UNIVERSITI TEKNOLOGI MARA

FAKULTI KEJURUTERAAN MEKANIKAL

Program: Bachelor of Mechanical (Hons) Mechanical (EM220)

Course : Dynamic and Materials Lab 1
Code : MEC 424

Lab 1
Introduction to Sample Preparation and Optical Microscope
For Metallographic Observation

Name
: Haziman Bin Abdullah
I/D Student: 2007126805
Group
: EMD4M5
Date
: 21 July 2008
Lecture
: Pn. Koay Mei Hyie

Lab Session

: 21 JULY 2008
(Date)

Report Submission

: 28 JULY 2008
(Date)

Staff Approval

:
(Signature)

CONTENT:
page

1.0) INTRODUCTION AND THEORY

02

1.1) Sample Preparation:

a) Cutting.

02

b) Molding.

03

c) Grinding.

04

d) Polishing.

04

e) Etching.

05

1.2) Introduction to Optical Microscope

05

2.0) EXPERIMENTAL PROCEDURE

06

3.0) RESULT

07

4.0) DISCUSION

08

5.0) CONCLUSION

10

6.0) REFERENCE

10

1.0) INTRODUCTION AND THEORY

Metallographic is the study of a materials microstructure. Analysis of a materials
microstructure aids in determining if the material has been processed correctly and is
therefore a critical step for determining product reliability and for determining why a
material failed. The basic steps for proper metallographic specimen preparation include:
cutting and sectioning, mounting, grinding, polishing, etching and microscopic analysis.
1.1 Sample Preparation:
In the study of metallic materials it is often to analyze the phase exists and grain size
in the structure. Details of the structure of metals are not readily visible through
naked eyes, but grain structures in metals may be seen with the aid of microscope.
Metal characteristics such as grain sizes, effect of heat treatment, and carbon content
of steels may be determined by studying the micrograph. For this purpose, the metal
that we use in metallurgical examination must prepare and polished carefully before a
good microscopic picture can be seen. There is important to ensure that the surface is
totally flat and smooth before seeing it under microscope. Any irregularity will
appear as a dark surface and will confuse the observer who attempts to analyze a
structure. In order to obtain this smooth flat surface, several preparatory steps are
required.
(a) Cutting.
- The first step in sample preparation is raw material selection. After the specimen
had been selected, it goes to the cutting process. When cutting a specimen from a
larger piece of material, care must be taken to ensure that it is representative of the
features found in the larger sample, or that it contains all the information required to
investigate a feature of interest.
One problem is that preparation of the specimen may change the microstructure of
the material, for example through heating, chemical attack, or mechanical damage.
The amount of damage depends on the method by which the specimen is cut and the
material itself.

Abrasive wheel cutter

Low speed precision cutter

(b) Molding.
- Mounting of specimens is usually necessary to allow them to be handled easily. It also
minimizes the amount of damage likely to be caused to the specimen itself. Specimens
can be hot mounted (about 150 C) using a mounting press either in a thermosetting
plastic example phenolic resin or a thermosoftening plastic example acrylic resin. If hot
mounting will alter the structure of the specimen a cold-setting resin can be used
example epoxy, acrylic or polyester resin. Porous materials must be impregnated by
resin before mounting or polishing, to prevent grit, polishing media or etching being
trapped in the pores and to preserve the open structure of the material. Cold mounting
materials are used to encapsulate samples that cannot withstand the heat and pressure of
compression mounting, when better flow and penetration of the mounting material is
needed or when a large quantity of samples must be encapsulated at once.

Apparatus hot mounting:

Electro-hydraulic specimens mount press

Small specimen mounted in thermosetting

plastic

Apparatus cold mounting:

Disposable Mounting Cups

Small specimen mounted in thermosoftening

plastic

(c) Grinding.
- Grinding is required to planar the specimen and to reduce the damage created by
sectioning. The planar grinding step is accomplished by decreasing the abrasive
grit/ particle size sequentially to obtain surface finishes that are ready for polishing.
The specimen is first moved back and forth on the coarse grit paper until all the
scratches go in one direction and then the specimen must be thoroughly cleaned
before moving to a finer grit. Rough grinding is to remove rough scale and gross
imperfections on the surface of sample. Fine grinding is to improve surface until it
begin to shine and reflect light slightly.

Roller grinder.
(d) Polishing.
- Polishing can categories by two steps, rough polishing and fine polishing. Rough
polishing, the purpose of the rough polishing step is to remove the damage produced
during cutting and grinding. Proper rough polishing will maintain specimen flatness
and retain all inclusions or secondary phases. By eliminating the previous damage
and maintaining the micro structural integrity of the specimen at this step, a minimal
amount of time should be required to remove the cosmetic damage at the final
polishing step. Fine polishing, the purpose of final polishing is to remove only surface
damage. It should not be used to remove any damage remaining from cutting and
planar grinding. If the damage from these steps is not complete, the rough polishing
step should be repeated or continued.

Manual polishing a specimen.

(e) Etching.
- The purpose of etching is to optically enhance micro structural features such as grain
size and phase features. Etching selectively alters these micro structural features
based on composition, stress, or crystal structure. The most common technique for
etching is selective chemical etching and numerous formulations have been used over
the years. Other techniques such as molten salt, electrolytic, thermal and plasma
etching have also found specialized applications. Chemical etching selectively attacks
specific micro structural features. It generally consists of a mixture of acids or bases
with oxidizing or reducing agents.

Etching the specimen.

1.2 Introduction to Optical Microscope:

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 had been observe, it is important to understand some basic operations of optical
microscope. The optical microscope magnifies images by sending a beam a light
through the object as seen in schematic diagram. The condenser lens focuses the light
on the sample and the objective lenses magnify 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, phases can be often identified and sequence in which they
formed can be traced.

