TITLE

Microstructure Examination of Steel

OBJECTIVES
 To observe the constituents and structure of metals and their alloys by means of an optical
microscope

INTRODUCTION

Microscopic examination with digital imaging Microstructure analysis is conducted by microscopic

examination, a process that studies the structure of materials under magnification. The properties of a
material determine how it will perform under a given application and these properties are dependent on the
material’s structure. Industrial processes or treatments such as casting, welding and heat treating are often
applied to metals to prepare them for particular applications and to improve their characteristics and
properties. A microscopic examination may be conducted to evaluate the effects of a process on material
using optical microscopy at low magnification or scanning electron microscopy (SEM) under high
magnification.

There may be residual effects of these processes and treatments, inclusion or contaminants that can be
explained by microstructure analysis and microscopic examination. In many cases, the investigation centers
on the correlation between the resulting microstructure and the material properties.
For example, exposure of carbon and alloy steels to elevated temperatures during heat treatment can cause
a loss or gain of carbon near the surfaces of the parts if the atmosphere in the furnace is not properly
controlled. Decarburization causes the surface to be soft and weak with little wear resistance, while
unwanted carburization can cause the surface to become too brittle.
Also, if austenitic stainless steel does not see sufficient temperature for enough time or does not receive a
sufficiently rapid quench during heat treating, the carbon in the alloy will form chromium carbides on the
grain boundaries which will make the material brittle and susceptible to inter granular corrosion. A
sensitization test will reveal this problem.

THEORY
Before examining the steel specimen, there are some before in hand procedures to follow for a better
observation. Initially the specimen should be prepared for the examination;

 Mounting:
Is done for the ease of holding the specimen during the grinding and polishing process. Here, in one
process, cold mounting is conducted where using two components resins which are liquid to start
with but which set solid shortly after mixing. Cold mounting requires very simple equipment
consisting of a cylindrical ring which serves as a mold and a flat piece which serves as the base of
the mold. The sample is placed on the flat piece within the mold and the mixture poured in and
allowed to set. Cold mounting takes few hours to complete. Another method is hot-mounting which
uses a heating method.

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  Grinding:
Is done using rotating discs covered with silicon carbide paper and water. There are a number of
grades of paper, with 180, 240, 400, 1200, grains of silicon carbide per square inch. 180 grade
therefore represents the coarsest particles and this is the grade to begin the grinding operation. We
should always use light pressure applied at the center of the sample. Continuation of this grinding
should be carried out until the blemishes are removed.

 Polishing:
Is done to get a mirror like surface to clearly observe the structure here it is being polished by
polishers which has rotating discs covered with soft cloth impregnated with a pre-prepared slurry
of hard powdery alumina particles (Al2O3, the size ranges from 0.5 to 0.03 μm). This is done due to
fact that the surface unevenness will be removed.

The specimen should be put in acid in which the acid will attack the grain boundaries taken into a
reaction.

 Etching:
Is done due to Grinding and polishing operations produce a highly deformed, thin layer on the
surface which is removed chemically during etching. Secondly, the etchant attacks the surface with
preference for those sites with the highest energy, leading to surface relief which allows different
crystal orientations, grain boundaries, precipitates, phases and defects to be distinguished in
reflected light microscopy. (Figure 4: Surface reflections)

Figure 4: Surface reflections

Before Etching After Etching

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To calculate the average grain size, the average grain interception method is used. How it is conducted is
initially drawing a set of equal length parallel lines on the micrograph. After that, counting the number of
times the line segment cuts the grain boundary, and thereafter finding the ratio of intercepts to the line
length.
(Number of Lines)×(Length of a Line)
Avarage Grain Size = (Total Number of Grains Cut)

MATERIALS AND APPARATUS

 Optical Microscope with 50x and 1000x magnification.
 A light source.
 Piece of steel of which its surface fully polished (using abrasive papers and powders).
 Meter ruler
 25ml of alcohol
 25ml of Nitric Acid (HNO3)
 Alumina Powder

PROCEDURE
 A piece of steel was chosen.

 The grinding and polishing machine was switched on and piece of steel was grinded until smooth
face is coming.

Grinding and Polishing machine

 The piece of steel was polished by using the grinding and polishing machine ( Alumina powder
was used for polish)

 Next, the piece of steel was embossed 10 seconds one by one in 25ml of alcohol and 25ml of
HNO3.

 It was then placed under an optical microscope and a light was shown on to the cut surface of the
piece of steel while the sample was under the microscope.
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 Optical Microscope

 A printout of the microstructure was taken to scale on a paper

 About five parallel equally lengthen of straight lines were drawn on the printed paper.

 Afterwards the number of grains were counted which each line was cut. Started from the middle
of a grain.

 The counted number of grains were then summed up.

 The number of grains was then divided by the number of lines to find the average number of
grains.

 The length of the line was taken to the scale of the. Taken the length of the line according to the
scale of the printed microstructure and divided it by the number of grains to find the average size
of a grain.

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RESULT

Average Grain Size = 1.22 cm

Scale = 9.9 cm : 400µm
Actual Grain Size = 49.29 µm

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CONCLUTION
 Average grain size was given by :-

(𝐍𝐮𝐦𝐛𝐞𝐫 𝐨𝐟 𝐋𝐢𝐧𝐞𝐬)×(𝐋𝐞𝐧𝐠𝐭𝐡 𝐨𝐟 𝐚 𝐋𝐢𝐧𝐞)

𝐀𝐯𝐚𝐫𝐚𝐠𝐞 𝐆𝐫𝐚𝐢𝐧 𝐒𝐢𝐳𝐞 = (𝐓𝐨𝐭𝐚𝐥 𝐍𝐮𝐦𝐛𝐞𝐫 𝐨𝐟 𝐆𝐫𝐚𝐢𝐧𝐬 𝐂𝐮𝐭)

 The microstructure examination experiment provided an important information of any

crystalline structure, may it be metallic or non-metallic. The observation through optical microscope
gave a clearer understanding of the grains. The grain boundary and size determination made in the
experiment demonstrates the practical way of calculating grain size from SEM (scanning electron
microscopy) image. After observing different samples of metals the observatory comparisons
satisfied the objective of the experiment. This examination is conducted in the industry to identify
failure of materials and evaluation specifications.

REFERENCES

 https://gradesfixer.com/free-essay-examples/title-microstructure-examination-of-steel/
 https://en.wikipedia.org/wiki/Microstructure
 https://www.researchgate.net/publication/274633732_Microstructure_Examination_and_Hardness
_Test
 http://www3.telus.net/BrentBeach/Sharpen/metallography.html
 https://pubs.acs.org/doi/abs/10.1021/ie50030a018

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