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INVESTIGATION OF POROUS GLASSES BASED ON SODIUM- BOROSILICATE GLASS SYSTEM MUHAMMAD HASANUZZAMAN (B.Sc., M.Eng.) A thesis submitted for the degree of Doctor of Philosophy School of Mechanical and Manufacturing Engineering DUBLIN CITY UNIVERSITY Supervisor: Dr. Abdul-Ghani Olabi March 2013 DECLARATION I hereby certify that this material, which I now submit for assessment on the programme of study leading to the award of Ph.D. is entirely my own work, and that I have exercised reasonable care to ensure that the work is original, and does not to the best of my knowledge breach any law of copyright, and has not been taken from the work of others save and to the extent that such work has been cited and acknowledged within the text of my work. Signed : ______________________________________ (Muhammad Hasanuzzaman) ID No. : 53126505 Date : March 2013 i ACKNOWLEDGEMENTS It is with deep gratitude and appreciation that I would like to thank the many people who made this thesis possible. I would like to express my sincere thanks and gratitude to my supervisor Dr. Abdul- Ghani Olabi. He provided knowledge, guidance, and advice that was invaluable throughout the course of this research. Without his continuous help and advice this work would not have been possible. I am very much grateful to Professor M. S. J. Hashmi for his continuous support while I carried out my study. I would also like to thank Dr. Joseph Stokes. As Head of School, he lent me his full and unreserved support. I am indebted to my previous supervisor Dr. Aran Rafferty for giving me the opportunity, advice, and encouragement to undertake this PhD. He provided sound advice, good teaching, good company, and many good ideas throughout the study. I would like to thank Chris Crouch, Michael May, Liam Domican, and all other staffs members of the school of Mechanical and Manufacturing Engineering. Special thanks are also to Yoann Glocheux, Queens University Belfast, for the use of the nitrogen adsorption porosimetry facility. I wish to thank my elder brother Dr. A.R.M. Harunur Rashid, my entire family, and all my friends, for helping me to get through challenging times, and for all the emotional support, comradeship, entertainment, and caring they generously provided. I wish to thank my parents, Muhammad Isa and Syeda Raihana Begum. They bore me, raised me, supported me, taught me, and loved me. Lastly and most importantly, very special thanks and appreciation go to my beloved wife and son, Samira Sharmin Mahbub and Nayl Hasan. Their love, patience, and ii constant encouragement have made my PhD journey more meaningful. To embark on this PhD was a serious decision. I was then newly married and we both had jobs and a settle life in Bangladesh. My wife provided generous encouragement and made my decision easier to enable me to pursue my longstanding dream. During my PhD, I encountered some hurdles along with the good times. My son was born the year I started my PhD. There was a gap of almost two years, while I deferred my PhD work and spent time in Bangladesh. But, even though circumstances were going against continuing my PhD work, I did not give up. Without their continuous encouragement, patience, and tolerance, completing my PhD would simply not have been possible. My son spent almost two years without having me at his side. He was strong and always asked me when I would be finished. Nothing compared to the motivation that he gave me, and to the strength that he showed at his young age. To my wife Samira Sharmin Mahbub and my son Nayl Hasan, I dedicate this thesis. iii TABLE OF CONTENTS DECLARATION.................................................................................................................... I ACKNOWLEDGEMENTS ................................................................................................. II LIST OF FIGURES ......................................................................................................... VIII LIST OF TABLES ........................................................................................................... XIII ABBREVIATIONS ............................................................................................................ XV ABSTRACT ..................................................................................................................... XVII CHAPTER ONE GENERAL INTRODUCTION ............................................................................................. 1 1.1 MOTIVATION AND BACKGROUND ............................................................................... 1 1.2 RESEARCH OBJECTIVES ............................................................................................... 5 1.3 THESIS OUTLINE .......................................................................................................... 5 CHAPTER TWO LITERATURE REVIEW ..................................................................................................... 7 2.1 DEFINITION OF GLASS ................................................................................................. 7 2.2 THE GLASS TRANSITION .............................................................................................. 8 2.3 STRUCTURE OF GLASS ................................................................................................. 9 2.3.1 Random network model ...................................................................................... 9 2.4 AMORPHOUS PHASE SEPARATION ............................................................................. 11 2.4.1 Spinodal decomposition ................................................................................... 11 2.4.2 Nucleation and growth ..................................................................................... 13 2.5 COMMON GLASS SYSTEMS ........................................................................................ 14 2.5.1 Soda-lime glass or commercial glass ............................................................... 14 2.5.2 Lead glass......................................................................................................... 15 2.5.3 Aluminosilicate glass ....................................................................................... 15 2.5.4 Borosilicate glass ............................................................................................. 16 2.6 POROUS GLASSES ...................................................................................................... 16 2.6.1 Pore size classification ..................................................................................... 17 iv 2.6.2 Porous glasses in general ................................................................................ 18 2.6.2.1 Porous glass based on alkali borosilicate ...................................................... 19 2.6.2.2 Other porous materials synthesised by the sol-gel and other process ............... 19 2.7 PREPARATION OF POROUS GLASS USING THE SODIUM BOROSILICATE GLASS SYSTEM . .................................................................................................................................. 20 2.7.1 Early development ............................................................................................ 20 2.7.2 The ternary Na2O–B2O3–SiO2 system .............................................................. 22 2.7.3 ZrO2–SiO2 binary phase diagram .................................................................... 23 2.7.4 Effect of composition on glass properties ........................................................ 24 2.7.5 Porous glass preparation process using Na2O–B2O3–SiO2 system .................. 27 2.7.6 Amorphous phase separation mechanism ........................................................ 28 2.7.7 Influence of heat-treatment time and temperature on phase separation .......... 32 2.7.8 Acid leaching and alkali washing .................................................................... 34 2.7.9 Applications ...................................................................................................... 37 2.8 ALKALI RESISTANCE ................................................................................................. 39 2.8.1 Approaches for improving alkali resistance .................................................... 40 2.8.2 Non-porous alkali-resistant glass .................................................................... 47 2.9 PORE CHARACTERISATION TECHNIQUES ................................................................... 48 2.9.1 Mercury porosimetry ........................................................................................ 48 2.9.1.1 Theory....................................................................................................... 48 2.9.1.2 Pore size and total pore volume ................................................................... 49 2.9.1.3 Density and porosity measurement ............................................................... 50 2.9.1.4 Pore size distribution .................................................................................. 51 2.9.1.5 Advantages and limitations of mercury porosimetry ...................................... 54 2.9.2 Other methods for meso to macropore characterisation ................................. 55 2.9.3 Surface area determination .............................................................................. 56 2.9.3.1 Using mercury porosimetry ......................................................................... 56 2.9.3.2
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