MT1011 Engineering Materials

The Microstructural
Examination of Steel - Report
Ms. Vithiya 26/03/2024
09/04/2024 09/04/2024

EN23534018 Ratnasena L. W. D. L.
 SRI LANKA INSTITUTE OF
INFORMATION TECHNOLOGY
Faculty of Engineering

Engineering Materials
Microstructural Examination of Steel

MT1011

Lecturer Name: Dr. Mudith Karunaratne

Laboratory Instructor: Ms. Vithiya
Group: 05 – C
L. W. D. L. Ratnasena
EN23534018

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List of Tables
Table 1: Table presenting line number and intercept counts. ................................................................... 8

List of Figures
Figure 1: A modern optical stereo microscope (Sina Ebnesajjad PhD, in Surface Treatment of Materials
for Adhesive Bonding, Second Edition, 2014, Elsevier Inc). .................................................................. 3
Figure 2: Jeol JSM-IT800 Scanning electron microscope (Source:jeol.co.jp). ....................................... 4
Figure 3: Provided Steel Micrograph ....................................................................................................... 7

Table of Contents
List of Tables ............................................................................................................................................ 2
List of Figures .......................................................................................................................................... 2
Table of Contents ..................................................................................................................................... 2
Title: The Microstructural Examination of Steel...................................................................................... 3
1. Objectives ......................................................................................................................................... 3
2. Introduction ...................................................................................................................................... 3
3. Theory .............................................................................................................................................. 5
3.1. Alternate Experiment to Analyze Microstructure of Steel ....................................................... 5
3.2. Theoretical Examination of Steel’s Microstructure Using Light Microscope ......................... 5
4. Materials and Apparatus ................................................................................................................... 6
5. Procedure .......................................................................................................................................... 6
6. Observations ..................................................................................................................................... 7
7. Results .............................................................................................................................................. 7
8. Calculations .......................................................................................................................................... 8
9. Discussion ........................................................................................................................................ 9
10. Conclusion .................................................................................................................................. 10
References .............................................................................................................................................. 10

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Title: The Microstructural Examination of Steel

1. Objectives
At the end of the laboratory exercise, the student will be able to prepare metallurgical specimens for
analysis using optical microscopic techniques.

2. Introduction
Metallography is the study of the microstructure of metals by observing a specially prepared surface
under high magnification on a fine scale. Optical and electron microscopes are widely used in
metallography. The techniques used in metals are extended to ceramics, polymers, and composites.
Structures which occur on a coarser scale are termed macrostructure and can be studied by the naked
eye or under low magnification using microscopes.
Optical microscopes are used for resolutions down to roughly the wavelength of light whereas electron
microscopes are used for detail below this level, down to atomic resolution.
The most commonly used optical microscope is the conventional light microscope. In principle, optical
microscopes may be used to look through specimens (transmission) or in reflection. Metals, however,
do not transmit light and therefore only the surface of a specimen can be observed with an optical
microscope.
Microscopy can provide information about the composition of the material which can be used to
determine the properties and previous treatment (history). Some information about metals that can be
obtained using optical microscopes is:
• Grain size
• Phases present and their distribution
• The shape (morphology) of phases
• Cracks and other damages
• Porosity
• Particles

Figure 1: A modern optical stereo microscope (Sina Ebnesajjad PhD, in Surface Treatment of Materials
for Adhesive Bonding, Second Edition, 2014, Elsevier Inc).
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In electron microscopes, all of the above features can be observed at high resolution and magnification.
In addition, modern electron microscopes can provide information such as
• Chemical composition of a fine region
• Grain orientation
• Atomic scale structure
• Dislocation
• 3D structure of grains and defects
• Effects of heat treatments and reactions in real time
Careful surface preparation is necessary to obtain the important details of the microstructure. The
specimen surface must be ground and polished first to a smooth and mirror like finish. This is achieved
by using successively finer abrasive papers and powders.

Figure 2: Jeol JSM-IT800 Scanning electron microscope (Source:jeol.co.jp).

The microstructure is revealed by a surface treatment using an appropriate chemical reagent in an etching
procedure. The reagent depends on the material used and after etching the specimen must be cleaned
with alcohol and ether to remove any grease or other debris.
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 identified when viewed under
a microscope because they reflect light at an angle different from that of the grains themselves. Different
phases can also be revealed by the technique.

