Effect of Microstructure on Sliding Wear Behaviour

of Modified 9Cr-1Mo steel

A thesis submitted in partial fulfillment of the requirement for the degree

of

Master of Technology
in
Metallurgical and Materials Engineering

Submitted by
Ipsa Tripathy
Roll No. 209MM1244

Department of Metallurgical and Materials Engineering

National Institute of Technology,
Rourkela-769008
2011
 Effect of Microstructure on Sliding Wear Behaviour
of Modified 9Cr-1Mo steel

A thesis submitted in partial fulfillment of the requirement for the award of degree
of

Master of Technology
in
Metallurgical and Materials Engineering

Submitted by
Ipsa Tripathy
Roll No. 209MM1244

Under the Supervision Of

Dr. B.B.Verma Dr. B.B. Jha, Scientist G

Dept. of Metallurgical & Materials Engg. IMMT, Bhubaneswar
National Institute of Technology
Rourkela
 National Institute of Technology, Rourkela

Certificate

This is to certify that the thesis entitled Effect of microstructure on sliding wear behaviour of
modified 9Cr-1Mo steel submitted by Miss. Ipsa Tripathy in partial fulfillment of the
requirements for the award of the degree of Master of Technology in Metallurgical and Materials
Engineering at National Institute of Technology, Rourkela is an authentic work carried out by
her under our supervision and guidance.

To the best of our knowledge, the matter embodied in the thesis has not been submitted to any
other university/institute for the award of any degree or diploma.

Date:
Place: Rourkela

Dr. B.B.Verma Dr. B.B. Jha, Scientist G

Dept. of Metallurgical & Materials Engg. Surface Engg. Dept
National Institute of Technology IMMT Bhubaneswar
Rourkela
 Acknowledgement

All praises to Almighty GOD, the most merciful and compassionate who enabled me to complete
my journey till here colorfully.
I would like to express my gratitude to all those who helped me during my thesis work.
First and foremost, I wish to thank my supervisor Dr. B.B.Verma, Prof. and Head Metallurgical
and Materials Engineering Department, NIT Rourkela and my co-supervisor Dr. B.B.Jha,
Scientist-G, IMMT Bhubaneswar with generosity those who have provided me an opportunity to
work in such a novel and exciting research area under their great supervision.
I am sincerely thankful to Dr.P.K.Ray, Prof. Mechanical Engineering Department, NIT Rourkela
for his valuable and kind suggestions.
I am extremely grateful to Mr. T.K.Sahoo, Technical Officer, IMMT Bhubaneswar for his
persistent support and advice during the project work.
My sincere regards to Prof. K. Dutta, Metallurgical and Materials Engineering Department, for
his co-operation during the period of work.
I wish to extend my warmest thanks to laboratory members of Department of Metallurgical and
Materials Engineering, NIT Rourkela, especially Mr. S. Hembram, Mr. R. Pattanaik, and Mr. U.
K. Sahu for their help during the execution of experiment.
I am also thankful to Mr. S.Behera, Laboratory member, IMMT Bhubaneswar for his help during
project work.
Special thanks to my family members, without their blessings and support, I could not have
reached this destination.
Last but not the least, I wish to place my deep sense of thanks to my friends especially to Ms.
Preeti Verma and Mrs. Manila Mallik for their cooperation and critical suggestion during my
project work and studies.

Place: Rourkela Ipsa Tripathy

 Contents

Chapters Page No.

Abstract i
List of Figures iii
List of Tables vi
1 Introduction 1-5
1.1 Background of modified 9Cr-1Mo ferritic steel 2
1.2 Objective of the present project work 4
2 Literature Review 6 27
2.1 Steel 7
2.2 Alloy steels 8
2.3 Heat Treatment of Steels 9

2.3.1 Stages of Heat Treatment 9

2.3.2 Types of Heat Treatment 10
2.3.2.1 Annealing 10
2.3.2.2 Normalizing 10
2.3.2.3 Stress relieving 11
2.3.2.4 Aging 11
2.3.2.5 Quenching 11
2.3.2.6 Tempering 12
2.3.3 Effects of time and temperature 13
2.3.4 T-T-T Diagram of Cr-Mo steel 14
2.4 Wear 15
2.4.1 Factors affecting the wear performance of materials 15
2.4.3 Wear mechanisms 16
2.4.3.1 Adhesive wear 16
2.4.3.2 Abrasive wear 17
2.4.3.3 Fretting wear 18
2.4.3.4 Surface fatigue 19
2.3.4.5 Corrosive wear 19
2.3.4.6 Erosion wear 20
 3 Experimental 28 37
3.1 Materials 28
3.2 Experimental Procedures 28
3.2.1 Tensile Test 28
3.2.2 Heat Treatment of samples 29
3.2.3 Material Characterization 29
3.2.3.1 Optical Microscopy 31
3.2.3.2 Scanning Electron Microscopy 32
3.2.4 Vickers hardness Test 33

3.2.5 Sliding Wear Test 33

4 Results and Discussions 38 55
4.1 Tensile test Results 38
4.2 Microstructural Characterization 38
4.2.1 Optical Microscopy 38
4.2.2 Phase Analysis 40
4.2.3 Scanning Electron Microscopy with EDS analysis 41
4.3 Hardness determination 43
4.4 Wear Test Results 44
4.5 Worn surfaces analysis by SEM 50
5 Conclusions & Future work 56 57
5.1 Conclusions 57
5.2 Scope for future work 57
6 References 58 61
 Abstract

Modified 9Cr1Mo ferritic steel finds wide application in petroleum industries, chemical
processing and thermal power plants because of its excellent mechanical properties and corrosion
resistance. This material has become a favoured tubing material in the reheater and super heater
portions of fast reaction steam generators. Excellent mechanical properties, oxidation and
corrosion resistance combined with low creep rate and low thermal expansion makes it a
wonderful material for high temperature applications. The present investigation aims to study the
effect of microstructural variations in wear performance of modified 9Cr-1Mo steel using dry
sliding wear test. Total twelve samples of the material were subjected to three different heat
treatments i.e. annealing, normalizing and water quenching (to develop lower bainite) heated to a
temperature of 1050C. One from each heat treated types was prepared for microstructural and
hardness studies. Optical and Scanning electron microscopy along with Energy Dispersive
Spectrum (EDS) analysis have been used to characterize the microstructures. The shape and
percentage of phases present in the microstructure were obtained from optical microscope with
image analyzer which plays a vital role in determining the wear behaviour of the material. The
hardness of the three different heat treated samples was measured by Vickers hardness testing
machine. Wear behaviour of this steel was investigated on a disc-on-roller multiple wear tester of
model TR-25 under dry sliding condition, rubbing against EN-31 steel. Three samples of the
each heat treated types were subjected to three different load variations of 30N, 50N and 100N at
a constant sliding speed of 250 RPM and the results obtained were compared. The comparison
among three heat treated types has been done for a constant load of 100N. SEM micrographs of
worn surfaces have been used to correlate the results obtained.

Following are the conclusions based on the present investigations:

The results obtained for the annealed samples exposed to three different load variations
of 30N, 50N and 100N shows that with increase in load, the wear rate increases as there
is increase in friction at the contact surface.
For normalized and water quenched samples exposed to 100N load, deviation occurs due
to formation of oxide scales on the material surface leading to oxidative wear pattern.
The formation of oxide scale is due to the generation of high temperature when high load

i
 is applied on the material. These oxide scales protects the material surface inhibiting the
further wear of the material.
A comparison graph which has been drawn to show the variations in wear of three heat
treated types at a constant load of 100N gives information that the water quenched
sample experiences less wear in comparison to normalized and annealed ones. This is due
to the formation of fully bainitic structure in case of quenched sample which results in
higher hardness of the material and least wear among the three.
The wear rate with respect to time or sliding distance for all the three types of samples in
different loading conditions follows the decreasing trend.

