Sarath Krishna e Seminar 1

Seminar Report on
EFFECT OF HOT ROLLING IN TRIBOLOGICAL

BEHAVIOUR OF SHAPE MEMORY ALLOYS
Submitted by
SARATH KRISHNA E. (NCE18ME044)
in partial fulfillment of the requirements for the award of the degree
of BACHELOR OF TECHNOLOGY in Mechanical Engineering
Guide
Ms. ASWATHY V.G.

Assistant Professor
Department of Mechanical Engineering
DEPARTMENT OF MECHANICAL ENGINEERING

NEHRU COLLEGE OF ENGINEERING AND RESEARCH CENTRE
THRISSUR–680597
JANUARY 2022
DEPARTMENT OF MECHANICAL ENGINEERING
NEHRU COLLEGE OF ENGINEERING AND RESEARCH CENTRE
THRISSUR–680597
Certificate
This is to certify that this report entitled “EFFECT OF HOT ROLLING IN TRIBOLOGICAL
BEHAVIOUR OF SHAPE MEMORY ALLOYS” is a bonafide record of the seminar presented
by SARATH KRISHNA E. (NCE18ME044) towards the partial fulfillment for the award of Degree
of Bachelor of Technology in Mechanical Engineering under APJ Abdul Kalam Technological
University, Kerala, during the year 2022.
Guided By Head of the Department
Ms. Aswathy V.G. Prof. Dr. George Job K

(Assistant Professor) (Professor)
Dept. of Mechanical Dept. of Mechanical
Engineering Engineering
ACKNOWLEDGMENT
It is a great pleasure for me to acknowledge all those who have advised and supported me to lead
my seminar to success. First of all, I would like to thank GOD Almighty for blessing me with his
grace and taking me Endeavor to successful culmination. I submit this seminar work at the lotus
feet of beloved chairman, Late Dr. P. K. Das, founder chairman, Nehru Group of Institutions and
seek his blessings. I am extremely thankful to most respected Adv. Dr. P. Krishnadas, Chairman
and Managing Trustee, and Dr. P. Krishnakumar, CEO and secretary of Nehru Group of
Institution for all helps extended to me. I am very grateful to Dr. Ambikadevi Amma T, Principal
of our institute for her valuable advice, kind encouragement, creative suggestions and supports for
the completion of this seminar work. Next, I would like to show my sincere gratitude to
Prof. Dr. George Job K, Head of the Department of Mechanical Engineering, who helped me in
every possible way. I would like express my sincere heartfelt thanks to my seminar coordinator
Prof. Dr. George Job K and my guide Ms. Aswathy V.G., Assistant Professor, Department of
Mechanical Engineering for his creative suggestions and immense advice which helpe d to
overcome all obstacles successfully. I thank all my faculty members and staff of our college for
the helps they have extended. I finally thank my parents and friends for their moral support.
SARATH KRISHNA E. (NCE18ME040)
i
ABSTRACT
Shape memory alloys are used for making wires and tubes in application with hot fluids flowing through
them. Shape memory alloys can retain their shape even in a heated environment. Hot rolling is a metal
forming process in which the temperature of metal is above the recrystallisation temperature. Tribology
is the Engineering science of interacting surface in relative motion. Here the effect of hot rolling in
tribological behavior of Ti-50.8Ni alloy during various test is studied. As the shape memory alloy is an
important manufacturing material the change in its structure under hot cooling is studied . In these
different microstructures to tribological behaviors of Ti−50.8Ni (mole fraction, %) in reciprocating
mode at room temperature (20 °C). Hot-rolled alloys with B2 phase exhibit lower coefficient of friction
and wear rate compared to the ones with B19ʹ. Stress-induced martensitic transformation occurs during
sliding. However, multi-pass hot rolling weakens the wear resistance. In this study, microstructures were
characterized through electron backscatter diffraction and transmission electron microscopy
(EBSD/TEM). From the concept of energy conservation, the effects of weak intensity of hot -rolled
textures on the wear resistance are minimal. Based on the result that the alloy with a higher portion of
coincidence site lattice boundaries shows lower martensitic start transformation temperature in the DSC
curves
ii
TABLE OF CONTENTS
Title Page
No:
Acknowledgement i
Abstract ii
List of Tables iv
List of figures v
1. Introduction 1
2. Hot rolling 3
2.1 General Background 3
2.2 Advantages of Hot Rolling 4
2.3 Applications 4
3 Shape Memory Alloys 6
4 Application of Shape memory alloy 8
4.1 Aircraft& Spacecraft 8
4.2 Automotive 9
4.3 Robotics 9
4.4 Medical Field 10
5 Types of Shape memory Alloy 11
5.1 Copper-Aluminum- Nikel SMA 11
5.2 Nickel-Titanium SMA 12
6 Experiments on Ti-50.8Ni Alloy 13
7 Results 15
7.1 DSC Curves and XRD pattern 15
7.2 Microstructure of hot deformed alloys 16
7.3 Wear result 22
8 Conclusions 24
9 References 25
v
LIST OF TABLES
Table no Title Page no
1 Description of rolling applied for TN-S and 13

