LAB MANUAL

ME 2151-1 COOLING RATE EFFECT

SESSION: 2017/2018

Department of Mechanical Engineering

National University of Singapore
 CONTENTS

Page No.

TABLES OF CONTENTS (i)

TERMINOLOGY (ii)

INTRODUCTION 1

THEORY 1

DESCRIPTION OF APPARATUS 7

EXPERIMENTAL PROCEDURE 9

REFERENCES 9

APPENDIX I 10

APPENDIX II 11

APPENDIX III 12
 TERMINOLOGY

The term phase may be defined as a chemically and structurally homogeneous region
of material.

A phase diagram is a graphical representation of the phases present and the ranges in
composition, temperature, and pressure over which the phases are stable.

Phases in the Fe-Fe3C System

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Atomic
Phase packing Description and comments
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Liquid d.r.p Liquid solution of C (carbon) in Fe (iron)

(densely random packing)

(also called delta iron) b.c.c Random interstitial solid solution of C in

(body- centered cubic) b.c.c. Fe.

(also called austenite) f.c.c Random interstitial solid solution of C in

(face- centered cubic) f.c.c. Fe. Maximum solubility is 2 wt%
at 11470C. It is normally not stable at
room temperature.

(also called ferrite) b.c.c Random interstitial solid solution of C in

b.c.c. Fe. Maximum solubility is 0.02
wt% at 7230C. It is the softest structure
appears on the diagram.

Fe3C(also called iron orthorhombic A hard and brittle interstitial compound

carbide or cementite) of Fe and C containing 25 atomic % (6.7
wt%) C.

( + Fe3C) Pearlite -It is very fine platelike or lamellar

eutectoid mixture of ferrite and
cementite containing 0.8 wt% C and
formed at 7230C on very slow cooling
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Martensite- It is a supersaturated solid solution of carbon in b.c.t (body-centered
tetragonal) iron. This meta-stable phase is formed under very rapid cooling.
 INTRODUCTION

The purpose of this manual is to provide instructions to enable student to investigate

the effects of cooling rate and carbon content on the microstructure and hardness of
commercial steel.

This manual contains some fundamental theory for understanding the experiment and
description of the apparatus for hardness measurement.

THEORY

Pure iron is undergone polymorphic changes depending upon temperature, as

indicated in Fig.1. When liquid iron first solidifies at 15390C, it is in form. Upon
further cooling at 14000C, a phase change occurs and the atoms rearrange themselves
into the form, which is nonmagnetic. When the temperature reaches 9100C, another
phase change occurs from to iron (magnetic). Alloys of iron and carbon (with
other elements intentionally added for special purposes) comprise the commercially
important ferrous-base alloys known as steels and cast irons. These alloys,
particularly the steels, are susceptible to heat-treatment, and a wide range of
properties can be obtained by proper variation and timing of heating and cooling
cycles.

Fig.1 Temperature ranges in which allotropic forms of iron exist under equilibrium
conditions.

Carbon atoms are small compared to iron atoms, and have a radius ratio (carbon to
iron) of 0.63. Consequently, any solute carbon forms an interstitial solution. Since the
biggest interstices in gamma (f.c.c) iron are larger (0.52 A radius) than the largest in
alpha (b.c.c) iron (0.36 A radius). We expect greater solubility of carbon in than in
. This does occur as indicated in Fig. 2, the so-called Iron-Carbon Equilibrium Phase

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Diagram which indicates that can dissolve a maximum of 2.0 wt% carbon at
11470C, while can dissolve a maximum of only 0.02 wt% carbon at 7230C.

Fig.2 The Fe-Fe3C meta-stable portion of iron-carbon equilibrium phase

diagram.

Plain carbon steels are generally considered to contain up to 2 wt% carbon whereas
cast irons range from 2 to 5 wt% carbon.

Consider in detail three alloy steels containing of 0.4% carbon, 0.8% carbon, and
1.2% carbon cooled from slightly above the upper critical temperature.

At the temperature of starting cooling all three alloys are in the form of austenite. The
lowest temperature for an alloy of iron and carbon to exist in the form of 100%
austenite or gamma iron is 7230C and the alloy composition is austenite containing
0.8% carbon.

At 7230C the austenite changes to a structure known as pearlite. The structure of

pearlite consists of alternate layers of ferrite and cementite. When a steel is cooled
below 7230C there is a driving force for the eutectoid reaction of:

(f.c.c iron + 0.8 wt% dissolved carbon) (b.c.c iron + 0.02 wt% dissolved
carbon) + Fe3C (6.67 wt% carbon).

