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MASTER'S THESIS
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List of Figures
Fig 1. Model of deformation in adhesive asperity contact………………………………….….4
Fig 2. Two and three body abrasive wear mechanism………………………………………....5
Fig 3. Five processes of abrasive wear………………………………………………………..6
Fig 4. Schematic Stribeck curve……………………………………………………………….8
Fig 5. Ion - electron discharged mechanism…………………………………………………13
Fig 6. Schematic of the test specimens used in these studies…………………………...........16
Fig 7. Pin on disc machine setup…………………………………………………………......17
Fig 8. Schematic representation of Scanning Electron Microscope (SEM)……………...…...18
Fig 9. Schematic representation of Bragg’s law……...………………………………...…….20
Fig 10. Schematic representation of the high temperature test……………………………….22
Fig11. Surface topography of samples……………………………………….……………….25
Fig 12. X-rd spectra for tool steel specimens…………………………………………………27
Fig13. Friction coefficient of tool steel 3 - post oxidation 1, 2 and 3 sliding against high
strength boron disc at room temperature……………………………………………….……..29
Fig 14. Friction coefficient of tool steel 1 and tool steel 2 - post oxidation 1 sliding against
high strength boron steel disc at room temperature………………………...………………...30
Fig15. Friction coefficient of tool steel 3 - post oxidation 1, 2 and 3 at 400 ºC sliding against
high strength boron steel disc at 16 mm radius……………………………………………….31
Fig16. Friction coefficient of tool steel 3 - post oxidation 1, 2 and 3 at 400 ºC sliding against
high strength boron steel disc at 22 mm radius……………………………………………….33
Fig 17. Pin and disc volume wear loss (a) Tool steel 3 at room temperature (b) Tool steel 1
and 2………………………………………………………………….……………………….34
Fig18. SEM images of wear scars of tool steel 3 pin (top) and boron steel disc (bottom)
specimens at room temperature ………………………………………………………………35
Fig 19. SEM images of wear scars of pin (top) and disc (bottom) specimens………………..37
Fig 20. Pin and Disc volume wear loss of tool steel 3 at 400 ºC……………………………..38
Fig 21. SEM images of wear scars for tool steel 3 Pin (top) and boron steel disc at 400 º C at
16 mm wear track radius ..……………………………………………………………………39
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List of Tables
Table 1. Commonly used height parameters………………………………………….……...10
Table 2. Compositions (wt %) of the materials employed in these studies……………….....15
Table 3. Technical specification of Pin on disc machine………………………………….....17
Table 4. Technical specifications of Wyko 1100 NT optical profiler………………………..18
Table5. Test parameters for tests at room temperature……………………………………….21
Table 6. Test parameters for high temperature tests………………………………………….21
Table 7. Vickers Hardness measurements of test samples…………………………………...28
Table 8. High temperature test combinations……………………………………………...…31
Table 9. Weight % of elements present on tool steel 3aftert test at 400 °C and 16 mm wear
track radius …...………………………………………………………………………………32
Table 10. Weight % of elements present in tool steel 3 specimens at room temperature (after
test)…………………………………………………………………………………..………..36
Table 11. Weight % of elements present in tool steel 1 and 2 at room temperature test (after
test)…………………………………………………………………………………………....37
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TABLE OF CONTENTS
Ι. Introduction..............................................................................................................................1
1. Tribology.........................................................................................................................1
2. Friction............................................................................................................................1
3. Wear................................................................................................................................3
3.1. Adhesive wear............................................................................................................4
3.2. Abrasive wear.............................................................................................................5
3.3. Fretting wear...............................................................................................................6
3.4. Surface fatigue............................................................................................................7
3.5. Tribo chemical or Corrosive wear..............................................................................7
4. Lubrication......................................................................................................................8
5. High temperature Tribology............................................................................................9
6. Effect of surface quality on Tribochemical properties..................................................10
7. Surface treatments.........................................................................................................11
7.1. Microstructural treatments........................................................................................11
7.2. Diffusion treatments.................................................................................................11
7.3. Nitriding...................................................................................................................12
II. Objectives.............................................................................................................................14
III. Experimental approach.......................................................................................................15
1. Experimental materials.................................................................................................15
2. Surface treatments and specimen geometry..................................................................15
3. Experimental equipments..............................................................................................16
3.1 Pin on disc machine.................................................................................................16
3.2 Wyko 1100 NT optical profiler...............................................................................17
3.3 Scanning Electron Microscope (SEM)....................................................................18
3.4 X-ray diffraction......................................................................................................19
3.5 Micro hardness tester..............................................................................................20
4. Test parameters..............................................................................................................20
5. Test procedure................................................................................................................21
IV. Results and discussion........................................................................................................23
1. Surface characteristics of the unworn specimens...........................................................23
2. Hardness measurements.................................................................................................28
3. Friction results...............................................................................................................28
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3.1 Frictional behaviour at room temperature...............................................................28
3.2 Frictional behaviour at 400 ºC.................................................................................31
3.3 Friction results using 16 mm wear track radius.......................................................31
3.4 Friction results using 22 mm wear track radius.......................................................33
4. Wear results....................................................................................................................34
4.1 Wear loss and surface damage at room temperature...............................................34
4.2 Wear loss and surface damage at 400 ºC................................................................38
V. Conclusions..........................................................................................................................40
VI. Future work.........................................................................................................................41
References................................................................................................................................42
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I. Introduction
1. Tribology
The word Tribology was first reported in a landmark report by Jost (1966) which was
published by the UK department of education and science. The word is derived from the
Greek word Tribos meaning rubbing, so the literal translation would be “the science of
rubbing”. The committee led by Peter Jost, was given the task of highlighting the need for
more education and research within in the field of lubrication. The jost report concluded that
approximately 1% of the gross national product of the UK could be saved by decreasing
friction and wear. Historically it can be found that even the ancient Egyptians possessed some
knowledge about Tribology even though they did not use that term. Leonardo da Vinci
performed his friction experiments in the 1490’s and showed that friction was dependant in
the normal load on the material but not on the contact area [1].
