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Metallographic Observation Lab Report

The document outlines a laboratory report for the Applied Mechanics Lab course at Universiti Teknologi Mara, focusing on sample preparation and optical microscopy for metallographic observation. The experiment aims to analyze the microstructure of materials through various preparation techniques and magnifications, ultimately demonstrating how grain structures can be observed using an optical microscope. The report includes sections on objectives, theory, experimental procedures, results, discussions, and conclusions.

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0% found this document useful (0 votes)
9 views17 pages

Metallographic Observation Lab Report

The document outlines a laboratory report for the Applied Mechanics Lab course at Universiti Teknologi Mara, focusing on sample preparation and optical microscopy for metallographic observation. The experiment aims to analyze the microstructure of materials through various preparation techniques and magnifications, ultimately demonstrating how grain structures can be observed using an optical microscope. The report includes sections on objectives, theory, experimental procedures, results, discussions, and conclusions.

Uploaded by

ibnuhakeemz
Copyright
© All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
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Applied Mechanics Lab – MEC 424/Hakim/2024/V1

UNIVERSITI TEKNOLOGI MARA


SCHOOL OF MECHANICAL ENGINEERING

Program : Bachelor of Mechanical Engineering (Hons) - CEEM 222


Course : Applied Mechanics Lab
Code : MEC 424
Lecturer : MADAM FAUZIAH BT MD YUSOF
Group : EMD4M5C (CLUSTER 2)

MEC 424 - LABORATORY REPORT

TITLES: Introduction to Sample Preparation and Optical Microscope for


Metallographic Observation

No NAME STUDENT ID SIGNATURE


MUHAMMAD IBNU HAKEEM BIN
1 2023622674
ZAMRI
MUHAMMAD ZULHAKIMI BIN
2 2023491526
NOORDIN
MUHAMMAD ZAHIR ANWAR BIN
3 2023690552
ABDULLAH
MUHAMMAD SYAHMI JAZMI BIN
4 2023679984
JAMHARI
LABORATORY SESSION : 12/06/2025
(DATE)

REPORT SUBMISSION : 27/06/2025


(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 A1 A2 A3 A4 A5 A6 A7 A8
1
2
3
4
5

LEGENDS
A1 -Abstract A3 – Theory A5 – Results A7 - Conclusion
A2 -Introduction A4 - Procedure A6 – Discussions A8 - Overall Impressions
1.0 ABSTRACT

This experiment is about introduction to sample preparation and optical microscope for
metallographic observation. This experiment was done to investigate the metallographic
observation from the specific sample using optical microscope with different magnification,
which is x50, x100, x200 and x400. The experiment involved with the cutting, moulding,
grinding (fine, coarse), polishing and etching process. Every process has their precaution to
ensure that the sample specimen is in good condition to get the clear grain size. In a conclusion,
we get the images become immense and clear when the magnification is increase. We also
identified the structure of images that has been formed from the surface of sample specimen
with different magnification.

2
TABLE OF CONTENT

1.0 ABSTRACT ................................................................................................................... 2


TABLE OF CONTENT ............................................................................................................. 3
LIST OF FIGURES ................................................................................................................... 4
LIST OF TABLES ..................................................................................................................... 5
2.0 INTRODUCTION ......................................................................................................... 6
2.1 OBJECTIVES ............................................................................................................ 6
3.0 THEORY ....................................................................................................................... 7
4.0 EXPERIMENTAL PROCEDURE ................................................................................ 9
4.1 APPARATUS ............................................................................................................ 9
4.2 PROCEDURE .......................................................................................................... 10
5.0 RESULTS .................................................................................................................... 13
6.0 DISCUSSIONS ............................................................................................................ 13
6.1 MOHD RAMZAI BIN ZAINAL ABIDIN (202212345)Error! Bookmark not
defined.
6.2 MOHD ROKHANMI ZAKARIA (201112131) ...... Error! Bookmark not defined.
6.3 NG YEE TATT (201112131) .................................. Error! Bookmark not defined.
6.4 BALASUBRAMANIAM A/L RAMASAMY (201112131) .................................. 14
7.0 CONCLUSIONS.......................................................................................................... 15
8.0 REFERENCES ............................................................................................................ 16
9.0 APPENDICES AND RAW DATA ............................................................................. 17

3
LIST OF FIGURES

Figure 1: Metallographic etching ............................................................................................... 7


Figure 2: Cutter Machine ........................................................................................................... 9
Figure 3: Auto Mounting Press Machine ................................................................................... 9
Figure 4: Grinder Machine......................................................................................................... 9
Figure 5: Polishing Machine ...................................................................................................... 9
Figure 6: Optical Microscope .................................................................................................. 12

4
LIST OF TABLES

Table 1 : Sample under Microscope with magnification ......................................................... 13

5
2.0 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 metallic
materials have their 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 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 to obtain their
suitable surface such as mirror-like metal before analysis structure process by using optical
microscope. The optical microscope has 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
determined through the schematic diagram

2.1 OBJECTIVES

1. To understand the procedure metallographic sample preparation.


2. To understand the basic function of optical microscope and its operation.
3. To perform an analysis from the observed microstructure.
4. To understand theoretical background of sample preparation and metallographic
specimens.

