Applied Mechanics Lab – MEC 424/AHA/MCM Rev.

01-2014

UNIVERSITI TEKNOLOGI MARA

FAKULTI KEJURUTERAAN MEKANIKAL
___________________________________________________________________________

Program : Bachelor of Engineering (Hons) Mechanical (EM220/EM221)

Course : Applied Mechanics Lab
Code : MEC 424
Lecturer : Mohamad Zulfazli Arief Bin Abd Latif
Group : EMD4M13 – G1
___________________________________________________________________________
MEC 424 - LABORATORY REPORT
TITLE:INTRODUCTION TO SAMPLE PREPARATION AND
OPTICAL MICROSCOPE FOR METALLOGRAPHIC
OBSERVATION

No NAME STUDENT SIGNATURE

ID
1 MUHAMMAD AIMAN BIN HASHIM 2016499402
2 ARIF HAKIMIN BIN MOHD HASBI 2016218434
3 AHMAD TAUFIQ BIN MAHATHIR 2016297108

4 MOHAMAD ALIF AIMAN BIN MOHAMAD 2016229392

LABORATORY SESSION : 18/5/18

(DATE)

REPORT SUBMISSION : 25/5/18

(DATE)

*By signing above you attest that you have contributed to this submission and confirm that all work you have contributed to this
submission is your own work. Any suspicion of copying or plagiarism in this work will result in an investigation of academic msconduct
and may result in a “0” on the work, an “F” in the course, or possibly more severe penalties.

Marking Scheme

No 1 2 3 4 5 6 7 8 Total
ABSTRACT

This experiment is carried out to understand the procedure metallographic sample preparation. In
this experiment, we study the structure of metallic material, the phase exist and grain size. All of
this characteristics cannot be seen through naked eyes, but the grain structures can be observed
through the microscope. This process is full of procedures that need to be discussed as the grain
size in metal structural can’t be seen by naked eye and simple handling of metal. Equipment and
machines used in analyzing the structural of metals for observation would also be considered here.

The main objective of this experiment is to understand the procedure metallographic

sample preparation. Besides, the aim of this experiment also to learn the basic function of optical
microscope and its operation. Lastly, from this experiment also, we are able to understand the
procedure metallographic sample preparation which consist of six steps which are cutting,
molding, grinding, polishing and etching.

This experiment is quite complicated especially to prepare the metallographic sample. It

is important for us to know the characteristics of metal as each metals have different metallurgy.
From the data and information collected in the lab, the experiment is done as we follow each of
the procedure provided. Overall, we fulfilled the objectives of this experiment.

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 TABLE OF CONTENTS

No Table content Page

1 Abstract 1

2 Table of content 2

4 Introduction 3

5 Objectives 9

6 Theory 10

7 Apparatus 13

8 Procedure 17

9 Result and Calculation 19

10 References 32

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INTRODUCTION

Our understanding of the behaviour of materials depends on our ability to relate properties
to microstructures. The microstructure is the geometric arrangement of grains and the different
phases present in a material.

Grain Boundaries. The first thing we want to learn about any given microstructure is the
size and shape of the grains (crystals). Most engineering alloys are polycrystalline (Figure 1).
This means that each piece of a metal is made up of a great number of single crystals, or grains,
each having a regular crystal structure (for example, FCC, BCC, or HCP). Each grain will have a
different crystallographic orientation relative to its neighbouring grains. There is a region between
adjacent grains where the crystal lattice is disordered due to abrupt change in crystallographic
directions. This region is called the grain boundary. The grain size (i.e., the spacing between grain
boundaries) greatly influences many properties of a polycrystalline material and thus measuring
the grain size in a given microstructure is a routine practice in materials testing. Materials
specialists are interested to see the grain boundaries in order to estimate the grain sizes. The
average grain size in metals is usually in the order of several to tens of micrometres, which can
be measured only by the use of an optical or light microscope.