Illumination in a metallurgical microscope.

2.0) EXPERIMENTAL PROCEDURE:

1. First step in sample preparation is raw material selection. After the specimen had
been selected, it goes to the cutting process. Cut the specimen using the
recommended machine.
2. Use a mounting press if hot mounting to clothing the specimen and grind any
rough surface lightly to make them level.
3. Sand the surface from rough to finer grit paper. Important, grinding process most
do in one direction and then the specimen must be thoroughly cleaned before
moving to a finer grit.
4. Change to a finer grit and rotate the specimen to show the new lines. Be sure to
clean the specimen thoroughly between each grit change and carefully avoid
contaminating the felt on the polishing wheel.
5. Take a mounted specimen to the polishing wheel. Turn on the wheel and add a
little slurry to the felt surface. Gently press the specimen to the wheel surface and
move it opposite direction of the wheel rotation. Move the specimen around the
wheel several times and clean with distilled water then check the surface. When it
becomes mirror bright, it is ready to etching.
6. Apply the etchant the surface of the specimen using a reagent and count the
limitation time. Rinse with water and immediately follow with an alcohol rinse
from the wash bottle. This will remove the water and prevent rusting. Allow the
alcohol to dry.
7. If the microstructure is not visible, apply the step number 5.
8. Observe each specimen and determine the microstructure and sketch the result.
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3.0) RESULT:

1) Lens focuses M5/0.10

Ferrite

Martensite

2) Lens focuses M20/040

Ferrite

3) Lens focuses M40/0.65

Ferrite

Pearlite

4.0) DISCUSION:

Grinding One Direction.

The orientation of the specimen can have a significant impact on the preparation
results, especially for specimens with coatings. In general, when grinding and
polishing materials with coatings the brittle component should be kept in
compression. In other words, for brittle coatings the direction of the abrasive should
be through the coating and into the substrate. Conversely, for brittle substrates with
ductile coatings, the direction of the abrasive should be through the brittle substrate
into the ductile coating.
Specimen Microstructure.
Grinding process cannot change or affect the microstructure specimen because when
the grinding process, firstly we are use low grid size for abrasive paper to remove
rough scale and gross imperfections on the surface of sample. After that change the
high grid size when the surface specimen clean to improve the surface until it begins
to shine and reflect light slightly before go to polishing process.
Purpose Etching the Specimen.
The purpose of etching is to optically enhance microstructural features such as grain
size and phase features. Etching selectively alters these microstructural features based
on composition, stress, or crystal structure. The most common technique for etching
is selective chemical etching and numerous formulations have been used over the
years.
Different Phase Exist In Iron-Iron Carbide during Microstructures Changes.
All materials exist in gaseous, liquid, or solid form (usually referred to as a phase),
depending on the conditions of state. State variables include compositions,
temperature, pressure, magnetic field, electrostatic field, gravitational field, and so on.
The term "phase" refers to that region of space occupied by a physically
homogeneous material. However, there are two uses of the term: the strict sense
normally used by scientists and the somewhat looser sense normally used by
materials engineers.
In a phase diagram, however, each single-phase field (phase fields are discussed in a
following section) is usually given a single label, and engineers often find it
convenient to use this label to refer to all the materials lying within the field,
regardless of how much the physical properties of the materials continuously change
from one part of the field to another. This means that in engineering practice, the
distinction between the terms "phase" and "phase field" is seldom made, and all
materials having the same name are referred to as the same phase.

Cooling curve for pure iron. As iron is cooled

slowly from the liquid phase.

The iron-carbon diagram.

Iron-Iron Carbide Phase Transformation on the T-T-T Diagram.

The T-T-T curves correspond to the start and finish of transformation, which extend
into the range of temperature where austenite transforms to pearlite. Above 550C,
austenite transforms completely to pearlite. Below 550C, both pearlite and bainite are
formed and below 450C, only bainite is formed. The horizontal line C-D that runs
between the two curves marks the beginning and end of isothermal transformations.
The dashed line that runs parallel to the solid line curves represents the time to
transform half the austenite to pearlite. Below we have listed some simple examples as
an exercise at other temperatures that result in different phase transformation and hence
different microstructures.

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5.0) CONCLUSION:

Microstructural analysis is extremely important in today's world where metals,

ceramics, polymers, and composites are used to improve our everyday lives by insuring
safety and reliability in the products that we use. In order, to correctly analyze these
microstructures, proper specimen preparation is required to eliminate preparation induced
microstructural artifacts. By knowing the physical properties of the material such as
hardness, recrystallization temperature, fracture toughness; an appropriate specimen
preparation procedure can be developed. In general, minimizing the damage early in the
microstructural preparation stage by choosing the correct abrasive, lubricant, and
equipment parameters, the steps required to highlight the representative materials
microstructure obtained by following the basic preparation guidelines outlined in this
paper.
The optical microscope is a very useful tool for the observation of materials and can be
used to gain valuable information about a large variety of specimens. Some knowledge of
the material and the information that is required is essential to determine the best
techniques to employ when preparing and examining specimens. Sample preparation is a
critical part of microscopy, as this determines the quality of the images produced. Many
techniques, when correctly applied to a specimen, can enhance the information present.

6.0) REFERENCE
1) Lab sheet: Introduction to sample preparation and optical microscope for
metallographic observation
2) Materials science and engineering an introduction, William D. Callister. Jr.
6 Edition Wiley & Sons
3) Pace Technologies Educational Web page at http://www.metallographic.com

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