Keywords: 9Cr-1Mo steel, microstructural change, sliding wear, oxide scales, wear rate

ii
 List of Figures

Chapter 1
1.1 Flow sheet of plan of work
Chapter 2
2.1 Types of heat treatment in steels
2.2 Time-temperature transformation (TTT) diagram for steel
2.3 T-T-T diagram of 2.25Cr-1Mo steel
2.4 Adhesive wear mechanism
2.5 Two and three body abrasive wears mechanism
2.6 Five processes of abrasive wear (a) Plowing (b) Wedge (c) Cutting (d) Micro fatigue
(e) Micro cracking
2.7 Fretting wear
2.8 Surface Fatigue
2.9 Corrosive wear
2.10 Erosion wear
2.11 Variation of wear rate with martensite volume fraction in DP Steels
2.12 Wear on the flank face for workpiece hardness of HRc 50 under V = 82 m/min
2.13 Wear rates of studied sintered steels at 1180 C using both cooling rates
2.14 The typical delamination wear of studied sintered steels with fine grooves parallel to
the sliding direction and flake-like fragments (a) and with mild oxidation wear (b)
2.15 Shows Variations of Wear Rate of Spring Steel with Sliding Distance.
2.16 Variations of Wear Rate of Spring Steel with Load
2.17 Variations of Wear Rate of Spring Steel with Speed
2.18 Variation of wear rate with sliding distance for samples with and without boron
addition
2.19 SEM of worn surface of 316L stainless steel: (a) without and (b) with boron addition
at 10.8 N, 0.21 m s-1 speed and sliding distance 6000 m
Chapter 3
3.1 Instron 8801 servo hydraulic testing machine
3.2 Carbolite Furnace
3.3 Rotating disc for polishing

iii
 3.4 Image Analyzer LEICA DMI3000 M
3.5 Scanning Electron Microscope JEOL JSM-6510
3.6 Vickers hardness testing machine
3.7 Multiple Tribo Tester TR-25
3.8 Display of results by WINDUCOM 2008 software
3.9 Sample for wear test having dimension 6.35 x 6.35 x 9 mm
3.10 Disc-on-roller arrangements
Chapter 4
4.1 (a) Optical microstructure of Annealed sample (b) Optical microstructure of
Normalized sample (c) Optical microstructure of Water Quenched sample
4.2 Phase analysis of heat treated samples
4.3 (a) Scanning electron micrograph of annealed sample (left), (b) EDS analysis of
annealed sample (right).
4.4 (a) Scanning electron micrograph of annealed sample (left), (b) EDS analysis of
annealed sample (right).
4.5 (a) Scanning electron micrograph of water quenched sample (left), (b) EDS analysis
of water quenched sample (right).
4.6 Comparison graph of hardness values of different heat treated samples by Vickers
hardness test.
4.7 (a) Wear versus time graph of annealed sample subjected to load variations of 30N,
50N and 100N (left), (b) Wear versus sliding distance graph of annealed sample
subjected to load variations of 30N, 50N and 100N (right).
4.8 (a) Wear rate versus time graph of annealed sample subjected to load variations of
30N, 50N and 100N (left), (b) Wear rate versus sliding distance graph of annealed
sample subjected to load variations of 30N, 50N and 100N (right).
4.9 Wear versus time graph of normalized sample subjected to load variations of 30N,
50N and 100N.
4.10 Wear rate versus time graph of normalized sample subjected to load variations of
30N, 50N and 100N.
4.11 Wear versus time graph of water quenched sample subjected to load variations of
30N, 50N and 100N.

iv
4.12 Wear rate versus time graph of water quenched sample subjected to load variations
of 30N, 50N and 100N.
4.13 Wear versus time graph of different heat treated samples at a constant load of 100N.
4.14 Wear rate versus time graph of different heat treated samples at a constant load of
100N.
4.15 Worn out surface of annealed sample subjected to 30N load (a) at 50X, (b) at 400X.
4.16 Worn out surface of annealed sample subjected to 50N load (a) at 50X, (b) at 400X.
4.17 Worn out surface of annealed sample subjected to 100N load (a) at 50X (left), (b) at
400X (right).
4,18 Worn out surface of normalized sample subjected to 30N load (a) at 50X (left), (b)
at 300X (right).
4.19 Worn out surface of normalized sample subjected to 50N load (a) at 50X (left), (b)
at 300X (right).
4.20 Worn out surface of normalized sample subjected to 100N load (a) at 50X (left), (b)
at 200X (right).
4.21 EDS Analysis of normalized sample subjected to 100N load
4.22 Worn out surface of quenched sample subjected to (a) 30N load (left), (b) 50N load
(right).
4.23 Worn out surface of quenched sample subjected to 100N load

v
 List of Tables

Chapter 1
1.1 Typical properties of carbon and alloy steels at room temperature.
Chapter 3
3.1 Chemical composition of 9Cr-1Mo steel
Chapter 4
4.1 Tensile test results

vi
 Chapter 1
Introduction

1
 1. Introduction
1.1 Background of modified 9Cr-1Mo ferritic steel
Steels represent the most important group of engineering materials as they have the widest
diversity of applications of any of the engineering materials. Generally, carbon is the most
important element profoundly affecting the mechanical properties of the steels. Increasing the
carbon content of steels increases the hardness and strength. More-over, plain carbon steels have
moderate strengths and can resist satisfactorily ordinary temperatures and atmospheres and also
are available in large quantities, in quite large variations of shapes and sizes with a much lower
cost. For enhancing further the prominent characteristics of the plain carbon steels or to ensure
some specific properties, one or more elements are intentionally added to steel. The added
elements are known as alloying elements and the steel is known as alloy steels. The addition of
alloying elements not only improve the hardenability, improve corrosion and oxidation
resistance, increase resistance to softening on tempering, increase high temperature properties,
but also increase resistance to abrasion. They increase strength of the parts that cannot be
quenched due to physical limitation of parts or the structure in which it is employed [1]. The
following table 1.1 lists the typical properties of steels at room temperature (25C) showing the
superior properties of alloy steels over plain carbon steels.
Properties Carbon Steels Alloy Steels
Density (1000 kg/m3) 7.85 7.85
Elastic Modulus (GPa) 190-210 190-210
Poisson's Ratio 0.27-0.3 0.27-0.3
Thermal Expansion (10-6/K) 11-16.6 9.0-15
Thermal Conductivity (W/m-K) 24.3-65.2 26-48.6
Specific Heat (J/kg-K) 450-2081 452-1499
Electrical Resistivity (10-9-m) 130-1250 210-1251
Tensile Strength (MPa) 276-1882 758-1882
Yield Strength (MPa) 186-758 366-1793
Percent Elongation (%) 10-32 4-31
Hardness (Brinell 3000kg) 86-388 149-627

Table 1.1 Typical properties of carbon and alloy steels at room temperature.

2
To withstand against high temperature and pressure, alloy steels are made with several
modifications to meet the requirements. 9Cr-1Mo steel with small amounts of vanadium addition
for grain refinement makes it modified 9Cr-1Mo ferritic steel. 9Cr1Mo ferritic steel (ASME
T91) finds wide application in petroleum industries, chemical processing and thermal power
plants because of its excellent mechanical properties and corrosion resistance [2, 3-7]. This
material is widely used as a thick steam pipe component in thermal power plants and this
possesses superior mechanical and oxidation resistance under an operating temperature of 550C
[8]. This material has become a favoured tubing material in the reheater and super heater
portions of fast reaction steam generators in the normalized and tempered conditions. It has low
thermal expansion at service temperatures and has a high resistance to stress corrosion cracking
in water steam systems. This material is the best considerated construction material for sodium to
air decay heat exchangers to be used during the emergency shutdowns. High thermal
conductivity and low thermal expansion coefficient coupled with enhanced resistance to stress
corrosion cracking in steam-water systems have widen the application of this steel for steam
generator applications [9]. The material conjointly possesses better monotonic tensile and creep
strengths at elevated temperatures compared with the plain 9Cr-1Mo steel. Excellent weldability
and microstructural stability while having long periods of exposure to very high temperature
performance make this alloy a different from others [10-13]. Material of this composition is also
being considered for fast reactor structural components such as wrappers due to its low swelling
rate, low irradiation, creep rate and resistance to high temperature embrittlement [14]. Looking to
its wide variety of applications, the properties for example, creep behavior, welding
characteristics and micrographic heterogeneities, high temperature oxidation, corrosion behavior,
electrochemical / potentiodynamics studies, fatigue behavior, grain morphology were widely
investigated [2, 14-26]. Though numbers of alloying elements have been added in modified 9Cr-
1Mo steel to stabilize the microstructure for high temperature application, the alteration in
microstructure occurs due to time dependent deformation mechanisms. However, the effect of
microstructural variations upon the wear properties of 2.25Cr-1Mo steel has been studied using a
dry sliding wear test [27]. Actually wear refers to the progressive removal of material from a
surface and plastic deformation of material on a surface due to the mechanical action of the other
surface [28]. The necessity for relative motion between the operating surfaces and initial
mechanical contact between asperities leads an important role between mechanical wear

