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PERFORMANCE OF TERNARY BLENDED CEMENT MORTAR CONTAINING
PALM OIL FUEL ASH AND METAKAOLIN
JAMILU USMAN
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
SEPTEMBER 2015
Dedicated to
my family
ACKNOWLEDGEMENTS
I wish to express my sincere appreciation to my main thesis supervisor.
Associate Professor Dr. Abdul Rahman Bin Mohd. Sam, for motivations, guidance,
critics and full academic support. 1 am also very appreciative to my co-supervisor,
Dr. Yahya Bin Mohammad Yatim, for his diligent advices and encouragements.
Without their continued support and interest, this thesis would not have been the
same as presented here.
I am greatly indebted to Universiti Teknologi Malaysia (UTM) for given me
this golden opportunity to pursue Ph.D., most especially; School o f Graduate Studies,
Faculty of Civil Engineering, Department of Materials and Structure, Sultanah
Zanariah Library and Technicians-Structural and Materials laboratory UTM.
I gratefully acknowledge the support for this research from Ahmadu Bello
University Zaria (ABU) Nigeria and TETFUND. Finally, 1 am grateful to all my
family members.
V
ABSTRACT
The partial substitution of Portland cement with pozzolans in concrete greatly reduces the environmental pollution due to CO2 emission during cement production. Pozzolans equally enhance mechanical properties and guarantee the production of concrete with minimum costs. These added benefits, result in the increasing use of pozzolans as a significant innovation in the construction industry. Although palm oil fuel ash (POFA) as pozzolan improves strength and durability of concrete, it however delays early strength development due to its low pozzolanicity. Conversely, metakaolin (MK) improves early strength development but equally reduces workability and increases heat of hydration which can be detrimental to the durability of concrete. MK is also deficient in magnesium sulfate environment and at high temperatures. Thus, the scope of application of the binary blends of POFA and MK in the construction industry may be limited. However, the simultaneous use of these materials in the form of ternary blend has the potential to compensate for the deficiencies due to their synergistic interactions. Hence, this study was set out to investigate the effects of the combination of POFA and MK on the properties of cement mortar. Accordingly, a total of 17 different mortar mixtures of binary and ternary blends of POFA and MK at up to 30% replacement levels by weight, and water to binder ratio of 0.55 were used. An optimal ternary blend in terms of strength development and porosity reduction was selected for further detailed investigation. The properties of the optimal ternary assessed at its fresh state include; consistency, setting times, workability and temperature rise. While at its hardened state, compressive strength, sorptivity and microstructures were evaluated. The durability was studied in terms of resistance to sulfuric acid attack, sulfates attack and at high temperatures. The properties of the binders were also examined and their conformity to the relevant standards was confirmed. The results showed that the optimal ternary blend was 10% POFA and 10% MK. The ternary blend significantly improved the workability of mortar with minimal use of superplasticizer compared to MK binary blend. It was also discovered that while the MK binary blend increased the semi- adiabatic temperature by 7% compared to plain OPC, the ternary blend showed a reduction by 4%. Besides, the ternary blend was not only effective in offsetting the low compressive strength of POFA binary at early ages but also enhanced the longterm strength compared to MK, and POFA binary. The TGA and XRD data proved that the early strength improvement of the ternary blend was due to the high pozzolanicity of MK. Furthermore, the ternary blend exhibited superior performance over the MK binary blend and plain OPC in terms of resistance to magnesium sulphate attack and at high temperatures. Generally, the optimal ternary blend of OPC, MK and POFA showed better performance and can be used in construction particularly where the binary blends of either POFA or MK proved deficient. The combined use of POFA and MK would contribute not only to the development of environmental friendly material but also the reduction of CO2 emission.
