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U DECLARATION OF THESIS / UNDERGRADUATE PROJECT PAPER AND COPYRIGHT Author’s full name : NUR HAFIZAH BINTI ABD KHALID Date of birth : 15 th June 1984 Title : BINDER AND MICRO-FILLER CHARACTERIZATION AND PROPERTIES OF PALM OIL FUEL ASH POLYMER CONCRETE Academic Session : 2015/2016-1 I declare that this thesis is classified as: I acknowledged that Universiti Teknologi Malaysia reserves the right as follows: 1. The thesis is the property of Universiti Teknologi Malaysia. 2. The Library of Universiti Teknologi Malaysia has the right to make copies for the purpose of research only. 3. The Library has the right to make copies of the thesis for academic exchange. Certified by : SIGNATURE SIGNATURE OF SUPERVISOR 840615-01-5316 Professor. Ir. Dr. Mohd Warid Bin Hussin (NEW IC NO./PASSPORT NO.) NAME OF SUPERVISOR Date : 19 th November 2015 Date : 19 th November 2015 NOTES :If the thesis is CONFIDENTAL or RESTRICTED, please attach with the letter from the organization with period and reasons for confidentiality or restriction. UNIVERSITI TEKNOLOGI MALAYSIA CONFIDENTIAL (Contains confidential information under the Official Secret Act 1972)* RESTRICTED (Contains restricted information as specified by the organization where research was done)* OPEN ACCESS I agree that my thesis to be published as online open access (full text) PSZ 19:16 (Pind. 1/07)

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√U

DECLARATION OF THESIS / UNDERGRADUATE PROJECT PAPER AND COPYRIGHT

Author’s full name : NUR HAFIZAH BINTI ABD KHALID

Date of birth : 15th June 1984

Title : BINDER AND MICRO-FILLER CHARACTERIZATION AND PROPERTIES OF PALM OIL FUEL ASH POLYMER CONCRETE

Academic Session : 2015/2016-1

I declare that this thesis is classified as:

I acknowledged that Universiti Teknologi Malaysia reserves the right as follows:

1. The thesis is the property of Universiti Teknologi Malaysia.

2. The Library of Universiti Teknologi Malaysia has the right to make copies for the

purpose of research only.

3. The Library has the right to make copies of the thesis for academic exchange.

Certified by :

SIGNATURE SIGNATURE OF SUPERVISOR

840615-01-5316 Professor. Ir. Dr. Mohd Warid Bin Hussin

(NEW IC NO./PASSPORT NO.) NAME OF SUPERVISOR

Date : 19th November 2015 Date : 19th November 2015

NOTES :If the thesis is CONFIDENTAL or RESTRICTED, please attach with the letter from the

organization with period and reasons for confidentiality or restriction.

UNIVERSITI TEKNOLOGI MALAYSIA

CONFIDENTIAL (Contains confidential information under the

Official Secret Act 1972)*

RESTRICTED (Contains restricted information as specified by

the organization where research was done)*

OPEN ACCESS I agree that my thesis to be published as online

open access (full text)

PSZ 19:16 (Pind. 1/07)

ii

“We hereby declare that we have read this thesis and in our

opinion this thesis is sufficient in terms of scope and quality for the purpose of

awarding the degree of Doctor of Philosophy (Civil Engineering)”

Signature : ........................................................................

Name of Supervisor I : Professor Ir. Dr. Mohd Warid Bin Hussin

Date : 19th November 2015

Signature : .............................................................................

Name of Supervisor II : Professor Dr. Mohammad Bin Ismail

Date : 19th November 2015

Signature : .............................................................................

Name of Supervisor III : Associate Professor Dr. Mohamed A. Ismail

Date : 19th November 2015

BAHAGIAN A – Pengesahan Kerjasama*

Adalah disahkan bahawa projek penyelidikan tesis ini telah dilaksanakan melalui kerjasama

antara ________________________ dengan _________________________

Disahkan oleh:

Tandatangan :………………………………………….. Tarikh: …………

Nama :…………………………………………..

Jawatan :………………………………………….. (Cop rasmi)

* Jika penyediaan tesis/projek melibatkan kerjasama.

BAHAGIAN B – Untuk Kegunaan Pejabat Sekolah Pengajian Siswazah

Tesis ini telah diperiksa dan diakui oleh:

Nama dan Alamat Pemeriksa Luar : _______________________________________

: _______________________________________

Nama dan Alamat Pemeriksa Dalam : _______________________________________

: _______________________________________

Nama dan Alamat Pemeriksa Dalam : _______________________________________

: _______________________________________

Nama Penyelia lain (jika ada) :

Disahkan oleh Timbalan Pendaftar di Sekolah Pengajian Siswazah:

Tandatangan : ……………………………………………………. Tarikh:…………..

Nama : …………………………………………………….

BINDER AND MICRO-FILLER CHARACTERIZATION AND

PROPERTIES OF PALM OIL FUEL ASH POLYMER CONCRETE

NUR HAFIZAH BINTI ABD KHALID

A thesis submitted in fulfilment

of the requirements for the award of the degree of

Doctor of Philosophy (Civil Engineering)

Faculty of Civil Engineering

Universiti Teknologi Malaysia

NOVEMBER 2015

ii

DECLARATION

I declare that this thesis entitled “Binder and Micro-Filler Characterization and

Properties of Palm Oil Fuel Ash Polymer Concrete” is the result of my own research

except as cited in the references. The thesis has not been accepted for any degree

and is not concurrently submitted in candidature of any other degree.

Signature :………………………………….

Name :………………………………..

Date :…………………………………

Nur Hafizah Binti Abd Khalid

19th November 2015

iii

DEDICATION

Alhamdulillah, praise to Allah for giving me the strength and opportunity to

complete this study.

I dedicate this thesis to my beloved husband, Azman Bin Mohamed and my gorgeous

son, Ariff Akhtar Bin Azman for their love and sacrifice.

To my beloved parents and in laws: Abd. Khalid Bin M. Latiff and Rukiah Abd

Rahman, Mohamed Bin Jaffar and Jamilah Bt Sulaiman. Thank you for your prayers

and support, and for always being there for me through happiness and sadness.

To my close friend: Tang Horng Eng, Tengku Elly Malini Tengku Ahmad, Nur

Zulaikha Mohd Bekeri, Nur Farhayu Ariffin and Nor Hasanah Abdul Shukor Lim.

Thanks for always listening, supporting and encouraging me. You are true friends.

Love you all

iv

ACKNOWLEDGEMENT

I would like to thank Allah S.W.T for blessing me with excellent health and ability

during the process of completing my thesis.

Special thanks to my supervisor Professor Ir. Dr. Mohd Warid Hussin (Universiti

Teknologi Malaysia) and co-supervisors Professor Dr. Mohammad Ismail

(Universiti Teknologi Malaysia) and Professor Dr. Mohamed A. Ismail (Hanyang

University, Korea) who have given me the opportunity to learn a great deal of

knowledge, and guiding me towards fulfilling this achievement.

My gratitude is also extended to the “Structures and Materials Laboratory” staff.

Thank you for the support and friendship showered upon me throughout the

experimental periods.

I would like to thank the Ministry of Science, Technology and Innovation (MOSTI),

University Teknologi Malaysia (UTM) as my Research University, and the Research

Management Centre (RMC) for the financial and management support provided

under Research University Grant (RUG); Q.J. 130000.7122.03H35.

