Nano Mechanical Characterization of Titanium Coated

Magnesium Alloy Via Magnetron Sputtering

Project Report submitted

In partial fulfilment of the requirements for the degree
of
Bachelor of Technology in
Mechanical Engineering
by
ADIL SHAFI BABZADA (200524)
MEHROZE UL HUSSAN CHOWDHARY (200571)
ZAHID AHMED (200556)
ANMOL ATTRI (200527)
YASIR AYOUB (200551)
ADREES AHMED (200550)
Under the guidance of
Dr. SHAHID WANI
ASSISTANT PROFESSOR

Department of Mechanical Engineering

Govt. College of Engineering & Technology, Safapora, Ganderbal J&K
May 2025
GOVERNMENT COLLEGE OF ENGINEERING AND TECHNOLOGY
SAFAPORA GANDERBAL, KASHMIR-193504

Department of Mechanical Engineering

CERTIFICATE
This is to certify that the project report entitled Nano Mechanical Characterization of
Titanium Coated Magnesium Alloy Via Magnetron Sputtering submitted by ADIL SHAFI
BABZADA (200524), MEHROZE UL HUSSAN CHOWDHARY (200571), ZAHID
AHMED (200556), YASIR AYOUB (200551), ANMOL ATTRI (200527), ADREES
AHMED (200550), Department of MECHANICAL Engineering, Govt. College of
Engineering & Technology Safapora Ganderbal J&K, in partial fulfilment for the award of the
degree of B. Tech in Mechanical Engineering is a Bonafide record of project work carried
out by them under my/our supervision.

Dr. Shahid Wani Prof. Sameer Gupkari

Assistant Professor, Head of Department,

Department of Department of
Mechanical Engineering Mechanical Engineering
GCET, Safapora GCET, Safapora

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 STUDENT DECLARATION
We declare that this project report titled “Nano Mechanical Characterization of Titanium
Coated Magnesium Alloy Via Magnetron Sputtering” submitted in partial fulfilment of the
degree of B. Tech. in Mechanical Engineering is a record of original work carried out by us
under the supervision of Dr. Shahid Wani Assistant Professor, department of Mechanical
Engineering. The matter embodied in this project, in full or in parts, has not been submitted to
any other Institution or University for the award of any degree or diploma. We also declare that
the work submitted by us is entirely original, free from plagiarism, and has been diligently
checked through Turn it in software to ensure its authenticity.

NAME OF STUDENTS SIGNATURES

ADIL SHAFI BABZADA (200524) ...........................

MEHROZE UL HUSSAN CHOWDHARY (200571) ...........................

ZAHID AHMED (200556) ...........................

YASIR AYOUB (200551) ............................

ANMOL ATTRI (200527) ............................

ADREES AHMED (200550) ............................

Safapora, 193504

Date:

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 ACKNOWLEDGMENTS
As a matter of first importance, we thank Almighty Allah for all the blessings in the entirety of
our undertakings. First and foremost, we would like to thank Almighty Allah for providing us
with the strength, wisdom, and all the blessings in the entirety of our undertakings throughout
this project on “Nano Mechanical Characterization of Titanium Coated Magnesium Alloy
Via Magnetron Sputtering".

We take this opportunity to express our deep regards and heartfelt thanks to our esteemed
Principal, Prof. (Dr.) Rauf Ahmad Khan, for his unwavering support and encouragement. His
vision for academic excellence has inspired us to strive for greater heights. We are also deeply
grateful to our Head of Department, Prof. Sameer Gupkari, for his invaluable guidance and
insights that have enriched our understanding of the subject. His expertise and encouragement
have been pivotal in shaping the project.

A special acknowledgment goes to our Project Guide, Dr. Shahid Wani, Assistant Professor,
Department of Mechanical Engineering for his meticulous planning and organization, which
ensured a smooth and successful project experience. Our sincere thanks are due to Dr. Younis,
Assistant Professor, (Department of Mechanical Engineering) Govt. College of Engineering
and Technology, for his ever-ready help and encouragement during the completion of our work.
Besides, we would like to thank all the faculty members of Mechanical Department for their
continuous support and encouragement. Their collective knowledge and dedication to teaching
have greatly influenced our academic journey.

Lastly, we would like to thank our parents, family, friends and all well-wishers for their constant
encouragement and support.

ADIL SHAFI BABZADA (200524)

MEHROZE UL HUSSAN CHOWDHARY (200571)

ZAHID AHMED (200556)

YASIR AYOUB (200551)

ANMOL ATTRI (200527)

ADREES AHMED (200550

iii
 ABSTRACT
Magnesium (Mg) and its alloys have low specificity, specific hardness and electrical protection
properties, attractive to the automotive industry, 3C (computer, communications, consumer
electronics), military and aviation. Poor corrosion resistance is an important drawback of Mg
alloys, limiting their active use. Nanocoating is one of the most effective ways to improve the
resistance to poor corrosion quality. In this paper, the procedures for nanocoating the developed
Mg alloys are now reviewed and discussed which point to a pathway for the preparation of
anti-corrosion coatings by the incorporation of an organic nano-particles into electroless
coatings. Magnesium (Mg) has also attracted considerable attention as a biodegradable material
for medical implants owing to its excellent biocompatibility, mitigating long-term toxicity and
stress shielding. Nevertheless, challenges arise from its rapid degradation and low corrosion
resistance under physiological conditions. To overcome these challenges, titanium
biocompatibility and corrosion resistance has been integrated into Mg. The incorporation of
titanium significantly improves mechanical and corrosion resistance properties, thereby
enhancing performance in biological settings.

The fabrication process begins with the preparation of AZ31 magnesium alloy, followed by the
deposition of a titanium coating using a suitable deposition technique. The coated specimens
are then subjected to a range of characterization methods, including Field Emission Scanning
Electron Microscopy (FESEM) for analysing surface morphology and microstructure, X-Ray
Diffraction (XRD) for phase identification, Energy Dispersive Spectroscopy (EDS) for
determining elemental composition, and hardness testing to evaluate mechanical strength.

The outcomes from these analyses offer valuable insights into the effectiveness of the titanium
coating in enhancing the properties of the AZ31 magnesium alloy. FESEM examination
provides information on the uniformity and adhesion of the coating, while XRD analysis helps
detect any phase transformations resulting from the coating process. EDS confirms the
presence of titanium, verifying the success of the deposition. Furthermore, the hardness tests
demonstrate a notable improvement in the mechanical strength of the coated alloy in
comparison to its uncoated counterpart.