3
compared to other processes with similar outcomes [29]. The sliding wear behavior of various
steels is a vast subject which has received much attention in recent years. Tribological behavior
of metals which are in sliding contact depends on the many variables such as normal Load
applied on the material, sliding speed, sliding distance, surface geometry, surface hardness,
roughness of operating surface, working environment, etc., which affect the wear mechanism and
results in change of wear rate [30]. Modified 9Cr-1Mo steel (P91) is widely used as the tubing
material for reheater and super heater tubes in thermal power plants experiences erosion and little
sliding wear. This material is used in steam generators of fast breeder reactors encountering
contact with NiAl based alloy coating undergoes flow-induced vibration, results material damage
due to deformation. The contacting materials experience micro scale sliding between each other
which can also tend towards fatigue-induced wear [31]. Hence the study of sliding wear is one of
the essential criteria to determine the life of component which are made of this 9Cr-1Mo steel
material. These are mostly used in normalized and annealed conditions in power plants.
Although these possess many attractive properties, they are having certain drawbacks and
undergo degradation in properties as a result of long term exposure to aggressive environment at
a higher temperature. Therefore, it is interesting to examine the effect of these microstructural
variations on wear behaviour of this steel. As its sliding wear behaviour in different heat treated
condition is not known, hence we are interested to work on this area.

1.2 Objective of the present project work

In the present investigation, the effect of microstructure on the wear behaviour of Modified 9Cr-
1Mo ferritic steel is our main area of interest.

1. Determination of yield strength and tensile strength of the material by tensile testing.
2. Heat treatment of 12 samples having dimensions 7.5 x 7.5 x 10 mm subjected to three
types of heat treatments i.e. annealed, normalized and water quenched types.
3. Material characterization by Optical microscopy, Scanning Electron Microscopy (SEM)
with EDS analysis and phase analysis of one of the samples from each heat treated types.
4. Determination of hardness of one of the samples from each heat treated types by Vickers
hardness test.
5. Study of sliding wear behaviour of three of the samples from each heat treated types at
varying loads at constant speed having dimensions 6.35 x 6.35 x 9 mm by wear test.

4
6. Analysis of their worn surfaces by SEM.

9Cr-1Mo steel (12 samples)

Heat treatment (12 samples)

Annealed (4 samples)

Normalized (4 samples)

Quenched (4 samples)

Annealed (3 nos.), Normalized (3 nos.) Annealed (1 no.), Normalized (1 no.)

and Quenched (3 nos.) and Quenched (1 no.)

Wear test and Worn surface analysis Material Characterization and

Hardness Test

Figure 1.1 Flow sheet of plan of work

5
 Chapter 2
Literature Review

6
2 Literature Review
2.1 Steel
The term steel generally refers to different alloys of iron. These alloys vary by means of ways
they are formed and also by the proportions of the materials added to the iron. All steels,
however, contain little amounts of carbon and manganese. In alternative terms, it is said that steel
is nothing but a crystalline alloy of iron, carbon and several other components that hardens
higher than its critical temperature. Steels represent the most important group of engineering
materials as they have the widest diversity of applications of any of the engineering materials [1].
Increasing carbon content increases hardness and strength and improves hardenability. But
carbon also increases brittleness and reduces weldability because of its tendency to form
martensite. This means carbon content can be both a blessing and a curse when application of
commercial steel is taken into account. Most commercial steels are classified into two groups:

Plain carbon steels

Alloy steels
Limitations of plain carbon steel [1]

Like everything, the plain carbon steels do have some appreciable properties however they have
some drawbacks. These are:

i. There can't be strengthening beyond one hundred thousand psi without having any
significant loss in toughness as well as ductility.
ii. Large sectional areas can't be formed with a martensite structure throughout, and
therefore don't found to be deep hardenable.
iii. Rapid rate of quenching are necessary for full hardening in medium-carbon results in
distortion of shape and cracking of heat-treated steels.
iv. At low temperatures plain-carbon steels have poor impact resistance.
v. Plain-carbon steels have poor corrosion resistance from point of engineering issues.
vi. Plain-carbon steel has high oxidizing tendency at elevated temperatures.

The limitations of carbon steels are overcome by the successful use of alloy steels. The presence
of alloying elements, not only accelerates the outstanding properties of plain carbon steels, but
improves some other characteristics, or even induces specific properties.

7
General effects of alloying components are:

i. Improve tensile strength without any appreciable reduction in ductility.

ii. Improve toughness of material.
iii. Improve hardenability that allows hardening of larger sections than attainable with
plain carbon steels or allows quenching with less drastic rates.
iv. Reduce the hazard due to distortion and quench cracking.
v. Retain high temperature strength.
vi. Obtain superior corrosion resistance.
vii. Improve wear resistance.
viii. Impart a fine grain structure to the steel.
ix. Improve special properties like abrasion resistance and fatigue resistance.

2.2 Alloy steels

Based on the features of alloying elements, alloy steels can be classified as follows [32]:

Classification on the basis of the amount of alloying element:

a) Low alloy steel (Total alloying element is less than 10 percent)
b) High alloy steels (Total alloying content is above 10 percent)
Classification on the basis of composition:
Depending on the alloying elements, alloy steels are classified into nickel steels,
chromium steels, Cr-Ni steel and Cr-Ni-Mo steels. They are classified according to the
presence of various alloying elements.
Classification on the basis of structure:
Various structures such as ferrite, martensite, austenite or bainite constitute steels.
Accordingly they are called ferritic steel, martensitic steel, and so on.
Classification on the basis of application:
Corrosion resistant steel, heat resistant steel, magnetic steel, tool steel, electrical
steel, etc.

Chromium-molybdenum heat-resistant steels contain 0.5 to 9% Cr and 0.5 to 1.0% Mo. The
carbon content is usually below 0.2%. The chromium provides improved oxidation and corrosion
resistance, and the molybdenum increases the creep resistance at elevated temperatures. They are

8
generally supplied in form of the normalized and tempered, quenched and tempered or annealed
types. Chromium-molybdenum steels are widely used in the thermal power plants and nuclear
power plants. 9Cr-1Mo ferritic steel is a low alloy steel commercially included in this category.

2.3 Heat Treatment of Steels

Heat treatment is the method of heating and cooling of metals to attain the desired physical and
mechanical properties through modification of their crystalline structure. The temperature, time
duration, and cooling rate after heat treatment will have their dramatical impact on properties.
The most important and also common reason to heat treat includes increasing strength or
hardness, increasing toughness, improving ductility and maximizing corrosion resistance [1, 32].

2.3.1 Stages of Heat Treatment

Heat treating is accomplished in three major stages [1, 32]:
Stage l Heating the metal to a specified temperature.
Stage 2Soaking (holding) the metal at that temperature for a specific period of time
Stage 3 Cooling that material to again room temperature.

Stage l - The primary objective in the heating stage is to maintain uniform temperatures. If
uneven heating occurs, one section of a part can expand faster than another and result in
distortion or cracking. Uniform temperatures are attained by slow heating.
Stage 2 - After the metal is heated to the proper temperature, it is held at that temperature until
the desired internal structural changes take place. This process is called soaking. The length of
time held at the proper temperature is called the soaking period. This is used for metals that
require a rapid cooling rate, and soaking period depends on the chemical analysis of the metal
and the mass of the part. When steel parts are uneven in cross section, the soaking period is
determined by the largest section.
Stage 3 - After a metal has been soaked, it must be returned to room temperature to complete the
heat treating process. To cool the metal, the material can be directly in contact with a cooling
medium composed of a gas, liquid, solid, or in combination of any of these. The rate at which the
metal is cooled depends on the metal and the properties desired. The rate of cooling depends on
the medium; therefore, the choice of a cooling medium has an important influence on the
properties desired.

9
2.3.2 Types of Heat Treatment

Figure 2.1. Types of heat treatment in steels

2.3.2.1 Annealing
Annealing is a process in which the metal is heated to a specific temp & cooled at a defined rate
to produce refined microstructure. It helps the metal to be used for cold working by making it
softer, enhances machinability, or to improve electrical properties. In ferrous alloys, annealing is
done by heating it above upper critical temperature and then slowing cooling it to the room
temperature, so that pearlite forms as the resulting microstructure. This process is used to remove
hardness which arises due to cold working, in cases like pure metals and other alloys that cannot
be heat treated. Here the defects caused by plastic deformation are repaired by heating the metal
above the re-crystallization temperature. Here the rate of cooling has a little effect to the final
properties.
Ferrous alloys are annealed by 2 types-
Full annealed: - Very slow cooling rates resulting in coarse pearlite.
Process annealed: - The cooling rate may be faster, resulting in a uniform microstructure
[33].
2.3.2.2 Normalizing
Main purpose is to impart uniformity in grain size as well as composition throughout an alloy.