Finally, I would like to thank my lovely husband Azman Bin Mohamed for his

unconditional support and assistance in various occasions. All your kindness will

not be forgotten.

v

ABSTRACT

Polymer concrete (PC) is less popular in tropical countries because its common binders such as thermoset resins are very sensitive towards temperature. This problem potentially accelerates the polymerization process until it jeopardizes its early strength development and ultimately produces PC with low workability, high porosity and weaker material bonding. To address this, polymer inhibitor additive of Methyl Methacrylate (MMA) was introduced. Before that, characterization work on binder formulation was done using Nuclear Magnetic Resonance (NMR), X-Ray Diffraction (XRD) and Fourier Transform Infrared Spectroscopy (FTIR). Characterization on fillers was done under microstructure examination to gauge its fineness, thermal behaviour, and morphology. Ground POFA (GPOFA) and calcium carbonate (CaCO3) were categorized as fine micro-filler while unground POFA (UPOFA) and silica sand (Sand) were taken as coarse micro-filler. The blended polymer and PC with optimum mix proportion with low binder (11%, 12%, and 13%) and different micro-filler content (8%, 10%, 12%, 14%, and 16%) was investigated under flowability (worakability) and compression tests. Four types of PC (PC-GPOFA, PC-CaCO3, PC-UPOFA, and PC-Sand) with two polyester binders (Isophthalic and Orthophthalic) were produced to investigate its physical, mechanical and microstructure properties. GPOFA gave excellent flowability and led to high compressive strength at 12% binder content and 14% filler content. PC incorporating fine micro-filler had the best compressive, flexural, splitting tensile strength. Also, with its great dispersal characteristics, denser PC with reduced water absorption and formation of pores was achieved. Isophthalic PC-GPOFA to normal concrete (NC) bond substrate had 57% of improved bonding strength compared to Isophthalic PC-UPOFA to NC bond substrate, tested under slant shear and splitting tensile tests. As a conclusion, POFA is a highly promising filler for PC after being physically modified. This work also aims to assist both researchers and engineers in the field of PC incorporated with agricultural waste as micro-filler, especially in the tropical countries.

vi

ABSTRAK

Konkrit polimer (polymer concrete-PC) adalah kurang popular di negara-negara tropika kerana pengikat biasanya seperti resin termoset adalah sangat sensitif terhadap suhu. Masalah ini boleh mempercepatkan proses pempolimeran sehingga memudaratkan pembentukan kekuatan awal dan akhirnya menghasilkan PC dengan kebolehkerjaan yang rendah, keliangan yang tinggi dan ikatan bahan yang lemah. Keadaan ini boleh ditangani dengan penambahan polimer perencat tambahan daripada metil metakrilat (MMA). Pencirian formulasi pengikat telah dilakukan melalui Nuclear Magnetic Resonance (NMR), X-Ray Diffraction (XRD) dan Fourier Transform Infrared Spectroscopy (FTIR). Pencirian pengisi telah dikaji melalui pemeriksaan mikrostruktur untuk mengetahui kehalusan, tingkah laku haba, dan morfologinya. Ground POFA (GPOFA) dan kalsium karbonat (CaCO3) dianggap sebagai mikro-pengisi halus manakala unground POFA (UPOFA) dan pasir silika (Pasir) dikategorikan sebagai mikro-pengisi kasar. Campuran polimer dengan PC pada kadar campuran yang optimum dengan kandungan pengikat rendah (11%, 12%, dan 13%) dan mikro-pengisi yang berbeza (8%, 10%, 12%, 14%, dan 16%) telah melalui ujian kebolehaliran (kebolehkerjaan) dan mampatan. Empat jenis PC (PC-GPOFA, PC-CaCO3, PC-UPOFA, dan PC-Sand) dengan dua pengikat poliester (Isophthalic dan Orthophthalic) telah dibuat untuk mengkaji sifat fizikal, mekanikal dan mikrostruktur. GPOFA mempunyai kebolehaliran dan kekuatan mampatan yang tinggi pada 12% kandungan pengikat dan 14% kandungan pengisi. Campuran PC dan mikro-pengisi halus mempunyai kekuatan mampatan, lenturan, dan kekuatan tegangan belahan yang terbaik serta struktur yang padat dan kadar penyerapan air dan pembentukan liang yang rendah. Gabungan Isophthalic PC-GPOFA dengan konkrit biasa (NC) mempunyai 57% peningkatan kekuatan ikatan daripada gabungan PC-UPOFA dengan NC semasa diuji di bawah ujian ricih condong dan tegangan belahan. Kesimpulannya, POFA adalah pengisi yang berpotensi untuk PC selepas pengubahsuain fizikal dijalankan. Kerja-kerja ini bertujuan membantu para penyelidik dan jurutera dalam bidang penggabungan PC dengan sisa pertanian sebagai mikro-pengisi, terutamanya di negara-negara tropika.

vii

TABLE OF CONTENT

CHAPTER TITLE PAGE

DECLARATION .............................................................................. ii

DEDICATION ................................................................................. iii

ACKNOWLEDGEMENT .............................................................. iv

ABSTRACT ...................................................................................... v

ABSTRAK ....................................................................................... vi

TABLE OF CONTENT ................................................................. vii

LIST OF TABLES ........................................................................ xiv

LIST OF FIGURES ...................................................................... xix

LIST OF ABBREVIATIONS .................................................. xxviii

LIST OF SYMBOLS .................................................................. xxxi

LIST OF APPENDICES .......................................................... xxxiii

