Date:

Experiment No 2
AIM: To study procedure of specimen preparation for microscopic
examination and to carry out a specimen preparation.
Objective:
To study procedure of specimen preparation for micro-examination and
to carry out a specimen preparation
Apparatus and Material:
Metallurgical microscope, 1/0, 2/0, 3/0 and 4/0 emery papers, paper
mounting boards, dry and wet polishing mills, alumina powder, fine
polishing clothes, suitable enchant.
Relevance:
A little can be learned regarding the structural characteristics of a metal
by microscopic examination unless the surface that is to be examined is
first prepared according to more to less rigid and precise procedure.
With the use of modern metallurgical microscopic and precision optical
parts where the obtainable resolution may be as great as a fraction of the
wavelength of the light used to illuminate the specimen, it is evident that
perfect specimen preparation is of the greatest importance. Metals and
alloys being opaque, the preparation of specimen is a must to microexamine them. A perfectly reflective surface has to be prepared for the
same to reveal internal details like grain, grain boundaries and
segregation of impurities. Improper preparation- is likely to remove all
important inclusions, erode grain boundaries or temper hardened steel

specimens, ultimately producing a structure superficially at least, which,

upon micro examination, will appear entirely different from that which
is truly representative and characteristic of metal. Obviously an
examination of such a prepared specimen will lead only to erroneous
interpretations and unreliable conclusions.
Theory:
In general, the procedure of specimen preparation consists of first
obtaining a flat semi polished surface by means of polishing the
specimen on series of emery paper of decreasing grit size, or by grinding
on suitable abrasive laps followed by fine and final polishing on one or
more cloth covered lap wheels. This operation ultimately produces a flat,
scratch free (virgin) mirror like surface; the required condition of the
specimen surface before it can be etched and the metallography
appropriately revealed.
The whole procedure involves following steps:
1.
Cutting the specimen or sampling
2.
Mounting the specimen (if required)
3.
Polishing the specimen
4.
Etching
Procedure:
1. Determine the appropriate location and orientation of the specimen
to be cut.
2. Determine the method of cutting.
3. If the specimen is difficult to handle, select suitable amount and
mounting conditions.

4. If the surface to be observed is too uneven or burrs, etc. are present

achieve plane surface by either filing or grinding on coarse grade
emery paper.
5. Take emery papers from coarse to abrasive grit (i.e. 1/0, 2/0, 3/0
and 4/0).The first polishing paper used after the roughing operation
is usually No. O French- Hubert paper (1/0) or its equivalent. The
emery paper is placed on any clean, hard & level surface. The
specimen is rubbed back and forth across the entire length of paper
under moderately applied pressure. While being polished, the
specimen is held so that the new finer scratches being introduced
on the surface are approximately at right angles to the old scratches
resulting from previous flattening/polishing operation. Switch over
to the next finer grade and repeat the same procedure; This is dry
polishing.
6. Select the suitable polishing cloth (geuerally Selvyt cloth) and
polishing abrasive powder (e.g. alumina slurry) for the given
specimen during wet polishing.
7. The polishing wheel mounted with polishing cloth is rotated at
appropriate speed and the specimen is moved continuously from
the center to the periphery of the polishing wheel with moderate
pressure.
The suspended abrasive may be applied to the polishing cloth by
means of a shaker bottle or the other means. This completes wet
polishing.
Note: At frequent intervals during the procedure the specimen
undergoing preparation, as well as hands of the technician should
be thoroughly washed with soap or water.

8. Select suitable etchant (e.g. NITAL) for the specimen and carry out
etching.
9. Immediately after etching, wash the specimen under running water
and dry it with alcohol.
10. Observe the specimen under microscope.
Observation:
1.
Record step-by-step procedure followed indicating the facilities
used and end result obtained at each step in a suitable format.
2.
Observe the etched specimens under a magnifying glass (say 20X)
and comment on the quality preparation.
3.
Develop suitable data-sheet of appropriate abrasive grit or final
polishing and etchant to be used with contributing reasons.
Questions:
1.
What is the significance of preparation of specimen for the microexamination?
2.
List down the various steps required for the preparation of
specimen.
3.
What is the basic difference between low grade numbered emery
paper and high grade numbered emery paper in the intermediate (dry)
polishing process?
4.
What is etchant? Why etching is required? List atleast eight names
of etchant used for different materials, along with their compositions.
5.
List atleast 5 names of cloth used in wet polishing process.
6.
Name the etchant used by you. Give its composition too.
7.
Explain briefly the function f etchant with suitable sketches.
Reference:
1. Principle of Metallographic Practice: G. L. Kehl