Figure 1: Atomic Disorder at Grain Boundary

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SAMPLE PREPARATION

In the study of metallic materials it is often to analyse the phases exist 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. Metals characteristics such as
grain sizes, effects of heat treatment, and carbon content of steels may be determined by studying
the micrograph. For this purpose, the metal use in the metallurgical examination must be prepared
and polished carefully before a good microscopic image can be seen. It is important to ensure that
the surface is totally flat and smooth before microstructure observation under the microscope.
Any irregularity will appear as a dark image and may create confusion to the observer who
attempts to analyse a structure. The process of sample preparation is schematically summarized
in Figure 2.

Figure 2: The summary of sample preparation.

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In order to obtain this smooth flat surface, several preparatory steps are required.

 Cutting

Cutting process is carried out in order to get the desired size of the sample so that it can be easily
moulded/handle. Separate test pieces or coupons attached to castings or forgings should be
designed so that a minimum of sectioning is required for producing metallographic specimens.
Sectioning becomes necessary when studying parts that have failed in service where specimen
has been taken from a large block of material. Therefore, metallographic studies of such samples
often involve more than one sectioning operation.

 Molding

Small samples can be difficult to hold safely during grinding and polishing operations, and their
shape may not be suitable for observation on a flat surface. They are therefore mounted inside a
polymer block or mount. Cold mounting can be done using two components resins (epoxies)
which are liquid to start with but which set solid shortly after mixing. Cold mounting requires
very simple equipment consisting of a cylindrical ring which serves as a mould and a flat piece
which serves as the base of the mould. The sample is placed on the flat piece within the mould
and the mixture poured in and allowed to set. Cold mounting takes few hours to complete.

In hot-mounting the sample is surrounded by an organic polymeric powder which melts under the
o
influence of heat (about 200 C). Pressure is also applied by a piston, ensuring a high quality
mould free of porosity and with intimate contact between the sample and the polymer. This is not
the case with cold mounting where the lack of proper contact and the presence of porosity can
cause problems such as the entrapment and seepage of etchant during the final stages of
preparation. Consequently, hot-mounting should be the preferred way of encapsulating specimens
assuming that time and resources permit, and assuming that the heat involved in the process does
not influence the sample. Because of time limitation in the lab, specimens have already been
mounted for you using hot mounting.

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  Grinding

Grinding is done using rotating discs covered with silicon carbide paper and water. There are a
number of grades of paper, with 180, 240, 400, 1200, grains of silicon carbide per square inch.
180 grade therefore represents the coarsest particles and this is the grade to begin the grinding
operation. Always use light pressure applied at the centre of the sample. Continue grinding until
all the blemishes have been removed, the sample surface is flat, and all the scratches are in a
single orientation. Wash the sample in water and move to the next grade, orienting the scratches
from the previous grade normal to the rotation direction. This makes it easy to see when the
coarser scratches have all been removed. After the final grinding operation on 1200 paper, wash
the sample in water followed by alcohol and dry it before moving to the polishers. The grinding
can be divided into two types:

1. Rough grinding: To remove rough scale and gross imperfections on the surface of sample.
2. Fine grinding: To improve the specimen's surface until it begins to shine and reflect light
slightly.

 Polishing

The polishers consist of rotating discs covered with soft cloth impregnated with a pre-prepared
slurry of hard powdery alumina particles (Al2O3, the size ranges from 0.5 to 0.03 μm). Begin with

the coarse slurry and continue polishing until the grinding scratches have been removed. It is of
vital importance that the sample is thoroughly cleaned using soapy water, followed by alcohol,
and dried before moving onto the final stage. Any contamination of the final polishing disc will
make it impossible to achieve a satisfactory polish. Examining the specimen in the microscope
after polishing should reveal mirror like surface. Polishing have two types of polishing:

1. Rough polishing: To remove the imperfections that grinding has left.

2. Fine polishing: To remove all scratches and leave a mirror like on the surface.

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  Etching

Various etchants are used to selectively attack the surfaces of metals to reveal grain boundaries,
phase, precipitates, inclusion and variations in composition.

