School of Materials Science & Engineering

Second Year Undergraduate Experiment

MS2082 Laboratory

Formal Report

For

EB5

Microstructure of Materials

Name: Aryacitta Adijaya

Matric: U1640068L

Lab Group: GB5

Academic Year 2017-2018

Nanyang Technological University

Table of Contents
1. Objectives ................................................................................................3
2. Theory ......................................................................................................3
2.1. Metallography ..............................................................................3
2.2. Optical Microscopy ......................................................................4
2.3. Microstructure of Metals..............................................................6
2.4. Polycrystalline single-phase structure ..........................................6
2.5. Eutectic/Eutectoid metal alloys ....................................................6
2.6. Martensitic and tempered martensitic steel alloy .........................7
3. Experimental Procedures .........................................................................8
3.1. Sample Preparation ......................................................................8
3.2. Sample Preparation ......................................................................9
4. Experimental Results and Discussion ......................................................9
4.1. Sample 1 (Hypoeutectoid Steel 0.4%C).......................................9
4.2. Sample 2 (Hypereutectoid Steel 0.8%C) ...................................11
5. Conclusion .............................................................................................12
6. References ..............................................................................................12

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1. Objectives
The objectives of this experiment is to:

• Learn sample preparation techniques for metallography

• Learn how to apply optical microscopy to view the microstructure of metals
• Learn identification of microstructures
• Learn how to use ImageJ to obtain quantitative data on the microstructure

2. Theory
Metals are metallic elements bonded by metallic bonds, which result in sea of
electrons. As a result, metals are typically good thermal and electrical conductor
due to this delocalization of electrons.

Microstructure involves the arrangement of larger groups of atoms that are

normally agglomerated together, which requires microscopy techniques to reveal. In
metal, microstructure consists of grain size and shape. Microstructure is closely
related to properties and performance. For instance, smaller fine grains will be
stronger than coarse grains, due to larger area of grain boundaries that hinders
movements of dislocations. Therefore, metallography and microscopy is very
important as it allows the analysis of microstructure, which in turns allows the
prediction of performance and properties

Figure 1 – MSE Tetrahedron: Structure/composition is related to properties and performance

2.1. Metallography
Metallography is the preparation of materials surface such that microstructure
can be observed by using optical or electron microscopy. Metallography consists of
three steps: Mounting, Grinding & Polishing, and Etching.

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 Mounting involves trimming the sample to smaller size to fit the mold of the
mount. The sample is then implanted to a mold and casted in a polymer. Mounting
is done to enable easier holding of sample during the grinding and polishing step.

Figure 2 – Example of mounted sample. The

sample is white and the mount is black

After the sample is mounted, the next step is grinding and polishing. The
objective of grinding and polishing is to produce flat and defect-free surface to
produce clearer image in microscopy.

Grinding is done by rubbing the mounted sample with progressively finer grit
sandpapers. The sandpapers will abrade the surface and remove defects and
unevenness.

After grinding, polishing is needed to remove damages accumulated from the

previous step. There are two types of polishing: mechanical and chemical.
Mechanical polishing is done by rubbing the sample with special clothing
containing very fine abrasives. On the other hand, chemical polishing is done by
immersing the sample in a reactive environment.

The final step after grinding and polishing is etching, which is done chemically
by a reactive reagent. In this process, the surface of a polished metal will react with
the ragent to reveal the microstructure underneath the surface.

2.2. Optical Microscopy

The basic principle of optical microscopy is as follows: a light source emits
lightbeam that goes through a series of apertures and lenses. The beam is then
focused onto the specimen surface, and the light reflected is collected and viewed
through the eyepiece.

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 There are five basic controls of microscope:

1. Magnification, controlled by using different objective lenses,

2. Focus, controlled by turning the large and small knobs located at the side
of the microscope

3. Brightness, altered by changing the aperture,

4. Brightfield/Darkfield mode, changed by toggling the button. Brightfield

mode will form images from reflected lightbeams that align with the
optical axis, while Darkfield mode will form images from beam reflected
to the off-axis.

5. Polarizer, controlled by installing cross-polarizers into the light path.

Polarizer can be used to show surface features that are sensitive to
polarization of light

Another important aspect of microscopy is resolution, which is defined as the

smallest distance in which two different objects can be distinguishable. Resolution
of a microscope can be calculated by using formula: d = 0.61 λ / NA, where λ is the
wavelength of light and NA is the numerical aperture of objective lens. Smaller d is
desirable, and therefore there are methods to decrease the wavelength of light and
increase the numerical aperture of objective lens. For instance, changing the
medium of light from air to oil by using immersion lenses. However, for
microscopes operated in air with typical lenses, the resolution is 0.2µm.