vi
ABSTRAK
Penggantian sebahagian simen Portland dengan bahan pozolana dalam konkrit dapat mengurangkan masalah pencemaran alam sekitar disebabkan oleh pembebasan CO2 semasa pengeluaran simen. Pozolana juga meningkatkan sifat mekanikal dan menjamin pengeluaran konkrit dengan kos yang minima. Kelebihan ini meningkatkan penggunaan pozolana sebagai satu inovasi dalam industri pembinaan Walaupun abu kelapa sawit (POFA) sebagai bahan pozolana meningkatkan kekuatan dan ketahanlasakan konkrit bagaimanapun perkembangan kekuatan awal adalah kurang disebabkan rendah sifat pozolananya. Sebaliknya Metakolin (MK.) meningkatkan perkembangan kekuatan awal tetapi mengurangkan kebolehkerjaan dan meningkatkan haba penghidratan yang boleh menimbulkan masalah ketahanlasakan konkrit. MK juga tidak tahan kepada persekitaran bermagnesium sulfat dan pada suhu yang tinggi. Oleh itu skop penggunaan adunan penduaan POFA dan MK di dalam industri pembinaan adalah terhad. Walau bagaimana pun, penggunaan bersama bahan ini secara sinergi dalam adunan pertigaan mempunyai potensi mengatasi kelemahan-kelemahan tersebut. Oleh yang demikian kajian ini dijalankan untuk mengkaji kesan gabungan POFA dan MK terhadap sifat simen motar. Sebanyak 17 jenis campuran adunan penduaan dan pertigaan POFA dan MK yang berbeza dengan penggantian sehingga 30% mengikut berat dan nisbah air-simen 0.55 telah dibuat. Campuran yang optima adunan pertigaan berpandukan peningkatan kekuatan dan pengurangan keporosan telah dipilih untuk kajian selanjutnya. Sifat campuran optima simen motar semasa basah dikaji dari aspek konsistensi, masa set, kebolehkerjaan dan peningkatan suhu. Sementara dalam keadaan keras, kekuatan mampatan, tahap serapan dan mikrostruktur adunan diuji. Ketahanlasakan diuji terhadap rintangan asid sulfurik, serangan sulfat dan pada suhu tinggi. Ciri-ciri pelekat juga dikaji dan pematuhannya kepada piawaian yang berkaitan dibuktikan. Keputusan menunjukkan campuran pertigaan optima adalah 10% POFA dan 10% MK. Aduan pertigaan didapati meningkatkan kebolehkerjaan mortar dengan penggunaan superpemplastik yang sedikit berbanding adunan penduaan MK. Kajian menunjukkan adunan penduaan MK meningkatkan suhu separuh adiabatik sebanyak 7% berbanding campuran simen (OPC) manakala adunan pertigaan menunjukkan pengurangan sebanyak 4%. Selain daripada itu, adunan pertigaan bukan sahaja mengatasi masalah kekuatan awal yang rendah bagi adunan penduaan POFA tetapi meningkatkan kekuatan jangka panjang berbanding adunan penduaan MK dan POFA. Data TGA dan XRD membuktikan peningkatan kekuatan awal adunan pertigaan disebabkan oleh sifat pozolana MK. Tambahan pula adunan pertigaan memperlihatkan prestasi yang lebih baik berbanding adunan penduaan dan campuran OPC terhadap serangan sulfat dan suhu yang tinggi. Secara keseluruhan adunan pertigaan yang optima OPC, MK dan POFA menunjukkan prestasi yang lebih baik dan boleh digunakan dalam pembinaan terutamanya bagi mengatasi kelemahan adunan penduaan MK dan POFA. Kombinasi POFA dan MK bukan sahaja dapat membangunkan bahan yang mesra alam sekitar tetapi juga dapat mengurangkan kadar pembebasan CO2.
TABLE OF CONTENTS
CHAPTER TITLE PAGE
DECLARATION ii
DEDICATION iii
ACKNOWLEDGEMENT iv
ABSTRACT v
ABSTRAK vi
TABLE OF CONTENTS vii
LIST OF TABLES xvi
LIST OF FIGURES xviii
LIST OF SYMBOLS xxiv
LIST OF ABBREVIATIONS xxvi
LIST OF APPENDICES xxviii
INTRODUCTION 1
1.1 Background to the Study 1
1.2 Research Problem 3
1.3 Aim and Objectives 4
1.4 Scope of the Study 5
1.5 Significance of the Study 6
I
viii
1.6 Thesis Organization 7
2 LITERATURE REVIEW 9
2.1 Introduction 9
2.2 Description of Binders 10
2.2.1 Portland Cement 10
2.2.2 Metakaolin 11
2.2.3 Palm Oil Fuel Ash 13
2.3 Hydration and Reaction Characteristics of Cement
and Pozzolans 15
2.3.1 Portland Cement 15
2.3.2 Metakaolin 17
2.3.3 Palm Oil Fuel Ash 19
2.4 Fresh and Hardened Properties of Binary
Blended Concrete 20
2.4.1 Fresh Properties 20
2.4.2 Heat of Hydration 22
2.4.3 Strength Development 24
2.5 Durability Properties of Binary Blended Concrete 27
2.5.1 Porosity 28
2.5.2 Sorptivity 30
2.5.3 Resistance to Sulphuric Acid Attack 32
2.5.3.1 Effect of Metakaolin 33
2.5.3.2 Effect of Palm Oil Fuel Ash 34
2.5.4 Resistance to Sulphate Attack 35
2.5.4.1 Effect of Metakaolin 37
2 5.4.2 Effect of Palm Oil Fuel Ash 38
IX
2.5.5 Resi stance to El evated Temperature 40
