UNIVERSITI TEKNIKAL MALAYSIA MELAKA

THE INFLUENCE OF BENTONITE ON GLASS WASTE FILLED

SPENT BLEACHING EARTH (SBE) COMPOSITE.

This report submitted in accordance with requirement of the Universiti Teknikal

Malaysia Melaka (UTeM) for the Bachelor Degree of Manufacturing Engineering

(Engineering Materials) (Hons.)

by

NUR LIYANA BINTI MOHD DAUD

B051110237

880507065312

FACULTY OF MANUFACTURING ENGINEERING

2014

UNIVERSITI TEKNIKAL MALAYSIA MELAKA

BORANG PENGESAHAN STATUS LAPORAN PROJEK SARJANA MUDA

TAJUK: The influence of bentonite on glass waste filled spent bleaching earth (SBE) composite

SESI PENGAJIAN: 2013/14 Semester 2 Saya NUR LIYANA BINTI MOHD DAUD mengaku membenarkan Laporan PSM ini disimpan di Perpustakaan Universiti Teknikal Malaysia Melaka (UTeM) dengan syarat-syarat kegunaan seperti berikut: 1. Laporan PSM adalah hak milik Universiti Teknikal Malaysia Melaka dan penulis. 2. Perpustakaan Universiti Teknikal Malaysia Melaka dibenarkan membuat salinan

untuk tujuan pengajian sahaja dengan izin penulis. 3. Perpustakaan dibenarkan membuat salinan laporan PSM ini sebagai bahan

pertukaran antara institusi pengajian tinggi. 4. **Sila tandakan ( )

SULIT

TERHAD

TIDAK TERHAD

(Mengandungi maklumat yang berdarjah keselamatan atau kepentingan Malaysia sebagaimana yang termaktub dalam AKTA RAHSIA RASMI 1972) (Mengandungi maklumat TERHAD yang telah ditentukan oleh organisasi/badan di mana penyelidikan dijalankan)

Alamat Tetap: No. 24 Kampung Lembah Jamuan

33600 Kuala Kangsar

Perak Darul Ridzuan Tarikh: 23rd June 2013

Disahkan oleh:

Cop Rasmi: Tarikh: _______________________

** Jika Laporan PSM ini SULIT atau TERHAD, sila lampirkan surat daripada pihak berkuasa/organisasi berkenaan dengan menyatakan sekali sebab dan tempoh laporan PSM ini perlu dikelaskan sebagai SULIT atau TERHAD.

FAKULTI KEJURUTERAAN PEMBUATAN

Tel : +606 331 6019 | Faks : +606 331 6431/6411

Rujukan Kami (Our Ref) : Rujukan Tuan (Your Ref) :

23 Jun 2014 Pustakawan Perpustakaan UTeM Universiti Teknikal Malaysia Melaka Hang Tuah Jaya, 76100 Durian Tunggal, Melaka. Tuan/Puan, PENGKELASAN LAPORAN PSM SEBAGAI SULIT/TERHAD LAPORAN PROJEK SARJANA MUDA KEJURUTERAAN PEMBUATAN (MANUFACTURING PROCESS): NUR LIYANA BINTI MOHD DAUD Sukacita dimaklumkan bahawa Laporan PSM yang tersebut di atas bertajuk “The Influnce of Bentonite on Glass Waste Filled Spent Bleaching Earth (SBE) Composite” mohon dikelaskan sebagai *SULIT / TERHAD untuk tempoh LIMA (5) tahun dari tarikh surat ini. 2. Hal ini adalah kerana IANYA MERUPAKAN PROJEK YANG DITAJA OLEH SYARIKAT LUAR DAN HASIL KAJIANNYA ADALAH SULIT. Sekian dimaklumkan. Terima kasih. Yang benar, ________________ Tandatangan dan Cop Penyelia * Potong yang tidak berkenaan

NOTA: BORANG INI HANYA DIISI JIKA DIKLASIFIKASIKAN SEBAGAI SULIT DAN

TERHAD. JIKA LAPORAN DIKELASKAN SEBAGAI TIDAK TERHAD, MAKA

BORANG INI TIDAK PERLU DISERTAKAN DALAM LAPORAN PSM.

