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PERFORMANCE OF EPOXY-BASED SELF-HEALING MORTAR

NUR FARHAYU BINTI ARIFFIN

UNIVERSITI TEKNOLOGI MALAYSIA

i

PERFORMANCE OF EPOXY-BASED SELF-HEALING MORTAR

NUR FARHAYU BINTI ARIFFIN

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

MAY 2016

iii

DEDICATION

Praise be to Allah s.w.t, the Lord of the Worlds

Who says (interpretation of the meaning):

“Give thanks to Me and to your parents. Unto Me is the final destination”

[Quraan, Luqmaan 31:14]

All glory and honor to Him

To my parents

Fadzillah Binti Idris and Ariffin Bin Sulaiman

To my greatest supporters

Nur Farhana, Mohd Syafiq Fauzan, Muhammad Syafiq Sazzuann, Nur Abyan

Nabilah, Alif Dzulfieka and Qaireen Nur Amani

And also to all who supported me by Doa and work. Thanks for everything. May

Allah bless you. Amin

iv

ACKNOWLEDGEMENT

Praise Be To Allah S.W.T, the Lord of the World

First and foremost, I like to express my sincere appreciation and profound

gratitude to my beloved thesis supervisors, Prof. Ir. Dr. Mohd Warid Hussin, Assoc.

Prof. Dr. Abdul Rahman Mohd Sam and Prof. Han Seung Lee, for encouragement,

guidance, critics and friendship. Without their continued support and interest, this

thesis would not have been the same as presented here.

I am thankful to Materials and Structures laboratory, Faculty of Civil

Engineering, Universiti Teknologi Malaysia and Hanyang University of South Korea

for providing the facilities for my research. My thanks also go to technicians and

staffs for their assistance in this research. The financial supports from Universiti

Teknologi Malaysia Research Management Centre, towards the research projects:

03H35 and 03H36, MyBrain15 and Ministry of Education, are appreciated.

Most importantly, I must thank my amazing family for their steadfast support,

love and encouragement. Mom and Dad, I cannot thank you enough for raising me

to be an independent thinker and instilling the traits of ambition and perseverance in

me from a young age. To my siblings, thank you for your constant support, for

always making me laugh, and for reminding me not to take life too seriously. I love

all of you with all my heart, and I am so lucky to call you my family.

My sincere appreciation also extends to all my colleagues and friends who

have provided assistance at various occasions. Your views and tips are useful indeed.

To all of you, thank you for everything.

v

ABSTRACT

Concrete is one of the oldest and versatile construction materials. After

water, it is the most utilised material in the world. However, due to various reasons,

the formation of micro-cracks can lead to a major problem such as corrosion of steel

reinforcement and further deterioration of the structure. The cost of repairing

deteriorated concrete structures is expensive as effective remedial requires special

repair materials and skilled labours. Thus, the development of new technologies and

material that can automatically repair cracks, consequently restore or even increase

the strength of both mortar and concrete to prolong the service life is highly needed.

Nowadays, the self-healing by using bacteria as a healing agent had gained interest

among researchers. However, limited study had been conducted on the use of

polymer as a healing agent. Thus, the aim of this study is to investigate the effects

and behaviour of epoxy resin without hardener as a self-healing agent in mortar. The

epoxy resin was used without hardener based on the understanding that it can harden

inside the mortar through the reaction between the epoxy resin and hydroxyl ions

produced from the cement hydration process. In this study, the mortar specimens

were prepared with mass ratio of 1:3 (cement: fine aggregates), water-cement ratio of

0.48 and 5% to 20% epoxy resin of cement content. Two types of curing regimes

were used namely dry-curing and wet-dry curing. Normal mortar was also prepared

as a control sample. Various tests were carried out to determine the characteristics of

materials including viscosity, Fourier transform infrared spectroscopy, X-ray

fluorescence and sieve analysis. The performance of the hardened mortar containing

epoxy resin without hardener was determined through compressive strength, flexural

strength, splitting tensile strength, initial surface absorption, water absorption,

apparent porosity, drying shrinkage and strength development. Furthermore, various

techniques including X-ray diffraction, scanning electron microscopy and

thermogravimetric analysis were used to study the microstructure of the hardened

epoxy-modified mortar. The ultrasonic pulse velocity, permeability, damage degree

and healing efficiency were conducted to determine the crack healing process by the

epoxy resin inside the cracked mortar specimens. The experimental results show that

the optimum percentage of epoxy resin used in the mix was 10% as it gives the

highest engineering properties compare to other percentage. The wet-dry curing

regime was found to give better performance of the sample containing epoxy resin

compared to dry curing. The epoxy resin without hardener as a healing agent was

found to perform effectively as the compressive strength, ultrasonic pulse velocity

and permeability of the cracked mortar samples regain the initial reading with

prolonged curing time. The microstructure study also revealed that the epoxy resin

reacts with the hydroxyl ions to heal the micro-cracks in the mortar specimen.