2.5.5. lEffect o f Metakaolin 41
2.5.5.2 Effect of Palm Oil Fuel Ash 41
2.6 Fresh and Hardened Properties of Ternary Concrete 42
2.6.1 Fresh Properties 42
2.6.2 Heat of Hydration 43
2.6.3 Strength Development 44
2.7 Durability of Ternary Concrete 49
2.7.1 Sorptivity 50
2.7.2 Resistance to Chemical Attack 54
2.7.3 Resi stance to El evated Tem peratures 5 7
2.8 Summary of Literature Review 58
3 RESEARCH METHODOLOGY 61
3.1 Introduction 61
3.2 Experimental Programme 61
3.3 Materials 63
3.3.1 Binders 63
3.3.2 Fine Aggregate 63
3.3.3 Water 64
3.3.4 Chemical Admixture 64
3.4 Preparation of Binders 64
3.4.1 Production of Palm Oil Fuel Ash 64
3.4.2 Production of Metakaolin 66
3.4.2. IThermogravimetric and Differential
Thermal Analysis (TG/DTA) 67
3.4.2 2 Calcination of Kaolin 68
X
3.4.2 3 X-Ray Diffraction (XRD) and Fourier
Transformed Infrared (FTIR) 68
3.4.2.4 Pozzolanicity 68
3.5 Characterization of Material 69
3.5.1 Physical Properties 69
3.5.1.1 Specific Gravity and Loss on Ignition 69
3.5.1.2 Particle Size Distribution 69
3.5.1.3 Specific Surface Area 70
3.5.2 Chemical Compositions 70
3.5.3 Mineralogical Compositions and
Morphological Features of Binders 71
3.5.3.1 X-Ray Diffraction (XRD) 71
3.5.3 2 Fourier Transformed Infrared (FTIR) 72
3.5.3 3 Field Emission Scanning Electron
Microscopy (FESEM) 73
3.5.5 Pozzolanic Activity 73
3.5.5.1 Strength Activity Index 73
3.5.5 2 The Modified Chappelle’s Test 74
3.5.6 Characterization of Fine Aggregate 75
3.6 Mix Proportions of Mortar 75
3.7 Preparation of Specimens 77
3.7.1 Mixing 77
3.7.2 Casting and Curing 78
3.8 Testing: Fresh Properties 80
3.8.1 Consistency 80
3.8.2 Setting Times 81
3.8.3 Temperature Rise during Hydration 82
xi
3.9 Testing: Hardened Properties 83
3.9.1 Compressive Strength 83
3.9.2 Flexural Strength 84
3.9.3 Porosity 84
3.9.4 Sorptivity 85
3.10 Testing: Durability 87
3.10.1 Sulphate Resistance 87
3.10.2 Acid Resistance 88
3.10.3 Elevated Temperature Endurance 89
3.11 Microstructures 90
3.11.1 X-Ray Diffraction (XRD) 91
3.11.2 Fourier Transformed Infrared (FTIR) Analysis 91
3.11.3 Thermogravimetry Analysis (TGA) 93
3.11.4 Field Emission Scanning Electron Microscopy
(FESEM) 94
4 MATERIAL CHARACTERIZATION AND
PROPERTIES OF POFA AND METAKAOLIN
BLENDED MIX 95
4.1 Introduction 95
4.2 Optimization of Calcination Temperature and Time
for Converting Kaolin to Metakaolin 96
4.2.1 Differential and Thermogravimetry Analysis 96
4.2.2 X-Ray Diffraction 97
4.2.3 Fourier Transformed Infrared Analysis 98
4.2.4 Strength Activity Index 100
4.2.5 Chappelles Test Results 101
xii
4.3 Characterization of Material 102
4.3.1 Chemical Compositions of Binders 102
4.3.2 Fineness: Particle Size Distribution of
Binders 103
4.3.3 Particle Morphologies of Binders 104
4.3.4 Specific Gravity and Surface Area 105
4.3.5 Mineral Compositions of Binders 106
4.3.6 Pozzolanicity 108
4.3.7 Particle Size Distribution and Other Physical
Properties of Fine Aggregate 108
4.4 Properti es of B1 ended M ortars 109
4.4.1 Flow/ Workability of Mortar 110
4.4.2 Compressive Strength of Mortar 111
4.4.3 Flexural Strength of Mortar 113
4.4.4 Porosity of Mortar 115
4.4.5 Compressive Strength-Porosity Relationship 116
4.5 Summary of Results 117
5 FRESH AND HARDENED PROPERTIES AND
MICROSTRUCTURE OF POFA AND
METAKAOLIN BLENEDED MORTARS 119
5.1 Introduction 119
5.2 Fresh Properties 119
5.2.1 Consistency of Plain and Blended Pastes 120
5.2.2 Setting Times of Plain and Blended Pastes 121
5.2.3 Mortar Flow/Workability 122
5.2.4 Hydration Temperature Rise 124
5.3 Hardened Properties o f Mortars 125
5.3.1 Compressive Strength 126
5.3.2 Relative Compressive Strength 128
5.3.3 Sorptivities of Mortars 131
5.3.4 Relationship between Compressive Strength
and Sorptivity 132
5.4 Microstructures of Blended Mortars 132
5.4.1 Thermogravimetry Analysis 134
5.4.1.1 Calcium Hydroxide Content 135
5.4.1.2 Calcium Hydroxide Depletion 138
5.4.2 X-Ray Diffraction 141
5.5 Summary of Results 144
6 DURABILITY OF POFA AND METAKAOLIN
BLENDED MORTARS 146
6.1 Introduction 146
6.2 Effect of Elevated Temperatures 146
6.2.1 Residual Compressive Strength 147
6.2.2 Ultra Pulse Velocity 149
6.2.3 X-Ray Diffraction Analysis 151
6.2.4 Fourier Transformed Analysis 154
6.2.5 Field Emission Scanning Electron
Microscopy 157
6.3 Sulphuric Acid Resistance 159
6.3.1 Compressive Strength Loss 159
