Muhammad Athar Mahmood 2018 (S) - MS-AME-17 Research Supervisor: Dr. Ghulam Moeen Uddin 2022

EXPERIMENTAL INVESTIGATION OF TRIBO-
MECHANICAL PROPERTIES OF TIALN COATING ON 316L

STAINLESS STEEL SUBSTRATE USING 80:20 TIAL ALLOY
CATHODIC ARC TARGETS
By
Muhammad Athar Mahmood

2018(S)-MS-AME-17
Research Supervisor:
Dr. Ghulam Moeen Uddin
2022
DEPARTMENT OF MECHANICAL ENGINEERING

UNIVERSITY OF ENGINEERING AND TECHNOLOGY,
LAHORE
EXPERIMENTAL INVESTIGATION OF TRIBO-MECHANICAL
PROPERTIES OF TIALN COATING ON 316L STAINLESS
STEEL SUBSTRATE USING 80:20 TIAL ALLOY CATHODIC
ARC TARGETS
by
2018(S)-MS-AME-17
A THESIS
presented to the university of engineering and technology, Lahore
in partial fulfillment of the requirements for the degree of
Master of Science
in
Automotive Engineering
APPROVED BY:
Primary Advisor/Internal Examiner External Examiner

Prof. Dr. Ghulam Moeen-Ud-Din
Department of Mechanical Engineering
UET, Lahore
Chairman Dean
Department of Mechanical Engineering Faculty of Mechanical Engineering
UET, Lahore UET, Lahore
Approval date
DEPARTMENT OF MECHANICAL ENGINEERING

UNIVERSITY OF ENGINEERING & TECHNOLOGY, LAHORE
 2022
All Rights Reserved
Any part of this thesis cannot be copied, reproduced or published without the written approval of the
Scholar.
ABSTRACT
Stainless steel (SS) plays an important role in automotive sector and biomedical implant
manufacturing. It has relatively lower mechanical and tribological properties but having high
temperature oxidation resistance and high corrosion resistance. In order to enhance its
tribomechanical performance physical vapor deposition (PVD) based Titanium Aluminum
Nitride (TiALN) coatings are deposited on its surface. TiAl alloy (80:20) cathodic arc target
based PVD coatings of TiAlN have not been investigated in terms of tribo-mechanical
performance.
Investigation is being done of tribo-mechanical properties of 316L stainless steel by 80:20
Titanium Aluminum alloy target based PVD coating . Comparative analysis of coating
thickness and surface roughness effect on mechanical and tribological properties is carried out in
order to evaluate the optimum tribo-mechanical properties. Comparison is made between coated
316L stainless steel with Titanium Aluminum Nitride coating and the uncoated 316L stainless
steel (SS). The tribo-mechanical characteristics of PVD-coated stainless steel formed of an 80:20
titanium aluminium alloy will be compared to those of coatings made of 50:50 and 30:70
titanium aluminium alloys from earlier investigations. (. Experimentation is carried out to
evaluate tribologoical and mechanical properties of 80:20 TiAl based TiAlN coatings. Physical
vapor deposition method is used for coating process. Scratch tests and Nano indentation analysis
are performed on coated samples. Tribological performance of Titanium Aluminum Nitride
80:20 coating is better than 50:50 & 30:70 TiAl alloy target base TiAlN coatings. By increasing
coating thickness, the hardness and coating adhesion is increased. The reverse is true for
coefficient of friction and wear rate.

ACKNOWLEDGMENTS
Firstly, and most importantly my Gratitude and acknowledgment goes to ALLAH Subhanaho-
Wa Ta’ala for His countless help and blessings. His kindness and consideration being the key to
every happening. Allah Subhanaho- Wa Ta’ala said :
“If you are grateful, I will certainly increase you”
Also millions and millions of salutations upon The Prophet Mohammad ‫ ﷺ‬and His Family, who
came as the light of knowledge for all mankind. He ‫ ﷺ‬came as a role model and as someone
who enlightened not only the whole mankind. He ‫ ﷺ‬said:
“He, who is not thankful to the people, is not thankful to ALLAH”.
My appreciation and gratitude for my parents who were always there to help me out in
everything I did in life especially there support in my education and research work. Words
cannot describe the efforts and hard work they have done in upbringing me and motivating me to
reach my goals.
Prof. Dr. Nasir Hayat (Chairman Mechanical Engineering Department) deserves all the due
credit for providing research environment in the department which helped me to complete this
job. I also want to pay thanks to the faculty, administrative and lab staff, and all those who
extended help at any stage of my work. Furthermore, I would like to express my special
gratefulness to my advisor Dr. Ghulam Moeen Uddin for the continuous support of my Masters
study and related research, for his patience, motivation, and immense knowledge. His sincere
guidance and support helped me at every moment while doing this research and accomplishing
this task.
I am grateful to Iftikhar Trading Company (ITC) and PITMAEM at PCSIR for providing
technical facilities that helped me in coating process and testing.

STATEMENT OF ORIGINALITY
It is stated that the research work presented in this thesis consists of my own ideas and research
work. The contributions and ideas from others have been duly acknowledged and cited in the
dissertation. This complete thesis is written by me.

TABLE OF CONTENTS
ABSTRACT................................................................................................................................................4
ACKNOWLEDGMENTS...........................................................................................................................5
STATEMENT OF ORIGINALITY.............................................................................................................7
TABLE OF CONTENTS............................................................................................................................8
LIST OF FIGURES.....................................................................................................................................9
LIST OF TABLES....................................................................................................................................10
1. INTRODUCTION.............................................................................................................................11
1.1. OVERVIEW..................................................................................................................................11
1.2. TRIBOLOGY................................................................................................................................13
1.3. SURFACE ENGINEERING.........................................................................................................14
1.4. THIN FILM COATING................................................................................................................14
1.5. PHYSICAL VAPOR DEPOSITION (PVD)..................................................................................15
1.5.1. PVD Coating Properties.........................................................................................................16
1.6. CHEMICAL VAPOR DEPOSITION (CVD) COATING.............................................................17
1.7. TRIBOLOGY AND COATING CORRELATION.......................................................................17
1.8. EVALUATION OF TRIBOLOGICAL PROPERTIES.................................................................18
1.9. TRIBOLOGY AND SURFACE ROUGHNESS CORRELATION...............................................18
1.10. CERAMIC COATING..............................................................................................................19
1.11. BIOMEDICAL TRIBOLOGY..................................................................................................20
1.12. TEST FOR TRIBOLOGICAL PROPERTIES...........................................................................21
1.13. ALLOY COATING...................................................................................................................21
2. LITERATURE REVIEW..................................................................................................................24
3.1. SAMPLE PREPARATION...........................................................................................................33
3.1.1. Sample Preparation................................................................................................................34
3.1.2. Cutting...................................................................................................................................35
3.1.3. Drilling..................................................................................................................................35
3.1.4. Numbering.............................................................................................................................36
3.1.5. Surface Roughness Preparation..............................................................................................37
3.1.6. Cleaning.................................................................................................................................40
3.1.7. Sonication..............................................................................................................................40
3.1.8. Heating And Drying...............................................................................................................41
3.2. PHYSICAL VAPOR DEPOSITION (PVD) COATING...............................................................41
4. ANALYSIS.......................................................................................................................................47
4.1. TRIBO-MECHANICAL TEST.....................................................................................................47
4.2. NANO INDENTATION TEST.....................................................................................................48
4.2.1. Indentation Test Results Of Coating Time (15 Mint).............................................................51
4.2.2. Indentation Test Results Of Coating Time (60 Mint).............................................................52
4.2.3. Indentation Test Results Of Coating Time (120 Mint)...........................................................53
4.3. SCRATCH TEST..........................................................................................................................55
4.3.1. Case 1 Scratch Test................................................................................................................57
4.4. TRIBOLOGICAL ANALYSIS.....................................................................................................64
4.4.1. Tribo Testing.........................................................................................................................64
5.1. RESULTS AND DISCUSSION....................................................................................................68
6.1. CONCLUSION.............................................................................................................................73
REFERENCES..........................................................................................................................................74
LIST OF FIGURES
Figure 1 Coating techniques [11]...............................................................................................................15