1 INTRODUCTION 1

1.1 Introduction 1

1.2 Background of Study 3

1.3 Background of Problem 4

1.4 Aim and Objectives 6

1.5 Scope of Study 7

1.6 Research Methodology 8

viii

1.7 Significance of Study 10

1.8 Thesis Outlines 10

2 LITERATURE REVIEW 12

2.1 Introduction 12

2.2 Polymer concrete 13

2.2.1 Polymer Binder ....................................................... 13

2.2.2 Polymer Additive .................................................... 15

2.2.2.1 Curing Agent (Catalysts) ........................ 16

2.2.2.2 Curing Agent (Accelerator) .................... 18

2.2.2.3 Inhibitors .................................................. 18

2.2.3 Aggregate and Filler ................................................ 19

2.2.3.1 Aggregate ................................................. 19

2.2.3.2 Filler ......................................................... 20

2.2.3.2.1 Palm Oil Fuel Ash (POFA) ... 24

2.3 Curing Process of Polymer Concrete 28

2.4 Filler in Fresh Blended Polymer 29

2.4.1 Physical Properties ................................................... 30

2.4.2 Filling Ability ........................................................... 31

2.5 Filler in Hardened Polymer 32

2.5.1 Amorphous Solid ..................................................... 33

2.5.2 Morphology Properties ............................................ 34

2.5.3 Tensile Properties .................................................... 36

2.6 Filler in Polymer Concrete 37

2.6.1 Physical Properties .................................................. 38

2.6.1.1 Water Absorption .................................... 38

2.6.1.2 Dense Packing Structure ......................... 39

ix

2.6.2 Mechanical Properties .............................................. 40

2.6.3 Microstructure Properties ......................................... 42

2.6.3.1 Porosity .................................................. 42

2.6.3.2 Morphology Properties .......................... 43

2.7 Application of Polymer Concrete 45

2.7.1 Structural Concrete-to-Concrete Interfaces ............. 46

2.8 Summary of Research Gap 50

3 RESEARCH METHODOLOGY 53

3.1 Introduction 53

3.2 Research Framework 54

3.3 Characterizations of Raw Materials 62

3.3.1 Characterizations of Polymer Binder ....................... 62

3.3.1.1 Viscosity ................................................. 62

3.3.1.2 Working Life ........................................... 64

3.3.1.3 Hardness .................................................. 66

3.3.1.4 X-Ray Diffraction (XRD) ....................... 68

3.3.1.5 Fourier Transform Infrared

Spectroscopy (FTIR) ............................. 69

3.3.1.6 Nuclear Magnetic Resonance (NMR) ... 69

3.3.1.7 Tensile Test ........................................... 70

3.3.2 Characterizations of Micro Filler ............................ 74

3.3.2.1 Apparent Density ................................... 76

3.3.2.2 X-Ray Fluorescence (XRF) ................... 78

3.3.2.3 Particle Size Analyzer (PSA) ................ 79

3.3.2.4 Brunauer/Emmett/Teller Nitrogen

Absorption Test (BET) .......................... 79

3.3.2.5 Morphology ........................................... 80

x

3.3.2.6 Termogravimetric and Differential

Thermal Analysis (TGA and DTA) ....... 81

3.4 Properties of Polymer Concrete Incorporating

Micro-Filler 82

3.4.1 Mix proportion of Polymer Concrete ....................... 82

3.4.2 Mix Proportion of Normal Concrete ........................ 91

3.4.3 Preparation of Polymer Concrete .............................. 92

3.4.4 Post-Curing Regime of Polymer Concrete ............... 95

3.4.5 Desired Mix Proportion of Polymer concrete ........... 95

3.4.5.1 Flowability ............................................. 96

3.4.5.2 Cube Compressive Strength .................. 97

3.4.6 Physical Properties of Polymer Concrete ................. 98

3.4.6.1 Apparent Density ................................... 98

3.4.6.2 Ultrasonic Pulse Velocity (UPV) .......... 98

3.4.6.3 Water Absorption of Polymer Concrete 100

3.4.7 Mechanical Properties of Polymer Concrete ......... 101

3.4.7.1 Cylinder Compressive Strength ........... 101

3.4.7.2 Flexural Strength ................................. 104

3.4.7.3 Splitting Tensile Strength .................... 107

3.4.8 Microstructure Properties ...................................... 108

3.4.8.1 Mercury Intrusion Porosimetry (MIP) 108

3.4.8.2 Morphology ......................................... 111

3.5 Bonding Behaviour of Polymer Concrete to

Normal Concrete Substrate 112

3.5.1 Preparation and Bond Test of Polymer

Concrete to Normal Concrete Substrate............... 113

3.5.1.1 Slant Shear Test ................................... 113

3.5.1.2 Splitting Tensile Test ........................... 116

xi

3.5.2 Mode of Failure .................................................... 117

3.5.3 Mohr-Coulomb Theory ........................................ 119

4 CHARACTERIZATIONS OF RAW MATERIALS OF

POLYMER BINDER AND MICRO-FILLER 122

4.1 Introduction 122

4.2 Characterization of Raw Materials 122

4.2.1 Characterization of Polymer Binder .................... 123

4.2.1.1 Viscosity .............................................. 123

4.2.1.2 Working Life ....................................... 125

4.2.1.3 Hardness .............................................. 127

4.2.1.4 X-Ray Diffraction (XRD) .................... 129

4.2.1.5 Fourier Transform Infrared

Spectroscopy (FTIR) ........................... 130

4.2.1.6 Nuclear Magnetic Resonance (NMR) 131

4.2.1.7 Tensile Properties ................................ 134

4.2.2 Characterizations of Filler .................................... 144

4.2.2.1 Apparent Density ................................. 144

4.2.2.2 Chemical Composition ........................ 145

4.2.2.3 Particle Size Distribution ..................... 147

4.2.2.4 Surface Area ........................................ 148

4.2.2.5 Morphology Image .............................. 149

4.2.2.6 Termo-gravimetric and Differential

Thermal Analysis (TGA and DTA) ..... 150

4.3 Summary 153

4.3.1 Characterization of Polymer Binder .................... 153

4.3.2 Characterizations of Filler .................................... 154

xii

5 PROPERTIES OF POLYMER CONCRETE

INCORPORATING MICRO-FILLER 156

5.1 Introduction 156

5.2 Post-Curing of Polymer Concrete 156

5.3 Optimum Desired Mix Proportion of Polymer concrete 160

5.3.1 Flowability ........................................................... 161

5.3.2 Compressive Strength .......................................... 173

5.4 Properties of Polymer Concrete 185

5.4.1 Physical Properties ............................................... 185

5.4.1.1 Apparent Density ................................. 185

5.4.1.2 Ultrasonic Pulse Velocity (UPV) ........ 195

5.4.1.3 Water Absorption ................................ 201

5.4.2 Mechanical Properties .......................................... 207

5.4.2.1 Compressive Strength .......................... 208

5.4.2.2 Flexural Strength ................................. 217

5.4.2.3 Splitting Tensile Strength .................... 225

5.4.3 Microstructure Properties ..................................... 228

5.4.3.1 Porosity ................................................ 228

5.4.3.2 Morphology Image .............................. 237

5.5 Summary 239

5.5.1 Desired Post-Curing Regime of Polymer

Concrete ............................................................... 239

5.5.2 Optimum Desired Mix Proportion of Polymer

Concrete ............................................................... 239

5.5.3 Properties of Polymer Concrete ........................... 240

xiii

6 BONDING BEHAVIOUR OF POLYMER CONCRETE TO

NORMAL CONCRETE SUBSTRATE 243

6.1 Introduction 243

6.2 Polymer Concrete to Normal Concrete 243

6.2.1 Slant Shear ........................................................... 244

6.2.2 Splitting Tensile ................................................... 248

6.3 Mode of Failure 249

6.4 Mohr-Coulomb Theory 252

6.5 Summary 255

7 CONCLUSIONS AND RECOMENDATIONS 256

7.1 Conclusions 256

7.2 Recommendations 258

REFERENCES ............................................................................. 259

Appendices A-H 269-286

xiv

LIST OF TABLES

TABLE NO. TITLE PAGE

2.1 Properties of Isophthalic and Orthophthalic polyester

resin (Gorninski et al,. 2007)

15

2.2 Common filler used in polymeric system (Roger and

Hancock, 2003; Sung et al., 1997)

22

2.3 Chemical composition and properties of POFA (Awal

and Shehu, 2013)

26

2.4 Summary of curing system 29

2.5 Summary of tensile properties of polymer composites

filled with various type of filler

37

2.6 Water absorption of PC incorporating filler 39

2.7 Effect of filler on mechanical properties of PC 41

2.8 Applications of polymer mortar in Japan (Yoshihiko

Ohama, 1997)

45

2.9 Applications of PC in Japan (Yoshihiko Ohama, 1997) 46

3.1 Type of testing, standard method and number of

specimens

61

3.2 Properties of Isophthalic and Orthophthalic polyester

resin

64

3.3 Grinding mill information. 76

3.4 Mix proportion of PC incorporating GPOFA and

UPOFA

84

3.5 Mix proportion of PC incorporating calcium carbonate

(CaCO3)

85

xv

3.6 Mix proportion of PC incorporating silica sand 86

3.7 Mix proportion of normal concrete 92

4.1 Average, standard deviation (SD), coefficient of

variation (COV) of accuracy and viscosity value of

Isophthalic and Orthophthalic polyester resin

124

4.2 Functional groups of polymer inhibitor 131

4.3 1H NMR and 13C NMR data of metyl methacrylate

(MMA)