6.3.2 Residual Mass 161
6.3.3 Relationship between Residual Compressive
xiv
Strength and Residual Mass 162
6.3.4 X-Ray Diffraction Analysis 164
6.3.5 Fourier Transformed Infrared Analysis 165
6.4 Sulphate Resistance 167
6.4 .1 Compressive Strength of Mortars Exposed to
MgSO-t and Na2SO.| Solutions 167
6.4.2 Expansion of Mortars Exposed to MgSC>4
and Na2SO.t Solutions 170
6.4.3 X-Ray Diffraction 173
6.4.4 Fourier Transformed Infrared Analysis 176
6.5 Summary of Results 178
7 CONCLUSIONS AND RECOMMENDATIONS 180
7.1 Introduction 180
7.2 Conclusions 180
7.2.1 On Characterization of Metakaolin and
POFA 181
7.2.2 On Optimum Replacement level of
Ternary Mix 181
7.2.3 On Fresh Properties of Optimized
Ternary Mortar 182
7.2.4 On Hardened Properties of Optimized
Ternary Mortar 182
7.2.5 On Durability of Optimized Ternary
Mortar 183
7.3 Recommendations for Further Investigations 184
REFERENCES
Appendices A-C
186
204-209
x v
xvi
LIST OF TABLES
TABLE NO. TITLE PAGE
2.1 Typical oxide compositions of metakaolin 12
2.1 Requirements of metakaolin as pozzolan (ASTM C 618) 12
2.3 Oxide compositions of palm oil fuel ash found within
literature 14
2.4 Physical properties of Portland cement and palm oil fuel ash 15
2.5 Effect of POFA on workability and setting times of concrete 22
2.6 Pore volume and % of pores of paste containing metakaolin 30
2.7 Sorptivity of bagasse ash concrete 32
2.8 Consistency and setting times of binary and ternary cement
paste 43
2.9 Mix composition in weight (%) of blended cements 48
2.10 Test results for RCPT, sorptivity and water permeability 52
2.11 The dry mix compositions of blended cement 58
2.12 Summary of researches extracted from literature on ternary
blends of pozzolanic materials other than that of
POFA and MK 60
3.1 Mix proportions used for optimization (first stage) 76
3.2 Mix proportions used at second stage 77
3.3 Specimens cast for optimization (first stage) per mix 79
3.4 Specimens cast for testing at the second stage per mix 79
3.5 Wave number of functional groups 92
xvii
4.1 Summary of IR Bands of Kaolin and calcined kaolin 100
4.2 Chemical compositions of binders 103
4.3 Specific gravity and surface area of binders 106
4.4 Pozzolanicity of POFA and metakaolin 108
4.5 Physical properties of fine aggregate 109
5.1 Flow and superplasticizer (sp) content o f the mixes 123
5.2 Tim e-temperature history of mixes 125
5.3 Compressive strengths of blended mortars at different
water binder ratio and curing ages 127
5.4 Calcium hydroxide content of mortars 137
5.5 Calcium hydroxide depleted at different water binder ratio 140
6 .1 Quality of concrete as a function of UPV 149
6.2 Residual compressive strengths of mortar after exposure to
sulphate 170
6.3 Expansion of mortars after being exposed to sulphate 173
xviii
LIST OF FIGURES
FIGURE NO. TITLE PAGE
2.1 Heat evolution of concrete mixed with ground POFA 24
2.2 The effect of metakaolin on the compressive strength
at various ages 26
2.3 Relative strength of HSGC with different ultrafine
POFA content 27
2.4 Porosity of HSGC with different ultrafine POFA content 30
2.5 Weight loss for mortar immersed in 2.5% H2SO4 33
2.6 Weight loss for mortar immersed in 1% HC1 34
2.7 Reduction of compressive strength in 2% sulphuric acid 34
2.8 Effect of solution concentration and metakaolin
Replacement levels on the expansion and reduction in
compressive strength of mortar exposed to MgSO.* solutions 38
2.9 Expansion of high strength concrete due to 10% MgSO.j
solution 39
2 .1 0 Compressive strength of high strength concrete cured in
water and immersed in a 10 % MgSO-t solution for 180 days 40
2.11 Percentage drop in cumulative heat of hydration of ternary
PC-MK-PFA Blends at 20% replacement and at 120 hours
relative to PC 44
2.12 Compressive strength developments in concrete effect of
2.14
2.15
2.16
2.17
2.18
2.19
2.20
2.21
2.22
2.23
2.24
2.25
xix
silica fume and Low lime fly ash 46
Compressive strength of Portland
cement-fly ash- silica fume concretes 46
Influence of varying GGBS content at 0%, 10%,
and 20% MK 47
Variation of compressive strength with time for different
cement mortars 48
Compressive strength of hardened specimens made from
PC and MK with/without RHA 48
Bulk density of hardened specimens made from
PC and MK with/without RHA 49
Total porosity of hardened specimens made from
PC and MK with/without RHA 49