Figure 2 PVD Coating process..................................................................................................................16
Figure 3 Knee and hip joint implants [16].................................................................................................21
Figure 4 Positive material gun (PMI) for material inspection....................................................................34
Figure 5 Sample cut in required shape from steel sheet.............................................................................35
Figure 6 Drilled samples............................................................................................................................35
Figure 7 Sample preparation......................................................................................................................37
Figure 8 Carbide papers.............................................................................................................................37
Figure 9 Diamond paste.............................................................................................................................38
Figure 10 Courtesy: The University of Punjab, Corrosion Engineering Lab.............................................39
Figure 11 samples before and after surface roughness...............................................................................39
Figure 12 Acetone.....................................................................................................................................40
Figure 13 Courtesy: The University of Punjab, Corrosion Engineering Lab.............................................41
Figure 14 Internal view of PVD coating machine during coating..............................................................44
Figure 15 Complete view of PVD coating machine at Iftikhar Trading Company (ITC)..........................46
Figure 16 Experimental setup and test performed......................................................................................47
Figure 17 Nano Indentation testing machine.............................................................................................49
Figure 18 Loading-unloading indentation curve of sample........................................................................51
Figure 19 Loading-unloading indentation curve of sample........................................................................52
Figure 20 Loading-unloading indentation curve of samples......................................................................53
Figure 21 Scratch test................................................................................................................................55
Figure 22 Scratch images for Case 1.........................................................................................................58
Figure 23 Acoustic emissions of case 1.....................................................................................................59
Figure 25 Acoustic emissions of case 2.....................................................................................................61
Figure 27 Acoustic emissions of case........................................................................................................63
Figure 28 Tribo Meter for tribo testing......................................................................................................64
Figure 29 Graphical curve of tribo tests.....................................................................................................66
Figure 30 Graph between hardness (H) and coating time (t).....................................................................69
Figure 31 Graph between Elastic modulus (E) and coating time (t)..........................................................70
Figure 32 Graph between Adhesion (A) and time (t).................................................................................71
Figure 33 shows coefficient of friction (CoF) vs time (t).........................................................................72
LIST OF TABLES
Table 1 Classification of samples before coating process..........................................................................42

Table 2 Coating parameters.......................................................................................................................45
Table 3 Indentation test parameters...........................................................................................................50
Table 4 shows the value of hardness (H) and Elastic modulus (E)............................................................54
Table 5 Machine parameters for scratch test..............................................................................................56
Table 6 Critical Loads for Case 1..............................................................................................................59
Table 7 Critical Loads for Case 1..............................................................................................................61
Table 8 adhesion values of sample from scratch test.................................................................................63
Table 9 Tribology test parameters.............................................................................................................65
Table 10 coefficient of friction values of the samples...............................................................................66
Table 11 comparison coated and uncoated 316L SS..................................................................................68
Table 12 comparison of result 30:70,50:50 and 80:20...............................................................................68
CHAPTER 1
1. INTRODUCTION
1.1. OVERVIEW
Stainless steel was first introduced in 1912-1913 (by Brearley in the UK and Maurer and
Strauss in Germany). Stainless steel includes Carbon (C), Nickel (Ni), Manganese (Mn),
Molybdenum (Mo), Copper (Cu), Silicon (Si), Sulphur (S), Phosphorus (P) And Nitrogen (N).
Stainless steel product forms include plate, sheet, strip, tube, bar, cold-formed and hot-rolled
structural sections, castings, fasteners and fixings. The stress-strain behavior of stainless steel is
different from that of carbon steel. stainless steel has a high initial material cost almost four times
of carbon steel. the stainless steel aesthetics has been an important factor in its specification for
applications [1]. The word ‘steel’ means that iron comprise the bulk of the material and stainless
is an adjective means absence of rusting, staining and corroding in environment. Three types of
microstructures exist in stainless steels, i.e., ferritic, austenitic and martensitic [2]. Steel is a
material that is used in various engineering applications, from the production of automotive parts
to biomedical implants. . Steel resist to rusting due to presence of chromium. Catalytic converter
and components of automotive exhaust systems are made up of stainless steel due to its
resistance against corrosion. steel is material that is very suitable for biomedical implant.
Biomedical material selection is very carefully examined because metals and their alloys
contact with human body for long time. Some metals and their alloys can show reaction with
other metals can cause harmful effects in human body [2,3] . There must be some properties
present in material according to utilization of material for the selection procedure of biomedical
inserts, medical equipment and devices. Some implants may be ductile and brittle [2] according
to point of application. Therefore, implant material selection depends upon the place of
utilization of material [2] (add reference). Stainless steel, cobalt chrome alloy, titanium and
nickel titanium alloy are commonly used materials for biomedical applications [3].
There is an increased demand of safety in addition to efficiency, strength and light weightiness,
in automobile and biomedical equipment design. Stainless steel is very cost effective and durable
option when our priority is safety. Due to high weight to strength density Stainless steel is not
suitable for manufacturing of automobile body as manufacturers and designers try to reduce
weight of automobile to compete the mileage of automobile with other companies therefore steel
is used for vehicle body manufacturing but many other parts of vehicles are made up of stainless
steel like catalytic converters, fuel tank and chasses [4]. Due to its qualities including ductility,
toughness, corrosion, and stress cracking, stainless steel is used in many places than just the
construction of automobiles and biomedical devices (restructure rather than utilize [5]. [5]
Titanium and Aluminium alloys were widely used in medicine, aerospace, and other fields.
Titanium is metal that gives result to higher weight of steel because it has high strength and low
density. In chemical, petrochemicals and aerospace industry, titanium is used in many
engineering applications due to its high strength to weight ratio provide weight saving [5].
Titanium has dual properties at high and low temperature give inertness and also has cryogenic
temperature for different structure. Pure titanium does not require regular maintenance therefore
it mostly used in petrochemical industries [6].
Metals, alloys, ceramics, and polymers are the commonly used as biomaterials. Biomaterials play
an important role in the modern era. Due to recent developments in medicine and material
processing, a great variety of biomaterials with characteristics employed in several applications
have been developed.. stainless steels are an important class of alloys from low-end to high-end
applications, like cooking utensils and furniture to space vehicle respectively [7]. This
metallurgical procedure involves mixing two or more metals, both the same and distinct to form
new element, having different properties as compared to parent element for example brass is the
first alloy which is made up of copper and zinc. Brass has its unique properties as compare to
properties of copper and zinc[6,7] Most common method to prepare alloy is powder metallurgy,
reduction method, fusion method and electro deposition method. Powder metallurgy is
characterized by formation of powder of and then blending the powder of different elements to
form an alloy powder. This alloy powder is sintered in controlled environment to bond the
particles.
1.2. TRIBOLOGY
Tribology covers a large section of science and technology. It plays a vital role in
mechanical, automotive engineering, industrial, biomedical engineering and many others
engineering applications. In our daily life we see many application of tribology. Tribology is the
study of friction, lubrication and wear in any interacting surface when surfaces are in relative
motion to each other [7] (add reference). Tribology is the important in biomedical implants and
pharmaceutical products like bone fixation, orthodontic wire filling and artificial joints [8].
Engine is the backbone of automotive industry, main component of engine is piston and cylinder.
Piston and cylinder in engine are in relative motion during the working condition. Engine
performance depends upon engine efficiency. Efficiency of engine depends upon its component
life. Lubrication is crucial to the study of tribology. restructure it too much use of plays
important role. It covers chemistry and mechanical engineering [8]Because they are moving
and rubbing against one another when cars are on roadways, many automobile parts and human
joints need lubrication.. Proper lubrication increases the life of engine performance and decrease
wear [9]. Friction also plays a vital role in tribology. Reduction in friction increases the fuel
efficiency of vehicle. Therefore, we can say that study of tribology is the most important role in
life of automobile components and reducing friction.
1.3. SURFACE ENGINEERING
Safe and clean environment is also basic need of now a day. Clean green energy is
sustainable development goal of the world. Thus, several contemporary surface engineering
techniques have been developed in this subject of surface engineering over the past few years.
treatments such as high-performance surface solutions, especially plasma deposition processes
have developed to provide cost effective, economic and stable solutions. Surface engineering is
technique in which we achieving required surface properties. It covers many fields aerospace,
automotive, chemical and petrochemical and construction industries. The technique has many
applications in biomedical[10]. In order to maintain straigh body posture, corrosion and wear
must consider in inserts and implants that replace the body part. Implant material must be
comfortable with human body. A lot of prosthesis work is done to produce stable, durable and
long lasting products.
1.4. THIN FILM COATING
Generally, coatings are used on metals and metal alloys. In biomedical engineering and
biomaterials research, surface coating is one of the most efficient methods for surface
engineering and modification. Coating provide a feature oflubrication to hold oil to give
lubrication to mating parts [11]
Several different coating techniques are currently being used in the industry based on its
application and requirement shown in Fig 1.