Dictionaries define tribology as the science and technology of interacting
surfaces in relative motion and related subjects and practices [1]. In a larger sense, the study
of how things change with time and of the forces that cause them to do so is the objective of
dynamic investigation [2]. The function of tribological research is to bring about a reduction
in the friction and wear of mechanical components and protect them against failure and
provide long, reliable life by selection of materials, operating parameters and lubricants.
Mechanical systems such as bearings, seals and gears are the examples of components that are
investigated. Whenever two or more solid surfaces are in contact with relative motion
between the surfaces, tribology is involved [1]. The bodies in relative motion may be gas and
solid (aerodynamic friction), or liquid and solid (lubrication friction) or a solid and solid (dry
or solid friction) or the friction may be due to the internal heat dissipation process (internal
friction) [3].
2. Friction
The first part in tribology is friction which can be defined as the force resisting the relative
motion of two or more surfaces in contact or a surface in contact with fluid. Two of the most
significant inventions of early man are friction related. Use of frictional heating to cooking,
and discovered that rolling friction is much lower than that of sliding friction. The second
discovery led to the invention of the wheel. Friction plays an important role not only in the
daily life activities but also in the field of industrial applications. It aids in starting the motion
of a body and changing its direction and subsequently stopping it, if there is no friction we
1
could not move and grip objects. Without the presence of friction rolling mills could not
operate, most threaded joints would not hold, friction welding would not exist neither the
sound of the violin nor the squeal sound of brake [3].
In moving machinery friction is responsible for dissipation and loss of much
energy. For example, it has been estimated that 10% of oil consumption in the United States
used simply to overcome friction. The energy loss caused by friction requires an energy input
in order to maintain the sliding motion. The energy dissipated from the system is primarily in
the form of heat which may have to be removed by cooling to avoid the damage of
machinery. Not all of the energy will dissipate as heat but some of the energy dissipates in
the form of various deformation processes, which results in the wear of the material where the
contact has been occurred and resulting in their eventual degradation of point where
replacement of whole component may be essential [3].
The fundamental experimental laws that govern friction of solid bodies are quite
simple and are usually named after Coulomb, who formulated them in 1875 (much of this
work was built on earlier work bye Leonardo da Vinci and Amontons). The laws stated by
Coulomb are in very general terms [3]:
• Static friction may be greater than kinetic or dynamic friction
• Friction force is proportional to applied load
• Friction is independent of sliding velocity
• Friction force is independent of contact area
Even though these are very simple and applicable in many instances; there are also numerous
conditions under which they may break. Friction is commonly represented by friction
coefficient (µ). The friction coefficient is a dimensionless scalar value which is the ratio
between the friction force, F, and the load, N. The frictional force is always normal to the
applied load or force [3].
Coefficient of friction µ= F/N
The friction coefficient typically ranges from 0.03 for a very well lubricated bearing, to 0.5 to
0.7 for dry sliding and even ≥5 for clean metal surface in vacuum. The coefficient of friction
depends on whether the objects are initially moving or stationary and on the types of materials
involved. For flat surfaces the normal force is equal to the weight of the object, for inclined
surfaces only a fraction of the object’s weight pushes directly into the surface, so the normal
force is less than the object’s weight. Different kinds of relative motion between objects give
rise to different types of friction between them which are [3]:
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• Static friction
• Sliding or kinetic friction
• Rolling friction and
• Fluid friction
Static friction occurs between stationary objects. The coefficient of friction for
two materials may differ depending on the type of friction involved. Static friction prevents an
object from moving relative another surface. It is the force that keeps an object from sliding
off on a surface, even when the surface is slightly tilted. The static friction is time dependent,
the length of the rest time will affect the static friction. It can either increase or decrease with
rest time. In order to move something, you must first overcome the force of static friction
between the object and surface on which it is resting. This force depends on the coefficient of
static friction between the object, surface and the normal force of the object (µs) [4].
An object sliding on a surface or brakes slowing down the wheel are both
examples of sliding or kinetic friction. Sliding friction acts in the direction opposite to the
direction of motion. When sliding friction is acting another force must be present to keep an
object in motion. In the case of object sliding over a surface, this force is gravity. The force of
sliding or kinetic friction depends upon the coefficient of kinetic friction between the object
and the surface on which it is moving (µk) [4].
Rolling friction hinders the motion of an object rolling along a surface. Rolling
friction slows down a ball rolling on a surface, and it slows down the motion of tire rolling
along the ground. Rolling friction is caused by energy dissipation inside the material, also
called hysteresis. The coefficient of rolling friction is 1/100 that of sliding friction [4].
Objects moving through a fluid experiences fluid friction. It acts between the
object and fluid and hinders the motion of the object. The force of fluid friction depends upon
the object´s shape, material, speed and as well as the fluid´s viscosity [4].
3. Wear
The second part of tribology, wear, can be defined as the loss of material from a tribological
surface. However, this does not mean that material is lost from the tribo–system since
material can be transferred from one surface to another. In most cases wear is detrimental for
a system and will reduce its efficiency or even lead to complete failure. Wear, just like
friction, is not a material property, it is a system response. Wear can be reduced by proper
selection of materials, lubricants and operating conditions. In some systems, there can be
components that are designed to wear (brake pads). There are several different wear
3
mechanisms that can occur either alone, more commonly, and simultaneously. Examples of
wear mechanisms are [5]:
• Adhesive wear
• Abrasive wear
• Fretting wear
• Surface fatigue and
• Tribochemical or corrosive wear
These are not distinct mechanisms, but rather combinations of the adhesive, chemical and
abrasive forms of wear. Most of the industrial wear situations occur because of adhesive and
abrasive wear mechanisms. Wear by all mechanisms, except by fatigue mechanism, cause
gradual removal of material.
