Investigation Of Mechanical And Morphological Properties Of Spent Bleach Earth (SBE) Reinforced Glass Waste Composite.

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UNIVERSITI TEKNIKAL MALAYSIA MELAKA

INVESTIGATION OF MECHANICAL AND MORPHOLOGICAL

PROPERTIES OF SPENT BLEACH EARTH (SBE) REINFORCED

GLASS WASTE 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.)

KHAIRIL AZWA BIN KHAIRUL B051110169

921013146153

FACULTY OF MANUFACTURING ENGINEERING 2015

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UNIVERSITI TEKNIKAL MALAYSIA MELAKA

BORANG PENGESAHAN STATUS LAPORAN PROJEK SARJANA MUDA

TAJUK: Investigation of mechanical and morphological properties of spent bleach earth (SBE) reinforced glass waste composite

SESI PENGAJIAN: 2014/15 Semester 2

Saya KHAIRIL AZWA BIN KHAIRUL

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:

22, Jalan TU 31, Taman Tasik Utama, Ayer Keroh, 75450

Melaka

Tarikh: 2nd_{July 2015}

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.

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DECLARATION

I hereby declare this report entitled INVESTIGATION OF MECHANICAL AND MORPHOLOGICAL PROPERTIES OF SPENT BLEACH EARTH (SBE) REINFORCED GLASS WASTE COMPOSITE is the results of my own research except as cited in the references.

Signature :

Author’s Name : KHAIRIL AZWA BIN KHAIRUL Date : 2nd_{July 2015}

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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

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ABSTRAK

Tujuan projek ini adalah untuk mengkaji sifat-sifat mekanikal dan morfologi lebihan peluntur bumi (SBE) bertetulang sisa kaca komposit.SBE adalah satu sisa pepejal yang dihasilkan daripada kilang penapis minyak sawit dan biasanya dilupuskan di tapak pelupusan begitu sahaja. Objektif projek ini adalah untuk menentukan komposisi yang ideal bagi komposit kaca dan untuk mencirikan sifat-sifat mekanikal. Selain itu, objektif projek ini adalah untuk menganalisis hubungan fasa, mikrostruktur dan sifat mekanik komposit kaca. Bahan yang digunakan dalam projek ini adalah kaca soda kapur silikat (SLSG) dan SBE di mana ianya bertindak sebagai matriks dan pengisi masing-masing. Serbuk kaca dihancurkan dan disaring untuk mendapatkan saiz 75 μm. Peratusan berat SBE dalam komposit kaca dibezakan pada 30 wt.%, 35 wt.%, dan 40 wt.%. Sampel dibakar pada suhu 750 ° C dengan kadar pemanasan 2 ° C / minit. Terdapat beberapa ujian yang terlibat dalam projek ini seperti ujian fizikal (pemerhatian fizikal, ketumpatan, keliangan, dan penyerapan air), ujian mekanikal (lenturan dan ujian kekerasan) dan analisis mikrostruktur (imbasan elektron mikroskop-SEM, dan pembelauan sinar X-XRD). Hasil kajian menunjukkan bahawa sampel 30 wt.% SBE mempunyai peratusan penyerapan air dan peratusan keliangan yang lebih rendah daripada sampel 40 wt.% SBE. Selain itu, sampel 30 wt.% SBE menunjukkan kekerasan mikro dan MOR tertinggi iaitu 4.95 GPa dan 23.62 MPa. Kesimpulannya, sampel 30 wt.% SBE mempunyai sifat fizikal yang bagus, di samping sifat mekanikal dan morfologi yang baik.