Overall test results together with microstructure study showed that epoxy resin

without hardener can be used as a self-healing agent in repairing the micro-cracks.

vi

ABSTRAK

Konkrit merupakan bahan binaan tertua dan serba boleh yang paling banyak

digunakan di dunia selepas air. Walau bagaimanapun, disebabkan faktor tertentu,

penghasilan retakan mikro boleh menyebabkan masalah seperti pengaratan tetulang

keluli dan kerosakan kepada struktur. Kos membaikpulih struktur konkrit adalah

mahal kerana kerja-kerja pemulihan memerlukan bahan terpilih dan tenaga kerja

mahir. Oleh itu, teknologi dan bahan yang dapat membaiki retakan secara automatik

dan mampu meningkatkan kekuatan mortar dan konkrit seterusnya memanjangkan

hayat perkhidmatan adalah sangat diperlukan. Pada masa ini, konkrit penyembuhan

automatik dengan menggunakan bakteria sebagai agen penyembuhan telah mendapat

perhatian para penyelidik. Walau bagaimanapun, kajian menggunakan polimer

sebagai agen penyembuhan masih tidak meluas. Oleh itu, tujuan penyelidikan ini

adalah untuk mengkaji kesan dan perlakuan resin epoksi tanpa pengeras sebagai agen

penyembuhan dalam mortar. Resin epoksi yang digunakan adalah tanpa pengeras

berdasarkan pemahaman bahawa ia boleh mengeras di dalam mortar melalui tindak

balas diantara resin epoksi dan ion hidroksil yang terhasil daripada proses

penghidratan simen. Dalam kajian ini spesimen mortar telah disediakan dengan

nisbah 1: 3 (simen: pasir), nisbah air-simen 0.48 dan 5% hingga 20% resin epoksi

daripada kandungan simen. Dua jenis pengawetan digunakan iaitu pengawetan

kering dan pengawetan basah-kering. Mortar biasa disediakan sebagai sampel

kawalan untuk perbandingan. Pelbagai ujian telah dijalankan untuk menentukan ciri-

ciri bahan termasuk ujian kelikatan, Fourier transform infrared spectroscopy, X-ray

Fluorescent dan analisis ayak. Prestasi mortar keras yang mengandungi resin epoksi

tanpa pengeras telah dikaji melalui kekuatan mampatan, kekuatan tegangan,

kekuatan lenturan, penyerapan air dipermukaan, penyerapan air, jumlah keliangan,

pengecutan kering and peningkatan kekuatan. Disamping itu, pelbagai teknik,

termasuk X-ray diffraction, scanning electron microscopy dan ujian

thermogravimetric telah digunakan untuk mengkaji mikrostruktur epoksi mortar.

Halaju denyutan ultrasonik, ketelusan, tahap kerosakkan dan keberkesanan

penyembuhan telah dilakukan untuk menentukan proses penyembuhan retakan oleh

resin epoksi dalam spesimen mortar yang telah diretakkan. Keputusan kajian

menunjukkan peratus optimum resin epoksi yang digunakan adalah 10% kerana ia

memberikan kekuatan mampatan mortar yang tertinggi. Pengawetan kering-basah

didapati telah memberikan prestasi yang lebih baik bagi spesimen yang mengandungi

resin epoksi tanpa pengeras berbanding pengawetan kering. Resin epoksi tanpa

pengeras juga didapati sangat efektif sebagai bahan penyembuh berasaskan kekuatan

mampatan, halaju denyutan ultrasonik dan ketelusan air spesimen mortar yang

diretakkan memberikan bacaan seperti bacaan awal pada jangkamasa pengawetan

yang lama. Kajian mikrostruktur juga menunjukkan resin epoksi bertindak balas

dengan ion hidroksil dan menyembuhkan keretakan mikro dalam spesimen mortar.

Keputusan keseluruhan beserta kajian mikrostruktur menunjukkan resin epoksi tanpa

pengeras boleh digunakan sebagai agen penyembuhan keretakan mikro.

