EP110 CHEMICAL ENGINEERING LABORATORY II

BEP1031 MATERIAL ENGINEERING LABORATORY

& EG 104 PETROLEUM ENGINEERING I

NO. OF EXPERIMENT: 7

TITLE OF EXPERIMENT: METALLOGTAPHIC TECHNIQUES AND

MICROSCOPY

NAME & ID: ARRIANNA PAULINA PETER 1002162633

JOEL LEE CHERN TERN 1002265669
TIANG SOON LIN 1002267948

GROUP: 6

DATE OF EXPERIMENT: 27 JUNE 2023

TUTOR: MS. RAFIZAH BINTI ZAITON

SCHOOL OF ENGINEERING
FACULTY OF ENGINEERING, TECHNOLOGY &
BUILT ENVIRONMENT
2023
Table of Contents
Introduction ............................................................................................................................................. 3

Objectives ............................................................................................................................................... 5

Problem statements ................................................................................................................................. 5

Hypothesis .............................................................................................................................................. 5

Materials and apparatus .......................................................................................................................... 6

Procedure ................................................................................................................................................ 7

Discussion ............................................................................................................................................... 9

Limitations ............................................................................................................................................ 13

Conclusion ............................................................................................................................................ 15

Reference .............................................................................................................................................. 16

Appendix ............................................................................................................................................... 17

Rubrics .................................................................................................................................................. 26
Introduction
In this experiment, the study of microscopic structure of various materials through the
method of metallographic and microscopy will be used. There are multiple steps that needed
to be complete before the microscopy can be commenced. There are 5 steps in total for the
entire process. And in this experiment, the main focus will be in the latter 4 steps. The 5 steps
are as following:

1. Sectioning
2. Mounting
3. Grinding
4. Polishing
5. Microscopy

The first step is basically the process of cutting the samples into smaller pieces that is more
suitable for the mounting process. Next, the sectioned samples are put into a small cylindrical
container called the sample cup and the appropriate ratio of resin and hardener is mix and
poured into the sample cup with the sample at the bottom of the sample cup. After that, The
sample was put under sunlight for at least 24 hours so that the resin will be hardened. After
the resin has fully hardened, the grinding and polishing process will be commenced to
prepare the material so that it can be observed with a microscope. Then lastly, the microscopy
step was done, and the pictures of the sample that showed the structure of the samples will be
recorded and studied.

In the grinding and polishing steps, a machine called grinder, which consists of two
horizontally spinning wheels that have sandpapers fixed on the top. The sample is pressed
against the spinning grinding wheels and the abrasive grit is progressively changed to finer
ones to help smoothen out the surface of the sample. The polishing step is very similar to the
grinding step, but the purpose of this process is to make sure that the surface which is to be
observed would be flat and scratch-free, and will present a mirror-like appearance.

The microscopy part of this experiment will be conducted with a microscope. The
main usage of microscope in this scenario is to help observe the structures that are too small
to be observed directly with the human eye. The structure of different structures would be
vastly different in the view of microscope and this can help researchers to find out the
relationship between the structures and the properties of the said material. Microscopy can
also give information concerning a material’s composition, previous treatment and properties.
Particular features of interest are

1. Grain size
2. Phase present
3. Chemical homogeneity
4. Distribution of phases
5. Elongated structures formed by plastic deformation

Figure 1: illustration of crystal structures

With optical microscopy, the light microscope is used to study the microstructure;
optical illumination systems are its basic elements. For materials that are opaque to visible
light (all metals, many ceramics and polymers), only the surface is subject to observation, and
the light microscope must be used in a reflective mode. Contrasts in the image produced
result from differences in reflectivity of the various regions of the microstructure. Careful and
meticulous surface preparations are necessary to reveal the important details of the
microstructure. The specimen surface must first be ground and polished to a smooth and
mirror like finish. This is accomplished by using successively finer abrasive papers and
powders. The microstructure is revealed by a surface treatment using an appropriate chemical
reagent in a procedure termed etching. The etching reagents depend on the material used and
after etching the specimen must be washed with alcohol and ether to remove the grease. The
atoms at the grain boundaries are chemically more active, and consequently dissolve more
readily than those within the grains forming small grooves. These grooves become
discernible when viewed under a microscope because they reflect light at an angle different
from that of the grains themselves. When the microstructure of a two-phase alloy is to be
examined, an etchant is chosen that produces a different texture for each phase so that the
different phases may be distinguished from each other.