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ABSTRACT

The aim of this project is to investigate the mechanical and morphological properties of spent bleach earth (SBE) reinforced glass waste composite.SBE is a solid waste generated from the palm oil refinery and usually is being simply disposed off in landfills. The objectives of this project is to determine the ideal composition of the glass composite and to characterize the mechanical properties. Besides that, the objectives is to analyze the correlation of phase, microstructure and mechanical properties of the glass composite. The material used in this project are sod lime silicate glass and SBE in which act as matrix and filler respectively. The glass powder is crush and sieved to get the size of 75 µm. The SBE weight percentage in the glass composite is varied from 30 wt.%, 35 wt.%, and 40 wt.%. The sample is sintered at 750 °C with the heating rate of 2 °C/minute. There were few testing involved in this project such as physical testing (physical observation, density, porosity, and water absorption), mechanical testing (flexural and hardness test) and microstructure analysis (scanning electron microscope-SEM, and X-ray diffraction-XRD). The results showed that 30 wt.% SBE sample has lower water absorption and porosity percentage than 40 wt.% SBE sample. Besides that, 30 wt.% SBE sample shows the highest microhardness and MOR which is 4.95 GPa and 23.62 MPa respectively. In conclusion, the 30 wt.% SBE sample has better physical properties as well as good mechanical and morphological properties than other composition.

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DEDICATION

This report is dedicated to my respective parents; Mr. Khairul Bin Taib and Mrs. Faridah Binti Ahmad, my supervisor; Dr. Zurina Binti Shamsudin, my family’s members and also to all my friends who have been supported and inspired me to do this research study

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ACKNOWLEDGEMENT

Bismillahirrahmanirrahim, in the name of Allah, the most gracious and most merciful. First of all, I would like to extend my gratitude to Allah S.W.T. for His generous blessing and undying strength bestowed upon me during completing this research.

I would also 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 who had given me guidance and support for completing this research.Her enthusiasm, encouragement and faith in me throughout have been extremely helpful

I would also extend my gratitude to the Faculty of Manufacturing Engineering staff and my project partners for giving full cooperation to complete this project. Last but not least, I would thank to everyone, especially my beloved parents and family for giving me an endless support to complete this report.

