CHARACTERIZATION OF MG ALLOY MATRIX

COMPOSITES REINFORCED CARBON NANOTUBE

FAKHRUL HAKIM BIN SAHAMENDAN

BACHELOR OF SCIENCE (Hons.) PHYSICS

FACULTY OF APPLIED SCIENCES
UNIVERSITI TEKNOLOGI MARA

AUGUST 2023
 AUTHOR’S DECLARATION
This Final Year Project Report entitled “Characterization of Mg Alloy Matrix
Composites Reinforced Carbon Nanotube” was submitted by Fakhrul Hakim bin
Sahamendan in partial fulfilment of the requirements for the Degree of Bachelor of
Science (Hons.) Physics, in the Faculty of Applied Sciences, and was approved by

_____________________________________________
PROF. MADYA. DR. SAIDATULAKMAR SHAMSUDDIN
Supervisor
B. Sc. (Hons.) Physics
Faculty of Applied Sciences
Universiti Teknologi MARA
Perlis Branch, Arau Campus,
02600, Arau, Perlis.

DR. NURHIDAYAH AHMAD ZAIDI

Co-Supervisor
B. Sc. (Hons.) Physics
Faculty of Chemical Engineering & Technology
Kompleks Pusat Pengajian Jejawi 3, Kawasan Perindustrian Jejawi,
Universiti Malaysia Perlis (UniMAP),
02600 Arau, Perlis.

DR. KHUZAIMAH NAZIR DR. ROSYAINI BINTI AFINDI

Project Coordinator ZAMAN
B. Sc. (Hons.) Physics Programme Coordinator
Faculty of Applied Sciences B. Sc. (Hons.) Physics
Universiti Teknologi MARA Faculty of Applied Sciences
Perlis Branch, Arau Campus, Universiti Teknologi MARA
02600, Arau, Perlis. Perlis Branch, Arau Campus,
02600, Arau, Perlis.

Date:

ii
 ABSTRACT

CHARACTERIZATION OF MG ALLOY MATRIX COMPOSITES

REINFORCED CARBON NANOTUBE

Magnesium has received a lot of attention in recent years due to its light weight,
high specific strength, and ease of recycling. In this research study, the
microstructural, mechanical, and strengthening behavior of Mg alloy composites
reinforced with carbon nanotubes (CNTs) was examined. Magnesium and its
composites are used in restricted technical applications because of its strong
chemical reactivity, low wear, and creep resistance due to possesses poor bulk
qualities like as strength and stiffness, as well as saline corrosion resistance. Thus,
in this study, magnesium alloy matrix composites reinforced carbon nanotube
using (CNTSs) powder metallurgy has been fabricated. In this research study, the
main method being used was powder metallurgy. Powder metallurgy (PM) is a
solid-state technique for producing particle reinforced Mg-based composites.
Powder metallurgy consists of mixing, compaction, grinding, and sintering.
Furthermore, Rockwell hardness test and Archimedes Principle been carried out
to see the effectiveness of the samples. Microstructure analysis were observed by
using optical microscope. The phase composition and crystallographic structure of
the composites are evaluated using X-ray diffraction (XRD) analysis. Moreover,
from Rockwell hardness test that has been obtained from this research is 42.23
with temperature reading of 350°C. The addition of CNTs also improved the
thermal and strength of the composites, making them ideal for high-performance
applications in industries such as aerospace and automotive. In conclusion, the
characterization of magnesium alloy composites reinforced with CNTs has shown
great potential for enhancing the properties of magnesium alloys, expanding their
applications to a wider range of industries by referring to the porosity and
hardness tests. The research provides valuable insights into the use of CNTs as a
reinforcing agent and highlights the importance of efficient stress transfer and
interfacial bonding in the design of metal matrix composites.

iii
 ABSTRAK

CIRI-CIRI KOMPOSIT MATRIKS ALOI MG BERTETULANG KARBON

NANOTUBE

Magnesium telah menerima banyak perhatian dalam beberapa tahun kebelakangan

ini kerana beratnya yang ringan, kekuatan khusus yang tinggi, dan kemudahan
kitar semula. Dalam kajian penyelidikan ini, kelakuan mikrostruktur, mekanikal,
dan pengukuhan komposit aloi Mg yang diperkukuh dengan tiub nano karbon
(CNT) telah diperiksa. Magnesium dan kompositnya digunakan dalam aplikasi
teknikal terhad kerana kereaktifan kimia yang kuat, haus rendah, dan rintangan
rayapan kerana mempunyai kualiti pukal yang lemah seperti kekuatan dan
kekakuan, serta rintangan kakisan masin. Oleh itu, dalam kajian ini, komposit
matriks aloi magnesium komposit nanotube karbon bertetulang menggunakan
(CNTSs) serbuk metalurgi telah dibuat. Dalam kajian penyelidikan ini, kaedah
utama yang digunakan ialah metalurgi serbuk. Metalurgi serbuk ialah teknik
keadaan pepejal untuk menghasilkan komposit berasaskan Mg bertetulang zarah.
Metalurgi serbuk terdiri daripada pencampuran, pemadatan, pengisaran, dan
pensinteran. Tambahan pula, ujian kekerasan Rockwell dan Prinsip Archimedes
telah dijalankan untuk melihat keberkesanan sampel. Analisis struktur mikro
dicerap menggunakan mikroskop optik. Komposisi fasa dan struktur kristalografi
komposit dinilai menggunakan analisis pembelauan sinar-X (XRD). Selain itu,
daripada ujian kekerasan Rockwell yang telah diperolehi daripada penyelidikan
ini ialah 42.23 dengan bacaan suhu 350°C. Penambahan CNT juga meningkatkan
terma dan kekuatan komposit, menjadikannya sesuai untuk aplikasi berprestasi
tinggi dalam industri seperti aeroangkasa dan automotif. Kesimpulannya,
pencirian komposit aloi magnesium yang diperkukuh dengan CNT telah
menunjukkan potensi besar untuk meningkatkan sifat aloi magnesium,
mengembangkan aplikasinya kepada julat industri yang lebih luas dengan merujuk
kepada ujian keliangan dan kekerasan. Penyelidikan ini memberikan pandangan
berharga tentang penggunaan CNT sebagai agen pengukuhan dan menyerlahkan
kepentingan pemindahan tegasan yang cekap dan ikatan antara muka dalam reka
bentuk komposit matriks logam.

iv
 ACKNOWLEDGEMENTS

In the name of Allah, the Most Gracious, the Most Merciful.

First and foremost, I would want to express my heartfelt gratitude and
thanks to Allah the Greatest creator of all for His countless blessing in giving me
strength, pretty health, and guidance through my whole journey in completing my
Final Year Project report.
Then, with wholeheartedly I want to express my sincere gratitude and
appreciation to my beloved university which is University Technology MARA
(UiTM) Arau, Perlis especially to my Faculty of Applied Science for providing
me with all equipment and machine to conduct my research smoothly.
Next, very special thanks and unspoken appreciation dedicated for my
dearest supervisor Assoc. Professor Dr. Saidatulakmar Shamsuddin for all the
things that she has delivered and taught, knowledges that has been shared,
attention and her time that has been spent for the whole semester, the patience in
helping the problems that I encountered in this journey, and the encouragement.
In addition, I also like to say thank you to my co-supervisor, Dr.
Nurhidayah Ahmad Zaidi, from University Malaysia Perlis (UniMAP), for being
caring and very committed in helping me and my group members. I pray that
Allah will give you the best health again and hoping to see you again soon.
To my project coordinator, Dr. Khuzaimah binti Nazir who is truly a great
person, I want to say thank you for always be there and never stop from guiding
me from the start until the very end of what should have been done.
Furthermore, no words can describe on how grateful I am to have
supportive parents that always gave their best moral support from afar. Not to
mention, their relentless prayer, motivational words, and their blessing that make
me came this far.
I could not have undertaken my journey without final year project
members which are Nur Aina Solehah, Nur Farhan Natasha, Nur Hazimah, Nur
Laila, and Siti Nurhaziroh. With all their help, I manage to make my Final Year
Project went better and lively.
Last but not least, thank you to all my friends for their unconditional
support and kind words in rising up my self-enthusiasm.
Lastly, only Allah can repay all of the kindness been given towards me
and may He grant us the best thing as return.