Sorptivity with age at 10 %, 20%, 30% and 40% cement
replacement for water-cured concrete 51
Effect of using the binary and ternary blends of
cementitious materials on chloride permeability 53
Effect of using the binary and ternary blends of
cementitious materials on sorptivity 53
Effect of using the binary and ternary blends of
cementitious material on water absorption 54
Effect of silica fume and fly ash on sulphate resistance
(A STM C1012) 56
Weight losses due to immersion in 5% sulphuric acid
solution (a) RHA concrete (b) MK concrete
(c) RHA+MK concrete 56
Expansion of mortar bars containing 20% HCFA
2.26
3.1
3.2
3.3
3.4
3.5
3.6
3.7
3.8
3.9
3.10
3 .11
3.12
3.13
3.14
3.15
3.16
3.17
3.18
3.19
4.1
4.2
4.3
and increasing levels of slag 57
Thermal shock resistance of control and blended cement
paste 58
Research methodology flow chart 62
Modified Loss Angeles grinding machine 65
Grinding curve for POFA 66
KM 40 Kaolin 67
Schematic structure o f kaolinite 67
X-ray fluorescence spectrometer 71
X-ray diffractometer 72
FTIR spectrometer 72
The modified Chappelle’s Test apparatus 74
Mortar mixer 78
Typical casting operation of mortar specimens 80
Mortar flow test 81
Setting time test set up using V1CAT apparatus 82
Temperature of hydration test set-up 83
Porosity test set-up 85
Sorptivity test set-up 87
Furnace 90
Temperature exposure regimes 90
Thermogravimetry Instrument 94
Thermogravimetry and differential thermal analysis for
kaolin 97
X-ray diffraction patterns of kaolin and calcined kaolin at
different temperatures 98
IR spectra of kaolin and calcined kaolin at different
xxi
temperatures 99
4.4 Strength activity indexes of kaolin and calcined kaolin at
different temperatures 1 0 1
4.5 Chemical reactivity of calcined kaolin 102
4.6 Particle size distributions of binders 104
4.7 FESEM micrographs o f OPC, POFA and metakaolin 105
4.8 X-ray diffraction patterns of (a) OPC, (b) POFA and
(c) metakaolin 107
4.9 Particle size distribution of fine aggregate 109
4.10 Flow of plain and blended mortars 111
4 . 1 1 Compressive strength and relative strength of blended
mortars 113
4.12 Flexural strength of plain and blended mortars 114
4.13 Compressive strength-flexural strengths relationship 115
4.14 Porosity o f plain and blended mortars 116
4.15 Compressive strength-porosity relation of blended mortar 117
5.1 Standard Consistencies of pastes 121
5.2 Setting times of pastes 122
5.3 Fleat of hydration temperature of mixes 125
5.4 Compressive strengths of mortars at different
water to binder ratios (a) 0.55 (b) 0.35 128
5.5 Relative compressive strength of mortars at
different water to binder ratios (a) 0.55 (b) 0.35 130
5.6 Sorptivities of plain and blended mortars at
different water to binder ratios 132
5.7 Relationship between compressive strength and sorptivity
of mortars 133
5.8 TG/DTG curves for plain and blended mortars (w/b = 0.35)
after 7 days 134
5.9 TG/DTG curves for plain and blended mortars (w/b = 0.35)
after 180 days 135
5.10 Calcium hydroxide content for w/b ratio of 0.55 137
5.11 Calcium hydroxide content for w/b ratio of 0.35 138
5.12 Calcium hydroxide depleted for w/b of 0.55 140
5.13 Calcium hydroxide depleted for w/b of 0.35 141
5.14 X-ray diffraction patterns of mortars at 7 days 142
5.15 X-ray diffraction patterns of mortars at 28 days 142
5.16 X-ray diffraction patterns of mortars at 90 days 143
5.17 X-ray diffraction patterns of mortars at 180 days 143
6 . 1 Compressive strength and residual compressive
strength of blended mortars at different temperatures 148
6.2 Pulse velocities and residual pulse velocities of
blended mortars at different temperatures 150
6.3 Relationship between compressive strength and
pulse velocity of mortars 151
6.4 XRD patterns of mixes at ambient temperature 153
6.5 XRD patterns of mixes at 400°C 153
6.6 XRD patterns of mixes at 800°C 154
6.7 FTIR spectra of mixes at ambient temperature 155
6.8 FTIR spectra of mixes at 400°C 156
6.9 FTIR spectra of mixes at 800°C 156
6 .10 FESEM images of plain OPC mix at different temperatures 157
6 .11 FESEM images of 20PF mix at different temperatures 158
6.12 FESEM images of 20MK mix at different temperatures 158
xxii
6.13
6.14
6 15
6.16
6.17
6.18
6.19
6.20
6.21
6.22
6.23
6.24
6.25
6.26
XXUI
FESEM images of ternary mix at different temperatures 158
Compressive strengths of mortars after immersion in