134

4.4 Average, standard deviation (SD) and coefficient of

variation (COV) on stress and strain of hardened

Isophthalic based polyester resin cured in room

temperature

140

4.5 Average, standard deviation (SD) and coefficient of

variation (COV) on stress and strain of hardened

Orthophthalic based polyester resin cured in room

temperature

141

4.6 Average, standard deviation (SD) and coefficient of

variation (COV) on stress and strain of hardened

Isophthalic based polyester resin cured in cool

temperature

142

4.7 Average, standard deviation (SD) and coefficient of

variation (COV) on stress and strain of hardened

Orthophthalic based polyester resin cured in control

temperature

143

4.8 Average of Young’s modulus, E of hardened Isophthalic

and Orthophthalic based polymer resin

144

4.9 Apparent density of various filler 145

4.10 Chemical compositions of POFA, calcium carbonate and

silica sand

146

4.11 Comparison on chemical composition of POFA 146

4.12 Fineness of fine and coarse fillers 149

xvi

5.1 Percentage different of flow spread diameter of blended

polymer (with and without filler) at different filler

content

165

5.2 Percentage different of flow spread diameter of blended

polymer (with and without filler) at different filler

content

166

5.3 Percentage different of flow spread diameter of blended

polymer (with and without filler) at different filler

content

167

5.4 Percentage different of flow spread diameter of blended

polymer (with and without filler) at different filler

content

168

5.5 Maximum and minimum values of standard deviation

(SD) and coefficient of variation (COV) for various flow

spread diameter of blended polymer incorporating fine

micro-filler

172

5.6 Maximum and minimum values of standard deviation

(SD) and coefficient of variation (COV) for various flow

spread diameter of blended polymer incorporating

coarse micro-filler

172

5.7 Percentage different of compressive strength, σc of PC

(with and without filler) at different filler content

177

5.8 Percentage different of compressive strength, σc of PC

(with and without filler) at different filler content

178

5.9 Percentage different of compressive strength, σc of PC

(with and without filler) at different filler content

179

5.10 Percentage different of compressive strength, σc of PC

(with and without filler) at different filler content

180

5.11 Maximum and minimum of standard deviation (SD)

and coefficient of variation (COV) for various PC

184

5.12 Maximum and minimum of standard deviation (SD)

and coefficient of variation (COV) for various PC

184

5.13 Average apparent density for overall PC 187

xvii

5.14 Percentage different of average density of PC (with and

without fine filler)

188

5.15 Percentage different of average density of PC (with and

without coarse filler)

189

5.16 Standard deviation (SD) and coefficient of variation

(COV) for various PC

192

5.17 Average, standard deviation and coefficient of variation

of UPV travel time for Isophthalic PC

197

5.18 Average, standard deviation and coefficient of variation

of UPV travel time for Orthophthalic PC

197

5.19 Average, standard deviation and coefficient of variation

on water absorption of Isophthalic PC

205

5.20 Average, standard deviation and coefficient of variation

on water absorption of Orthophthalic PC

205

5.21 Assessment of water absorption of PC 206

5.22 Average, standard deviation (SD) and coefficient of

variation (COV) on stress and strain of Isophthalic PC

213

5.23 Average, standard deviation (SD) and coefficient of

variation (COV) on stress and strain of Orthophthalic

PC

214

5.24 Average cube and cylinder compressive strength of PC 215

5.25 Average Young’s modulus, E of PC 216

5.26 Average Poisson’s ratio of PC 217

5.27 Average, standard deviation (SD) and coefficient of

variation (COV) on load and deflection of Isophthalic

PC

223

5.28 Average, standard deviation (SD) and coefficient of

variation (COV) on load and deflection of Orthophthalic

PC

224

5.29 Average flexural strength of Isophthalic and

Orthophthalic PC

225

xviii

5.30 Average, standard deviation (SD) and coefficient of

variation (COV) on splitting tensile strength of

Isophthalic PC

227

5.31 Average, standard deviation (SD) and coefficient of

variation (COV) on splitting tensile strength of

Orthophthalic PC

227

5.32 Correlation between cumulative pore volume and pore

diameter at primary boundary

232

6.1 Average, standard deviation (SD) and coefficient of

variation (COV) on load and deflection of overall bond

substrate under slant-shear test

247

6.2 Average, standard deviation (SD) and coefficient of

variation (COV) on splitting tensile strength of overall

bond substrate

249

6.3 Summary of desired parameter to be considered and

used in Mohr-Coulomb analysis under slant-shear

results

252

6.4 Summary of desired parameter to be considered and

used in Mohr-Coulomb analysis under splitting tensile

results

252

xix

LIST OF FIGURES

FIGURE NO TITLE PAGE

1.1 Classification of concrete-polymer composites 1

1.2 Research phases 9

2.1 Skeleton of literature review 12

2.2 Polyester polymer chain (Carraher, 2007) 14

2.3 Chemical structure of MEKP (Lim et al., 2009) 17

2.4 Cross linking process of polyester resin by peroxide curing

agent (Lim et al., 2009)

17

2.5 SEM of hardened polyester resin using MEKP (Mahdi et

al., 2009)

17

2.6 Classical bimodal packing effect (Roger and Hancock,

2003)

21

2.7 Some particle shape in common filler(Roger and Hancock,

2003)

24

2.8 Process of producing palm oil fuel ash (a) palm bunch (b)

production of mesocarp during palm extraction process (c)

combustion process of mesocarp (d) palm oil fuel ash

25

2.9 SEM image of POFA particles (a) original size of POFA

particles (b) medium size of POFA particles (c) small size

of POFA particles (1000 times magnifications)

27

2.10 Schematic illustration of the particle structure of occluded

polymer (Roger and Hancock, 2003)

30

xx

2.11 Resin absorption of various fillers; GC: ground calcium

carbonate, FT: fine tailing, KA: kaolin, GF: glass fiber

powder, AH: aluminium hydroxide, MC: mica powder

(Mun et al., 2007)

31

2.12 XRD pattern of hardened polymer resin from recycle PET

plastic waste depolymerized through glycolysis to produce

unsaturated polyester resin (Mahdi et al., 2009)

33

2.13 XRD pattern of hardened polymer mortar (Mahdi et al.,

2009)

34

2.14 SEM images of cryofracture surface of AT/PP composites

(a) and (c) untreated AT/PP composites (b) and (d) treated

AT/PP composites (Zhai et al., 2014)

35

2.15 SEM image of asbestos tailing after thorough grinding

process (Zhai et al., 2014)

35

2.16 Stress-strain behaviour of hardened polymer (Haidar et al.,

2011)

36

2.17 The proposed model for strength of concrete and porosity

(Lian et al. ,2011)

43

2.18 Polymer mortar incorporating different filler (a) ground

calcium carbonate (b) fine tailings (Mun et al., 2007)

44

2.19 (a) Orthophthalic-polyester concrete incorporating 8%

filler content in acetic acid (b) Orthophthalic-polyester

concrete incorporating 8% filler content in sulfuric acid

(Gorninski et al., 2007)

44

2.20 Slant-shear configuration and Mohr circle (Austin et al.,

1999)

48

2.21 Mode of failure (a) adhesive failure (b) cohesive failure

(Saldanha et al., 2013)

49

2.22 Failure envelope using Mohr-Coulomb (Saldanha et al.,

2013)