(Fakhrul Hakim bin Sahamendan)

v
 TABLE OF CONTENTS

ABSTRACT iii
ABSTRAK iv
ACKNOWLEDGEMENTS v
TABLE OF CONTENTS vi
LIST OF TABLES viii
LIST OF FIGURES ix
LIST OF SYMBOLS xi
LIST OF ABBREVIATIONS xii
CHAPTER 1 INTRODUCTION 1

1.1 BACKGROUND OF STUDY 1

1.2 PROBLEM STATEMENT 3
1.3 SIGNIFICANCE OF STUDY 4
1.4 OBJECTIVES OF STUDY 6
CHAPTER 2 LITERATURE REVIEW 7

2.1 INTRODUCTION 7
2.2 MAGNESIUM ALLOY COMPOSITE MATRIX REINFORCED
CARBON NANOTUBE 8
2.3 APPLICATIONS OF MAGNESIUM ALLOYS 9
2.3.1 In medical application 9
2.3.2 In automotive application 10

2.4 CARBON NANOTUBE 11

2.5 FABRICATION OF MAGNESIUM ALLOY MATRIX
COMPOSITES REINFORCED CARBON NANOTUBE 12
2.6 POWDER METALLURGY PROCESS 13
2.7 SINTERING PROCESS 15
CHAPTER 3 METHODOLOGY 18

3.1 DESCRIPTION OF METHOD 18

3.2 STARTING MATERIAL AND SAMPLE PREPARATION 18
3.3 MIXING 19
3.4 COMPACTING 20
3.5 SINTERING 22
3.6 GRINDING 22
3.7 POLISHING 25
3.8 MEASURING THE PHYSICAL AND MECHANICAL
PROPERTIES OF THE SAMPLES: 26
3.8.1 X-Ray Diffractions (XRD) 26

vi
3.8.2 Archimedes Principle 27
3.8.3 Rockwell hardness test 28

3.9 EXPERIMENTAL FLOWCHART 29

CHAPTER 4 RESULTS AND DISCUSSION 31

4.1 INTRODUCTION 31
4.2 RAW MATERIAL CHARACTERIZATIONS 32
4.2.1 Magnesium powder 33
4.2.2 Zinc powder 34
4.2.3 Carbon nanotube powder 36

4.3 XRD ANALYSIS 38

4.4 FABRICATION OF MG-ZN ALLOY WITH 5 WT% OF CARBON
NANOTUBE 40
4.5 RELATIVE DENSITY 42
4.6 POROSITY 45
4.7 HARDNESS 48
4.8 MICROSTRUCTURE ANALYSIS USING OPTICAL
MICROSCOPE. 50
CHAPTER 5 CONCLUSION AND RECOMMENDATIONS 54

5.1 CONCLUSION 54
5.2 RECOMMENDATION 55
CITED REFERENCES 57
APPENDIX 61
Curriculum Vitae 63

vii
 LIST OF TABLES

Table Caption Page

Table 2.1 Tensile properties of the experimental alloys at room temperature......13

Table 3.1 The weigh for each raw material used..................................................19

Table 3.2 Polishing Stages of the Sample.............................................................24

Table 4.1 Relative density table for 3 samples with different temperature...........42

Table 4.2 Porosity table for 3 different samples with different temperature........46

Table 4.3 Relative hardness for 3 samples with different temperature.................49

viii
 LIST OF FIGURES

Figure Caption Page

Figure 2.1 Various metallurgical procedures for making composites for (a)
powder metallurgy (Radhamani et al., 2018), ((b) hot press sintering, (c) hot-
extrusion, (d) hot rolling, (e) spark-plasma sintering (SPS), (f) stir casting (SC))
(Abazari et al., 2020), (g) disintegrated melt deposition (DMD) (Tjong, 2013),
and (h) high- pressure die casting (Radhamani et al., 2018)................................15

Figure 2.2 An example of Mg/CNT fabrication employing Gemini dispersion

(Abazari et al., 2020)..............................................................................................17

Figure 3.1 Roll mill machine................................................................................20

Figure 3.2 Lab hydraulic press parts cylindrical press mould..............................21

Figure 3.3 Hydraulic press....................................................................................21

Figure 3.4 Grinding process..................................................................................25

Figure 3.5 Solid densimeter meter........................................................................27

Figure 3.6 Hardness machine................................................................................29

Figure 3.7 Flow chart of steps in powder metallurgy...........................................30

Figure 4.1 The result analysis report of particle size for Magnesium powder. 33

Figure 4.2 The result analysis report of particle size for Zinc powder.................35

Figure 4.3 The result analysis report of particle size for Carbon Nanotube powder.

............................................................................................................................... 37

Figure 4.4 XRD result...........................................................................................38

Figure 4.5 Four sample that has been sintered and grinded for four different

temperature. For (a), the sample was sintered in 400°C, (b) for 350°C, (c) for

250°C, and for sample (d) for 200°C.....................................................................41

ix
Figure 4.6 Graph of temperature vs relative density.............................................44

Figure 4.7 Graph of temperature vs porosity........................................................47

Figure 4.8 Graph of temperature vs hardness.......................................................49

Figure 4.9 Optical image of 5x magnification of the composites at varying

sintering temperature after grinding, (a)200°C, (b)250°C, (c)350°C, (d)400°C. . .51

Figure 4.10 Optical image of 5x magnification of the composites at varying

sintering temperature after polishing, (a)200°C, (b)250°C, (c)350°C, (d)400°C. 52

Figure 4.11 Photos from the Surface View of Composite Samples (a)200°C,

(b)350°C, (c)350°C................................................................................................53

x
 LIST OF SYMBOLS

Symbols

°C Celsius

Cm centimeter

D diameter

G gram

K Kelvin

m meter

m milli

μ Mu

ρ Density

W Watt

wt% weight percentage

Al Aluminium

O Oxygen

C Carbon

Co Cobalt

Cr Chromium

Mg Magnesium

Ni Nickel

Ti Titanium

Zn Zinc

xi
 LIST OF ABBREVIATIONS

CNTs : Carbon nanotubes

GNPs : Graphene nanoplatelets

HPS : Hot-press sintering

MMNCs : Magnesium-based metal matrix nanocomposites

MWNTs : Multi-walled carbon nanotubes

PM : Powder metallurgy

PSD : Particle size distribution

SPS : Spark plasma sintering

RPM : Revolutions per minute

XRD : X-ray diffraction

xii
 CHAPTER 1

INTRODUCTION

1.1 Background of study

In recent years, the development of advanced materials has become a critical area

of research, driven by the need for lightweight and high-performance materials in

various industrial applications. Among these materials, magnesium (Mg) alloys

have gained significant attention due to their excellent mechanical properties, low

density, and potential for use in lightweight structures and components. Recently,

because of its small weight, high specific strength, and simplicity of recycling,

magnesium has received a lot of attention (Abazari et al., 2020). Magnesium's

density of 1.738 g/cm3, which is approximately two-thirds that of aluminum,

allows it to be employed in critical applications, making it the lightest structural

material (Upadhyay et al., 2022).

Magnesium-based metal matrix nanocomposites (MMNCs) reinforced with

ceramic nanometer sized particles, graphene nanoplatelets (GNPs), or carbon

nanotubes (CNTs) were created in response to the increased need for lightweight

materials in the aerospace, medical, and automotive sectors (Abazari et al., 2020).

CNTs are commonly mixed with the Mg matrix to create lightweight, high-

strength composites (Sun et al., 2020). The development of magnesium-based

composites can enhance the elastic modulus, wear resistance, and high

1
temperature resistance greatly. Carbon nanotubes, with their potentially high

characteristics, are of particular interest for incorporation into metallic matrix

materials. CNTs' mechanical characteristics are often claimed to have an average

modulus of

2
elasticity of 1-2 TPa, the average age bending strength of multi-walled carbon

nanotubes (MWNTs) was measured to be 14.2 8 GPa, while the tensile strength

ranges from 11 to 63 GPa (Neubauer et al., 2010). CNTs and GNPs offer

outstanding qualities such as a high aspect ratio, a high Young's modulus and

strength, and great electrical and thermal conductivity (Isaza Merino et al., 2017).

Carbon nanotubes (CNTs) are potential reinforcements for lightweight, high-

strength composites. This is because to their tiny diameters, high Young's

modulus, high tensile strength, and chemical stability (Isaza Merino et al., 2017).

Thus, a well-organized of magnesium carbon nanotubes (CNTs) have been

popular as reinforcement in metal matrix composites (MMCs) in recent years due

to their distinctive tubular structure and remarkable mechanical characteristics

(Jagannatham et al., 2020). CNTs, according to (Song et al., 2021), have a good

influence on the conflict between the strength and toughness of Mg matrix

composites. CNTs were discovered to perform a twofold effect in splitting

fracture resistance: homogenizing local strain and slowing crack initiation and

propagation. Moreover, according to Say et al., 2020, Mg alloy metal matrix

composites (MMCs) reinforced with carbon reinforcements (sheet or nanotube

forms) have a lower density and higher specific strength than their ceramic-phased

equivalents.