3% H2SO4 solution 158
Residual compressive strengths of mortars after
immersion in 3% H2SO4 solution 161
Residual mass of mortars after immersion in 3% H2SO4 162
Relationship between residual compressive strength and
residual mass of mortars exposed to H2SO4 solution 163
XRD patterns of plain and blended mortars after 180 days
in 3% H2SO4 solution 164
XRD patterns of plain and blended mortars after 180 days
in limewater 165
FTIR spectra of plain and blended mortars after 180 days in
limewater 166
FTIR spectra of plain and blended mortars after 180 days in
3% H2S 0 4 167
Residual compressive strength of mortars in Na2S0 4 solution 169
Residual compressive strength of mortars in MgS(>4 solution 169
Expansion of plain and blended mortars in Na2SC>4 and
MgSC>4 solution 172
XRD patterns of plain and blended mortar after 180 days
in water, Na2SC>4 and MgSC>4 solution 175
FTIR spectra of plain and blended mortars after 180 days
in Na2SC>4 and MgSC>4 solution 177
xxiv
LIST OF SYMBOLS
A - Cross-sectional area of specimen
A - Angstrom
°c - Degree Celsius
d - Density of water
D50 - Median particle size
fm - Compressive strength
Hr - Hour(s)
H* - Hydrogen Ion
/ - Water absorption
Kv - Kilovolt
KBr - Potassium bromide
MPa - Mega Pascal
Mi - Initial mass of specimen
M„ - Mass of specimen at n days
m, - Change in mass due to water absorption of specimen
n - Age in days
P - Total maximum load
Pr Porosity
S - Second
X XV
5 - Sorptivity
Sf - Flexural strength
T - Time
Vl, \>2 - symmetric stretches vibration mode
Vj - antisymmetric stretches vibration mode
vp - variabl e-pressure
WA - Weight of saturated specimen in air
WD - Weight of oven-dried specimen
Ww - Weight of saturated specimen in water
pm - Micrometer
> - Greater than or equal to
< . less than or equal to
9 - Theta
X - Lambda
0 - Diameter
XXVI
LIST OF ABBREVIATIONS
ANOVA - Analysis of Variance
ASTM - American Society for Testing and Materials
BA - Bagasse Ash
BET - Brunauer Emmett Teller
BS - British Standard
CaC 03 - Calcium Carbonate
Ca(OH)2 - Calcium Hydroxide
CSH - Calcium Silicate Hydrate
DSC - Differential Scanning
DTA - Differential Thermal Analysis
FESEM - Field Emission Scanning Electron Microscopy
FA - Fly Ash
FTIR - Fourier Transformed Infrared
GGBS - Ground Granulated Blast Slag
GLM - General Linear Model
GPOFA - Ground Palm Oil Fuel Ash
HCFA - High Calcium Fly Ash
HCl - Hydrochloric Acid
HSGC - High Strength Green Concrete
LOI - Loss on Ignition
MK - Metakaolin
N 2 - Nitrogen
OPC - Ordinary Portland Cement
PC - Portland Cement
PFA - Pulverized Fly Ash
POFA - Palm Oil Fuel Ash
RHA - Rice Husk Ash
RILEM - International Union of Laboratories and Experts
Construction Materials, Systems and Structures
SCC - Self-Compacting Concrete
SF - Silica Fume
sp - Superplasticizer
TGA - Thermogravimetric Analysis
UPV - Ultrasonic Pulse Velocity
w/b - Water to Binder Ratio
XRD - X-Ray Diffraction
LIST OF APPENDICES
APPENDIX TITLE PAGE
A Sorptivity Calculation Example 204
B Determination of Ca(OH)2 Content and
amount of Ca(OH)2 Depleted in Blended Sample 205
C List of Publications 208
CHAPTER 1
INTRODUCTION
1.1 Background to the Study
Concrete is second to water as the most widely used material in the globe
(Mehta and Monteiro, 2006). The superior niche of concrete in the construction
industry over other materials, such as steel and timber is undoubtedly attributed to its
strength, durability, versatility nature and relative cheapness. However, concrete
constitutes Portland cement as its most important component because of its binding
characteristic but the key contributor to the embodied CO2.
Cement production contributes to global warming due to CO2 emission. For
every one ton of Portland cement produced, an average of 0.87 ton of CO2 is emitted
to the atmosphere (Saca and Georgescu, 2014). In fact, due to the bulky annual
global cement production output; which had reached 3737 metric ton (Mt) in the year
2012 and projected to increase to 4368 Mt by the year 2016 (Armstrong, 2013),
cement production accounts for 5 to 8% of the total anthropogenic CO2 emitted in
the planet (Femandez-Carrasco et al., 2012). However, the use of pozzolanic
materials to partially substitute Portland cement in concrete has been recognized as
one of the sustainable approaches for reducing CO2 emission that arise from cement
production (Saca and Georgescu, 2014).