49

2.23 Schematic of slant-shear test (a) characteristic dimensions

(b) interface stresses (Saldanha et al., 2013)

50

2.24 A novel taxonomy in concrete-polymer composites 51

xxi

3.1 Characterizations on raw materials of polymer binder 55

3.2 Development and properties of raw materials of filler 56

3.3 Development and properties of PC 58

3.4 Properties of PC incorporating micro-filler 59

3.5 Bonding test of PC to NC substrate 60

3.6 Test procedure for viscosity test 63

3.7 Test procedure for working life test 65

3.8 Test procedure for barcol hardness test 67

3.9 Test procedure for XRD test 68

3.10 FTIR machine 69

3.11 NMR machine 70

3.12 Test procedure for tensile test 71

3.13 Homogenize process on unground POFA (UPOFA) 75

3.14 Test procedure for density test of powder materials (filler) 77

3.15 XRF machine 78

3.16 PSA machine 79

3.17 Test procedure for morphology test by using FESEM 80

3.18 Test procedure for TGA and DTA test 81

3.19 Main materials for PC (a) unsaturated polyester resin (b)

coarse aggregate (c) fine aggregate (d) filler

83

3.20 Fine filler: (a) ground POFA (b) calcium carbonate; coarse

filler: (c) unground POFA (d) silica sand

83

3.21 Test procedure of density test of coarse aggregate 87

3.22 Test procedure for density test of fine aggregate 89

3.23 Main materials for normal concrete (a) cement

(b) coarse aggregates (c) fine aggregates (d) water

91

3.24 Step-by-step preparation for PC 93

3.25 Test procedure for flowability test 96

3.26 Test procedure of UPV test 99

3.27 Test procedure for determining density and water

absorption of hardened PC

100

3.28 Test procedure of cylinder compressive strength test 103

3.29 Arrangement of loading of three point loading 105

xxii

3.30 Test procedure of flexural test under three-point loading 106

3.31 Test procedure of splitting tensile test 107

3.32 MIP equipment 109

3.33 Test procedure of MIP test 109

3.34 Miniature of crushed specimen 112

3.35 Dimension of slanted specimen 114

3.36 Step of specimen preparation and testing procedure of

slant-shear test

114

3.37 Step of specimen preparation and testing procedure of

splitting tensile test

116

3.38 Test procedure for observing the failure mode of PC to NC

substrate using close range photogrammetry and particle

imaging velocimetry (PIV) technique

118

3.39 Adhesive failure envelope using Mohr-Coulomb under

combined test of (a) slant shear (b) splitting tensile

121

4.1 Viscosity of Isophthalic and Orthophthalic polyester resin 124

4.2 Effect of inhibitor on working life at ambient room

temperature

126

4.3 Effect of inhibitor on working life at control room

temperature

126

4.4 Barcol hardness at ambient room temperature 128

4.5 Barcol Hardness at control room temperature 128

4.6 XRD pattern of polyester resin with and without inhibitor 129

4.7 Fourier Transform Infrared Spectroscopy spectrum of

polymer inhibitor

130

4.8 1H NMR spectrum of polymer inhibitor 132

4.9 13C NMR spectrum of polymer inhibitor additive 133

4.10 Structure of monomer methyl methacrylate (MMA) 133

4.11 Stress-strain behaviour of Isophthalic based polymer resin

cured in room temperature (a) 0% inhibitor additive

content (b) 0.1% inhibitor additive (c) 0.15% inhibitor

additive (d) 0.2% inhibitor additive

135

xxiii

4.12 Stress-strain behaviour of Isophthalic based polymer resin

cured in control temperature (a) 0% inhibitor additive

content (b) 0.1% inhibitor additive (c) 0.15% inhibitor

additive (d) 0.2% inhibitor additive

136

4.13 Stress-strain behaviour of Isophthalic based polymer resin

cured in room temperature at different inhibitor additive

content

137

4.14 Stress-strain behaviour of Orthophthalic based polymer

resin cured in room temperature at different inhibitor

additive content

137

4.15 Stress-strain behaviour of Isophthalic based polymer resin

cured in control temperature at different inhibitor additive

content

138

4.16 Stress-strain behaviour of Orthophthalic based polymer

resin cured in control temperature at different inhibitor

additive content

138

4.17 Apparent density of various filler 145

4.18 Particle size distribution for different type of fillers 148

4.19 Morphology images of fine micro-filler (a) GPOFA (b)

calcium carbonate; and coarse micro-filler (c) UPOFA (d)

silica sand (1000 times magnifications)

150

4.20 TGA and DTA analysis for POFA 151

4.21 TGA and DTA analysis for calcium carbonate 152

4.22 TGA and DTA analysis for silica sand 152

5.1 Compressive strength of Isophthalic and Orthophthalic PC

at different curing period with curing temperature of 30 oC

157

5.2 Compressive strength of Isophthalic and Orthophthalic PC

for different curing period at curing temperature of 50 oC

158

5.3 Compressive strength of Isophthalic and Orthophthalic PC

for different curing period at curing temperature of 70 oC

159

5.4 FESEM image of Isophthalic PC under 6 hours of curing

period at 50 oC of curing temperature (250 times

magnifications)

159

xxiv

5.5 Flow spread diameter of blended polymer incorporating

12% Isophthalic binder and fine filler at different filler

content

162

5.6 Flow spread diameter of blended polymer incorporating

12% Orthophthalic binder and fine filler at different filler

content

163

5.7 Flow spread diameter of blended polymer incorporating

12% Isophthalic binder and coarse filler at different filler

content

163

5.8 Flow spread diameter of blended polymer incorporating

12% Orthophthalic binder and coarse filler at different

filler content

164

5.9 Flow spread diameter of blended polymer incorporating

various polymer binder content at different filler content

170

5.10 Flow spread diameter of blended polymer incorporating

various polymer binder content at different filler content

171

5.11 Compressive strength of polymer concrete incorporating

12% Isophthalic binder and fine filler content at different

percentage of filler content

174

5.12 Compressive strength of polymer concrete incorporating

12% Orthophthalic binder and fine filler content at

different percentage of filler content

175

5.13 Compressive strength of polymer concrete incorporating

12% Isophthalic binder and coarse filler content at different

percentage of filler content

175

5.14 Compressive strength of polymer concrete incorporating

12% Orthophthalic binder and coarse filler content at

different percentage of filler content

176

5.15 Compressive strength of polymer concrete incorporating

various polymer binder content at different filler content

182

5.16 Compressive strength of polymer concrete incorporating

various polymer binder content at different filler content

183

xxv

5.17 Average density of PC incorporating fine micro-filler (a)

PC-GPOFA

186

5.18 Average density of PC incorporating fine micro-filler (a)

PC-GPOFA

187

5.19 Density of PC incorporating fine micro -filler (a) Iso-

GPOFA (b) Ortho-GPOFA (c) Iso-CaCO3 (d) Ortho-

CaCO3

190

5.20 Density of PC incorporating coarse micro-filler (a) Iso-

UPOFA (b) Ortho-UPOFA (c) Iso-Sand (d) Ortho-Sand

191

5.21 Effect on filler on compressive strength and apparent

density of PC (a) Iso-GPOFA (b) Iso-CaCO3 (c) Iso-

UPOFA (d) Iso-Sand

193

5.22 Effect of filler on between compressive strength and

porosity of PC (a) Ortho-GPOFA (b) Ortho-CaCO3 (c)

