MET 147

Student’s Copy

ACTIVITY 1: SPECIMEN PREPARATION FOR METALLOGRAPHIC EXAMINATION

I. Introduction

Metallography is concerned with the study of the structures of metals and alloys in
relation to their properties. The true constitution and properties of alloys can be examined
with a microscope only after their representative specimens have been properly prepared.

II. Objectives

1. To familiarize the students with the mechanical techniques in the preparation of metal
specimens for macro- and micro-examinations.
2. To achieve satisfactory specimen preparation in terms of flatness, scratch-free and
mirror-like specimen surface.

III. Materials and Equipment Required

1. Samples of deformed steel bar (bar size nos. 25, 32 or 36)

2. Hacksaw
3. Grinding paper/Emery paper grit nos. 36/40, 60, 100/120, 220/240, 320/360, 600,
800/1000 & 1200/1500
4. Polisher
5. Polishing cloth (3-6 & 0.5-3 microns)
6. Coarse alumina abrasive powder (3-5 microns)
7. Fine alumina abrasive powder (0.5-1 micron)
8. Hair dryer
9. Ethyl alcohol or Methyl alcohol
Diamond suspension/paste (grain sizes: 15, 9, 6, 3, 1 and ¼ µm)
Alumina Oxide suspension (grain sizes: 5, 1, 0.3, 0.1, 0.05 µm)
10. Cotton
11. Tissue Paper
12. Metallurgical Microscope

IV. Procedure

1. Cutting
Metallographic specimen must be a representative of the material to be studied,
and therefore must be properly selected. Prior to cutting, the location where to take the
specimen must be properly chosen.In this activity, use a hacksaw to cut a specimen
from the material under study.The size of the specimens, if applicable,are generally “not
more than 12 to 25 mm (0.5 to 1.0 in.) square, or approximately 12 to 25 mm in diameter
if cylindrical”.The height of the specimen should be enough to make handling during
grinding/polishing convenient (such as 25-30mm). Circular steel samples are cut along
the transverse sections.

2. Mounting
Test specimens which are too small to handle during grinding, are to be mounted.
There are several types of mounting compounds to be used(such as phenolic/bakelite),
depending on the mounting method and type of material to mount.

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3. Grinding
“Grinding should start with the finest paper, platen or stone capable of flattening
the specimen and removing the effects of prior operations, such as sectioning. The
subsequent steps should remove the effects of previous ones in a short time. Grinding
consists of two stages- planar (rough) and fine.”
Hand grinding is to be done uni-directionally on water-irrigated SiC papers (i.e.
120, etc.).Excessive pressure must be avoided which may lead to deep-seated
scratches which are hard to remove but may also alter the structure.

Guidelines:
a. Specimens must be flat on both sides.The section for inspection should be properly
ground to a fine-finished surface depending on the type of examination to perform.
b. The objective of each grinding stage is to grind out completely the old, coarser
scratches and replace them withone set of unidirectional finer grinding
scratches.“When grinding manually, the specimen should be moved back and forth
across the paper to allow for even wear. Between grinding steps, the specimen
should be rotated 45-90º”.
c. Cleanliness is very important throughout the operation to obtain a properly prepared
specimen. Before each stage, the hands and the specimen should be carefully
washed with running water to make sure that no loose, coarse particles are carried
over to the next finer grit grinding stage. Great care must be exercised to prevent any
change in the structure of the specimen, either by overheating or by
deformation.Using water during grinding will wash away grinding debris and act as
coolant. It is good technique never to permit the specimen to feel warm at any stage
of grinding.

After all grinding is done, the specimen must be cleaned thoroughly. Ultrasonic
cleaning in a water/soap solution containing a corrosion inhibitor may prove
beneficial”.

4. Polishing
“Polishing is usually distinguished from grinding by the use of loose abrasive
(≤6µm) embedded in an appropriately lubricated supporting surface. Polishing can be
divided into rough and fine (final) stages”.
It is mandatory that specimen must be carefully cleaned to prevent contamination
by coarser abrasive.

a. After properly cleaning the specimen, rinse with alcohol and then dry with the hair
dryer.
b. Place the appropriate polishing cloth in the polishing wheel and then pour a sufficient
amount of coarse alumina powder (3-5 microns) suspension. The cloth should not
be too wet for this will retard polishing nor too dry as it may cause tarnishing and
may also wear the cloth.
c. In manual polishing, hold the specimen firmly by hand against the rotating polishing
wheel. You may just hold the specimen in steady position or move the specimen
from periphery to center of the wheel and then back. High speeds and excessive
amount of water are avoided for these may pull out embedded materials such as

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inclusions or remove any coatings on the specimen. The ideal time for rough
polishing takes about 2 to 5 minutes.
“The amount of force applied along with the rate of movement of the specimen
during grinding and polishing is a matter of personal preference and experience. In
the preparation of difficult materials such as thermally sprayed coatings or
composites, the operating parameters must be strictly controlled. .
d. From time to time visually inspect the polished surface to check if the desired finish is
sufficient to proceed to the next finer stage. If unable to clearly check the surface,
remove specimen from the polishing wheel and then wash with water and soap.
Rinse with alcohol and then dry.
e. If the surface finish is sufficient, proceed to the next stage. Replace the polishing
cloth in the polishing wheel and pour the fine alumina powder (0.5-1micron)
suspension. At this stage, it is desired to move the specimen in a circular path
around the wheel against the direction of rotation of the wheel. Remember to inspect
the surface from time to time. Ideal time for fine polishing is 1 to 2 minutes.
f. When it appears to have a mirror-like finish, thoroughly wash the specimen with soap
and water. Rinse with alcohol and then blow dry.
g. Examine the polished surface in the microscope to verify if it is free of scratch. If not,
repeat with the polishing steps, either rough or fine polishing, depending on the
depth of scratch.
h. In an as-polished surface, the following features can be detected:
1. Constituents with more than 10% difference in reflectivity (i.e, non-metallic
inclusions in alloys, coatings)
2. Constituents with strong color differences
3. Constituents with large hardness differences
4. Defects such as cracks, pores and pits
i. Polished specimens are ideally stored in desiccators to preserve a mirror-like finish
surface.