Figure 1 Coating techniques [11]
Two processes are usually used for coatings deposition:
 Physical Vapor Deposition (PVD) Coating
 Chemical Vapor Deposition (CVD) Coating
1.5. PHYSICAL VAPOR DEPOSITION (PVD)
A procedure called physical vapour deposition uses ions to create coatings or films in a
largely vacuum environment.. In this process, there is no chemical reaction takes place during
coating [11] . PVD also describes as a process of coating or prepare thin film on substrate surface
by producing ions. In PVD coating process, temperature can reach up to 600C and it should be
noted that melting point of substrate material should be higher than PVD coating process
temperature. PVD is not just used to create thin and fine layers; it may also create thick layers.
These are commonly used PVD coating process:

 Cathodic arc deposition
 High voltage triode electron beam
 Magnetron sputtering
 Low voltage electron beam
PVD
Cathodic Electron Pulsed Ion Beam
Sputtering Arc Beam Laser Assisted
Deposition Deposition Deposition Deposition
Figure 2 PVD Coating process
1.5.1. PVD Coating Properties
 High wear resistance
 Low coefficient of friction
 Fine grain
 Chemically inherent
 Good adhesion to substrate
 Low heat transfer coefficient
 Smooth surface morphology
 High toughness
 High hardness
1.6. CHEMICAL VAPOR DEPOSITION (CVD) COATING
Chemical vapor deposition is the process of coating in which material is not pure and it is
mixed with volatile precursor that acts as a carrier. Chemical reaction takes place during coating
process. The deposition process can be accelerated through plasma or heat.
Most commonly used CVD techniques are
 Laser Chemical Vapor Deposition (LCVD)
 Metal-Organic Chemical Vapor Deposition (MOCVD)
 Plasma Assisted Chemical Vapor Deposition (PACVD)
 Low Pressure Chemical Vapor Deposition (LPCVD)
 Photochemical Vapor Deposition (PCVD)
 Chemical Vapor Infiltration (CVI)
 Plasma Enhanced Chemical Vapor Deposition (PECVD)
 Atmospheric Pressure Chemical Vapor Deposition (APCVD)
1.7. TRIBOLOGY AND COATING CORRELATION
Coating of metal or metal alloy on different substrate prolong their properties. Metal and
its alloys have gained importance for its unique tribological and mechanical propertiesFor a
longer duration, titanium aluminium nitride coating has been improved.Tribology plays an
important role to obtain better mechanical and coating properties. In manufacturing of
automobile, the vehicle body requires highly thermal resistance to keep friendly environment
inside the vehicle. A body covers outer surface with diamond like carbon and PVD coating
process is applied. Result shows that improved tribological mechanical properties [12]. The
coating layers developed as a result of this technique is known as in-situ structured DLC layer.
The results of the in-situ structured DLC layer reveal that they improve the lightness and
dependability of machine parts. Successfull resultsare obtained by PVD coating of DLC.
Coating is carried out with this technique gives high elastic recovery and pass the
biocompatibility test for implant devices. This technique also used in biomedical and industrial
application.
1.8. EVALUATION OF TRIBOLOGICAL PROPERTIES
Friction, wear and lubrication are the basic properties that are mentioned under tribology.
Various types of coatings and surface enhancement techniques are used for tribo-wear
enhancements depending upon the requirements .In order to evaluate some of the tribological
properties, with the aim of improving tribological properties, for this purpose tribo-meter is is
utilized. This Tribo Meter is available in different forms like pin on disc, ball on disc, block on
ring, pin on flat and vacuum tribo-meter [13]. This meter is utilized for evaluation tribo related
properties.Testing conditions are varied according to application condition. In biomedical
implant, normal body flow condition is applied. Friction and wear of implants are measured
from tester by adjusting the conditions. In automobile engine, real time lubrication test is
difficult and much expensive but with the help of tester it is easy and show valid results on real
time conditions.
1.9. TRIBOLOGY AND SURFACE ROUGHNESS CORRELATION
Profilometer is a device which is used to measure surface roughness. In recent research
and development, companies and researchers focus on desired surface roughness with improved
tribo mechanical properties. Surface roughness of metal and alloy play a vital role in adhesion.
Roughness of materials achieved after coating also plays important role in tribological
properties. In case sliding, lower value of surface roughness is required to get better result.
Lower surface roughness will result in lower friction and increase the engine life and efficiency.
A vehicle needs a smoother surface because of the force of aerodynamics.. Better tribo-
mechanical in biomedical qualities demand materials with lower surface roughness.
1.10. CERAMIC COATING
Ceramic coating is the process in which ceramic is coated on another material for
creating new material properties. In Automotive Engineering, vehicle body is the application of
ceramic coating. Ceramic coating on vehicle body create a strong semi-permanent bond with the
paint but it cannot be used as replacement of paint just create a new set of properties on coated
surface.
Some ceramic coating properties are given below:
 Enhanced glow
 Protection from stains
 Ease of cleaning
 Protection from etching
 Protection for oxidation
Bioceramics is utilised to replace or repair broken bone tissues. Depending on the use,
bioceramics can directly interact with the tissue in the area, either promoting tissue growth or, in
the case of bioactive ceramics, triggering fresh tissue regeneration. Bioceramic play an
important role in modern medicine such as zirconia are hard alumina. These are chemically inert
material that can be polished to a high finish. Knee and hip joint are made up of ceramic coating.
Ceramic coating is used in dental implant and orthopedic operations.

Modern ceramics are employed in a growing number of sectors, including fridge magnets.
including metal production and processing, electronics, aerospace, personal protection and
automotive [14]. Some advance ceramics are:
 Typical oxides used are alumina (Al2O3) and zirconia (ZrO2)
 Non-oxides are often carbides, borides, nitrides and silicides, for example, boron carbide
(B4C), silicon carbide (SiC) and molybdenum disilicide (MoSi2)
1.11. BIOMEDICAL TRIBOLOGY
Many human body parts are in relative motion to each other like bones, teeth and heart valves.
Tribology has an importance for making biomedical equipment and implants. Many devices are
involved with relative moving parts, either in contact to tissues or within the biomaterials.
Friction and wear have a negative impact on natural tissues in addition to affecting how tissues
operate. [15].
one million artificial joints implanted yearly into patients world-wide [16]. Artificial joints are
most important and successful medical device used in human being. Surface of artificial joints
are made up of biomaterial combinations. Stainless steel is first generation of biomedical
materials. Then comes the alloys of cobalt and chromium that are termed as second generation of
biomedical materials. These alloys are used in fabrication of artificial hip and knee joints because
of wear resistant properties. Titanium alloys are very important, Titanium and its alloys are the
third generation biomedical materials that fulfil most of mechanical, tribological and
biocompatibility tests. particularly for total disc replacements in the spine, due to its lower elastic
modules (E) [17].

