FACULTY OF MECHANICAL ENGINEERING

___________________________________________________________________

Programme : Bachelor of Engineering (Hons) Mechanical (EM220)

Course : Applied Mechanics Lab
Code : MEC 424
Lecturer : PM Dr Mimi Azlina
Group : EMD4M9B
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MEC 424 - LABORATORY REPORT

TITLE: Introduction to Sample Preparation and Optical Microscope for

Metallographic Observation

No NAME STUDENT ID
1. NURUL SHUHADA BINTI SULAIMAN 2019848042
2. SITI HAJAR BINTI ABDULLAH 2019660454
3. WAN AHMAD BALYA BIN WAN MAT 2019819216
4. WAN ALIF IKMAL BIN BARUDDIN 2019689676
5. WAN NOR HAFIZAH BINTI WAN MOHD OTHMAN 2019601792

REPORT SUBMISSION: 10 MAY 2020

(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
misconduct 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

The experiment was prepared to perform analysis from the microstructure’s observation. The
sample went under the preparation process consist of cutting, molding, grinding, polishing and
etching. When a mirror-like metal surface has been obtained, the structure was observed with
the aid of optical microscope. It was observed under the optical microscope with different
magnifications which are x50 x100, x200, and x400. The grain size increase as the
magnification increase. According the photomicrograph obtained after preparation process, the
microstructure consist of ferrite and pearlite. In conclusion, the preparation process is the most
important process in metallography examination to produce a good microscopic.
TABLE OF CONTENT

Title Page
1.0 Introduction 1
2.0 Theory 2
3.0 Experimental Procedures 4-9
4.0 Result 10-11
5.0 Discussion 11
6.0 Conclusion 12
7.0 References 13
8.0 Appendices and Raw Data 14-16
LIST OF FIGURES

Figure Page
Figure 1: Use of microscope Brightfield (BF) 3
Figure 2: Use of microscope Darkfield (DF) 3
Figure 3: Cutting Process 4
Figure 4: Cold Mounting Process 5
Figure 5: Hot Mounting process 6
Figure 6: Grinder Process 7
Figure 7: Polishing 8
Figure 8: Etching Process and Finishing 9
Figure 9 Sample under Optical Microscope with magnification x50 10
Figure 10 Sample under Optical Microscope with magnification x100 10
Figure 11 Sample under Optical Microscope with magnification x200 10
Figure 12 Sample under Optical Microscope with magnification x400 11
Figure 13 Ferritic-pearlitic metal microstructure 12
1.0 INTRODUCTION

The optical metallography is the examination to provide a magnified structure of the

microstructure and macrostructure of the materials. The relationships among structure and
properties, metallographic characterization is used in quality control ,quality assurance, material
specifications and failure analysis. Due to that, this experiment is important to studies ranging
from fundamental research to production evaluations for the industry. All of metallic materials
have theirs characteristics such as grain size, carbon content of steel and effect of heat treatment.
The purpose of this experiment is to analysis the phases and grain size in the structure because all
of the metal structure are not readily visible with the naked eyes but by the microscope, the grain
patterns can be seen. So that, the characteristics can be obtain by the studying micrograph result
of this experiment. Due to the objective to get the real structure, the metal would have to go through
under the grinding process or polishing and etching in order to obtain theirs suitable surface such
as mirror-like metal before analysis structure process by using optical microscope. The optical
microscope have function to obtain the schematic diagram by using three different type of lens
such as x50 x100, x200, and x400. The grain structure can be determine through the schematic
diagram.

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2.0 THEORY

Analysis of a material’s microstructure aids is decisive if the material has been processed properly,
and is thus commonly a essential issue in several industries. the essential steps for proper
metallographic examination include sampling, specimen preparation (sectioning and cutting,
mounting, grinding, rough and final polishing, etching), microscopic observation, digital imaging
and documentation, and quantitative data extraction through stereological or image
analysis methods.