Ortho-UPOFA (d) Ortho-Sand

194

5.23 UPV travel time of Isophthalic PC at different filler content 196

5.24 UPV travel time of Orthophthalic PC at different filler

content

196

5.25 Effect of filler on compressive strength and UPV travel

time of PC (a) Iso-GPOFA (b) Iso-CaCO3 (c) Iso-UPOFA

(d) Iso-Sand

199

5.26 Effect of filler on compressive strength and UPV travel

time of PC (a) Ortho-GPOFA (b) Ortho-CaCO3 (c) Ortho-

UPOFA (d) Ortho-Sand

200

5.27 Correlation between compressive strength and UPV travel

time of PC

201

5.28 Effect of filler on compressive strength and water

absorption of PC (a) Iso-GPOFA (b) Iso-CaCO3 (c) Iso-

UPOFA (d) Iso-Sand

203

5.29 Effect of filler on compressive strength and water

absorption of PC (a) Ortho-GPOFA (b) Ortho-CaCO3 (c)

Ortho-UPOFA (d) Ortho-Sand

204

xxvi

5.30 Correlation between compressive strength and water

absorption of PCs

206

5.31 Correlation between UPV travel time and water absorption

of PCs

207

5.32 Stress-strain curve for Isophthalic PC (a) Iso-GPOFA (b)

Iso- CaCO3 (c) Iso-UPOFA (d) Iso-Sand

209

5.33 Stress-strain curve for Orthophthalic PC (a) Ortho-GPOFA

(b) Ortho-CaCO3 (c) Ortho-UPOFA (d) Ortho-Sand

210

5.34 Average stress-strain curve of Isophthalic PC 211

5.35 Average stress-strain curve of Orthophthalic PC 211

5.36 Load-deflection for Isophthalic PC (a) Iso-GPOFA

(b) Iso- CaCO3 (c) Iso-UPOFA (d) Iso-Sand

219

5.37 Load-deflection for Orthophthalic PC (a) Ortho-GPOFA

(b) Ortho-CaCO3 (c) Ortho-UPOFA (d) Ortho-Sand

220

5.38 Load-deflection curve of Isophthalic PC 221

5.39 Load-deflection curve of Orthophthalic PC 221

5.40 Splitting tensile strength of Isophthalic PC 226

5.41 Splitting tensile strength of Orthophthalic PC 226

5.42 Incremental pore volume versus normal-log pore diameter

distribution (a)PC-GPOFA (b) PC-CaCO3 (c) PC-UPOFA

(d) PC-Sand

229

5.43 Cumulative pore volume-pore diameter behaviour; primary

and secondary boundary

230

5.44 Cumulative pore volume-pore diameter behaviour (a) PC-

GPOFA (b) PC-CaCO3 (c) PC-UPOFA (d) PC-Sand

231

5.45 Average pore diameter at different filler content 233

5.46 Total porosity at different filler content. 234

5.47 Effect of filler content on compressive strength and

porosity of PC (a) Iso-GPOFA (b) Iso-CaCO3 (c) Iso-

UPOFA (d) Iso-Sand

235

5.48 Correlation between compressive strength and total

porosity

236

xxvii

5.49 Correlation between porosity and water absorption of PC

incorporating filler

237

5.50 PC incorporating fine micro-filler (a) PC-GPOFA (b) PC-

CaCO3 PC with coarse filler (c) PC-UPOFA (d) PC-Sand.

238

6.1 Load-deflection behaviour of PC to NC bond substrate

under uniaxial loading (a) NC-PC GPOFA (b) NC-PC

CaCO3 (c) NC-PC UPOFA (d) NC-PC Sand

245

6.2 Load-deflection behaviour of PC to NC bond substrate

under uniaxial loading

246

6.3 Splitting tensile strength of PC to NC bond substrate under

splitting tensile loading

248

6.4 Adhesive failure of PC to NC bond substrate under slant-

shear test

250

6.5 Vector image of PIV analysis for overall bond substrate (a)

PC GPOFA-NC (b) PC CaCO3-NC (c) PC UPOFA-NC (d)

PC Sand-NC

251

6.6 Adhesive bond failure envelope using Mohr-Coulomb

theory (a)PC GPOFA-NC (b) PC CaCO3-NC (c) PC

UPOFA-NC (d) PC Sand-NC

254

xxviii

LIST OF ABBREVIATIONS

13C - Carbon-13 NMR

1D - One dimension 1H - Proton NMR

AH - Aluminium hydroxide

Al 2O3 - Aluminium oxide

ASTM - American society for testing and materials

AT/PP - Asbestos tailings filler content

BET - Brunauer/Emmett/Teller nitrogen absorption test

BFLA-5-8-1L - Type of strain gauge for hardened polymer

BS - British standard

BS-EN - Eurocode Standard

CaCO3 - Calcium carbonate

CaO - Calcium oxide

CDCl3 - Deuteratedchloroform

CoNp - Cobalt naphthenate

CoOc - Octoate

COV - Coefficient of variation

Fe2O3 - Ferric oxide

FESEM - Field emission scanning electron microscopy

FT - Fine tailing

FTIR - Fourier transform infrared

GC - Ground calcium carbonate

GF - Glass fiber

GPOFA - Ground POFA

xxix

Iso-CT - Isophthalic polyester resin cured at control temperature

Iso-RT - Isophthalic polyester resin cured at room temperature

JIS - Japanese industrial standard

K2O - Potassium oxide

KA - Kaolin

LOI - Loss on Ignition

LVDT - Linear variable differential transformer

MC - Mica

MEKP - Methyl ethyl ketone peroxide

MgO - Magnesium oxide

MIP - Mercury intrusion porosimetry

MMA - Methyl methacrylate

Na2O - Sodium oxide

NC - Normal concrete

NMR - Nuclear magnetic resonance

Ortho-CT - Orthophthalic polyester resin cured at control temperature

Ortho-RT - Orthohthalic polyester resin cured at room temperature

P2O5 - Phosphorus pentoxide

PC - Polymer concrete

PC CaCO3-NC - Polymer concrete incorporating calcium carbonate substrate to

normal concrete substrate

PC GPOFA-NC - Polymer concrete incorporating ground POFA substrate to

normal concrete substrate

PC Sand-NC - Polymer concrete incorporating silica sand substrate to normal

concrete substrate

PC UPOFA-NC - Polymer concrete incorporating unground POFA substrate to

normal concrete substrate

PET - Polyethylene terephthalate

PIV - Particle imaging velocimetry

PL 60-1L - Type of concrete strain gauge

POFA - Palm oil fuel ash

PSA - Particle size analyzer

RH - Relative humidity

xxx

RHA - Rice husk ash

SD - Standard deviation

SEM - Scanning electron microscopy

SiO2 - Silica dioxide

SO3 - Sulfur trioxide

TDS-303 - Brand of data logger

TGA and DTA - Termogravimetric and differential thermal analysis

TMS - Tetra methyl silane

UP - Unsaturated polyester

UPOFA - Unground POFA

UPV - Ultrasonic pulse velocity

XRD - X-ray diffraction

XRF - X-ray fluorescence

δC - NMR carbon signal

δH - NMR proton signal

xxxi

LIST OF SYMBOLS

ρ - Density of material

A - Cross section’s area of the specimen

Ac - Compression area

Aci - Shear area

At - Tension area

Ati - Shear area

D - Diameter of the specimen

Ec - Compression Young’s modulus of concrete

Et - Tensile Young’s modulus

ET - Young’s modulus in bending

F - Maximum load

F/A - Load divided to area (stress)

