TITLE

Microstructure examination of steel

OBJECTIVE
To observe the constituents and structure of metals and their alloys by means of an optical
microscope.
INTRODUCTION
Metallography is the study of microstructures of metals. This is performed in order to analyze
microstructures in materials, to better understand materials behavior and performance. This is
usually done for examining defects in materials. The aim of this experiment was to inspect the
microstructure, the shape and size of the grains for a given sample. To observe microstructures, it
requires high magnification therefore either optical or electron microscopes are used.
Microstructure
Microstructure refers to the surface structure of materials that can be revealed under
magnification higher than 25×. The structure of a material can be described through its
microstructure and crystal structure. The microstructure of a material can strongly affect physical
properties such as strength, toughness, ductility, hardness, corrosion resistance, high/low
temperature behavior and wear resistance.
Why is metallography important?
Metallography plays an important part in the engineering field as it helps to determine several
physical and chemical properties of a material. This helps in deciding whether to accept or reject
a material with respect to its intended purpose. Through metallography grain size and shape,
porosity, cracks, second phases, and fracture processes are investigated.

The microstructure study of the metallic materials is done by a specific microscope called
“Metallurgical Microscope”. However optical and electron microscopes can be used as well.
Optical Microscope Electron Microscope
 Uses light (approx wavelength 400-  Uses an electron beam (approx
700 nm). equivalent wavelength 1 nm).
 Image formation is controlled by glass  Beams of electrons can be focused
lenses . using electromagnets
 Relatively low resolution.  Much higher resolution.
 Colorful images are formed which are  Produce greyscale images.
mostly visible due to stains in the
specimen.
 Figure 2 : An electron microscope

Figure 1 : An optical microscope

Microscopy can give information regarding a the composition, previous treatment and properties
of a material. Metallography may determine the below features of interest :
1. Grain size
2. Phases present
3. Chemical homogeneity
4. Distribution of phases
5. Elongated structures formed by plastic deformation.
6. Porosity
To reveal the important details of the microstructure, it is important to prepare for the surface for
observation.
THEORY
Generally there are a several steps to be followed before observing the microstructure of a
material.
1. Sectioning
 Sectioning suggests that removal of convenient size specimen from massive sample with
lowest damage to microstructure with the assistance of abrasive cut off machine.

2. Mounting
Mounting facilitates handling throughout preparation and handling. It conjointly avoids
injury to polishing wheels throughout polishing. The most commonly used mounting
method is Bakelite which uses a thermosetting plastic compound to encapsulate the
specimen known as the hot-mounting process. The other method uses a room temperature
curing epoxy known as cold mounting process.

3. Grinding
Grinding helps to remove the damages on the specimen that might have been created
during sectioning. Grinding is achieved by abrading the specimen surface through a
sequence of operations using progressively finer abrasive grits and wheels.

4. Polishing
Polishing is that the final step in preparing a surface that's flat, scratch free, and mirror-
like in appearance. Polishing should be carried out in a relatively dust-free area, ideally
removed from the area for sectioning, mounting and grinding. There are several different
abrasives used for polishing. Diamond, alumina and Silicon carbide are some of the
commonly used abrasives.

5. Etching
Etching is used to reveal unique structural characteristics of a metal. This commonly
involves immersing the sample in an etchant such or swabbing the surface with an
etchant. This is done typically to remove the surface layer of the material which could
have been distinctly deformed during previous procedures.

Figure 3:Section of a grain boundary

and its surface groove produced by
etching (Callister, Jr and
G.Rethwisch,2000)
Figure 4 : Photomicrograph of the surface of apolished etched polycystalline specimen. (Callister,
Jr and G.Rethwisch,2000)

MATERIALS AND APPARATUS

 A section of mild steel

 A Grinding and Polishing machine
 HNO3 Acid
 Ethyl alcohol
 A light microscope
 Water
 Steel ruler
 Pencil

PROCEDURE
 First a piece of mild steel is obtained which had been sawed prior to the experiment.

 Second the piece of metal is subjected to grinding in the grinder. The metal piece was
held tightly in one position and rotation controlled with the knob on the grinder.

 This was done repeatedly for about roughly 20 to 25 minutes until a smooth, mirror-like
surface is revealed.

 Then the piece of steel is subjected to polishing in the polisher with a red velvet surface.
Some of the diamond paste is placed on the velvet and the metal placed on it. Then the
machine is switched on again with the rotation controlled by the knob. As the plate
rotates the diamond paste rubs against the surface of the steel.
 Next etching was performed with 2% concentrated Nitric acid solution. The specimen
was dipped in the acid and left for a few seconds.

 The etched specimen was then washed in some ethyl alcohol. (This was done in order to
remove any signs of acid on the purpose and neutralize it)

 Then the specimen was left for a few minutes to dry.

 The prepared surface was placed with the mirror like side facing upwards on the
microscope. The microstructure of the material was observed through the eye piece.