The first step of metallographic analysis sampling is essential to the success of any resultant study,
the specimen to be analyzed should be representative of the material being evaluated. Moreover,
equally necessary step is for proper prepare a metallographic specimen,
and there's no distinctive ways to achieve a desired result
Some of the earliest correlations between microstructure and macroscopic properties established
in metallography using light microscopes include:

 A general increase in yield strength and hardness with decreasing grain size
 An isotropic mechanical property with elongated grains and/or preferred grain orientations
 A general tendency of decreased ductility with increasing inclusion content

Metallography has been traditionally described as both a science and an art, and the reason for this
statement lies in the fact that experience and intuition are equally important for exposing the true
structure of the material without causing significant change or damage, in order to reveal and make
measurable the features of interest.
Etching is perhaps the foremost variable step, therefore careful choice of the most
effective print composition and management of etchant temperature and etch time square
measure necessary to get assured and repeatable results. Very often an effort and error scientific
method is needed to seek out the optimum parameters for this step.

The metallurgy can be found more in detail in D. Diez, J. DeRose, T. Locherer, Report and
Webinar: Rate the Quality of Your Steel: Overview of standard analysis methods and practical
solutions for evaluating steel inclusions, Science Lab (2019) Leica Microsystems.

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Figure 1: Use of microscope Brightfield (BF)
illumination

Figure 2: Use of microscope Darkfield (DF)

illumination

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3.0 EXPERIMENTAL PROCEDURES

Lab Material Science, Faculty of Mechanical Engineering, UiTM Shah Alam, Selangor.

a) Cutting Process - To get desired size of the sample so that it can be easily molded

Apparatus:

Sample Specimen

Abrasive Blade Maxcut

Abrasive Cutter Abrasive
Machine Cutting Fluid

Figure 3: Cutting Process

Procedure:
1. The sample to be cut was measured.
2. Sample that had been cut, placed in clamps and clamped it slowly until tight.
3. The machine cover has been closed for safety. The machine was turned on and the blade
was rotating, waiting for the fluid to rise at the blade.
4. To maintain the blade life and quality of the sample, the handle was pressed slowly until
the blade was finished cutting the sample.
5. When the sample has been cut, the machine was turned off, the cover machine was opened
after the blade had stooped rotating. Then clamps were loosed, and sample have been
taken.

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b) Molding/Mounting Process-To make the sample easier to hold throughout the polishing
i) Cold Mounting
Apparatus:

Mold Exopy Harden

Resin er

Figure 4: Cold Mounting Process

Procedure:
1) 10g Epoxy Resin and 1g Hardener was mixed and poured into mold.
2) The sample was put into a mold and then left to harden room temperature for 24hours.
3) Samples was removed from mold after 24hours. Cold mounting sample was produced.

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 ii) Hot Mounting
Apparatus:

Automatic Mounting Press Phenolic

Machine Powder

Figure 5: Hot Mounting process

Procedure:

1) The RAM was raised, and the sample was placed, then the Ram was lowered slightly.
2) 10g of Phenolic powder is put into it and then the Ram was lowered to the bottom.
3) The powder was cleaned and rubbed into it.
4) Bayonet cover was pressed and locked to the left.
5) Parameter set:
I. Solidity Time : 10 min
II. Cooling Time : 8 min
III. Pressure : 200 bar
IV. Temperature : 180c
6) Start button pressed.
7) After the process was over, the RAM was lowered, and the bayonet cover was pulled up.
The RAM was lifted, and the completed mount sample have been removed.

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 c) Grinding Process
-Rough grinding: To remove the imperfections that grinding has left.
-Fine grinding: To remove all scratches and leave a mirror like finish on the surface.
Apparatus:

Grinder
Sand paper

Figure 6: Grinder Process

Procedure:
1) Sandpaper with grit 240 was attached on the grinder.
2) The machine was turned on, then the water pump and motor have been turned on.
3) The sample was held and pressed in the grinding in the opposite direction.
4) When the scratches were reduced, the machine is stripped and steps 1 to 4 are repeated
using grit in the order of 320, 400, 600 and 1200.
5) After completing the step up to grit 1200, a smooth sample surface was produced.

