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Titanium Dioxide Nanomaterials, Synthesis, Stability and Mobility in Natural and Synthetic Porous Media

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Titanium Dioxide Nanomaterials, Synthesis, Stability and Mobility in Natural and Synthetic Porous Media TITANIUM DIOXIDE NANOMATERIALS, SYNTHESIS, STABILITY AND MOBILITY IN NATURAL AND SYNTHETIC POROUS MEDIA by Ghulam Raza A Thesis submitted to The University of Birmingham for the degree of DOCTOR OF PHILOSOPHY School of Geography, Earth and Environmental Sciences The University of Birmingham December 2016 i University of Birmingham Research Archive e-theses repository This unpublished thesis/dissertation is copyright of the author and/or third parties. The intellectual property rights of the author or third parties in respect of this work are as defined by The Copyright Designs and Patents Act 1988 or as modified by any successor legislation. Any use made of information contained in this thesis/dissertation must be in accordance with that legislation and must be properly acknowledged. Further distribution or reproduction in any format is prohibited without the permission of the copyright holder. Abstract Titanium oxide (TiO2) nanomaterials (NMs) improve potential value to commercial products like sun creams, cosmetics, paints, self-cleaning products, textiles, sports equipment etc. Research on the fabrication of NMs to develop or invent probable new methods and functionalities is an ongoing process. Stabilization of these NMs to retain their nanometric scale is a major issue: and to accomplish this goal, different surfactants and coating agents are used to modify NMs properties. Synthesis of highly ordered, stable, reproducible and cost effective TiO2 NMs remains a challenge. A need of further research still exists in order to develop an in depth understanding of synthesis, aggregation kinetics and transport through porous media, and to determine the ultimate fate and interactions of these NMs with environmental constituents after their release in the natural ecosystem. This research work was typically divided into three phases; synthesis, stabilization and transport. Synthesis was accomplished with sol-gel, hydrothermal and a mix of both methods. The effects of pH, precursors, temperature and different alcohol concentrations were studied in detail. Stability was achieved after extensive research on different surfactants including polyethylene glycol (PEG), Polyvinylpyrrolidone (PVP), Sodium citrate, Sodium Dodecyl Sulfate (SDS), Suwannee River fulvic acid (SRFA). Aggregation kinetics of stabilized NMs was evaluated in detail in the presence of mono and divalent electrolytes (NaNO3, NaCl, CaN2O6, CaCl2). Two different types of morphologies of TiO2 NMs were used during these studies i.e. round anatase NPs and rutile ellipsoids. The stabilized NMs were checked for their mobility through different natural and synthetic porous media (sandstone and glass bead columns) in the third and final phase of this research work. i Different forms of Titanium dioxide nanomaterials including nano-powders and stabilized suspensions were synthesized. The effect of pH, precursors, temperature and zeta potential on nanoparticles nucleation, agglomeration, shape, size, and phase transformation was investigated. Initially the variation of pH from 1 to 11 was systematically studied at different temperatures (25-700oC). The morphological differences as a function of pH were studied in detail. A temperature of 400oC was considered best for crystalline growth while a pH value of 4 gave round and well dispersed TiO2 with a shape factor of >0.9. From the data generated it is obvious that with an increase in pH there is a decrease in agglomeration and increase in dispersion and vice versa. Stable titania suspensions were fabricated by controlling the synthesis solution chemistry. Titanium trichloride and tetrachloride were used to fabricate NPs at room or near room temperature. Different alcohols and alcohol water ratios helped to control the NPs morphology at room or very low temperatures. TiCl4 was evaluated as the best precursor in controlling shape and size in low temperature synthesis processes. Various shapes of TiO2 including spherical NPs with shape factor of 0.9 or more, nanocubes, nanorods and ellipsoids were synthesised with different alcohols and water mixture ratios. In the next phase a couple of synthesized NPs were checked for their stability with 5 different surfactants; PEG, PVP, SDS, SRFA and sodium citrate. The stability of anatase spherical attenuated as sodium citrate, SRFA, PVP, PEG and SDS while this attenuation was SRFA, sodium citrate, PEG, SDS and PVP for rutile ellipsoids. SRFA and sodium citrate at 0.3% weight concentration proved to be the best stabilising agents without any change in the hydrodynamic diameter over a period of 2 weeks. These two types of NPs stabilized with two different