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TABLE OF CONTENT

Abstrak i

Abstract ii

Dedication iii

Acknowledgement iv

Table of Content v

List of Tables x

List of Figures xi

List of Abbreviations, Symbols and Nomenclatures xiii

1. CHAPTER 1: INTRODUCTION 1

1.1 Background of study 1

1.2 Problem statement 2

1.3 Objectives 3

1.4 Scope of study 3

2. CHAPTER 2: LITERATURE REVIEW 4

2.1 Glass waste 4

2.1.1 Definition of glass 4

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2.1.3 Type of glass 5

2.1.4 Soda lime glass 6

a) Chemical composition 7

b) Characteristics 8

c) Application 8

2.2 Natural waste 8

2.2.1 Definition of natural waste 8

2.2.2 Spent Bleach Earth (SBE) 9

2.2.3 Studies on SBE 9

2.3 Composite 10

2.3.1 Definition of composite 10

2.3.2 Type of composite 10

2.3.3 Ceramic matrix composite 11

2.3.4 Studies on glass waste composite 12

2.4 Sintering 12

2.5 Properties characterization 13

2.5.1 Definition of properties characterization 13

2.5.2 X-ray Diffraction (XRD) 14

a) Working principle 15

2.5.3 Scanning Electron Microscopy (SEM) 15

a) Working principle 16

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vii

a) Working principle 17

2.5.5 Flexural testing 18

a) Working principle 18

2.5.6 Density, Water absorption, and Porosity 19

2.6 Conclusion 20

3. CHAPTER 3: METHODOLOGY 21

3.1 Scope of work 21

3.2 Powder preparation 23

3.2.1 Glass waste powder 23

3.2.2 Spent bleach earth powder 23

3.3 Sample preparation 24

3.3.1 Batching 24

3.3.2 Mixing 24

3.3.3 Forming 25

3.3.4 Sintering 25

3.3.4.1 Sintering profile 26

3.4 Properties characterization 28

3.4.1 Bulk density, porosity, and water absorption 28

3.4.2 Hardness test 30

3.4.3 Flexural test 30

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viii

3.4.5 Scanning electron microscopy (SEM) 32

3.5 Conclusion 33

4. CHAPTER 4: RESULTS AND DISCUSSION 34

4.1 Physical properties analysis 35

4.1.1 Physical observation 35

4.1.2 Porosity, water absorption, and bulk density 36

4.2 Mechanical properties analysis 38

4.2.1 Microhardness testing 38

4.2.2 Flexural testing 39

4.3 Material characterization 41

4.3.1 X-ray diffraction (XRD) 41

4.3.2 Scanning electron microscope (SEM) 42

4.4 Conclusion 44

5. CHAPTER 5: CONCLUSION AND RECOMMENDATION 45

5.1 Conclusion 45

5.2 Recommendation 46

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7. APPENDICES 52

Appendix A

Data for XRD analysis Appendix B

Gantt Chart for Final Year Project (PSM I) Gantt Chart for Final Year Project (PSM II)

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LIST OF TABLES

2.1 Types and uses of the glass 6

2.2 Composition of common commercial soda lime glasses 7

3.1 The batches for the project 24

4.1 Physical observation for sample A, B, and C 35

4.2 The dry mass (D), suspended mass (S) and saturated mass (M) 36 for samples A, B, and C.

4.3 The hardness test results for sample A, B, and C 38

4.4 The modulus of rupture for sample A, B, and C 39

4.5 SEM results for sample A, B, and C with the magnification 43 of 100X and 500X

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LIST OF FIGURES

2.1 Classification of composite based on the shape of filler 11 2.2 XRD pattern for the glass composite material with different 14

bottom slag loading

2.3 SEM micrograph for sample 30%, 40%, 50%, and 60% 16 bottom slag

2.4 Illustration of SEM working principle 17

2.5 The three-point bend test 18

3.1 Flow chart of the experimental work 22

3.2 Sintering profile at 750°C with 2°C per minute for heating rate 26

3.3 Vickers microhardness machine 30

3.4 Schematic figure of sample testing 31

3.5 The rectangular mould of 65 mm x 15 mm x 4 mm 31

3.6 Scanning electron microscope, SEM 33

4.1 Apparent porosity and water absorption percentage for 37 samples A (30 wt.%), B (35 wt.%), and C (40 wt.%)

4.2 Bulk density for samples A (30 wt.%), B (35 wt.%), and 37 C (40 wt.%)

4.3 Vickers microhardness for samples A (30 wt.%), B (35 wt.%), 39 and C (40 wt.%)

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xii

4.4 Modulus of rupture for samples A (30 wt.%), B (35 wt.%), 40 and C (40 wt.%)

4.5 X-ray diffraction results for samples A (30 wt.%), B (35 wt.%), 41 and C (40 wt.%)

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xiii

LIST OF ABBREVIATIONS, SYMBOLS AND

NOMENCLATURES

ASTM - American Standard Testing Material

CaO - Calcium Oxide

GPa - Giga Pascal

MOR - Modulus of rupture

MPa - Mega Pascal

Na2_O _- _{Natrium Oxide}

SBE - Spent Bleach Earth

SEM - Scanning Electron Microscopy

SiO2 _- _{Silicon Oxide, Coesite, Cristobalite}

SLSG - Soda-lime silicate glass

XRD - X-ray Diffraction

Wt. % - Weight percentage

μm - Micron meter

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CHAPTER 1 INTRODUCTION

1.1 Background of study

Waste has been a major environmental issue everywhere since the industrial revolution. The waste need to be managed carefully as it can be harmful to the people. One of the waste management method is recycling. Recycling is the processing of used products to attain materials that can be used to make a new products (Morgan, 2006). For example, the glass waste such as glass food and beverage container can be recycled over and over again. This recycle glass costs less than the raw materials, prolong furnace life and saves energy since it melts at a low temperature (Trzupek, 2010).

