UNIVERSITI PUTRA MALAYSIA ACTIVATION AND …

UNIVERSITI PUTRA MALAYSIA

ACTIVATION AND CHARACTERIZATION OF DUNE SAND AS PARTIAL CEMENT REPLACEMENT FOR CONCRETE

ASIAH ABDULLAH

FS 2012 2

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ACTIVATION AND CHARACTERIZATION OF DUNE SAND AS PARTIAL

CEMENT REPLACEMENT FOR CONCRETE

By

ASIAH ABDULLAH

Thesis Submitted to the School of Graduate Studies, Universiti Putra Malaysia,

in Fulfillment of the Requirements for the Degree of Master of Science

January 2012

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To my precious parents who always give me fabulous love,

spectacular care and support, to my adorable brothers, and

sisters.

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Abstract of the thesis presented to the Senate of Universiti Putra Malaysia in

fulfillment of the requirements for the degree of Master of Science

ACTIVATION AND CHARACTERIZATION OF DUNE SAND AS PARTIAL

CEMENT REPLACEMENT FOR CONCRETE

By

ASIAH ABDULLAH

January 2012

Chairman: Professor Taufiq Yap Yun Hin, PhD

Faculty: Science

Dune sand obtained in the vicinity of Riyadh, Saudi Arabia has been investigated to

be used as partial cement replacement materials for concrete. Physical and chemical

properties of dune sand were evaluated and it was found that it has potential to be

processed and used as partial cement replacement due to the high silica content of

about 93.4%. However, dune sand is inert and chemically inactive under normal

condition. Results show that the strength decreases with the increase of cement

replacement by dune sand under normal condition. Therefore, different methods have

been developed to enhance the reactivity of dune sand. Three ways were used to

improve the pozzolanic reactivity including chemical activation, mechanical

activation and thermal activation. For chemical activation, four inexpensive materials

which are NaCl, Na2SO4, CaSO4·2H2O and CaCl2·2H2O were chosen for this study.

Results showed that the addition of chemical activators did not demonstrate an

obvious effect on the strength development of the cement. In the mechanical

activation, the dune sand with prolonged grinding was investigated to study the effect

of using different particle size on the dune sand reactivity. However, it did not result

in substantial improvements to strength. For thermal activation, two different

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techniques were used which are calcination (heat treatment) and autoclave curing.

The calcination process was done to activate the raw material of dune sand at

temperature ranging from 400oC to 1000°C. Experimental results indicated that the

ultimate strength of cement pastes decreased with increasing calcination temperature.

The autoclave curing increased the pozzolanic activity of dune sand with significant

improvement in strength. The maximum compressive strength was found at 30%

replacement of cement by dune sand. The final products obtained were further

analyzed by X-ray diffraction (XRD), scanning electron microscope (SEM),

differential thermal analysis (DTA) and thermogravimetric analysis (TGA) to

investigate the mechanism that caused the increase in the compressive strength.

Elimination of Ca(OH)2 peaks in the XRD analysis clearly proved that crystalline

SiO2 in dune sand can quickly react with Ca(OH)2 that are formed from cement

hydration to form a new type C-S-H hydrate (tobermorite) which improve the

strength and concrete structure under autoclave curing. The compressive strength of

autoclaved concrete containing 30% dune sand as partial cement replacement

increased by 28% compared to concrete that have been subjected to the standard

curing after 154 days. Free Ca(OH)2 content was reduced from 26% in control paste

under standard curing to about 3% in autoclaved cement paste containing 30% dune

sand as partial cement replacement which experienced a reduction of about 89%.

DTA results are also in good agreement with findings by TGA showing lower

content of free Ca(OH)2 in autoclaved products compared to the standard curing. In

general, SEM investigation revealed that the utilization of concrete containing 30%

dune sand as partial cement replacement subjected to autoclave curing produced

more compact microstructure compared to those cured under normal curing.

