Heaven’s Light is Our Guide

Rajshahi University of Engineering & Technology

Course No.: MSE 2104
Course Title: Metallography Sessional
Experiment No.: 06
Experiment Title: Microstructure study of Hypereutectoid Steel or
High Carbon Steel
Date: 23 November, 2020

Submitted By:
Name: Kazi Mamunur Rahman Rifat
Student ID: 1813052
Department: Materials Science and Engineering

Submitted To:
Maliha Rahman
Lecturer, Department of Materials Science and Engineering,
Rajshahi University of Engineering & Technology (RUET)
Introduction
Steel is an alloy of iron with typically a few percent of carbon and small amount of silicon,
phosphorus, sulphur and oxygen to improve its strength and fracture resistance compared to
iron. But the main elements of steel are iron and carbon. But the carbon percentages do not
cross above the 2%. In this study we will consider the percentages of manganese, phosphorous,
sulphur and oxygen. The main purpose of this report is to study about the high carbon steel, its
phase diagram (phases, eutectoid point and reaction) and microstructure. The other purposes
of this experiment are to know about the microstructural change with the other carbon
percentages in iron, the effect of heat treatment on the microstructure, what will be the
difference in practical life with ideal microstructure and the problem what we can be faced to
the procedure how we prepared a specimen to see the microstructure.

Theory:
Steel is an alloy of iron with a carbon content that can range from 0.02% to 2% of its
composition, depending on its grade. Steel is not the same as iron and should not be confused.
Iron is a metal relatively hard and tough, with atomic diameter 2.48 Å with melting temperature
of 1535° C and boiling point 2740° C. Steel often melts at around 1370 degrees C (2500°F).
But the temperature can be varied with the various percentages of carbon content. The main
difference between iron and steel lies in the carbon content.
Steel retains the metal characteristics of iron in its purest form, but the addition of carbon and
other elements either metallic or non-metallic improves its physical-chemical properties,
especially its resistance. There are many types of steel according to the content of alloying
elements. Each type of steel will allow different uses and applications, making it a versatile
and widely used material in modern life.

Figure 1: Fe-FeC3 Phase Diagram

From the figure 1, with the several percentages of carbon atom steel can be classified into four
types. These are:
1. Dead Soft Steel: Carbon percentages will be 0.02% to 0.3%.
2. Low Carbon Steel: Carbon percentages will be 0.3% to 0.6%
3. Medium Carbon Steel: Carbon percentages will be 0.6% to up to 0.8%
4. High Carbon Steel: Carbon percentages will be above the 0.8% to up to 2%
In this types, low and medium carbon steel is called hypo-eutectoid steel; carbon content will
be 0.3% to up to 0.8% and high carbon steel is known as hyper-eutectoid steel. There is another
type of steel which eutectoid steel or pearlite. It is the alternate mixture of ferrite and cementite.
It is formed for 0.8% carbon content bellow the temperature of 723° C. In this report we will
study briefly about the hyper-eutectoid steel and its microstructure.

Hyper-eutectoid Steel
Hyper carbon steel is the high carbon steel in which the percentages is above the 0.8% to up to
2%. Above the 2% of carbon content it is not so long called steel, then it is known as cast iron.
At room temperature equilibrium structures of hypereutectoid steels are a mixture of β-Fe and
Fe3C phases. Upon cooling γ-Fe into the two-phase β-Fe + γ-Fe field, proeutectoid β-Fe
nucleates at the prior γ grain boundaries. The situation is not unlike rejection of a proeutectoid
phase from a prior liquid in a eutectic system. Just above the eutectoid isotherm, the lever rule
indicates that the amount of γ-Fe present is (C0 − 0.8)/ (2 – 0.8), where C0 is the initial
hypereutectoid steel composition. Below 723°C all of this γ-Fe transforms to a two-phase
mixture of β-Fe + Fe3C. Just as eutectic two-phase mixtures have a characteristic appearance,
so does pearlite. It consists pearlite structure, the eutectoid appears to have a fingerprint-like
lamellar structure. Slowly cooled hypereutectoid steels then contain varying proportions of
cementite and pearlite depending on steel composition.

Figure 2: Equilibrium phase transformations in hypoeutectoid and hypereutectoid steels

microstructures
Properties:
In hypereutectoid steel, pearlitic grains are of great importance in a number of extremely
demanding structural applications, in large part because of their combination of strength and
toughness. Strength and toughness are controlled by the microstructures developed by pearlitic
grain, especially interlamellar spacing, pearlite colony size, carbon content and prior austenite
grain size. Because of the more carbon atoms in cementite, it is a hard, brittle phase and outlines
potential paths for crack propagation. A Fe3C coarse network is, therefore, viewed with
concern. The basic requirements for these steels are: sufficient hardenability, wear resistance
as high as possible strength and fracture toughness.