vii

TABLE OF CONTENTS

CHAPTER TITLE PAGE

DECLARATION ii

DEDICATION iii

ACKNOWLEDGEMENT iv

ABSTRACT v

ABSTRAK vi

TABLE OF CONTENTS vii

LIST OF TABLES xiii

LIST OF FIGURES xv

LIST OF ABBREVIATIONS xx

LIST OF SYMBOLS xxi

LIST OF APPENDICES xxii

1 INTRODUCTION 1

1.1 Introduction 1

1.2 Problem Statement 3

1.3 Aim of the Study 5

1.4 Objectives of the Study 5

1.5 Research Question 6

1.6 Scope and Limitation of Study 6

1.7 Significance of Research 8

1.8 Thesis Outline 9

2 LITERATURE REVIEW 11

2.1 Introduction 11

viii

2.2 Problems of the Crack 14

2.3 Types of Repair 17

2.4 Cost Estimating For Structure Repairing 19

2.5 Self-Healing Concrete 22

2.6 Type of Healing Agent 25

2.6.1 Epoxy Resins 26

2.6.2 Cyanoacrylates 28

2.6.3 Alkali–silica Solution 29

2.7 Self-Healing Method 30

2.7.1 Encapsulation 30

2.7.2 Expansive Agent and Mineral Admixtures 32

2.7.3 Bacteria 32

2.8 Limiting Crack Width for Autogenic Self-Healing 35

2.9 Thermosetting Polymer 39

2.10 Polymer in Concrete 42

2.10.1 Epoxy Resin 44

2.10.2 Polymer-modified Concrete 47

2.11 Concluding Remarks 49

3 METHODOLOGY 51

3.1 Introduction 51

3.2 Experimental Programs 51

3.3 Materials 53


3.3.2 Ordinary Portland Cement (OPC) 54

3.3.3 Fine Aggregates 55

3.3.4 Water 55

3.4 Mix Proportion 56

3.5 Mixing Procedure 57

3.6 Curing Conditions 57

3.7 Tests 58

3.7.1 Fresh Properties 59

3.7.1.1 Viscosity Measurement 59

ix

3.7.1.2 Flow Tests 60

3.7.1.3 Setting Time Test 61

3.7.2 Hardened Properties 62

3.7.2.1 Compressive Strength Tests 62

3.7.2.2 Flexural Test 63

3.7.2.3 Splitting Tensile Test 64

3.7.2.4 Initial Surface Absorption Test 64

3.7.2.5 Water Absorption Test 65

3.7.2.6 Apparent Porosity Test 66

3.7.2.7 Drying Shrinkage 67

3.8 Self-Healing Evaluation 68

3.8.1 Test Degree of Hardening 68

3.8.2 Pre-loading 70

3.8.3 Ultrasonic Pulse Velocity 72

3.8.4 Damage Degree of Concrete after Self-Healing 73

3.8.5 Permeability Test 74

3.9 Microstructure tests 75

3.9.1 Fourier Transform Infrared Spectroscopy 75

3.9.2 X-Ray Fluorescence 76

3.9.3 X-Ray Diffraction 77

3.9.4 Scanning Electron Microscopy 78

3.9.5 Thermogravimetric Analysis 79

4 ENGINEERING PROPERTIES OF EPOXY-MODIFIED

MORTAR

81

4.1 Introduction 81

4.2 Properties of Materials 81


4.2.1.1 Viscosity 82

4.2.1.2 Fourier Transformation Infrared

Spectroscopy

83

4.2.2 Cement 85

4.2.2.1 X-Ray Fluorescence 85

x

4.2.2.2 X-Ray Diffraction 86


Spectroscopy

87

4.2.3 Fine aggregates 89

4.2.3.1 Sieve Analysis 89

4.2.3.2 X-Ray Fluorescence 90


Spectroscopy

90

4.3 Effect of Curing Regime 91

4.4 Fresh Properties of Epoxy-Modified Mortar 94

4.4.1 Flow Tests 94

4.4.2 Setting Time Test 94

4.5 Physical Properties of Epoxy-Modified Mortar 96

4.6 Mechanical Properties of Epoxy Modified Mortar 97

4.6.1 Compressive Strength 98

4.6.2 Flexural Test 100

4.6.3 Splitting Tensile Test 101

4.6.4 Relationship between Compressive, Flexural and

Tensile Strengths

103

4.6.5 Scanning Electron Microscopy Morphology 104


4.5.7 Thermogravimetric Analysis 108

4.5.8 Initial Surface Absorption Test 113

4.5.9 Water Absorption Test 114

4.5.10 Apparent Porosity Test 115

4.5.11 Drying Shrinkage 117

4.7 Comparison between Optimum Epoxy-Modified Mortar

and Normal Mortar

119

4.7.1 Strength Development 119

4.7.2 Porosity 120



4.7.5 Fourier Transform Infrared Spectroscopy 125

xi

4.7 Summary 127

5 EVALUATION OF SELF-HEALING EPOXY-MODIFIED

MORTAR

128

5.1 Introduction 128

5.2 Visualization of Crack Formation after Pre-Loading 129

5.2.1 Normal Observation 130

5.2.2 UV-light Observation 131

5.3 Observation of Epoxy Resin without Hardener 132

5.4 Degree of Hardening 134

5.5 Self-Healing Mechanism of Epoxy resin without

hardener

135

5.6 Reaction between Epoxy Resin and Hydroxyl Ion 136

5.7 Self-Healing of Epoxy-Modified Mortar 139

5.7.1 Ultrasonic Pulse velocity 139

5.7.2 Compressive Strength 144

5.7.3 Relationship between Compressive Strength and

Pulse Velocity

149

5.8 Damage Degree of Concrete after Self-Healing 150

5.9 Permeability Test 152

5.10 Microstructure of Self-Healing Epoxy-Modified Mortar 154


5.10.2 X-Ray Diffraction Analysis 159

5.10.3 Fourier Transformation Infrared Spectroscopy 160

5.11 Summary 163