Since optical microscopy involves lightbeam, it is important to understand which

information is carried by which attributes of lightwaves. There are four attributes of
waves including lightwaves: amplitude, wavelength, phase, and polarization.
However, only amplitude and wavelength carries information which naked human
eyes can tell.

Amplitudes is perceived as brightness, and the difference in amplitudes between

neighboring regions is seen as contrast. Wavelength also carries information about
brightness and contrast. Phase also carries information regarding contrast, but it
requires to be transformed into amplitude differences by using techniques such as
Normarski contrast.

On chemically etched metals, the reactivity of grains might depend on the

crystallographic orientations, therefore different grains will have different contrasts.
Furthermore, grain boundaries area would be etched differently from the internal
grain, and therefore the grain boundaries and internal grains will also have different
contrasts.

The result of optical microscopy is an image of the microstructure. To do

quantitative analysis of this microstrutcture, an image analyzing software, ImageJ,
is used.

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 2.3. Microstructure of Metals
2.4. Polycrystalline single-phase structure

In single phase metals, the revealed microstructure is the grains and the grain
boundaries. The grain boundaries will be shown as sharp dark lines in brightfield
mode. By using image analysis, we can quantitatively measure the grain size
distribution and the number of sides per grain (grain shape).

Figure 3 - Micrograph of polycrystalline metal etched by acid (Pleshakov, 2008)

2.5. Eutectic/Eutectoid metal alloys

In a binary solid solution, in eutectic or eutectoid composition, the two phases

will be arranged in a lamellar microstructure. Example of eutectoid alloys is Fe-C,
with ~0.76%C.

Figure 4 - Eutectoid steel structure, lamellar structure of cementite and ferrite (Bhadeshia,
2008)

In hypoeutectoid alloys, whereby the solute concentration is below the eutectoid

composition, another phase is formed before the inception of the lamellar structure.
In Fe-C alloys, proeutectoid ferrite is formed before the remaining austenite
transforms into lamellar ferrite and cementite structure.

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Figure 5 - SEM micrograph of hypoeutectoid steel, pearlite in ferrite matrix (McGill University,
2009)

On the other hand, in hypereutectoid alloys, the solute concentration is above the
eutectoid composition. Similar to hypoeutectoid alloys, another phase is also
formed before the inception of the lamellar structure. In Fe-C alloys, proeutectoid
cementite is formed before the remainder of austenite transforms into lamellar
ferrite and cementite structure.

Figure 6 - Hypereutectoid structure, pearlite in cementite matrix (Callister, 1997)

2.6. Martensitic and tempered martensitic steel alloy

Martensitic transformation of steel happens when austenite is quenched, so

diffusion of carbon out of austenite is not allowed to happen. The transformation
results in a single-phased, highly strained BCT lattice, supersaturated by carbon.
The amount of carbon induces solid-solution strengthening. Furthermore, the
transformation contributes a lot of stress, resulting in huge number of discloation
networks, which strengthens the material. Combined with less number of slip
system in BCT, Martensite is a very hard, strong, and brittle structure.

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 Due to its brittleness, martensite can not be utilized and needs to be tempered
first before used. Tempering is done by putting the metal in an elevated temperature
for a certain amount of time, so that diffusion takes place, forming the equilibrium
phases of ferrite and cementite.

Figure 7 - Martensitic structure of 0.35%C steel (Anonymous, 2007)

3. Experimental Procedures
3.1. Sample Preparation

There are two types of samples used in this experiment: 0.4%C steel and 0.8%C
steel. Both samples have been grinded beforehands, so only regrinding by using
P1200 and P2500 grit sandpapers is needed. The P1200 grit sandpaper will remove
the oxides layer, while the P2500 grit sandpaper will remove microscratches

To carry out the regrinding: first, mount the P1200 grit sandpaper into the
grinding machine. Then, turn on the machine and hold the sample on the spinning
sand paper to abrade the surface. During this process, periodically spray with water
to lubricate and rinse the sample. After 3 – 5 minutes, turn off the machine and
repeat the process, but instead of using P1200 grit sandpaper, use P2500 grit
sandpaper instead.

After regrinding, next is polishing the sample. Polishing is done to remove the
surface damage from regrinding process. The polishing procedure is the same as the
regrinding procedure. However, instead of using sandpapers, polishing paper with
diamond paste is used. Polishing is done for 5-8 minutes.

After polishing, the sample needs to be etched so that the microstructure can be
revealed. To etch, the sample is exposed to 2% nital solution for 30 seconds.
Afterwards, rinse the sample off using a suitable solvent. After etching, the sample
needs to be observed under the microscope immediately, because the sample would
get oxidized easily.

