1.

0 ABSTRACT

The experiment was about to determine and describe metallographic

and its application to study the microstructure of materials. Metallographic is
the art of preparation of specimens that can be examined by an optical
microscope. Examining a metal sample in the microscope without prior
preparation will not revel informative image of the microstructure. A sample of
stainless steel was used in a series of steps as outlined in the procedure. The
preparation starts by cutting small representative piece of the stainless steel to
be studied. The sample was treated at each stage using different apparatus
and reagents. Thorough cleaning was done at the end of every stage to avoid
transfer of large granules from one step to another. The final product of the
experiment was observed under the metallographic microscope, the
micrographs of both the unetched specimen and the etched specimen were
taken as indicated in the result. The result were analysed and there is a
distribution of grain size. Material specialists are interested to see the grain
boundaries in order to estimate the grain size. The average size in stainless
steel is usually in the order of several to tens micrometres, which can measure
only by use of an optical or light microscope. It will be discussed further in
comparison to the theory and conclusion deduced from discussion of the
result.
1.1 TABLE OF CONTENT

NO CONTENT PAGE

1. List of Figure 1

2. Introduction 2

2.1 Background 2

2.2 Objective 4

2.3 Problem Statement 4

3. Theory 5

4. Experimental Procedure 7

5. Result 15

6. Discussion 18

7. Conclusion 24

8. Reference 25
1.2 LIST OF FIGURES

NO FIGURES PAGES

1 Figure 1.0: Abrasive Cut 7

2 Figure 2.0: Abrasive Cutter 7

3 Figure 3.0: Automatic Mounting Presser 8

4 Figure 4.0: Sample with Hot Mold 9

5 Figure 5.0: Phenolic Powder 9

6 Figure 6.0: Sample with Cold Mold 10

7 Figure 7.0: Grinder 11

8 Figure 8.0: Polisher 12

9 Figure 9.0: Etching 13

10 Figure 10: Optical Microscope 14

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2.0 INTRODUCTION

2.1 BACKGROUND

Metallography consists of the study of the constitution and structure of metals

[1]
and alloys . Much can be learned through specimen examination with the
naked eye, but more refined techniques require magnification and preparation
of the material's surface. Optical microscopy is sufficient for general purpose
examination; advanced examination and research laboratories often contain
electron microscopes (SEM and TEM), x-ray and electron diffractometers and
possibly other scanning devices.

Incorrect techniques in preparing a sample may result in altering the true

microstructure and will most likely lead to erroneous conclusions. It necessarily
follows that the microstructure should not be altered. Hot or cold working can
occur during the specimen preparation process if the metallurgist is not
careful. Expertise at the methods employed to produce high-quality
metallographic samples requires training and practice. The basic techniques
can be learned through patient persistence in a matter of hours. This
experiment takes the student through the metallographic sample preparation
process step-by-step with demonstrations and explanations of sectioning,
mounting, course & fine grinding, polishing, etching and microscopic
examination.

Because of its ability to study objects with highly polished like metals, a
metallurgical microscope ids different from other microscopes. The many
metallurgical microscopes will allow them to explore different fields and
broaden their knowledge with just one tool. The study of metals and alloys and
more specifically metallographic, the microscopic examination of metals and
alloys, a metallurgical microscope, especially a high end one, is generally

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equipped to provide great help in other fields of materials science as well.
After a mirror-like metal surface has been prepared, now the structure can be
observed under optical microscope for analysis. Before interpreting of the
structure that you observe, it is important to understand some of basic
operations of optical microscope in metallurgical study. The optical microscope
magnifies an image by sending a beam of light through the object as seen in
the schematic diagram. The condenser lens focuses the light on the sample
and the objective lenses (10X, 50X, 100X and 400X) magnifies the beam, which
contains the image, to the projector lens so the image can be viewed by the
observer. In interpreting the microstructure, it is helpful to consult with the
phase diagram and to have some knowledge of the composition and thermal
history of the specimen. If both resources are used, phase can be often
identified and the sequence in which they formed can be traced.