 A hard copy of the photomicrograph was obtained and 5 lines with a length of 6 cm was
drawn on it, not parallel to one another. The amount of grains across each line was
counted and used to calculate the average grain size. (Grain size is important as it
influences the properties and behavior of the material)
OBSERVATIONS
CALCULATIONS
Calculation for grain size :

Average grain size = (Number of lines x Length of each line) / Total number of intersections

Line a : 2.5
Line b : 5.0
Line c : 5.5
Line d : 4.0
Line e : 5.0
Total no number of intersections = 22.0

⸫ Average grain size = (5x6)/22 cm

= 1.3636 cm → 55.08µm
Discussion
Phases present in the observed microstructure
Microstructures become meaningful when examined in the context of their metallurgical theory.
Microstructures of metal alloys are characterized by number of phases present and their
arrangements.
Phase : A phase is a specific arrangement of atoms in a regular repeating array, with a defined
range of atomic compositions on each symmetrically unique site in the array.
(core.materials.ac.uk)
Phases can be divided into two categories :
1. Single phase (homogeneous)
2. Multi phase (Heterogeneous)

Phase Symbol
Austenite γ
Allotriomorphic ferrite α
Idiomorphic ferrite αI
Pearlite P
Widmanstätten ferrite αw
Upper bainite αb
Lower bainite αlb
Acicular ferrite αa
Martensite α'
Cementite θ
Figure 5 :Phases and the symbols used to represent them (phase-trans.msm.cam.ac.uk)

Figure 6 : Crystal structures of

austenite, ferrite and cementite,
and the Fe-C equilibrium phase
diagram.(core.materials.ac.uk)
Austenite
This has a Face Centered Cubic (FCC) structure with closely packed carbon atoms. Austenite is
formed when an iron-based alloy is heated above about 750°C.
Allotriomorphic ferrite
The word allotriomorph means that the shape of the ferrite does not reflect its internal crystalline
structure. This is because it tends to nucleate at the austenite grain surface
Idiomorphic ferrite
Has a crystallographic ally deoformed shape.

Figure 7 :Allotriomorphic and Idiomorphic

(Phasetrans.msm.cam.ac.uk, 2017)

Pearlite
This microstructure is a mixture of both ferrite and cementite. This microstructure is formed after
Eutectoid Reaction at 723°C.
Martensite
Martensite is formed when austenite is cooled to a temperature below MS. In this process the FCC
body of austenite is converted to a body centered tetragonal structure.

Figure 8: The arrangement of atoms in martensite.

Bainite
Upper bainite- consists of clusters of platelets of ferrite adjacent to each other and in almost
identical crystallographic orientation, so that a low–angle boundary arises whenever the adjacent
platelets touch. (phase-trans.msm.cam.ac.uk)

Figure 9: Upper and lower bainite. (phase-

trans.msm.cam.ac.uk)

Cementite
It is a harder but brittle phase which contains 6.67% Carbon at room temperature. It has a
chemical formula of Fe3C and a orthorhombic crystal structure.

Importance of metallography
1.Industrial importance
Metallography is a valuable method of testing and investigation that enables us to
identify the physical and chemical properties of a material. This is a vital part in
engineering and industrial fields, for identifying which materials are to be used for
specific purposes. By observing the microstructures we are able to make changes that
affects the physical properties of the materials.
2. Metallographic sampling of archaeological artifacts
The metallographic study of an archaeological artifact involves the removal of a small
sample of metal from the artifact and the subsequent microscopic examination of the
sample.( ocw.mit.edu)
Information obtained through metallography about an artifact :
 The process of how an object was manufactured
 Temperatures the object could have been subjected to
 Type and extent of corrosion
 The percentage composition of different metals and alloys in the object.
 Impurities in the material
3. Material sciences
 To observe the extend of carburization.
Sources of error and how to avoid them
Errors:
 Damages to structure during the sectioning process.
 Too much diamond paste used during polishing
 pH of HNO3 acid too high/too low
 Contaminated pad.
 Surface of specimen not properly dried.

Steps taken to minimize/eliminate errors

 Adding water to the rotating wheel to reduce scratches.
 Apply proper amount of diamond paste carefully.
 Carefully measure the concentration of the acid and alcohol.
 Dry the specimen well
 Draw more lines on the photomicrograph to determine the grain size more accurately.

Precautions
 Keep the grinding and polishing areas clean and dust free. Keep power switched off and
cover the wheels with a cloth after use.
 Properly dispose the etchants. Throw the etchants into the sink and dilute it with water.
Wash all containers with water after use.
 Wear goggles and gloves when handling the chemicals as they may be harmful.
 Wash hands thoroughly after handling the chemicals.

Alternative method to calculate grain size

The grain size is also calculated in another way which is more common and is devised by the
American Society for Testing and Materials (ASTM). Using comparison charts they have
assigned average grain sizes to a number ranging from 1 to 10. These numbers are called grain
size number, denoted as n. Although a standard of 100X magnification is used in the provided
formula other magnifications can used in the calculation by simple conversions.
(researchgate.net)
N=2n-1
Here N is the average number of grains per square inch at a magnification of 100X.
CONCLUSION
In conclusion the microstructure examination of steel experiment is a very useful experiment
which should be carried out carefully to obtain the correct results. Metallography provides
important information about any crystalline structure, metallic or non-metallic. After observing
the grain structure of steel, the objective of this experiment was satisfied.
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