Objectives
1. To prepare metallographic samples for microscopic examination and techniques of
grinding and polishing will be gained hands-on.
2. To identify the microstructure of the sample using a microscope.
3. To identify the type of material that was observed from the results of the microscopy.

Problem statements
The methods of preparing the samples for microscopy are crucial to the study of
microstructures and properties of the material. Therefore, this experiment will help students
understand how the whole process of metallographic techniques and microscopy works and
help to gain the experience through practice. The microstructure of the sample is observed
through a microscope. In this experiment, the goal is to observe the microstructure of various
materials and to find out what are the relationship between the structure of materials and the
physical properties of the materials.

Hypothesis
In this experiment, the goal is to experience the process of preparing metallographic
samples and to study the material with the use of microscope. It is speculated that different
types of materials and different methods that formed the materials can result in different
structures being observed. The microstructure of the materials is also speculated to have a
direct relationship to the properties of the materials, such as density, hardness, ductility and
others. For bainite steel, bainitic ferrite platelets are lath like or lenticular plate like structures.
With increasing carbon content, bainite morphology changes from lath-like to plate-like. It is
believed that the bainitic ferrite platelets grow to a limited size, which is usually smaller than
the austenite grain size. Further bainite transformation occurs by the formation of new
parallel platelets in clusters known as sheaves. The sheaves are sometimes in the form of a
wedge shaped plate on a macroscopic scale. Studies on bainite generated around or below Ms
(martensite start temperature), through an austempering process show that a bainite and
martensite phase mixture will be generated. In this bainite-martensite mixture structure, the
lower bainite is present in not only acicular units but also in irregularly shaped laths. Spear-
like bainitic sheaves and narrow needle- like martensite plates, both dark etching, are
uniformly distributed in the microstructure along with light etching retained austenite. For
brass, the mechanism of grain refinement in copper-base alloys is less popular as compared to
other metal systems. The usual purpose of grain refinement is to decrease the grain size of
cast metal which enhances mechanical properties. Reducing the grain size also improves hot
tearing resistance, casting fluidity and enhances surface finish of various alloy systems. The
main purpose of refinement in copper alloys is to combat hot tearing, since the strength is
usually adequate.

Materials and apparatus

• Cold mounting kit complete for sample preparation (resin and epoxy) figure 2

• Sample cup and mixing stick figure 3

 • Metal specimen (brass and steel) figure 4

• Grinder and polisher machine figure 5 and 6

• Microscope figure 7

Procedure
(a) mounting
1. Appropriate ration of resin and hardener are measured according to the
manufacturer’s recommendation. (10:1)
2. The resin and hardener are mixed together in a sample cup using a mixing stick.
Air bubbles should be avoided during mixing.
3. The sample (steel and brass) are placed in the mould and the mixture is poured.
The level of mixture is ensured to cover the level of the specimen.
4. The sample is dried within 24 hours.
5. If the prepared sample was not completely dried, it is advisable to redo it and wait
for another 24 hours.
(b) Manual grinding
1. The tap of the grinder is turned on. The sample is placed face down onto the
grinder paper and abrade in one direction only. The abrasive paper used for this
step is 240.
2. The action is continued until a flat surface is achieved.
3. Then, proceed to the next station by using abrasive paper of grid size 400.
4. The abrading process is repeated with the sample, still face down, but in
orthogonal direction.
5. The process is continued until scratches from the previous operation is totally
removed.
6. Step 1 to 5 is repeated with abrasive paper of grid size 600 and 1000.

(c) Manual polishing

1. The polisher is turned on and is adjusted at low speed.
2. Some amount of polycrystalline suspension (6μm) is dropped on the Texpan
polishing nap.
3. The sample is placed face down onto the polishing plate and even pressure is
applied by hand. The sample is polished until it has a mirror-like appearance and
scratch free.
4. The sample is washed and dried.
5. Step 1 to 5 is repeated with using a finer suspension (1μm).
6. After that, the steps are repeated using alumina suspension (0.3μm and 0.05μm)
on micro cloth.