TN-M samples
iv
LIST OF FIGURES
Figure Title Page

No:
no:
01 Hot Rolling 5
02 Shape memory alloy 7
03 Aircraft parts 8
04 Automobile Parts 9
05 Shape memory alloy prosthetics 10
06 SMA In dentistry 10
07 Nitinol Wires 12
08 Wear test 14
09 DSC curves for TN-O (a), TN-S (b) and TN-M (c) samples, and XRD 15
patterns (d)
10 Grain orientation spread map for TN-S sample 16
11 Optical micrographs of TN-O (a), TN-S (b) and TN-M (c) samples, and 17
IPF maps for TN-S (d) and TN-M (e) samples
12 Grain boundary maps of TN-S (a) and TN-M (b) samples 17
13 Histograms (a, c) and KAM maps (b, d) for TN-S (a, b) and TN-M (c, d) 18
samples
14 14 Histogram of CSL boundaries of TN-S and TN-M samples 19
15 TEM micrographs for TN-S bright field (BF) image (a), selected area 20
electron diffraction (SAED) patterns (b) of region A in (a) and
corresponding schematic diagram (c), dark field (DF) image
corresponding to T (1 21) (d) and dislocation structures (e, f)
iv
LIST OF FIGURES
16 TEM micrographs for TN-M BF image showing grain boundary and
21
SAED pattern of area A inserted in (a), BF image showing high density
of dislocation (b), BF image showing dislocation structure (c), BF image
showing twins (d), corresponding SAED pattern (e), and DF image (f) of
M, T (1 10) diffraction spot in (e)
17 SEM micrographs of wear scars: (a1, a2, a3) TN-O sample; (b1, b2, b3) 23
TN-S sample; (c1, c2, c3) TN-M sample
18 3D profiles and cross-sectional area of wear tracks for TN-O (a), TN-S
(b) and TN-M (c) samples, COF (d), and XRD patterns of wear scars (e) 23
v
` EFFECT OF HOT ROLLING IN TRIBOLOGICAL
SEMINAR REPORT BEHAVIOUR OF SHAPE MEMORY ALLOYS
1. INTRODUCTION
Hot rolling is an important Manufacturing Process used for making components from steel into
structural steel. The rolling mills used to convert semifinished casting products into finished products.
Tribology is the study and application of principles of friction, lubrication and wear. Shape memory
alloys are widely used in the manufacturing of tube, wires and used in bridge structures. Hot rolling will
cause the change in the microstructures of the shape memory alloys and it affects the tribological
behavior. TiNi shape memory alloys (TiNi SMAs) can be widely applied in industrial fields because of
their irregular shape memory effect and pseudo elasticity attributed to stress introduced transformation
(SIM). Researchers conducted extensive investigations on the deformation mechanisms and shape
memory property of the alloy subjected to the hot rolling. Generally, the dislocation slip and mechanical
twinning are involved in the deformation. A significant grain -size reduction, considerable number of
coherent precipitates, and defects introduced by ausforming will strengthen B2 matrix enormously. In
addition to the dynamic recrystallization (DRx) and dynamic recovery (DRv) during the manufacturing
at high temperatures, the microstructures of the alloys are crucial in determining their performance.
Moreover, the function, if any, of small angle grain boundaries (SAGBs, misorientation angle of θ
existing extensively in the material in its tribology behaviors has never been explored in our view.
Additionally, the twinning in the B2 phase is a crucial aspect of microstructure in the ausformed TiNi-
based SMAs. The {112} and {114} twins in austenite phase directly correspond to the {113} and {201}
twins in the B19ʹ phase, respectively. The Σ notation for various twins in the austenite phase is applied
in the TiNi-based SMAs to explore their properties. Furthermore, the correspondence between
coincidence site lattice (CSL) boundaries and twin boundaries was explored in the TiNi alloy. However,
research exploring the phase transformation behaviors and performance of the complex microstructures
under different service conditions is insufficient.
Recent studies concerning the applications of the alloy have reported that the alloys show outstanding
wear resistance compared to the conventional metal materials. Moreover, porous TiNi alloys display
significant tribological performance owing to their self -adaptive behavior. Therefore, studies
demonstrating the tribological behaviors of the alloy have been conducted to explore their applications
as wear-resistant materials. WANG et al revealed that the superior pseudo elasticity and transformation
capacity of the TiNi SMAs endow them with excellent wear-resistance. Their unique stress–strain
DEPT. OF MECHANICAL ENGG. 1 NCERC, PAMPADY

features have profound influence on the tribological behaviors under different experimental conditions.
Comprehensive experimental analyses of the effects of the grain size and phase state on their tribological
behaviors were conducted.
Hot rolling significantly influences the microstructure of the TiNi alloys, but the roles of the hot-rolled
microstructures in wear performance of the alloys are ignored in current studies. Therefore, our study
focuses on this topic. Through electron backscatter diffraction (EBSD) and transmission electron
microscopy (TEM), we identified the characteristics of the microstructures subjected to hot rolling.
Additionally, reciprocating sliding wear tests were carried out to evaluate the corresponding tribological
properties carefully. The findings elaborate the significant influence of the microstructure introduced
from the thermomechanical processing on wear performance of the TiNi SMAs. Near equiatomic Ti-Ni
conventional SMAs exhibit superior properties in strength, ductility, biocompatibility, and corrosion
resistance, in addition to appreciable functional properties, i.e., shape memory effect (SME) and super
elasticity (SE). Although they are the most commercially successful SMAs, their current practical uses
are limited to temperatures below 373 K, due to the low martensitic transformation temperatures which
define the temperature range of the functional properties. To fulfil the increasing demands of high
temperatures SME and SE properties above 373 K in aerospace and automotive industries for lightweight
and compact actuators, HTSMA becomes an intensively pursued function al alloy in recent years.
Different from other alternative actuators (e.g., ferroelectrics and ferro magnetics), the ferro elastic
SMAs possess an unrivalled combination of ductility, toughness, transformation strain (εB19') and work
output.
Shape-memory alloys (SMA) belong to a family of materials, which are able to recover large
deformations. In fact, for temperature greater or lower than a certain value, they present the so -called
pseudo elastic (super elastic) behavior or the shape memory effect, i.e., they can recover large
deformations during the unloading or through a suitable thermal cycle. The very special behavior of the
shape-memory alloys is due to their capability to undergo reversible changes of the crystallographic
structure, depending on the temperature and on the stress state.