The purpose of etching is two-fold. Grinding and polishing operations produce a highly deformed,
thin layer on the surface which is removed chemically during etching. Secondly, the etchant
attacks the surface with preference for those sites with the highest energy, leading to surface relief
which allows different crystal orientations, grain boundaries, precipitates, phases and defects to
be distinguished in reflected light microscopy as demonstrated in Figure 4. Please adhere to the
general safety regulations provided to you at the beginning of this handout. A polished sample is
etched using a cotton tip dipped in the etchant.

Etching should always be done in stages, beginning with light attack, an examination in the
microscope and further etching only if required.

Figure 3: Surface groove produce by etching and observed in the microscope.

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  Metallographic Observation

The study of the physical structure and components of metals, typically using microscopy (optical
microscope).

OPTICAL MICROSCOPE

When a mirror-like metal surface 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 as seen in the schematic diagram. The condenser lens focuses the light on
the sample and the objective lenses (50X, 100X, 200X, 400X) magnifies the beam, which contains
the image, to the projector lens so the image can be viewed by the observer.

OBJECTIVES

Upon completion of this experiment, students should be able to:

1. Understand the procedure metallographic sample preparation

2. Understand the basic function of optical microscope and it’s operation.

3. Perform analysis from the microstructure’s observation.

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 4. Understand theoretical background of sample preparation and metallographic
specimens.

THEORY
i) Cutting

Metallography is the art of preparation of specimens that can be examined by a microscope.

Examining a metal sample in the microscope without prior preparation will not reveal informative
image of the microstructure because roughness and scratches at the surface will reflect the
incident light randomly. The preparation starts by cutting a small representative piece of the metal
to be studied.

ii) Molding

Small samples can be difficult to hold safely during grinding and polishing operations,
and their shape may not be suitable for observation on a flat surface. They are therefore molded
inside a polymer block or mount. Cold molding can be done using two components resins
(epoxies) which are liquid to start with but which set solid shortly after mixing. Cold molding
requires very simple equipment consisting of a cylindrical ring which serves as a mould and a flat

9
piece which serves as the base of the mould. The sample is placed on the flat piece within the
mould and the mixture poured in and allowed to set. Cold molding takes few hours to complete.

In hot molding process, the sample is surrounded by an organic polymeric powder which
melts under the influence of heat (about 200˚C). Pressure is also applied by a piston, ensuring a
high quality mould free of porosity and with intimate contact between the sample and the polymer.
This is not the case with cold molding where the lack of proper contact and the presence of
porosity can cause problems such as the entrapment and seepage of etchant during the final stages
of preparation. Consequently, hot molding should be the preferred way of encapsulating
specimens assuming that time and resources permit, and assuming that the heat involved in the
process does not influence the sample. Because of time limitation in the lab, specimens have
already been mounted for you using hot molding.

iii) Grinding

Grinding is done using rotating discs covered with silicon carbide paper and water. There
are a number of grades of sandpapers, with 180, 240, 400, 1200, grains of silicon carbide per
square inch. 180 grade therefore represents the coarsest particles and this is the grade to begin the
grinding operation. Always use light pressure applied at the centre of the sample. Continue
grinding until all the blemishes have been removed, the sample surface is flat, and all the scratches
are in a single orientation. Wash the sample in water and move to the next grade of sandpaper,
orienting the scratches from the previous grade normal to the rotation direction. This makes it
easy to see when the coarser scratches have all been removed. After the final grinding operation
on 1200 paper, wash the sample in water followed by alcohol and dry it before moving to the
polishers.

iv) Polishing

The polishers consist of rotating discs covered with soft cloth impregnated with a pre-
prepared slurry of hard powdery alumina particles (Al₂O₃, the size ranges from 0.5 to 0.03µm).