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d) Polishing Process
-Rough polishing: To remove the imperfections that grinding has left.
-Fine polishing: To remove all scratches and leave a mirror like finish on the surface.
Apparatus:

Polishing cloth

Polisher alumina powder

Figure 7: Polishing
Process

Procedure:
1) Polished cloth was placed on the plate.
2) The machine was turned on. 9.5-micron alumina powder was placed on a cloth.
Distilled water was turned on.
3) Specimen was held and grinded to the fabric.
4) After finishing that process, the cloth on the plate was cleaned by hand to remove the
powder.
5) Step 1 to step 5 was repeated using alumina powder which is 5-micron, 3 micron and
1 micron
6) Finish up to 1 micron. A sample surface like a mirror has been produced.

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 e) Etching Process and Finishing- Various etchants are used to selectively attack the surfaces
of metals to reveal grain boundaries, phases, precipitates, inclusions and variation in
composition. The structure of sample observed with the aid of optical microscope.

Apparatus:

Microscope
Nital liquid

Lab
Consumables

Figure 8: Etching Process and Finishing

Procedure:
1) Nital liquid was placed in lab consumables.
2) Sample carved every 10s for 60s.
3) After finishing the etching process, the sample was washed with water, then dried
using a pressure air gun.
4) Then, the sample was placed under microscope. The results has been recorded.

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NURUL SHUHADA BT SULAIMAN
2019848042
4.0 RESULT
The samples shown under the Optical Microscope with different magnifications as shown in
Figures 1 – 4.

Figure 9 Sample under Optical Microscope with magnification x50

Figure 10 Sample under Optical Microscope with magnification x100

Figure 11 Sample under Optical Microscope with magnification x200

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NURUL SHUHADA BT SULAIMAN
2019848042

Figure 12 Sample under Optical Microscope with magnification x400

5.0 DISCUSSION

In the sample preparation, the preparation step was done in order to produce a good
microstructure image. The sample was grind to ensure it was free from scratches and keep a flat
surface. The polishing process produce a mirror like surface. It is instructed to not touch the
sample surface from this point because at this point, the sample will be very smooth to the eye
and even the oils and dirt on your fingers will scratch it with larger scratches than the Abrasive.
The last step in the process is to etch the sample to bring out the microstructure. Grains cannot be
seen without etching. Cracks, pores and defects are observed without etching. Etchant reacts with
atoms and dissolves them. Atoms at grain boundaries dissolve quickly. Dissolved grain
boundaries appear dark. The etchants used for this sample is nital. Then, the sample was
observed using optical microscope with different magnifications. Figure 9 shows the
microstructure with 50x magnification. The image seen was a very small grain. The shape of the
grain cannot be seen. Same goes to figure 10 under 100x magnification. The grain size is bigger
but the shape still cannot be seen. In figure 11, the grain starts to show the shape under the
magnification of 200x. The grain can be seen clearly when the microscope magnification is
400x.
Based on my observation, the microstructure happen to be a Ferritic-pearlitic steel with
approx. 0.2 % C, etched with Nital. The carbon is primarily present as a cementite lamellar in a
harder proportion of pearlite adjacent to the ferritic grains. This causes the cementite to appear
streaky. The pearlitic grains reflect less light than the ferritic grains and thus appear darker. A
matrix of this type has higher hardness, but lower ductility[8].