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Abstrak tesis yang dikemukakan kepada Senat Universiti Putra Malaysia sebagai

memenuhi keperluan untuk Ijazah Master Sains

PENGAKTIFAN DAN PENCIRIAN DUNE SAND SEBAGAI BAHAN

SEPARA GANTI SIMEN BAGI KONKRIT

Oleh

ASIAH ABDULLAH

Januari 2012

Pengerusi: Profesor Taufiq Yap Yun Hin, PhD

Fakulti: Sains

Dune sand yang didapati dari kawasan Riyadh, Arab Saudi telah dikaji untuk diguna

pakai sebagai bahan separa gantian simen dalam bancuan konkrit. Ciri-ciri fizikal

dan kimia bagi dune sand telah dikaji. Bahan ini telah dikenalpasti mempunyai

potensi untuk diproses serta digunakan sebagai bahan separa gantian untuk simen

kerana mempunyai peratus kandungan silika yang tinggi iaitu sebanyak 93.4%.

Walau bagaimanapun, dalam keadaan biasa, dune sand lengai dan tidak aktif secara

kimia. Keputusan menunjukkan yang kekuatan spesimen semakin berkurangan

dengan peningkatan penggantian ke atas simen oleh dune sand dalam keadaan biasa.

Oleh itu, pelbagai kaedah telah dijalankan bagi meningkatkan kereaktifan dune sand.

Tiga kaedah telah digunakan untuk meningkatkan kereaktifannya termasuklah

pengaktifan secara kimia, pengaktifan secara mekanikal dan pengaktifan secara

terma. Bagi pengaktifan secara kimia, empat bahan kimia dengan kos yang rendah

iaitu NaCl, Na2SO4, CaSO4·2H2O dan CaCl2·2H2O telah dipilih untuk kajian ini.

Keputusan menunjukkan penambahan bahan-bahan kimia ini ke dalam sistem tidak

menunjukkan kesan yang ketara terhadap perkembangan kekuatan simen. Bagi

pengaktifan secara mekanikal, dune sand telah dikisar kepada saiz yang lebih kecil

untuk mengkaji kesan perbezaan saiz zarah terhadap kereaktifan dune sand. Walau

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bagaimanapun, hasilnya juga tidak menunjukkan perkembangan kekuatan simen

yang memberangsangkan. Bagi pengaktifan secara terma, dua teknik telah digunakan

iaitu rawatan suhu (calcination) dan rawatan autoclave. Proses rawatan suhu telah

dijalankan ke atas dune sand bermula dari suhu 400oC ke 1000

oC. Keputusan

menunjukkan kekuatan simen semakin berkurang dengan peningkatan suhu. Namun

begitu, rawatan autoclave telah berjaya meningkatan kereaktifan dune sand

berdasarkan peningkatan kekuatan simen yang telah terhasil. 30% penggantian ke

atas simen oleh dune sand dikenalpasti sebagai peratus yang dapat memberi kekuatan

yang maksimum kepada sampel. Produk akhir yang terhasil untuk sampel terpilih

telah dicirikan dengan menggunakan pembelauan sinar-X (XRD), mikroskop

elektron imbasan (SEM), analisis pembezaan terma (DTA) dan analisis

termogravimetrik (TGA) bagi mengkaji mekanisme yang menyebabkan peningkatan

kekuatan sampel. Kehilangan puncak bagi Ca(OH)2 dalam analisis XRD jelas

menunjukkan bahawa hablur SiO2 di dalam dune sand dapat bertindak balas dengan

Ca(OH)2 yang terhasil dari proses hidrasi simen untk menghasilkan C-S-H jenis baru

(tobermorite) yang dikenalpasti telah meningkatkan kekuatan dan struktur konkrit

melalui rawatan autoclave. Kekuatan bagi konkrit yang mengandungi 30% dune

sand sebagai bahan separa gantian simen dan dikenakan rawatan autoclave telah

meningkat sebanyak 28% berbanding konkrit yang dirawat dalam keadaan biasa.

Kandungan Ca(OH)2 di dalam sampel paste telah berkurang sebanyak 89% iaitu dari

26% bagi paste kawalan yang dirawat dalam keadaan biasa kepada 3% bagi paste

yang mengandungi 30% dune sand sebagai bahan separa gantian simen dan

dikenakan rawatan autoclave. Keputusan DTA juga adalah selari dengan keputusan

TGA di mana menunjukkan kandungan Ca(OH)2 yang rendah bagi produk yang

terhasil dengan rawatan autoclave berbanding rawatan biasa. Secara amnya,

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berdasarkan keputusan SEM, penggunaan 30% dune sand sebagai bahan gantian

untuk simen bagi konkrit yang dikenakan rawatan autoclave telah menghasilkan

struktur mikro yang lebih mampat berbanding konkrit yang dirawat dalam keadaan

biasa.