The results of this research proposal will provide valuable insights into the use of

CNTs as a reinforcing agent in magnesium alloy matrix composites. The findings

can be used to optimize the composition of the composites for specific

3
applications

4
and provide a basis for further development of magnesium alloy composites

reinforced with CNTs. The outcomes of this research proposal have the potential

to impact a wide range of industries, including aerospace, automotive, and

biomedical, by offering lightweight, high-strength, and durable materials.

1.2 Problem statement

Despite numerous intriguing studies on CNT-enhanced composites, CNT-

enhanced Mg matrix composites, particularly at high CNT concentrations, have

not seen widespread application due to three major challenges: CNT dispersion in

the matrix, consolidation with defect-free CNT, and proper bonding at the

CNT/matrix interface to achieve good load transfer between phases (Mindivan et

al., 2014). Moreover, a major challenge in the manufacture of CNT-containing

metal matrix composites is distributing the CNTs uniformly (Mindivan et al.,

2014). Besides, magnesium and its composites are used in restricted technical

applications because to its strong chemical reactivity and low wear and creep

resistance (Say et al., 2020) due to possesses poor bulk qualities like as strength

and stiffness, as well as saline corrosion resistance (Jayasathyakawin et al.,

2020b). Nonetheless, Mg alloys have lesser mechanical strength, particularly at

high temperatures, worse creep behavior, and weaker corrosion resistance when

compared to Al (Abazari et al., 2020). Before introducing carbon nanotubes as an

excellent choice for reinforcing metals and alloys, concerns such as nanoparticle

aggregation and porosity in the synthesis and manufacturing processes should be

5
addressed (Abazari et al., 2020). According to the Shen et al., 2022 study,

although numerous researches on damage simulation in

6
micrometer-scale fiber reinforced polymer composites have been conducted, only

a few have examined the damage behavior of nanoscale CNTs-reinforced

composites, notably MMCs. Perhaps with this contributing research, it can help a

lot of researcher, science society and especially Physics community to produce

more sample of magnesium alloy matrix composites reinforced with carbon

nanotube. Thus, in this study, the use of carbon nanotubes CNTs as reinforcing

agents in magnesium alloy matrix composites will be found. The addition of

CNTs to magnesium alloys can significantly enhance their strength, stiffness, and

toughness, making them ideal for high-performance applications in industries such

as aerospace, automotive, and biomedical and can determine their mechanical and

degradation properties will be determined.

1.3 Significance of study

From this study, it is important to recognize the properties of Mg alloy matrix

composites reinforced carbon nanotube and enhance their uses in various

applications and sectors such as for engineering and medical field. Furthermore,

this research of study is to determine physical and mechanical properties of the

Mg alloy matrix composites reinforced with carbon nanotubes such as its density,

hardness and porosity. The other important of this research of study is to make

sure that it

7
will be one of the effective and methodical way to use in producing a favorable

outcome by using powder metallurgy which consist of weigh, mixing,

compacting, sintering and the selected finishing. As powder metallurgy is one of

the easiest and cheapest method to be access, so it would not be a troublesome to

be done. All of the methodology in powder metallurgy can be optimize by setting

the parameter throughout each process such as the mass of the metal powder in

mixing, mass of the metal powder before compacting and the sintering

temperature due to the melting point of the metal used.

The purpose of this research in the future is to create a great product for various

sector such as automotive, engineering, and even medical as the mechanical and

physical properties being improve and can enhance the strongness and the life

span. Magnesium (Mg) and its alloys are generally regarded as one of the most

promising biomaterials for biological applications among medical practitioners

(Miao et al., 2017). This is due to the fact that Mg alloys strongly show

biodegradable and bioabsorbable properties, plus it is safe to be used in human

body with minimum side effect (Torroni et al., 2017). It can help this sector to be

more advance with this outcome and move forward in coming years. With the

optimization of the parameter, it can hopefully contribute in giving effective,

likeable, and methodical for further and upcoming research. This research can be

simply said that it is still manageable and does not give troublesome in running

the experiment.

8
1.4 Objectives of study

The main objectives of this research are:

1. To fabricate Mg alloy matrix composites reinforced carbon nanotube

(CNT) using powder metallurgy method.

2. To determine physical and mechanical properties of the Mg alloy matrix

composites reinforced with carbon nanotubes (CNT).

9
 CHAPTER 2

LITERATURE REVIEW

2.1 Introduction

Lightweight but strong materials in load-bearing applications are in high demand

in modern technology. Being the lightest structural metal, magnesium (Mg) has a

density of 1.738 g/cm3, which is roughly two-thirds that of aluminium (Abazari et

al., 2020). Mg is also appealing due to its outstanding particular mechanical

properties, good recycling ability, acceptable machinability, good damping

response, nutritional features, adequate electromagnetic shielding, and availability

(Ali et al., 2015), (Chai et al., 2014), (Saberi et al., 2020). However, Mg alloys

have lesser mechanical strength, particularly at high temperatures, worse creep

behavior, and weaker corrosion resistance when compared to Al. Deformation of

materials with an HCP lattice, such as Mg alloys, at room temperature is difficult

due to the restricted number of slip systems (Abazari et al., 2020).

CNTs are thermally and electrically conductive, as strong as diamonds while as

light and malleable as graphite. As a result, carbon nanotubes have the

characteristics of diamond and graphite (Radhamani et al., 2018). It has been

demonstrated that CNTs have ultra- high modulus and strength, as well as

anisotropic electrical conductivity, and that when integrated in a matrix, they may

10
significantly improve manufactured nanocomposites. As a result, using

nanotechnology in material science and

11
engineering might offer up new prospects and research areas for generating

unique metal matrix nanocomposites (MMNCs) (Abazari et al., 2020).

2.2 Magnesium alloy composite matrix reinforced carbon nanotube

According to the study by Hou et al., 2019, the need to reduce energy

consumption and greenhouse gas emissions has pushed the development and

application of lightweight materials. Thus, magnesium has been chosen. The

density of magnesium has been discovered by Upadhyay et al., 2022, to be lower

than that of aluminium and titanium. Magnesium's weaker ductility and lower

strength are features that limit its usage in industrial applications. Furthermore,

because of the limitations with magnesium, it is necessary to improve its

properties in order to increase its usage in diverse applications by adding

reinforcing agents via various process routes (Upadhyay et al., 2022). In recent

years, thorough and critical research have been done to reduce the weight of

materials used in numerous applications without affecting their strength

(Upadhyay et al., 2022). Then, to increase the strength and some other

characteristics of pure magnesium, nanoscale reinforcing agents such as CNTs in

Mg matrices has been chosen to perform in this research study. The uniform

distribution of CNTs in the Mg matrix is required for improvement of the

properties of MMCs reinforced with CNTs. However, the research by Upadhyay

et al., 2022 mentioned that MMCs formed by reinforcing CNTs do not have as

refined mechanical characteristics as MMCs formed by reinforcing nano-platelets

(GNPs). This weakness in the characteristics of MMCs generated using CNTs is

attributed to poor reinforcement bonding with the Mg matrix material. This poor

12
bonding is owing to CNTs' poor wettability in Mg matrix material. Mg and its

alloys are limited in their

13
application due to its low mechanical qualities, poor corrosion resistance, and

limited ductility. CNTs were incorporated into the matrix of Mg material to

improve the properties of Mg and its alloys. The study indicated the above-

described noteworthy alterations in corrosion behavior of MMC caused by the

formation of galvanic corrosion in-between the Mg matrix and the CNTs.

2.3 Applications of magnesium alloys

2.3.1 In medical application

According to (Radha & Sreekanth, 2017), magnesium (Mg) and its alloys have

recently received a lot of attention for orthopaedic applications. Mg alloys

outperform commercially available stainless steel, Co-Cr-Ni alloy, and titanium

implants. Extensive mechanical, in-vitro, and in-vivo research has been conducted

to improve the biomedical performance of Mg alloys by alloying, processing

conditions, surface modification, and other means. Because of their unique mix of

mechanical, biological, and biodegradable qualities, magnesium alloys have

attracted substantial interest in orthopaedic applications. Here are some ways

magnesium alloys are connected to orthopaedic applications:

i. Magnesium alloys have mechanical qualities similar to natural bone, such

as elasticity and compressive strength. This makes them excellent for

orthopaedic implants since they can withstand the weight and strains of the

surrounding bone without producing excessive stress shielding.