As the sliding continues, the transferred fragments may come off the surface to which they are
transferred and be transferred back to the original surface, or be ejected as loose wear
particles. The formation of loose particle often results from chemical changes in the fragment.
The fragments have large surface area and tend to oxidised readily, which reduces adhesive
strength, and readily break loose. In some cases the formation of loose particles involves the
residual elastic energy of adherent fragments [1].
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3.2 Abrasive wear
Abrasive wear occurs when asperities of a rough, hard surface or hard particles slide on a
softer surface and damage the interface by plastic deformation or fracture. In the case of
ductile materials with high fracture toughness, hard particles or hard asperities results in
plastic flow of softer material. In the case of brittle materials, wear occurs by brittle fracture.
In these cases the worn zone consists of significant cracking [1]. The rate at which the surface
abrades depends on the characteristics of material surface, presence of abrasive particles, the
speed and other environmental conditions. Abrasion is typically categorized according to
types of contact, as well as contact environment. Types of contacts include two-body and
three-body wear. The former occurs when an abrasive slides along a surface, and the later,
when an abrasive is caught between one surface and another [3]. Fig 2 shows the schematic
representation of two body and three body wear mechanisms.
Several mechanisms have been proposed to explain how material is removed from a surface
during abrasion. These mechanisms include fracture, fatigue and melting. Because of the
complexity of abrasion, no mechanism completely accounts for all the loss. Fig 3 depicts
some of the processes that are possible when a single abrasive tip transverses a surface. They
include plowing, wedge formation, cutting, microfatigue and micro cracking [3].
5
Plowing is the process of displacing material from a groove to the sides. This occurs under
light loads and does not result in any real material loss. When the ratio of shear strength of the
contact interface relative to the shear strength of the bulk rises to a high level, it has been
observed that a wedge can develop on the front of abrasive tip. The most severe form of wear
for ductile material is cutting. During cutting process the abrasive tip removes a chip, results
in the removal of material [3].
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when fretting wear is takes place between two flat surfaces or cylindrical surfaces, the
progress with time can be observed in three stages
• In the initial stage when metal-to-metal contact will occur which results in local welding,
roughening of the surface, high friction and low contact resistance. If the movement is
cyclic, fatigue cracks are initiated in this stage.
• In the second stage, reduction of the coefficient of friction will occur because of the
formation of beds of compacted oxide.
• Onset of steady state in which the friction is more or less constant and the contacting
resistance is generally high with occasional momentary falls to a low value.
Fretting wear can be controlled or prevented by improved design, surface finish, coatings,
inserts and lubrication [3].
7
friction and chemical reaction can result in total material losses that are much greater than the
additive process taken alone [1].
In the absence of sliding, the chemical products forms a protective layer of less than a
micrometer thick on the surface, which would tend to slow down or even arrest the corrosion,
but the sliding action wears the chemical film away, so that the chemical attack continues [1].
4. Lubrication
Finally, the third part of tribology is lubrication, a method to reduce friction and wear between
two moving surfaces. This is achieved by introducing an easily sheared material (liquid, solid
or gas) between two surfaces. These sheared materials are called lubricants, reduces friction
and wear at the interface and carry away the heat and debris generated during the sliding
process. Depending on the lubricant film thickness, the interfacial height and the degree of
geometric conformity, different lubrication regimes can be distinguished [1]. The lubrication
regime is usually determined by using Stribeck curve which is shown schematically in Fig 4.
There are three lubrication regimes; boundary lubrication (BL) where the load is carried by
the asperities and friction is governed by the surface films that are formed. In mixed
lubrication (ML) a hydrodynamic pressure starts to build up and the load is partially carried
out by the oil film. In full film lubrication (FL) the two surfaces are completely separated and
the entire load is carried by the lubricant film [5].
As previously mentioned, lubricants may be in the form of liquid, solid and
gaseous. The choice of an appropriate lubricant depends on system needs, cost, safety and
environmental conditions. Minimizing the number of lubricants used generally reduces the
8
maintenance cost. Liquid lubricants contain different additives which are added to the base oil
to improve certain properties such as load carrying capacity, viscosity or oxidation behaviour.
The lubricant can also be solid material with a lamellar structure that allows easy shearing
(graphite, molybdenum disulphide or boric acid). Today’s advanced engineering technologies
allow for preparation of multilayer surface coatings with built in layer with friction reducing
properties [5].
5. High temperature Tribology
High temperature tribological studies (typically above 300 ºC) play an important role in the
technological applications where the components operate at elevated temperatures. Examples
of such applications can be found in aerospace, power generation and metal working
industries. In such applications, lubrication by conventional means (liquid lubricants) is not
possible because of the rapid decomposition and deterioration of the lubricants. To overcome
these problems, solid lubricants are used which reduce the friction and wear. The behaviour of
all tribochemical layers will not have same effect; it will depend on their properties. As in the
case with the most other metals, steels are thermodynamically unstable in air, and form oxide
layers which may protect or adversely affect the surfaces depending upon the nature of oxides
formed.
Alloying elements play important role in the formation of oxide layers.
Fontalvo et al. [6] studied the effect of aluminium and silicon on the friction and wear
behaviour of hot work steel. They concluded that the aluminium and silicon yield a reduction
of oxide film thickness thus lead to an increase in wear as temperature is increased.
