Khulna University of Engineering & Technology

Department of Materials Science and Engineering

Course Title: Compositional and Microstructural Analysis

Course No: MSE 2106

Experiment No: 01

Experiment Name: Introduction to Microstructural and

Compositonal Analysis

Submitted by

Name: Asif Reza Shadhin

Roll: 2127006
Year: 2nd

Semester: 2nd

Date of performance: 03.09.2024

Date of submission: 08.09.2024

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 Introduction to Microstructural and Compositional
Analysis

Objectives:

After the class we came to know about:

 What is microstructural and compositional analysis.

 to detect the microstructure of a metal sample.
 to study five steps for preparation of a metal sample like sectioning, mounting grinding,
polishing, etching for microstructural detection.
 To know the usage of different apparatus which are used for the mentioned steps like
diamond paste for polishing, acidic nitral solution for etching, emery paper for grinding
etc.

Introduction:

Microstructural and compositional analysis labs are essential for understanding material
properties and ensuring quality. By examining a material’s structure we can easily predict
performance, optimize manufacturing processes, and identify the causes of material failures.
They play a critical role in quality control, research and development, and improving materials
for advanced applications in industries like aerospace, automotive, and electronics. These
insights allow for better material design and enhanced product reliability.

Methodology

5 steps to prepare a metal sample or detect its microstructure:

1.Sectioning-

Sectioning is generally classified into two types: longitudinal and transverse. To detect the
microstructure of a sample, it is important to identify the position of its grains and grain
boundaries. Longitudinal sectioning, which involves cutting the sample along its length, is
particularly effective for this purpose. This method provides a clearer view of the alignment
and orientation of grains and grain boundaries, making it the most suitable technique for
determining their precise location within the material.

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 Fig 01: Sectioning
2.Mounting-

Samples are usually very small, making them difficult to handle during preparation and
analysis. To facilitate easy handling, a polymer or resin is attached to the sample in a process
known as mounting. Mounting provides a secure grip on the sample and helps minimize the
risk of damage during machining operations, ensuring the sample remains intact throughout
the process.

Fig 02: Mounting

3.Grinding-

After sectioning the sample to the required size, the resulting surfaces are typically rough. To
achieve a smoother surface, the metal sample undergoes a grinding process by using emery
paper. Emery paper contains silica particles and is available in nine grades: 120, 220, 400, 500,
600, 800, 1000, 1200, and 1500. The grade refers to the number of particles per square foot,
with grade 120 having 120 particles and grade 1500 having 1500 particles. As the grade
increases, the particle size decreases, meaning grade 1500 provides a finer, smoother surface,
while grade 120, with its larger particles, produces a rougher surface.

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The grinding process begins with emery paper, such as grade 120, and progresses through finer
grades to achieve the desired smoothness. It is important to follow this sequential approach,
starting with the lower grades and moving up to higher grades, to gradually refine the surface.
The silica particles in the emery paper help to abrade the surface, removing imperfections and
scratches left from earlier machining or sectioning processes.

A key step in the grinding process is rotating either the specimen or the emery paper by 90
degrees when transitioning to a finer grade. For example, after using grade 120 paper, the next
step would involve switching to grade 220 paper and rotating the sample or paper by 90
degrees. This technique helps to effectively abrade the deep scratches created by the emery
paper, resulting in a smoother and more uniform surface finish.

Fig 03: Grinding and Emery paper

4.Polishing-

To ensure optimal light reflection under an optical microscope, it is essential to achieve a shiny
surface on the sample, which requires polishing. In our process, diamond paste is applied in a
polishing machine to achieve the desired finish. Before polishing, the sample is rubbed on
1500-grade emery paper, and during polishing, the rubbing direction is adjusted to 90 degrees
opposite to the last direction used on the emery paper. This helps to abrade the deep scratches
created by the emery paper, resulting in a smoother and more uniform surface finish.

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 Fig 04: Polishing and Grinding machine

5.Etching:
The last and final step is etching. The main reason for etching is that grain boundary erosion
will create dark spots on the surface, which will cause light scattering in the eroded grain
boundary under the optical microscope and we can easily detect the grain and grain boundary.
The etching solution used is a nitrile mixture containing 2% nitric acid and 98% ethanol. The
polished surface typically reacts after 2–3 dips in the etching solution, highlighting the
microstructural details needed for analysis.
There are two types of etching: under etching and over etching. Under etching occurs when the
reaction is insufficient. In this case we have to dip the sample in the etching solution again.
Over etching happens when the surface is excessively eroded. In this case, we have to grind
with 1500 grade emery paper again. After etching, the sample must be wiped with water or
acetone to prevent the reaction from continuing.

Fig 05: Etching

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