Figure 3 Knee and hip joint implants [16]
1.12. TEST FOR TRIBOLOGICAL PROPERTIES
Hardness (Mechanical property), adhesion (scratch properties), wear, and coefficient of
friction (tribological properties) are the important parameters achieved as result of coating in
most of industrial applications. Nano indentation test is performed for hardness. Diamond
indenter is used in machine for precise calculations. Hardness value is calculated by applied load
and corresponding displacement curve. Friction and wear are measured by tribometer. Friction,
wear will be improved as a result of coating. Scratch test are used for adhesion between substrate
and coating layer.
1.13. ALLOY COATING
Coatings of different metal on substrate materials are done for getting improved tribo-
mechanical properties. Recently, alloy coating has made its way to the industry for its range of
properties. Alloys of different proportions can be coated through physical vapor deposition
(PVD) method. Alloy coatings have resulted improvements in cost effective coatings with
improved tribo-mechanical properties.
Commonly used substrate metals for alloy coatings include:

• Stainless steel
• Titanium
• Aluminum
• Zinc
• Chromium
• cobalt
• Nichrome
• Bronze
In our experimental research work, we have selected stainless steel(SS) as the substrate surface
and alloy of titanium and aluminum for coating. We have performed coating of titanium
aluminum nitride in two different ratios on stainless steel.
Mileti et al. 2014 [37] highlighted how important base material roughness is in determining the
coated material's adherence. He conducted a number of studies using different base materials'
surface roughness. Their research indicates that the overall adhesion will increase with surface
roughness.. They demonstrated the same through his (her) experiments.
Lorenzo-Martin et al. [38] demonstrated that the coating thickness is the most crucial factor in
determining the efficacy of coating techniques. In the case of the CrN coating, he demonstrated
how the quality of the coating may be altered by simply adjusting the thickness, and in doing so
provided a significant basis for understanding the relationship between coating thickness and
tribological properties.
Martinez et al. [39] examine the coatings' chemical and physical characteristics. He
demonstrated how changing the coating time can alter the coating thickness. By adjusting the
coating period, he was able to achieve coating thicknesses ranging from 20 to 120 nm in his
experiment.
Arc evaporation is the method of coating used in this research effort, which makes it extremely
distinctive and adds the element of novelty to it. Gahlin et al. [40] discuss the physical vapor
deposition process. He connected numerous physical qualities of the material with the chemical
composition of the basic material, which is distinctive feature of their research. The compressive
stress and hardness values of the TiN coatings have significantly increased as a result of their
work. He has connected the micro level structural impact to the rise in the harness, elastic
modulus, and compressive stress. Gahlin's research is thus very important to the field of coated
surface tribology
CHAPTER 2
2. LITERATURE REVIEW
In this rowing world of science and technology, Stainless Steel (316 L SS) is material
used in engineering application from manufacturing automotive parts to biomedical implants.
316 L SS and titanium alloy used in bio-medical implant manufacturing as bone plate materials
and many pharmaceutical products. In automotive industry SS 316L is used in manufacturing of
fuel tanks, 50% exhaust system are made of 316 L SS along with chassis of trucks and bus and
Components of automotive engines.
Biocompatibility of titanium, it mostly used in biomedical equipment and implants. Titanium and
its alloys remains inert at very high temperatures without reaction and highly resistant to
corrosion under oxidizing, neutral and reducing conditions. Aluminum because of its unique
characteristics has been used in automotive industry. Aluminum as the clear choice of
automakers because of its environment friendly nature and high strength to weight ratio.
Titanium aluminum nitride coatings have been performed for a longer period of time
Alloy coating has recently gained importance for its unique mechanical and tribological
properties. Achieving better mechanical and tribological properties are directly related to coating
of metal or metal alloys on substrate surfaces
Subramanian et al. (2011) studied Electrochemical corrosion behavior and cytotoxic effect
studied in this paper. DC reactive magnetron sputtering method is used. Titanium substrates were
machined using conventional turning and wire cut through electric discharge machining (EDM)
from commercially pure titanium conforming to ASTM B348 Grade 2. This was done by hand
emerging using SiC emery papers (240to 600) mess sizes. Final polishing was taken out using a
centrifugal tumbling machine. The vacuum of the chamber was below 1.33 × 10−4 Pa and the
substrate temperature was kept at 400 °C. High purity argon was fed into the vacuum chamber
for the plasma Structural analysis was studied of titanium nitride (TiN), titanium oxynitride
(TiON) and titanium aluminum nitride (TiAlN) coated on titanium by DC magnetron sputter
deposition. TiAlN coating showed high corrosion potential and high resistance for corrosion than
others under simulated body flow condition. All these three coating did not produce toxic
material, hence passed cytotoxic test [17].
Ipaz et al. (2012) investigated mechanical, structural and tribological properties of steel, coated
with double layer of titanium aluminum and titanium aluminum nitride on silicon (100) and AISI
D3 steel substrate. the pressure of vacume chamber is 10-6 mbar and deposition coating time is 20
minutes. The mechanical analysis are performed via nano-indentations by an Ubi1-Hysitron
device and a diamond Berkovich tip at different loads [18]. Magnetron co-sputtering pulsed DC
method is used Double layer coating on steel improved its properties by applying magnetron co-
sputtering pulsed DC method. Double layer of coating showed better result of hardness and
elastic modulus. Adhesion friction coefficient showed optimum value in double layer coating
Aihua et al. (2012) carried out studies on friction and wear properties of some coated cemented
carbides. Cathodic arc evaporation method was used for titanium aluminum nitride (TiAlN),
aluminum titanium nitride (AlTiN), titanium nitride (TiN) and chromium aluminum nitride
(CrAlN) coating. Test were conducted by scanning electron microscopy and using ball on disc
method on CETR UMT-2micro tribo meter. SEM (scanning electron microscope) was used to
examine the cross section and micro structure of wear. Hardness is measured by hardness tester.
Optical profilometer is used for analysis of surface roughness of coating. Coatingsurface is
smooth and uniform. Experimental result showed improvement in coefficient of friction and
wear resistance properties. Friction coefficient of TiN < TiAlN< CrAlN< AlTiN. High value of
friction coefficient of Aluminum titanium nitride was due to high aluminum content. Titanium
nitride showed least friction coefficient value than others [19].
Samani et al. (2015) investigated thermal conductivity and thermal diffusivity of single and
double layer of titanium nitride and titanium aluminum nitride coating deposited on 304 stainless
steel to improve the efficiency of cutting and forming tool. Lateral Rotating cathodic arc is used
in this experiment. There are two cathodes rotating at a speed of 12 revolutions per minute
during coating deposition on 304 stainless steel. Direct current is applied on two cathodes to
control the composition of deposited coating Multilayer coating is superior to single layer in
many mechanical properties [20]. In this experiment deposition time is fixed. Grain size of
coating decrease with increase bilayer coating. Result showed that coating of single and double
layer reduced thermal conductivity. Increasing the coating layer decreased the value of thermal
conductivity therefore we can say that thermal conductivity depends on coating microstructure
and number of layers.
Kong et al. (2016) carried out research on corrosion resistance pattern of different alloys using
unbalanced magnetron sputtering method. In artificial sea water. Corrosion behavior is
investigated. Electrochemical properties of chromium nitride coating doped with aluminum and
titanium under sea water conditions were studied. During the deposition process, the pressure
was remained at 4.0 × 10-4 Pa in the chamber. Chromium nitride gives favorable corrosion
resistance with higher charge transfer resistance [21]. Corrosion resistance pattern was as such
that chromium aluminum nitride < Chromium nitride < chromium titanium nitride. Electrical
resistivity of these materials measured was in sequence of chromium titanium nitride <
chromium nitride < chromium aluminum nitride. Chromium nitride coating gives better
compactness than other coating and also show that stronger anti corrosion behavior. In this
research work, improved mechanical such as hardness and tribological properties.
Ishigaki et al. (2018) evaluated the results of Effect of aluminium content on mechanical and
structural properties of titanium aluminium nitride. Chemical vapor deposition method was used
to coating TiAlN on cemented carbides. Nano indentation and adhesion test is investigated in
this research. The effect of aluminium content in aluminium titanium nitride on mechanical and
structural properties has been studied. Hardness and adhesion decrease with decrease in
aluminium content [22].
Ozkan et al. (2018) analyzed the three coatings of titanium aluminium nitride, aluminium
titanium nitride and aluminium chromium nitride on steel surface at different lubrication
conditions and their properties for cam tappet in IC engines which run on condition of boundary
lubrication. Coefficient of friction values were observed at steady state condition [23].. Elastic
modulus of AlCrN < AlTiN < TiAlN and hardness of TiAlN < AlCrN < AlTiN
[24] Zhang et al. (2018) studied tribological properties and COF values of titanium aluminum
nitride coated on substrate at three different nano surface structure. These three surfaces coated
with titanium aluminum nitride improved friction properties and macro/nano showed best result
and also improved tribological properties like less value coefficient of friction
Al-Bukhaiti et al. (2014) investigated the structural, mechanical, tribological properties of coated
titanium nitride, titanium aluminum nitride and TiAlCN on steel. Physical deposition method
was used for coating [25]. The properties were elaborated for aluminum oxide Al2O3 and
chromium tool for sliding and normal conditions. X rays diffraction analysis done on different
stages as TiN, AlTi3(CN) and AlTi3N. Conclusion showed increase in adhesion and hardness
due to carbon content and multi-layer coating. Wear rate and friction coefficient of coated
sample were lower than uncoated sample. Chromium tool sliding system showed lower friction
and wear than Al2O3 tool sliding system
Uddin et al. (2018a) Mechanical and tribological properties of titanium nitride on bearing steel
were studied. Titanium nitride is deposited by physical deposition method. Experiments were
performed at four different values of coating thickness and two surface roughness values.
Experimental results showed adhesion and elastic modulus of titanium nitride increased with
increased coating thickness for both fine and rough samples but rough sample showed high
adhesion than fine surface [26]. Hardness of titanium nitride increased up to a critical value of
coating thickness but after critical value it declined with increase in coating thickness. Result
also showed that tribological properties like wear and COF decreased with increase in coating
thickness. Both mechanical and tribological properties showed improvement at higher roughness
values
[27] Uddin et al. (2018b) explored the Tribological and micromechanical properties of four
diesel engine piston ring cylinder liner (PRCL) interface system. Titanium nitride is deposited by
PVD method. Experiments were performed at three different values of coating thickness and two
surface roughness values. Different tests were performed to assess the adhesion, hardness and
coating thickness. Experimental result showed that adhesion and hardness increased with
increased the coating thickness but higher roughness sample showed higher properties than lower
roughness sample. COF decreased with increase in coating thickness when titanium nitride
coated cylinder liner interface with titanium nitride coated piston rings but coefficient of friction
increased with increase in thickness when titanium nitride coated cylinder liner interface with
chromium coated piston ring. Rough samples have higher COF than fine samples
Uddin et al. (2019) carried out experimental studies on Tribological, mechanical and chemical
properties of titanium nitride for implants applications. Experiments were performed at two
different values of surface roughness. Experimental results showed surface roughness 0.4µm and
coating thickness 3.3µm gave optimum results of hardness, COF, wear rate, corrosion resistance
and adhesion strength in simulated body fluid. Results also showed that titanium nitride coated
were eight times more corrosion resistance and four times more wear resistance than bare
titanium substrate [28].
In order to determine the overall effectiveness of the implants, Diamond et al. [29] looked into
the joint angles for level gait, including flexion, extension, abduction, adduction, internal
rotation, and external rotation.
[30] elaborate the importance of thermal stability of coatings performed for improved tribo-
mechanical properties. magnetron sputtering method is used in four different coating, were
performed on steel substrate by the and tribo-mechanical of all samples were investigated. Effect
of change in the properties were observed as a result of different thermal treatments of all the
samples. Results of scratch tests highlighted the importance of carbon based films that are
observed to be soft and exhibits improved frictional behavior even at elevated temperatures.
Tribological Mechanical Properties Study of Chlorinated Titanium Nitride on stainless steel
surface. Tested for tribo-mechanical properties. It is carried out in the presence of lubricants.
Hank's Balanced Salt solution (HBSS) and a mixture of HBSS and bovine serum albumin (BSA)
Used as a lubricant. The test results were very good and meaningful. Wear reduction was
achieved on HBSS lubricated surfaces. to attract The reduction is due to the presence of a soft
titanium oxide layer. better The results of the coefficient of friction were obtained in the case of
lubrication of the mixture. In both cases, improved associative properties were obtained
Recommended use of titanium nitride coatings in biomedicine Applications [31].
After investigating titanium nitride, titanium niobium nitride, and titanium carbon nitride, A.P.
Serro et al. proposed titanium niobium nitride as a coating material for wear-resistant ortho joint
implants. This material was chosen following extensive tribomechanical and cytocompatibility
testing [32]. The outcomes of each test revealed that the coated surfaces all had the same surface
characteristics and fulfilled the biocompatibility test. On both direct and indirect contact with
cells, no surface generated any toxic materials. Because of the protein layer which was absorbed
on the surface, TiNbN was ranked first in tribological tests as tried to compare to other coated
surfaces.
On the substrate of titanium, aluminium, and zirconium, S. Sathish carried out comparative
investigation of single and double layer ceramic coatings of nanostructured aluminium, titanium,
and zirconium alloy (Al2O3-13TiO2, ZrO2) (Ti-13Nb-13Zr). Plasma spray coating was used to
coat both single and multiple layer surfaces [33]. In order to investigate the potential for these
two materials in biomedical applications, reciprocating wear experiments on both samples were
carried out under simulated body flow circumstances. Both samples underwent wear tests in
Hanks solution, and the wear rate was determined using the weight loss method with an
electronic balance with an accuracy of 0.0001g. All samples underwent scratch and hardness
tests in order to determine the degree of adhesion. Comparing double layer coating to other
samples, harness tests revealed that it had the highest level of toughness.
[34] J. Probst et al. investigated the wear-resistant adhesive characteristics of titanium samples
covered with mixed binary crystals of titanium, niobium, and zirconium oxynitrides and nitrides.
The enhancement of tribo-mechanical characteristics brought about by coating was investigated.