Tribological behaviour at elevated temperatures in reciprocating sliding
condition was investigated by Glascott et al. [7]. They concluded that at 300 ºC the oxide
layers are brittle, resulting in higher friction and wear. Oxide layers at 600 ºC are smooth and
protecting the surface, resulting in lower friction and wear.
Stott et al. [8] studied the effect of load and hardness on friction and wear
behaviour of different dissimilar combinations of pin and disc specimens in reciprocating
sliding condition at 500 – 600 ºC and revealed that the temperature and load will have
significant effect on the tribological behaviour of material. At lower loads, the protective
layers are able to sustain longer durations than at higher loads. In high speed steel and carbon
steel combinations at 500 ºC, the wear mechanism is abrasion of the pin as hard oxide debris
were observed. Loose debris cannot be retained in between the contacting surfaces and
formed shallow grooves and cause high wear. But in the case of soft material (high- chrome
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steel) wear grooves are deeper and facilitated the entrapment of wear debris leading to
development of wear protective glaze.
Table 1 shows the commonly used height parameters. The typical amplitudes between the
peaks and valleys for engineering surfaces are about one micrometer. Almost every known
surface, apart from the cleaved faces of mica, is rough. Height characteristics are commonly
described by parameters such as centre - line average or roughness average (CLA or Ra), root
means square roughness (RMS or Rq), mean value of the maximum peak - to - valley height
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(Rtm), ten - point height (Rz) and many others. In engineering practice, however, the most
commonly used parameter is the roughness average [9].
7. Surface treatments
Surface treatments of materials become a vital factor for improving the properties of a
component, and/or extending its lifetime. Surface treated materials can have one or several
functions. For example, the application of paint can have both an anticorrosion and decorative
effect. The surface treatments are widely used for the ferrous based materials. The process of
surface treatments tailors the surface of engineering materials to
• Control friction and wear
• Improve corrosion resistance
• Change physical properties (e.g. conductivity, resistivity and reflection)
• Vary appearance
• Reduce cost.
Surface treatment processes may be classified into two main categories, microstructural
treatments and diffusion treatments.
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beam milling are the most prominent for tribological applications. Other techniques which are
also used include chromizing, aluminizing, siliconizing and shearardizing [10].
7.3 Nitriding
Among all of the other surface treatments methods which are applied to improving the
tribological properties, nitriding is one of the most commonly used methods applied for steel
and its alloys, especially for tool steel to improve the hardness and surface wear resistance at
elevated temperatures. Nitriding treatments are ferritic surface hardening heat treatment that
introduces nitrogen atoms into the surface of metal at a temperature range of 500 to 590 ºC
where the metal is in ferritic phase. The nitrogen is introduced in the surface of the steel by
reaction with a solid phase, gas or plasma containing nitrogen. The processing time is rather
long (100 hours at 500 ºC to obtain a depth of 0.5 mm) when compared to carburizing. This
process does not need quenching which minimise the distortion and a good surface finish is
possible. Nitrogen is most effective when the steel contains Al, Cr, Mo, V, and M, these
elements from stable nitrides. All hardenable steels must be hardened and tempered before
being nitrided. Process methods for nitriding are
• Gas (box furnace)
• Liquid
• Nitro carburizing and
• Plasma nitriding.
Gas nitriding is a case hardening process in which nitrogen is introduced into
the surface by exposing it to the nitrogenous gas, mostly Ammonia at particular temperature
(quenching is not required).
Liquid nitriding (salt bath) is a generic term for number of different salt
processes. It is a subcritical case hardening process which contains either cyanides or
cyanates. The metal is immersed in salt bath at a subcritical temperature. The surface
properties may vary with the chemical control and the process used.
Plasma (ion) nitriding is an extension of conventional nitriding process in
combination with plasma. Fig 5 shows the schematic representation of ion - electron
discharged mechanism. It is a low temperature and low distortion surface treatment process.
This process is performed in vacuum, where a high electrical energy is used to form plasma.
The furnace will act as an Anode and the specimen will act as Cathode. The high energy
current mainly consists of two factors, the negatively charged ions move towards the anode
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and positively charged ions will move towards the cathode. The nitrogen atoms are positively
charged and accelerated towards the negative electrode and hit the surface with a high kinetic
energy due to which the specimens are heated to high temperature and the nitrogen ions
diffuse easily in to the surface and form the compound as Fe2N or Fe4N.
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II.Objectives
The main objectives of this thesis are
¾ To experimentally investigate the friction and wear behaviour of different tool steels
during sliding against high strength boron steels at room temperature and at high
temperature.
¾ To understand the various mechanisms involved in the friction and wear process of
tool steels and high strength boron steel.
¾ To study the plasma nitrided and post oxidised samples at different temperatures.
The improved knowledge of high temperature tribological behaviour of these materials
will enable in proper selection of materials and surface treatments.
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III. Experimental approach
The experimental work performed in this thesis has been carried out by using standard
tribological test equipments. It is a systematic approach to investigate the different steel
specimen performance against high strength boron steel at room and high temperatures.
1. Experimental materials
The studies presented in this thesis involved three different compositions of tool steels.
1. Tool steel 1 (TS 1)
2. Tool steel 2 (TS 2)
3. Tool steel 3 (TS 3)
The tool steels specimens have been studied in this thesis work are in nitrided and post
oxidised condition. Tool steel 1 and tool steel 2 were post oxidised at 500 ºC whereas, tool
steel 3 was post oxidised three different temperatures i.e. post oxidation 1 at 500 ºC, post
oxidation 2 at 520 ºC and post oxidation 3 at 480 ºC respectively.
The high strength boron steel is a commercially available material and it was
hardened through quenching and the surface was then ground and polished to a low surface
roughness. The chemical composition of both the tool steel specimens and boron steel disc are
presented in Table 2.