14
 ii. Biodegradability is a significant benefit of magnesium alloys. They decay

and are absorbed by the body naturally over time, removing the need for a

second procedure to remove the implant. This characteristic is especially

useful for temporary implants, such as fracture fixation devices, since it

allows natural bone to progressively replace them as the healing process

advances.

iii. Stress shielding occurs when a hard implant absorbs the majority of the

strain, resulting in bone resorption and weakening of the surrounding

bone. Magnesium alloys have a comparable elastic modulus to bone,

decreasing stress shielding effects and encouraging adequate load

transmission, which can improve the bone's long-term health.

However, it is crucial to emphasize that the clinical usage of magnesium alloys in

orthopedic applications is still in its early phases. Researchers are continuously

studying alternative alloy compositions, surface changes, and processing

processes to tackle issues like as corrosion rates, mechanical strength, and

managing the deterioration rate to match the healing process. Clinical trials and

more research are required to prove the safety and efficacy of magnesium alloys

for orthopedic applications.

2.3.2 In automotive application

Magnesium (Mg) alloy is finding increasing use in automobiles, rail

transportation, aerospace, medical, and electrical goods(Liu et al., 2023). Besides,

study by Balaji et al., (2020) stated that magnesium alloys are commonly

employed in automotive

15
applications where heat treatment is crucial. Because of their high strain hardening

rates and plastic strain ratios, magnesium alloys are chosen over many other

known light metals for the fabrication of sheet metal components used primarily

in the automobile sector. According to (Wang & Weiler, 2023), the usage of

magnesium alloy high pressure die cast (HPDC) components for structural

applications is growing, particularly in the automotive and transportation

industries, where weight reduction is critical. Magnesium HPDC components may

be linked in multi- material automotive applications with thread forming fasteners

in ascast states, avoiding the need for drilling and tapping.

Traditional industrial alloys used for high-pressure diecasting in the automobile

sector are based on the Mg-Al system, with the introduction of high-purity

compositions over 40 years ago being the most recent enhancement (Wang &

Weiler, 2023).

2.4 Carbon nanotube

Based on the research by Abazari et al., 2020, it has been demonstrated that CNTs

have ultra-high modulus and strength, as well as anisotropic electrical

conductivity, and that when integrated in a matrix, they may significantly improve

manufactured nanocomposites. CNTs, a form of one-dimensional nanomaterial,

have a high specific surface area ranging from 50 to 1315 m 2/g. CNTs have nano-

sized radial dimensions but micron-sized axial dimensions. The aspect ratio of

CNTs is 100 to 1000, which is significantly larger than that of typical fiber

materials, and the

16
density is as low as 1.3 g/cm3 (Abazari et al., 2020). The C-C covalent bonds in

carbon rings are the most durable chemical bonds in nature, with thermal

conductivity of over 3000 W/mK, equivalent to diamond conductivity. Aside from

their electrical and thermal characteristics, CNTs' exceptional mechanical

capabilities and low density make them ideal for use as reinforcement in the

fabrication of durable nanocomposites (Abazari et al., 2020).

2.5 Fabrication of magnesium alloy matrix composites reinforced carbon

nanotube

The powder metallurgy (PM) technique is the most common and commonly used

method for producing Mg/CNTs composites. Melting and solidification is a

suitable method for metals with low melting temperatures, such as Mg and bulk

metallic glasses. Aside from the aforementioned approach, many efforts on

indigenous processes for manufacturing Mg matrix-CNT composites have been

developed (Abazari et al., 2020). However, certain key challenges in the

fabrication of CNT- reinforced MMCs remain:

i. It is difficult to achieve a homogeneous dispersion due to readily

agglomeration of CNTs caused by robust Van DerWaals forces, the

attractive or repulsive interactions between the carbon atoms.

ii. To maintain the structural integrity of CNTs during the

manufacturing process.

iii. To control sound bonding and compact interfaces for achieving an

appropriate load transfer between phases due to the poor wettability

17
 between carbon and metals, including Mg [(Han et al., 2015),(C. D.

Li et al., 201)].

Table 2.1 shows the tensile characteristics of the AZ91 with TiO2@ CNTs and Pr

additions at room temperature.

Table 2.1 Tensile properties of the experimental alloys at room temperature.

Alloy YS (MPa) UTS (MPa) %E

AZ91 157.23 213.96 5.0
AZ91-Pr 172.39 261.32 4.7
AZ91-Pr-1.0 CNTs 174.63 258.47 4.5
AZ91-Pr-0.5CNTs@TiO2 180.77 346.99 5.3
AZ91-Pr-1.0CNTs@TiO2 194.19 389.67 7
AZ91-Pr-1.5CNTs@TiO2 190.12 377.76 6.7
Source: (N. Li et al., 2021)

2.6 Powder metallurgy process

Powder metallurgy (PM) a solid-state process and casting a liquid-state method

are two commonly used large-scale procedures for manufacturing particle

reinforced Mg-based composites (Abazari et al., 2020). The standard powder

metallurgy approach entails the following steps: mechanical alloying or grinding

to generate a combination of Mg and CNT particles, compression of the obtained

mixture by sintering (Upadhyay et al., 2022). According to the study of Upadhyay

et al., 2022, powder metallurgy is a series of procedures that include establishing a

uniform combination of fine powder elements, compacting the uniform

constituent's mixture, and ultimately sintering the compacted shape. The steps that

has been mentioned above are carried out and been done just to increase the

density of the composites by decreasing the porosity. Through the finding by

Upadhyay et al., 2022, the qualities of the composites, such as poor

machineability, substantially low

18
fracture toughness, and a bad inclination to deform readily, may be easily

addressed by lowering the size of the reinforcement from the particle to the nano

level, and the characteristics are refined as a consequence. Regardless of the

method steps, the main focus has been on producing suitable reinforcement,

which has been accomplished by establishing a uniform distribution of CNTs in

the Mg-based matrix and enough bonding at the Mg/CNT interface (Abazari et al.,

2020). Figure

2.1 shows on various steps that can be use in this research, method (a) and (b) are

chosen.

19
 Figure 2.1 Various metallurgical procedures for making composites for
(a) powder metallurgy (Radhamani et al., 2018), ((b) hot press sintering,
(c) hot-extrusion, (d) hot rolling, (e) spark-plasma sintering (SPS), (f) stir
casting (SC)) (Abazari et al., 2020), (g) disintegrated melt deposition
(DMD) (Tjong, 2013), and (h) high-pressure die casting (Radhamani et al.,
2018).

2.7 Sintering process

Basically, there are many types of sintering which are hybrid microwave-assisted

2-directional sintering method, conventional sintering, hot-press sintering (HPS),

20
spark plasma sintering (SPS). The compressed components are fused in a furnace

to make the final goods. In certain investigations, instead of conventional

sintering, the blended powder was subjected to hot-press sintering (HPS) [(Ding et

al., 2020),(Xiang et al., 2019)]. According to Abazari et al., 2020, the compacted

components were sintered using a hybrid microwave-assisted 2-directional

sintering process at a temperature close to the melting point of Mg before being

hot extruded. The sintering temperature estimate to be around 580°C and put for 2

hours. The main downside of working with CNTs at temperatures above roughly

500°C is the development of carbides at the interface of metal and CNTs, which

can reduce the strength of the composite (Abazari et al., 2020). Figure 2.2

schematically depicts the fabrication process of Mg/CNT composites utilizing

Gemini dispersant.

21
Figure 2.2 An example of Mg/CNT fabrication employing Gemini
dispersion (Abazari et al., 2020).

22
 CHAPTER 3

METHODOLOGY

3.1 Description of method

In this experiment, powder metallurgy method been used. Powder metallurgy is

more adaptable than casting, forging, or extrusion, and it improves interfacial

bonding strength and thermal characteristics (Sharma et al., 2022). The major goal

of this research is to look at the mechanical characteristics and microstructure of

magnesium that has been reinforced with CNT utilizing powder metallurgy

method and sintering in argon atmosphere. Powder metallurgy has various

advantages, including the capacity to construct complicated forms and

sophisticated geometries, the ability to eliminate material waste, and the ability to

use a wide range of metal alloys. It is widely utilized in sectors like as automotive,

aerospace, electronics, and medical devices, where it permits the fabrication of

high-performance components with qualities customized to specific technical

needs. According to the study by Kumar & Pandey, 2020, the final compressive

strength and heating rate are affected by compaction pressure, sintering

temperature, heating rate, and soaking time in powder metallurgy.