10
Generally in this process, ferrous alloy is heated above the upper critical temperature followed
by cooling in open air [33].
2.3.2.3 Stress relieving
It is done to remove the internal stresses in a metal that may have aroused from cold working
and/or non uniform cooling. Generally in this process, Metal is heated below the lower critical
temperature followed by uniform cooling. [33]
2.3.2.4 Aging
By quenching some metals that are known as precipitation hardening metals, the alloying
elements present in it are trapped in solution which results in a softer metal. Aging helps a
"solutionized" metal to increase its strength, by allowing the alloying elements to form
intermetallic particles by diffusing through the microstructure. These intermetallic particles act
as a reinforcing phase by nucleating and falling out of solution.
Alloys may age in 2 types
Naturally: - Precipitates form at room temperatures.
Artificially: - Precipitates form at elevated temperatures.
In some applications, naturally aging alloys are stored in a freezer to prevent hardening until
further operations like assembly of rivets.
Examples of precipitation hardening alloys include some stainless steels. Steels that are harden
by aging are termed as a combination of "martensite aging"[33] and generally referred to as
maraging steels.
2.3.2.5 Quenching
In this process the metal is cooled in a rapid rate resulting in martensite transformation.
Resulting in-
Harder Metal:- In case of Ferrous Metal
Softer than normal: - In case of Non- Ferrous.
Here the metal (usually steel or cast iron) is heated above the upper critical temperature and then
cooled rapidly. The Cooling medium depends on the alloy and other considerations (such as
concern for maximum hardness vs. cracking and distortion). Cooling medium includes, Forced
air or other gases (such as nitrogen) & Liquids with good thermal conductivity such as water, oil,
a polymer dissolved in water, or brine thermal conductivity. The Martensite thus formed from
the austenitic portion has a hard and brittle crystalline structure. The chemical composition and

11
quenching method determines the quenched hardness of a metal. Polymer (i.e. silicon) has the
fastest cooling rate followed by brine, fresh water, oil, and forced air. But due to the possibility
of cracking due to very fast cooling, Oil should be used as the quenching medium in high-tensile
steels such as AISI 4140 should, Forced air to be used in tool steels such as ISO 1.2767 or H13
hot work tool steel, and Brine or water is to be used in low alloy or medium-tensile steels such as
XK1320 or AISI 1040.
However, most non-ferrous metals, soften when quenched. Ex: - alloys of copper, aluminum, or
nickel, and some high alloy steels such as austenitic stainless steel (304, 316),
Austenitic stainless steels must be quenched to become fully corrosion resistant, as they work-
harden significantly [33].
2.3.2.6 Tempering
Martensitic steel formed after quenching is very hard and brittle. So they cannot be used in any
application. This problem is solved by tempering. To impart some toughness in steel, it is heated
below the lower critical temperature, (often from 400 to 1105 F or 205 to 595 C, depending on
the desired results).
To impart further ductility in a metal higher tempering temperatures, (may be up to 1,300F or
700C, depending on the alloy and application), are used, but at a cost of yield strength.
Normalized steels can be tempered also.
Other methods of tempering consist of quenching the metal to a temperature, above the
martensite start temperature, and then holding it there till pure bainite is formed or internal
stresses are relieved. These include austempering and martempering [33]. The different types of
heat treatments in steel are schematically illustrated in Fig. 2.1.

12
2.3.3 Effects of time and temperature

Figure 2.2. Time-temperature transformation (TTT) diagram for steel

Fig. 2.2 shows the TTT diagram for steel. Control over temperature is very critical in a heat
treatment, for example the amount of time that an alloy is hold at a certain temperature and in the
cooling rates of a particular cooling medium [32]. All heat treatment except stress-relieving,
tempering, and aging, begin by heating an alloy above A3 temperature. The heat penetrates the
alloy, which results in a complete solid solution. Since Mechanical properties like toughness,
shear strength and tensile strength are enhanced because of a smaller grain structure, the metals
is kept to a temperature above the upper critical temperature, which prevent large grain growth.
For example, the austenitic grains are fine just above the upper critical temp and grow bigger as
we increase the temperature. This affects the martensite grain structure when quenched. Larger
grains with large grain-boundaries act as weak spots in the structure. So, the probability of
breakage of the metal is governed by its grain structure. [32]
Diffusion transformation is time controlled. Cooling a metal usually suppress the precipitation to
a much lower temperature. For Example, when rapidly cooled Austenite can exist in a highly
unstable form hundreds of degree below the lower critical temperature. With time it will

13
precipitate to ferrite and cementite. So, the rate of grain growth or to form partially martensitic
microstructures can be controlled by the cooling rate. [33]
The austenite grain size affects the rate of nucleation when it is cooled slowly and martensitic
transformation doesnt occur. But normally temperature and the rate of cooling control the grain
size and microstructure. "Sphereoidite." is formed when austenite is cooled extremely slowly; it
results in large ferrite crystals filled with spherical inclusions of cementite. Coarse pearlite is
formed for a faster cooling rate. Even faster cooling rate will result in fine pearlite. If cooling
rate is still increased the result will be bainite. Similarly, these microstructures will form if the
metal is held at a certain temperature after cooling till that temperature. [32]
In case of non-ferrous alloys heat treatment is done to form a solution. Mostly, these quenched to
result in a martensite transformation, which puts the solution into a supersaturated state. The
alloy can be cold worked as they are in a softer state, and these plastic deformation results in
defects which in turn speed up precipitation, resulting in increased hardness and strength of the
metal.
Even if not cold worked, the solutes in these alloys will usually precipitate, although the process
may take much longer. Sometimes in order to speed-up the precipitation these metals are heated
to a temperature below A1 temperature, so that re-crystallization is prevented. [32, 34, 35]
2.3.4 T-T-T Diagram of Cr-Mo steel

Figure 2.3 T-T-T diagram of 2.25Cr-1Mo steel

Cooling rates faster than the rate to produce pearlite and slower than that required to form
martensite will result in bainite (By both isothermal & athermal process).

14
In carbon steels, however, the overhanging pearlite nose eclipses the bainite transformation. It
results in formation of pearlite, or martensite or a mixture of both if austenite is continuous
cooled. But bainite can be formed easily in some alloy steels containing elements like Cr, Mo, B
etc. these elements retard the pearlitic transformation & help in the bainitic formation on
continous cooling of austenite [1]. This is reflected by the T-T-T diagram of 2.25Cr-1Mo steel in
Fig. 2.3. With greater hardenability of the steel possibility of bainitic formation is increased.
2.4 Wear:
Wear refers to the progressive removal of material from a surface and plastic deformation of
material on a surface due to the mechanical action of the other surface [28]. The necessity for
relative motion between the operating surfaces and initial mechanical contact between asperities
leads an important role between mechanical wear compared to other processes with similar
outcomes [29].
2.4.1 Factors affecting the wear performance of materials
Wear behavior of a material depends on many factors.
It is highly depends upon the surface material, the shape of the contacting surfaces,
environment, operating conditions and also on the type of material of which the
components are made. As wear will be very different between tool steel on tool steel and
tool steel on aluminum.
Surface of solids, ranging from bulk surface distortion to local microscopic irregularities,
exert a strong influence on wear.
More is the surface roughness; more is the probability of wear.
The effects of alloying element have a great impact on wear and friction. For example,
presence of high sulphur content (about 100 ppm) in the bainitic steels leads to a high
fraction of MnS inclusion. The removal of material is enhanced by the presence of such
inclusions as they come close to the surface and form open cracks [36].
Wear behavior can also greatly affected by crystal structure, grain size, and grain
boundaries. The presence of grain boundaries in polycrystalline materials influences
friction as well as wear behaviour. When sliding motion occurs, surface dislocations are
blocked in their movement by a grain boundary and they accumulate at the grain
boundary which results in strain-hardening of the surface layers. This action makes

15
 sliding motion more difficult and increases frictional force for materials in sliding contact
leads to wear of the material [37].
The presence of more aggressive atmosphere results in formation of oxides on the worn
surfaces. The type of loading is an important factor that means the wear of two objects
rubbing together is different than wear occurs due to one object impacts the other.
Speed, temperature, and lubrication also affect the wear of components.
2.4.3 Wear mechanisms
The several wear mechanisms acting either alone, or simultaneously on a material are as follows:
Adhesive wear
Abrasive wear
Fretting wear
Surface fatigue and
Tribochemical or corrosive wear
2.4.3.1 Adhesive wear
Adhesive wear occurs due to materials adhering or sticking with each other under loading which
results in material transfer between the two surfaces or the loss of material from either surface
[38]. Adhesive wear mechanism is schematically shown in Fig. 2.4.