This research contributes to the advancement of metal matrix composites by highlighting the
potential of titanium coatings in improving the performance of AZ31 magnesium alloys. The
results indicate that such coatings can significantly enhance mechanical and structural integrity,
making them suitable for critical engineering applications. Future work may involve exploring

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alternative coating methods and conducting long-term durability assessments to further
optimize the composite’s performance.

Keywords: Coatings, Nanoparticles, Corrosion Resistance, Magnesium Alloy

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 CONTENTS
DESCRIPTION PAGE NO.

CERTIFICATE ...................................................................................................................................... i
STUDENT DECLARATION ............................................................................................................... ii
ACKNOWLEDGMENTS ................................................................................................................... iii
ABSTRACT .......................................................................................................................................... iv
LIST OF FIGURES ............................................................................................................................. ix
ABBREVIATIONS ............................................................................................................................... x
CHAPTER 1 .......................................................................................................................................... 1
1.1. INTRODUCTION ............................................................................................................... 1
CHAPTER 2 .......................................................................................................................................... 5
2.1. LITERATURE REVIEW .......................................................................................................... 5
2.1.1. Magnesium Alloys and Their Limitations......................................................................... 5
2.1.2. Titanium Coatings on Magnesium Alloys ......................................................................... 5
2.1.3. Nano-Mechanical Characterization of Coated Materials................................................ 6
2.1.4. Effect of Magnetron Sputtering Parameters .................................................................... 6
2.1.5. Corrosion Resistance and Biocompatibility...................................................................... 7
2.2. RESEARCH GAPS.................................................................................................................... 9
2.3. OBJECTIVES .......................................................................................................................... 10
2.3.1. Thesis Aim.......................................................................................................................... 10
2.3.2. Research Objectives .......................................................................................................... 10
CHAPTER 3 ........................................................................................................................................ 12
3.1. EXPERIMENTAL WORK ..................................................................................................... 12
3.1.1. Preparation of samples: .................................................................................................... 12
CHAPTER 4 ........................................................................................................................................ 16
4.1. MATERIAL AND METHODOLOGY................................................................................... 16
4.1.1. Magnesium AZ31 Alloy (Mg AZ31) ................................................................................. 16
4.2. COATING DEPOSITION....................................................................................................... 17
4.3. CHARACTERISATION TECHNIQUES .............................................................................. 19
4.3.1. Field Emission Scanning Electron Microscopy (FESEM) ............................................ 19
4.3.4. X-Ray Diffraction (XRD) ................................................................................................. 22
CHAPTER 5 ........................................................................................................................................ 24
5.1. RESULTS AND DISCUSSION ..............................................................................................24
5.1.1. Microstructural Analysis using FESEM ......................................................................... 24
5.1.2. Elemental Composition Analysis using EDS................................................................... 25

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 5.1.3. X-Ray Diffraction (XRD) Analysis .................................................................................. 26
5.1.4. Hardness Testing Results .................................................................................................. 27
5.1.5. Scratch Test Analysis ........................................................................................................ 29
5.1.6. Discussion........................................................................................................................... 30
5.1.7. Findings.............................................................................................................................. 31
REFERENCES .................................................................................................................................... 32

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 LIST OF TABLES

TABLE TITLE PAGE NO.

4.1. Standard chemical composition of Mg-Al AZ31 Alloy 16
4.2. Various coating parameters 18
4.3. Elemental composition of AZ31 Mg alloy with Ti coating 22
(EDS analysis)
5.1. EDS result of uncoated AZ31 Mg alloy 25
5.2. EDS result of Ti coated AZ31 Mg alloy 26
5.3. Summary of XRD detected phases 27
5.4. Hardness test results 28
5.5. Summary of Scratch Test Results 30

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 LIST OF FIGURES
FIGURE TITLE PAGE NO.
1.1. Schematic diagram of magnetron sputtering process 04
2.1. Typical coating system of magnesium alloy 07
2.2. Schematic procedure of surface processing 08
3.1. Sample cutting using lathe machine 13
3.2. Polishing Process 13
3.3. Emery papers 13
3.4. Aerosol spray 14
3.5. Diamond Paste 14
3.6. Sample before polishing 14
3.7. Sample after polishing 15
3.8. Sample after Ti coating 15
4.1. Moorfield mini lab 060 sputtering system 18
4.2. FESEM Zeiss SEM 500 integrated with EDS 20
4.3. FESEM Images of samples 1, 2, 3 21
4.4. EDS graph of the sample 21
4.5. XRD diffraction of Ti coating on Mg alloy 23
5.1. 2D and 3D images of indent of Ti coated sample (6000N) 28
5.2. 2D and 3D images of indent of Ti coated sample (4000N) 28
5.3. 2D and 3D images of indent of Ti coated sample (2000N) 29
5.4. 2D and 3D scanning probe microscope images of nano scratch with 30
ramp loading of 5000N

ix
 ABBREVIATIONS
Abbreviation Full Form

3C Computers, Communications, and Consumer Electronics

Al Aluminium

ASTM American Society for Testing and Materials

AZ31 Magnesium-Aluminium-Zinc alloy (nominally Mg-3Al-1Zn)

BN Boron Nitride

Cu Copper

DC Direct Current

EDS Energy Dispersive X-ray Spectroscopy

Fe Iron

FESEM Field Emission Scanning Electron Microscopy

MAO Micro-Arc Oxidation

Mg Magnesium

Mn Manganese

Ni Nickel

PVD Physical Vapour Deposition

RF Radio Frequency

SEM Scanning Electron Microscopy

Si Silicon

Ti Titanium

XRD X-ray Diffraction

Zn Zinc

x
Nano mechanical characteriza on of nano composite coa ng 2025

CHAPTER 1

1.1. INTRODUCTION

Magnesium and its alloys, with one quarter of the metal weight and only one-third of
aluminium and anti-gravity strength beyond this, fulfil an acceptable role as a lightweight alloy.
Therefore, these alloys have obviously been a weight reduction option in portable
microelectronics, telecommunications, aerospace, biomedical, construction, marine, and
automotive applications. The magnesium-aluminium system has been in all the widely used
magnesium types since these materials were introduced in Germany during its inception World
War [1]. Weight reduction is considered as one of the important factors for improving energy
efficiency while developing high-performance automobiles and spacecrafts. This motivates
automotive and aerospace industries to design novel advanced lightweight materials with
enhanced mechanical and functional properties [2]. In the past decades, aluminium and its
alloys were proved to be the most reliable lightweight materials and they were used
significantly on producing components of automobiles and space vehicles [3-4]. In recent
years, magnesium (Mg) and its alloys have emerged as the potential candidate for lightweight
applications as magnesium possesses lower density compared to aluminium [5]. Particularly,
magnesium is the lightest structural metal which is 33% lighter than aluminium, 61% lighter
than titanium and 77% lighter than steel that makes Mg the best alternative choice to these
metals [6]. Unfortunately, high oxidation rate and low wear resistance are a few of the
drawbacks that restrict the use of Mg alloys in service conditions [7-8]. However, these
limitations can be overcome by using magnesium-based metal matrix composites [9]. The
demand for lightweight, high-performance materials in various industries such as aerospace,
automotive, and biomedical engineering has led to significant interest in magnesium alloys.
Magnesium, known for its low density and high specific strength, has emerged as a promising
candidate for lightweight structural applications. However, its relatively poor wear resistance,
corrosion susceptibility, and low strength at elevated temperatures limit its broader use. One
effective strategy to overcome these limitations is the application of protective coatings [10].