Application:
As hypereutectoid steel contains more carbon steel, it becomes brittle. So, it is not so much
suitable for the long-lasting work. But mixing some ingredients like manganese, sulphur,
nickel, copper, zinc etc. we can use hypereutectoid steel in different way such as surgical
instrument, chef knife, frying pan, sharpener blade, cookware, cutlery set and so on.

Findings:
To see the microstructure, we have to follow a process to make the specimen properly. For this
we have to follow some steps properly. If the processes are not maintained properly, the
microstructure of the alloy under a microscope machine is not seen properly. A well-prepared
metallographic specimen is:
• Represent sample.
• Sectioned, ground and polished so as to minimize disturbed or flowed surface metal
caused by mechanical deformation, and thus to allow the true microstructure to be
revealed by etching.
• Free from polishing scratches and pits and liquid staining.
• Polished so that inclusions are preserved intact.
• Flat enough to permit examination at high magnification.
To achieve these conditions, we have to do the experiment under the following steps:
1. Sectioning:
Many metallographic specimens are used for process control. Separate test pieces or
coupons attached to castings or forgings should be designed so that a minimum of
sectioning is required for producing metallographic specimens. Important uses of
metallography other than process control include: examination of defects that appear in
finished or partly finished products and studies of parts that have failed in service.
Investigations for these purposes usually require that the specimen be broken from a large
mass of material, and often involve more than one sectioning operation. The first thing to
remember when cutting samples, is to preserve the sample axes orientation. Cut the sample
in such a manner that important sample directions, like the Rolling Direction, Transverse
Direction and Sample Normal are not lost. The second thing to remember that the cutting
process must not damage or change the sample as this would lead to erroneous results.
Avoid aggressive cutting methods that generate heat or cause deformation at the cut
surface. The selection of abrasive wheel is therefore important to avoid introducing
unnecessary levels of damage when cutting materials.
2. Mounting of Specimens:
The primary purpose of mounting specimens is for convenience in handling specimens of
difficult shapes or sizes during the subsequent steps of preparation and examination. A
secondary purpose is to protect and preserve extreme edges or surfaces defects during
preparation. Specimens also may require mounting to accommodate various types of
automatic devices used in laboratories or to facilitate placement on the microscope stage.
An added benefit of mounting is the ease with which a mounted specimen can be identified
by name, alloy number, or laboratory code number for storage by scribing the surface of
the mount without damage to the specimen. Small specimens generally require mounting
so that the specimen is supported in a stable medium for grinding and polishing. The
medium chosen can be either a cold curing resin or a hot mounting compound.

3. Coarse Grinding:
Grinding is a most important operation in specimen preparation. During grinding the
operator has the opportunity of minimizing mechanical surface damage that must be
removed by subsequent polishing operations. Even if sectioning is done in a careless
manner, resulting is severe surface damage, the damage can be eliminated by prolonged
grinding. Grinding can be achieved in a variety of ways, using a variety of abrasives. Fixed
abrasive surfaces are available using diamond or cubic boron nitride (CBN) abrasives. The
method used to bind the abrasives to the wheel affects the grinding characteristics, the
harder or more rigid the bonding medium, the more aggressive the grinding action of the
surface. Therefore, metal bonded fixed abrasive wheels are the most aggressive grinding
surfaces, whereas resin bonded wheels are less aggressive.