DECLARATION

I hereby declare this report entitled THE INFLUENCE OF BENTONITE ON GLASS

WASTE FILLED SPENT BLEACHING EARTH (SBE) COMPOSITE is the result

of my own research except as cited in the references.

Signature :

Author’s Name : NUR LIYANA BINTI MOHD DAUD

Date : 23rd June 2014

APPROVAL

This report is submitted to the Faculty of Manufacturing Engineering of UTeM as a partial

fulfillment of the requirements for the degree of Bachelor of Manufacturing Engineering

(Engineering Materials) (Hons.). The member of the supervisory is as follows:

...................................................................................

Dr. Zurina Binti Shamsudin

(Project Supervisor)

ABSTRAK

Tujuan utama projek ini adalah untuk menganalisa kesan yang dipengaruhi oleh bentonite

apabila digabungkan bersama lebihan peluntur bumi (SBE). Objektif utama projek ini

adalah untuk mengenalpasti komposisi yang paling sesuai untuk kaca komposit dan untuk

menilai sifat-sifat termo-fizikalnya. Selain itu, objektif lain adalah untuk mengkategorikan

mikrostruktur dan fasa di dalam kaca komposit ini. Kaca komposit digunakan kerana

kobinasi di antara kaca soda kapur (SLG), kaca borosilikat (BSG) bersama sisa semulajadi

(SBE) dan kelebihan kaca ini ada ia sangat bergantung kepada mikrostruktur dan fasanya.

Bahan-bahan yang digunakan dalam projek ini adalah SLG, BSG, SBE dan bentonite yang

mana ia digunakan sebagai pengikat. Nisbah peratus berat untuk SLG dan BSG telah

ditetapkan kepada 65% bagi kombinasi kedua-dua gelas. Serbuk kaca ini telah

disumbangkan oleh Pusat Penyelidikan Mineral (PPM) dalam saiz 75μm dan kemudian

ditapis ke saiz 45μm di UTeM. Nisbah peratus berat bentonite adalah 0wt%, 2wt%, 5wt%,

10wt%, 15wt% dan 20wt%; dibakar pada suhu 750°C dan 850°C dengan kadar pemanasan

2°C/minit. Nisbah lebihan sampel adalah SBE. Sampel telah dibentuk menggunakan

kaedah tekanan kering ekapaksi. Beberapa ujian telah dilakukan seperti ujian fizikal

(pemerhatian mata, ketumpatan dan penyerapan air), ujian mekanikal (kekerasan mikro)

dan ujian mikrostruktur (imbasan mikroskop elektron (SEM), tenaga serakan sinar-x

spektroskopi (EDX) dan pembelauan sinar-x (XRD). Selepas pembakaran,hasil sampel

adalah kasar. Walau bagaimanapun, selepas dikurangkan kandungan peratusan bentonite

kepada 0 dan 2wt%, rupa permukaan telah menjadi lebih baik. 10% kandungan bentonite

mempunyai kekerasan yang paling tinggi sebanyak 230kg/mm², yang mana sangat rendah

dan hanya boleh digunakan untuk kegunaan yang lembut seperti alat hiasan dalaman rumah

dan aksesori wanita. Kesimpulannya gabungan di antara komposisi ini tidak sesuai untuk

digabungkan bersama BSG kerana ia cenderung menyebabkan sampel menjadi lembut.

i

ABSTRACT

The aim of this project is to investigate the influence of bentonite on spent bleaching earth

(SBE) composite. The objectives of this project are to determine the suitable batch for glass

composites and to evaluate the thermo-physical properties. Other than that, the objective of

this project is to characterize the microstructure and the phases on the glass composites.

