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Study of Phosphorus Behaviour in Levitated Silicon-Iron Droplets

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Study of Phosphorus Behaviour in Levitated Silicon-Iron Droplets STUDY OF PHOSPHORUS BEHAVIOUR IN LEVITATED SILICON-IRON DROPLETS by Katherine Le A thesis submitted in conformity with the requirements for the degree of Master of Applied Science Department of Materials Science and Engineering University of Toronto © Copyright by Katherine Le 2016 ii Study of Phosphorus Behaviour in Levitated Si-Fe Droplets Katherine Le Master of Applied Science Department of Materials Science and Engineering University of Toronto 2016 Abstract While the treatment of relatively inexpensive ferrosilicon alloys is a potential refining route in order to generate solar grade silicon, phosphorus is one of the more difficult impurities to remove by conventional processing. In this project, electromagnetic levitation was used to investigate the dephosphorization of ferrosilicon alloy droplets exposed to H2-Ar gas mixtures under various experimental conditions including, refining time, temperature (1450°C-1720°C), H2-Ar gas concentrations and flow rate, iron alloying content, and initial phosphorus concentration. Reaction rates increased with higher refining times, temperatures, and H2 gas concentrations. With unknown parameters associated with the kinetics of gas phase reactions, the approach involved comparison of apparent activation energies derived for the chemical reaction and gas diffusion steps of the dephosphorization process. The phosphorus removal rate is thought to be controlled by the interfacial reaction step; further work is required to confirm this conclusion. iii Acknowledgements I would like to express my gratitude and respect to my supervisor, Prof. Alex McLean for the opportunity to work on this research. I am thankful for his guidance, wisdom and encouragement throughout the course of my studies. He is a truly inspiring person, and a great enabler of new learning opportunities. I would like to thank Prof. Mansoor Barati for all his support and kindness. His recommendations and advice allowed me to further explore and analyze the significance of my results, and to attain the overall findings reported in this thesis. I would also like to express my thanks to Dr. Yindong Yang for his unwavering support and constructive input over the course of this thesis, and during my time as an undergraduate in the research group. His knowledge and perspectives in research and industry have been a great source of encouragement and inspiration. A special thank you to Dr. Paul Wu, for his mentorship in this project. I am indebted to him for his valuable advice, and always being available to share his knowledge and perspectives in research. I would also like to thank past co-investigators on this project, Dr. Wei Yan and Andrew Hue. I would like to thank Dr. Hiroshi Soda for his advice and wonderful stories. I am also grateful for my colleagues at U of T who have contributed to this work whether it be through experimental preparations and analysis, discussions, suggestions, and support: Dr. Karim Danaei, Sridevi Thomas, Dr. Sherry Esfahani, Dr. Leili Tafaghodikhajavi, Dr. Dawei Yu, Xue Yin, Bennett Yan, Richard Elliott, and Kevin Yu. Financial assistance from the Natural Science and Engineering Research Council of Canada, the Ontario Graduate Scholarship, and the Department of Materials Science and Engineering at the University of Toronto is gratefully acknowledged. I am thankful for my family and friends for their unending encouragement and moral support. To my siblings, Helen and David for their patience and reassurance. Finally, to my loving parents who have taught me the values of hard work, discipline, perseverance, and importance of lifelong learning. iv TABLE OF CONTENTS Abstract ........................................................................................................................................................ ii Acknowledgements .................................................................................................................................... iii CHAPTER 1 ................................................................................................................................................ 1 Introduction ................................................................................................................................................. 1 References ............................................................................................................................................. 3 CHAPTER 2 ................................................................................................................................................ 4 Background for Proposed Research .......................................................................................................... 4 2.1 Silicon ............................................................................................................................................. 5 2.2 Solar Grade Silicon Production ....................................................................................................... 8 2.3 Thermodynamics of Phosphorus in Molten Silicon Alloy Systems ............................................. 20 2.4 Kinetics of Phosphorus Removal from Molten Silicon Alloys ..................................................... 22 References ........................................................................................................................................... 24 CHAPTER 3 .............................................................................................................................................. 26 Electromagnetic Levitation ...................................................................................................................... 26 3.1 Principle ........................................................................................................................................ 26 3.2 Review of Experimental Aspects of Levitation Melting ............................................................... 27 3.3 Applications of the Levitation Technique ..................................................................................... 31 3.4 Advantages of Levitation Melting ................................................................................................ 37 3.5 Disadvantages of Levitation Melting ............................................................................................ 38 3.6 Proposed Metallurgical Refining Route ........................................................................................ 39 References ........................................................................................................................................... 41 CHAPTER 4 .............................................................................................................................................. 44 Experimental Considerations................................................................................................................... 44 4.1 Electromagnetic Levitation Apparatus .......................................................................................... 44 4.2 Materials ....................................................................................................................................... 48 4.3 Chemical Analysis of Samples: Inductively Coupled Plasma-Optical Emission Spectrometry (ICP-OES) ........................................................................................................................................... 50 References ........................................................................................................................................... 52 v CHAPTER 5 .............................................................................................................................................. 53 Results and Discussion .............................................................................................................................. 53 5.1 Experimental Results .................................................................................................................... 53 5.2 Dephosphorization of Levitated Si-Fe Droplets in H2-Ar gas: Effect of Process Variables ......... 55 5.3 Thermodynamic Study of Si-Fe Dephosphorization under Reducing Gas Atmosphere: FactSage Study ................................................................................................................................................... 59 5.4 Kinetic Study of Phosphorus Evaporation from Si-Fe Droplets ................................................... 65 References ........................................................................................................................................... 77 CHAPTER 6 .............................................................................................................................................. 78 Conclusions and Future Work ................................................................................................................. 78 6.1 Conclusions ................................................................................................................................... 78 6.2 Future Work .................................................................................................................................. 79 Appendix A FactSage Equilibrium Reaction Products ........................................................................ 80 A.1 Si-Fe-P System – Pure Components ...........................................................................................
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