types of surfactants i.e. SRFA and sodium citrate were further used for aggregation kinetics and transport studies through natural and artificial porous media. The aggregation kinetic studies showed that rutile ellipsoids behaved well against different mono and divalent ii cations. The critical coagulation concentrations (CCC’s) observed for sodium citrate stabilized NMs were significantly higher than SRFA stabilized NMs, showing that sodium citrate is a better stabilizing agent than SRFA. TEM analysis of aggregated samples in slow and fast regime of aggregation showed different morphologies of aggregates which were analysed with fractal dimension analysis. Most of the aggregating salts gave a fractal dimension of more than 1.5 which means presence of consolidated aggregates after addition of different salts. In the last phase the stabilized NMs with SRFA and sodium citrate were studied for porous media column transport by using glass bead as an artificial and sandstone as more complex natural environmental media. The transport of the rutile ellipsoids is greater than spherical anatase. Bare anatase NPs gave no breakthrough and the NPs clogged both the sandstone and glass bead columns; while bare rutile ellipsoids gave nearly 100% breakthrough curves. In most of the cases for glass beads the C’/Co values remained above 80% and after retention NPs release gave more than 80% of retained NPs. Only 40% or less NPs were released from sandstone columns and rest of injected NPs were retained within the columns. For both sandstone and glass bead media SRFA proved a better flushing agent than sodium citrate. Stabilized anatase showed no difference in mobility as compared to stabilized rutile but bare rutile NPs behaved entirely different from bare anatase. Bare anatase showed difficulty in movement through both sandstone and glass bead media. Both stabilizers i.e. have different effects on mobility of nanomaterials as SRFA gave steric while sodium citrate gave electrostatic stabilization. Tailing was seen in all runs and it is more physical in glass bead followed by sandstone columns while a little tailing is seen in fluorescein. This tailing behaviour shows probably a non-equilibrium attachment process which suggests that colloid filtration theory (CFT) not likely to be correct. The total release in case of glass bead columns was nearly 100% which was much greater than the total release from sandstone columns. Only iii 40% or less NPs were released from sandstone columns and rest of injected NPs were retained within the columns. From overall experimental results it is concluded that glass bead columns are analogous to sandstone columns, in style, though not in degree. So it is encouraging for laboratory experimentation. More release of NPs with SRFA flush is also important as it reflects the ultimate fate and behaviour of TiO2 NPs in natural environment which is rich in humic substances. iv Dedication I dedicate this study to my son, Muhammad Hassan Raza and my daughter, Pakiza Raza v Acknowledgements I would like to take this opportunity to acknowledge the people who have been tremendously helpful, patient and kind during this exciting journey of my second PhD. To my advisors, Professor Jamie Lead and Eva Valsami Jones, I would like to express my sincerest thanks for their unwavering support: this thesis would simply not have been possible without their assistance. A special thank you is due to my co-supervisors, Professor John Tellam and Dr Mohammed Baalousha, for their guidance and technical support during my laboratory work and the writing up of this dissertation. Thank you to my colleagues, Dr. Yusuf Nur, Dr. Mila Tejamaya, Indrani Mahapatra, Inder Kaur, Dr. Auwal Farouk Abdussalam and Isaac Aidoo for their help, moral support, and above all, friendship. To Hasan Shikoh, I extend my most sincere gratitude for being there for me when I needed it most: his kind words and constructive criticism will forever be appreciated. I am grateful to the National Environmental Research Council (NERC), United Kingdom and Natural History Museum (NHM) London, for funding my PhD research project. I would like to thank my extended family, especially my parents, for continuously reminding me that the journey towards my PhD was indeed worth it. I pray for their good health and long vi life because the foundations of my achievements to date are a direct result of their ardent prayers and guidance. Finally, I would like to thank my beloved wife, Sobia Raza, my son, Muhammad Hassan Raza, and daughter, Pakiza Raza, for their unconditional love and support. I could not possibly have reached this landmark without their continuous patience and encouragement throughout my research. On occasions, when I felt it was too difficult to continue, it was only their love and the sparkle in their eyes which helped me carry on with renewed zest to achieve this success. vii Table
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