Additionally, biocompatibility tests were carried out for application in the relevant field. The
results of the tests done on the samples showed that the hardness had improved and the oxygen
content increased the biocompatibility. Based on the findings, titanium, niobium, and zirconium
oxynitride binary coatings can be employed to increase hardness.
Biomedical model is a broad field with a variety of applications that require a wide range of
materials. By co-sputtering titanium, zirconium, niobium, tungsten, and hafnium multi-principal
element coatings on an alloy comprising titanium, aluminium, and vanadium, Braic et al. [35]
examined the following properties are element composition, phase composition, crystalline
structure, morphology, residual stresses, hardness, friction performance, wear resistance,
corrosion resistance and cell viability.
The results of tests done on samples coated with many layers of carbide and nitride showed a
tremendous improvement in characteristics. The hardest coating outperformed the other two was
carbide. With a coefficient of friction of 0.12, the coating with the highest carbon content also
demonstrated the greatest resistance to wear. Wear resistance tests carried out under artificially
created simulated body flow circumstances yielded better results with the greatest resistance for
carbide samples. All samples were examined by osteoblasts for 72 hours to determine their
biocompatibility, and none of the samples elicited a cytotoxic reaction. These multi-principal
element coatings with carbide and nitride coatings can be used in biomedical applications due to
the enhanced tribo-mechanical qualities they have attained.
Perillo [36] identified the prerequisites needed for the cathodic arc technique of deposition. In his
research, he provided explanations for various parameters, including the required voltage, the
chamber pressure, and the nitrogen to argon ratio. Using Perillo's research, it is possible to derive
the general base conditions that are required.

Through their research, Lorenzo-Martin et al. [38] demonstrated that the coating thickness is the
most crucial factor in determining the efficacy of coating techniques. In the case of the CrN
coating, he demonstrated how the qualities of the coating may be altered by simply adjusting the
thickness, and in doing so provided a significant basis for understanding the relationship between
coating thickness and tribological capabilities.