Glass composites are used due to the combination of soda-lime glass (SLG) and borosilicate

glass (BSG) powders with natural waste spent bleaching earth (SBE) and the specialty of

it, is depending on the microstructure and its phases. The materials used in this project

are SLG, BSG, SBE and bentonite which acting as the filler. The weight percent ratio for

SLG and BSG have been fixed to 65% for the combinations of both glasses. The glass

powders were supplied by Pusat Penyelidikan Mineral (PPM) in 75μm and were further

sieved to 45μm in ceramic laboratory. The bentonite weight percent has been

distinguished to 0wt%, 2wt%, 5wt%, 10wt%, 15wt% and 20wt%; sintered at 750°C and

850°C with the heating rate of 2°C/minute. The rest of the weight percent is SBE. The

samples were pressed using the uniaxial dry pressing method. A few testing have been done

like physical testing (optical observation, density and water absorption), mechanical testing

(microhardness) and microstructure analysis (scanning electron microscope-SEM, energy

dispersive X-ray spectroscopy-EDX and X-ray diffraction-XRD). The samples were rough

after the sintering process. However, after reducing the bentonite weight percent ratio to 0

and 2wt%, the surface appearance has improved. 10% of bentonite have the highest

hardness was 230kg/mm², which is very low and only can be used for simple soft

application like indoor home decoration and jewelry. BSG is not suitable to be mixed in

this composition because it caused the samples to be soft.

ii

DEDICATION

For my supportive family, lecturer, friends, UTeM, Pusat Penyelidikan Mineral, and

especially for my religion, race and country.

iii

ACKNOWLEDGEMENT

Bismillahirrahmanirrahim, in the name of Allah, the most gracious and most merciful. First

of all I would like to thank to Allah for his blessing to complete PSM I and PSM II

successfully. I would like to express my gratitude to those who gave me the possibility to

complete this PSM report. I am also grateful to Dr Zurina Binti Shamsudin for showing me

the road and helped me to get me started on the path to this final year project. Her

enthusiasm, encouragement and faith in me throughout have been extremely helpful. She

was also available for my questions and she was positive and gave generously of her time

and vast knowledge. She always knew where to look for the answers to obstacles while

leading me to the right source, theory and perspective.

A special thanks also goes to Pusat Penyelidikan Mineral (PPM) staff, Mr Khor Peng Siong,

Mr Aminudin Bin Mahmud, Tuan Haji Mohamad Haniza Bin Mahmud, Encik Mohd Idham

Bin Mustaffar, Puan Marlinda, Encik Suaid, Puan Zaidah Binti Sulaiman and other staff

for never get bored answering my curiosity and questions. They were also having given me

some materials like SLG, BSG and Bentonite. Other than that, they were also offered me

to use their facilities but due to time and distance constraints, I could not attend to their

offers.

I would also gratitude my thanks to Faculty of Manufacturing Engineering staff and my

project partners for giving full cooperation to complete this project. Last but not least,

thanks to everyone, especially my family for giving me an endless support to complete this

report.