10
Begin with the coarse slurry and continue polishing until the grinding scratches have been
removed. It is of vital importance that the sample is thoroughly cleaned using soapy water,
followed by alcohol, and dried before moving onto the final stage. Any contamination of the final
polishing disc will make it impossible to achieve a satisfactory polish. Examining the specimen
in the microscope after polishing should reveal mirror like surface.

v) Etching

The purpose of etching is two-fold. Grinding and polishing operations produce a highly
deformed, thin layer on the surface which is removed chemically during etching. Secondly, the
etchant attacks the surface with preference for those sites with the highest energy, leading to
surface relief which allows different crystal orientations, grain boundaries, precipitates, phases
and defects to be distinguished in reflected light. A polished sample is etched using a cotton tip
dipped in the etchant. Etching should always be done in stages, beginning with light attack, an
examination in the microscope and further etching only if required. If you over etch a sample on
the first step then the polishing procedure will have to be repeated. The table below gives the
etchants for alloys that will be examined in this experiment.

SAMPLE ETCHANT
Al alloys Keller’s (2ml HF + 3ml HCL + 5ml HNO₃
+ 190 ml water)
Cu-Zn alloy (brass) 10 ml HNO₃ + 90 ml water

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Steel and cast irons Nital (2% HNO₃ + 98% Ethanol)

TABLE 1 : Common etchants for engineering alloys

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APPARATUS

Figure 1: Microscope

Figure 2: Etching Machine

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Figure 3: Equipment For Cutting Process

Figure 4: Cutting Machine

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Figure 5: Grinding Machine

Figure 6: Polishing Machine

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Figure 7: Molding Machine

Figure 8: Microscope

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EXPERIMENTAL PROCEDURES
Cutting
1. the length of steel rod is measured and marked using vernier caliper.
2. The screw is adjusted of to put the steel rod on it
3. The screw was tightened so the rod will not vibrate when being cut by the grinder.
4. The cover of the grinder is closed and the grinder is switched on afterwards.
5. Cooler liquid is checked continuously flowing to prevent the blade from overheat during
cut process
6. The paddle is pulled downward slowly so the steel will be cut smoothly and to prevent
the blade from fracture.
7. After the steel completely cut, we pushed the stop button and pulled the paddle upward
to move the blade away from the steel.
8. After the blade stop spinning, we switched off grinder and opened the cover and loosen
the screw to take out the steels that had been cut.

Molding
1. The compressor and the molding machine id switched on.
2. The base is lowered to its maximum and put the steel is was put inside with the surface
that being cut was positioned below.
3. The 10g fendic power was poured after measure the mass of it.
4. The cover is cleaned, closed and locked to prevent the cover from stuck after molding
process.
5. The start button was pressed and waited for 10 minutes it the steel sample is completely
molded.
6. The cover is opened and the base is was moved upward to collect the molded steel.
7. The machine was switched off and the sample is brought to the polishing machine

Polishing
1. The rough sand paper is put into the polishing machine.
2. The machine is switched on and the water is dropped onto it.
3. The sample is pressed softly on the rotated sand paper.
4. The process is repeated by changed with softer sand paper until the surface of the
sample was smooth enough.
5. The sample is brought to another polishing machine for surface finishing using specific
powder until the surface of the sample become can mirrored the image reflected.

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Etching
1. The sample was brought to the fume laboratory to do etching process.
2. The agent is poured into the small cup
3. The sample’s surface was dipped into the cup for 5 seconds
4. The sample is carefully dried without wiping it to prevent the steel surface from
scratched.

Observing with Microscope

1. The microscope was switched on and the brightness of the lamp was adjusted to 5.
2. The sample was placed below the lens of the microscope.
3. The 50x zoom lens is adjusted until the image of the sample under microscope become
clear.
4. The images of the microstructure was drew onto the paper.
5. The process repeated with using different lens (50x, 100x, 200x and 400x).

RESULTS, DISCUSSIONS, CONCLUSIONS

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REFERENCES

 Material Science and Engineering- An introduction by W. D. Callister

 Engineering Metallurgy- Part I by R. A. Higgins • Materials Science and Engg. By V.
Raghavan
 Manufacturing Engineering and Technology by S. Kalpakjian

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