6 CONCLUSIONS AND RECOMMENDATIONS 165

6.1 Introduction 165

6.2 Conclusions 165

6.2.1 Characterize the Properties of Materials 166

6.2.2 Optimum Mix Proportions of Epoxy-Modified

Mortar

166

6.2.3 Engineering Properties of Epoxy-Modified Mortar

xii

without Hardener 166

6.2.4 Self-Healing Mechanism of Epoxy Resin in

Hardened Mortar

167

6.2.5 Performance of Epoxy-Modified Mortar under

Microstructure Tests

168

6.3 Contribution of Presented Research Work 169

6.4 Recommendations for Future Research 170

REFERENCES 171

Appendices A-B 181-186

xiii

LIST OF TABLES

TABLE NO. TITLE PAGE

2.1 The advantages and disadvantages of self-healing agents 37

2.2 Advantages and disadvantages of thermosetting resins (Ray

and Rout, 2005)

41

3.1 Mix proportion of epoxy-modified mortar 56

3.2 The stages in producing the crack in epoxy modified and

normal mortars

71

3.3 Classification of the quality of concrete on the basis of

Pulse velocity (Levitt, 1970)

73

4.1 Properties of Diglycidyl Ether of Bisphenol A-type epoxy

resin

82

4.2 Composition and structure of raw epoxy resin 85

4.3 Chemical composition of cement by XRF analysis 86

4.4 Composition and structure of Portland cement 88

4.5 Chemical composition of fine aggregates 90

4.6 Composition and structure of fine aggregates 91

4.7 Compressive strength of epoxy-modified mortar 92

4.8 Optimum mix proportion of epoxy-modified mortar 99

4.9 Epoxy-modified mortar elements from XRD analysis 108

4.10 Result of thermogravimetric analysis 112

4.11 Percentage of gases decomposition 112

4.12 Comparison of composition and structure of normal and

epoxy-modified mortars

126

5.1 The crack generated to epoxy-modified and normal mortar 129

5.2 Velocity of epoxy and normal mortar after loaded at 28

xiv

days 141


days

141


days

142

5.5 Compressive strength of epoxy and normal mortar after

loaded at 28 days

146


loaded at 180 days

146


loaded at 365 days

147

5.8 Composition and structure of epoxy-modified mortars 162

5.9 Composition and structure of normal mortars 163

xv

LIST OF FIGURES

FIGURE NO. TITLE PAGE

1.1 Research Significant 8

2.1 Process of aggressive solution penetration (Interval,

2015)

12

2.2 Blood clotting in an injured vessel (Porter, 2006) 14

2.3 Cause of cracking (Kumar and Chandana, 2015) 16

2.4 Performance and cost comparison between normal

concrete material and self-healing material (Breugel,

2012)

20

2.5 Main mechanisms of autogenous healing (Tang et al.,

2015)

24

2.6 Hollow tube contains epoxy resin and hardener (Aïssa et

al., 2012)

28

2.7 Basic method of the microcapsule approach (White et al.,

2001)

31

2.8 Optical photomicrograph (1000×magnification) of

bacteria (Jonkers et al. 2010)

34

2.9 Research gap of the study 39

2.10 Classifications of polymer modifiers of cement paste

(Ohama and Ramachandran 1996)

40

2.11 System of classification of concrete-polymer composites 42

2.12 The cross-linking compound of epoxy resin (Zhengl et

al., 1995)

45

2.13 The global markets of epoxy resins (Massingill and

Bauer, 2000)

46

xvi

2.14 The reaction of epoxy resin with hydroxyl ion (Ohama et

al., 1993)

48

2.15 Number of publications per year containing the phrase

“self-healing polymer” (Scheiner et al., 2015)

48

3.1 Experimental Programme 53

3.2 Digital Brookfield Viscometer for epoxy resin viscosity

test

59

3.3 Type of spindle for viscosity test 60

3.4 The flow table and spreaded mortar 61

3.5 Initial surface absorption test equipment 65

3.6 Mechanical extensometer for drying shrinkage

measurement

68

3.7 Testing procedure of degree of hardening 69

3.8 The procedure to generating cracks 70

3.9 Different conditions that may be encountered when

testing an element

72

3.10 The apparatus and equipment for permeability test 74

3.11 (a) Pellet compress machine (b) FTIR analyser 76

3.12 X-Ray Diffraction machine at Hanyang University of

South Korea

77

3.13 Coating machine and the mortar sample after coating 78

3.14 Scanning Electron Microscopy and Energy-dispersive X-

ray machine at Hanyang University of South Korea

79

3.15 Thermogravimetric machine at Hanyang University of

South Korea

80

4.1 Formulation of epoxy resin with cement hydration

(Ohama et al., 1993)