A particle size analyzer is a scientific equipment used to measure and analyze

the particle size distribution in a sample. All metal powders (Mg, Zn, graphite)

were sieved at 65 m before analyzing particle size. The particle size analyzer's

laser beam is sent through the dispersed powder sample, and the scattered
23
light is measured at various angles. The dispersed light's intensity and pattern

reveal information about the particle size distribution. The particle sizes

distribution is calculated using mathematical techniques based on the diffraction pattern.

3.2 Starting material and sample preparation

For each metal substance, the calculation has been made to get the precise weight

and to produce enough amount of green sample and suitable size when get into

compressing. Magnesium powder (83wt%), zinc powder (12wt%), carbon

nanotube powder (5wt%), and stearic acid (2wt%) were mixed. For each metal

powder, the weightage be multiplied with 3g and then as it be made for 5 samples

then it was multiplied with 5. In table 3.1, the calculation of each raw metal

substance been calculated showed.

24
 Table 3.1 The weigh for each raw material used.

Mg → 83% × 3g = 2.49g × 5 = 12.45g Eq. (3.1)

Zn → 12% × 3g = 0.36g × 5 = 1.8g Eq. (3.2)

Carbon nanotube → 5% × 3g = 0.15g × 5 = 0.75g Eq. (3.3)

+2wt% of stearic acid × 3g = 0.06g × 5 = 0.3g Eq. (3.4)

3.3 Mixing

Powdered Mg and CNTs been combined to make a homogeneous mixture; this

mixture was then shaped in a true shape die, and the compressed and compacted

shape of the powder combination was sintered in a furnace to form the final

reinforced product (Upadhyay et al., 2022). Mixing device putted for 120 rpm and

after all substance has been weigh and put together, then it was set on mixing

device for 20-30 minutes. Figure 3.1 shows the roll mill machine that been used to

mixing the elements.

25
 Figure 3.1 Mixing miller by Panasonic DVUX960W.

3.4 Compacting

After been mixing, the metal powders inserted into the mould for compacted by

using hydraulic press at 8 tons and after that it let for rest for 2 minutes. There are

two types of pressing method which are cold pressing and hot pressing. In this

study, cold pressing was chosen by using hydraulic press. The product obtained

then named as green sample and the amount of green sample that should be done

are 5 samples. Figure 3.2 showed the mould that being used to put the mixed

powder before compacting by using the hydraulic press showed in figure 3.3.

26
Figure 3.2 Lab hydraulic press parts cylindrical press mould.

Figure 3.3 Specac Hydraulic press.

27
3.5 Sintering

After compacting process, the green samples go through sintering in a sintering

furnace. Sintering is a process which the compacted product heated to a

temperature just right below their melting point. This process will help in make

the bond of the particles to become together and formed a solid mass. The green

sample be heated in 5 different temperatures which are 200°C, 250°C, 300°C,

350°C, and 400°C. For each temperature, heating rate of 5°C/min been applied for

one hour of heating. After been sintered, the sintered part let to rest and cool

down. Then, it will be finish by grinding as the aim is to achieve the required form

mechanical and physical properties.

3.6 Grinding

To study the properties and behaviors of metallic materials, the metallographic

process is commonly used in materials science, metallurgy, and engineering. A

metallographic technique is a set of steps used to prepare, evaluate, and analyze

the microstructure of metallic materials. It is also known as metallographic sample

preparation or metallographic analysis. This procedure required generating a thin,

polished piece of the material that can be examined under a microscope in order to

analyze its internal structure, grain size, grain boundaries, phases, inclusions, and

other microstructural properties According to Zhang et al., (2023), grinding is

critical in assuring the final machining quality of composite components during

the production process. In this method, the sintered sample then been grinded by

many layers of sand paper with different grit started from 240 which was the

roughest that

28
been used then changed to 320, 400, 500, 600, 800, 1000, 1500, 2000, 3000, 5000,

and 7000 which was the smoothest that been used. The machine that been used

was grinding/polishing machine. Table 3.1 shows polishing stages of sample

meanwhile Figure 3.4 showed how the grinding process been carried.

Figure 3.4 Grinding process.

29
 Table 3.2 Polishing Stages of the Sample

Order of Surface Abrasive Disc Rotating Lubricant

stages No. Speed (rpm)

1 SiC paper 320 300 water

2 SiC paper 400 300 water

3 SiC paper 600 300 water

4 SiC paper 800 300 water

5 SiC paper 1000 300 water

6 SiC paper 2000 300 water

7 Polishing 6μ diamond 70 glycerin

cloth pastes

8 Polishing 3μ diamond 70 glycerin

cloth pastes

9 Polishing 1μ diamond 70 glycerin

cloth pastes

30
3.7 Polishing

The samples then were polished by using diamonds with value of 6-micron, 3-

micron, and 1-micron. Polishing is important in powder metallurgy for various

reasons such as polishing serves to increase the surface polish of powder

metallurgy components. During the compaction and sintering operations, the

pieces may obtain a rough or uneven surface. Polishing eliminates surface

abnormalities including holes, cavities, and roughness, resulting in a smoother and

more visually attractive surface. This is especially crucial for parts that must have

a high level of appearance, such as automobile components, consumer items, or

medical gadgets. Then, polishing can also be used to improve the mechanical

qualities of powder metallurgy components. It can decrease surface flaws like

microcracks and voids that function as stress concentrators and degrade the

component. Polishing can increase the part's strength, fatigue resistance, and

overall mechanical performance

31
by eliminating these faults. The most important thing was polishing helps in the

cleaning of the surface of powder metallurgy components by eliminating any

leftover impurities or oxides that may have accumulated during the production

process.

3.8 Measuring the physical and mechanical properties of the samples:

In these methods, three tests been carried out which were X-Ray Diffraction,

Archimedes Principle, and Rockwell hardness test. These three tests were carried

out to test on the physical and mechanical properties of the fabricated samples that

has been created and obtained.

3.8.1 X-Ray Diffractions (XRD)

X-ray diffraction (XRD) is an effective analytical method for studying the atomic

and molecular structure of materials. Its principal role is to identify a sample's

crystallographic information, such as the atomic arrangement inside the crystal

lattice and the space between crystal planes. XRD is often used to determine the

presence of crystalline phases in a material. Each crystalline phase has a different

diffraction pattern due to its unique atom arrangement. The phase composition of

a sample can be identified by comparing the diffraction pattern of an unknown

sample to a database of known patterns. Besides, XRD is used to determine a

material's crystal structure.

32
3.8.2 Archimedes Principle

The buoyant force experienced by an object immersed in a fluid is described by

Archimedes' principle, a basic principle in physics. It asserts that when an item is

partially or completely immersed in a fluid, an upward buoyant force equal to the

weight of the fluid displaced by the object is experienced. The weight of the

sample is measured in both air and distilled water. Here is the formula for density:

Bulk density
Relative × 100% Eq. (3.5)
density = Theoretical
density

Dry weight
Bulk density × Density of Water Eq.
= Soak weight − wet (3.6)
weight

Theoretical Density

ρ = (Density Mg) (83%) + (Density Zn) (12 wt%) + (Density CNT) (5%)
Eq. (3.7)

Figure below used to find the wet and soaked weight of samples to use in the

relative and bulk density formula.

33
Figure 3.5 Electronic densimeter MD-300

34
3.8.3 Rockwell hardness test

Rockwell hardness testing is one of the most often used procedures for

determining the state of a metal in response to heat and/or mechanical treatments

(Shabel, 1987). The Rockwell hardness test is a popular method for determining

the hardness of a substance, especially metals. It calculates the depth of an

indenter’s penetration into a material under a given load. On the Rockwell scale,

the Rockwell hardness value is given as a hardness number.

The Rockwell hardness test is normally performed as follows:

i. Setup the test by making sure the sample material is level, clean, and free

of any surface imperfections or coatings. The sample should be thick

enough to accommodate the depth of the indentation.

ii. Based on the material and predicted hardness range, select the suitable

Rockwell scale and indenter.

iii. Position the sample on the anvil of the Rockwell hardness testing

equipment at first. During the test, the anvil offers a steady support for the

sample.

iv. Lower the indenter until it makes preliminary contact with the sample

surface. This is accomplished by delivering a modest load, referred to as

the preliminary test force. The preliminary contact ensures that the

indenter is oriented correctly and in touch with the sample.

v. Apply the total test load by adding the major load to the preliminary test

force. The specified Rockwell scale is used to determine the primary load.

It is normally kept for a set amount of time to allow for appropriate

indentation.