6
3.0 THEORY

Microstructure analysis is often an important concern in many businesses since it helps


determine whether a material has been handled correctly. Sampling, specimen preparation
(sectioning and cutting, mounting, grinding, rough and final polishing, etching), microscopic
observation, digital imaging and documentation, and quantitative data extraction using
stereological or image analysis techniques are all necessary for a proper metallographic
examination.

The initial stage of metallographic testing the outcome of any additional research
depends on sampling; the specimen to be examined must be representative of the substance
under consideration. Furthermore, the preparation of the specimen is equally important, and
there are no ways to get the intended metallographic result.

Metallography has historically been referred to as both a science and an art. This is
because both experience and intuition are crucial for revealing the material's actual structure
without causing major alteration or damage, as well as for making the features of interest
measurable.

Because etching is arguably the most variable process, selecting the best print
composition and controlling the etch temperature and duration are essential for reliable and
consistent results. To find the ideal parameters for this stage, a scientific procedure including
trial and error is frequently required.

Figure 1: Metallographic etching

7
The process above in Figure 1 is known as metallographic etching, a critical technique
used in material science to reveal the microstructure of metals and alloys. After a sample is
carefully polished to produce a smooth surface, it is chemically etched using a suitable reagent
that selectively attacks specific microstructural features. Grain boundaries, which are more
chemically reactive than the interior of the grains, are preferentially etched, forming surface
grooves. These grooves scatter light differently compared to flat areas, allowing the grain
structure to become visible under an optical microscope. This technique is essential for
analysing grain size, phase distribution, and other structural characteristics that influence the
mechanical and physical properties of materials.

8
4.0 EXPERIMENTAL PROCEDURE

4.1 APPARATUS

Figure 2: Cutter Machine

Figure 3: Auto Mounting Press Machine

Figure 4: Grinder Machine

Figure 5: Polishing Machine

9
4.2 PROCEDURE

• Cutting: The cutting procedure was used to bring the sample to the right size so that it
could be handled or moulded with ease.
1. The sample was measured to determine the correct cutting dimensions.
2. The cutter cover was opened, and the sample was placed securely in the clamps.
3. The clamps were tightened slowly to ensure the sample was firmly held.
4. The cutter cover was closed to ensure safe operation.
5. The main power switch of the cutting machine was turned on.
6. The pump and cutting buttons were activated to start the blade rotation and fluid
circulation.
7. Once the cutting fluid was properly flowing with the rotating blade, the handle was
slowly lowered to begin cutting.
8. The blade was pressed gently through the sample to ensure a clean cut and to protect
the blade and sample.
9. After cutting was completed, the cutting, pump, and light buttons were turned off.
10. The main power switch was turned off.
11. Once the blade had completely stopped rotating, the cutter cover was opened.
12. The clamps were loosened, and the cut sample was carefully removed.

• Moulding: To make the sample simpler to grip during the polishing process, a
moulding method was used.
1. The machine was switched on and the air flow was opened.
2. The surface of sample that wanted should be facing down.
3. The button was pushed to lower the sample down to the bottom and 10 grams of
phenolic powder was applied into the mounting machine.
4. The machine was pressed and locked to the left.
5. The green button was turned on and leaves for 18 minutes until the hot mounting
process done.

10
• Grinding
➢ 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.)

1. Sandpaper with grit 240 (the lowest grade) was clipped onto the grinder.
2. The machine was turned on, followed by activating the water pump and motor to
ensure continuous cooling and cleaning during grinding.
3. The sample was pressed onto the rotating sandpaper in the opposite direction of
the existing scratches, applying moderate pressure.
4. Grinding continued until the initial surface marks were reduced and a more
uniform surface appeared.
5. The grinding process was repeated sequentially using finer grit sandpapers in the
following order: 320, 400, 600, and finally 1200.
6. At each stage, the sample was ground in the opposite direction to the previous step
to effectively remove earlier scratches.
7. After completing the final stage with grit 1200, a smooth and refined sample
surface was obtained, ready for polishing.

• Polishing

➢ 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.)

1. Polished cloth was placed on the plate. alumina powder.


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.

11
• Etching: Metal surfaces are selectively targeted by a variety of etchants to expose
inclusions, phases, precipitates, grain boundaries, and analytical differences.