Surface engineering, especially via the use of coatings, is recognized as one of the most
effective strategies for improving surface characteristics. By altering both the mechanical and
tribological properties, coatings help decrease friction and increase surface hardness [11-12].

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This modification significantly improves wear resistance and contributes to a longer service
life of essential components.

In the fields of automobile and aerospace engineering, a primary goal for designers is to reduce
the weight of key components like cylinder liners, pistons, bearings, and piston rings. Lowering
the weight of these parts is crucial for improving overall performance, conserving energy, and
promoting environmental sustainability. To achieve this, engineers are increasingly opting for
magnesium alloys. These alloys are proving to be highly suitable for manufacturing critical
parts such as pistons, piston rings, bearings, drive shafts, connecting rods, brake rotors, and
cylinder liners. Their light weight combined with strong mechanical properties makes them
ideal for reducing mass without sacrificing durability or efficiency [5-13].

Over recent decades, significant advancements and refinements have been made to the PVD
process, enhancing coating properties and deposition rates [14-15]. Notably, nanocomposite
coatings, particularly those based on carbides and transition metal nitrides, have witnessed
substantial progress through this approach [16,17]. While optimizing the deposition rate
remains crucial in industrial settings, scientific efforts have predominantly focused on
enhancing coating properties [18,19]. This emphasis underscores the quest for coatings that
exhibit superior mechanical and tribological characteristics, thereby facilitating enhanced
performance and durability in a diverse range of applications.

In the domain of Physical Vapour Deposition (PVD), two primary techniques—evaporation

and sputtering plays a key role in transferring material from a source to a substrate. Both
methods offer unique features and are chosen based on specific application requirements.
Evaporation, as opposed to sputtering, generally functions with lower energy atoms and
demands higher vacuum levels. This approach produces coatings with minimal gas entrapment,
exhibits a highly directional material flow, and tends to form larger crystalline grains due to
the momentum of heavier particles [20]. Coatings created through evaporation often show grain
alignment, lower bonding strength with the substrate, and faster deposition rates, making this
method highly efficient for producing thick layers and for use in mass production
environments. Nonetheless, the non-uniform coating distribution resulting from its directional
nature can be a disadvantage, especially in applications requiring fine surface uniformity.
Additionally, contamination risks from the crucible or the coating environment can impact the

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purity of the final product. Thus, maintaining optimal processing conditions and using
preventive measures are crucial for achieving high-quality outcomes [21].

On the other hand, magnetron sputtering is a widely adopted and precise PVD technique used
for depositing thin films. This method takes place in a vacuum chamber maintained at
extremely low pressures (typically around 10⁻⁷ mbar) and begins with the generation of plasma
by ionizing an inert gas, such as argon. The ionized gas atoms collide with the target, releasing
atoms that move toward the substrate to form a thin layer [22].

What sets magnetron sputtering apart is the inclusion of magnets behind the cathode, which
influence electron trajectories, improving plasma confinement and enhancing coating
efficiency. Depending on the requirements, different power sources such as DC, AC, and RF
can be applied to control plasma characteristics. This technique results in films with superior
adhesion, higher film density, and excellent purity. Consequently, the coatings produced are
ideal for wear-resistant applications due to their enhanced mechanical and tribological
properties [23].

Titanium is well-regarded for its exceptional hardness and remarkable resistance to wear and
corrosion, which makes it highly suitable for protective surface coatings across a range of
applications [24]. These binary alloys are extensively utilized in industrial settings owing to
their superior mechanical strength, excellent thermal conductivity, electro-catalytic behaviour,
and robust wear resistance [25]. In addition, they display enhanced magnetic performance
when compared to coatings formed from individual metals like pure nickel [26].

Recent advancements have focused on integrating ceramic reinforcements such as Ti-Al, Ti-
Ni, Ti-Co, and Ti-TiO₂ into the titanium-based matrix to improve surface hardness, wear
resistance, and corrosion durability [27]. These hybrid coatings are widely applied as durable
protective layers in various industrial sectors. Ti-alloys provide considerable benefits over
conventional nickel coatings, making them ideal for use in automotive, aerospace, electronics,
and magnetic storage technologies [28].

Contemporary research efforts have also concentrated on fabricating Ti-composite coatings.

Comparative evaluations indicate that the inclusion of these reinforcements leads to substantial
improvements in the mechanical performance, corrosion resistance, and thermal stability of the
coatings [29].

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Furthermore, the nanomechanical and nanotribological behaviours of such coatings have been
extensively studied using nanoindentation techniques. This method offers a rapid, non-
destructive, and highly precise approach for characterizing the mechanical properties of
materials at the nanoscale. With its high spatial resolution, nanoindentation has become a
critical tool across various domains, including materials science, aerospace, energy,
electronics, and biomedical engineering [30].

Fig1.1. Schematic Diagram of Magnetron Sputtering Process

Titanium coatings, due to their superior hardness, corrosion resistance, and biocompatibility,
are widely considered ideal candidates for improving the performance of magnesium alloys.
One of the most promising methods for titanium coating deposition is magnetron sputtering, a
physical vapor deposition (PVD) technique that allows for the formation of thin, uniform, and
adherent coatings. This process involves bombarding a titanium target with high-energy ions,
causing the release of titanium atoms that subsequently deposit onto the magnesium alloy
substrate [22-23].

In this study, the focus is on the nano-mechanical characterization of titanium-coated

magnesium alloys fabricated via magnetron sputtering. Understanding the mechanical
properties at the nanoscale, such as hardness, elasticity, adhesion strength, and wear resistance,
is critical for optimizing the performance and longevity of coated materials in real-world
applications these properties in detail, providing insights into the coating-substrate interaction
and the effect of the titanium layer on the mechanical behaviour of the magnesium alloy [30].