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 3.2. Sample Preparation

After the sample preparation, the sample needs to be put under a optical
microscopy in order to see the microstructure. To do so, the first step is to use the
5x magnification objective lens, and then putting the sample on the stage of
microscopy. Use the knobs to focus the image, and see the overall features of the
sample. After finding areas that are of interest, increase the magnification by
changing the objective lens. Refocus the image, and capture the final image by
using the camera.

4. Experimental Results and Discussion

4.1. Sample 1 (Hypoeutectoid Steel 0.4%C)

Proeutectoid ferrite

Pearlite

Figure 8 - 0.4%C Hypoeutectoid Steel magnified 20 times

From the optical microscopy image (shown in Figure 8), the brighter area
corresponds to proeuctectoid ferrite, while the darker area corresponds to pearlite
(Laminar structure of eutectoid ferrite and eutectoid cementite).

Figure 9 - 0.4%C Hypoeutectoid steel with brightness and contrast processed using ImageJ

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 Figure 10 - ImageJ quantitative data analysis for sample 1

The data shown in figure 10 reveals that the pearlite takes up to 85.082% of the
area of the image. Therefore, the proeutectoid ferrite takes up 100% - 85.082% =
14.918% of the area.

Figure 11 - Iron and Carbon Phase Diagram (Callister, 1997)

From figure 11, we observe that in room temperature, the weight percentage of
carbon that Cementite phase is approximately 6.70wt%, while the weight
percentage of carbon in Ferrite phase is approximately 0.02wt%.

Therefore, by applying the lever rule, the total fraction of ferrite in the system is
(6.7-0.4) / (6.7-0.02) = 0.943 = 94.3%. The total fraction of cementite in the system
is then 5.7%. Since, the proeutectoid ferrite takes up 14.918% of the system, the
fraction of eutectoid ferrite in the system is then 94.3% - 14.918% = 79.382%.

Therefore, the amount of eutectoid ferrite in pearlite is 79.382 / 85.082 = 0.933 =

93.3%, while the amount of eutectoid cementite in pearlite is 6.67%.

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 4.2. Sample 2 (Hypereutectoid Steel 0.8%C)

Proeutectoid Cementite

Pearlite

Figure 12- 0.8%C Hypereutectoid steel magnified 20 times

From the optical microscopy image (shown in Figure 8), the brighter area
corresponds to proeuctectoid cementite, while the darker area corresponds to
pearlite (Laminar structure of eutectoid ferrite and eutectoid cementite).

Figure 13 - 0.8%C Hypereutectoid steel with brightness and contrast processed using ImageJ

Figure 14 - ImageJ quantitative data analysis for sample 2

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 The data shown in figure 14 reveals that the pearlite takes up to 84.236% of the
area of the image. Therefore, the proeutectoid ferrite takes up 100% - 84.236% =
15.764% of the area.

Applying the lever rule, the total fraction of ferrite in the system is (6.7-0.8) /
(6.7-0.02) = 0.883 = 88.3%. The total fraction of cementite in the system is then
11.7%. Since, the proeutectoid ferrite takes up 15.764% of the system, the fraction
of eutectoid ferrite in the system is then 88.3% - 15.764% = 72.536%.

Therefore, the amount of eutectoid ferrite in pearlite is 72.536 / 84.236 =

86.11%, while the amount of eutectoid cementite in pearlite is 13.89%

5. Conclusion
To prepare for microscopy, metallography is an important step to prepare the
sample so that the microstructure can be revealed by using microscopy.
Metallography includes three steps: mounting, grinding and polishing, and etching.

From the optical microscopy, we observe that hypoeutectoid steel has brighter
proeutectoid ferrite phase and darker pearlite phase. On the other hand, for
hypereutectoid steel, there are brighter proeutectoid cementite phase and darker
pearlite phase.

By using ImageJ, brightness and contrast can be adjusted to distinguish darker

and brighter parts of image. ImageJ is then able to supply data of the area fraction
of the darker and brighter part of image which is the fraction of
pearlite/proeutectoid phase in the system. By applying lever rule, we can then
calculate the fraction of all phases that are present in the system.

6. References
Anonymous. (2007). 0.35%C Steel, water quenched from 870°C Taken during
my engineering course at Nanyang Technological University.

Bhadeshia, H. K. (2008). Another optical micrograph showing colonies of

pearlite. Interpretation of the Microstructure of Steels.

Callister, W. D. (1997). Materials Science and Engineering: an Introduction.

Wiley.

McGill University. (2009, March 31). Secondary electron image of a polished

and etched section of a steel helical gear. Microstructure consists of pearlite in a
ferrite matrix. Etched in 3% nital. 2000X.

Pleshakov, E. (2008, April). Microstructure of VT22 (Ti5Al5Mo5V1,5Cr) after

quenching.

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