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NURUL SHUHADA BT SULAIMAN
2019848042

Figure 13 Ferritic-pearlitic metal microstructure

6.0 CONCLUSION

In conclusion, the preparation process is the most important step to observe the microstructure of
the specimen. The process done will reveal grain boundaries, phases, precipitates, inclusions and
variations in composition especially etching process. Besides, the microscope magnification with
high power helps the image viewed clear that the lower power of magnification. 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 and 400X) magnifies the beam, which contains the image, to the projector
lens so the image can be viewed. According the photomicrograph obtained, the grain size
increase as the magnification increase. The microstructure happen to be a Ferritic-pearlitic steel

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7.0 REFERENCES

1) Lab sheet Material Science-Introduction to Sample Preparation and Optical Microscope for
Metallographic Observation
2) https://youtu.be/nm5Zt4MW7K4 - Mec424 Material Lab Experiment 1
3) https://www.google.com/url?sa=i&url=https%3A%2F%2Fptop.only.wip.la%3A443%2Fhttps%2Fwww.indiamart.com%2Fproddeta
il%2Fphenolic-powder-
9779047188.html&psig=AOvVaw1uDFRW4M3MbdRPxFPf1wpn&ust=1588556262419000
&source=images&cd=vfe&ved=0CAIQjRxqFwoTCLDo79bUlukCFQAAAAAdAAAAABA
D –Image for Phenolic Powder
4) https://www.google.com/url?sa=i&url=https%3A%2F%2Fptop.only.wip.la%3A443%2Fhttps%2Fwww.homesciencetools.com%2F
product%2Fhome-1000x-
microscope%2F&psig=AOvVaw047yoAXzFAmq2OTK62faaa&ust=1588559199866000&s
ource=images&cd=vfe&ved=0CAIQjRxqFwoTCMjG56rSlukCFQAAAAAdAAAAABAD –
Imange for Microscope
5) Dr Mike Keeble., “Error and Uncertainty in Metallographic Measurement” TechNotes
Journal,” Vol. 7, Issue 4.
6) Aznifa Mahyam., Firdaus Sukarman., Hazriel Faizal., Ilya Izyan., Jamilah Talib., Mohd
Faizul., Rasdi Deraman., Samsiah Ahmad., “MEC281 Material Science” pp. 91. March 2018.
7) Dionis , D. (2020). Metallography – an Introduction. Retrieved 7 May, 2020, from
https://www.leica-microsystems.com/science-lab/metallography-an-introduction/
8) Stuers. (2020). THE STRUCTURAL PROPERTIES OF METALS. Retrieved 7 May,
2020, from https://www.struers.com/en/Knowledge/Materials/Metallic-grain-
structures#microscopic

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9) 8.0 APPENDICES AND RAW DATA

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15
 FACULTY OF MECHANICAL ENGINEERING

Teamwork Assessment Form

Name & ID

BIl Name Matrix Number

1. SITI HAJAR BINTI ABDULLAH 2019660454
2. WAN AHMAD BALYA BIN WAN MAT 2019819216
3. WAN ALIF IKMAL BIN BARUDDIN 2019689676
4. WAN NOR HAFIZAH BINTI WAN MOHD OTHMAN 2019601792
5. NURUL SHUHADA BINTI SULAIMAN 2019848042

Scale 1 2 3 4 5
Level Poor Acceptable Excellent

You will rate yourself and your team members on the following criteria

Earned Assessment
Element Members
Self
1 2 3 4
I was ready to work with my team 5 5 5 5 5
I did my assigned work well and always on time 5 5 3 5 5
I was fair to my teammates and myself 5 5 5 5 5
I listened to others appreciatively and was supportive 5 5 5 5 5
I was very committed and focused in my team 5 5 4 5 5
I put extra efforts to finish or accomplish our task 5 5 4 5 5
I encouraged others in my team and was helpful 5 5 3 5 5
I managed and coordinated team efforts effectively 5 5 4 5 5
I was able to lead discussions and provide solutions 5 5 5 5 5
Overall, I was very satisfied and enjoyed my work 5 5 5 5 5
Total 50 50 43 50 50
Comment
Self: committed with work

Member 1: Lead the group well

Member 2: Listen to others well
Member 3: Show his effort to finish his work
Member 4: Finish her work on time

16