CHAPTER 3
3.1. SAMPLE PREPARATION
A sheet of 316L stainless steel sheet was purchased from the market. sheet was composition
of pure 316L stainless steel. Positive material gun was used for testing the sheet. After
confirming the pure 316L stainless steel sheet. Coating process was carried out at a laboratory in
Sialkot. Three different coating thicknesses were coated by changing coating time
• T1= 15 minutes
• T2= 60 minutes
• T3= 120 minutes
After successful completion of PVD coating process, all samples were tested for mechanical and
tribological tests. Mechanical properties for testing include hardness and adhesion and
tribological properties include coefficient of friction

Figure 4 Positive material gun (PMI) for material inspection
3.1.1. Sample Preparation
316L stainless steel samples were prepared for performing coatings by passing through
following processes
 Cutting
 Drilling
 Numbering
 Surface roughness preparation
 Cleaning
 Sonication
 Heating and drying

3.1.2. Cutting
Electric discharge machine wire cut machines was used for cutting samples having
dimensions (19 mm diameter and 2.5 mm thick). Samples were cut from sheet of required coin
shape using EDM. Figure shows the sample prepared from the steel sheet
Figure 5 Sample cut in required shape from steel sheet
3.1.3. Drilling
After cutting the samples from the SS sheet, then drilling machine was used for small
hole and drilled at the corner of each sample of just 1mm diameter. In coating process, samples
were hanged on the hanger present in coating machine. The position of hole in the corner of the
sample because hole was not effected coating process and properties of substrate.
Figure 6 Drilled samples

3.1.4. Numbering
After drilling process, numbers were punched on all samples near the drilled holes to
identify the samples during coating and experimentation. Punching machine is used for
numbering
Figure 3.4: Numbered samples
Figure 7 Sample preparation

3.1.5. Surface Roughness Preparation
Samples are ready to create desired surface roughness. Silicon carbide paper also called
emery paper are used. Different grit range of paper available in market like 100 grit to 5000 grit
paper. SiC grinding papers of 100, 500, 320, 1000, 800, 1200, 2000, 1500, 2000, 3000, 2500, and
4000 grades were utilized to finish the samples.
When we require fine to ultrafine substrate finish moving towards lower grit to higher grit.
samples were rubbed on emery papers with hands covered with gloves.
Figure 8 Carbide papers
Diamond paste is used for final polishing

Figure 9 Diamond paste
 First nine samples of roughness less than 0.1 µm
 Ten to eighteen samples of roughness in between 0.1 µm to 0.2 µm
 Nineteen to twenty-seven samples of roughness in between 0.2 µm to 0.3 µm
Lower and higher surface roughness value were gained by using higher grade and lower
grade of carbide paper respectively. Twenty to thirty minutes were spent on each sample for
surface preparation. Both side of samples were prepared for coating and same roughness
value achieved for both sides of samples.
Profilometer Mitutoyo SJ-201 was used to measure the surface roughness in Punjab university
Corrosion Engineering Lab

Figure 10 Courtesy: The University of Punjab, Corrosion Engineering Lab
Figure 11 samples before and after surface roughness

3.1.6. Cleaning
After preparing the desired surface roughness, all samples were cleaned by using acetone
to remove any dust particles on the surface. Sample properties were affected by other material
and hydrocarbons. After completing the acetone cleaning process by hand.
3.1.7. Sonication
After preparing the samples of desired surface roughness, then samples are ultra sonicated for
least in five minutes at temperature of 80󠇈degree centigrade.
Figure 12 Acetone
Figure 13 Courtesy: The University of Punjab, Corrosion Engineering Lab
3.1.8. Heating And Drying
After sonication, samples were heated in a heater to a higher temperature of 900 to 1000C just
before coutting them to PVD coating machine. Heating of samples at high temperature dries the
samples that were in wet state after sonication. Heating of substrate samples to a higher
temperature and drying process prepares them for performing coating. Samples were put in to
plastic bags after drying.
3.2. PHYSICAL VAPOR DEPOSITION (PVD) COATING
Iftikhar Temper Company (ITC) Sialkot applied PVD coating on samples. It is one of
Pakistan's premier industries that offers a variety of PVD coating services. On finish applying the
coats to the three group of samples, all samples were hung on the PVD coating machine's hooks
before being introduced in the machine

Table 1 Classification of samples before coating process
Group No. Set No Surface Coating time No of samples
Roughness
First 1st >0.1 15 minutes 3
2nd 0.1 to 0.2 3
3rd 0.2 to 0.3 3
Second 4th >0.1 60 minutes 3
5th 0.1 to 0.2 3
6th 0.2 to 0.3 3
Third 7th >0.1 120 minutes 3
8th 0.1 to 0.2 3
9th 0.2 to 0.3 3
Targets of 80:20 titanium aluminium alloy were installed and the first set of samples were added
to the machine. Figure depicts the samples after they have been installed in the machine, hanging
on the hangers. Lack of air in the coating machine and creation of a vacuum are essential
conditions for high density PVD coating. After creating a vacuum inside the chamber of around
1.0 x 10-3 Pa, voltage was then applied to remove material from targets and coat the samples.
The arc between the target cathode and substrate anode discharges when power is applied to the
PVD device. The cathode becomes the focal point of the arc current, which increases the current
density there. The cathode mode transitions from a solid state to a plasma as a result of the high
current and high density. Under vacuum, the freshly produced plasma immediately travels to the
anode layer. The actual vapour is deposited on the sample substrate, but plasma ions exhibit
differing kinetic energies, with light molecules having a kinetic energy of around 20 electron
volts and heavy molecules having a kinetic energy of about 200 electron volts. To preheat
samples and encourage the creation of a coating layer on the substrate surface, the temperature
within the chamber is kept at roughly 250C. Nitrogen, an inert gas that aids in the evaporation of
the titanium aluminium alloy from the target surface, is also given throughout the coating
process. So under these condition
 Vacuum pressure
• High temperature
• High voltage
• Nitrogen supply
Figure 14 Internal view of PVD coating machine during coating
The surface of the substrate is coated with the desired alloy, and coating thickness is adjusted by
varying coating time. When the coating process is finished, the bias voltage is withdrawn, and
the coating process is then terminated. When the applied bias voltage is removed, the coating
process truly ceases, and the chamber's temperature gradually drops to about 50C. Normal
pressure is also kept inside the PVD machine chamber to enable the removal of coated samples
from the chamber. Heaters are turned off to lower the temperature of the chamber, and then fresh
air or pure oxygen is supplied to maintain pressure. Normal pressure, normal temperature, and
the removal of the bias voltage really make it possible to remove samples from the chamber in its
current state. Actually, coating time is measured from the moment bias voltage application
begins till the time. The amount of time needed to create vacuum pressure and for post-
processing is not factored into the coating time. The real coating period is when the material
from the alloy target is removed and applied to the substrate's surface. The coating time does not
account for preheating or post-processing time. As shown in the tables above, the first group of
set A samples are coated for 15 minutes, followed by the second group of set A samples for 60
minutes, and finally the coating process is completed for 120 minutes. Three distinct coating
times result in samples with three different coating thicknesses.
Table 2 Coating parameters
Basic Bias Current Temperature(C) Nitrogen Argon flow Deposition
voltage flow rate rate (sccm) time (mint)
(sccm)
60 90 250 350 20 15
60 90 250 350 20 60
60 90 250 350 20 120

Figure 15 Complete view of PVD coating machine at Iftikhar Trading Company (ITC)
. Coating machines used for performing above mentioned PVD coatings at Iftikhar Temper
Company (ITC) are shown in Fig3.13. Coating process was completed in three different time 15,
60, 120 minutes of fine intermediate time