2. HOT ROLLING
2.1GENRAL BACKGROUND
Hot rolling is rapid method of forming metals into desired shapes by plastic deformation in between
rolls. The metal is subjected to high compressive stress and it causes friction and there will be change in
microstructure. In rolling metal is heated above recrystallisation temperature and it is passed in between
the two rollers which are operated in opposite direction. Hot rolling is an economical and rapid process.
Hot rolling needed less power to finish the work. Shape memory alloys can be easily machined by hot
rolling. Hot rolling is used to produce simple cross sections such as railway tracks. Rolling is classified
according to the temperature of the metal rolled. If the temperature of the metal is above
its recrystallization temperature, then the process is known as hot rolling. If the temperature of the metal
is below its recrystallization temperature, the process is known as cold rolling. In terms of usage, hot
rolling processes more tonnage than any other manufacturing process, and cold rolling processes the most
tonnage out of all cold working processes. Roll stands holding pairs of rolls are grouped together
into rolling mills that can quickly process metal, typically steel, into products such as structural steel (I-
beams, angle stock, channel stock), bar stock, and rails. Most steel mills have rolling mill divisions that
convert the semi-finished casting products into finished products.
There are many types of rolling processes, including ring rolling, roll bending, roll forming, profile
rolling, and controlled rolling. Hot rolling is a metalworking process that occurs above
the recrystallization temperature of the material. After the grains deform during processing, they
recrystallize, which maintains an equiaxed microstructure and prevents the metal from work hardening.
The starting material is usually large pieces of metal, like semi-finished casting products, such
as slabs, blooms, and billets. If these products came from a continuous casting operation, the products are
usually fed directly into the rolling mills at the proper temperature. In smaller operations, the material
starts at room temperature and must be heated. This is done in a gas- or oil-fired soaking pit for larger
workpieces; for smaller workpieces, induction heating is used. As the material is worked, the temperature
must be monitored to make sure it remains above the recrystallization temperature. To maintain a safety
factor a finishing temperature is defined above the recrystallization temperature; this is usually 50 to

100 °C (90 to 180 °F) above the recrystallization temperature. If the temperature does drop below this
temperature the material must be re-heated prior to additional hot rolling.
Hot-rolled metals generally have little directionality in their mechanical properties or deformation-
induced residual stresses. However, in certain instances non-metallic inclusions will impart some
directionality and workpieces less than 20 mm (0.79 in) thick often have some directional properties. Non-
uniform cooling will induce a lot of residual stresses, which usu ally occurs in shapes that have a non-
uniform cross-section, such as I-beams. While the finished product is of good quality, the surface is
covered in mill scale, which is an oxide that forms at high temperatures. It is usually removed
via pickling or the smooth clean surface (SCS) process, which reveals a smooth surface. [10] Dimensional
tolerances are usually 2 to 5% of the overall dimension.
2.2ADVANTAGES OF HOT ROLLING
• Mechanical Properties Improved: The mechanical properties like toughness, resistance to shock,
ductility, and percentage elongation are improved.
• Grain Structure Refined: The grain structure of the metal is refined i.e.; the coarse grains are
converted into fine grains which changes the properties of metal.
• Porosity Eliminated: The porosity of the metal is eliminated, thus producing strong and uniform
structure.
• Impurities Uniformly Distributed: The impurities like slag are evenly distributed throughout the
metal. Otherwise, they concentrated at one position inside the metal, shall make it weaker at that
position.
• Low Pressure Required: The deformation of metal is easy due to higher temperature of metal
being rolled. This reduces the pressure requirements.
2.3 APPLICATIONS
Hot-rolled mild steel seems to have a wider tolerance for the level of included carbon than does cold-
rolled steel, and is, therefore, more difficult for a blacksmith to use.

Also, for similar metals, hot-rolled products seem to be less costly than cold-rolled ones. Hot rolling is
used mainly to produce sheet metal or simple cross-sections, such as rail tracks. Other typical uses for
hot-rolled metal:
• Truck frames
• Automotive clutch plates, wheels and wheel rims
• Pipes and tubes
• Water heaters
• Agricultural equipment
• Strappings
• Stampings
• Compressor shells
• Metal buildings
• Railroad hopper cars and railcar components
• Doors and shelving
• Discs
• Guard rails for streets and highways
Fig 1 Hot rolling

3 SHAPE MEMORY ALLOYS
An alloy that can be deformed when cold but return to its pre deformed shape when heated. It is also
called as smart alloy, memory metal, or muscle wire. Used for medical guide wires, couplings and
actuators. The alloy appears to have a memory. Shape Memory Alloys exhibits super-elastic behaviour
also known as pseudo elastic behaviour. SMAs deformed above a critical temperature show a large
reversible elastic deformation (recoverable strains up to 10%. much exceeding the elasticity) as a result of
stress-induced martensitic transformation.
Shape-memory alloys (SMA) belong to a family of materials, which are able to recover large
deformations. In fact, for temperature greater or lower than a certain value, they present the so -called
pseudo elastic (super elastic) behaviour or the shape memory effect, i.e., they can recover large
deformations during the unloading or through a suitable thermal cycle. The very special behaviour of the
shape-memory alloys is due to their capability to undergo reversible changes of the crystallographic
structure, depending on the temperature and on the stress state. These changes can be interpreted as
martensitic transformations between a crystallographic more-ordered parent phase, the austenite (A), and
a crystallographic less-ordered product phase, the martensite (M). In general, the austenite is stable at high
values of temperature and low values of stresses, while the martensite is stable at low values of temperature
and high values of stresses. Due to the pseudo elasticity and shape memory effects, shape-memory alloys
are successfully adopted in a broad set of advanced and innovative applications in aeronautical,
biomedical, mechanical and civil engineering. The high interest toward the use of SMA in commercially
valuable applications clearly requires the use of accurate constitutive models during the design phase of
devices. Several models able to reproduce the SMA constitutive behaviour were proposed in literature. A
recent state of the art regarding the behaviour, the modelling and the applications of SMA can be found
in the book, where wide reference lists on the different SMA aspects are reported. The available models
can be framed into three categories: the micro-level models which describe micro-scale level effects, such
as, nucleation, interface motion, twin growth; the micro–macrolevel models which combine micro-
mechanical elements, such as habit planes, martensitic variants, with macroscale thermodynamics and
adopt proper homogenization techniques to derive macro/global parameters from the micro/local ones the
macro-level models which are able to describe some of the major SMA macroscopic features. The macro-
models are particularly suitable for the study of SMA structural elements as they can be implemented