Transformation of austenite to pearlite starts by formation of cementite nuclei at

austenite grain boundaries (see Fig.3). Carbon diffuses from the surrounding austenite
to the cementite, and the growth of carbide begins. As carbon diffuses, the adjacent
austenite is depleted in carbon and transforms to ferrite. With formation of ferrite,
there is rejection of carbon from the ferrite region, i.e., effective enrichment of the
adjacent austenite. This results in the formation of additional nuclei of cementite.
Because of the alternate formation of cementite and ferrite, cementite can only grow
away from the boundary of the original austenite grain as a platelet.

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Fig. 3 Schematic representation of pearlite formation by nucleation and growth; (a)
through (d) indicate successive steps in time sequence.

Nucleation and growth of alternate plates of cementite and ferrite occur at several
points along the austenite grain boundaries. This forms pearlite colonies, which are
approximately hemispherical regions of alternate parallel plates of cementite and
ferrite. These pearlite colonies grow until the entire austenite grain has been
consumed and has become a pearlite structure. The process of pearlite formation is
sometimes referred to as sidewise nucleation and edgewise growth.

All alloys cooling from the austenite range down to room temperature are compelled
to produce some pearlite as part of their final structure. Alloy 1 is a hypoeutectoid
steel containing 0.4% carbon i.e. the initial carbon content of the alloy is below the
0.8% carbon value. The starts to transform as soon as the alloy enters the austenite,
+ ferrite, field (Fig.4). "Primary" nucleates at grains boundaries and grows as the
steel is cooled from A3 to A1. At A1 the remaining (which is now of eutectoid
composition) transforms to pearlite as usual. The room temperature microstructure is
then made up of primary + pearlite.

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Fig. 4 The sequences of change of phases of the three alloys cooling from the
austenite region to room temperature.

Alloy 2 is a eutectoid steel containing of 0.8% C. Hence no transformation takes place

until the steel is cooled to eutectoid temperature (7230C), where though eutectoid
reaction austenite to pearlitic transformation takes place. Hence at room temperature
we get 100% pearlite in the microstructure (see Fig.4).

Alloy 3 is a hypereutectoid steel containing 1.2% carbon i.e. in excess of 0.8% carbon
and therefore during cooling from the austenite range this extra carbon must be
removed from the austenite. The excess carbon is precipitated out of solid solution but
during the process it brings with it ferrite atoms and the final precipitate is not pure

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carbon but is cementite. As cooling and cementite precipitation continue the
remaining austenite becomes gradually lower in carbon content until only 0.83%
carbon content. Then it changes to pearlite the reaction temperature being 7230C.
Finally we get a room-temperature microstructure of primary Fe3C plus pearlite
(Fig.4).

Under slow or moderate cooling rates, the carbon atoms are able to diffuse out of the
austenite structure resulting proeutectoid ferrite, proeutectoid cementite, and/or
pearlite, This transformation takes place by a process of nucleation and growth and is
time dependent. With a very rapid cooling rate, insufficient time is allowed for the
carbon atoms to diffuse out of solution, and although some movement of the iron
atoms takes place, the structure cannot become b.c.c while the carbon is trapped in
solution thus transform austenite into a metastable phase known as martensite which
is a single-phase, supersaturated solution of carbon in ferrite with carbon atoms
located interstitially in a body-centered tetragonal lattice; i.e., the excessive
supersaturation distorts the normal b.c.c structure to body-centered tetragonal. The
lattice distortion is reflected in mechanical properties of high strength and hardness
and low ductility. Figure 5 shows that the hardness of martensite increases rapidly
with carbon content.

Fig. 5 The hardness of martensite increases with carbon content because of the
increasing distortion of the lattice.

The cooling rate for martensite formation must exceed a critical value, which depends
on composition and metallurgical history. Martensite will not form unless austenite is
cooled below a certain critical temperature (Ms), which depends on composition.
Formation continues only if temperature continues to decrease. There is a lower
temperature (Mf) at which transformation to martensite is complete. Martensite
formation is essentially independent of time.

On the TTT (time temperature transformation), also called CCT (continuous cooling
transformation) diagram (see Fig.6) curves X, Y and Z, representing different
continuous cooling rates that are superimposed.

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Fig. 6 The relationship between true TTT curves and those representing continuous
cooling conditions.

Curve X represents a rate of cooling such as might prevail during a normalising (air
cooling) process. Transformation of the unstable austenite begins at K and is complete
at N and product is fine pearlite. A very rapid cooling is represented by curve Y which
just touches the modified transformation-begins curve so unstable austenite persists
until at O (on the Ms line) transformation direct to martensite begins. It should be
noted that the above discussion is mainly for 0.8% C steel. If the carbon content is
either above or below this amount the curves are displaced to the left so that the CCR
(critical cooling rate) required to produce a fully martensite structure will be even
greater.