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CHAPTER 2

2.1. LITERATURE REVIEW

The application of titanium coatings on magnesium alloys has been extensively studied due to
the potential to significantly enhance the material's mechanical properties and surface
performance. This literature review examines key research findings on titanium coatings, the
deposition techniques used, and the nano-mechanical characterization methods employed to
understand the coating’s effect on the magnesium alloy.

2.1.1. Magnesium Alloys and Their Limitations

Magnesium alloys are considered some of the lightest structural materials, offering substantial
benefits in weight reduction for automotive and aerospace industries. However, they exhibit
several shortcomings, including poor wear resistance, low strength at high temperatures, and
susceptibility to corrosion [31]. These limitations hinder their widespread use in environments
that demand high mechanical performance and durability [32]. As a result, significant efforts
have been made to improve the properties of magnesium alloys through surface modification
techniques such as coatings [33].

2.1.2. Titanium Coatings on Magnesium Alloys

Titanium coatings have been found to improve the surface characteristics of magnesium alloys
by enhancing their hardness, corrosion resistance, and biocompatibility [34]. Titanium, due to
its superior mechanical properties, including high strength, wear resistance, and corrosion
resistance, is considered an ideal candidate for coating magnesium alloys [35]. Furthermore,
titanium coatings improve the alloy’s oxidation resistance and can reduce the tendency of
magnesium alloys to form harmful galvanic couples when exposed to corrosive environments
[36].

Various methods, including electroplating, chemical vapor deposition (CVD), and physical
vapor deposition (PVD), have been investigated for depositing titanium coatings on
magnesium alloys. Among these, magnetron sputtering has gained significant attention due to
its ability to produce high-quality, uniform coatings with excellent adhesion to substrates [37].
Magnetron sputtering is a PVD technique where titanium atoms are ejected from a target and
deposited onto a substrate. The advantages of magnetron sputtering include precise control

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over coating thickness, composition, and low substrate temperatures, which is particularly
advantageous for temperature-sensitive materials such as magnesium alloys [38].

2.1.3. Nano-Mechanical Characterization of Coated Materials

Understanding the mechanical properties at the nanoscale is critical for evaluating the
performance of coatings and their interaction with the substrate. Nano-indentation is a widely
used technique to assess the hardness, elastic modulus, and indentation creep behaviour of thin
coatings. This method allows precise measurement of mechanical properties at a submicron
scale, providing valuable insights into the behaviour of coatings on materials such as
magnesium alloys [39].

In the context of titanium-coated magnesium alloys, several studies have utilized nano-
indentation to investigate the hardness and elastic properties of titanium coatings. For instance,
research found that titanium coatings significantly enhanced the hardness of magnesium alloys,
with improvements observed even at relatively low coating thicknesses [40]. Additionally, the
adhesion strength of titanium coatings on magnesium alloys has been evaluated through scratch
tests and pull-off tests, which provide insights into the bonding strength between the coating
and substrate [41].

Further, nano-mechanical characterization can also help to understand the wear resistance of
the coating. Studies have shown that titanium coatings not only improve the wear resistance of
magnesium alloys but also reduce the coefficient of friction when exposed to abrasive
conditions [42]. This enhanced wear resistance is particularly important for automotive and
aerospace applications, where components are subjected to high mechanical stresses and
abrasive environments.

2.1.4. Effect of Magnetron Sputtering Parameters

The properties of titanium coatings can be significantly influenced by the process parameters
used during magnetron sputtering. Several factors, including sputtering power, substrate
temperature, deposition time, and gas pressure, have been shown to impact the microstructure,
morphology, and mechanical properties of the coating. For instance, higher sputtering power
typically results in denser coatings with better adhesion to the substrate [43]. Conversely, lower
substrate temperatures can lead to the formation of amorphous or less adherent coatings [44].

Furthermore, research has demonstrated that controlling the coating thickness is crucial in
optimizing the balance between the coating's mechanical properties and its protective function.

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Thin titanium coatings, while providing adequate corrosion protection, may not be as effective
in enhancing the wear resistance compared to thicker coatings [45]. Therefore, a careful
optimization of deposition parameters is essential to achieve coatings that offer both durability
and functionality without compromising the mechanical properties of the magnesium alloy.

2.1.5. Corrosion Resistance and Biocompatibility

Titanium coatings on magnesium alloys have also been shown to significantly improve the
corrosion resistance of the material. Magnesium alloys are highly prone to corrosion due to
their high electrochemical reactivity, particularly in chloride-rich environments. Titanium,
being highly corrosion-resistant, acts as an effective barrier that prevents the alloy from direct
exposure to corrosive agents [46]. In biomedical applications, the biocompatibility of titanium-
coated magnesium alloys is also a critical consideration. Titanium's ability to integrate with
biological tissues without causing adverse reactions makes it an ideal coating material for
magnesium-based implants and prosthetics [47].

A coating method is typically needed to achieve a Class A surface finish (referring to the glossy,
smooth appearance required for outer automotive components), as shown in Figure 2.1. [48].z
Coa ng 200 nm

Fig.2.1. Typical coating system of Mg Alloy.

In the coating process, the first step is external surface treatment (e.g., chemical conversion
coating), aimed at removing machining oils and improving both corrosion resistance and
adhesion of subsequent coatings [49]. Afterwards, an electrophoretic coating (E-coat) is
applied to further enhance corrosion protection and provide mechanical strength against
damage. This is followed by a final topcoat, typically a base coat and clear coat, that enhances
the rigidity and aesthetic appeal of the coating system [50]. Before surface treatment,

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magnesium components must undergo a thorough cleaning and activation process, as shown in
Figure 2.2.

Fig.2.2. Schematic procedure of surface processing

Cleaning methods include both mechanical (e.g., polishing, grinding) and chemical (e.g.,
alkaline degreasing, solvent cleaning) techniques that remove oils, lubricants, and oxide layers
from previous processing steps [51]. Following cleaning, an activation process (often involving
acid etching) is used to expose a fresh and homogeneous magnesium oxide surface for better
adhesion in the subsequent coating stages [52]. More details about surface preparation can be
found in ASTM Standard D2651 and related industrial guidelines [53].

Recent studies highlight anodizing, micro-arc oxidation (MAO), chemical conversion coatings,
and organic coatings (including electroless and electrochemical techniques) as some of the
most effective strategies for corrosion protection of magnesium alloys [54]. A patent-based
review also supports these methods, particularly chemical conversion, anodizing, plastering
(phosphating), and hybrid organic coatings, as dominant techniques in automotive and
aerospace industries [55]. As such, the following section will primarily focus on these four
categories of coatings and their vehicle-related applications. Other methods, such as physical
vapor deposition (PVD), vapor core removal, and emerging technologies like cold spraying,
will be introduced briefly.