Another waste that may also be recycled rather than being exposed is Spent Bleach Earth (SBE). SBE is a solid waste generated from the palm oil refinery and usually is being simply disposed off in landfills. (Loh et al., 2013). The SBE waste can recycled and used as a filler in a ceramic composite material.

In this research, the glass matrix composite material manufactured by a sintering process which uses waste glass as the main raw material is studied. The SBE will act as the filler in the glass composite. The samples will be prepared at different formulation and sintered

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at fixed temperature. The sample will be further analyzed for the material’s properties which consist of mechanical properties with respect to their microstructure.

1.2 Problem statement

Nowadays, solid waste management is an important thing that need to be carried out as the solid waste can give the negative impact to environment. One of the major components of the solid waste is waste glass. Waste glass has become a considerable burden on the landfills throughout the world. Therefore, it is vital to find an ecological alternative to reuse and recycle the waste glass. Besides, the process of turning waste glass into usable products instead of discarding the glass is usually very advantageous.

It has been reported that recycle glass microstructural properties has contribute to the strong improvement of the mortar mechanical performance (Corinaldesi et al., 2005). The improvement on the mechanical properties is attractive for replacing conventional materials.

Recently, SBE performance as the cement replacement in concrete has been studied. It is reported that lower SBE concrete gives better mechanical properties than higher SBE content (Khai, 2010). Tokaman et al (2014) studied on compressive strength of concrete block with addition of SBE. Results showed the compressive strength decreased with increasing cement replacement (Torkaman, et al., 2014). Thus, this research will focus on the flexural strength of the glass waste/ SBE composite.

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1.3 Objectives

The main objective of this research was to study the mechanical properties and morphological properties of the glass waste composite. The study objectives include:

i. To determine the ideal composition of the soda lime silicate glass (SLSG) waste with addition of spent bleach earth (SBE) at a fixed sintering temperature.

ii. To characterize the physical and mechanical properties of the glass composite sample.

iii. To analyze the correlation of phases, microstructure and mechanical properties of the glass composite sample.

1.4 Scope of study

This research is focusing on the thermo-mechanical properties of the glass composite samples. This study started by preparing the glass waste in powder form as the raw material and SBE as the filler. The glass powder was then mixed with the SBE in different compositions. Subsequently, the mixtures were pressed to a pellet and rectangular shape. This compaction is done using an uniaxial pressing method. The next step was sintering the samples in the furnace under specified condition. Finally, the sintered samples were subjected to sample characterization and testing. The physical and mechanical testing is conducted to analyze the properties of the glass composite. The physical analysis includes the size, color and surface roughness of the samples while the mechanical analysis includes the Vickers microhardness test and flexural test. As for the microstructure and phase analysis, scanning electron microscopy (SEM) and X-ray diffraction (XRD) technique will be used.

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CHAPTER 2 LITERATURE REVIEW

This literature review provides an overview of the glass waste and natural waste. It covers the inclusive review on the material properties and their constituent. Furthermore, the characterization methodologies are also included in this literature review. It comprises the scanning electron microscopy (SEM), X-ray diffraction (XRD), flexural test, and Vickers microhardness test and density measurement.

2.1 Glass waste

2.1.1 Definition of glass

Glass is a hard, brittle and usually transparent material. In scientific term, glass refer to any rigid substance that is amorphous, with the exception of plastic and several other substances containing carbon (How Stuff Work, 2009). Glass is solid at room temperature and it is formable at approximately 1000°C. Similarly, it melts at temperatures of between 1400°C and 1650°C (Bvglas.de, 2014).

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In another view, glass is created from natural and abundant raw material of sand, soda ash and limestone. The raw material is melted at very high temperature to form glass. Glass is structurally similar to liquids at high temperature though behave like solid at ambient temperature. This characteristic make glass can be poured, press and molded into various shapes (Glass Alliance Group, 2012).

2.1.2 Definition of glass waste

Glass waste is the glass product that has been discarded or no longer in use. Waste glass disposal come from glass container, flat glass and domestic glass is one of the major environmental challenges. It becomes more challenging as the quantity of waste glass increase and reducing the landfill space capacity (Rashad, A. M., 2014).