more easily in numerical codes. One of the most interesting features is the SMA response under cyclic
loading conditions. In fact, the material response progressively changes during the cycles, reaching a limit
and stable path after a certain number of stress/temperature loading–unloading cycles, i.e., after the so-
called material training.
Near equiatomic Ti-Ni conventional SMAs exhibit superior properties in strength, ductility,
biocompatibility, and corrosion resistance, in addition to appreciable functional properties, i.e., shape
memory effect (SME) and super elasticity (SE). Although they are the most commercially successful
SMAs, their current practical uses are limited to temperatures below 373 K due to the low martensitic
transformation temperatures which define the temperature range of the functional properties. To fulfil the
increasing demands of high temperatures SME and SE properties above 373 K in aerospace and
automotive industries for lightweight and compact actuators, HTSMA becomes an intensively pursued
functional alloy in recent years. Different from other alternative actuators (e.g., ferroelectrics and ferro
magnetics), the ferro elastic SMAs possess an unrivalled combination of ductility, toughness,
transformation strain (εB19') and work output. Several HTSMA systems, such as Cu -Al-based, Co-Ni-
based, Ni-based and β-Ti alloys, have been developed and investigated widely. However, the
contemporary commercial applications of HTSMAs have been prohibited due to the drawbacks in the
mechanical properties and phase stability. For example, the Co-Ni-based and Ni-based HTSMAs are quite
brittle, especially under tension; β-Ti HTSMAs with excellent ductility is heavy in density and prone to
the iso-ω precipitation that causes adverse brittleness. Considerable and continuous efforts have been
made on the exploration of the Ti-Ni SMAs for the potential high temperature service above 373 K.
Fig 2 Shape memory alloy.

4.APPLICATIONS OF SHAPE MEMORY ALLOYS
The applications of shape memory alloys are;
4.1 AIRCRAFT & SPACECRAFT
Boeing, General Electric Aircraft Engines, Goodrich Corporation, NASA, Texas A&M
University and All Nippon Airways developed the Variable Geometry Chevron using a NiTi SMA. Such
a variable area fan nozzle (VAFN) design would allow for quieter and m ore efficient jet engines in the
future. In 2005 and 2006, Boeing conducted successful flight testing of this technology . SMAs are being
explored as vibration dampers for launch vehicles and commercial jet engines. The large amount
of hysteresis observed during the super elastic effect allow SMAs to dissipate energy and dampen
vibrations. These materials show promise for reducing the high vibration loads on payloads during launch
as well as on fan blades in commercial jet engines, allowing for more lightweight and efficient
designs. SMAs also exhibit potential for other high shock applications such as ball bearings and landing
gear.
There is also strong interest in using SMAs for a variety of actuator applications in commercial jet engines,
which would significantly reduce their weight and boost efficiency. Further research needs to be
conducted in this area, however, to increase the transformation temperatures and improve the mechanical
properties of these materials before they can be successfully implemented. A review of recent advances
in high-temperature shape-memory alloys (HTSMAs) is presented by Ma et al. A variety of wing-
morphing technologies are also being explored.
Fig 3. Aircraft parts.

4.2 AUTOMOTIVE
The first high-volume product (> 5Mio actuators / year) is an automotive valve used to control low
pressure pneumatic bladders in a car seat that adjust the contour of the lumbar support / bolsters. The
overall benefits of SMA over traditionally-used solenoids in this application (lower
noise/EMC/weight/form factor/power consumption) were the crucial factor in the decision to replace the
old standard technology with SMA.
The 2014 Chevrolet Corvette became the first vehicle to incorporate SMA actuators, which replaced
heavier motorized actuators to open and close the hatch vent that releases air from the trunk, making it
easier to close. A variety of other applications are also being targeted, including electric generators to
generate electricity from exhaust heat and on-demand air dams to optimize aerodynamics at various
speeds.
Fig. 4 Automobile parts
4.3 ROBOTICS
There have also been limited studies on using these materials in robotics, for example the hobbyist
robot Stiquito (and "Roboterfrau Lara"), as they make it possible to create very lightweight robots.
Recently, a prosthetic hand was introduced by Loh et al. that can almost replicate the motions of a human
hand [Loh2005]. Other biomimetic applications are also being explored. Weak points of the technology
are energy inefficiency, slow response times, and large hysteresis.

Fig. 5 Shape memory alloy prosthetics
4.4 MEDICAL FIELD
Shape-memory alloys are applied in medicine, for example, as fixation devices

for osteotomies in orthopaedic surgery, as the actuator in surgical tools; active steerable surgical needles
for minimally invasive percutaneous cancer interventions in the surgical procedures such
as biopsy and brachytherapy,[41] in dental braces to exert constant tooth-moving forces on the teeth,
in Capsule Endoscopy they can be used as a trigger for biopsy action.
The late 1980s saw the commercial introduction of Nitinol as an enabling technology in a number of
minimally invasive endovascular medical applications. While more costly than stainless steel, the self -
expanding properties of Nitinol alloys manufactured to BTR (Body Temperature Response), have
provided an attractive alternative to balloon expandable devices in stent grafts where it gives the ability
to adapt to the shape of certain blood vessels when exposed to body temperature. On average, 50% of all
peripheral vascular stents currently available on the worldwide market are manufactured with Nitinol.
Fig. 6 SMA In dentistry.