Fc - Compression maximum load

fc - Concrete compressive strength

Fci - Shear compression load

fci - Interface compressive strength

fct - Flexural strength

ft - Splitting tensile strength

ft - Concrete tensile strength

Ft / Fti - Tension maximum load

fti - Interface tensile strength

L - Length of specimen/distance between the supporting roller

M - Slope of the tangent to the initial -straight-line portion from the load-

deflection

P - Load

xxxii

V - Volume of mould

W - Weight of material

ΔL/Lo - Different of length divided to total of length/Strain

ε - Strain

εL - Longitudinal strain

εT - Transverse strain

ν - Poisson’s ratio

σt - Tensile stress

τ/ τo - Pure shear strength

xxxiii

LIST OF APPENDICES

APPENDIX TITLE PAGE

A STRESS-STRAIN BEHAVIOUR UNDER TENSION

LOAD

269

B FLOWSPREAD DIAMATER OF BLENDED POLYMER 273

C COMPRESSIVE STRENGTH OF POLYMER

CONCRETE

277

D SUMMARY PROPERTIES OF ISOPHTHALIC AND

ORTHOPHTHALIC POLYESTER RESIN

281

E SUMMARY PROPERTIES OF FINE AND COARSE

MICRO-FILLERS

282

F SUMMARY PROPERTIES OF PHYSICAL,

MECHANICAL AND MICROSTRUCTURE OF PC

283

G SUMMARY BONDING PROPERTIES OF PC TO NC

BOND SUBSTRATE

284

H LIST OF PUBLICATIONS 285

1

CHAPTER 1

INTRODUCTION

1.1 Introduction

Generally, concrete-polymer composites is a concrete that contains polymers.

Development of concrete-polymer composites such as polymer-modified concrete,

polymer concrete, and polymer-impregnated concrete aims to produce high-

performing and multifunctional construction materials. Figure 1.1 shows the

classification of disciplines in concrete-polymer composites.

Figure 1.1 Classification of concrete-polymer composites

2

Polymer-modified concretes are composites materials which have two solid

phases - the aggregates that are discontinuously dispersed through the materials and

the binders in which itself contains a cementitious phase and a polymer phase

(Gemert, 2007). The polymer added acts as polymeric admixtures/modifier in

normal concrete, and this is also called a ‘polymer modified cementitious system’

(Shaw, 1985). There are commercially available polymeric admixtures/modifiers in

Japan which can be classified into polymer dispersions, redispersible polymer

powder, water-soluble polymers, and liquid polymers (Ohama, 2007). On the other

hand, the term ‘polymer-impregnated concrete’ coined by Bhutta et al. (2013) refers

to concrete produced by impregnating or infiltrating the hardened conventional

concrete with a liquid monomer and subsequently completing the polymerizing of

monomer in-situ. The usage of polymer-impregnated concrete has been identified in

precast products, though in limited application, primarily for improving the water

proofing ability and durability of concrete structure (Ohama, 2007).

The only non-cementitious concrete-polymer composites are polymer

concrete. Polymer concrete (PC) is produced by polymerizing (hardening) dry

aggregate and monomers (binder) after the addition of additive, catalysts, and

accelerator. The fresh PC are then cured totally without water and cement binder

(Ohama, 2007). Its composition depends on its intended application.

PC has unlimited potential applications in the construction industry. It can be

used to fabricate box culverts, hazardous waste containers, trench lines, floor drains,

and for the repair and overlaying of damaged concrete surface (bridge and

pavements). However, some improvement and modification have to be made to

enhance the properties of PC. For this reason, many researchers have conducted

numerous studies to develop intelligent materials that can be incorporated into PC,

mainly by introducing fillers into the PC mixture.

3

In Japan, the concrete-polymer composites are used as sustainable

construction materials, and have been continuously improved since the early 1920s

(Ohama, 1997). Its application in the Japan construction industry is common,

popular, and dominant during the 1950s to 1970s (Ohama, 1997; Shaw, 1985). Other

than Japan, the United States, United Kingdom, Russia and Germany have also

published their standardization works of concrete-polymer composites with,

sometimes, stark differences in the content. In Malaysia, the use of concrete-polymer

composites is still not popular. This also applies to research on PC because polymers

are very sensitive to hot temperature and Malaysia is a tropical country. As such, the

lack of knowledge among local fabricators and engineers has become a constraint for

the production of PC.

1.2 Background of Study

The development of new composite materials possessing enhanced strength

and durability as compared to conventional materials is crucial in the construction

industry. Ever since terms like ‘sustainability’ and ‘green materials’ have jumped

onto the bandwagon, it has sparked the interest of experts from various fields to

develop sustainable composite materials to become superior construction materials.

In this study, only polyester resin was employed as binders. Since this

polymer binder is temperature sensitive, polymer inhibitor additive was introduced

into the binder formulation to initiate the intended modification. It was expected that

this would give rise to lower yet sufficient binder concentration for PC.

4

This study used palm oil fuel ash (POFA) from agricultural waste, which

were added into concrete mix with low binder concentration as fillers. POFA was

opted as the filler under scrutiny since it could be easily found in Malaysia. POFA, a

by-product from palm oil mills, is mostly disposed as agricultural waste in landfills.

Its reutilization has the potential to create sustainable and productive materials.

Another reason that POFA had been chosen was because of its attested efficiency in

PC as fillers. Meanwhile, this study also involved low cost thermosetting polyester

resin as binder. The performance of PC incorporated with POFA filler was evaluated

from an engineering perspective. Currently, there are no published findings and data

for such PC in Malaysia incorporating agricultural waste. This study had conducted

extensive experiments to develop and encourage innovative usage of such

sustainable and intelligent material in the construction industry.

1.3 Background of Problem

In PC, thermoset polymer resin is used as the binder. Thermoset resins that

are commercially available include epoxy, vinyl ester, and unsaturated polyester

resin. These are typical resins used in the construction industry because of their

higher strength and stiffness than thermoplastic polymers. However, epoxy and

vinyl ester resins are more expensive than polyester resins. Thus, most researchers

often choose unsaturated polyester resin, even though it is very sensitive towards

temperature. Generally, high temperature can accelerate the polymerization process,

resulting in PC which fails to achieve its early strength and causing other problems

such as poor workability; high porosity and honeycomb; and less material bonding.

This can be solved by casting the PC in a cool room, but this is not cost effective

since the production cost has to be competitive enough to price the PC in Malaysia at

a reasonable value. Therefore, polymer modification should be considered to solve

the aforementioned problem by prolonging the working life and giving sufficient

time for PC production in ambient temperature.

5

Agricultural waste like palm oil fuel ash (POFA) disposed on open fields can

negatively impact our environment. It pollutes the surroundings and is increasingly

demanding for more landfill areas to cater its escalating disposal. This can be

disastrous if left unattended and handled properly at the early stage. Therefore, it is

crucial that a study is performed to put forth an alternative solution to this problem.

This study was therefore conducted to serve this purpose by introducing the

reutilization of POFA as fillers in PC. This new product can become a cost-effective

material since PC products manufactured without fillers are expensive.

Nevertheless, not all waste ashes have the potential to become PC filler. The wrong

selection of filler material may lead to worsened PC quality. Not only that, it affects

the PC’s workability and process ability (Bignozzi et al., 2000). The most abundant

natural waste from agricultural plant is the cellulose (Raveendran et al., 1996;

Kaddami et al., 2006), which has a structure that attracts liquid into the PC. This can

lead to excessive resin consumption, which is not cost effective and jeopardizes the

production of PC even when filler is used.