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ACKNOWLEDGEMENTS

I wish to express my outmost gratitude to Allah subhanahua ta’ala for the strength

and patience He bestowed on me to undertake this research project.

I would like to acknowledge my sincere appreciation to my supervisor, Prof. Dr.

Taufiq Yap Yun Hin for his trust, dedicated supervision, outstanding guidance,

patience and unconditional support throughout the duration of my master’s studies

and thesis project. My special thanks also dedicated to my project leader (co-

supervisor), Prof. Ir. Dr. Mohd. Saleh Jaafar. If not for the generous help and advice

offered by him, this project would have been a much more difficult task to

accomplish.

I would also like to thank Mr. Halim Othman, Mr. Fairuz Ismail and Madam

Khatijah Hassan from the Department of Civil Engineering, Faculty of Engineering

for their support with technical advice, materials and laboratory facilities; also to

Madam Norazlina Shari, Madam Zaidina Md. Daud and other Science Officers in the

Department of Chemistry, Faculty of Science for their assistance in the

characterization works. Not to forget officers in Characterization Lab and Electron

Microscopy Unit, Department of Chemical and Environmental Engineering, Faculty

of Engineering especially Mr. Ismail Abdul Ghani and Mr. Adli Nazri Mohd Kassim

for their help and advice in running SEM and particle size analysis.

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Special thanks are extended to Prof. Dr. Jamaloddin Noorzaei, Mr. Omer Abdalla

Alawad, Ms. Farhana Abang Abdul Rahim, Mr. Lai Fok How, colleagues and friends

for their help, valuable comments and suggestions during the course of this work.

Most especially, I wish to thank my parent and family for their love, never ending

support and encouragement throughout these years.

Last but not least, sincere and great appreciation goes to the Management of the King

Saud University (KSU), Saudi Arabia especially Prof. Dr. Abdurrahman M.

Alhozaimy and Dr. Abdulaziz Al-Negheimish for providing research grant and to the

Management of Universiti Putra Malaysia (UPM) for unfailing support for us to

undertake this first ever joint research between the KSU and UPM. Financial support

from Universiti Teknologi Mara and Ministry of High Education through Young

Lecturer Scheme is gratefully acknowledged.

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I certify that an Examination Committee has met on 10 January 2012 to conduct the

final examination of Asiah Abdullah on her Master of Science thesis entitled

“Activation and Characterization on Dune Sand as Partial Cement Replacement for

Concrete” in accordance with the Universities and University College Act 1971 and

the Constitution of the Universiti Putra Malaysia [P.U.(A) 106] 15 March 1998. The

Committee recommends that the student be awarded the Master of Science.

Members of the Examination Committee were as follows:

Kamaliah Sirat, PhD

Faculty of Science

Universiti Putra Malaysia

(Chairman)

Anuar Kassim, PhD

Professor

Faculty of Science


(Internal Examiner)

Mansor Hj Ahmad @ Ayob, PhD

Associate Professor

Faculty of Science


(Internal Examiner)

Yang Farina Abdul Aziz, PhD

Professor

Faculty of Science and Technology

Universiti Kebangsaan Malaysia

(External Examiner)

_________________________

SEOW HENG FONG, PhD

Professor and Deputy Dean

School of Graduate Studies


Date: 2 March 2012

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This thesis was submitted to the Senate of Universiti Putra Malaysia and has been

accepted as fulfilment of the requirement for the degree of Master of Science. The

members of Supervisory Committee were as follows:

Taufiq Yap Yun Hin, PhD

Professor

Faculty of Science


(Chairman)

Mohd. Saleh Jaafar, PhD

Professor

Faculty of Engineering


(Member)

________________________________

BUJANG BIN KIM HUAT, PhD

Professor and Dean

School of Graduate Studies


Date:

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DECLARATION

I declare that the thesis is my original work except for the quotations and citations

which have been duly acknowledged. I also declare that it has not been previously,

and is not concurrently, submitted for any other degree at Universiti Putra Malaysia

or at any other institution.