5 TYPES OF SHAPE MEMORY ALLOYS
The commercially used shape memory alloys are 2 types. They are
5.1 COPPER-ALUMINIUM-NICKEL SMA
The Copper/aluminium binary alloy displays shape memory characteristics but has a transformation
temperature that is generally considered too high for practical use. The addition of nickel to this system
has resulted in another family of shape memory alloys (SMA’s), the CuAlNi alloys with transformation
temperatures in the range 80 to 200°C. CuZnAl alloys also exhibit shape memory capabilities, but are less
common than the CuAlNi alloys. CuAlNi SMA’s are popular due to their wide range of useful
transformation temperatures and small hysteresis. They are also the only SMA’s that can be used at
temperatures over 100°C. Compared to Ni-Ti SMA’s, the CuAlNi alloys are much cheaper to make as
they use cheaper raw materials and do not require sophisticated processing as do the NiTi alloys.
CuAlNi SMA’s usually contain 11-14.5% aluminium and 3-5% nickel, with the balance being copper.
The aluminium content strongly influences the alloys’ transf ormation temperature. Reducing the
aluminium content below 12% can also improve the alloys’ mechanical properties. Adding manganese
(approximately 2%) can reduce the transformation temperature, while the addition of small quantities
(approximately 1%) of boron, cerium, cobalt, iron, titanium, vanadium and zirconium are also commonly
added to control grain size. However, additions should be made carefully as they can upset the stability of
the structure.
The most common method of producing these alloys is induction melting. Powder metallurgy processes
can also be used to produce fine grained structures without the need to grain size control additives. Hot
working is the only satisfactory fabrication method. CuAlNi alloys can be hot worked in air. Following
hot working, they are subject to a suitable solution heat treatment involving controlled cooling (often
water quenching), which will help to dictate properties such as transformation temperature. Post quench
ageing is often required to establish the transformation temperature, as the as-quenched transformation
temperature is usually unstable. This process is normally carried out above the A f.

5.2 NICKEL-TITANIUM SMA
The basis of the Nickel-Titanium alloy is the binary, equi-atomic inter-metallic compound of Ti-Ni. The
inter-metallic compound is extraordinary because it has moderate solubility range for excess Nickel or
Titanium, as well as most other metallic elements. This solubility allows alloying with many of the
elements to modify both the mechanical properties and the transformation properties of the system. Excess
Nickel strongly depresses the transformation temperature and increases the yield strength of the austenite.
The contaminants such as Oxygen and Carbon shift the transformation temperature an d degrade the
mechanical properties. Therefore, it is also desirable to minimize the amount of such elements.
The Ni-Ti alloys have greater shape memory strain upto 8.5% tend to be much more thermally
stable. They have excellent corrosion resistance and susceptibility, and have much higher ductility.
Machining by turning or milling is very difficult except with special tools. Welding, brazing or soldering
the alloys is generally difficult. The material does respond well to abrasive removal suc h as grinding, and
shearing. Punching can be done if thicknesses are kept small. Nitinol alloys exhibit two closely related
and unique properties: the shape memory effect and superelasticity (also called pseudo elasticity). Shape
memory is the ability of nitinol to undergo deformation at one temperature, stay in its deformed shape
when the external force is removed, then recover its original, undeformed shape upon heating above its
"transformation temperature". Superelasticity is the ability for the metal to undergo large deformations
and immediately return to its undeformed shape upon removal of the external load. Nitinol can deform
10–30 times as much as ordinary metals and return to its original shape. Whether nitinol behaves with the
shape memory effect or superelasticity depends on whether it is above the transformation temperature of
the specific alloy. Below the transformation temperature it exhibits the shape memory effect, and above
that temperature it behaves super elastically
Fig 7. Nitinol wires

6 EXPERIMENTS ON Ti-50.8 Ni ALLOY
The commercial 3.0 mm Ti−50.8Ni (at. %) sheets (TN-O) were subjected to hot rolling) at 850 °C to
produce ausformed pieces with different microstructures. The samples were reduced to 2.0 mm in
thickness via single pass hot rolling (TN-S). Multi-pass rolling (TN-M) was performed on the TN-S
samples to reduce the thickness further. Before each pass rolling, the samples were annealed at 850 °C for
6 min. The hot rolling steps are summarized in Table 1. The transformation temperatures were analyzed
by differential scanning calorimetry (DSC; NetzschSTA449F3). X-ray diffraction (XRD) with Cu Kα
radiation on EMPYRE was carried out to identify the major phases of the pieces. EBSD measurements of
the hot-rolled samples were conducted. TEM samples were twin-jet polished in a solution of 6 vol.%
HClO4 + 34 vol.% CH3(CH2)3OH + CH3OH after being mechanically worked to 40 μm. TEM images
were obtained at an acceleration voltage of 300 kV using a Tenai F30.
Table 1 Description of rolling applied for TN-S and TN-M samples
All disks for wear tests were cut from hot-rolled sheets via electrical discharge machining. Before sliding
wear, the alloys were mechanically polished and then electro-polished in an electrolyte of 20 vol.%
H2SO4 + 80 vol.% CH3OH. Ball-on plate wear tests were done at room temperature under linear
reciprocating model with constant normal loading of 3 N. GCr15 balls with diameter of 6 mm acted as
counter faces. The steel ball was slided against the rolled surface (ND) of the TiNi SMA at an average
speed of 10 mm/s along the rolling direction (RD). The transverse direction (TD) is displayed in Fig. 7.
The corresponding maximum contact stress (σmax) was estimated based on the Hertzian contact model,
which was approximately 536 MPa. 3D profiles were used to calculate the wear rate carefully, and the
worn surfaces were observed through scanning electron microscopy (SEM).
Fig. 8 Wear test