On the other hand, air voids entrained or entrapped in hardened PC during the

mixing and placing of fresh PC can significantly influence the permeability of the

hardened PC. These air voids can be easily identified as visible pores on the

hardened concrete. An increasing number of pores can reduce the strength of the PC

(Rashid and Mansur, 2009), but the development of air voids can be potentially

lessened by using appropriate micro-filler.

Incompatibility between PC and concrete substrate is the most critical

problem; failure can occur due to poor interaction between these two materials. In

most cases, this happens due to the difference in concrete properties. Nevertheless, it

should be emphasized that, in order to improve the interaction between two different

materials, proper bonding techniques to be considered as well.

6

Incorporating agricultural waste of palm oil fuel ash into PC promises a high

possibility in producing a type of filler that is able to overcome the aforementioned

challenges. However, some modifications on the raw materials including the filler

are needed to improve their characteristics and enhance their engineering properties.

This research can be a novelty research especially in Malaysia and others tropical

countries.

There are two main research questions in this study:

i. Can polymer concrete be produced and perform well in tropical countries?

ii. Can agricultural waste be incorporated in polymer concrete as micro-filler?

1.4 Aim and Objectives

This study aims at developing polymer concrete incorporating agricultural

waste of palm oil fuel ash as micro-filler. Five objectives were formulated to achieve

the aim of the study, they are:

i. To characterize binder formulation using polymer inhibitor additive with

respect to its physical, mechanical and chemical properties.

ii. To investigate the filler characteristics of palm oil fuel ash under

microstructural examination.

iii. To determine the optimum desired mix proportion of various polymer

concrete incorporating micro-filler with low binder content under workability

and compressive strength.

iv. To investigate the physical, mechanical and microstructure properties of

polymer concrete incorporating micro-filler.

v. To evaluate bonding behaviour of polymer concrete to normal concrete

substrate

7

1.5 Scope of Study

The scope of this study was established to achieve the objectives

abovementioned and focused mainly on experimental works. The testing methods

and work procedures were specified according to the British Standard (BS),

Eurocode Standard (BS-EN), American Society for Testing and Materials (ASTM),

and other recommended test procedures proposed by previous researchers. Some

testing methods and work procedures related to PC were specified according to the

Japanese Industrial Standard (JIS) since concrete polymer materials had long been

adopted in Japan.

PC is produced by replacing all cement hydrate binders of conventional

mortar or concrete with polymer binders, without cement and water. The major

component is the thermosetting polyester resins. In this study, only Isophthalic and

Orthophthalic polyester resin were involved as binders. The chemical addition was

limited to 0.5% cobalt naphthenate (CoNp) and 1% Methyl ethyl ketone peroxide

(MEKP) to produce the intended binder formulation. However, different percentage

of inhibitor additive of Methyl Methacrylate (MMA) was added to have sufficient

working time in producing the PC. The effects of the inhibitor additive in the binder

formulation were investigated from the fresh concrete’s working life, strength, and

chemical reaction. Low binder content of 11%, 12% and 13% were employed to

produce high strength PC. To get consistent outcomes, the PC specimens were cast

in room temperature with the relative humidity around 68 ± 2%. After that, all

specimens were post-cured. Control specimens had been produced where no filler

was incorporated.

POFA was used to replace silica sand and calcium carbonate in conventional

filled-PC. The filler and its size were limited to those passing through the sieve sizes

of 300 µm to 45 µm. POFA was physically modified to obtain the particles passing

through 45 µm sieve size. Inert granular materials such as coarse and fine aggregates

were utilized as well and this was similar to conventional concrete. To obtain a

8

uniform mix and strength of PC, the size of coarse and fine aggregates were also

limited to those retained at 10 mm and passing 5 mm sieves, respectively. All fillers

and inert granular materials were oven-dried and the moisture content was

maintained at below 0.5%.

The characteristic of POFA as fillers in PC was examined to determine its

performance from an engineering perspective after the suitable mix design and mix

proportion had been produced. Silica sand and calcium carbonate were also included

as filler to allow comparisons to be made with POFA. Two types of POFA was

employed; ground and unground POFA. In this study, ground and unground POFA

was paired with calcium carbonate and silica sand, respectively. The assessment on

the engineering properties of PC with optimum mix design and mix proportion was

done because it was an important factor in developing the potentially valuable

construction material. The research proceeded with bonding test and covered

investigation on bonding behaviour of PC to normal concrete (NC) substrate.

Therefore, this study provides knowledge on the engineering properties and bonding

behaviour of PC incorporating POFA as micro-filler.

1.6 Research Methodology

This sub-chapter briefly presents the research sequences and method used in

this study. The details explanation on research methodology is discussed in Chapter

3. Three phases had been designed to achieve the research aim and objectives, as

shown in Figure 1.2. Phase 1 addresses the characterizations of raw materials of

polymer binder and filler. Phase 2 addresses the properties of PC incorporating

micro-filler. Meanwhile, the last phase focuses on bonding behaviour of PC.

9

Characterizations of Raw Material:

Binder modification (Objective 1)Filler determination (Objective 2)

Properties of Polymer Concrete Incorporating Micro-Filler:

Optimum mix design and mix proportion (Objective 3)Engineering properties of materials (Objective 4)

Bonding Testing:

Bonding behaviour (Objective 5)

Phase 2

Phase 3

Phase 1

Figure 1.2 Research phases

Phase 1: Characterizations of raw materials of polymer binder and micro-filler The experimental works for binder modification and micro-filler examination were

included at this stage to achieve objective 1 and objective 2.

Phase 2: Properties of polymer concrete (PC) incorporating micro-filler

Comprehensive experimental works were done on identifying the desired optimum

mix proportion of PC and also the corresponding engineering properties. This phase

was carried out to achieve objective 3 and objective 4.

Phase 3: Bonding behaviour of Polymer Concrete to Normal Concrete Substrate

Last phase encompassed testing on the bonding between PC and NC substrate. This

last phase was executed to achieve objective 5.

10

1.7 Significance of Study

The significant findings of this research will be beneficial in the following

ways:

i. Facilitate in promoting environmental awareness through revival of local

natural resources and agricultural waste with less intensive emission of

carbon dioxide.

ii. Encourage production of PC under tropical temperature and its usage among

Malaysian fabricators and contractors.

iii. Aid in providing novelty database of concrete polymer composites and its

application in the construction industry.

iv. Assist fabricators and engineers in improving the quality of materials and

providing an established database for design works in the future.

v. Assist in developing value-added products from local resources to promote

green materials in the construction industry.

vi. Facilitate the introduction of intelligent materials with proven performance to

contractors

vii. Provide significant market value where the final product can be

commercialized as a novelty in Malaysia.

1.8 Thesis Outlines

This research is presented in seven chapters to achieve the research aim and

five objectives. This thesis has been structured to present the research in such

arrangement:

11

Chapter 1 : Introduction

Chapter 2 : Literature Review

Chapter 3 : Research Methodology

Chapter 4 : Characterizations of Raw Materials of Polymer Binder and Micro-

Filler

Chapter 5 : Properties of Polymer Concrete Incorporating Micro-Filler

Chapter 6 : Bonding Behaviour of Polymer Concrete to Normal Concrete Substrate

Chapter 7 : Conclusions and Recommendations