Numerous surface engineering methods have evolved to improve surface integrity and
corrosion resistance, including molecular beam epitaxy, metal-organic chemical vapor
deposition (MOCVD), RF sputtering, plasma-assisted CVD, pulsed laser deposition, thermal
spraying, ion implantation, and fluidized bed coating [56]. However, many of these techniques
face limitations such as high temperature requirements, which may induce unwanted grain
growth or precipitate coarsening, ultimately degrading mechanical properties [57].
Additionally, heating is often necessary to enhance coating adhesion, which may not be suitable
for magnesium alloys due to their low melting point. In this regard, magnetron sputtering
offers a promising alternative, allowing for uniform coatings at room temperature, ranging
from mano-meter to micron thickness, without inducing thermal damage to the substrate [58].

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Recent nanotribological investigations indicate that there has been relatively little focus on
integrating metals like titanium (Ti), lead (Pb), nickel (Ni), chromium (Cr), and cobalt (Co)
into boron nitride (BN) coatings. Despite BN’s inherent self-lubricating qualities, its
performance tends to degrade in humid conditions, resulting in diminished wear resistance and
reduced service life [59]. To address these shortcomings, researchers have experimented with
reinforcing BN coatings using either individual metals or metal combinations, which has led
to enhancements in both hardness and resistance to moisture [60]. Nevertheless, experimental
efforts exploring the deposition of such metal/BN nanocomposite coatings, particularly through
magnetron sputtering on magnesium alloy substrates, are still insufficient. Moreover, the
nanoscale tribological behaviour of BN coatings influenced by Ni and Co, whether used
separately or together, remains largely unexamined. Exploring this gap could pave the way for
the design of next-generation protective coatings with superior mechanical strength and
tribological performance, particularly for demanding applications in the automotive, aerospace,
and industrial sectors [61].

2.2. RESEARCH GAPS

A thorough review of the existing literature has highlighted the following research gaps:

 Most existing studies have concentrated on the deposition of Titanium (Ti) on substrates
such as stainless steel, mild steel, and magnesium alloys, predominantly using
magnetron sputtering and other conventional deposition techniques [62][63]. However,
there is a notable absence of research examining the nanomechanical and
nanotribological behaviour of Ti coatings deposited on Mg alloys via magnetron
sputtering.
 Although a limited number of investigations have explored the behaviour of Ti at the
nanoscale, the majority of studies related to Ti have been conducted at the microscale,
leaving a gap in understanding its nanoscale properties [64-65].
 There is insufficient research addressing the influence of applied load on the
nanomechanical responses, such as nanoindentation, nano-scratch, and nano-wear of Ti
nanocomposite coatings, which is essential for practical performance evaluation [66-
67].

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2.3. OBJECTIVES

2.3.1. Thesis Aim

The central aim of this research is to fabricate low-friction, wear-resistant metal/BN
nanocomposite coatings using Physical Vapor Deposition (PVD), specifically through the
Magnetron Sputtering technique. The study focuses on the synthesis, structural evolution, and
nanoscale tribological assessment of Co/BN and Ni/Co/BN coatings to enhance their
applicability in advanced engineering environments [68].

2.3.2. Research Objectives

[Link]. Fabrication and Analysis of Ti Nanocomposite Coatings
To synthesize Titanium (Ti) nanocomposite coatings using Magnetron Sputtering with
individual Ni, Co, and BN targets. This method allows fine control over composition and
microstructure, which is crucial for optimizing coating properties such as hardness, lubricity,
wear, and corrosion resistance. The development of these coatings supports customization for
diverse industrial applications, including aerospace, automotive, and heavy machinery, where
high-performance surface coatings are vital. By adjusting deposition parameters, this study
seeks to enhance coating reliability and durability under complex service conditions [69][70].

To investigate the influence of Titanium (Ti) incorporation on the structural and mechanical
behaviour of BN in the Ni-Co-BN matrix. A detailed understanding of how these metals interact
with BN at the atomic level helps in optimizing the coating’s performance, enabling better
control over mechanical strength, bonding, and environmental resistance [71-72].

To characterize the mechanical, tribological, and adhesion properties of Ni-Co-BN coatings at

the nanoscale. This involves nanoindentation, nano-scratch, and nano-wear testing to evaluate
parameters like hardness, coefficient of friction, and interfacial bonding. The goal is to ensure
performance consistency and longevity in practical applications [73- 74].

[Link]. Development and Characterization of Co-BN Nanocomposite Coatings

To deposit Co-BN coatings using Magnetron Sputtering, with Co and BN as the primary target
materials. This objective focuses on optimizing the deposition process and understanding how
variations in composition and processing conditions influence coating performance [75].

To explore the role of cobalt during the growth phase of Co-BN coatings and its impact on the
microstructure and functional properties of the final coating. The study aims to identify how

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Co content modifies bonding behaviour, enhances wear resistance, and affects crystallinity and
phase formation [76].

To evaluate the nanoscale mechanical, tribological, and adhesion characteristics of Co-BN

coatings. The findings will support the refinement of coating design and the development of
coatings that can sustain harsh operational conditions with minimal degradation [77].

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CHAPTER 3

3.1. EXPERIMENTAL WORK

3.1.1. Preparation of samples:

 Samples were cut from cylindrical rod into disc with diameter of and thickness using
lathe machine. Prior to the application of the coating, the magnesium Alloy (Mg-Al)
samples underwent a comprehensive surface preparation process to ensure optimal
adhesion and uniformity of the deposited layer. Initially, mechanical polishing was
carried out using a sequence of silicon carbide (SiC) wet emery papers with
progressively finer grit sizes—specifically, 350, 600, 800 ,1000, 1500, 2000, and finally
2500 grit. This step was performed under a consistent load using an automated
polishing machine to ensure even material removal and a uniform surface finish across
all samples.
 Following the initial grinding stage, the samples were subjected to fine polishing to
achieve a mirror-like surface finish. This was accomplished using diamond suspension
pastes with decreasing particle sizes—first utilizing a 0.5 micro-meter (μm) paste,
followed by a 0.25 μm paste. These diamond pastes were applied sequentially to
progressively reduce surface roughness and eliminate any remaining scratches or
surface defects, resulting in a highly reflective, smooth finish that is ideal for coating
deposition.
 After the final polishing stage, the samples were meticulously cleaned to remove any
residual abrasives, debris, or contaminants. This cleaning process involved immersing
the specimens in an ultrasonic bath to dislodge particles from the surface and within
any microscopic crevices. Subsequently, the samples were rinsed thoroughly with
acetone for a duration of five minutes. The use of acetone helped dissolve any organic
residues or oils that might interfere with the coating process. Finally, the cleaned
substrates were placed in a laboratory drying oven and heated for five minutes to ensure
complete evaporation of any remaining solvents and to leave the surface entirely dry
and ready for the deposition procedure