35
 vi. Once the complete force is applied, the machine automatically measures

the depth of penetration of the indenter. This depth is reported as the

Rockwell hardness value. It is often represented on a dial or digital

readout.

vii. After the measurement is finished, the whole load is withdrawn and the

indenter is retracted from the sample.

viii. Document the acquired Rockwell hardness value, as well as the related

Rockwell scale and test conditions.

Figure 3.6 showed hardness machine in UNIMAP’s lab.

Figure 3.6 AFFRI Rockwell hardness test.

3.9 Experimental flowchart

Figure 3.7 showed the flow chart of the methodology for this research

study from the first step until the final step.

36
Figure 3.7 Flow chart of the powder metallurgy methods.

37
 CHAPTER 4

RESULTS AND DISCUSSION

4.1 Introduction

Due to their unusual mix of features, magnesium (Mg) alloy matrix composites

reinforced with carbon nanotubes (CNTs) have received a lot of interest in recent

years. CNT insertion into Mg alloys has the potential to improve mechanical,

thermal, and electrical characteristics, making them ideal for a wide range of

applications. The goal of this data characterization is to offer a thorough

knowledge of the behavior and performance of Mg alloy matrix composites

reinforced with CNTs.

The information and data collected and shown here concerned with the

characterization of Mg alloy matrix composites with varied CNT content,

manufacturing processes, and reinforcement topologies. The characterization

process encompasses a variety of analytical procedures and experiments that

analyses the composites' structural, mechanical, thermal, and hardness

characteristics.

Mechanical characterization, which includes Rockwell hardness testing, is used to

assess the strength and toughness of composites. The findings show how the

38
inclusion of CNTs affects mechanical parameters, particularly strength, hardness,

and fracture behaviors. Density and porosity check also can be use to determine

the benefits and uses for each sample. Optical image also can be really useful as to

determine the microstructure of the sample. The data characterization of Mg alloy

matrix composites supplemented with CNTs reveals important information about

the potential benefits and limits of these materials.

4.2 Raw material characterizations

Three metal powders that been used in this research which were Mg, Zn, and C

has undergone particle size analysis process. Particle Size Distribution (PSD)

analysis helps in understanding the range and distribution of particle sizes within a

sample. PSD data may be used to learn about particle packing, segregation, and

the existence of agglomerates or fines. This data is critical for improving

operations including powder handling, fluidization, filtering, and blending.

39
4.2.1 Magnesium powder

With the fast expansion of the construction, automobile, and other industries

(Danzi & Marmo, 2019), the need for high-strength low-sulfur steel is rising, and

many steel mills frequently employ magnesium powder to extensively desulfurize

ordinary steel in order to produce high-quality steel. Furthermore, magnesium

powder is widely employed in the aerospace, military, petroleum, chemical,

pharmaceutical, smelting, and other sectors [(Guo et al., 2011),(Jayasathyakawin

et al., 2020a)]. In this part, the particle size distribution of the powder is an

important parameter that will be discussed as it affects the flowability,

compaction, and sintering behavior. Techniques such as laser diffraction,

sedimentation, or microscopy can be used to determine the particle size

distribution and average particle size of the powder. Figure 4. Below showed the

particle size for magnesium powder. Below is the figure of particle size for

Magnesium.

Figure 4.1 The result analysis report of particle size for Magnesium powder.

From the graph, the particle size distribution of magnesium powder can be

described using the values d (0.1), d (0.5), and d (0.9). These values represent the

particle diameter at which a certain percentage of particles are smaller than or

40
equal

41
to that diameter. From the information, the three situations can be described in

more detail.

For d (0.1) = 32.717: This number shows that 10% of the magnesium particles

have a diameter of 32.717 units or less. To put it another way, it reflects the

particle size at which 10% of the particles fall.

Then, for d (0.5) = 65.363: This number shows that 50% of the magnesium

particles have a diameter equal to or less than 65.363 units. It indicates the median

or average particle size, often known as the D50 value. This signifies that half of

the particles are less or equal to this size, while the other half are bigger.

Finally, d (0.9) = 120.401 This number shows that 90% of the magnesium

particles have a diameter of 120.401 units or less. It denotes the particle size at

which 90% of particles fall.

The particle size distribution of magnesium powder may be calculated using these

data. In this scenario, the bulk of the particles had sizes ranging from 32.717 to

120.401 units, with the average particle size being about 65.363 units. This data is

useful for understanding and managing particle size ranges in powder metallurgy

operations.

4.2.2 Zinc powder

Zinc powder is a thin metallic powder that contains zinc particles. It is

commercially available in a variety of particle sizes, surface coatings, and purities.

Zinc powder is generally made up of pure elemental zinc (Zn) for its makeup.

It is primarily

42
made by reducing zinc oxide (ZnO) or electrolytically refining zinc. Furthermore,

the physical qualities of zinc powder are often grey or silver in color. It has a wide

range of particle sizes, from coarse particles to exceedingly small powders. The

morphology of the particles can also vary, with irregular or spherical particles

being the most prevalent. The purity of zinc powder varies, ranging from high-

purity zinc with few impurities to industrial-grade powders with greater impurity

levels. The purity of the powder is determined by the application and criteria.

Particle size result analysis report for Zinc shown below for discussion.

Figure 4.2 The result analysis report of particle size for Zinc powder.

For d (0.1) = 6.342: This number shows that 10% of the zinc particles have a

diameter of 6.342 units or less. To put it another way, it reflects the particle size at

which 10% of the particles fall.

Next, d (0.5) = 12.792: This number shows that 50% of the zinc particles have a

diameter of 12.792 units or less. It indicates the D50 value, which is the median or

43
average particle size. This signifies that half of the particles are this size or less,

while the other half are bigger.

Then, d (0.9) = 26.003: This number shows that 90% of the zinc particles have a

diameter equal to or less than 26.003 units. It reflects the particle size at which

90% of the particles fall.

The particle size distribution of zinc powder may be calculated with these data. In

this situation, it shows that the bulk of the particles had sizes ranging from 6.342

to

26.003 units, with the average particle size falling somewhere between 12.792 and

6.342 units. This information is useful for understanding and regulating the

particle size range during operations such as powder handling, compaction,

sintering, or blending, where particle size can affect attributes like as flowability,

packing density, and reactivity.

4.2.3 Carbon nanotube powder

Carbon nanotube powder is a powdery aggregate of carbon nanotubes. Carbon

nanotubes are cylindrical structures made of carbon atoms organized in a

hexagonal lattice. CNT powders can have a variety of qualities based on

parameters such as the kind of nanotube (single-walled or multi-walled), diameter,

length, and surface functionalization.

Last but least, carbon nanotube particle size result analysis report discussed based

on the figure below.

44
 Figure 4.3 The result analysis report of particle size for Carbon Nanotube
powder.

To begin, d (0.1) = 13.815: This figure shows that 10% of carbon nanotubes have

a diameter of 13.815 units or less. To put it another way, it reflects the particle

size at which 10% of the particles fall.

Next, d (0.5) = 34.722: This figure implies that 50% of the carbon nanotubes have

a diameter of 34.722 units or less. It indicates the D50 value, which is the median

or average particle size. This signifies that half of the particles are this size or less,

while the other half are bigger.

For d (0.9) = 68.068, then: This figure implies that 90% of carbon nanotubes have

a diameter of 68.068 units or less. It denotes the particle size at which 90% of

particles fall.

The particle size distribution of carbon nanotubes may be calculated using these

data. In this scenario, the bulk of the carbon nanotubes had diameters ranging

from
45
13.815 to 68.068 units, with an average particle size of 34.722 units. This

knowledge is useful for understanding and managing the particle size range

throughout a variety of processes, including dispersion, mixing, and composite

production, where particle size can impact attributes like as stability, packing

density, and reinforcing effects.

4.3 XRD Analysis

Figure 4.4 XRD analysis of Mg alloy matrix composites sintered at 400°C.

X-ray diffraction (XRD) is used to examine the atomic and molecular structure of

materials. XRD is a powerful method that uses X-ray scattering by a sample's

crystal lattice to offer information on its crystallographic characteristics.

46
XRD is commonly used to determine the crystalline phases of a substance. Each

crystalline phase has a particular diffraction pattern due to the unique arrangement

of atoms inside the crystal lattice. The phase composition of a sample can be

47
determined by comparing the observed diffraction pattern to known reference

patterns or databases. Based on the Figure 4.4, from the peak that has been shows,

only the highest peak one was chosen to be discussed as the remaining peaks were

considered as noise. In this research, Mg, Zn, and C elements were expected to be

appeared in the XRD result. Even though the main elements which are Mg and Zn

does not appear as single element but it comes with the combination of those two

elements which was Magnesium Zinc. This demonstrates that the created sample

includes the correct elements that correspond to the research project. In addition,

those elements that has been found in the XRD data analysis were after search and

match step been carried out until the black peak went missing. This also met the

match from the database that being used which is PDF-2 Release 2023.