Figure 6: Optical Microscope

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 have been recorded

12
5.0 RESULTS

The samples shown under the Optical Microscope with different magnifications as shown in:

Description Sample

Sample under Optical


Microscope with magnification
X50

Sample under Optical


Microscope with magnification
X100

Sample under Optical


Microscope with magnification
X200

Sample under Optical


Microscope with magnification
X400

Table 1 : Sample under Microscope with magnification

13
6.0 DISCUSSIONS

6.1 MUHAMMAD IBNU HAKEEM BIN ZAMRI (2023622674)

6.2 MUHAMMAD ZULHAKIMI BIN NOORDIN (2023491526)

6.3 MUHAMMAD ZAHIR ANWAR BIN ABDULLAH (2023690552)

6.4 MUHAMMAD SYAHMI JAZMI BIN JAMHARI (2023679984)

14
7.0 CONCLUSIONS

15
8.0 REFERENCES

16
9.0 APPENDICES AND RAW DATA

17

Common questions

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Each stage in the metallographic sample preparation process has a specific role. Cutting sizes the sample for easy handling. Moulding helps in securely gripping the sample during subsequent stages. Grinding smoothens the sample surface, removing major imperfections. Polishing removes minor scratches, creating a mirror-like finish crucial for clear imaging. Etching reveals microstructural details by highlighting grain boundaries and other features. Together, these stages ensure the sample is accurately prepared for analysis, providing reliable data about its microstructure, which impacts material properties .

Increasing the magnification power of an optical microscope enhances the clarity and size of observed microstructures, allowing for a detailed analysis of the sample's surface features. At higher magnifications, such as x400, subtler structural details like grain boundaries become more distinct, facilitating a more precise characterization of the material. This magnification-dependent clarity is crucial for accurately identifying and analyzing the material's microstructure, which is essential for applications in quality control and failure analysis .

The selection of different magnifications in optical microscopy impacts the analysis by determining the level of detail visible in a metallographic sample. Lower magnifications, such as x50, allow for an overview of the sample, revealing large-scale features and overall structure. In contrast, higher magnifications, like x400, enable the observation of finer details, such as individual grain boundaries and phase distinctions. The choice of magnification must balance the need for detail against the broader context of the sample structure, helping to provide a comprehensive understanding of the material's properties and behavior .

Metallographic analysis serves as a quality assurance tool by enabling the detailed examination of metallic materials' microstructures, which informs their mechanical and physical properties. It helps identify inconsistencies, defects, or deviations from specified characteristics, such as grain size and phase distribution, ensuring materials meet quality standards and performance requirements. By analyzing these microstructural features, engineers can verify that materials have been correctly processed and handled, thereby preventing future failures and ensuring product reliability .

Trial and error is often essential in finding the ideal parameters for the etching stage because the process is highly variable and dependent on factors such as the composition of the etchant, etch temperature, and duration. These parameters must be finely tuned to reliably and consistently reveal the microstructural features without causing excessive dissolution or insufficient reaction. The variability of material composition and desired outcomes necessitates this experimental approach to optimize the etching process for different materials and structures .

The metallographic etching process involves carefully polishing the sample to create a smooth surface, followed by chemical etching with a suitable reagent. This reagent selectively attacks specific microstructural features, such as grain boundaries, because they are more chemically reactive than the grains' interiors. As a result, these boundaries form surface grooves that scatter light differently, making the grain structure visible under an optical microscope. This process is essential for analyzing grain size, phase distribution, and other structural characteristics which influence the material's mechanical and physical properties .

The etching process enhances microstructure visibility by using a chemical reagent that selectively reacts with certain features of the sample, particularly grain boundaries, which are more reactive than the inner grains. This reaction etches these borders, creating surface grooves that scatter light differently, making grain structures visible under the microscope. This difference in light scattering enables detailed visualization and analysis of the grain size and distribution, which are crucial for understanding the material's properties .

Improper sample preparation can lead to inaccurate metallographic analyses, which may obscure or misrepresent the sample's true microstructure. Consequences include the presence of scratches, unwanted residues, or surface artifacts that can interfere with optical examination, misleading the interpretation of grain size, phase distribution, or other critical features. This can result in incorrect conclusions about the material's properties and performance, potentially affecting quality control, materials specification, and failure analysis processes in mechanical engineering contexts .

The purpose of metallographic sample preparation and examination is to analyze the microstructure and macrostructure of metallic materials to provide a schematic diagram of their grain size, phase distribution, and structural characteristics. This helps to determine if a material has been correctly handled and is critical for quality control, material specifications, and failure analysis in mechanical engineering. The preparation involves sectioning, mounting, grinding, polishing, and etching the material to reveal its internal structure, which is not visible to the naked eye but observable under an optical microscope .

The preparation process ensures accuracy in metallographic analysis by methodically eliminating imperfections that could obscure the true structure of the sample. It begins with cutting the sample to the right size for handling, followed by grinding to achieve a uniformly smooth surface. Polishing further refines the surface, and etching selectively reveals microstructural features. Each step aims to preserve the material's integrity without introducing artifacts. This meticulous preparation allows for clear observation under a microscope, which is crucial for accurate evaluation of the material's properties and performance in engineering applications .

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