iv

TABLE OF CONTENT

Abstrak i

Abstract ii

Dedication iii

Acknowledgment iv

Table of content v

List of Tables xi

List of Figures xiii

List of Abbreviations, Symbols and Nomenclatures xv

1. CHAPTER 1 : INTRODUCTION

1.1. Background 1

1.2. Problem Statement 4

1.3. Project Objectives 5

1.4. Scope of Studies 5

1.5. Outline of Thesis 6

1.6. Conclusion 7

2. CHAPTER 2 : LITERATURE REVIEW

2.1. Glass Waste 8

2.1.1. Definition of Glass 8

2.1.2. Definition of Glass Waste 9

2.1.3. Types of Glass 9

2.1.3.1. Soda Lime Glass (SLG) 10

v

a) Chemical Composition 11

b) Characteristics 11

c) Applications 11

2.1.3.2. Borosilicate Glass (BSG) 11

a) Chemical Composition 12

b) Characteristics 12

c) Applications 12

2.1.4. Properties of Glass Waste 12

2.1.4.1. Physical Properties 13

a) Density 13

b) Color 14

c) Dimensional Stability 14

2.1.4.2. Mechanical Properties 16

a) Thermal Properties 17

2.1.4.3. Microstructure and Phases 17

2.2. Natural Waste 18

2.2.1. Definition of Natural Waste 18

2.2.2. Spent Bleaching Earth (SBE) 19

2.2.3. Properties of SBE 20

2.2.4. Studies on SBE 20

2.3. Composites 21

2.3.1. Definition of Composites 21

2.3.2. Types of Composites 23

2.3.3. Properties of Composites 24

2.3.4. Studies on Glass Waste Composites 25

vi

2.4. Filler 25

2.4.1. Definition of Filler 25

2.4.2. Bentonite 25

2.4.3. Bentonite Usage in Composites 29

2.5. Properties Characterization 29

2.5.1. Definition of Properties Characterization 29

2.5.1.1. X-ray Diffraction Testing (XRD) 30

a) Working Mechanism 31

b) Advantages of XRD Testing 31

2.5.1.2. Hardness Vickers Testing (HV) 32

a) Working Mechanism 32

b) Advantages of Vikers Testing 33

2.5.1.3. Scanning Electron Microscopy (SEM) 34

a) Working Mechanism 34

b) Advantages of SEM 35

2.5.2. Density, Water Absorption and Porosity 35

2.6. Conclusion 37

3. CHAPTER 3 : METHODOLOGY

3.1. Scope of Project Work 38

3.2. Powder Preparation 40

3.2.1. Glass Waste Powder (SLG and BSG) 40

3.2.2. Spent Bleaching Earth (SBE) 41

3.2.3. Bentonite Powder 41

3.3. Sample Preparation 42

vii

3.3.1. Batching 42

3.3.1.1. Procedures 43

3.3.2. Sieving 43

3.3.2.1. Procedures 43

3.3.3. Pestle Mortar 44

3.3.3.1. Procedures 44

3.3.4. Mixing 45

3.3.4.1. Procedures 45

3.3.5. Forming 46

3.3.5.1. Procedures 47

3.3.6. Sintering 47

3.3.6.1. Procedures 48

3.3.6.2. Sintering Profile 49

3.4. Materials Characterization 50

3.4.1. Bulk Density, Porosity and Water Absorption 51

3.4.1.1. Procedures for Bulk Density 53

3.4.1.2. Procedures for Water Absorption 54

3.4.2. Hardness 55

3.4.2.1. Procedures 55

3.4.3. X-ray Diffraction (XRD) 56

3.4.3.1. Procedures 56

3.4.4. Scanning Electron Microscopy (SEM) 58

3.4.4.1. Procedures 58

3.5. Conclusion 59

viii

4. CHAPTER 4 : RESULTS AND DISCUSSION

4.1. Results 60

4.1.1. Physical Properties 61

4.1.1.1. Optical Observation 61

4.1.1.2. Density, Porosity and Water Absorption 65

4.1.2. Mechanical Properties 68

4.1.2.1. Microhardness Testing 68

4.1.3. Materials Characterization 70

4.1.3.1. X-ray Diffraction (XRD) 70

4.1.3.2. Scanning Electron Microscopy (SEM) and Energy Dispersive X-ray Spectroscopy (EDX) 71

4.2. Discussion 76

4.2.1. Physical Properties Analysis 76

4.2.1.1. Optical Analysis 76

4.2.1.2. Density, Porosity and Water Absorption Analysis 77

4.2.2. Mechanical Properties Analysis 78

4.2.2.1. Microhardness Analysis 78

4.2.3. Materials Characterization Analysis 79

4.2.3.1. XRD 79

4.2.3.2. SEM and EDX 80

4.3. Conclusion 81

5. CHAPTER 5 : CONCLUSION AND RECOMMENDATION

5.1. Optical Observation 82

5.2. Density, Water Absorption and Porosity 83

ix

5.3. Hardness 83

5.4. XRD 84

5.5. SEM and EDX 84

6. REFERENCES 85

7. APPENDICES

Appendix A

A1 Gantt Chart PSM I (Planned)