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 3. Theory
3.1. Alternate Experiment to Analyze Microstructure of Steel
Scanning Electron Microscopy (SEM) is a versatile tool that allows us to obtain micro images with high
resolution and to obtain valuable information about the surface state and chemical composition of objects
under study. In Optical Microscopy, visible light is needed to illuminate specimens for an optical
microscope unlike in SEM where electrons are focused as a beam used to probe the specimen.
• SEMs exhibit electron beam sources, which can be produced from two types of sources: using
tungsten filament or field emission guns. A beam is accelerated to a very high energy level and
then directed towards the sample (Tsutsui et al., 2020).
• A thin film of the conductive material must be applied on all samples for SEM analysis as it
removes statistical charge and improves imaging quality. A sample is usually mounted on an
adhesive-conductive substrate with the help of adhesive tape (Tsutsui et al., 2020).
• The electron beam is focused to scan the sample in a rasterized pattern, across its surface. The
beam interacts directly with the atoms in the sample, giving rise to different signals, such as
secondary, backscattered, and characteristic X-rays. These signals carry information regarding
the crystal structures of the specimen (Tsutsui et al., 2020).
• Polarized detectors placed at a certain height above or below a sample can record signals that are
emitted or bounced back from the surface. X-ray beams sent from the sample under analysis can
be examined by EDS detectors giving information about the chemical elements present in the
sample (Tsutsui et al., 2020).
• The detectors receive signals to process and generate images of the surface beam. SEM images
can disclose spots that appear as grain boundaries, surface roughness and cracks to a range of
magnifications up to several hundreds of thousands (Tsutsui et al., 2020).

3.2. Theoretical Examination of Steel’s Microstructure Using Light Microscope

To get information on the microstructure of a material, it is important to do a surface preparation before
imaging. There may be small micro-cracks or some impurities between the grains after the grinding,
polishing, etching and mounting procedures of sample preparation.
Grinding
The surface of a small steel specimen which is cut out from a workpiece needs to be ground first. For
that, the specimen should be mounted in a resin. Then the grinding process is done by using a laboratory
grinding machine with abrasive papers. The surface of the specimen should be ground until the blemishes
are removed (Switzner, 2010).
Polishing
The surface of the steel specimen should be polished using alumina powder or diamond paste to obtain
a clear, smooth, and reflective finish (Switzner, 2010).
Etching
In the etching process, the surface of the specimen should be coated with an appropriate chemical reagent
solution for microstructure observation and then polished with alcohol. Grain boundary atoms release
certain chemical activity which forms small grooves. These grooves are fairly easy to spot when looking
through a microscope because the atoms give off the light at a different angle than those grains (Switzner,
2010).
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Grain Size Determination
Finally, straight lines should be drawn on the sketched or printed microstructural image of the specimen.
Then the number of grain intersections by each line should be counted and noted down. After that, the
grain size is derived as follows (Switzner, 2010).

4. Materials and Apparatus

• Steel Specimen
• Small vial of alcohol
• Optical Microscope
• Grinder/Polisher Machine
• Diamond Lapping paste
• Dilute acid (2% Nital for steel)
• Mounting Resin water

5. Procedure
• Firstly, a small steel specimen was sectioned out from a workpiece while being cooled with water
to keep the sample cold during the cutting process.
• After that, the specimen was air-dried using a hair dryer.
• Next, liquid resin was poured into the mould after placing the plane of the examination sample
facing downwards.
• The specimen with the resin mould was placed in a light curing machine under blue light for
about half an hour to allow the resin to complete polymerization.
• Subsequently, the surface of the specimen was ground to obtain an even surface with different
grits of sandpaper. The grinding process involved using a coarse-grained paper followed by a
finer-grained paper.
• After the grinding process, the specimen was cleaned again with water and air-dried using a hair
dryer.
• The specimen was then polished several times to obtain a smooth, reflective, and shiny surface.
• Following polishing, the sample was washed under gently running water, wiped with cotton
wool, and rinsed with alcohol.
• The testing sample was dipped in an etchant (2% Nital) for about half a minute and air-dried to
observe the microstructure of the specimen.
• The sample was then placed under a focused optical microscope and the microstructure of the
prepared steel specimen was observed.
• Lastly, a chosen number of straight lines of the same length were marked on the microstructure
image, and then the average grain size was calculated using this information.
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6. Observations

Figure 3: Provided Steel Micrograph

7. Results

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Table 1: Table presenting line number and intercept counts.

8. Calculations

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9. Discussion

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 10. Conclusion
Finally, the study regarding the microstructural investigation of steel conducting metallography
techniques guarantees significant information about the material. With careful preparation, including
cutting, polishing, grinding, and etching, the microstructure of the steel sample was exposed by the
optical microscope. The benefits of metallography in industries, as well as in our everyday life were
presented, showing its involvement in the control of quality, selection of materials, product design and
development, analysis and investigations, research, and education. By gaining an understanding of
metals, professional scientists can suggest improvements, develop optimized products, and make sure
the quality of the materials produced is high. In general, the experiment shows the importance of
metallographic examination in the expansion of materials knowledge and the efficiency and
development of products.

References
Switzner, N.T. (2010) Stainless steel microstructure and mechanical properties evaluation [Preprint].
doi:10.2172/1129927.
Tsutsui, K., Terasaki, H., Uto, K., Maemura, T., Hiramatsu, S., Hayashi, K., Moriguchi, K., & Morito,
S. (2020). A methodology of steel microstructure recognition using SEM images by machine learning
based on textural analysis. Materials Today Communications, 25, 101514.
https://doi.org/10.1016/j.mtcomm.2020.101514

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