Figure 2.4. Adhesive wear mechanism [38]

16
2.4.3.2 Abrasive wear
Abrasive wear takes place due to rubbing of softer surface by the harder surface. In the case of
ductile materials, hard particles or hard asperities results in plastic flow of softer material. In
brittle materials, wear occurs by brittle fracture [38]. Abrasion is categorized depending on the
types of contact, as well as contact environment. Depending on the types of contacts, abrasive
wear can be classified as two-body and three-body wear. The former occurs due to an abrasive
slides along a surface, and the later, due to an abrasive is caught between one surface and another
[39]. Fig. 2.5 shows the schematic representation of two body and three body wear mechanisms.

Figure 2.5. Two and three body abrasive wears mechanism

Fig. 2.6 represents some of the processes that are possible in case of abrasive wear. They include
plowing, wedge formation, cutting, micro fatigue and micro cracking [39]. Plowing is the
process of displacing material from a groove to the sides, away from wear particles. The most
severe form of wear for ductile material is cutting. During cutting materials separated from the
surface like conventional machining [39].

17
Figure 2.6. Five processes of abrasive wear (a) Plowing (b) Wedge (c) Cutting (d) Micro
fatigue (e) Micro cracking
2.4.3.3 Fretting wear
Fretting wear refers to small amplitude oscillatory motion that occurs between contacting
surfaces which are usually at rest. The movement is usually because of the external vibration, but
in most cases it occurs due to one of the members being in contact subjected to cyclic stress
which gives rise to early fatigue cracks. This is known as fretting fatigue [39]. It is affected by
different variables such as amplitude of slip, normal load applied on the material, frequency of
vibration and also on fretting situation, such as type of contact, mode of vibration and the
condition of surfaces. Fig. 2.7 illustrates the schematic representation of Fretting wear.

Figure 2.7. Fretting wear

18
2.4.3.4 Surface fatigue
Surface fatigue occurs when surface undergoes repeated cycles of stress. It is represented in Fig.
2.8. This may be due to sliding or rolling motion of surfaces. When material is subjected to
several cycles of stress, there may be crack formation in/near the surface. However, in an
interface of materials the contacting stresses are very high and surface fatigue wear mechanism
can be operative [38].

Figure 2.8. Surface Fatigue

2.3.4.5. Corrosive wear

Corrosive wear occurs when sliding takes place in a corrosive environment. The most dominant
corrosive medium is oxygen. The combined effect of friction and chemical reaction leads to total
material losses that are much greater than any of the process taken alone [38]. In the absence of
sliding, the chemical products form a protective layer on the surface, which tends to lower the
corrosion, but the sliding motion wears the chemical film away, so that the chemical attack
continues [38]. The schematic diagram of corrosive wear is illustrated in Fig. 2.9.

19
 Figure 2.9. Corrosive wear [38].
2.3.4.6. Erosion wear
Erosive wear results from sharp particles impinging on a surface such as the cutting of materials
by hard particles. This action is similar like sandblasting. Figure 2.10 shows the erosion wear
schematically.

Figure 2.10. Erosion wear

A mixture of commercial grade nickel and aluminum powder is coatable on metal substrates by a
thermal plasma spraying technique. The coating developed in study is harder than that of the
substrate materials; hence, these coatings can be recommended for tribological applications. The
solid particle erosion wear resistance of these coatings is fairly good. The rate of erosion of the
coating is found to be greatly affected by the angle of impact and the velocity of impact of the
eroding particles. For brittle materials subjected to erosion, the maximum wear rate occurs at 900
impact and for ductile material it is between 15 and 300 [40]. Ferrite martensite dual phase (DP)
steels have microstructures comprising hard martensite islands embedded in a soft and ductile

20
ferrite matrix. This distinct microstructure leads to characteristic mechanical properties like
absence of yield point phenomena, large ratio of tensile strength to yield strength, high rates of
work hardening, high total and uniform elongation, excellent forming characteristics and high
fracture toughness [41-44]. The main mechanism involved in wear in DP steel is primarily due to
delamination in the range of loads and sliding speed used in the present study for all the DP
steels investigated, as revealed from the wear debris and the worn sub surfaces. With increasing
volume fraction of martensite wear rate of the dual phase steels decreases which may tends to (a)
increasing of hardness of steels and (b) decreasing the possibility of cracks formation during
delamination [45]. Fig. 2.11 shows the variation of wear rate in DP steels.

Figure 2.11. Variation of wear rate with martensite volume fraction in DP Steels [45]

Tool wear mechanisms in turning of high hardness alloy steels by CBN tools under various
speeds are investigated by experimental studies. When the cutting temperature is comparatively
low (i.e. at low speed cutting), there is generation of high cutting forces because the degree of the
softening of work material is not significant. So, the tool face would be scratched by the hard
carbide particles of work material and the binder of the CBN is removed. The main mechanism
of wear occurs in this case is abrasion, and there are scratched marks on tool face. As cutting
speed is increased, the softening of work material becomes significant which in turn, causes
cutting forces to reduce. The diffusion and oxidation would be more pronounced in higher
cutting temperature. A layer with oxidized compounds exhibiting a lower melting point is

21
generated which protects the cutting tool from wear. Hence, tool wear is reduced and tool life is
increased. When cutting temperature is very high, the sticking layer is worn away due to a great
friction force. In addition to that, the bond between the CBN particles of the cutting tool is
weakened leading to severe diffusion of work and tool materials. Hence, CBN particles are
removed from the tool face. Subsequently, cutting edge is weakened, and results in increase of
flank wear represented in Fig. 2.12 [46].

Figure 2.12.Wear on the flank face for workpiece hardness of

HRc 50 under V = 82 m/min [46]
The influence of new type heat treatment - sinter hardening on the wear characteristics of high-
strength sintered steels has been studied. Wear resistance of investigated sintered steels were
improved due to shifting ferrite - bainite to dominant martensitic microstructure. The
microscopic investigation reveals that delamination and oxidation wear are the dominant wear
mechanisms in wear tests as illustrated in Fig. 2.13 and Fig. 2.14. The results of friction
coefficient show that the steady-state value of friction coefficient decreases with the increasing
amount of porosity. The pores play an important role indicating the potential sites of the first
micro cracks forming and positively influencing the wear process [47].

22
 Figure 2.13. Wear rates of studied sintered steels at 1180 C using both cooling rates [47]

Figure 2.14. The typical delamination wear of studied sintered steels with fine grooves
parallel to the sliding direction and flake-like fragments (a) and with mild oxidation wear
(b) [47]
The heat treated spring steel material has maximum strength in comparison to the normal
material. The strength has more influence on hardness. Compared to normal material, heat
treated material have more hardness. Wear rate of spring steel material increased with increasing
load, speed and distance. Wear rate of material depends on the heat treated conditions of the

23
material and also on the applied load, speed and distance as illustrated in Fig. 2.16, Fig. 2.17 and
Fig. 2.15 respectively [48].

Figure 2.15. Shows Variations of Wear Rate of Spring Steel with Sliding Distance. [48]

Figure 2.16. Variations of Wear Rate of Spring Steel with Load [48]

Figure 2.17. Variations of Wear Rate of Spring Steel with Speed [48].

24
Materials condition influences the wear rate. High wear rate is formed in tempered material as
compared to cryogenic specimen [48]. The influence of elemental boron addition on the wear
resistance and structure of PM 316L stainless steel was investigated. During sintering addition of
boron in PM parts forms liquid phase. The formed liquid phase fills the contact and pore area
leading to higher theoretical density and hardness values of the samples. The formation of boron
rich phases in particle contact area resulted in a decrease in the wear rate of boron added sample
as shown in Fig. 2.18. By the addition of 0.6 wt. % boron to stainless steel maximum density,
hardness and low wear rate was obtained. Hence the boron addition increases sintered density
and hardness [49]. Fig. 2.19 shows the worn surface of steel with and without boron addition.