(d) Microscopy
1. The microscope is turned on.
2. The objective lens is turned to the lowest magnification.
3. The sample is place on the stage by adjusting the stage travel distance.
4. The eyepiece is adjusted to suit the eyes.
5. The focus of the object is adjusted by turning the focusing knob.
6. The observations are noted through the microscope.
Results
Specimen’s Specimen Microscopic view (100μm)
material
Steel

Brass

Discussion
The purpose of this experiment was to gain practical experience in metallographic
techniques and microscopy. To achieve this goal, the most important operations in
metallographic sample preparation were performed: cutting, mounting, grinding, polishing
and microscopy.

The first step, cutting, was performed using grindstone cutting, a method widely used
in metallographic laboratories. A thin cut-off wheel was used to minimize deformation
damage. By assembling after cutting, it is possible to handle samples with complicated
shapes. For this experiment, the compressed implementation (hot mount) and cold
implementation were chosen. In the next step, grinding, finer abrasive grains are used to
remove the surface of the sample. The initial stage used coarse grit to establish a flat surface
and remove the effects of sectioning. A finer grit was then used to achieve a smoother surface.
The final step, polishing, aims to create a flat, scratch-free, mirror-like surface for subsequent
metallographic examination. Various polishing methods such as mechanical polishing and
chemical polishing were used in the experiments. The polishing process involves the
application of polycrystalline suspensions and the use of various polishing pads with
decreasing particle size.

Microscopy played an important role in this experiment as it allowed observation and

analysis of the microstructure of the prepared samples. Microscopes have been used to
observe objects and areas that are invisible to the naked eye. The microstructure of the
samples was examined by adjusting the objective lens and focusing the microscope.
Experimental procedures were performed according to prescribed techniques including
mounting, grinding, polishing and microscopy. Results of the analysis include delineating the
microstructure of the sample, identifying defects, morphology, and features such as grain size,
orientation, and segregation. Overall, this experiment provided valuable practical experience
in metallographic techniques and microscopy. By following specific procedures of cutting,
mounting, grinding, polishing, and microscopy, the students were able to produce high-
quality metallographic samples and examine their microstructure.

Bainite Steel:

Bainite is formed at cooling rates slower than that for martensite formation and faster
than that for ferrite and pearlite formation. There are two forms of bainite, known as upper
and lower bainite.

(a)
 (b)

Figure 8: microstructure of bainite steel (a)upper bainite; (b)lower bainite

Upper bainite generally forms at temperatures between 550 and 400°C. There are
several proposed formation mechanisms, based on the carbon content and transformation
temperature of the steel, resulting in slightly different morphologies. Low carbon steels
exhibit fine bainitic laths, nucleated by a shear mechanism at the austenite grain boundaries.
Carbon solubility in bainitic ferrite is much lower than in austenite, so carbon is rejected into
the austenite surrounding the bainitic ferrite laths. When the carbon concentration in the
austenite is high enough, cementite nucleates as discrete particles or discontinuous stringers
at the ferrite/austenite interfaces. As the carbon content increases, the cementite filaments
become more continuous, and at high carbon contents, the bainitic ferrite laths are finer with
the cementite stringers more numerous and more continuous. The structure can appear more
like pearlite, and is termed 'feathery' bainite.

Lower bainite generally forms at temperatures between 400 and 250°C, although the
precise changeover temperature between upper and lower bainite depends on the carbon
content of the steel. The transformation nucleates, like upper bainite, by partial shear. The
lower temperature of this transformation does not allow the diffusion of carbon to occur so
readily, so iron carbides are formed at approximately 50-60° to the longitudinal axis of the
main lath, contiguously with the bainitic ferrite. With low levels of carbon, the carbide may
precipitate as discrete particles, following the path of the ferrite/austenite interface. However,
the overall mechanism of lower bainite formation is independent of carbon content in the
main. The appearance of lower bainite strongly resembles that of martensite, but lower
bainite is formed by a mixture of shear and diffusional processes rather than just shear.
 Figure 9: microstructure of steel (from experiment)

Brass:

The cast structure is characterized by a typical Widmanstätten morphology consisting

of α-intersecting crystals in a β-phase matrix, which has resulted from solidification processes
during casting. Brass bars of a wide range of diameters are fabricated by further
metalworking by employing hot extrusion and cold drawing. The normal metallurgical
condition corresponding to the high-machinability brass bars is that of the so-called half-hard
temper.