Table 2. Compositions (wt %) of the materials employed in these studies
Material C Mn Cr Si B P S Ni Mo V
1.0 - 0.14 - 0.2 -
Boron steel 0.25.0.25 1.3 0.26 0.35 0.005 > 0.03 >0.01
- - -
15
different temperatures with a view to obtain different friction and properties. The post-
oxidation was a part of the plasma nitriding process.
The upper specimens are the tool steel specimens of pin shape (diameter 10 mm
x 10 mm long) with one end spherical and the lower specimen is flat disc made from high
strength boron steels (diameter 24 mm x 7.9 mm thickness). See Fig 6.
3. Experimental equipment
3.1 Pin on disc machine
The TE-67 Pin on disc machine consist of a pin carrier assembly and disc carrier assembly is
held fixed by the base frame in order to maintain the alignment between the specimens to
enable usage of flat-on-flat geometry. Fig 7 shows the Pin on disc machine set up for room
temperature and high temperature. The test disc is secured by a central bolt on to the disc
carries spindle. The spindle is driven through a pulley belt by the D.C. motor beneath the
machine. The motor has tachogenerator feed back to ensure stable running speeds. The speed
range can be changed by adjusting the wear track radius the test. The scale rule is used to set
the radius to the middle of the pin.
The pin specimen has 8 mm mounting diameter so that it can be clamped in the
collet chuck. The pin assembly is pivoted to the frame so that it will move up and down. The
strain gauge transducer mounted at the rear end of the pin carrier head measures the friction
force exerted on the pin during the rotation. Two types of force transducers are available, for
low load 5 kg and for high loads 100 kg.
16
(a) (b)
Fig 7. Pin on disc machine setup. (a) Room temperature. (b) High temperature
The standard configuration allows test at room temperature. Temperature is measured using a
simple trailing thermocouple running on the disc surface. For high temperature (max 400 ºC)
applications an external air blower is used. At high temperatures the trailing thermo couple
and optical pyrometer are used to record temperature. The pneumatic load actuator can handle
steady and fluctuating loads with sine or triangular shaped waves. A linear potentiometer
measures the movement of the pin piston and can provide in- situ wear measurements. Both
dry and lubricated situations are possible. For the lubricated situation there is an enclosure to
submerge the disc, which features two electrical resistance heating elements to control
temperature. Table 3 refers to the technical specifications of pin on disc machine.
Table 3. Technical specification of Pin on disc machine
Technical specifications of Wyko 1100 NT optical profiler are shown in table 4. The Wyko
1100 NT optical profiler uses interferometry to measure a surface. It has two main features,
Vertical Scanning Interferometry (VSI) and Phase Shifting Interferometry (PSI). In VSI
mode, it utilizes the white light interferometry which is a bright and dark. The bright pattern
originates from the smooth reference surface and the dark pattern from the test specimen. The
17
pattern will be photographed by a CCD camera and transferred to the computer. The PSI
mode is similar to the VSI but, it uses filtered light and the reference surface is translated
instead of the objective. It also uses the difference in intensity instead of fringes for height
data acquisition. The acquired data can be generated as a 2D and 3D mode for analysis.
Table 4. Technical specifications of Wyko 1100 NT optical profiler
18
electron imaging) and SEM images are much easier to interpret than Transmission Electron
Microscope (TEM) images.
Energy Dispersive Spectroscopy (EDS) is a technique used to qualitative
elemental analysis or chemical composition of a sample. The generation of X-rays due to
bombardment of electrons on to the sample are used for EDS. The X- rays are detected by the
EDS detector and sent to analysis. However some limitations are considered such as detection
of light elements, the detector should be kept at 77K all the time to reduce the noise in the
system.
The JSM 6460 is a low vacuum (1-270 Pa range) SEM with a conventional
tungsten filament electron source that is equipped for both imaging and micro analysis in low
vacuum and high vacuum. In high vacuum mode, SEM capable of giving secondary electron
images of resolution up to 3nm at the maximum acceleration voltage (30 Kv). The tungsten
filament will produce a strong extremely stable electron source with high beam current for
back scattered imaging. The magnification ranges from 5 to 300000 X and the accelerating
voltage ranges from 0-30Kv.
The microscope is equipped with Energy Dispersive Spectrometer (EDS)
capable of chemical analysis with a detectable range of Carbon (C) – Uranium (U). An
Electron Back- Scattered Diffraction (EBSD) camera is also available with mapping software
that can provide crystallographic information such as pole figures, grain boundary orientation
and crystal orientation.
19
λ- Wavelength of the X-rays
d - The spacing of the layers
θ- The incident angle of the photo
4. Test parameters
The test parameters for all the experiments are for constant sliding distance. The wear track
radius and rotational speed is different for the samples. Tests at room temperature and high
temperature (400 ºC) are carried out with constant load of 4.905 N. The test parameters for
tests at room temperature and high temperature are shown in table 5 and table 6 respectively.
20
Note: High temperature tests are performed at 400 ºC with 4.905 N loads. Two tests are
performed on each disc with different wear track radius , speed and time with two different
specimens of same composition.
Table5. Test parameters for tests at room temperature
TS 3 (Post oxidation at 500 ºC) 16 and 22 104 and 76 1211 and 1205
TS 3 (Post oxidation at 480 ºC) 16 and 22 104 and 76 1211 and 1205
TS3 (Post oxidation at 520 ºC) 16 and 22 104 and 76 1211 and 1205
5. Test procedure
We studied the tribological properties of five different tool steel specimens sliding against a
high strength boron steel disc. The tests are performed by standard test equipments at room
temperature and at high temperature (400 ºC) with dry friction (in the absence of lubrication).