Figure 2.18. Variation of wear rate with sliding distance for samples with and without
boron addition [49].

Figure 2.19. SEM of worn surface of 316L stainless steel: (a) without and (b) with boron
addition at 10.8 N, 0.21 m s-1 speed and sliding distance 6000 m [49].

25
The pearlitic steel showed higher sliding wear resistance than bainitic steel, which is due to the
excellent strain hardening of pearlite in comparison to bainite. Oxidative wear mechanisms were
observed in the pearlitic steel, while in the bainitic one adhesive wear was dominant mechanism,
leading to a much more accentuated damage of the surface [50].

26
 Chapter 3
Experimental

27
3. Experimental
3.1. Materials
Modified 9Cr1Mo ferritic steel (P91) is commonly used by power sector for power generation,
chemical processing and also in petroleum industries due to its radiant mechanical properties and
resistance to high temperature corrosion. This material is also, currently applied for fast reaction
steam generators in the normalized and tempered condition. This material has procured from
China 16 mm thick plate. Chemical composition of this material is as under.

Material C Si Mn P S Cr Mo Ni V
9Cr-1Mo 0.09% 0.25% 0.35% 0.02% 0.01% 9% 0.99% 0.4% 0.19%
steel

Table 3.1 Chemical composition of 9Cr-1Mo steel

3.2. Experimental Procedures

3.2.1 Tensile Test:

The tensile test is commonly done to provide basic design information, to identify the strength of
materials and as a means for specification of materials. The tensile test was done with the help of
ASTM E8M-04 using Instron-8800 testing machine. The plate type specimen was used for
tensile test.

Figure 3.1 Instron 8801 servo hydraulic testing machine

28
3.2.2 Heat Treatment of samples

The material of our investigation (9Cr-1Mo ferritic steel (P91)) was first subjected to different
heat treatments. Total numbers of 12 specimens having dimensions of 7.5 mm x 7.5 mm x 10
mm were machined from the supplied plate material. These specimens were subjected to
different heat treatment operations (annealing, normalizing and water quenching) heated to
austenitisation temperature of 10500C (1323 K). The heat treatments were done in Carbolite
furnace.

Figure 3.2 Carbolite Furnace

3.2.3 Material Characterization

Material characterization was performed by two methods.

1. Optical microscopy
2. Scanning Electron Microscopy (SEM)

Metallography is the microscopic study of the structural characteristics of a metal or an alloy.

The success in microscopic study depends mostly upon the care taken in the preparation of the
specimen. So the ultimate objective is to produce a flat, scratch-free, mirror like surface.

Steps involved in sample preparation:

The steps adopted in specimen preparation are as follows.

1. Cutting a specimen

29
2. Rough Grinding
3. Intermediate Polishing
4. Fine Polishing
5. Etching

1. Cutting of specimens: Cutting of specimens were performed by hack sawing. The

specimens were cut in dimensions of 7.5 mm x 7.5 mm x 10 mm. One from each heat
treated types of specimen was taken for microscopic study. Then three specimens i.e. one
from each heat treated types were taken to the second stage of specimen preparation i.e.
the rough grinding stage.
2. Rough Grinding: The sample was rough-ground on a belt sander, with the specimen
made cool by continuous dropping in water during the grinding operation. The specimen
was made to move perpendicular to the existing scratches. The rough grinding was
continued until the surface was made flat and free of nicks, burrs, etc., and no scratches
due to the hacksaw was found anymore visible.
3. Intermediate Polishing: After rough grinding, the specimens were ground with rotating
discs of abrasive paper, i.e., wet silicon carbide paper. The coarseness of the paper is
indicated by a number, that is, the number of grains of silicon carbide per square inch (for
example, 180 grit paper is coarser than 1200). The grinding procedure involves several
stages, using a finer paper (higher number) for each successive stage i.e. from 80, 120,
180, 220, 320, 400, 600, 800, 1000, and 1200 to at least 1500. Each grinding stage
removes the scratches from the previous coarser paper. This was more easily obtained by
orienting the specimen perpendicular to the previous scratches, and watching for these
previously oriented scratches to get obliterated. Typically, the finest grade of paper used
was the 1500, and once the only scratches left on the specimen were from this grade, the
specimen was thoroughly washed with soapy water and then allowed to dry.
4. Fine Polishing: The final approximation to a flat scratch-free surface was obtained by
use of a wet rotating wheel covered with a special cloth that was charged with cautiously
sized abrasive particles. The abrasive used was diamond paste. The selection of a paper
polishing cloth depends upon the specific material being polished and the purpose of the
metallographic study. The cloth used in our case was velvet cloth.

30
 Figure 3.3 Rotating disc for polishing

5. Etching: The purpose of etching is to make visible the many structural characteristics of
the metal or alloy. The process must be such that the various parts of the microstructure
should be clearly differentiated. This was accomplished by use of Vilellas reagent
having chemical compositions of 1 gram picric acid, 5 ml. HCl and 100 ml ethyl alcohol
in case of 9Cr-1Mo ferritic steel.

3.2.3.1 Optical Microscopy:

The micro-examination and phase analysis were done using optical microscope fitted with Image
Analyzer of model LEICA DMI3000 M as shown in Fig. 3.4. The percentages of phases present
in the microstructure were obtained according to ASTM E562.

31
 Figure 3.4 Image Analyzer LEICA DMI3000 M

3.2.3.2. Scanning Electron Microscopy

The specimen preparation for SEM was similar to that of optical microscopy. To study the
microstructures of heat treated specimens, JEOL-JSM 6510 Scanning Electron Microscope
(SEM) as shown in Fig. 3.5 was used. The microstructure was revealed under much higher
magnification from 500X to1500X.

Figure 3.5 Scanning Electron Microscope JEOL JSM-6510

32
3.2.4 Vickers hardness Test

The hardness of all heat treated samples was measured with the help of Vickers hardness testing
machine of model LECO MICROHARDNESS TESTER LM 247 AT as shown in Fig. 3.6. The
sample surfaces were made flat by mounting the specimens in Hot Mounting Press at 1350C for 5
minutes.

Figure 3.6 Vickers hardness testing machine

3.2.5. Sliding Wear Test:

The sliding wear test was conducted on 9Cr-1Mo ferritic steel (P91). The test was done in Multi
Tribo Tester, TR-25 (shown in Fig. 3.7). The Multiple tribo tester TR-25 has a significant
advance in terms of multiple contact geometry selection, convenience of operation, ease of
specimen clamping and removal, accuracy of measurements of test parameters load, speed,
temperature, wear and frictional torque. It facilitates study of friction and wear characteristics in
rolling sliding contacts under desired test conditions. Normal load, rotational speed and
temperature can be changed to suit varied test conditions. Tangential frictional force and wear
are measured with electronic sensors and recorded on PC. These parameters are available as
functions of load and speed.

33
 Figure 3.7 Multiple Tribo Tester TR-25
Test configuration can accommodate:

1. Roller on roller
2. Pin on roller
3. Cylinder on roller
4. Ball on roller and configurations

The TR 25 test instrument comes with the WinDucom 2008 software for data acquisition and
display of results. The WinDucom software and data acquisition system allows users to measure
applied test load, speed and friction. WinDucom software is used to present data in a variety of
ways and CompariView provides a powerful tool to view and compare test results for evaluation.
Fig. 3.8 shows the result display and data input page of WINDUCOM 2008 software.

Parameter Unit Min. Max.

Load N 0 1000
Speed RPM 0 2000
Temperature Deg C Ambient 120
Wear Micron 0 2000

34
 Figure 3.8 Display of results by WINDUCOM 2008 software

Sample preparation for Wear Test:

Total of 9 samples were taken for the wear test among which three samples were annealed, three
of normalized, and rest three are of water quenched type. For conducting sliding wear test, the
specimens were prepared with the dimensions of 6.35 x 6.35 x 9 mm3 as shown in Fig. 3.9. The
samples of required dimensions were prepared from the previously cut specimens of 7.5 x 7.5 x
10 mm3 dimensions by polishing. The sample surfaces were polished properly to give the
samples a mirror-like appearance by different sizes of grit papers.