7.RESULTS
The results of experiments carried on Ti-50.8Ni is discussed below
7.1 DSC CURVES AND XRD PATTERNS
DSC stand for differential scanning calorimetry. The transformation temperatures were analyzed by
differential scanning calorimetry. The figure shows the DSC curves and XRD patterns of TN-O, TN-S,
and TN-M samples. The transformation of all samples is a two-step process (B2-R, R-B19′) during
cooling. Because the austenite initial temperature (As) for TN-O sample is slightly higher than the room
temperature, the B19′ phase is retained if SIM occurs. The martensitic start transformation temperature
(Ms) and as of the TN-S sample decrease significantly compared to the TN-M sample. Evidently, the
martensitic transformation in the TN-S sample is retarded compared to that in the TN-M sample, though
both sheets are in the B2 state, as shown in the XRD patterns. It is necessary to distinguish the effect of
hot rolling on microstructures and reasonably elucidate the results.
Fig.9 DSC curves for TN-O (a), TN-S (b) and TN-M (c) samples, and XRD patterns (d)

7.2 MICROSTRUCTURE OF HOT- DEFORMED ALLOYS
Optical micrographs of the TN-O, TN-S, and TN-M samples in Figs. 11(a−c) show the presence of stripe-
microstructure. It is the B19' in the TN-O sample but the B2 twins in the hot-rolled alloy. As shown in
Figs. 11(d, e), inverse pole figure (IPF) maps of the TN-S and the TN-M samples clearly demonstrate the
reduction in grain size. Moreover, the grains are homogenized after multiple hot rolling. DRx occurs
during hot rolling, which is indicated from fine grains at triple boundaries (Fig. 11(d)). The abundant
nucleation sites at the grain boundaries facilitate the recrystallized grains to nucleate significantly.
Additionally, the grain orientation spread (GOS) map for the TN-S sample in Fig. 10 shows that the twins
in the grains actively assist the formation of recrystallized grains, which is characterized by low
misorientation angles. This can be attributed to the relatively large plastic strain in the twinned region.
Regions with relatively high misorientation values are also observed.
Generally, a significant texture exists in the hot-rolled sample, specifically for non-ferrous metals. As
shown by the IPF maps along the RD and TD for the TN-S and the TN-M samples, the γ-fiber, 111
parallel to TD, is the main texture fiber in the hot-rolled sheets. However, the texture intensity is weak.
Therefore, the effect of the texture on the tribology behaviors in the transverse direction can be negligible.
The major differences are in the RD. The 101 fiber texture is prominent along the RD in the TN-S sample
but it is the 111 fiber in the TN-M sample. To evaluate the local plastic strain and geometrically
necessary dislocation (GND) activity properly, Kernel Average Misorientation (KAM) criterion
presenting the average orientation difference between a point inside the grain and its adjacent neighbors
in the same grain is applied. A high relative frequency of the high KAM (more than 1°) implies high
density of dislocations.
Fig 10 Grain orientation spread map for TN-S sample

Fig 11 Optical micrographs of TN-O (a), TN-S (b) and TN-M (c) samples, and IPF maps for TN-S (d)
and TN-M (e) samples
Moreover, a more pronounced intergranular local misorientation in the TN-M sample implies that the
dislocation density is high, which will be ascribed to the minor thickness reduction at the final pass. The
KAM value of the microstructure subjected to hot deformation and DRv is lower than that of the DRx
grains. That is, DRx narrows the KAM distribution, as shown in Figs. 13(a) and (c). DRv and DRx will
consume SAGBs and high angle grain boundaries (HAGBs, misorientation angle of θ>15° because of
recrystallization. Black and green lines in Figs. 12(a) and (b) are the HAGBs and SAGBs, respectively.
The significant accumulation of the SAGBs inside the grains in TN-S sample indicates the widespread
occurrence of DRv. The annealing in-between the rolling passes increases the portion of the recrystallized
grains in the TN-M sample. Nevertheless, the storage energy available from final step with small thickness
reduction is insufficient for the occurrence of DRv. Therefore, a high KAM value is shown in Fig. 13(d).
Fig.12 Grain boundary maps of TN-S (a) and TN-M (b) samples

Fig.13 Histograms (a, c) and KAM maps (b, d) for TN-S (a, b) and TN-M (c, d) samples
Most studies on TiNi alloys focus on the martensitic transformation and corresponding performances.
Nonetheless, the significant defect of the microstructure of SMA is the twinning in the austenite structure.
CSL boundaries correspond to the twin boundaries in the TiNi alloy. The Σ values of {112}, {114}, {113},
and {115} boundaries are Σ3, Σ9, Σ11 and Σ27, respectively. The B2 phase is significantly refined during
the thermal cycling and heterogeneous Σ3 and Σ9 boundaries are established. Figure 14 shows the CSL
features in the hot-rolled samples. The fraction of the CSL boundaries reduces from 8.24% in the TN-S
sample to 4.7% in the TN-M sample. The proportion of the Σ3 boundary decreases significantly with
multirolling processes.