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2.2 OBJECTIVES

The objectives for this experiment are [2]:

 To understand the procedure metallographic sample preparation

 To understand basic function of optical microscope and its operation
 To perform analysis from the microstructure’s observation
 To understand the theoretical background of sample preparation and
metallographic specimen

2.3 PROBLEM STATEMENTS

In the study of metallic materials, it is often to analyze the phase exist and
grain size in the structure. However, the details of structure of metals cannot
be seen through naked eyes. In response to this problem, the structure of
metals need to be seen with the aid of microscope. For this experiment, the
metal must be prepared and polished carefully before a good microstructure
observation. Throughout this experiment, the sample need to be prepared by
following several preparatory steps which are cutting, molding, grinding,
polishing and etching.

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3.0 EXPERIMENTAL THEORY

Metallography consists of the study of the constitution and structure of

metals and alloys. Structures, which are coarse enough to be discernible by the
naked eye or under low magnifications, are termed macrostructures. Useful
information can often be gained by examination with the naked eye of the
surface of metal objects or polished and etched sections. Those, which require
high magnification to be visible, are termed microstructures. Thus,
microscopes are required for the examination of the microstructure of the
metals.

Optical microscopes are used for resolutions down to roughly the

wavelength of light (about half a micron) and electron microscopes are used
for detail below this level, down to atomic resolution. When a mirror- like
metal has been obtained, the structure can be observed with the aid of optical
microscope. The optical microscope magnifies an image by sending a beam of
light through the object. The condenser lens focuses the light on the sample
and objective lens with 10X,50X,200X,400X, magnifies the beam which
contains the image, to the projector lens so that the image can be viewed by
the observer.

Incorrect techniques in preparing a sample may result in altering the

true microstructure and will most likely lead to erroneous conclusions. It
necessarily follows that the microstructure should not be altered. Hot or cold
working can occur during the specimen preparation process if the metallurgist
is not careful. Expertise at the methods employed to produce high-quality
metallographic samples requires training and practice. Moreover, basic
techniques can be learned through patient persistence in a matter of hours.
This module takes the student through the metallographic sample preparation

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process step-by-step with demonstrations and explanations of sectioning,
mounting, course & fine grinding, polishing, etching and microscopic
examination.

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4.0 PROCEDURES ON SAMPLE PREPARATION

The preparation of the material for microscopic examination and micro

structural characterization in principal is very simple. There are five basic
processes that you will need to become familiar with such as sample cutting
and sectioning, metallographic mounting, Surface grinding and surface
polishing.

i. Sample Cutting

Sample cutting is the removal of convenient size specimen from large sample
with minimal damage to microstructure with the help of abrasive cut (Figure
1.0) off machine.

a. A suitable abrasive cutting wheel/saw is attached to cutting machine.

Use D-250 of abrasive cutter (Figure 2.0) for mild steel material.
b. Hold the work piece by using the vice provided on the machine
c. In order to minimize the heating of the sample due to the cutting, the
cut-off saws that is equipped with either water-cooling system such as
water.

Figure 1.0: Abrasive Cut Figure 2.0: Abrasive Cutter

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 ii. Mounting/ Moulding

The purpose of this process is to make a smaller specimen easy to hold so that
it can ease the process of grinding to avoid damage to the polishing wheels
during polishing. There are two basic mounting techniques used in this
laboratory such as hot and cold mounting. Cold mounting is used when the
specimen could not undergo hot temperature

Figure 3.0: Automatic Mounting Presser

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Hot moulding process

a. Place sample face down on the small piston inside the press, and lower
the piston into the cylinder by opening slightly the valve on the front of
the press.
b. Approximately 10 gram of Phenolic powder (Figure 5.0) is poured over
the sample, and it will have mounted under 200 psi
c. The cylindrical heater is plugged in and turned on
d. Place the heater around the mold. The heater is thermostatically
controlled and will heat the mold to about 180 °C. Close the valve, and
pump up the cylinder using the hand lever.
e. As the Phenolic heats, it will begin to flow to fill the void spaces, and the
pressure will drop.
f. When the pressure stops rapidly dropping, then let few minutes of
cooling the specimen
g. Crack the valve to release the pressure.
h. Clean any residual powder off of the mold surfaces

Figure 4.0: Sample with Hot Mold Figure 5.0: Phenolic Powder

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Cold Moulding Process

The following process is used to room temperature curing epoxy

process:

a. Place the specimen in the mounting cup

b. Mix epoxy powder and bonding liquid in 1:2 ration in a cup
c. Pour the mixture over the mold
d. Eject the mold.