Figure 3.9 Sample for wear test having dimension 6.35 x 6.35 x 9 mm

Test Program:
The test was performed on a disc-on-roller multiple wear tester under dry sliding condition
rubbing against EN-31 steel. The sample was put in the sample holder of the top roller and then
was tightened by the screws fitted with it. The sample was kept having 6.35 x 6.35 mm2

35
dimensions as base and 9 mm as height. The square surface touches the bottom roller. The top
roller was placed stationary and the load was given on the top roller and the bottom roller rotates.
The speed with which the bottom roller rotates and the load that was applied to the top roller was
fed from the operator in the computer. The machine attached with the computer takes the input
and operated accordingly. The bottom roller slides over the bottom surface of sample and wear
took place. The data were measured with electronic sensors and recorded on PC. The disc-on-
roller arrangement is shown in Figure 3.10.

Figure 3.10 Disc-on-roller arrangements

Details of the test:
Three samples from each heat treated types were assigned three different load variations of 30N,
50N and 100N at a constant speed of 250 rpm. The wear with respect to time or sliding distance
was recorded for all the heat treated types at three different load variations for each one. The
wear rate over time or sliding distance graph was obtained for every sample. Graphs were drawn
for each heat treated type to know how they respond to the load variations. Then a comparison
graph was plotted at a load of 100N among the annealed, normalized and water quenched
samples to show the variations of wear and wear rate over time.

36
 Chapter 4
Results & Discussion

37
4 Results and Discussions
4.1 Tensile test Results

Table 4.1 Tensile test results

The Table 4.1 shows the ultimate tensile strength and yield strength of the material. The tensile
strength of modified 9Cr-1Mo steel is found to be 601.37 MPa and yield strength is found to be
444.87 MPa.

4.2 Microstructural Characterization

4.2.1 Optical Microscopy

The following Fig. 4.1(a), Fig. 4.1(b) and Fig. 4.1(c) show the microstructures of annealed,
normalized and water quenched samples of Modified 9Cr-1Mo steel respectively.

Figure 4.1(a) Optical microstructure of Annealed sample

38
 Figure 4.1(b) Optical microstructure of Normalized sample

Figure 4.1(c) Optical microstructure of Water Quenched sample

Fig. 4.1(a) reveals that upper bainite and some amount of ferrites are formed in the annealed
specimen. Fig.4.1 (b) reveals that the normalized one also forms the same phases, i.e. bainite
with some amounts of ferrites present in the microstructure. But in this case relatively fine grains
are formed than the annealed one. In the case of normalized specimen the bainite plates are
closely spaced, where as in case of annealed steel the bainite plate spacing was more. On the

39
other hand fully bainitic structure is found in the water quenched specimens with negligible
amount of ferrite. Fig. 4.1(c) shows the microstructure of quenched specimen.

4.2.2 Phase Analysis

% of bainite present
% of ferrite present
100

80
1 Annealed
% of Phases present

60 2 Normalized

3 Water Quenched
40

20

0
1 2 3
Sample

Figure 4.2 Phase analysis of heat treated samples

Fig. 4.2 shows the percentages of ferrite and bainite present in different heat treated types of
samples. The sample of water quenched type shows almost fully bainitic structure as the
percentage of ferrite present is negligible in comparison to the amount of bainite present. The
annealed and normalized specimens exhibited nearly the same phase composition.

40
4.2.3 Scanning Electron Microscopy with EDS analysis

Figure 4.3 (a) Scanning electron micrograph of annealed sample (left), (b) EDS analysis of
annealed sample (right).

Fig. 4.3(a) shows the SEM micrograph of annealed specimen at 1000X magnification. These
micrographs are taken in the dark field. The white phases represent bainite and the dark phases
represent ferrite. The bainites are dispersed in the ferrite matrix. Relatively coarse grains are
formed. Fig. 4.3(b) shows the major elements present in the annealed specimen by forming
peaks. Along with iron, chromium, carbon and silicon are also present.

Figure 4.4 (a) Scanning electron micrograph of normalized sample (left), (b) EDS analysis
of normalized sample (right).

41
Fig. 4.4(a) shows the SEM micrograph of normalized sample at 1000X magnification. This
micrograph is the dark field image. The white phases represent bainite and the dark phases
represent ferrite. In this case, relatively finer grains are formed. Fig. 4.4(b) shows the EDS
pattern of the normalized sample. This pattern reveals the presence of iron, carbon and chromium
in the steel.

Figure 4.5 (a) Scanning electron micrograph of water quenched sample (left), (b) EDS
analysis of water quenched sample (right).

Fig. 4.5(a) shows the fully bainitic structure formed in the water quenched sample. Fig. 4.5(b)
shows the presence of same elements as that of annealed and normalized ones.

42
4.3. Hardness determination

Vickers Hardness

500

400
1 Annealed
Vickers Hardness

300
2 Normalized

200 3 Water Quenched

100

0
1 2 3
Samples

Figure 4.6 Comparison graph of hardness values of different heat treated samples by
Vickers hardness test.

Fig. 4.6 shows the hardness values of different heat treated samples. The water quenched sample
possesses highest hardness among the three types. This is due to the fully bainitic structure
formed in case of quenched sample as revealed by phase analysis. The annealed sample shows
the lowest hardness as due to the formation of coarse grains. The Vickers hardness values of
annealed, normalized and quenched structures are 390HV, 415HV and 482HV respectively.

43
4.4. Wear Test Results

350 Polynomial Fit of WEAR 30

Polynomial Fit of WEAR 30
Polynomial Fit of WEAR 50 350 Polynomial Fit of WEAR 50
300 Polynomial Fit of WEAR 100 Polynomial Fit of WEAR 100
300
250
250
200
200
WEAR

150

WEAR
150

100
100

50
50

0
0

-50 -50

-500 0 500 1000 1500 2000 2500 3000 3500 4000 0 500 1000 1500 2000 2500 3000
TIME SD

Units : Wear is in m, time is in seconds, sliding distance is in meters.

Figure 4.7 (a) Wear versus time graph of annealed sample subjected to load variations of
30N, 50N and 100N (left), (b) Wear versus sliding distance graph of annealed sample
subjected to load variations of 30N, 50N and 100N (right).

From Fig. 4.7(a) and Fig. 4.7(b) it can be clearly seen that the annealed sample which was
subjected to 100N load experiences more wear in comparison to those which were subjected to
30N and 50N load. The reason behind this variation is very clear. This is due to increase in
friction at the surface as the load on the material increases. The wear versus sliding distance
graph follows the same pattern as that of wear versus time as with increase of time the sliding
distance increases. Hence with increase in load, the wear with respect to time or sliding distance
increases. This can also be confirmed from the worn surfaces analysis of annealed samples by
SEM.

44
 WR 30 WR 30
WR 50 WR 50
0.09 WR 100 WR 100
Linear Fit of WR 30
0.09
Linear Fit of WR 30
0.08 Linear Fit of WR 50 0.08 Linear Fit of WR 50
Linear Fit of WR 100 Linear Fit of WR 100
0.07 0.07
0.06 0.06

WEAR RATE
0.05 0.05
WEAR RATE

0.04 0.04
0.03 0.03
0.02 0.02
0.01 0.01
0.00 0.00
-0.01 -0.01
500 1000 1500 2000 2500 3000 3500 4000 0 500 1000 1500 2000 2500 3000
TIME SD

Units: Wear rate is in m/sec, time is in seconds, sliding distance is in meters.

Figure 4.8 (a) Wear rate versus time graph of annealed sample subjected to load variations
of 30N, 50N and 100N (left), (b) Wear rate versus sliding distance graph of annealed
sample subjected to load variations of 30N, 50N and 100N (right).

Fig. 4.8 (a) and (b) shows the overall decreasing trend of wear rate with increase of time or
sliding distance. Initially the wear rate is high and gradually it decreases with progress of time or
sliding distance.

350
Polynomial Fit of wear 30 N
Polynomial Fit of wear 50 N
Polynomial Fit of wear 100 N
300

250

200
wear

150

100

50

-50
-500 0 500 1000 1500 2000 2500 3000 3500 4000
time

Figure 4.9 Wear versus time graph of normalized sample subjected to load variations of
30N, 50N and 100N.