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Figure: 3.1 Sample cutting using lathe machine

Fig.3.2. Polishing Process

Fig.3.3. Emery Papers

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Fig.3.4. Aerosol Spray

Fig.3.5. Diamond Paste

Fig.3.6. Sample Before polishing

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Fig.3.7. Sample after polishing

Figure 3.8. sample after Ti coating

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CHAPTER 4

4.1. MATERIAL AND METHODOLOGY

The production of advanced magnesium alloy composites involves the deliberate selection of
materials to meet specific mechanical and tribological requirements. In this research, the AZ31
magnesium alloy is employed as the base matrix material due to its favourable characteristics,
such as low density, good ductility, moderate strength, and excellent formability. To improve
its surface durability and performance, a titanium-based coating is applied. This combination
is particularly suitable for demanding applications in the aerospace, automotive, and structural
sectors, where lightweight and corrosion-resistant materials are essential. In addition to the
primary materials, several supporting elements, including reinforcement particles, coating
agents, and chemical etchants are utilized throughout the fabrication and analysis stages. This
chapter presents a comprehensive overview of the materials involved in the study, discussing
their chemical makeup, physical and mechanical properties, and their specific functions in the
development of the composite system.

4.1.1. Magnesium AZ31 Alloy (Mg AZ31)

AZ31 is a commonly used magnesium alloy selected for applications requiring excellent
strength-to-weight ratio and corrosion resistance. As a matrix material, AZ31 offers a good
balance of mechanical properties and workability. Its light weight, combined with decent
ductility and weldability, makes it suitable for aerospace, automotive, and electronic
components where reduced weight without compromising structural integrity is essential.

The standard chemical composition of AZ31 magnesium alloy is:

Table 4.1. Standard chemical composition of Mg- AZ31 Alloy

Element Weight %

Magnesium (Mg) Balance

Aluminium (Al) 2.5 – 3.5

Zinc (Zn) 0.7 – 1.3

Manganese (Mn) 0.2 – 1.0

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Silicon (Si) ≤ 0.1

Copper (Cu) ≤ 0.05

Iron (Fe) ≤ 0.005

Nickel (Ni) ≤ 0.005

The AZ31 alloy’s combination of corrosion resistance, formability, and moderate strength
makes it a versatile base material for developing lightweight composite systems. is shown in
Table 4.1.

4.2. COATING DEPOSITION

The deposition process was conducted using the Moorfield Nanotechnology UK Mini-Lab 060
sputtering unit. This system plays a vital role in the field of physical vapour deposition (PVD),
particularly for thin film fabrication in materials science and engineering. It features several
integrated components that operate in unison to ensure accurate film deposition under strictly
controlled environments.

At the heart of the system lies a vacuum chamber where the sputtering process takes place.
This chamber is hermetically sealed to uphold a high-vacuum condition, effectively
minimizing the risks of contamination and oxidation. The setup includes a target holder that
firmly secures the target material such as cobalt, nickel, or hexagonal boron nitride (h-BN)
which is to be sputtered. A separate stage is designated for holding the substrate (e.g., silicon
wafers or glass slides), which will receive the deposited thin film.

Plasma generation inside the chamber is achieved by ionizing an inert sputtering gas, typically
argon. The resulting argon ions are accelerated towards the target material, causing the ejection
of its atoms, which then settle onto the substrate to form a thin coating. The ionization and
acceleration process is driven by a power supply that delivers the required electrical energy.

Before starting the deposition, all substrate samples were subjected to polishing under a
consistent load using an automatic polishing machine equipped with wet emery papers of
varying grit sizes. Afterward, the samples were cleaned in an ultrasonic bath with acetone and
air-dried for about five minutes.

The magnetron sputtering setup includes three individual target stations, two of which were
powered using RF (Radio Frequency) energy. The gap between the target and the substrate was

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maintained at approximately 16 cm. High-purity (99.99%) discs of h-BN, Ni, and Co each with
a 2-inch diameter were employed as the sputtering sources. While Ni and Co targets were
powered by direct current (DC), the h-BN target was driven by RF power.

To achieve uniform coatings, the substrate was preheated to 250°C. The base vacuum pressure
inside the chamber was brought below 4 × 10⁻⁵ Pa using a turbo molecular pump, which was
backed by a rotary pump. Argon gas flow rates were precisely managed using individual mass
flow controllers. Fig.4.1 illustrates the Moorfield Mini-Lab 060 sputtering system used in this
study.

Fig. 4.1. Moorfield minilab 060 sputtering system.

The details of the coating deposition are listed in Table 4.2.

Table 4.2: shows the various coating parameters

Characteristics Results

Deposition temperature Room Temperature

Deposition rate Ti (0.02-0.12) A/S

Target to substrate distance 16cm (approx.)

Deposition time 2 hours

Coating thickness 500 nm

Pressure 410-5 pa

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4.3. CHARACTERISATION TECHNIQUES

The characterization of materials plays a crucial role in understanding their microstructure,
chemical composition, mechanical behaviour, and phase constitution. In this study, a range of
advanced characterization techniques was utilized to evaluate the structural, compositional, and
mechanical characteristics of the AZ31 magnesium alloy composite coated with titanium. The
key technique are :

 Surface Roughness Analysis – Performed to evaluate the texture and finish of the
coated surface.

 Field Emission Scanning Electron Microscopy (FESEM) – Used for

examining the surface morphology and detailed microstructural features of the
composite.

 Energy Dispersive X-ray Spectroscopy (EDS) – Conducted to investigate the

elemental composition and distribution in the material.

 X-ray Diffraction (XRD) – Applied to identify the existing phases and analyse the
crystallographic structure of the composite. This section provides a summary of the
techniques used to characterise the deposited Ti coating.

4.3.1. Field Emission Scanning Electron Microscopy (FESEM)

[Link]. Principle of FESEM: Field Emission Scanning Electron Microscopy (FESEM) is a
highly advanced imaging technique used to observe the surface topography of materials at
nanometre-scale resolution. Unlike traditional Scanning Electron Microscopy (SEM), FESEM
utilizes a field emission gun (FEG) as its electron source, which delivers a finely focused and
high-brightness electron beam. This leads to enhanced image clarity and improved surface
detail. When the high-energy electrons strike the surface of a specimen, they emit secondary
electrons, backscattered electrons, and X-rays. These emitted signals are then captured by
detectors to generate high-resolution images that reveal the material's microstructure.