83

4.2 Fourier transformation infrared spectroscopy of epoxy

resin

84

4.3 Scanning Electron Microscopy morphology of cement

hydrates without epoxy resin

86

4.4 X-ray diffraction of Portland cement 87

4.5 Fourier transformation infrared spectroscopy analysis of

xvii

Portland cement 88

4.6 Sieve analysis of fine aggregates 89

4.7 Fourier transformation infrared spectroscopy analysis of

fine aggregates

91

4.8 Relationship between curing condition and percentage of

epoxy in 28 days

92

4.9 Relationship between flow diameter and epoxy content 94

4.10 Relationship between setting time and epoxy content 96

4.11 Average density of epoxy-modified mortar 97

4.12 Compressive strength in wet-dry curing at 28 days 98

4.13 The visual different between 10% and 20% of epoxy-

modified mortar

100

4.14 Flexural strength and epoxy-modified and normal mortar 101

4.15 Relationship between splitting tensile strength and epoxy

content in 28 days curing

102

4.16 Relationship between compressive, flexural and splitting

tensile strengths in 10% epoxy content

103

4.17 Morphology of Scanning Electron Microscopy and

Energy-dispersive X-ray of epoxy-modified mortar

105

4.18 Calcium hydroxide present in 10% epoxy-modified

mortar

106

4.19 X-ray diffraction analysis of epoxy-modified mortar 108

4.20 Thermogravimetric analysis of 5% epoxy content 110




4.24 Initial surface absorption of epoxy-modified mortar and

normal mortar

113

4.25 Relationship between water absorption and epoxy content 114

4.26 Relationship between apparent porosity and epoxy

content

116

4.27 Morphology of pores between (a) 10% epoxy content and

(b) normal mortar

117

xviii

4.28 Relationship between polymer content and drying

shrinkage of epoxy-modified mortars

118

4.29 Strength development after 485 days of curing 120

4.30 Relationship between apparent porosity and strength

development in 360 days

121

4.31 Correlation between apparent porosity and compressive

strength

122

4.32 The morphology of epoxy-modified mortar containing

calcium hydroxide and calcium silicate hydrate gel

123

4.33 Comparison of X-ray diffraction analysis between epoxy-

modified mortar and normal mortar at 365 days

specimens

124

4.34 Fourier transformation infrared spectroscopy for epoxy-

modified mortar and normal mortar

126

5.1 Epoxy-modified mortar before produce crack 130

5.2 Crack generated under 80% of ultimate load of epoxy-

modified mortar

130

5.3 Crack generated in epoxy-modified mortar observe under

UV-light

131

5.4 Unhardened epoxy resin after 28 days curing in epoxy-

modified mortar

131

5.5 Epoxy resin under microscopy observation (Guimard et

al. 2012)

132

5.6 Degree of hardening of epoxy resin 132

5.7 Self-healing mechanism by epoxy resin (Łukowski and

Adamczewski, 2013)