45
Fig. 4.9 reveals the wear versus time graph of normalized sample subjected to load variations of
30N, 50N and 100N. In this case deviation has occurred for material subjected to 100N load and
material with 100N load experiences less wear as compared to the one subjected to 50N. This
case has happened due to formation of oxide scales on the surface. As the load applied on the
material increases, the friction at the surface increases, which again leads to increase of
temperature. This increase in temperature of the material favours the oxide scale formation
leading to oxidative pattern and is having high spalling resistance, which inhibits the further
wear of the material to takes place. The oxide scale formation has confirmed from the EDS
analysis of the worn out surface. The actual wear behavior can be recognized by means of
scanning electron micrographs of worn out surfaces.

WR 30 N
WR 50 N
0.16 WR 100 N
Linear Fit of WR 30 N
0.14 Linear Fit of WR 50 N
Linear Fit of WR 100 N
0.12

0.10
WEAR RATE

0.08

0.06

0.04

0.02

0.00
500 1000 1500 2000 2500 3000 3500 4000
TIME

Figure 4.10 Wear rate versus time graph of normalized sample subjected to load variations
of 30N, 50N and 100N.

Figure 4.10 shows the overall decreasing trend of wear rate with increase of time. Initially the
wear rate is high and gradually it decreases with progress of time.

46
 Polynomial Fit of WEAR 100
300
Polynomial Fit of WEAR 50
280
Polynomial Fit of WEAR 30
260
240
220
200
180
160

WEAR
140
120
100
80
60
40
20
0
-20
-40
-500 0 500 1000 1500 2000 2500 3000 3500 4000
TIME

Figure 4.11 Wear versus time graph of water quenched sample subjected to load variations
of 30N, 50N and 100N.

Fig. 4.11 reveals the wear versus time graph of water quenched sample subjected to load
variations of 30N, 50N and 100N. This figure shows the same deviations for sample subjected to
load of 100N. In quenched case, the sample having 100N load experiences least wear among the
three types of loads. The reason behind this fluctuation is same as that of normalized one which
is the result of formation of oxide layer on the surface inhibits wear. The formation of oxide
scales in this case can be clearly seen from the worn surface analysis of the quenched sample
subjected to 100N load.

47
 WR 30
WR 50
0.15 WR 100
0.14 Linear Fit of WR 30
0.13 Linear Fit of WR 50
Linear Fit of WR 100
0.12
0.11
WEAR RATE 0.10
0.09
0.08
0.07
0.06
0.05
0.04
0.03
0.02
0.01
500 1000 1500 2000 2500 3000 3500 4000
TIME

Figure 4.12 Wear rate versus time graph of water quenched sample subjected to load
variations of 30N, 50N and 100N.

Fig. 4.12 shows the overall decreasing trend of wear rate with respect to time of quenched
samples having different load variations.

Polynomial Fit of WEAR A 100

Polynomial Fit of WEAR N 100
300
Polynomial Fit of WEAR Q 100

250

200
WEAR

150

100

50

-50
-500 0 500 1000 1500 2000 2500 3000 3500 4000
TIME

Figure 4.13 Wear versus time graph of different heat treated samples at a constant load of
100N.

48
In Fig. 4.13, the red line shows the wear behavior of normalized sample, the black line indicates
the wear behavior of annealed sample and the blue one shows the wear behavior of water
quenched samples subjected to a constant load of 100N. It can be clearly seen from Fig. 4.13 that
the water quenched sample experiences least wear among the three heat treated types. This may
be due to the fully bainitic structure (lower bainite) formed in case of quenched sample leading
to highest hardness among the three types and results in least wear. Hardness decreases from
quenched to normalized and then to annealed one. So wear increases from quenched to annealed
through normalized. There is a little fluctuations occurring in case of annealed and normalized
types. This may be due to wear in the ferrite part of the material takes place results in
comparatively higher wear than wear occurring due to bainitic parts. This cant be easily
distinguished as it requires microscopic investigation.

WR A
0.10 WR N
WR Q
0.09 Linear Fit of WR A
0.08 Linear Fit of WR N
Linear Fit of WR Q
0.07
0.06
WEAR RATE

0.05
0.04
0.03
0.02
0.01
0.00
-0.01
500 1000 1500 2000 2500 3000 3500 4000
TIME

Figure 4.14 Wear rate versus time graph of different heat treated samples at a constant
load of 100N.

Fig. 4.14 shows the overall decreasing trend of wear rate with increase in time duration for all
the three heat treated types at a constant load of 100N.

49
4.5 Worn surfaces analysis by SEM

Sliding direction

Figure 4.15 Worn out surface of annealed sample subjected to 30N load (a) at 50X, (b) at
400X. Abrasive wear

Figure 4.16 Worn out surface of annealed sample subjected to 50N load (a) at 50X, (b) at
400X.

50
Figure 4.17 Worn out surface of annealed sample subjected to 100N load (a) at 50X (left),
(b) at 400X (right).

The white scratches seen on the worn out surface of Fig. 4.15, Fig. 4.16 and Fig. 4.17 reveals the
amount of wear occurs and also the direction in which the wear occurs and the pattern it follows.
Fig. 4.15 shows the least wear taking place of annealed sample subjected to 30N load than
subjected to 50N and 100N load. Fig. 4.17 shows the highest wear. Fig. 4.15, Fig. 4.16 and Fig.
4.17 shows the similar type of wear pattern i.e. the abrasive wear is taking place in the three
cases. The direction in which the wear takes place is represented by sliding direction which is
indicated in Fig. 4.15.

Figure 4.18 Worn out surface of normalized sample subjected to 30N load (a) at 50X (left),
(b) at 300X (right).

51
Figure 4.19 Worn out surface of normalized sample subjected to 50N load (a) at 50X (left),
(b) at 300X (right).

Figure 4.20 Worn out surface of normalized sample subjected to 100N load (a) at 50X (left),
(b) at 200X (right).

52
 Figure 4.21 EDS Analysis of normalized sample subjected to 100N load

Figs. 4.18 - 4.20 show the worn surfaces of normalized sample subjected to three load variations
of 30N, 50N and 100N respectively. Fig. 4.18 and 4.20 show the similar worn surface pattern
while the worn surface pattern of Fig. 4.20 shows a difference from these two types. This is due
to the oxide scales formed in case normalized sample subjected to load of 100N as illustrated in
Fig. 4.20. The formation of oxidative wear pattern which is the main reason of decrease in wear
in case of 100N is confirmed by the EDS analysis as shown in Fig. 4.21. Fig. 4.21 shows the
presence of oxygen peak in that sample confirming the formation of oxides as chromium has the
more affinity to form oxides.

53
Figure 4.22 Worn out surface of quenched sample subjected to (a) 30N load (left), (b) 50N
load (right).

Oxide scales

Figure 4.23 Worn out surface of quenched sample subjected to 100N load

54
Fig. 4.22 (a), (b) and Fig. 4.23 show the worn surface of quenched sample subjected to load of
30N, 50N and 100N respectively. From Fig. 4.23 it can be clearly seen that due to generation of
high temperature on application of high load, oxide scales are formed. These formation of oxide
scales are the main reason behind the least wear of 100N load among the three loadings.

55
 Chapter 5
Conclusions & Future Work

56
5.1 Conclusions
i. Microstructural variation is responsible for the sliding wear behavior of modified 9Cr-
1Mo steel.

ii. Variation of wear with respect to time increases with increasing level of load on the
material as with increase in load, there will be more friction at the surfaces in contact,
which leads to increase in wear of material. This type of trend has taken place in case of
annealed samples subjected to different load variations.

iii. Deviation has occurred in case of normalized and water quenched samples subjected to a
high load of 100N which is due to oxide scales formed on the material surface leading to
oxidative wear pattern which does not allow further more wear to occur, hence a decrease
in wear of the material takes place.

iv. The variations in wear behaviour of three heat treated types at a constant load of 100N
gives information that the water quenched sample experiences less wear in comparison to
normalized and annealed ones. This is due to the formation of fully bainitic structure in
case of quenched sample which results in higher hardness of the material and least wear
among the three.

v. The wear rate with respect to time or sliding distance for all the three types of samples in
various loading conditions follows the decreasing trend.

5.2 Scope for Future Work

i. Present work is based on the dry sliding wear behaviour study of modified 9Cr-1Mo
steel. Future investigation leaves a wide scope for the researcher to study on lubricating
wear condition of the same material.

ii. Modified 9Cr-1Mo steel is widely used as super heater tubes in power plants, where the
particles worn away the surface of material. So sprinkling of foreign particles can be
introduced as an aggravator with the sliding (abrasion) wear case to simulate the real life
situation.

57
Chapter 6
References

58
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