
Cu, Mn-Co alloys -
immersion up to a few
minutes.

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 For etching Ni, Ni-Cu and
10
CuSO4 Immerse or swab Ni-Fe alloys and
Marble's grams
Hydrochloric acid for superalloys. Add a few
Reagent 50 ml
Water 5-60 seconds. drops of H2SO4 to increase
50 ml
activity.