A2 Gantt Chart PSM I (Actual)

A3 Gantt Chart PSM II (Planned)

A4 Gantt Chart PSM II (Actual)

Appendix B

B1 Data for XRD Analysis

x

LIST OF TABLES

2.1 The most popular types of glasses. 10

2.2 Properties of BSG (Borosilicate Glass - Properties of Borosilicate Glass

(Pyrex/Duran) by Goodfellow Ceramic & Glass Division.

13

2.3 The density comparison between the compounding with and without SLG. 14

2.4 Mechanical Properties of SLG. 16

2.5 Thermal Properties of SLG. 17

3.1 The chemical composition of SLG and BSG. 40

3.2 The chemical composition of SBE. 41

3.3 The chemical composition of bentonite. 42

3.4 The batches for the project. 42

4.1 The optical observations result for sample C1, C2, B1 and B2. 62

4.2 Optical observations among B1, B2, C1, C2 and D1 samples. 64

4.3 The dry mass (D), suspended mass (S) and saturated mass (M) for samples C1, C2,

B1 and B2. 66

4.4 The porosity, water absorption and bulk density for sample C1, C2, B1 and B2.67

4.5 The hardness result for sample B1, B2, C1 and C2. 69

xi

4.6 SEM results for sample B1, B2, C1 and C2 with the magnifications of 50x, 200x and

500x. 72

4.7 EDX results for the element in sample C1, C2, B1, and B2. 74

xii

LIST OF FIGURES

1.1 Types of materials used in this project a) bentonite powder, b) borosilicate glass (BSG), c) soda-lime glass (SLG) and d) spent bleaching earth (SBE) 3

2.1 Shrinkage glass concrete with normal concrete. Mixture composition glass concrete 15

2.2 Life-cycle chain: extraction — production — consumption — waste. 18

2.3 The unprocessed SBE (wet palm oil dreg). 19

2.4 The tree diagram of composites. 23

2.5 The virtual of matrix and reinforcement. 24

2.6 The Classification of silicates. 28

2.7 The inside of XRD Testing Machine. 30

2.8 Hardness Vickers Testing Machine. 32

2.9 The indenter and indentation of HV machine. 32

2.10 The path of the electrons. 35

2.11 The digital balancer machine used to measure the density. 36

3.1 The scope of works for the project. 39

3.2 The pestle mortar. 44

3.3 The ball mill machine in UTeM laboratory. 45

3.4 The uniaxial die pressing machine in UTeM laboratory. 46

xiii

3.5 Schematic for the paths of surface energy reduction in sintering. Path 1 a) coarsening where small particles combine to form larger-sized particles and Path 2 b) the densification of particles followed by grain growth 48