Figure 6.0: Sample with Cold Mold

iii. Grinding

The goal of the surface polishing is to end up with a planar cross section of
sample free from scratches or disturbed metal introduced by the cutting and
sectioning

a. Ensure that you have a flat surface to begin with and draw the
specimens in one direction across the surface of the water lubricated
abrasive paper
b. A water-cooled abrasive grinder is available to form a flat initial surface
from which to begin.
c. After getting a flat sample on the belt grinder, WASH sample thoroughly.
The hand lapping station has four graded abrasive papers to produce a

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 sequentially finer surface finish. Be sure the water is turned on and
flowing uniformly over the abrasives.
d. Start with the coarsest grit (240) and slowly move the specimen forward
and back across the abrasive. This will produce parallel scratches of
uniform size.
e. Continue previous step until the entire surface of the sample is flat and
then wash the sample thoroughly, and move to the 320 grit abrasive.
f. Repeat this procedure for the 400 grit, 600 grit and the 1200 grit
abrasive, checking after each step to be sure that only those scratches
remain that are due to the smallest grit.

Figure 7.0: Grinder

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 iv. Polishing

Polishing involves the use of abrasives, suspended in a water solution, on a

cloth-covered electrically powered wheel. Standard sized aluminium oxide
powders are applied for general use purposes.

a. Make sure your specimen and hands have been thoroughly cleaned
before polishing
b. Begin with the 9-micron, nylon cloth polishing, apply a small amount of
the aluminium oxide abrasive solution to the polishing cloth.
c. When polishing the specimen, hold it with both hands, apply a moderate
amount of pressure for few minutes.
d. Before proceeding to the next polishing stage, wash and dry both the
specimen and your hands thoroughly then rinse the specimen.
e. Repeat steps 1 to 8 for the (5,3,1-micron) stage
f. Before proceeding to Etching, wash and dry both the specimen and your
hands thoroughly then rinse the specimen with distilled water.

Figure 8.0: Polisher

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 v. Etching

Chemical etching is accomplished by immersing the specimen in a suitable

etchant until the required structure is revealed. During etching, most metals
lose their bright appearance, indicating that etching is taking place. With
practice, one can ascertain the completion of etching by the degree of dullness
of the surface.

a. Place the specimen on the table under the Fume Hood with the polished
surface up.
b. Turn on the Fume Hood. Without touching the specimen surface, clean
the surface with alcohol and let it dry using the hot air gun.
c. Using the Eye-Dropper, apply a few drops of Etchant to the specimen
surface covering the entire metallic surface of the specimen.
d. After about 20 to 30 seconds, rinse the Etchant into the sink with water
and quickly rinse the specimen with alcohol
e. Proceed to Microscopic Examination and if further etching is required
you may return and proceed through steps 1 through 4
f. If the specimen has many scratches and marks or the microstructure
cannot be seen after several etches, return to fine grinding and go back
through the necessary steps.

Figure 9.0: Etching 13 | P a g e

4.1 EXPERIMENTAL PROCEDURE ON OPTICAL MICROSCOPE

a. The specimen was placed on the stage of the microscope under the lens.
b. The microscope’s light was switched on and the light intensity was
altered to number 5 by rotating the light knob.
c. The specimen then was observed by using M5 lens.
d. By using the coarse and the fine knob, the stage was being increased or
decreased until the microstructure of the specimen appear clearly.
e. Then, the magnifying was increased by rotating the turret using M10,
M20, and M40 respectively.
f. Lastly, the result was recorded by drawing a picture of the
microstructure of the specimen.

Eyepiece

Objectiveness
(Threaded into nosepiece)
Stages

Fine Focusing Knob

Illuminator with Bulb

Base

Figure 10: Optical Microscope

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