4. Fine Grinding:
Silicon Carbide (SiC) paper is the traditional method used for fine grinding and is adequate
when used properly. SiC paper blunts quickly and therefore should be discarded after a
short period of grinding in order to maintain efficient 'stock' removal. Grinding on a surface
that has blunt abrasives causes a great deal of surface damage by smearing, 'burnishing' and
local heating. Ensure that sharp abrasives are used and follow the manufacturer’s
instructions with regard to grinding speeds, direction, force, times and lubricants used.
Damage injected during grinding may be invisible in the polished surface. Remember that
different materials have different abrasion characteristics. The selection of grinding
material and conditions can therefore be specific to a given sample. To ensure the complete
elimination of the previous grinding scratches found by visual inspection, the direction of
grinding must be changed 45 to 90 degrees between successive grit sizes. In addition,
microscopic examination of the various ground surfaces during the grinding sequence may
be worthwhile in evaluating the effect of grinding. Each ground surface should have
scratches that are clean-cut and uniform in size, with no evidence of previous grinding
scratches. Success in grinding depends in part on the pressure applied to the specimen. A
very light pressure removes insufficient metal. Somewhat heavier pressure produces
polishing, while still heavier pressure brings about the desired grinding action. Very heavy
pressure results in nonuniform scratch size, deep gouges, and embedded abrasive particles.
Generally, a medium to moderately heavy pressure applied firmly gives the best results.
Specimens should be cleaned after each grinding steps to avoid any carryover of abrasive
particles to the next step.
5. Weight Polishing:
However soft cloths allow the abrasive to abrade different areas at different rates, giving
rise to 'relief'. 'Relief' is the term used to describe the undulations that form in a polished
surface. Extreme undulations or relief in the polished surface is to be avoided. Harder
polishing surfaces or cloths, conversely, produce a flatter or 'plane' surface, but may leave
polishing damage in the surface of the material, and promote superficial scratching.
Polishing is the final step in production a surface that is flat, scratch free, and mirror like in
appearance. Such a surface is necessary for subsequent accurate metallographic
interpretation, both qualitative and quantitative. Remove and dry the sample in the usual
manner, using a solvent with low water content and not so volatile as to cause water
condensation on the surface. Alcohol is ideal, whereas acetone is not.

6. Etching:
Although certain information may be obtained from as-polished specimens, the
microstructure is usually visible only after etching. Only features which exhibit a
significant difference in reflectivity can be viewed without etching. This is true of
microstructural features with strong color differences or with large differences in hardness
causing relief formation. Cracks, pores, pits, and nonmetallic inclusions may be observed
in the as-polished condition. In most cases, a polished specimen will not exhibit its
microstructure because incident light is uniformly reflected. Since small differences in
reflectivity cannot be recognized by the human eye, some means of producing image
contrast must be employed. Although this has become known as "etching" in
metallography, it does not always refer to selective chemical dissolution of various
structural features. There are numerous ways of achieving contrast. These methods may
classify as optical, electrochemical (chemical), or physical, depending on whether the
process alters the surface or leaves if intact. The purpose of etching is to optically enhance
microstructural features such as grain size and phase features. Etching selectively alters
these microstructural features based on composition, stress, or crystal structure. The most
common technique for etching is selective chemical etching and numerous formulations
have been used over the years. Etching is an oxidizing process which causes corrosion with
the grain boundary atoms. Because the grain boundary atoms are more energetic than the
grain atoms. So, they are more unstable and by joining the rection they want to make them
stable. Under the microscope we can see the corroded grain boundary.

7. Specimen Storage:
When polished and etched specimens are to be stored for long periods of time, they must
be protected from atmospheric corrosion. Desiccators and vacuum desiccators are the most
common means of specimen storage, although plastic coatings and cellophane tape are
sometimes used.
These seven steps are very much important to see the microstructure of an alloy. If these steps
are not maintained properly there are many defects on the microstructure. So, we should be
careful during doing these steps.
After doing all the discussed steps, we can see the microstructure of a hypereutectoid or high
carbon steel. The structure will be like the following picture:
 30 μm

Figure 3: Hypereutectoid Steel (20 μm) Figure 4: Hypereutectoid steel (30 μm)

Figure 5: Hypereutectoid steel (50 μm)

Required Apparatus:
Chemical Apparatus: Machinery Apparatus:
• 5% Nital (5% Nitric acid and 95% Ethanol) • Sectioning Machine
• Acetone • Rough Grinding Machine
• Silica Gel • Emery Paper
• Alumina (Al2O3) • Weight Polishing Machine
• Water (H2O) • Desiccator
• Microscope
Apparatus:

Figure 6: Sectioning Machine Figure 7: Rough Grinding Machine

Figure 8: Emery Paper Figure 9: Polishing Machine

Figure 10: Microscope

Figure11: Desiccator
Discussion:
1. Due to the pandemic situation of COVID-19, we cannot do the experiment practically in
laboratory. So, in this report we study about the microstructure of hypereutectoid or high
carbon steel and the required process by which we can see the structure properly.
2. As we cannot do our experiment in our laboratory, the microstructure of the alloy is taken
for different percentages of carbon percentages. So, there is no relation with one another
microstructure. It just helps us to understand how the microstructure will be seen in
different magnification level.
3. To see the microscope clearly, we should be careful about the surface of the specimen to
make it enough flat, scratches free and smooth. Other inclusions will be seen in the surface
microstructure and the image of the microstructure will be blur.
4. When cutting coated samples, the wheel should pass through the layer(s) first, so that the
base material can act as support and avoid the cracking of the surface.
5. During the sectioning, the direction should be maintained carefully so that there is no
damaged or change on the surface the sample.
6. During the rough grinding process, we should careful about the produced heat and the
applied pressure. Because over heating and pressure can damage the surface or change the
microstructure of the steel.
7. Mounting of specimen is used for the convenience in handling the specimen of difficult
shapes or sizes during the subsequent steps of preparation and examination.
8. At the step of fine grinding, we should be careful for the selection of the emery paper. The
selection of emery papers’ grit is to take in ascending order like as 180, 320, 600, 800,1200
and 1500.
9. If we take the descending order for the selection of emery paper the smooth surface of the
alloy is not achieved because the abrasiveness of higher grit emery paper is low than the
lower grit emery paper.
10. The direction of fine grinding process should be maintained carefully to make the surface
accurately flat.
11. The direction of fine grinding should be changed by 90 degree with the change of emery
paper grit. If we don’t follow the direction there will be the scratches at the surface.
12. Also, in this process we should careful about the produced heat and temperature because
of the damage of microstructure.
13. In weight polishing process, the direction of polishing is an important factor. To make the
surface properly smooth we have to careful about the direction.
14. In this process during the polishing water is used to keep the surface of the specimen cool
so that the heat cannot harm the microstructure.
15. Another reason of using water is to stop spreading alumina (Al2O3) powder; used in weight
polishing.
16. After weight polishing the surface of the specimen have to clean with alcohol or ethanol.
This remove the external particles from the surface.
17. Plastic deformation can result in subsurface defects after grinding, lapping or polishing for
the lacking of carelessness.
18. Residues, fingerprints, and inconspicuous films may interfere with etching, causing various
areas to be attacked at different rates.
19. When we will etch the surface of the specimen, we have to careful about that it should not
take more time, because over time etching can be burnt the microstructure.
20. Sometimes non-metallic inclusion like (oxides, sulphides and silicates) can harm the
microstructure.
21. When the specimen will be taken under the microscope, we should be careful to operate
the microscope properly to see the microstructure clearly.
22. If a blur image appears, by adjusting the coarse and fine adjustment regulator and changing
the mechanical stage horizontally, we have to select the enough flat surface so that the
image of microstructure more will be clearer.
23. By changing the magnification level of eye piece and nose piece we can take more and
more clear microstructure image at different magnification level.
24. Desiccator is used to storage the specimen. In desiccator, there are silica gel which can
absorb moisture and protect them from rust and corrosion.
References:
1. Book of “A Beginners Guide of Metallographic Laboratory Practice”
2. Book of “Fundamentals of Phase Diagram and Transformation”
3. https://www.alacero.org/en/page/el-acero/what-is-steel
4. https://www.google.com/search?q=iron+iron+carbide+phase+diagram&sxsrf=ALeKk
02zzOGH1Mra1Xli9dyTbKp_GDBv7w:1605726910318&source=lnms&tbm=isch&sa=X
&ved=2ahUKEwir4OHw5oztAhXUX3wKHYf6CjMQ_AUoAXoECAQQAw&biw=1536&bi
h=792#imgrc=7XqykQpWn3jLxM&imgdii=37gojr8ELYJksM
5. https://link.springer.com/article/10.1007/BF02700982
6.
7. http://heserver/help/sample_preparation/mounting_specimens.html
8. https://www.sciencedirect.com/topics/materials-science/hypoeutectoid-
steel?fbclid=IwAR0Lmp37jI4zPAWlKje7KY-
ZqRHt4aQWljEn816TUOQf8BNH7PFQRJTqwV8
9. https://www.google.com/search?q=olympic+microscope&tbm=isch&ved=2ahUKEwi
67o_MpZTtAhX-2nMBHVSoAGcQ2-
cCegQIABAA&oq=olympic+microscope&gs_lcp=CgNpbWcQAzIGCAAQChAYMgQIABA
YOgYIABAHEB5QyrgBWIKDAmD9iAJoAHAAeACAAd0CiAG7CZIBBzAuNy4wLjGYAQCgA
QGqAQtnd3Mtd2l6LWltZ8ABAQ&sclient=img&ei=B2C5X_rOBP61z7sP1NCCuAY&bih
=792&biw=1536#imgrc=_ZDfzUg2p0zMJM&imgdii=3ai64gWIJ-JEIM
10. https://www.microscopemaster.com/parts-of-a-compound-microscope.html