2
Pozzolanic materials are siliceous, and aluminous materials that react with
calcium hydroxide liberated during cement hydration to produce secondary
cementitious compounds that enhance strength and durability of concrete (Grist et
al., 2013). The commonly used pozzolanic materials include; fly ash, silica fume,
slag, metakaolin (MK), rice husk ash, palm oil fuel ash (POFA) and natural
pozzolans. Apart from the benefits of reducing CO2 emission as well as performance
improvement of concrete, the utilization of these pozzolanic materials; which are
mostly industrial wastes, helps in reducing not only the environmental burden related
to their disposal but also the cost of concrete production. In palm oil producing
countries such as Malaysia, Indonesia and Thailand, POFA is generated in huge
quantity from palm oil mills as waste with a significant amount of the ash disposed
off to landfills. For instance, according to Chandara et al. (2012), in 2009 alone, up
to 3 million tons of POFA was generated in Malaysia and with the growth of palm
oil industry, more waste generation should be anticipated and hence increase in
volume of waste to landfills.
In an attempt to reduce the environmental impact of disposing POFA to
landfills and cement production, as well as to produce affordable but high-
performance cement based materials, considerable effort of research into the use of
POFA as pozzolanic material is currently underway. POFA has been found to be a
useful pozzolanic material that improves the performance o f concrete (Awal and
Hussin, 1997). On the other hand, due to the global abundance of kaolin reserve
coupled with the prospective shortage of traditional pozzolanic materials (fly ash,
slag and silica fume), the use of MK as pozzolan has also been investigated
(Vejmelkova et al., 2010). Metakaolin is produced from the thermal treatment of
kaolinite clay or paper sludge at a controlled temperature of 500 to 800°C (Frias et
al., 2008a and Kadri et a l 2011).The incorporation of MK in the production of
concrete enhances its mechanical properties and durability performance (Siddique
and Klaus, 2009; Moser et al., 2010; Shekarchi et al., 2010). Moreover, the use of
MK is also environmentally friendly with respect to reduction in CO: emission to the
atmosphere by reducing the Portland cement consumption (Guneyisi et al., 2008;
Mermerda§ et al., 2012).
3
However, due to the variability in the properties of pozzolanic materials and
their different reaction patterns with the cement hydration products, the influence of
each of these materials on the properties of concrete varies. While some materials are
deficient, others exhibit contrasting influences on the properties of concrete. These
limit the extent to which each pozzolanic material can substitute cement to achieve
the desired concrete property. In view of the need to increase the level of alternatives
to cement and also produce concrete of high performance, the use of ternary blend
(combining two pozzolanic materials to partially replace Portland cement) utilizing
their synergistic interactions has currently become a common practice. To date,
intensive researches on the use of ternary blends such as MK and fly ash by Moser et
al. (2010), MK and slag by Khatib and Hibbert (2005), and POFA and fly ash by
Rukzon and Chindaprasirt (2009) have been conducted Yet there has not been
detailed study on the ternary blend of MK and POFA. It is, therefore, the intent of
this study to investigate the effect of a ternary blend of MK and POFA on the
properties of cement mortar.
1.2 Research Problem
Intensive researches on the use of pozzolanic materials have been undertaken
over an extended period, and the benefits of using binary blends o f POFA and
metakaolin (MK) are widely established (Awal and Hussin, 1997; Bai et al., 1999;
Kroehong et al., 2011; Kadri et al., 2011; Megat Johari et al.. 2012; Cassagnabere et
al., 2013). It is known that MK improves early strength development,
microstructures and some durability properties. But it was shown to reduce
workability (Bai et al., 1999; Cassagnabere et al., 2013) as well as to increase heat of
hydration (Bai and Wild, 2002; Kadri et al., 2011) which could be detrimental to the
durability of mainly mass concrete. Moreover, metakaolin was found to be deficient
in resisting magnesium sulphate attack (Lee et al., 2005) and elevated temperatures
(above 400 °C) (Poon et al., 2003; Nadeem et a l, 2014). On one hand, the use of
POFA showed improvement in reducing heat of hydration, in resistance to sulphate
attack and elevated temperatures but on the other hand, it is deficient in early
4
strength development (Tangchirapat et al., 2007). The deficiencies of these materials
when singly used may restrict the scope of their use in construction industry. For
instance, due to the slow strength development characteristic of POFA in concrete,
POFA may not be a suitable material in precast industry or where early strength
development is paramount. Also, due to the increase in heat of hydration, the use of
metakaolin in mass concrete may be a disadvantage. While there are abundant
information on the effects of POFA and MK as binary, limited information exists on
their combining influence in ternary blends. Therefore, the potential improvement in
the properties of the mortar due to the combining effect of POFA and MK through
their synergistic interaction needs to be studied. The study may consequently lead to
the development of environmental friendly cement-based materials with a wider
scope of applications in construction industry.
1.3 Aim and Objectives
The aim of the study is to evaluate the combined effects of metakaolin (MK)
and palm oil fuel ash (POFA) as pozzolanic materials on the performance of cement
mortar. The aim is to be achieved through the following objectives:
(i) To characterize the physical and chemical properties of POFA and MK used
in the study.
(ii) To determine the optimum replacement levels of POFA and MK ternary
blended cement mortar.