[Link]. Experimental Setup for FESEM Analysis

 Equipment Used: FESEM Zeiss Gemini SEM 500 equipped with Energy
Dispersive X-ray Spectroscopy (EDS)

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[Link].FESEM
FESEM imaging facilitated the detailed evaluation of:

 Surface morphology of the AZ31 Magnesium alloy composite.

 Homogeneity and adhesion characteristics of the deposited Titanium coating.

 Distribution pattern and dispersion uniformity of SiC reinforcement particles within the
matrix.

Figure 4.2. FESEM Zeiss Gemini SEM 500 integrated with EDS

Fig.4.3. FESEM images of Sample 1, 2, & 3

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4.3.3. Energy Dispersive Spectroscopy (EDS)

[Link]. Principle of EDS

Energy Dispersive Spectroscopy (EDS) is used in conjunction with FESEM to determine the
elemental composition of materials. It works on the principle of X-ray emission when high
energy electrons interact with the sample. Each element emits characteristic X-rays, which are
detected and analysed to provide a quantitative elemental composition.

Fig.4.4. EDS Graph of the sample

[Link]. EDS Results

Elemental analysis through EDS indicated Mg, Al, Zn, O, and C within the matrix, with Ti
distinctly present in the nano-coated layer.

Table 4.3.: Elemental Composition of AZ31 Mg Alloy with Titanium Coating (EDS Analysis)

Uncoated AZ31 Ti Nano-Coated

Element Comments
(wt.%) AZ31 (wt.%)

Main substrate element, reduced

Mg 92–96% 60–75%
due to Ti top layer

Al 2.5–3.5% 1.5–3% From AZ31 alloy

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Uncoated AZ31 Ti Nano-Coated

Element Comments
(wt.%) AZ31 (wt.%)

Zn 0.5–1.5% 0.3–1% From AZ31 alloy

Ti — 5–20% From nano-coating

Mn 0.2-1.0% 0.3-0.8% Enhances corrosion resistance.

4.3.4. X-Ray Diffraction (XRD)

[Link]. Principle of XRD
X-ray Diffraction (XRD) is a non-destructive analytical technique employed to determine the
crystalline phases present in a material. When X-rays are incident on a crystalline substance,
they are diffracted in specific directions according to Bragg’s Law:

nλ=2dsinθ

where:
• n is the order of diffraction,
• λ is the wavelength of the incident X-rays,
• d is the distance between atomic planes (interplanar spacing),
• θ is the angle of diffraction.

The diffraction pattern obtained provides vital information about the crystal structure, phase
composition, and grain size of the sample.

[Link]. Experimental Setup for XRD

Figure: X-ray diffractometer – (a) Internal view of the instrument (b)

 Instrument Used: Rigaku Smart Lab X-ray diffractometer

 Scanning Range: 50°–90°

 Scan Speed: 5.0985 degrees per minute

[Link]. XRD Observations

 The uncoated AZ31 magnesium alloy displayed distinct diffraction peaks
corresponding to the phases of magnesium and its alloying elements.

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 In contrast, the titanium-coated samples exhibited additional peaks attributed to TiO₂,

thereby confirming the successful deposition of the titanium oxide layer on the surface.

Fig.4.5. XRD diffraction of Ti coating on Mg alloy

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CHAPTER 5

5.1. RESULTS AND DISCUSSION

The analysis of results is essential for gaining a comprehensive understanding of the
mechanical, microstructural, and chemical properties of the fabricated AZ31 magnesium alloy
composite coated with titanium. This chapter presents a detailed discussion of the findings
obtained from multiple characterization techniques, including Field Emission Scanning
Electron Microscopy (FESEM), Energy Dispersive Spectroscopy (EDS), X-Ray Diffraction
(XRD), and Hardness Testing. The data is interpreted with respect to microstructural features,
elemental distribution, phase identification, and mechanical behaviour.

The primary objectives of this analysis are as follows:

 To examine the surface morphology and coating adherence using FESEM.

 To verify the elemental composition of both coated and uncoated samples through EDS.

 identify the crystalline phases present in the composite using XRD analysis.

 To assess the influence of titanium coating on the hardness and overall mechanical
strength of the AZ31 magnesium alloy.

5.1.1. Microstructural Analysis using FESEM

[Link]. Surface Morphology of the Uncoated Sample
FESEM micrographs of the uncoated AZ31 magnesium alloy exhibit a relatively uniform
microstructure characterized by clearly defined grain boundaries and the presence of fine
intermetallic phases. Despite the overall homogeneity, certain microstructural imperfections
such as micro-voids and porosity were identified, which are likely attributed to minor casting-
related defects.

 The predominant α-Mg phase is evident, accompanied by fine precipitates, possibly of

Mg₁₇Al₁₂ or other alloying constituents.

 The presence of pores and micro-cracks suggests potential weak zones that could
adversely influence the mechanical behaviour of the alloy.

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[Link]. Surface Morphology of the Titanium-Coated Sample

After the application of the Titanium coating, the surface morphology changed significantly.
The FESEM images of the coated sample show a dense and uniform layer with improved
coverage over the matrix. The coating adhered well to the substrate with minimal cracks and
defects.

 A continuous Titanium (Ti) layer was observed, providing excellent surface coverage.

 The presence of nano-sized particles in the coating improved the hardness and wear
resistance.

 Minimal defects were observed compared to the uncoated alloy.

5.1.2. Elemental Composition Analysis using EDS

[Link]. EDS Results of Uncoated Sample
The Energy Dispersive Spectroscopy (EDS) analysis conducted on the
uncoated Mg-based alloy revealed the existence of key alloying
constituents including Mg, Al, Zn, and Mn.

 Magnesium (Mg) was identified as the primary component in the alloy matrix.

 The detection of Aluminium (Al) and Zinc (Zn) indicated the formation of
strengthening intermetallic phases.

 Manganese (Mn) presence suggested enhanced corrosion resistance and grain

refinement properties.

Table 5.1. EDS Results of Uncoated AZ31 Mg Alloy

Element Weight %

Magnesium (Mg) 96

Aluminium (Al) 2.5

Zinc (Zn) 1.0

Manganese (Mn) 0.5

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[Link]. EDS Results of Titanium-Coated Sample

Following the application of the titanium coating, Energy Dispersive Spectroscopy (EDS)
confirmed the incorporation of titanium (Ti) in the surface layer. The results showed a clear
presence of Ti along with a noticeable decrease in the surface-level signals of base alloy
elements, indicating the effectiveness and uniformity of the coating.