All the test specimens’ surfaces are characterized by Wyko NT 1100 Topometer and the
topographical properties are measured. The phases present in the tool steel specimens are
measured with X-ray diffraction. Test procedure employed in this thesis work mainly consists
of four steps, cleaning, weighing, testing and surface analysis.
21
The test specimens and holders were cleaned using ultrasonic cleaner in petroleum spirit and
the specimens were then rinsed with ethanol in order to remove all contaminants. All test
specimens are then weighed by using a semi- microelectronic weighing balance. All samples
are weighed three times to reduce the errors and the average value is considered as final value.
For tests at room temperature the pin on disc machine is calibrated and suitable parameters
(speed and time) are calculated for each test, all tests are performed with constant sliding
distance and with a load of 4.905 N.
After completion of each test, the test specimens are cleaned again and weighed
to determine the weight gained or loss to the specimens and to calculate the volume loss of
specimens. The surface morphology is studied by SEM and Topometer and the chemical
composition of pin specimens and disc wear scars (after the test) are studied with the help of
EDS.
For high temperature tests, the test parameters have been listed in Table 6. In
high temperature tests (see Fig 10), first the heating sequence will run where the lower test
specimen (Boron steel disc) will be heated to 400 ºC with the help of an external blower and
the temperature is measured with the help of thermo couple and optical pyrometer. As the disc
specimen reached to the desired temperature, the pin specimen will be brought in to contact
immediately, loaded against the disc and the test was started. Upon completion of test the
specimens are allowed to cool to room temperature and the same cleaning, weighing and
surface analysis are performed as mentioned above.
For the second test at high temperature the same discs which have been used for the first high
temperature test are used with the same specimen geometry but with different wear track
radius (22 mm). After completion of the test the same cleaning, weighing and surface analysis
are performed.
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IV. Results and discussion
1. Surface characteristics of the unworn specimens
All the test samples surface characterization was done by topometer. The untreated disc
specimen (high strength boron steel) surface roughness was measured and ranges from 0.35 to
0.46 µm and for the tool steel pin specimens ranges from 0.65 to 1.35 µm. All the tests are
carried out with similar roughness values for all pin specimens. Fig 11 shows the surface
topography of disc and pin samples. Tool steel specimens curvature and tilt effects are
eliminated by using algorithm with the help of software in order to get good surface
characterization results.
(a)
(b)
23
(c)
(d)
(e)
24
(f)
Fig11. Surface topography of samples (a) Disc (b) Tool steel 1 (c) Tool steel 2 (d) Tool steel 3 Post
oxidation 1(e) Tool steel 3 Post oxidation 2 (f) Tool steel 3 Post oxidation 3.
The tool steel specimens are tested with the help of X-ray diffraction in order to know the
different phases present in the specimens. The results shown that different quantity of
oxide formation elements are present in all tool steel specimens which are post oxidised at
different temperatures. Fig 12 shows X-rd spectra of tool steel 3 which is post oxidised at
different temperatures.
(a)
25
(b)
(c)
26
(d)
(e)
Fig 12. X-rd spectra for tool steel specimens (a) Tool steel 1 post oxidation 1 (b) Tool steel 2 post oxidation
1 (c) Tool steel 3 post oxidation 1(d) Tool steel 3 post oxidation 2 (e) Tool steel 3 post oxidation 3
27
2. Hardness measurements
The surface hardness of boron steel disc and tool steel pin specimens also play an important
role in the friction results, wear mechanisms and amount of wear. Table 7 refers to the
hardness measurements of test samples. The measured hardness values are different for all the
specimens.
Table 7. Vickers Hardness measurements of test samples
Note: Hardness values are the average values for all the specimens at 25 grams load.
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3. Friction results
3.1 Frictional behaviour at room temperature
In our studies at room temperature the friction coefficient of pairs has been measured for
constant rotational distance (211.1 m). Constant sliding distance was maintained by varying
the speed, wear track radius and the rotating time of disc.
Fig13. Friction coefficient of tool steel 3 - post oxidation 1, 2 and 3 sliding against high strength boron steel
disc at room temperature
The results have shown that the coefficient of friction for tool steel 3 post oxidation at 500 ºC
is lower, post oxidation at 520 ºC is moderate and post oxidation at 480 ºC is higher. The
initial frictional behaviour for post oxidation 1 is different when compared to post oxidation 2
and 3 but the friction behaviour is similar and steady (refer Fig 13). The higher friction
coefficient in the beginning of the test is because of the hardness differences of three samples.
From X-ray diffraction it has been shown that different amount of iron oxide
(Fe3O4) is present in the three samples. In post oxidation 1, it is higher; in post oxidation 2
moderate and in post oxidation 3 the least. These results correlate to the friction coefficient, as
higher amount of iron oxides on the tool steel surface will reduce the adhesion and provide a
lower coefficient of friction. The flash temperature in between the pin and disc specimens is
enough to produce the compact oxide layers which reduce friction.
29
Fig 14. Friction coefficient of tool steel 1 and tool steel 2 - post oxidation 1 sliding against high strength
boron steel disc at room temperature
Fig 14 shows the friction coefficient for tool steel 1 and tool steel 2 post oxidised at 500 ºC.
From the results it can be observed that the initial friction is higher and similar, this may be
due to the hardness difference in the specimens when compared to the tool steel 3 post
oxidation 1 specimen. The frictional behaviour is similar for tool steel 1 and 2 and the test
results show higher and unsteady friction coefficient. X-ray diffraction shows lower amount
of iron oxides forming elements when compared to tool steel 3 samples, which cause higher
friction due to the less oxides on tool steel specimens. The unsteady and higher frictional
behaviour may be attributed to the fact that more force was needed for plastic deformation of
the steel disc
The friction coefficient and wear mechanisms are different for both tool steel 3
post oxidation 1, 2, 3 and tool steel 1 & tool steel 2 post oxidation 1. Tool steel 3 has lower
friction and less wear compared to the tool steel 1 and tool steel 2. Tool steel 3 shows initially
higher and end up with steady state friction where as the tool steel 1 and tool steel 2 shows
higher friction initially but has a more unsteady behaviour. The main reason for this behaviour
is the presence of less oxide compact layers during the test in both tool steel 1 and tool steel 2.