Fig. 14 Histogram of CSL boundaries of TN-S and TN-M samples
To investigate the microstructure characters at a more microscopic scale, TEM images of the hot-rolled
materials are shown in Figs. 15 and 16. The dominant planar defects are {112} compound twins in Fig. 9
whereas it is the {114} twins in Fig. 10. Furthermore, dislocations with various structures are established.
As shown in Figs. 15(e, f), the dislocation annihilation associated to DRv could introduce dislocation cells
in the TN-S sample, which is directly related to the SAGBs in Fig. 13(a). Fine grains characterized by low
misorientation angles in Fig. 10 confirm the appearance of DRx. This explains the lower KAM value in
the TN-S sample. The large portion of HAGBs in the TN-M sample is caused by DRx when it is subjected
to multiple intermediate annealing and rolling. However, low storage energy created because of the small
thickness reduction in the last pass cannot provide sufficient power to DRv. Consequently, as shown in
Fig. 13(d), high dislocation regions (Fig. 16(b)) with high KAM values are observed. Moreover,
dislocation couples showing the opposite Burgers vector are shown in Fig. 16(c). Notably, twinning in
bcc solid solution is disfavored. This is because the nearest neighbor relations must be changed for the
twinning in the B2-structure to indicate the formation of a new crystal structure. Consequently, the
dislocation slip becomes an easier process. For the typical twin-lamellated microstructure to originate in
a wide range of ausforming conditions, the twinning process competes successfully with the dislocation
slipping (Figs. 10 and 11). The main twins are the {112} and the {114} planes. Twinning of the B2
austenitic phase is significant to accommodate the arbitrary deformation of the TiNi alloy. The
combination of shear and shuffle in the B2 phase contributes to the occurrence of the {211} twin mirror
symmetry, whereas an interface shift also occurs for the {114} twin. The energy barriers for slip, {211},
and {114} twinning systems are 142, 79, and 148 mJ/m2, respectively; thus, the {211} twining is preferred
as a deformation mode. Therefore, the various planar defects and slip significantly influence the
deformation of the alloy at high temperatures. The non-homogeneous distribution of internal stresses
resulted from the specific arrangement of defects such as dislocations, twins, and point defects, which are
the cause of the multistage transformation. Dislocations and twins in the austenite phase hinder martensitic
transformation. Therefore, the obstruction to SIM from dislocations is slight compared to the {112} and
{114} twins although they may hinder it.
Fig. 15 TEM micrographs for TN-S bright field (BF) image (a), selected area electron diffraction
(SAED) patterns (b) of region A in (a) and corresponding schematic diagram (c), dark field (DF) image
corresponding to T (1 21) (d) and dislocation structures (e, f)

Fig. 16 0 TEM micrographs for TN-M BF image showing grain boundary and SAED pattern of area A
inserted in (a), BF image showing high density of dislocation (b), BF image showing dislocation
structure (c), BF image showing twins (d), corresponding SAED pattern (e), and DF image (f) of M,T (1
10) diffraction spot in (e)

7.3 WEAR RESULTS
The tribological behaviors of the samples are shown in Figs. 17 and 18 Furrows and plastic tearing in Fig.
17 suggest that abrasion occurs in all the samples. However, adhesive traces for the TN -M sample become
significantly apparent in Figs. 17(c1–c3). This is because delaminating is the main wear mechanism for
the TN-O and the TN-S samples. Wear rate (R) is based on a volumetric material loss using the following
expression:
❑ Where A = average cross-sectional area

L =Wear track length
N= Total sliding passes
Fn=Normal Load
The typical 3D profiles and cross-sectional area of scars are shown in Figs. 18(a−c). It is noteworthy that
the wear rate of TN-S sample is (0.67±0.05) × 10−3 mm3 /(N·m), which is lower than that of the TN-M
sample ((1.07±0.08) ×10−3 mm3 /(N·m)) while the COF at stable stage for them is closely comparable
(Fig. 18(d)). The COF of the TN-O sample is the highest in all the samples studied here, which is due to
the weaker strength of B19' in TN-O sample [20]. The XRD results of the wear scars identify the
understandable appearance of martensitic phase in all the scars (Fig. 18(e)). This demonstrates that the
materials of the scars experience the SIM transformation during the sliding wear.

Fig. 17 SEM micrographs of wear scars: (a1, a2, a3) TN-O sample; (b1, b2, b3) TN-S sample; (c1, c2,
c3) TN-M sample
Fig 18 3D profiles and cross-sectional area of wear tracks for TN-O (a), TN-S (b) and TN-M (c)
samples, COF (d), and XRD patterns of wear scars (e)
8. CONCLUSION
The TN-S and TN-D samples show the 111 fiber along the TD. TN-S sample displays the 101 fiber
along the RD, whereas the TN-M sample displays the 111 fiber along the RD. Based on the concept of
energy conservation, Taylor-type model for textured alloys, and the intensity of textures, the influences
of hot-rolled textures on the wear resistance are small. During hot rolling, the deformation of the
Ti−50.8Ni sample is governed by the {112} B2 and the {114} B2 mechanical twins and dislocations. In
particular, the {112} B2 is relatively dominant in the TN-S sample, but the {114} B2 is primary in the
TN-M sample. Moreover, dislocation cells are widely distributed in the TN-S sample whereas high
densities of dislocation regions and dislocation couples are obtained in the TN-M sample. The tribology
behaviors of the coarse grain Ti−50.8Ni are not only related to the phase composition, but also greatly
influenced by the substructures of the B2 matrix. The {112} B2 twins hinder the B2 -B19ʹ transformation
significantly compared with a high density of dislocation, but it cannot suppress the martensitic
transformation completely. SAGBs accommodate plastic deformation further. Therefore, the introduction
of a large proportion of SAGBs and low-Σ CSL boundaries in the austenite Ti−50.8Ni alloy via hot rolling,
specifically the Σ3, improves the wear resistance of the coarse grain alloy.