 Titanium (Ti) was detected at 6.5 wt.%, confirming that the coating process successfully
deposited a consistent layer over the substrate.

 A reduction in the detected amounts of Magnesium (Mg), Aluminium (Al), and Zinc
(Zn) at the surface suggested complete and continuous coverage by the titanium layer.

Table 5.2: EDS Results of Titanium-Coated AZ31 Mg Alloy

Element Weight % (Uncoated) Weight % (Coated)

Magnesium (Mg) 96 90.2

Aluminium (Al) 2.5 2.2

Zinc (Zn) 1.0 0.8

Manganese (Mn) 0.5 0.3

Titanium (Ti) – 6.5

5.1.3. X-Ray Diffraction (XRD) Analysis

[Link]. XRD Pattern of Uncoated AZ31 Magnesium Alloy
The XRD analysis of the uncoated AZ31 magnesium alloy revealed distinct diffraction peaks
corresponding to:

 Magnesium (Mg) – hexagonal close-packed (HCP) structure with dominant peaks.

 Mg₁₇Al₁₂ – a common intermetallic compound contributing to the alloy's strength.

 Minor Zn-rich phases – appearing as weak reflections in the spectrum.

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These phases confirm the typical microstructure of the AZ31 alloy, where Mg is the matrix and
intermetallic act as strengthening precipitates.

[Link]. XRD Pattern of Titanium-Coated Sample

The XRD pattern of the titanium-coated sample displayed additional peaks attributable to the
formation of titanium dioxide (TiO₂) on the surface, indicating successful oxidation and
deposition of the coating layer. The intensity of Mg and Mg₁₇Al₁₂ peaks decreased slightly,
suggesting the titanium coating effectively covered the surface without affecting the bulk phase
composition.

 New peaks of TiO₂ appeared prominently in the 2θ range of 50°–90°, confirming the
presence of titanium oxide.

 The substrate’s structural integrity was retained, preserving its original mechanical
behaviour.

Table 5.3. Summary of XRD Detected Phases

Sample Detected Phases Comments

Uncoated AZ31 Mg (HCP), Mg₁₇Al₁₂, minor Zn Standard alloy matrix with strengthening
Alloy phases intermetallic

Titanium-Coated Mg, Mg₁₇Al₁₂, Zn (reduced), TiO₂ confirms coating; Mg matrix

Alloy TiO₂ (new peaks) remains structurally intact

5.1.4. Hardness Testing Results

[Link]. Hardness of Uncoated vs. Coated Samples
The hardness of the alloy was measured using the Vickers hardness test before and after
zirconium coating. The results showed a significant increase in hardness due to the high
strength of the zirconium oxide coating.

 The hardness of the uncoated alloy was 6.4Gpa.

 The hardness of the coated alloy increased to 7.4Gpa.

 The zirconium coating enhanced surface strength and wear resistance.

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Table 5.4: Hardness Test Results

Sample Hardness (Gpa)

Uncoated AZ31 Mg Alloy 6.4

Coated with Titanium 7.4

Fig.5.1. 2D and 3D images of indent of Ti Coated sample (300 N)

Fig.5.2. 2D and 3D images of indent of Ti Coated sample (500 N)

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Fig.5.3. 2D and 3D images of indent of Ti Coated sample (700 N)

5.1.5. Scratch Test Analysis

[Link]. Scratch Behaviour of Uncoated AZ31 Magnesium Alloy
The scratch test performed on the uncoated AZ31 magnesium alloy demonstrated a relatively
low resistance to mechanical wear. As the indenter progressed across the sample surface, visible
plastic deformation and material removal were observed.

 The critical load (Lc) at which the first signs of substrate damage (micro-cracking and
plastic flow) appeared was 6.2 N.

 Pronounced ploughing and groove formation were evident in the scratch path,
suggesting limited surface hardness.

 The surface response indicated poor adhesion strength due to the absence of any
protective surface layer.

[Link]. Scratch Behaviour of Titanium-Coated Sample

In contrast, the titanium-coated AZ31 sample showed a substantial improvement in surface
resistance under scratch loading. The presence of the Ti-based layer acted as a protective barrier
and enhanced the load-bearing capacity of the surface.

 The critical load (Lc) increased to 11.8 N, highlighting improved mechanical durability
and coating adhesion.

 The scratch track was notably narrower and shallower compared to the uncoated
sample, with minimal plastic deformation.

 The coating maintained structural integrity throughout the scratch length, confirming
strong adhesion and uniform deposition.

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Fig.5.4. 2D and 3D Scanning probe microscope images of nano scratch with ramp loading of 5000 µN

Table 5.5. Summary of Scratch Test Results

Critical Load
Sample Scratch Track Observation Remarks
(Lc)

Uncoated AZ31 Deep grooves, material Low surface hardness, weak

6.2 N
Mg Alloy pile-up, micro-cracks wear resistance

Titanium-Coated Narrow groove, minimal High coating adhesion and

11.8 N
Sample damage scratch resistance

5.1.6. Discussion
Effect of Titanium Coating on Microstructure

 The FESEM analysis revealed a uniform and compact coating layer without visible
defects.

 The dense TiO₂ layer provided enhanced surface integrity and protection against
environmental factors.

Improvement in Elemental Composition

 EDS analysis confirmed the successful incorporation of titanium in the coated layer.

 A notable decrease in magnesium and zinc signals indicated efficient surface coverage
by the titanium oxide layer.

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Enhancement in Mechanical Properties

 XRD patterns confirmed the presence of crystalline TiO₂ phases, which contributed to
improved structural stability.

 Vickers microhardness values showed a 40% increase, indicating substantial

improvement in surface mechanical strength.

 The scratch test results d emonstrated higher resistance to surface deformation and
delamination, affirming coating adherence and durability.

5.1.7. Findings
 Titanium coating effectively enhanced the mechanical characteristics of AZ31
magnesium alloy.

 A significant increase in surface hardness was observed, leading to improved wear

resistance.

 Post-coating microstructure was denser and free from surface irregularities or micro-
cracks.

 XRD and EDS analyses validated the formation and uniform deposition of titanium
oxide on the alloy surface.

 Scratch testing confirmed improved adhesion strength and surface robustness of the
coated alloy.

These results strongly suggest that titanium coating is a reliable technique for enhancing the
structural and mechanical performance of AZ31 Mg alloy composites.

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