The presence of more wear debris in tool steel 1 and tool steel 2 will also leads to higher wear
of pin and disc.
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3.2 Frictional behaviour at 400 ºC
In our studies, we conducted high temperature test with tool steel 3 at different wear track
radius on different disc specimens for each set. The test parameters are presented in table 8. In
first set, the test was conducted at 16 mm wear track radius and the second test was conducted
at 22 mm wear track radius on the same disc as in the first test. Table 8 shows the test
combinations of specimens and table 6 shows the test sequence at 400 ºC.
Table 8. High temperature test combinations
Disc specimen Test 1, Wear track radius Test 2, Wear track radius
Disc 1 Post oxidation -1, 16 mm Post oxidation -1, 22 mm
Fig15. Friction coefficient of tool steel 3 - post oxidation 1, 2 and 3 at 400 ºC sliding against high strength
boron steel disc at 16 mm radius
As seen, post oxidation 1 has moderate friction coefficient where as post oxidation 2 and 3
has higher and lower friction coefficient respectively. Due to the high temperature the wear
debris will get oxidised which will cause increase or decrease in frictional behaviour. The
frictional behaviour is similar in all the cases which is gradually increasing and reaches to
31
steady state in the end. The difference in the friction coefficient is because of the hardness
difference of the pin samples, post oxidation 1 has moderate and post oxidation 2 and 3 has
higher and lower hardness.
Table 9. Weight % of elements present on tool steel 3aftert test at 400 °C and 16 mm wear track radius
From EDS spectra, the oxygen concentration is different for all the three samples wear scars
which lead to different friction coefficient values by the formation of oxide layers. Table 9
shows the weight % of elements present on tool steel 3 after test. The oxygen concentration is
negligible in both tool steel 3 post oxidation 2 and 3 when compared to post oxidation 1
Higher the oxides lower the friction and vice versa. The high friction coefficient may be the
cause of specimen geometry since the harder, spherical shaped pin will indent the softer disc
it may cause a lot of ploughing. If we reverse the geometry (pin specimen from high strength
boron steel and disc specimen from tool steel) we may get similar friction coefficient as at
room temperature.
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3.4 Friction results using 22 mm wear track radius
The second test was conducted on the same disc with different wear track radius. Before the
test, hardness measurements are done for all the disc specimens and observed drastic decrease
in the hardness to 485 HV. This is due to the heating and cooling effect during first test
which may changes the microstructure of the disc.
Fig16. Friction coefficient of tool steel 3 - post oxidation 1, 2 and 3 at 400 ºC sliding against high strength
boron steel disc at 22 mm radius
From the second test we can observe that there is a reduction in the friction coefficient and the
frictional behaviour is similar for all the three samples. Fig 16 shows the friction coefficient
of tool steel 3 post oxidation 1, 2 and 3. There is no frictional gradient between them and the
initial friction is also same. This is because of decrease in the hardness of the disc specimen.
There is much time to form thicker oxide layers which will have significant effect on the
frictional behaviour. The higher hardness pin specimen can penetrate into the softer disc
specimen and causes higher material removal from the disc rather than from the pin. The
deformation depends on mechanical properties such as young’s modulus, hardness and the
real contact conditions. From EDS analysis the amount of oxygen present on the disc wear
scar is same for all the three samples which cause similar frictional behaviour and frictional
coefficient.
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4. Wear results
4.1 Wear loss and surface damage of specimens at room temperature
Our studies have shown some interesting wear results of both tool steel and boron steel
specimens. Fig 17 shows the wear loss of disc and pin specimens of different tool steels. From
Fig 17 (a), tool steel 3 post oxidation 1 (500 ºC) wear loss is negligible compared to other two
and the respective disc wear loss is also lower. This is mainly due to the formation of oxide
layers.
(a)
(b)
Fig 17. Pin and disc volume wear loss (a) Tool steel 3 at room temperature (b) Tool steel 1 and 2
34
Fig 17 (b) shows wear loss of tool steel 1 and 2, higher volume loss of pin specimens and
lower volume loss of disc. The main reason behind it is the formation of fewer oxides during
the test which causes higher friction and wear and leads to severe adhesion.
Wear scars of pin specimens and disc specimens have been studied by
SEM/EDS and topometer for both room temperature and high temperature tests to get more
information about the amount of wear and the wear mechanism generated by sliding.
35
adhesive; the deep grooves are because of the presence of wear debris in the process which
results increase in the friction.
From Fig 18 (c), the post oxidation 3 sample will have higher wear rate when compared to the
other two tool steel 3 samples. The frictional and wear behaviour of this material shows
similar behaviour as the other two. The higher friction results because of the less compact
oxide layers and the deeper grooves on disc wear scar reveals the higher volume loss due to
interaction with wear debris during the sliding process. The steady state friction is caused by
the debris particles getting embedded in the grooves and there is no damage to the samples.
From EDS and SEM, the wear scars show low oxygen concentration. The
material adhering to tool steel reveals the change in chemical composition and the presence of
boron steel elements on to the pin sample is the evidence of material transfer form disc to pin
specimens. Table 10 shows the Weight % of elements present in tool steel 3 after test, from
which it is clear that oxygen concentration is different for all the three specimens.