134

5.8 The bonding between hydroxyl ion and epoxy resin 137

5.9 The morphology of self-healing reaction 142

5.10 Velocity of self-healing epoxy-modified and normal

mortars after loaded at 28 days

142


mortars after loaded at 180 days

143


xix

mortars after loaded at 365 days 143

5.13 Compressive strength epoxy and normal mortar after

loaded at 28 days

147

5.14 Compressive strength of self-healing epoxy-modified and

normal mortars after loaded at 180 days

148

5.15 Compressive strength of self-healing epoxy-modified and

normal mortars after loaded at 365 days

148

5.16 Relationship between compressive strength and velocity

of epoxy-modified mortar

149

5.17 Relationship healing rate and velocity of epoxy-modified

mortar

150

5.18 Healing efficiency of epoxy-modified mortar 151

5.19 Relationship between degree of damage and healing

efficiency

152

5.20 Time measurement for water permeability of mortar for

crack produce at 28 days

153

5.21 Scanning Electron Microscopy morphology and Energy-

dispersive X-ray analysis of calcium silicate hydrate in

massive ball shape

155

5.22 Scanning Electron Microscopy morphology of calcium

silicate hydrate in fine granular shape

156


silicate hydrate in Rosette shape

157


silicate hydrate in Fibrous shape

157

5.25 Bonding between epoxy resin without hardener and

calcium hydroxide

158

5.26 X-Ray Diffraction analysis of self-healing epoxy-

modified mortar

159

5.27 Fourier Transform Infrared Spectroscopy analysis of self-

healing epoxy-modified mortar

161

5.28 Fourier Transform Infrared Spectroscopy analysis of

normal mortar

162

xx

LIST OF ABBREVIATIONS

50EM - 50% Epoxy-Modified

50NM - 50% Normal Mortar

80EM - 80% Epoxy-Modified

80NM - 80% Normal Mortar

ASTM - American Society For Testing And Materials

BS - British Standard

CSH - Calcium Silicate Hydrate

C3S - Tricalcium Silicate

C2S - Dicalcium Silicate

C3A - Tricalcium Aluminate

C4AF - Tetracalcium Aluminoferrite

Ca(OH)2 - Calcium Hydroxide

EDX - Energy Dispersive X-Ray

SEM - Scanning Electron Microscopy

ISAT - Initial Surface Absorption Test

TGA - Thermogravmetry Analysis

UPV - Ultrasonic Pulse Velocity

XRD - X-Ray Differaction

XRF - X-Ray Fluorescence

xxi

LIST OF SYMBOLS

σc Compressive strength

σf Flexural strength

σT Splitting tensile strength

P Load

A Area

t Time

L Length

b Width

d Thickness

H Height

D Diameter

3.142

xxii

LIST OF APPENDICES

APPENDIX TITLE PAGE

A List of Publications 181

B Example Calculation of TGA 186

1

CHAPTER 1

INTRODUCTION

1.1 Introduction

Polymer-modified mortar or concrete represents a modification technique or

concept that had been used in order to enhance the properties of normal mortar or

concrete. As in 1923, the first patent of polymer modified mortar and concrete had

been submitted by Cresson. That patent referred to the paving mixture containing

natural rubber latexes as a polymer addition and cement was used as filler. In

following year (1924), Lefebvre patented the first concept of polymer modification

(Ohama, 1998). Since then, the development of polymer modification for cement,

mortar and concrete have been conducted in various countries for almost 70 years or

more. Currently, many effective polymer modification systems for cement mortar

and concrete have been developed and are used in various applications in the

construction industry.

Concrete is a strong and relatively cheap construction material and is

therefore presently the most widely used material in the construction industry. The

main constituent that contributes to concrete strength is Portland cement. It is

estimated that cement (Portland clinker) production alone contributes about 7% of

2

the global carbon dioxide emissions due to the burning of limestone and clay at a

temperature of 1500°C. During this process, calcium carbonate (CaCO3) is

converted to calcium oxide (CaO) and carbon dioxide is released (Worrell et al.,

2001). From an environmental standpoint, concrete does not appear to be a

sustainable material (Gerilla et al., 2007). Moreover, improperly manufactured

concrete may experience shorter service life as it can easily develop cracks due to

excessive loading applied and other environmental causes. A good quality of

concrete is needed which not only prolongs its service life but would also reduce the

production of cement. The main focus in this study is to develop a maintenance-free

self-healing concrete that can curtail the need for cement production as well as

reduce the carbon dioxide gas emissions in the atmosphere.

The major problem of concrete structures is cracking. A cracking of concrete

can cause greater damage such as corrosion of steel reinforcement that can lead to

the collapse of the structure. A number of cracks with different morphology and size

will appear during the construction and the design life of the structure. In various

environmental conditions, including temperature and humidity changes, the

formation and expansion of the cracks will lead to reinforcement corrosion and

reducing the load carrying capacity of the structure (Zhang et al., 2011). The

allowable crack appears to be limited to micro-cracks with width of up to 0.1 to

0.2mm (Li and Yang, 2007).

Small cracks or micro-cracks need to be repaired before they become a major

crack. There are many types of repair materials and methods that can be selected and

used for repairing micro-cracks. However, in certain cases micro-cracks will still

occur in the concrete structure. If the micro-crack cannot be repaired effectively, the

performance of the structure is affected and service life will be shortened. The cost

of repairing concrete is expensive as it requires many raw materials such as cement

and skilled labour. Therefore, the development of new technologies and materials

that can automatically repair cracks and restore/increase the strength of concrete

giving longevity to the structure is essentially needed. Such concrete material will

eventually reduce maintenance costs as well as fulfil the need for sustainability.

3

1.2 Problem Statement

In many concrete structures, tensile forces can lead to cracks and these can

occur relatively soon after the structure is built. Repair of conventional concrete

structures usually involves applying mortar which is bonded to the damaged surface.

Sometimes, the mortar needs to be keyed into the existing structure with metal pins

to ensure that it does not fall off. The bonding property between host concrete and

new repair materials needs to be carefully checked to avoid another problem leading

to extra repair cost. Repairs can be particularly time consuming and expensive; often

it is very difficult to gain access to the structure to make repairs, especially if they are

underground or at a great height.