As shown in Figure 4.4, impurity of the samples been detected such as diamond,

lignite, and magnesium zinc carbide. The amorphous or can be called as

impurities can be said came from the early sample preparation and processing.

The existence of amorphous or impurity signals can result from a variety of

sample preparation and processing parameters. Incomplete crystallization during

synthesis, insufficient annealing or heat treatment conditions, contaminants

introduced during material synthesis or processing processes, or the production of

glassy or amorphous phases owing to fast cooling or quenching are examples.

Lignite might be come from the sintering process and diamond might came from

polished sample.

Besides, chemical composition and impurity sources may also be factors, as

impurities can come from a variety of sources, including raw materials,

48
contamination during processing, or the existence of by-products or subsequent

phases. Understanding the chemical composition and impurity sources can aid in

identifying the precise impurities responsible for the XRD data signals.

4.4 Fabrication of Mg-Zn alloy with 5 wt% of Carbon Nanotube

Based on the objective to fabricate Mg Alloy, matrix composites reinforced

carbon nanotube (CNT) using powder metallurgy method, it has been achieved.

For this research, 3 samples were sent for sintering and that were 200°C, 350°C,

and 400°C. These 3 samples also have gone through until the final method,

hardness. Figures below shows 4 samples that has went through sintered and

grinding process.

49
 (a) (b)

(c) (d)

Figure 4.5 Four sample that has been sintered and grinded for four
different temperature. For (a), the sample was sintered in 400°C, (b) for
350°C, (c) for 250°C, and for sample (d) for 200°C.

50
4.5 Relative density

The function of relative density, also known as specific gravity or density ratio, is

to measure a substance's or material's density in relation to the density of a

reference substance. It is a dimensionless ratio that expresses crucial information

about the density of a material in respect to another component, commonly water.

The relative density, which is expressed as a percentage, shows how much denser

the substance is than water. Along with the tendency seen in bulk density, the

relative density rises with temperature as well. According to Archimedes'

principle, relative density is critical in determining buoyancy and the resulting

upward force felt by an item submerged in a fluid. Table 4.1 shows the value for

bulk density and relative density for 3 samples with different 3 temperatures.

Table 4.1 Relative density table for 3 samples with different temperature.

Sample Temperature Dry Wet Soaked Bulk Relative

𝒈
density
( ⁄
(°C) weight(g) weight(g) weight(g) density

𝒄𝒎𝟑
) (%)
1 200 1.61 0.74 1.73 1.63 67.63
2 350 1.76 0.77 1.75 1.80 74.69
3 400 1.84 0.84 1.81 1.90 78.84

As the temperature climbs from 200°C to 400°C, bulk density rises as well. This

is consistent with typical behaviors since at higher temperatures, the moisture

content decreases and the material becomes denser. In finding relative density by

using Archimedes' principle, it means to find an object's relative density is critical

for predicting its behaviors in a fluid. One may predict whether an object will

float, sink, or remain suspended by comparing the densities of the object and the

fluid. But in this research, the purpose is to find which density is the highest and

lowest
51
as it will determine the porosity. So, to find the relative density, formula in 3.8.2

been used. Calculation shown as below:

Bulk density
Relative × 100% Eq. ()
density = Theoretical
density

Dry weight
Bulk density × Density of Water Eq. ()
= Soak weight − wet
weight

Theoretical Density

ρ = (Density Mg) (83%) + (Density Zn) (12 wt%) + (Density CNT) (5%)
Eq. ()

Theoretical density

𝑔
𝜌 = (1.738) (0.83) + (7.13) (0.12) + (2.26) (0.05)⁄𝑐𝑚
= 2.41
Eq. ()
3

Bulk density for sample 1:

1.61 𝑔
× 1 = 1.63
⁄
1.73 − 0.74 𝑐𝑚3

Bulk density for sample 2:

1.76 𝑔
× 1 = 1.80
⁄
1.75 − 0.77 𝑐𝑚3

Bulk density for sample 3:

1.84
52
 𝑔
× 1 = 1.90
⁄
1.81 − 0.84 𝑐𝑚3

53
Relative density for sample 1:

1.63
2.41 × 100% = 67.63%

1.8
Relative density for sample 2:

0 × 100% = 74.69%
2.4
1

1.9
Relative density for sample 3:

0 × 100% = 78.84%
2.4
1

Figure 4.6 Graph of temperature vs relative density.

Based on the graph above, it is linear which means the relationship between the

temperature and relative density linear. This means that the changes in

temperature does not seem proportional change in relative density as the

temperature rises then the relative density increases.

54
Some compounds go through phase transitions, which cause their density to rise

with temperature. Temperature-dependent solubility changes, for example, might

55
cause an increase in relative density when temperature rises in some solutions or

combinations.

The atoms or molecules in a solid gain energy and vibrate more strongly as the

temperature rises, increasing the average distance between them. As the

interatomic/molecular separation increases, the density decreases, making the

solid less dense at higher temperatures.

Increased Mg concentration promotes dislocation density evolution and

dislocation-dislocation interactions, leading in significant strain hardening

(Thirathipviwat et al., 2022)
. Chemical reactions can also have an impact on the

temperature-density relationship. In some situations, increasing the temperature

can promote chemical reactions that result in denser compounds, resulting in an

overall rise in relative density. Certain materials may display unexpected or

aberrant behavior, resulting in a positive association between temperature and

relative density in unusual situations. These examples usually include one-of-a-

kind compositions, structures, or attributes.

Thermal expansion is responsible for the reduction in relative density with rising

temperature. When a material is heated, the average kinetic energy of its

molecules increases, forcing them to move faster and take up more space. As a

result, the substance's density reduces.

4.6 Porosity

The existence of empty spaces or pores within a substance is referred to as

56
porosity. It compares the volume of empty space or voids to the overall volume of

the material. Porosity may be found in a wide range of materials, including solids,

liquids, and gases. It is important in determining material qualities and behaviour

57
in domains such as materials science and engineering. The volume of empty

spaces or voids within a substance is represented by porosity. The size, shape, and

distribution of these spaces might vary. They can be linked together to form a

network of open pores, or they can be isolated, with minimal or no

interconnectivity.

Table 4.2 Porosity table for 3 different samples with different temperature.

Sample Temperature (°C) Relative Density (%) Porosity (%)

1 200 67.63 32.27

2 350 74.69 25.31

3 400 78.84 21.16

From the above data of relative density, the porosity can be calculated by using

the formula below:

𝑃𝑜𝑟𝑜𝑠𝑖𝑡𝑦 = 100% − 𝑟𝑒𝑙𝑎𝑡𝑖𝑣𝑒 𝑑𝑒𝑛𝑠𝑖𝑡𝑦 (%) Eq. ()

Porosity for sample 1:

Porosity = 100%-67.73% = 32.27% Eq. ()

Porosity for sample 2:

Porosity = 100%-74.69% = 25.31% Eq. ()

Porosity for sample 3:

Porosity = 100%-78.84 = 21.16% Eq. ()

58
 Figure 4.7 Graph of temperature vs porosity.

Temperature and porosity show a decreasing graph as shown in Figure 4.7. According to
(Li et al., 2022)
,researchers have sought to link the porosity of die casting Al and Mg alloys to their tensile

characteristics in recent decades. The anticipated area fraction of porosity (f) on the fracture surface

has been proposed as the primary factor influencing tensile characteristics . This indicates that the

change in porosity with temperature is not constant, but rather varies across temperature ranges. Curves,

bends, or inflection points in the graph may indicate complicated interactions between temperature and

porosity.

Numerous applications may be taken into account when porosity, which refers to

how many voids or open spaces are present within a material, is higher. The kind

of material used and the desired result would determine the precise application

such example in lightweight components or structures can be created using high

porosity materials. For applications where weight reduction is crucial, like in the

aerospace or automotive industries, the presence of voids lowers the total density.

High porosity materials can collect and hold onto gases or liquids in their voids.
59
For applications like sponges, absorbent pads, or even some forms of clothing

for

60
moisture control, this feature is helpful. So that, in this research, sample 1 is the

best for this application compared to other 2 samples.