Figure 10: Brightfield reflected light micrograph of a longitudinal section of the as-cast brass
billet showing a typical Widmanstätten phase structure.

Whereas by comparing Widmanstätten structures in microstructure of brass in

experiment which are separated from each other by grain boundaries. During solidification,
the alpha phase preferentially precipitates in the entire beta matrix to form the Widmanstätten
structure that is compatible with the hyper-peritectic (L + α → β) composition in the Cu–Zn
phase diagram. The microstructure of brass has two Widmanstätten morphologies, one is
needle-like formation, while the other is plate-like formation. The plate formation of
Widmanstätten α-phase is related to Zn atoms constantly diffusing out from the
Widmanstätten phase due to the fast mobile regions like grain boundaries. On the other hand,
slow mobile Zn atoms pave the way for the formation of needle-like Widmanstätten structure
due to the hindering diffusivity from alloy elements. As can be seen from figure 11, the island
formation is the same morphology as Widmanstätten structure but its orientation is different.

Figure 11: microstructure of brass (from experiment)

Limitations
Contact with resin, hardeners, mixed epoxy, and sanding dust from partially cured
epoxy should be avoided first and foremost. When working with epoxies, wear protective
gloves and clothing. If you get resin, hardener, or mixed epoxy on your skin, wash it off right
away. Because resin is not soluble in water, use a waterless skin cleanser to remove resin or
mixed epoxy from the skin. Although hardener is water-soluble, wash your skin with soap
and warm water to remove hardener or sanding dust. Furthermore, it is usually recommended
to wash completely with soap and warm water after working with epoxy, including sanding.
If epoxy gets on your clothes, change them right away. This is due to the fact that skin
cleansers can be used to remove any epoxy from the skin and clothing. Continue to wear
clothes that has epoxy on it. If the item is made of mixed epoxy, it can be worn again once
the epoxy has fully set. It is advised that solvents should not be used to remove epoxy from
the skin. Solvents, even weak ones like vinegar, can force the epoxy's components into the
skin, increasing the likelihood of overexposure. It is recommended that resin and epoxy be
disposed of in a garbage can since the substance in the resin and epoxy cannot be washed
away and can contaminate the environment.

Furthermore, when using a grinding machine, it is best to constantly try to position

your work against the remainder of the work on the disc and belt sanders. Use the downward
motion side of the disc sander to sand, not the upward motion side, since this can launch your
part upwards with considerable force. It is also not recommended to use machines with
broken or ripped belts or discs. When viewed through a microscope, this can result in uneven
grinding of the materials. Before moving on to the next phase, all damage in the previous
step's samples, such as scratches, pull-outs, or imbedded grains, must be entirely eliminated.
If this is not done, artefacts from an earlier phase may appear on the completed surface,
making it impossible to determine where they came from. To improve the approach, it must
be known when artefacts begin to appear.

When using a polishing machine, it is best to wear safety glasses, a dust mask, and
gloves to protect your eyes, lungs, and skin from the dust and debris generated during the
polishing process. Furthermore, ensure that the work area is well-ventilated to prevent dust
accumulation and to reduce the danger of fire hazards. Finally, before changing polishing
wheels or performing machine maintenance, turn off the power supply. Polishing compounds
are used to improve the polishing machine's performance by lubricating the surface and
removing any scratches or dullness. Select the appropriate polishing compound for the
material to be polished and add a tiny amount to the polishing wheel, distributing it evenly.
Small projects require only a pea-sized amount of compound, but larger tasks demand more.
Clean the surface with a soft cloth after polishing to remove any excess polishing product and
look for any missed locations. If there are any flaws, repeat the polishing process until the
required finish is achieved. When you're happy with the results, turn off the polishing
machine and unplug it from the power supply.