The occurrence of autogenous healing or self-healing of cracks in concrete

was recognized in a previous study by Reinhardt and Jooss (2003). In their study,

they develop a high-strength concrete and tested on permeability and self-healing

behaviour of cracked concrete. The self-healing performance was checked at the

temperature between 20 °C and 80 °C and crack width between 0.05 and 0.20 mm.

On the other hand, the research of Jonkers and Schlangen (2008) had developed a

microorganism that can heal the cracks automatically. The concrete that can repair

the crack automatically is called self-healing concrete. Self-healing concrete refers

to the ability of concrete to automatically repair the cracks without any external

intervention. This phenomenon has been adapted from the human skin healing

process.

The bacteria used in some studies are known as microorganism that can

survive in alkaline environment of concrete, as long as the air is available. In most

of these studies, an ureolytic bacterium of the genus Bacillus was used as a healing

agent for the biological production of calcium carbonate. The mechanism of calcium

carbonate formation from the bacteria is based on the enzymatic hydrolysis of urea to

ammonia and carbon dioxide (Hager et al., 2010). This reaction causes pH to

increase from neutral to alkaline conditions resulting in the formation of bicarbonate

4

and carbonate ions which precipitate in the presence of calcium ions to form calcium

carbonate minerals (Jonkers et al., 2010). This method proved promising for

repairing cracks in concrete, allowing the concrete to regain strength and decrease

permeability. Many research studies have been conducted using bacteria as a self-

healing agent. Bacteria is a good self-healing agent but the acceptance of using it in

the concrete is been a big issue among contractor. The perceptions of using bacteria

in the concrete become a serious concern due to the bacteria itself that have a

negative effect to human health.

The epoxy resin without hardener is introduced in this study as an additive

material and self-healing agent in the mortar. Epoxy resin has been used as one of

the repair materials to repair concrete for many decades. The use of epoxy resin

which is an external repair process entails the injection of epoxy resin solution

together with a hardener into existing concrete structure cracks. This method is well

known and usually used for concrete structure repair suffering from cracks. Epoxy

resin with different level of viscosity can repair cracks with different widths. Upon

injection, the pressure applied leads the epoxy to flow through the cracks. In

addition to using epoxy resin as a repair material, it can also be used as an additive or

replacement material in concrete mixtures. The main advantage of epoxy resin is its

amazing compressive strength, which can achieve 80 MPa or greater for most

concrete (Kanerva et al., 1991). Usually, the use of epoxy resin with the hardener

has been common practice. The hardener functions as hardening agent to the epoxy

which strengthens the binders in concrete.

However in this study, the epoxy resin is used without hardener based on the

understanding that epoxy resin can harden inside the concrete by reacting with

hydroxyl ion. Hydroxyl ion is produced from cement hydration and reacts with

epoxy resin to heal the cracks. The rationale for not using hardener was to let the

epoxy resin stay in the same state for later when cracks occurred. The unhardened

epoxy resin would then react with the hydroxyl ion to fill up the cracks. Quite

limited studies have been conducted by using epoxy resin without hardener in

concrete mixture and as a healing agent. This reported research focused on the

5

engineering properties and self-healing performance of epoxy resin without hardener

as an additive and self-healing agent as well as the microstructure studies.

1.3 Aim of the Study

The main aim of this research is to investigate the performance of epoxy resin

without hardener as a healing agent in mortar.

1.4 Objectives of the Study

Several objectives can be drawn according to the problem statement. The

objectives are as follow:

i. To characterize the properties of materials use in the study including epoxy

resin, fine aggregates and Portland cement.

ii. To determine the optimum mix proportions of mortar using various epoxy-

cement ratios.

iii. To investigate the engineering properties of self-healing epoxy-modified

mortar.

iv. To investigate the mechanism of self-healing process of epoxy resin in

hardened mortar.

6

v. To evaluate the self-healing performance of epoxy-modified mortar using

microstructure study.

1.5 Research Question

Four major questions needed to be answered from this research:

i. What are the mechanical properties of mortar by using epoxy resin without

hardener?

ii. How epoxy resin without hardener can contribute to the strength of the

mortar?

iii. How does the mechanism of epoxy resin as a self-healing agent work to heal

the cracks?

iv. What is the microstructure morphology of mortar with epoxy resin without

hardener?