CHAPTER 4
4. ANALYSIS
4.1. TRIBO-MECHANICAL TEST
This chapter explain the test performed and measurement of Tribo-mechanical properties
of 316L stainless steel by 80:20 titanium aluminium alloy target based PVD coating of all the
samples. This chapter also cover testing parameters and equipment feature details during
experimental testing. In order to investigate the properties of titanium aluminium nitride coating
on 316L stainless steel substrate. Mechanical and tribological tests were conducted on the
samples.
Experimental Setup
Mechanical Test Tribological Test
Nano Indentation Test (Hardness Scratch Test (adhesion) COF Friction

and Elastic Modulus)
Figure 16 Experimental setup and test performed
Nano hardness Test
 Hardness
 Elastic Modulus
Scratch test
 Adhesion
Tribological Analysis
 Coefficient of Friction (COF)
These are the test performed on the samples in order to evaluate the tribological and mechanical
properties of titanium aluminum nitride coating on316L stainless steel substrate.
4.2. NANO INDENTATION TEST
Nano indentation method is employed to measure the mechanical properties (Hardness
and Elastic modulus) of titanium aluminum nitride coating on 316L stainless steel substrate.
Nano indentation tests were also performed in Pakistan Council of Scientific and Industrial
Research (PCSIR). Nano indentation tests were carried out on machine (NHTX S/N: 01-2569).
Figure 17 Nano Indentation testing machine
Hardness values of TiAlN coated stainless steel samples is measured by performing Nano
indentation test. Test is a performed on samples, one sample from each group and all surface
roughness (Fine, Intermediate, Rough) of each group. Diamond indenter is used to load and
unload linearly on samples at the rate of 10mN/min. An indenter with the known geometry is
employed to penetrate into the coating. During indentation process, a record of the depth of
penetration is made, and then the area of the indent is determined using the known geometry of
the indentation tip. While indenting, various parameters such as load and depth of penetration
can be measured. A record of these values can be plotted on a graph to create a load-
displacement curve. Measurement of penetration depth at the corresponding normal force
provided the hardness value
Time and penetration depth are also drawn against each other. Indentation test also performed on
all samples.
Table 3 Indentation test parameters
Indentation Parameter
Instrument NHTX S/N: 01-2569
Dz Sensor Fine Range
Delta Slope Contact 100%
X Position 59.56 mm
Y Position 10.70mm
Hardware setting Linear Loading
Approach Speed Fine Range
Measurements
Loading Linear Max Load 10.00 mN
Loading rate 10.00 mN/min
Unloading rate 10.00 mN/min
Pause 10.0 s
Indenter
Type Berkovich
Serial Number BJ-48
Material Diamond
4.2.1. Indentation Test Results Of Coating Time (15 Mint)
Indentation test result performed under mentioned conditions the table are plotted in
terms of graphs. Normal force applied and indentation depth are plotted against each other to
calculate value of hardness (H) for the sample.
Case 1 Nano Indentation
Coating Time: 15 minutes TiAlN=80:20, Sample 1
Figure 18 Loading-unloading indentation curve of sample

calculate value of hardness (H) for the sample. Indentation results for the sample are shown in
Fig
Figure 19 Loading-unloading indentation curve of sample

calculate value of hardness (H) for the sample. Indentation results for the sample are shown in
Fig
Figure 20 Loading-unloading indentation curve of samples

Indentation test results of each sample are plotted in the form of graph. Normal force and
penetration depth are plotted against each other
Pmax
Hardness ( H )= P max = Force (Load)
A
A = Area of Indenter
E lastic Modulus =
S
2β √ π
A
sS = Slope of line
𝛽 = Machine Calibrated value
A = Area of Indenter
Nano Indentation results
Table 4 shows the value of hardness (H) and Elastic modulus (E)
Roughness Level Elastic Modulus Hardness

Sample ID
Ra (Gpa) (Gpa)
F-15 122.9 10.39
Fine F-60 30.7 3.45
F-120 66.5 7.37
I-15 94.6 12.31
Intermediate I-60 51.3 5.51
I-120 32.3 3.54
R-15 54.2 6.97
Rough R-60 35.5 5.73
R-120 43.9 3.66

4.3. SCRATCH TEST
Measurement of adhesion for the samples is carried out by performing scratch test on
them. A stylus is moved over a specimen surface with a linearly increasing load until failure
occurs at critical loads.
Figure 21 Scratch test

As substrate surface roughness also affects the adhesion of coating so this test was performed on
three samples, one sample from each group and each roughness level in all groups. During this
test Rockwell indenter of diamond was used and load was gradually increased to produce linear
type of scratch. Acoustic emissions were also recorded during test and pictures of samples during
test were taken at four critical loads. Acoustic emissions at critical loads helped in determination
of adhesion of samples. Adhesion values of all three samples were measured and testing
parameters were kept same during all tests.
Table 5 Machine parameters for scratch test
Scratch parameters
Scratch direction Linear
Type Progressive
Begin load 0.03 N
End load 27 N
Speed 2.5 mm/mint
Approach speed 2 % / sec
Indenter
Type Rockwell
Material Diamond
Radius 100 µm
Adhesion of the coatings was measured quantitatively by scratching them with the Rockwell
type diamond stylus 100-μm radius. The instrument can measure critical load, acoustic emission,
and the penetration depth simultaneously. The applied load was starting from 0.03 N and ended
on 30 N. The scratch length and loading rate was 3 mm and 9.99 N/min respectively during the
scratch tests
4.3.1. Case 1 Scratch Test
Coating time: 15 minutes TiAlN = 80:20 Sample 1
Table 4.4: Critical Loads for Case 1
Critical Load Newton (N)

Lc1 4.84
Lc2 8.76
Lc3 12
End of Scratch 25.33
Figure 22 Scratch images for Case 1
Figure 23 Acoustic emissions of case 1
Hence the critical load in the above-mentioned testing activity is almost 25.33 and it must be
remembered that above this point, the load becomes quite significant
Table 6 Critical Loads for Case 1

Lc1 6.5
Lc2 10.71
Lc3 16.77
Figure 25 Acoustic emissions of case 2
Table 7 Critical Loads for Case 1

Lc1 4.17
Lc2 6.91
Lc3 10.14
Figure 27 Acoustic emissions of case
Table 8 adhesion values of sample from scratch test
Roughness Level Sample ID Adhesion

Ra (N)
F-15 8.76
Fine F-60 8.94
F-120 5.3
I-15 3.1
Intermediate I-60 9.68
I-120 10.71
R-15 6.91
Rough R-60 10
R-120 6.36
4.4. TRIBOLOGICAL ANALYSIS
Tribology tests are performed on three samples of each group including all surface
roughness for measurement of coefficient of friction. Tribology tests are performed by tribo
tester at Pakistan council of scientific and industrial research (PCSIR). Samples of all three
groups including all surface roughness are tested for tribology to determine the effect of coating
time on the coefficient of friction. Tribology tests are performed under lubricating conditions and
humidity of 30.00%. Graphical curve for each sample is generated by the tester consisting of
penetration depth and coefficient of friction.
4.4.1. Tribo Testing
In tribo-meter, a pin is loaded onto the test sample with a precisely known force. The probe is
mounted on a stiff lever, designed as frictionless force transducer. The friction coefficient is
determined during the test by measuring the deflection of the elastic arm
Figure 28 Tribo Meter for tribo testing
The amount of time needed to create vacuum pressure and for post-processing is not considered
into the coating time. The real coating period is when the material from the alloy target is
removed and applied to the substrate's surface. The coating time does not account for preheating
or post-processing time. As shown in the tables above, the first group of set A samples are coated
for 15 minutes, followed by the second group of set A samples for 60 minutes, and finally the
coating process is completed for 120 minutes. Three distinct coating times result in samples with
three different coating thicknesses.
As a result, information regarding substrate cleaning, maximum speed, and humidity can be
easily assessed, and this information is also included in our calculation of the co-efficient of
friction, the findings of which will be described in relation to each sample
All samples were subjected to tribology testing under these circumstances, and the results were
graphed as with other experiments.
Under lubricated conditions, tribology experiments were conducted, and the coefficient of
friction was computed.
Table 9 Tribology test parameters
Tribo Testing Parameters