(iii) To evaluate the fresh and hardened properties as well as microstructures of
the optimized POFA and MK ternary blended cement mortar.
(iv) To investigate the durability performance of the optimized POFA and MK
ternary blended cement mortar exposed to hostile environments.
1.4 Scope of the Study
This study was purely experimental in nature and it focused on examining the
effects of combining MK and POFA on the properties of cement mortar. In the
beginning, material characterizations such as physical properties, chemical and
mineralogical compositions that are essential for explaining how these may influence
the properties tested in mortar were carried out. In order to obtain the optimum
ternary blend, tests on the properties of various binary and ternary blended mixes
made with varying replacement levels limited up to 30% by weight and a constant
water binder ratio of 0.55 were also performed. The properties considered were
mortar flow as well as compressive strength, flexural strength and porosity after
water-cured for up to 90 days. The established optimum ternary blend was used for
the detail investigations on the fresh and hardened properties, microstructures and
durability. However, for the detailed study, different water to binder ratios of 0.55
and 0.35 were used for the production of mortar.
At fresh state, the setting times, standard consistency, flowability and
temperature of hydration of the optimized ternary blend were investigated while at
the hardened state only the compressive strength, sorptivity, microstructures and
durability properties for up to 6 months were considered The durability was assessed
in terms of resistance to magnesium and sodium sulphate attack, sulphuric acid
attack and elevated temperature. The microstructure was evaluated using the
Thermogravimetry Analysis (TGA), X-Ray Diffraction (XRD), Fourier Transformed
Infrared (FTIR) and Field Emission Scanning Electron Microscope (FESEM)
techniques.
6
The series of tests conducted in this study are based on the procedures of
British Standards (BS), American Society for Testing and Materials (ASTM),
International Union of Laboratories and Experts in Construction Materials, Systems
and Structures (RILEM) and adopted methods in the literature reviewed. As these are
well established, this enabled comparison with related studies, with information on
their precision known.
In addition to compressive strength and sorptivity, the amount of Ca(OH)2
depleted was used as a variable for assessing the microstructure of the optimized
specimens at its hardened state. Meanwhile, residual compressive strength, residual
mass and expansion were used as parameters for measuring the resistance of
specimens to sulphuric acid, magnesium and sulphate attacks. The resistance to
elevated temperature was however, measured in terms of residual compressive
strength and ultrasonic pulse velocity (UPV). All the results were analyzed and
presented in the forms of graph and output from the XRD, TG/DTG and FTIR tests.
The findings were referred and compared with similar previous studies.
1.5 Significance of the Study
As this research study was aimed at gathering information on the use of
ternary blend from a systematic investigation, it can be useful for the development of
standard specifications for ternary blended system which are essential for their
practical application. It can also contribute to the development of environmental
friendly material that has a wide range of applications in construction industry. This
will be more beneficial for the palm oil producing countries like Malaysia, as waste
(POFA) from palm oil mills can be put to good use in addition to the environmental
benefit of solving disposal problems of POFA to landfills. The outcome of the study
can also provide the basis for further researches for better understanding of the
behaviour of a ternary blend of POFA and MK, which will ultimately increase
substance to the pool of existing knowledge.
7
1.6 Thesis Organisation
Chapter 1 provides a general appraisal and the rationale for conducting this
research. Also, concise description of background problem, aim and objectives,
scope and limitations, and significance of study are presented in this chapter.
Chapter 2 describes the properties of Portland cement and pozzolanic
materials. The chapter also presents the review of previous studies on the effect of
binary and ternary blends on the properties of paste, mortar and concrete. Although,
there few or no literature available on the ternary blend o f palm oil fuel ash and
metakaolin, the benefits of ternary blends of other pozzolanic materials such as fly
ash and silica fume over their binary counterparts are also reviewed
Chapter 3 provides a detailed account of the materials and sample
preparation as well as the test methods used during the experimental work.
Subsequent chapters then present the results of these tests.
Chapter 4 examines the physical and chemical properties of Portland
cement, palm oil fuel ash and metakaolin. The results of the optimization of
calcination temperature of kaolin to produce metakaolin are also presented. In
addition, the results and discussions on the optimization of the ternary blend used for
the detailed study are presented in this chapter.
Chapter 5 covers the results and discussions on the fresh and hardened
properties, and microstructures of the optimized ternary blended mortar. The
properties of mortar studied in its fresh state include consistency, setting times,
workability/flow, and adiabatic temperature rise. At the hardened state, the
characteristics of mortar considered were compressive strength and sorptivity. The
relationship between sorptivity and compressive strength of mortar was also
highlighted in order to establish a correlation. Furthermore, the results of the
8
microstmcture of blended mortars using the thermogravimetry Analysis (TGA) and
X-ray diffraction (XRD) are discussed.
Chapter 6 describes the results and discussions of the chemical attack
and elevated temperature tests on the blended mortars. Fourier transform infrared
(FTIR), X-ray diffraction (XRD) and field emission scanning electron microscopy
(FESEM) results of specimens after the attack are likewise presented in this chapter.
Chapter 7 shows the overall conclusions from this study and
recommendations for further researches.
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