3.6 Sintering profile at 750°C with 5°C per minute for heating rate. 49

3.7 Place the sample in the machine beam. 57

3.8 An example of XRD towards SLG and BSG glass tiles 57

3.9 SEM showing porosity a)through The thickness of the ceramic and b) on the electrode surface of the ceramic. 58

4.1 XRD results for sample B1, B2, B3, B4, C1 and C2. 71

4.2 SEM analysis for sample C1 with 500x magnification. 73

4.3 The porosity, water absorption and bulk density percentages for sample C1, C2, B1

and B2. 78

4.4 The mean hardness for the sample B1, B2, C1 and C2. 79

xiv

LIST OF ABBREVIATIONS, SYMBOLS AND

NOMENCLATURES

ASTM - American Standard Testing Material

B - Bentonite

BSG - Borosilicate glass

CaO - Calcium Oxide

CaAl2Si2O8 - Anorhite

EDX - Energy Dispersion X-ray Spectroscopy

ISO - International Organization for Standardization

K - Kelvin

KAl2(Si3Al)O10(OH,F)2 - Muscovite

LOI - Loss on ignition

mg - Mili gram

MPa - Mega Pascal

Na2O - Natrium Oxide

NaAlSiO4 - Carnegeite

PPM - Pusat Penyelidikan Mineral

xv

SBE - Spent Bleaching Earth

SEM - Scanning Electron Microscopy

SiO2 - Silicon Oxide, Coesite, Cristobalite

SLG - Soda-lime glass

XRD - X-ray Diffraction

Wt. % - Weight percentage

μm - Micron meter

°C - Degree Celsius

xvi

CHAPTER 1

INTRODUCTION

This chapter explains about the introduction of the product, covering the introduction,

problem statement, objectives, scope and the conclusion. Other than that, the structure of

the full report will be discussed in this chapter.

1.1. Background

Glass waste is unique, beauty and function-ability of glass composites has drawn interest

from many researches and manufacturer due to its special mechanical and physical

properties. It has attracted Stoneville to do research on it based on its uniqueness.

Stoneville is a company that produces products using waste glasses. The products are

usually beautiful, innovative, can be applied in many applications and eco-friendly

properties. Other than that, Stoneville is a well-known company for glass tile production,

which is made of waste glasses (Stoneville, 2012).

1

The aim of this project is to turn the waste into a beneficial product. Waste is used as the

main materials in this project. The purposes of using waste are to be environmentally

friendly and to save the cost of manufacturing a new product. Other than that, the usage

of raw materials such as silica can be reduced slowly.

There are several types of glasses, mainly are Borosilicate glass (BSG) and Soda-Lime

glass (SLG). Borosilicate glass waste comes from jars, glass kettle, mugs, cookware and

many more. Soda-lime comes from drinking glasses, bottles, wares and others. Both the

waste glasses are commonly used in production of tiles, slabs, dental composites cookware

and kitchen appliances. It is used for that application because it has low water absorption

(0.2%), low potential for scratches and can be repaired if scratched. Other than that, the

cost of producing a new glass product by using raw materials are increasing. Furthermore,

the source of raw materials is decreasing (J Dent Res, 1999; Condon, 1991).

Recycled Eco Glass compares favorably with that of other types of materials made of

recycled glass that are cheaper. Other benefits of this material include stain resistance,

hardness and color depth that creates a three dimensional effect (Stoneville, 2012).

The waste term also implied to natural resources. In Malaysia, there are a several types of

natural sources. Some of the natural waste in Malaysia are jute, kenaf, palm oil waste and

others. All the natural waste is safe to be used and not hazardous because it does not

contain any chemical composition (Smith and Sch Affer et al., 1999, pp. 761-763).

A recent study by Huda, 2012 reported that spent bleach earth (SBE) powder has

improved the hardness. However the studies only limited to the hardness measurement

based on the formulation between SBE and glass waste (SLG). Moreover, all

compounding needs a filler or also known as binder to increase and improve the properties

and to give a stronger bonding to the compounding.

2

The most important of the appearance of the ceramic product also need to be highlighted.

It has been reported, that additional filler such as Bentonite has shown an improvement in

the color appearance. Bentonite has been used as a binder in this project. Based on

previous studies by Liyana (2013) on BSG and SLG composite, the ideal addition of

Bentonite is between 5 to 10% of the formulation. If the temperature is too high, the

sample revealed burnt and changed in shape. Less Bentonite adding shows changes color

into more whiter. With the increasing of Bentonite, the color turned to brownish but less

change in shape has been observed.The results have proven that 10% of Bentonite have

improved the mechanical properties. The hardness shows approximately 400 HV and

ultimate tensile strength measured by flexural test approximately 35 MPa. Figure 1.1

shows the type of glass waste and filler.

(a)

(b)

(c)

(d)

Figure 1.1: Type of materials used in this project a) Bentonite powder, b) Borosilicate glass (BSG), c)

Soda-lime glass (SLG) and d) Spent Bleaching Earth (SBE) (Vasundhara Industries, 2011; Cargo

Handbook.Com, 2013).

3