Experiment No: 2

Aim:
To study procedure of specimen preparation for microscopic examination and to
carry out a specimen preparation.

Introduction

Specimen preparation or polishing is necessary to study its micro-structure, because the

metallurgical microscope discussed earlier makes use of the principle of reflection of light (from
the specimen) to obtain the metal structure. Satisfactory metallographic results can be obtained
only, when the specimen has been carefully prepared. Even the most costly microscope will not
reveal the metal structure if the specimen has been poorly prepared. A properly prepared metal
specimen is flat, does not contain scratches, its nicely polished, and suitably etched.

Metallography

 Metallography is the study of the physical structure and components of metals, typically
using microscopy.
 Precision metallurgical sample preparation is a key step in performing reliable
metallurgical testing.
 Facilitate examination and interpretation of microstructural features.
 To find out various phase present in material.
 Improper preparation methods may obscure features, and even

Procedure
The procedure for preparing the specimen for both macro and micro-examination is the
same, except that in the later case the final surface finish is more important than in the
former.
1. Selection of specimen
When investigating the properties of a metal or alloy, it is essential that the, specimen should
be selected from that area (of the alloy plate or casting) which can be taken as representative
of the whole mass.
2. Cutting of the specimen
After selecting a particular area in the whole mass, the specimen may be removed with the
help of a saw, a trepanning tool, an abrasive wheel, etc.
3. Mounting the specimen
If the specimen is too small to be held in hand for further processing, it should be mounted
machine in the thermoplastic resin or some other low melting point alloy.

Material Science & Metallurgy (2131904)

Mechanical Engineering Department
Government Engineering College Bhavnagar
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 Experiment No: 2

Mounted specimens

4. Obtaining Flat Specimen Surface

It is first necessary to obtain a reasonably flat surface on the specimen on the specimen. This
is achieved by using a fairly coarse file or machining or grinding, by using a motor driven
emery belt.
5. Intermediate and Fine Grinding
Intermediate and fine grinding is carried out using emery papers of progressively finer
grade. The emery papers should be of very good quality in respect of uniformity of particle
size Four grades of abrasives used are: 220 grit, 320 grit, 400 grit, and 600 grit (from coarse
to fine); the 320 grit has particle sizes (of the silicon carbide) as about 33 microns and 600
grit that of 17 microns ( 1 micron =1/1000 mm).The specimen is first ground on 220 grit
paper, so that scratches are produced roughly at right angle to those initially existing on the
specimen and produced through preliminary grinding or coarse filing operation.
Having removed the primary grinding marks, the specimen is washed free of No. 220 grit.
Grinding is then continued on the No. 320 paper, again turning the specimen through 90°
and polishing until the previous scratch marks are removed. The process is repeated with the
No. 400 and No. 600 papers. Grinding with the No.200, No.320, etc., papers could be done
in the following ways:
The specimen may be hand-rubbed against the abrasive paper, which is laid over a flat
surface such as a piece of glass plate. The abrasive paper may be mounted on the surface of
a flat, horizontally rotating wheel and the specimen held, in the hand, against it. In either
case, the surface of the abrasive paper (with water proof bases) shall be lubricated with
water so as to provide a flushing action to carry away the particles cut from the surface.

Material Science & Metallurgy (2131904)

Mechanical Engineering Department
Government Engineering College Bhavnagar
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 Experiment No: 2

Fine grinding Emery paper for grinding

Belt grinder Emery paper for belt grinder

6. Rough Polishing
A very small quantity of diamond powder (particle size about 6 microns) carried in a paste
that is oil-soluble is placed on the nylon cloth-covered surface of a rotating Polishing wheel.
The lubricant used during the polishing operation is specially prepared oil. The specimen is
pressed against the cloth of the rotating wheel with considerable pressure and is moved
around the wheel in the direction opposite to rotation of the wheel to ensure a more uniform
polishing action.

Material Science & Metallurgy (2131904)

Mechanical Engineering Department
Government Engineering College Bhavnagar
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 Experiment No: 2

Double Disc polishing machine Single Disc polishing machine

7. Fine Polishing
The polishing compound used is alumina (Al2O3) power (with a particle size of 0.05
microns) placed on a cloth covered rotating wheel. Distilled water is used as a lubricant.
Fine polishing removes fine scratches and very layer remaining from the rough polishing
stage.
8. Etching
Even after fine polishing, the granular structure in a specimen usually cannot be seen under
the microscope; because grain boundaries in a metal have a thickness of the order of a few
atom diameters at best, and the resolving power of a microscope is much too low to reveal.
In order to make the grain boundaries visible, after fine polishing the metal specimen are
usually etched. Etching imparts unlike appearances to the metal constituents and thus makes
metal structure apparent under the microscope

Sr. Type of
No. Etchant Composition Uses

1. Nital (i)Cone, Nitric acid 2CC For etching steels, grey cast
(ii) Absolute methyl 98CC iron
alcohol & black head malleable.

2. Acid ammonium (i)Hydrochloric acid 10CC For etching stainless steels.

persulphate (ii) Ammonium per- 10gms
sulphate 80CC
(iii) Water

3. Ammonia hydrogen (i)Ammonium 50CC The best general Etchant

peroxide hydroxide (0.880) 20- for copper, brasses and
(ii) Hydrogen peroxide 50CC bronze
(3%solution) 50 CC

Material Science & Metallurgy (2131904)

Mechanical Engineering Department
Government Engineering College Bhavnagar
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 Experiment No: 2

(iii) Water

4. Dilute hydrofluoric (i) Hydrofluoric acid 0.5 CC A good general Etchant for
acid (ii) Water 99.5 Al and its alloys (apply by
CC swabbing)

5. Keller’s Reagent (i)Hydrochloric acid 1 CC For (immersion) etching of

(ii) Hcl 1.5 CC Duralumin type alloys
(iii) HNO3 2.5 CC
(iv) Water 95 CC

6. Mixed nitric and (i) Nitric acid 50 CC For etching Nickel and
acetic acids (ii) Glacial acetic acid 50 CC Monel metal

Table. 1 Etching regents for Microscopic Examination

Method:
Before Etching, the polished specimen is thoroughly washed in running water.
Then, the etching is done either by
1. Immersing the polished surface (of the specimen) in the etching reagent or by
2. Rubbing the polished surface gently with a cotton swab wetted with the etching Reagent.
After etching, the specimen is again washed thoroughly and dried. Now, the specimen can be
studied under the microscope. Etching reagents for microscopic examination.

Conclusion:

A microstructural image showing microstructure of the sample prepared.

Material Science & Metallurgy (2131904)

Mechanical Engineering Department
Government Engineering College Bhavnagar
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