9. REFERENCES
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S N, IBRAHIM M K. Microstructure and superelastic properties of free forged Ti−Ni shape -memory alloy
[J]. Transactions of Nonferrous Metals Society of China, 2018, 28(3): 502−514
[3] JIANG Shu-yong, YU Jun-bo, ZHANG Yan-qiu, XING Xiao-dong. Mechanically-induced martensite
transformation of NiTiFe shape memory alloy subjected to plane strain compression [J]. Transactions of
Nonferrous Metals Society of China, 2020, 30(5): 1325−1334.
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Ni49.4Ti38.6Hf12 shape memory alloy during hot rolling [J]. Intermetallics, 2013, 42: 1−8.
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cycling behaviour of equiatomic NiTi shape memory alloy [J]. Material Science and Technology, 2012,
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[6] BENAFAN O, NOEBE R D, PADULA S A, GARG A, CLAUSEN B, VOGEL S, VAIDYANATHAN

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properties of warm deformed NiTi intermetallic alloy [J]. Materials Science and Engineering A, 2017,
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alloy: Effects on austenite−martensite phase transformation [J]. Journal of Alloys and Compounds, 2015,
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[9] COWDHURY P, SEHITOGLU H. Deformation physics of shape memory alloys: Fundamentals at

atomistic frontier [J]. Progress in Materials Science, 2017, 88: 49−88.
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NiTi shape memory alloy ausformed using equal channel angular extrusion [J]. Philosophical Magazine,
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Seminar Report on

EFFECT OF HOT ROLLING IN TRIBOLOGICAL

SARATH KRISHNA E. (NCE18ME044)

in partial fulfillment of the requirements for the award of the degree

of BACHELOR OF TECHNOLOGY in Mechanical Engineering

Ms. ASWATHY V.G.

DEPARTMENT OF MECHANICAL ENGINEERING

Guided By Head of the Department

Ms. Aswathy V.G. Prof. Dr. George Job K

SARATH KRISHNA E. (NCE18ME040)

Table no Title Page no

1 Description of rolling applied for TN-S and 13

Figure Title Page

14 14 Histogram of CSL boundaries of TN-S and TN-M samples 19

DEPT. OF MECHANICAL ENGG. 1 NCERC, PAMPADY

DEPT. OF MECHANICAL ENGG. 2 NCERC, PAMPADY

DEPT. OF MECHANICAL ENGG. 3 NCERC, PAMPADY

2.2ADVANTAGES OF HOT ROLLING

DEPT. OF MECHANICAL ENGG. 4 NCERC, PAMPADY

Fig 1 Hot rolling

DEPT. OF MECHANICAL ENGG. 5 NCERC, PAMPADY

3 SHAPE MEMORY ALLOYS

DEPT. OF MECHANICAL ENGG. 6 NCERC, PAMPADY

Fig 2 Shape memory alloy.

DEPT. OF MECHANICAL ENGG. 7 NCERC, PAMPADY

4.APPLICATIONS OF SHAPE MEMORY ALLOYS

The applications of shape memory alloys are;

4.1 AIRCRAFT & SPACECRAFT

Fig 3. Aircraft parts.

DEPT. OF MECHANICAL ENGG. 8 NCERC, PAMPADY

Fig. 4 Automobile parts

DEPT. OF MECHANICAL ENGG. 9 NCERC, PAMPADY

Fig. 5 Shape memory alloy prosthetics

4.4 MEDICAL FIELD

Shape-memory alloys are applied in medicine, for example, as fixation devices

Fig. 6 SMA In dentistry.

DEPT. OF MECHANICAL ENGG. 10 NCERC, PAMPADY

5 TYPES OF SHAPE MEMORY ALLOYS

5.1 COPPER-ALUMINIUM-NICKEL SMA

DEPT. OF MECHANICAL ENGG. 11 NCERC, PAMPADY

5.2 NICKEL-TITANIUM SMA

Fig 7. Nitinol wires

6 EXPERIMENTS ON Ti-50.8 Ni ALLOY

Table 1 Description of rolling applied for TN-S and TN-M samples

Fig. 8 Wear test

DEPT. OF MECHANICAL ENGG. 14 NCERC, PAMPADY

7.1 DSC CURVES AND XRD PATTERNS

DEPT. OF MECHANICAL ENGG. 15 NCERC, PAMPADY

7.2 MICROSTRUCTURE OF HOT- DEFORMED ALLOYS

Fig 10 Grain orientation spread map for TN-S sample

DEPT. OF MECHANICAL ENGG. 16 NCERC, PAMPADY

DEPT. OF MECHANICAL ENGG. 17 NCERC, PAMPADY

DEPT. OF MECHANICAL ENGG. 18 NCERC, PAMPADY

Fig. 14 Histogram of CSL boundaries of TN-S and TN-M samples

DEPT. OF MECHANICAL ENGG. 20 NCERC, PAMPADY

DEPT. OF MECHANICAL ENGG. 21 NCERC, PAMPADY

7.3 WEAR RESULTS

❑ Where A = average cross-sectional area

DEPT. OF MECHANICAL ENGG. 22 NCERC, PAMPADY

DEPT. OF MECHANICAL ENGG. 24 NCERC, PAMPADY

[2] BAHADOR A, HAMAZAH E, KONDOH K, ASMA ABUBAKAR T, YUSOF F, UMEDA J, SAUD

[4] SURESH K S, KIM D I, BHAUMIK S K, SUWAS S. Evolution of microstructu re and texture in

[6] BENAFAN O, NOEBE R D, PADULA S A, GARG A, CLAUSEN B, VOGEL S, VAIDYANATHAN

[7] ATAEI M, ZAREI-HANZAKI A, SHAMSOLHODAEI A. Shape memory response and mechanical