ASIAH ABDULLAH

Date: 10 January 2012

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TABLE OF CONTENTS

Page

ABSTRACT iii

ABSTRAK v

ACKNOWLEDGEMENTS viii

APPROVAL x

DECLARATION xii

LIST OF TABLES xvi

LIST OF FIGURES xvii

LIST OF ABBREVIATIONS xxi

CHAPTER

1 INTRODUCTION

1.1 General Introduction to Portland Cement 1

1.2 The Application of Portland Cement in Construction Industries 2

1.3 Pozzolanic Materials 3

1.3.1 Natural Pozzolanic Materials 4

1.3.2 Artificial Pozzolanis Materials 5

1.4 Problem Statements 6

1.5 Scope and Research Objectives 7

2 LITERATURE REVIEW

2.1 Manufacture of Portland Cement 9

2.1.1 Preparation of Raw Mixture 9

2.1.2 Formation of the Clinker 10

2.1.3 Production of the Cement 11

2.2 Chemical Composition of Portland Cement 12

2.2.1 Alite 15

2.2.2 Belite 15

2.2.3 Aluminate 17

2.2.4 Ferrite 17

2.3 Portland Cement Hydration 17

2.3.1 Hydration of Aluminates 19

2.3.2 Hydration of Silicates 23

2.4 Pozzolanic Reaction 26

2.5 Supplementary Cementitious Materials 28

2.5.1 Silica Fume 28

2.5.2 Fly Ash 30

2.5.3 Ground Granulated Blast Furnace Slag 32

2.6 Dune Sand 33

2.6.1 Properties of Dune Sand 34

2.6.2 Application of Dune Sand 34

2.7 Activation Method 35

2.7.1 Mechanical Activation 35

2.7.2 Thermal Activation 37

2.7.2.1 Calcination 37

2.7.2.2 Elevated Temperature Curing 39

2.7.3 Chemical Activation 42

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2.7.3.1 Alkali Activation 43

2.7.3.2 Sulfate Activation 45

2.7.3.3 Other Type of Activation 46

3 MATERIALS AND METHODS

3.1 Materials 48

3.2 Preparation of Paste 49

3.3 Activation of Dune Sand as Partial Cement Replacement 51

3.3.1 Thermal Activation 52

3.3.1.1 Autoclave Curing 52


3.3.2 Chemical Activation 55

3.3.3 Mechanical Activation 56

3.4 Preparation of Mortar and Concrete 57

3.5 Sample Characterization 58

3.5.1 Chemical Analysis 58

3.5.1.1 X-Ray Fluorescence Analysis 58

3.5.1.2 Energy Dispersive X-Ray 59

3.5.2 BET Surface Area Measurements 60

3.5.3 Particle Size Analysis 61

3.5.4 Compressive Strength 62

3.5.5 X-Ray Diffraction Analysis 63

3.5.6 Scanning Electron Microscope 64

3.5.7 Thermal Analysis 65

3.5.7.1 Thermogravimetric Analysis 65

3.5.7.2 Differential Thermal Analysis 66

4 RESULTS AND DISCUSSION

4.1 Characterization of raw materials 68

4.1.1 Chemical Analysis, BET Surface Area Measurements and

Particle Size Analysis

6

68

4.1.2 Phase Identification Using Powder XRD Technique 70


4.2 Effect of Cement Replacement by Dune Sand at Standard

Condition

72

4.2.1 Compressive Strength 72



4.2.4 Energy Dispersive X-Ray 78




4.3 Activation of Dune Sand as Partial Cement Replacement 86

4.3.1 Influence of Thermal Activation on Reactivity of Dune

Sand

86

4.3.1.1 Autoclave Curing 86


4.3.2 Effect of Chemical Activators on the Dune Sand

Reactivity

94

4.3.3 Influence of Mechanical Activation on the Reactivity of 98

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Dune Sand

4.4 Characterization of Activated Hardened Cement Pastes 101

4.4.1 Summary of Effects on Strength 101



4.4.4 Energy Dispersive X-ray 110




5 CONCLUSION AND RECOMMENDATIONS

5.1 Conclusion 120

5.2 Recommendations 123

REFERENCES 124

APPENDICES 132

BIODATA OF STUDENT 151

LIST OF PUBLICATIONS 152

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