Always start with the 4x objective lens (the lowest magnification) when using a
microscope. This will allow the microscope to focus on the sample and prevent the objective
lens from smashing into the stage. To increase magnification, move up one objective at a time,
focussing each time. When done using the microscope, always return the 4x (lowest and
smallest) objective lens to its original position for the next user. When focusing the
microscope, it is recommended that you never apply force. If the focus knob is tight and
won't turn, it's either locked, the tension needs to be adjusted, or it's colliding with an
objective lens. When looking through the microscope for the first time, the rheostat light
control or the condenser may need to be adjusted to achieve a clearer and sharper image. The
microscope rheostat regulates the strength of the light, dimming or brightening it. The
condenser can be moved up and down beneath the microscope stage.

Conclusion
In conclusion, the experiment on metallographic techniques and microscopy aimed to
provide practical experience in preparing metallographic samples and analysing their
microstructures. The experiment covered important operations such as sectioning, mounting,
grinding, polishing, and microscopy. The prescribed procedures were followed, including
resin and hardener mixing for mounting, sequential grinding using finer abrasive papers,
manual polishing with polycrystalline suspension and polishing pads, and observing the
prepared specimens under a microscope. As a result, high-quality metallographic samples
were successfully prepared, exhibiting flat and scratch-free surfaces. The sequential grinding
and polishing steps effectively transformed the initial rough surfaces into mirror-like
appearances suitable for microstructural analysis. Through the microscope observations, the
microstructures of the specimens were identified and sketched, revealing various
characteristic features such as grain size, orientation, and segregation. Additionally, the
examination of labelled specimens provided further insight into different microstructures.

Bainite steel is a plate-like microstructure that arises in steels from austenite when
cooling rates are too slow to make martensite but too fast to allow carbon to disperse and
form pearlite. Bainitic steels are stronger and harder than pearlitic steels in general, but they
also have a desirable mix of strength and ductility. In the case of brass, it is claimed that the
inclusion of additives enhances the production of beta prime phase, resulting in higher
hardness values of samples. Intergranular Widmanstätten formations degrade mechanical
characteristics by encouraging crack formation. Widmanstätten structures, on the other hand,
with needle-like shapes that usually formed at grain boundaries, improved mechanical
characteristics by preventing slip that plane movement. Due to Widmanstätten morphology
throughout the microstructure, brass exhibits low hardness, low mechanical characteristics,
and continuous chip shape when compared to other materials. The microstructure
morphology had a significant impact on the variation in chip size and shape as well as the
mechanical and hardness parameters. The presence of soft and hard phases in the
microstructure had a greater effect on machinability than mechanical qualities in several
circumstances.

Reference
1. Grinder Safety Rules. [online]. Available at:
https://www.lsu.edu/eng/mie/cuf/ammf/safetyrules/GrindersSanders.php
2. Metallographic grinding and polishing insight | Struers.com. [online]. Available at:
https://www.struers.com/en/Knowledge/Grinding-and-
polishing#grindingpolishingmethods
3. Epoxy Resin Safety Tips | Learn Our Safety Practices | Entropy Resins. [online].
Available at: https://entropyresins.com/safety/epoxy-safety-
tips/#:~:text=Wear%20goggles%2C%20safety%20glasses%2C%20gloves,with%20an
%20organic%20vapor%20cartridge...
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Step_Guide..
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Appendix

Figure 12: Materials needed for preparation of mould

Figure 13: Silicon mould release is wiped onto the mould

Figure 14: Metal specimen placed in the middle of mould

Figure 15: 1ml hardener + 10ml epoxy mixed together in a paper cup
Figure 16: Pour mould mixture into the moulds

Figure 17: Mould mixture poured to mould

Figure 18: Place mould to dry for 24 hours

Figure 19: Dried mould samples after 24 hours

Steel sample (left) and brass sample (right)
Figure 20: Grinding sample face down on grinding machine

Figure 21: Samples after grinding

Steel (left), brass (right)
Figure 22: Polishing of samples on polishing machine

Figure 23: Samples after polishing

Brass (left), steel (right)
Figure 24: Microscopy of steel sample

Figure 25: Microscopy of steel sample

Figure 26: Microscopy of brass sample

Figure 27: Microscopy of brass sample

Figure 28: Steel and brass specimens after grinding and polishing
Rubrics

Arrianna Peter, Joel Lee, Tiang Soon 1002162633, 1002265669, 1002267948

Lin