1.6 Scope and Limitation of Study

An epoxy resin with high viscosity namely Diglycidyl ether of bisphenol A

type was used. Only one type of polymer was used since this polymer provides high

reactivity even without hardener. The amount of epoxy resin without hardener was

added in the mortar mixture was 5%, 10%, 15% and 20% of cement content in order

to select the best amount of epoxy resin that can corporate as a healing agent inside

7

the mortar specimens. The epoxy resin was added as an addition material in the

mortar mixture so the mortar was categorized as a polymer-modified mortar or in this

research was called epoxy-modified mortar. There are two types of curing regime

applied to the mortar specimens which is dry curing and wet-dry curing. Various

tests were carried out to determine the characteristics of materials including

viscosity, Fourier transform infrared spectroscopy, X-ray fluorescence and sieve

analysis. The performance of the hardened mortar containing epoxy resin without

hardener was determined through compressive strength, flexural strength, splitting

tensile strength, initial surface absorption, water absorption, apparent porosity,

drying shrinkage and strength development. Furthermore, various techniques

including X-ray diffraction, scanning electron microscopy and thermogravimetric

analysis were used to study the microstructure of the hardened epoxy-modified

mortar. The ultrasonic pulse velocity, permeability, damage degree and healing

efficiency were conducted to determine the crack healing process by the epoxy resin

inside the cracked mortar specimens.

The main function of epoxy resin without hardener was to serve as self-

healing agent while producing high mechanical properties. The production of cracks

was generated by 50% and 80% of the ultimate load and was checked by using the

Ultrasonic Pulse Velocity (UPV) together with compressive strength test. the crack

was produced in epoxy-modified self-healing mortar at the age of 28 days, 180 days

and 365 days. The cube specimen of 70 mm × 70 mm × 70 mm size was used for

compressive strength test, 100 mm × 100 mm × 100 mm for self-healing evaluation,

40 mm × 40 mm × 160 mm prism for flexural strength test and cylindrical specimen

of Փ70 mm × 150 mm for splitting tensile test. Normal mortar was cast as a control

specimen and water curing was applied. The tests were conducted based on

American Standard Testing Method (ASTM) standard and British Standard (BS).

Some testing methods such as degree of hardening of epoxy resin were adopted from

previous researchers, since it was not stated in any other established standard.

8

1.7 Significance of Research

The programme of research significant is summarised in the flow chart shown

in Figure 1.1. The significant findings of this study by using epoxy resin without

hardener as a self-healing agent are as followed:

i. Enhance the service life of concrete structure by repairing micro-cracks

automatically before the cracks become worse and as result, the service life of

the concrete/mortar structure will be increase.

ii. Reduce the cost of repairs by self-healing repair phenomenon.

iii. Minimize environmental impact by reducing materials used for repair work

especially the production of cement that produce carbon dioxide gases.

iv. Develop a self-healing agent by using existing materials instead of bacteria.

SELF-HEALING EPOXY-

MODIFIED MORTAR

APPROACH

Addition of epoxy resin (5% – 20%)

PROPERTIES

Mortar strength > 30 MPa

Good performance in repairing cracks

BENEFITS

Reduce maintenance cost

Reduce environmental pollution

Prolong service life

PRODUCT FEATURES

Using epoxy resin without hardener

Automatic cracks repair

AUTOMATIC SELF-HEALING

MORTAR

Figure 1.1 Research Significant

9

1.8 Thesis Outline

Chapter 1 (Introduction): Chapter 1 discusses the background of the research

comprising the statement of problem, research objectives, research scope, the

significance of the research, and limitations of study.

Chapter 2 (Literature Review): Chapter 2 initially discusses the past research

from various researchers all around the world. The main focus is to identify

important performance criteria and test parameters that had been done and compared

with current research. This chapter then discusses the history, studies, science and

different approaches of self-healing performance and evaluation. The differing self-

healing performance evaluation methods are discussed by looking at the different

healing agents that each researcher had reported.

Chapter 3 (Methodology): Chapter 3 focuses on testing method that had been

conducted in order to evaluate the performance of epoxy-modified mortar. The

methodology is separated into three parts: a) fresh properties of epoxy-modified

mortar, b) hardened properties, and c) self-healing evaluation. All the testing

methods and parameters are discussed in this chapter.

Chapter 4 (Engineering Properties of Epoxy-Modified Mortar): Chapter 4

reports and explains the analyses undertaken for achieving the first, second and third

objectives of this research. The results of material properties and engineering

performance of epoxy-resin without hardener are discussed in this chapter. Some

sections from objective 5 based on microstructure morphology are also included.

Chapter 5 (Evaluation of Self-Healing Epoxy-Modified Mortar): Chapter 5

discusses the self-healing performance of epoxy-modified mortar as to achieve the

10

Objectives 4 and 5. The correlation analysis was carried out in order to evaluate an

epoxy resin as a self-healing agent.

Chapter 6 (Conclusions and Recommendations): Chapter 6 concludes the

findings of the overall research work that was undertaken. The contribution and

implications of the findings toward the construction industry in general and

performance evaluation in particular are explained. The limitations and possible

improvements for future undertakings are also discussed. Suggestions for future

research are conveyed in the final part of this chapter.

171

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