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.)

by

KHAIRIL AZWA BIN KHAIRUL

B051110169

921013146153

FACULTY OF MANUFACTURING ENGINEERING

2015

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.

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

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)

i

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.

ii

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.

iii

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

whether direct or indirectly way for completing this project.

iv

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.

v

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

2.1.2 Definition of glass waste 5

vi

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

2.5.4 Vickers Microhardness Testing 17

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

3.4.4 X-ray diffraction (XRD) 32

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

6. REFERENCES 47

ix

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)

x

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

xi

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.%)

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.%)

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

Na2O - 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

°C - Degree Celsius

1

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

2

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.

3

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.

4

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).

5

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.

6

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

7

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 -

SO2 0.2 -