Therefore, glass product need to be reused or recycled so that environmental problems can be avoided (Ali, E.E., 2012).

2.1.3 Type of glass

Glass can be differ based on the chemical composition, the processing method or processing behavior. Commonly, glass is classified based on the chemical composition (Bvglas.de, 2014). Table 2.1 show the types and the uses of glass.

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Table 2.1: Types and uses of glass (Siddique, 2008)

2.1.4 Soda-lime glass

Soda lime glass is the most predominant type of glass. It is prepared by melting the raw materials in a glass furnace at temperature up to 1675°C. The raw materials for soda lime glass are soda, lime, silica, alumina and small quantities of fining agents (Jnsglass.com, 2014).

Type of glass Main products

Bottles and jars Tableware

Flat glass Crystal tableware Television screens and display

screen equipment Glass fiber Wool insulation

Ovenware Scientific

Frits Optical Soda lime glass

Lead glasses

Borosilicate glasses

Technical glasses e.g. Alumino-silicate, Alkali-barium

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Technically, soda-lime glass can be divided into glass used for windows and glass for containers which are called float glass or flat glass and container glass respectively. Both types vary in the application, chemical composition and production method (Reade, 2014).

a) Chemical composition

Soda-lime glass typically contains 71 to 75 percent of silicon dioxide (SiO2), 12 to 16 percent sodium oxide (Na2O), 10 to 15 percent calcium oxide (CaO) and small quantities of other substances such as dyes (Bvglas.de, 2014). Table 2.2 shows the typical compositions of commercial soda lime glasses.

Table 2.2: Compositions of common commercial soda lime glasses (Shelby, 2005). Component (wt %) Windows Containers Incandescent Lamps

SiO2 73 74 72

Na2O 14 13 16

K2O - 0.3 1

MgO 4 0.2 4

CaO 9 11 3

Al2O3 0.1 1.5 2

Fe2O3 0.1 0.04 -

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at fixed temperature. The sample will be further analyzed for the material’s properties which consist of mechanical properties with respect to their microstructure.

1.2 Problem statement

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1.3 Objectives

The main objective of this research was to study the mechanical properties and morphological properties of the glass waste composite. The study objectives include:

i. To determine the ideal composition of the soda lime silicate glass (SLSG) waste with addition of spent bleach earth (SBE) at a fixed sintering temperature.

ii. To characterize the physical and mechanical properties of the glass composite sample.

iii. To analyze the correlation of phases, microstructure and mechanical properties of the glass composite sample.

1.4 Scope of study

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CHAPTER 2

LITERATURE REVIEW

2.1 Glass waste

2.1.1 Definition of glass

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2.1.2 Definition of glass waste

Therefore, glass product need to be reused or recycled so that environmental problems can be avoided (Ali, E.E., 2012).

2.1.3 Type of glass

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Table 2.1: Types and uses of glass (Siddique, 2008)

2.1.4 Soda-lime glass

Type of glass Main products

Bottles and jars Tableware

Flat glass Crystal tableware Television screens and display

screen equipment Glass fiber Wool insulation

Ovenware Scientific

Frits Optical Soda lime glass

Lead glasses

Borosilicate glasses

Technical glasses e.g. Alumino-silicate, Alkali-barium

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a) Chemical composition

Table 2.2: Compositions of common commercial soda lime glasses (Shelby, 2005).

Component (wt %) Windows Containers Incandescent Lamps

SiO2 73 74 72

Na2O 14 13 16

K2O - 0.3 1

MgO 4 0.2 4

CaO 9 11 3

Al2O3 0.1 1.5 2

Fe2O3 0.1 0.04 -

Investigation Of Mechanical And Morphological Properties Of Spent Bleach Earth (SBE) Reinforced Glass Waste Composite.

UNIVERSITI TEKNIKAL MALAYSIA MELAKA