Table 10. Weight % of elements present in tool steel 3 specimens at room temperature (after test)
Si - 0.43 0.38
C 4.28 1.64 0.50
Cr 1.19 5.10 5.31
Fe 87.68 86.33 93.06
From SEM images it is revealed that the wear mechanisms are different for three samples.
There is no specific wear on disc with tool steel 3 post oxidation 1 and the material is
adhering on to the tool steel pin specimen. The other two samples behaviour is also similar
but the disc volume loss is higher when compared to post oxidation 1.
Fig 19 shows the wear scars of tool steel 1, tool steel 2 and the respective boron
steel wear scars. The frictional behaviour and wear characteristics of these two materials are
different from tool steel 3. From the SEM images, clear evidence of the absence of material
transportation from boron steel disc to tool steel specimen. The wear mechanism is similar to
the tool steel 3 and the wider wear scars reveals the higher volume loss from the both tool
steel and boron steel specimens. The high friction obtained during room temperature test may
be attributed to the occurrence of severe adhesion which can be ascertained from the SEM
micrographs.
36
(a) (b)
Fig 19. SEM images of wear scars of pin (top) and disc (bottom) specimens
(a) Tool steel 1 (b) Tool steel 2
The image shows the longer and deeper grooves explaining the plastic deformation of
material and governing wear mechanism which appears to be mainly adhesive accompanied
by some abrading action of oxidised wear debris causing higher material removal. From XRD
and EDS, it shows the negligible amount of oxide forming elements on tool steel and the more
amounts of harder nitrided elements. Table 11 shows the weight % of elements present in tool
steel 1 and 2. The harder nitrided wear debris causes the higher friction coefficient and
unsteadiness in the behaviour which results in more material removal from disc rather than
from pin. When the nitrided layer was removed from the tool steel the softer pin material will
be in contact with the disc and causes the higher material removal from both pin and disc.
Table 11. Weight % of elements present in tool steel 1 and 2 at room temperature test (after test)
Si 0.22 0.57
C 0.65 1.49
Cr 1.87 1.39
Fe 96.06 95.68
37
From the SEM images we can observe clear and wider wear scars, higher volume loss of both
pin and disc specimens and more wear debris in these two tests which may cause the higher
and unsteadiness in the friction coefficient. The pin and disc SEM images clearly shows the
adhesive wear scars and deeper grooves of material removal on the disc.
Fig 20. Pin and Disc volume wear loss of tool steel 3 at 400 ºC
In order to compare the tests at room temperature and the tests at high temperature, two high
temperature tests are carried out with similar tool steels specimen of tool steel 3 on the same
disc with different wear track radius. First test was at 16 mm radius and second test was at 22
mm radius.
In tribological tests at elevated temperatures, the oxidation of test specimen
plays an important role to determining their friction and wear characteristics. The governing
wear mechanism is a combination of abrasion and adhesion and we can observe the change in
wear of the pin specimens, which is negligible at room temperature and remarkable at high
38
temperature. There are several ways that these oxides or oxide wear debris can influence the
wear behaviour. The higher wear is because the wear debris may be removed or retained in
the contact and form protective layers. The oxides can also act as third bodies and get
embedded and causes increasing wear with increasing in temperature.
The increase in friction towards the end of test and increase in wear of tool
steel is may be attributed to increasing the contact area and softening of the material.
Increasing wear with temperature has also been reported by Hardell et al. [12] and Wang et
al. [13] as a result of increased abrasive wear due to softening of the specimen thus
providing in sufficient support for the oxide layers to be formed. From SEM images, see Fig
21, the tool steel material is adhered to boron disc and the wear behaviour is different for all
the three.
Fig 21. SEM images of wear scars for tool steel 3 Pin (top) and boron steel disc at 400 º C at 16 mm wear
track radius
39
V. Conclusions
Experimental studies pertaining to the friction and wear behaviour of different tool steels
sliding against high strength boron steel have been carried out at room temperature and at
elevated temperatures (400 ºC). The experiments were carried out in ambient air without any
lubricants and the salient conclusions are as follows:
• At room temperature, the friction characteristics of tool steel 1 and 2 are different from
tool steel 3. Tool steel 1 and 2 have shown higher and more unsteady friction where as
tool steel 3 shows lower friction with a steadier behaviour. Different post oxidation
temperatures produces different amount of oxides, post oxidation 1(500 ºC) was
highest, post oxidation 2 (520 ºC) was moderate and post oxidation 3 (480 ºC) was
lowest. These oxides result in decreasing the friction and wear.
• At 400 0C, tribological properties are strongly influenced by the temperature and the
friction was higher and gradually increased. The hardness of tool steel 3 materials
have significant effect on the initial friction behaviour which influences the final
friction. The three post oxidation samples have similar frictional behaviour but
different wear rates. Wear increases from post oxidation 1 to 3 and the boron steel
wear loss is less when compared to tool steel due to the softening of the tool steel
specimens.
• The wear behaviour observed is mainly adhesive at room temperature and abrasive
and adhesive at higher temperature. There is hardly any wear of tool steel 3 post
oxidation 1 at room temperature.
• Tool steel 3 with post oxidation 1 has shown to have lower friction and wear
compared to the other investigated tool steel variants both at room temperatures and
high temperatures.
40
VI. Future work
Future work on tool steel 1, 2 and 3 should focus on the following aspects:
• For tool steel 3, varying the post oxidation temperature and time to find an
optimum combination of iron oxides and iron nitrides.
• For tool steel 1 and 2, experiments should carried out with post oxidation 2 and 3
and investigate the tribological properties.
• Experiments should be performed at elevated temperatures by reversing the
specimen geometry to investigate the tribological properties and compared them
with the present work.
• Experiments should be carried out by changing the heat treatment process time and
post oxidation process condition.
41
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