The porosity values change among the multiple temperature readings within each

data point, demonstrating that the porosity measurements are variable. The

porosity measurements consistently decrease as the temperature rises. For

temperatures of 200°C, 350°C, and 400°C, the average porosity values are

30.77%, 42.23%, and 38.43%, respectively. It is crucial to highlight that this

research is based on the available data points, and it is impossible to draw

conclusive conclusions regarding the link between temperature and porosity

without a bigger dataset and a more diversified temperature range.

4.7 Hardness

An understanding of a metal's mechanical qualities can be gained by determining

the inherent hardness of the metal through hardness testing. It enables the

evaluation of various materials' relative hardness levels and their comparison.

Testing for hardness is a crucial quality assurance step in the production of metal

components. Manufacturers may make sure that the produced parts satisfy the

necessary criteria and are of consistently high quality by checking the hardness.

The hardness test helps in deciding which metal is best for a given application.

The hardness test identifies metals that have the desired hardness levels and

mechanical qualities, depending on the requirements, such as load-bearing

capacity or wear resistance.

61
 Table 4.3 Relative hardness for 3 samples with different temperature.

Sample Temperature First Second Third Average

reading reading reading
1 200 40.9 17.3 34.1 30.77
2 350 54.1 43.2 29.4 42.23
3 400 31.5 54.2 29.6 38.43

Figure 4.8 Graph of temperature vs hardness.

The average hardness values for each temperature may be used to compare the

hardness of a material at different temperatures. Greater resistance to indentation

or penetration is indicated by higher average hardness levels.

From the above graph, it showed inconstant reading as maybe come from any

irregularities or unexpected patterns in the hardness-temperature connection may

62
be highlighted by the graph. These abnormalities may be caused by material

flaws, impurities, or particular phase transitions that alter hardness.

4.8 Microstructure analysis using optical microscope.

After all methods has been done, this was the last step that need to be do. Optical

microscope was used and 4 kind of magnification been used (5x, 10x, 20x, 50).

By using Dino application and Olympus camera, these photos were managed to be

taken.

It is possible to determine distinct phases existing in the material by studying the

microstructure under different illumination conditions or utilizing specialized

procedures. Different crystalline forms, solid solutions, or discrete areas with

diverse chemical compositions can all be considered phases.

Various sorts of uncontrolled insertion, such as contaminants, second-phase

particles, or voids, can be detected and analyzed using an optical microscope.

Defects like as dislocations, fractures, and porosity can also be seen. These

characteristics reveal information about the material's quality, production

circumstances, and possible mechanical flaws.

The optical microscope examines the surface topography of the material,

including properties such as roughness, scratches, and wear patterns. Surface

properties can reveal information about processing conditions, surface treatments,

and material interactions.

63
 (a) (b)

(c)

Figure 4.9 Optical image of 5x magnification of the composites at varying

sintering temperature after grinding, (a)200°C, (b)350°C, (c)400°C.

64
 (a) (b)

(c)

Figure 4.10 Optical image of 5x magnification of the composites at

varying sintering temperature after polishing, (a)200°C, (b)350°C,
(c)400°C.

65
 (a)

(b)

(c)

Figure 4.11 Photos from the Surface View of Composite Samples

(a)200°C, (b)350°C, (c)350°C.

66
 CHAPTER 5

CONCLUSION AND RECOMMENDATIONS

5.1 Conclusion

In conclusion, the characterization of magnesium (Mg) alloy composites with a

matrix reinforced by carbon nanotubes (CNTs) represents a viable path for

improving the mechanical and functional characteristics of these materials by

using powder metallurgy method. A thorough examination of the composite's

microstructure and mechanical behavior reveals that the insertion of CNTs into

the Mg matrix resulted in considerable gains in strength, porosity, and relative

density.

Testing the composite's mechanical characteristics, hardness offers information

about the reinforcing effect of CNTs and temperature of 400°C known to be an

optimal temperature in fabricating Mg-Zn alloy reinforced Carbon Nanotube

because of it is high in density, low in porosity, and quite high in hardness

reading. Temperature of 200°C is unperformable compared to another two-

temperature due to high porosity and low reading for Rockwell hardness test. The

microstructure of the Mg alloy-CNT composite is characterized using X-Ray

diffraction and an optical microscope to evaluate the distribution, alignment, and

interfacial bonding between the CNTs and the Mg alloy matrix. The inclusion of

well-dispersed and aligned CNTs may often improve the mechanical

67
characteristics of the Mg alloy, increasing its strength and stiffness.

68
The evaluation of Mg alloy matrix composites supplemented with carbon

nanotubes entails a thorough examination of the microstructure and mechanical

characteristics. These characterizations help to understand the efficacy of CNT

reinforcement and assist the development and optimization of Mg alloy-CNT

composites for a variety of applications.

From this research, the two objectives successfully achieved which were to

fabricate Mg Alloy matrix composites reinforced carbon nanotube (CNT) using

powder metallurgy and the second objective to determine physical and mechanical

properties of the Mg Alloy matrix composites reinforced with carbon nanotubes

(CNT) also completely been carried with Archimedes’ Principle, porosity,

hardness, and optical image method.

5.2 Recommendation

For recommendation, I assure that this research about Characterization of Mg

Alloy Matrix Composites Reinforced Carbon Nanotube is really a good research.

A lot of enhancement can be done in future especially in industry, medical,

transport, and even army. Here is some improvement that can be done in future

research:

i. In this research, lots of improvement on methodology should be taken care

especially at the preparing sample, mixing by using ball milling,

compacting, and sintering as this experiment is really important to the

future such as powder treatment, right way of milling, correct temperature

and precise time for sintering also should be taken care.

ii. Use sophisticated characterization techniques like as electron microscopy

69
 and spectroscopy to get insight into CNT dispersion and its influence on

composite characteristics. Examine the dispersion, alignment, and

interfacial bonding between CNTs and the Mg matrix using scanning

electron microscopy (SEM) and transmission electron microscopy (TEM).

High-resolution imaging may reveal the distribution of CNTs, the

existence of flaws, and the overall microstructure of the composite.

iii. To evaluate the mechanical characteristics of the composite, conduct a

variety of mechanical tests, including tensile, compressive, and hardness

testing. To evaluate the reinforcing impact of CNTs, compare these

parameters to those of the virgin Mg alloy. Consider fatigue testing as well

to verify the material's resilience under cyclic loads.

70
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 APPENDIX

Figures

The evolution of carbon nanotubes at various phases and their main advancements
in diverse applications over time.

Digital vernier caliper.

76
Olympus optical microscope.

77
Particle size analysis report for Magnesium powder.

78
Particle size analysis report for Zinc powder.
79
Particle size analysis report for Carbon Nanotube powder.

80
 CURRICULUM VITAE

A. Personal profile
Full name Fakhrul Hakim bin Sahamendan
National IC no 981105 06 66811
Birth date 5th November 1998
Citizenship MALAYSIA
Place of birth Kuantan, MALAYSIA
Gender Male
Correspondence address No. 31 Lorong BDK 1/9
Bandar Damansara
Kuantan 25559 Kuantan
Pahang
Telephone no.(H) 609 567 7913
Telephone no. (HP) 6019 999 4100
Email address [email protected]

B. Hobbies and interests

As for me, I love to listening to music, read novels that have
fantasy, mystery, and science-fiction genre, and watch some
good movies. Besides, I’m always excited to go for a treasure at
new places either in city or nature. That is because I’m deeply in
love with how amazing some building and the place were built
from the perspective of the design and the history behind it, and
for nature for some good reason it can give me peace even
when I just look at them.
In addition, I am very good at writing in English and Malay as
well as speaking. I also do have basic knowledge and still
learning on Japan and Mandarin language.

C. Academic qualifications
Degree Area Institution Year
Awarde
d
B. Sc. Physics Universiti Teknologi 2024
(Hons. MARA, Malaysia
)
Diplom Diploma Universiti Teknologi 2020
a in MARA, Malaysia
Science
SPM Scienc Sekolah Berasrama Penuh 2015
e Integrasi Kuantan, Malaysia

81
 D. Work experience
While I never have any working experience in any kind of sector
especially in my field of study which is Physics but still, I am a
fast learner, organized person, and I am quite confident that I
could do and manage any kind of task that will be given and
hoping that my future senior colleague, supervisor, and manager
will find that I have exceed their expectations.

E. Related experience
Post Place Year
Member Community Organization of Applied Sciences 2018
Tapah (ASET), Faculty of Applied Sciences,
Universiti Teknologi
Mara, Tapah
Facilitat English improvement between Faculty of Apllied 2018
or Sciences
and Sekolah Kebangsaan Satu, Tapah, Perak, Malaysia

82