Ms denotes the start and Mf the finish. It should be noted that if steels contain more
than 0.7% C the Mf temperature lies below 00C so that there is some retained austenite
unless sub-zero treatment is performed.

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 Description of Equipment

Rockwell hardness test:

Hardness may be defined as the resistance of the material to penetration/indentation.

The Rockwell hardness test is based on the measurement of the depth of penetration
of the indenter into the specimen. The salient features of a typical Rockwell Hardness
Testing Machine are shown in Fig. 7.

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Major load is supplied by a dead weight loading lever (L) having a ratio of 25 to 1.
Rockwell number is read from the dial gauge (D), connected to the plunger system in
the head of the tester by means of the Index Lever (M) having 5: 1 ratio.

The dial gauge is a 1 mm gauge, i.e. one revolution of the pointer equals 1 mm travel
of the dial rack. There are 100 divisions to a revolution and as the lever ratio is 5:1,
each division on the dial represents a depth of 0.002 mm. When minor load is applied
there is a fixed zero or set point. Two scales are provided on the dial gauge. The outer
circle is in black, and all readings with diamond indenter are taken on this. The inner
circle is in red, and all readings with ball indenters are taken from this. The set point
is always same regardless of the scale. Fig. 8 shows steel ball and diamond cone
indenter.

The general principals of the Rockwell hardness test are illustrated in Fig. 9 (ball
indenter) and Fig. 10 (diamond indenter) and the accompanying Tables 1 and 2 (in
appendix I).

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 Experimental Procedure

You will be provided four medium carbon steel specimens having composition of
0.45 % carbon with different cooling rates (furnace cooled, air cooled, fan cooled and
water quenched).

1. Observe the microstructures under the optical microscope, as high magnification

as possible.
2. Sketch neatly the different phases and structures of each specimen.
3. Determine the hardness of each sample using Rockwell Hardness Tester
(procedure and precautions are given in appendix II).
4. Convert all the harness values to Vickers' hardness (HV) through the conversion
table given in appendix III.
5. Analyse the results and establish the relationships amongst cooling rate,
microstructure and hardness of specimens.

References
1. R. A. Higgins, "The Properties of Engineering Materials".
2. M. F. Ashby & D. R. H. Jones, "An Introduction to Microstructures, Processing
and Design".
3. S. H. Avner, "Introduction to Physical Metallurgy".
4. C .O. Smith, "The Science of Engineering Material

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 Appendix I

Table 1 Symbols and Designation Associated with Fig. 9.

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Number Symbol Designation

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1 --- Diameter of ball = 1/16 in. (1.588 mm)

3 P0 Preliminary test force = 10 kgf
4 P1 Additional force = 90 kgf
5 P Total test force = P0 + P1 = 10 + 90 = 100 kgf
6 --- Depth of penetration under test force before
application of additional load
7 --- Increase in depth of penetration under additional
load
8 e Permanent increase in depth of penetration under
preliminary test force after removal of additional
force, the increase being expressed in units of
0.002 mm.
9 xx HRB Rockwell B hardness = 100-e
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Table 2 Symbols and Designation Associated with Fig. 10.

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Number Symbol Designation

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1 --- Angle at the top of the diamond indenter (120)

2 --- Radius of curvature at the tip of the cone (0.200
mm)
3 P0 Preliminary test force = 10 kgf
4 P1 Additional force = 90 or 140 kgf
5 P Total test force = P0 + P1 = 10 + 140 = 150 kgf
6 --- Depth of penetration under test force before
application of additional load
7 --- Increase in depth of penetration under additional
load
8 e Permanent increase in depth of penetration under
preliminary test force after removal of additional
force, the increase being expressed in units of
0.002 mm.
9 xx HRC Rockwell C hardness = 100-e
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 Appendix II
Measurement of Harness

1. Place the specimen on the plane anvil.

2. Raise the anvil by rotating the capstan slowly until the tip of the indenter touches the specimen.
3. Further elevate the anvil gently until the small pointer in the dial gauge points to the red dot i.e. set
position.
4. Turn the outer ring of the indicator gauge until the large pointer reads 0 on the appropriate scale.
5. Push the crank handle to apply the major load.
6. The load is to be maintained for about 10 seconds before pushing crank handle in the reverse
direction to remove the major load.
7. Read the hardness number while the minor load is still being applied.
8. Turn the capstan in the reverse direction to lower the anvil and remove the specimen.
9. The next test is carried out now as before.

Precautions
1. Ensure that both surfaces of the specimens are flat and positioned securely on the anvil.
2. Rotate the capstan gently during elevation of the anvil. Otherwise due to abrupt strike of the
indenter tip with the sample, the indenter may be destroyed.

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 Appendix III

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