Radius 3.01nm
Linear speed 7 cm/sec
Normal load 4N
Stop condition 13513 laps
Environment Conditions
Temperature 25 degree centigrade
Humidity 30 %
A pin is loaded with a precisely determined load on the test sample or substrate in a tribometer.
The same is used in our computation of the co-efficient of friction, and the findings will be
compared to each sample. The frictionless force transducers are an assembly that consists of a
stiff lever mounted with a probe. In the investigation, the entire deflection of the elastic arm is
determined in order to calculate the coefficient of friction. The parameters for the measurement
of tribological properties are of special importance, just like in the scratch test calculation,
because they enable the determination of final results, which will be covered in great detail in the
results portion also the overall impact it creates on the physical properties will be considered.
Figure 29 Graphical curve of tribo tests
In this graph, red green line shows the value of friction coefficient and penetration depth.
Initially when time is zero coefficient of friction is high, after some time coefficient of friction
decreases. When load is applied continuously depth is increase according to load applied
Table 10 coefficient of friction values of the samples
Roughness Level Coefficient of Friction

Sample ID
Ra (CoF)
Fine F-15 0.190
F-60 0.575
F-120 0.432
I-15 0.181
Intermediate I-60 0.490
I-120 0.264
R-15 0.447
Rough R-60 0.137
R-120 0.189
CHAPTER 5
5.1. RESULTS AND DISCUSSION
Test Uncoated 316L SS Coated 316L SS
Hardness GPa 1.52 12.31
Coefficient of friction > 0.2 0.137
The investigation of test findings on samples of titanium aluminium nitride coated stainless steel
is covered in this chapter. In this chapter, all the findings from Chapter 4 are carefully examined,
and the effects of surface roughness and coating thickness on hardness, adhesion, wear rate, and
coefficient of friction are discussed.
Hardness and Elastic modulus value increase in coated TiAlN on 316L SS as compared to
uncoated. Coefficient of friction decrease in coated TiAlN on 316L SS as compared to uncoated
Table 11 comparison coated and uncoated 316L SS
Maximum adhesion values are observed at 50:50 coating due to high deposition time. Average
coefficient of friction values of 50:50 coatings are observed to be low in comparison to 80:20
and 30:70 coatings. Comparison of the results have been made with 50:50 & 30:70 to 80:20
TiAlN coatings on the same substrate.
Table 12 comparison of result 30:70,50:50 and 80:20
Test Results 80:20 50:50 30:70
TiAlN
Hardness 12.31 24.08 13.9
GPa
Adhesion 10.71 18.48 10.49
Coefficient of 0.137 0.081 0.101
friction
Figure 30 Graph between hardness (H) and coating time (t)
In this graph, sample having roughness lies between 0.1 to 0.2 (Intermediate sample) and coating
time is fifteen minutes show high value of hardness as compared to all other samples of different
roughness and coating time. Sample having roughness < 0.1 (Fine sample) and coating time sixty
minutes show least value of hardness. Therefore, we can say that hardness depends upon surface
roughness of substrate
Figure 31 Graph between Elastic modulus (E) and coating time (t)
In this graph, sample having roughness less than 0.1 (fine sample) and coating time fifteen
minutes show high value modulus of elasticity as compared to all other samples of different
roughness and coating time. Sample having surface roughness less than 0.1 (fine sample) and
coating time sixty minutes show low value of modulus of elasticity. Therefore, we can say that
modulus of elasticity depends upon coating time.

Figure 32 Graph between Adhesion (A) and time (t)
In this graph, sample having roughness lies between 0.1 to 0.2 (intermediate sample) and coating
time one hundred and twenty minutes show highest value of adhesion as compared to all other
samples of different roughness and coating time. Sample having roughness also lies between 0.1
to 0.2 (intermediate sample) and coating time fifteen minutes show least value of adhesion.
Therefore, we can say that adhesion also depend upon coating time. Adhesion value of sample is
high when coating time high of intermediate samples.
Figure 33 shows coefficient of friction (CoF) vs time (t)
In this graph, sample having roughness less than 0.1(Fine samples) and coating time sixty
minutes show high value of coefficient of friction as compared to all other samples of different
roughness and coating time. Sample having roughness lies between 0.2 to 0.3 (rough samples)
and coting time sixty minutes show least value of coefficient of friction (CoF). Therefore, we can
say that Coefficient of friction (CoF) depend upon surface roughness of the sample.
CHAPTER 6
6.1. CONCLUSION
In this experimental research work, three surface roughness level and three coating time were
prepared. Improved tribo mechanical properties achieved of coatings 80:20 as compared to bare
stainless steel. Hardness and adhesion increase in coating and Coefficient of friction value
decrease in coating as compared to uncoated 316L stainless steel. Highest adhesion value has
been observed at 50:50 coating. 80:20 coatings are recommended for applications where higher
mechanical properties are required like cutting tools while 50:50 coatings are recommended for
higher tribological properties. TiAlN 50:50 is preferred as improved tribo-mechanical properties
are observed there. This experimental result showed three set of samples with 50:50 TiAlN,
30:70 TiAlN and 80:20 TiAlN. Experiment results show that the 50:50 TiAlN sample show
overall better results in terms of Hardness

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EXPERIMENTAL INVESTIGATION OF TRIBO-

MECHANICAL PROPERTIES OF TIALN COATING ON 316L

Muhammad Athar Mahmood

DEPARTMENT OF MECHANICAL ENGINEERING

Primary Advisor/Internal Examiner External Examiner

DEPARTMENT OF MECHANICAL ENGINEERING

tribomechanical performance physical vapor deposition (PVD) based Titanium Aluminum

Investigation is being done of tribo-mechanical properties of 316L stainless steel by 80:20

titanium aluminium alloys from earlier investigations. (. Experimentation is carried out to

are performed on coated samples. Tribological performance of Titanium Aluminum Nitride

coefficient of friction and wear rate.

every happening. Allah Subhanaho- Wa Ta’ala said :

“If you are grateful, I will certainly increase you”

who enlightened not only the whole mankind. He ‫ ﷺ‬said:

“He, who is not thankful to the people, is not thankful to ALLAH”.

technical facilities that helped me in coating process and testing.

dissertation. This complete thesis is written by me.

Muhammad Athar Mahmood

Figure 1 Coating techniques [11]...............................................................................................................15

Table 1 Classification of samples before coating process..........................................................................42

density. In chemical, petrochemicals and aerospace industry, titanium is used in many

it mostly used in petrochemical industries [6].

processing, a great variety of biomaterials with characteristics employed in several applications

mechanical, automotive engineering, industrial, biomedical engineering and many others

life of automobile components and reducing friction.

1.3. SURFACE ENGINEERING

treatments such as high-performance surface solutions, especially plasma deposition processes

long lasting products.

1.4. THIN FILM COATING

lubrication to mating parts [11]

application and requirement shown in Fig 1.

Two processes are usually used for coatings deposition:

 Physical Vapor Deposition (PVD) Coating

 Chemical Vapor Deposition (CVD) Coating

1.5. PHYSICAL VAPOR DEPOSITION (PVD)

These are commonly used PVD coating process:

 High voltage triode electron beam

 Low voltage electron beam

Figure 2 PVD Coating process

1.5.1. PVD Coating Properties

 High wear resistance

 Low coefficient of friction

 Good adhesion to substrate

 Low heat transfer coefficient

 Smooth surface morphology

process. The deposition process can be accelerated through plasma or heat.

Most commonly used CVD techniques are

 Laser Chemical Vapor Deposition (LCVD)

 Metal-Organic Chemical Vapor Deposition (MOCVD)

 Plasma Assisted Chemical Vapor Deposition (PACVD)

 Low Pressure Chemical Vapor Deposition (LPCVD)

 Photochemical Vapor Deposition (PCVD)

 Chemical Vapor Infiltration (CVI)

 Plasma Enhanced Chemical Vapor Deposition (PECVD)

 Atmospheric Pressure Chemical Vapor Deposition (APCVD)

1.7. TRIBOLOGY AND COATING CORRELATION

important role to obtain better mechanical and coating properties. In manufacturing of

dependability of machine parts. Successfull resultsare obtained by PVD coating of DLC.

1.8. EVALUATION OF TRIBOLOGICAL PROPERTIES

properties.Testing conditions are varied according to application condition. In biomedical

1.9. TRIBOLOGY AND SURFACE ROUGHNESS CORRELATION

Profilometer is a device which is used to measure surface roughness. In recent research

mechanical in biomedical qualities demand materials with lower surface roughness.