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Metallurgical Grade Silicon (MG-Si), Via Carbothermic Reduction

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Metallurgical Grade Silicon (MG-Si), Via Carbothermic Reduction Engineering Impurity Behavior on the Micron-Scale in Metallurgical-Grade Silicon Production By Sarah Bernardis B.S./M.S. Physics Università degli Studi di Padova, 2005 M.S. Materials Science and Engineering Massachusetts Institute of Technology, 2008 Submitted to the Department of Materials Science and Engineering in Partial Fulfillment of the Requirements for the Degree of Doctor of Philosophy in Materials Science and Engineering at the Massachusetts Institute of Technology February 2012 © 2012 Massachusetts Institute of Technology. All rights reserved. Signature of Author:_____________________________________________________________ Department of Materials Science and Engineering Certified by:___________________________________________________________________ Kenneth C. Russell Professor Emeritus of Metallurgy and Nuclear Engineering Thesis Supervisor Accepted by: __________________________________________________________________ Christopher Schuh Chair, Departmental Committee on Graduate Students - 2 - Engineering Impurity Behavior on the Micron-Scale in Metallurgical-Grade Silicon Production By Sarah Bernardis Submitted to the Department of Materials Science and Engineering on October 15th, 2012 in Partial Fulfillment of the Requirements for the Degree of Doctor of Philosophy in Materials Science and Engineering Abstract Impurities are detrimental to silicon-based solar cells. A deeper understanding of their evolution, microscopic distributions, and oxidation states throughout the refining processes may enable the discovery of novel refining techniques. Using synchrotron-based microprobe techniques and bulk chemical analyses, we investigate Fe, Ti, and Ca starting from silicon- and carbon bearing raw feedstock materials to metallurgical grade silicon (MG-Si), via carbothermic reduction. Before reduction, impurities are present in distinct micron- or sub-micron-sized minerals, frequently located at structural defects in Si-bearing compounds. Chemical states vary, they are generally oxidized (e.g., Fe2+, Fe3+). Impurity concentrations are directly correlated to the geological type of quartz: pegmatitic and hydrothermal quartz have fewer impurities than quartzite. Particles containing Cr, Mn, Fe, Ni, Cu, K, and/or Zn are also detected. In carbon- bearing compounds, Ca typically follows wood veins. In wood, Fe and Ti are diffused uniformly. In contrast, charcoal samples can contain particles of Fe, Ti, and/or Ca. The overall impurity content in the pine charcoal sample is higher than in the pine woodchip, suggesting that the charcoalization process introduces unintentional contamination. During reduction, silica evolution is analyzed in parallel to Fe. Fe is predominantly clustered in minerals which influence its oxidation state. Here, Fe is embedded in muscovite with predominance of Fe3+. Initially, Fe is affected by the decomposition of muscovite and it is found as Fe2+; as muscovite disappears, Fe diffuses in the molten silica, segregating towards interfaces. Contrary to thermodynamic expectation, Fe is oxidized until late in the reduction process as the silica melt protects it from gases present in the furnace, hence minimizing its reduction, only partially measured at high temperatures. After reduction, the initial low- to sub- ppmw concentrations measured in the precursor quartz increase drastically in the MG-Si. The refining process is responsible for the increased contamination. Yet, most impurities are clustered at grain boundaries and a leaching process could remove them. - 3 - Electrical fragmentation and a leaching treatment are tested as a method to expose grain boundaries of “dirty” quartzite and to remove impurities. The selective fragmentation proves to be a very important step in removing impurities via leaching. Thesis Supervisor: Kenneth C. Russell Title: Professor Emeritus of Metallurgy and Nuclear Engineering - 4 - Acknowledgments I crossed the finish line thanks to a handful of professors I had the luck to meet and to collaborate with throughout the last years. In chronological order: Sam Allen made me discover the beauty of the world of kinetics as well as dedicated his time to improve my graduate student experience. Ken Russell inspired me by always pointing out the most important scientific aspects and by providing broader perspectives. Tonio Buonassisi suggested and motivated this research; his contributions and scientific insights were invaluable. Marisa Di Sabatino drastically changed my life by inviting me to perform experiments with her. This thesis would have been very different without her long term vision, passion, and persistence. Merete Tangstad was always available to discuss anything from furnace thermodynamics to possible funding miracles. Her perspective both on life and the PhD experience should be written for the next generations of students. Rune Larsen, my quartz guru, without his expertise, quartz would have been a cryptic feedstock material rather than an amazing mineral. I feel deeply indebted to Dean Blance Staton. She has been extremely supportive and always suggested brilliant solutions to colorful situations. Her wisdom and experience were irreplaceable. To the MIT Glass Lab and to my close friends, their humor and support, infinite chats, and the many evenings spent together, Martina Poletti, Riccardo Pedersini, Anna Custo, Gabriele & Miriam Vanoni, Andrea Allais, Linda Valeri, Jon Gibbs, Mike Tarkanian, and Dana Shemuly. A special thank you to my sister Elena, always present and supportive. You know I really mean it. To all of you, my everlasting gratitude. - 5 - - 6 - Contents Abstract ....................................................................................................................................... - 3 - Acknowledgments....................................................................................................................... - 5 - Contents ...................................................................................................................................... - 7 - List of Figures ........................................................................................................................... - 11 - List of Tables ............................................................................................................................ - 14 - 1. Introduction ....................................................................................................................... - 15 - 1.1. Motivation .................................................................................................................. - 15 - 1.1.1. Selected Impurities: Fe, Ti, and Ca ..................................................................... - 17 - 1.2. Carbothermic Reduction ............................................................................................ - 18 - 1.3. Silica and Trace Elements during Carbothermic Reduction ...................................... - 19 - 1.3.1. Before Carbothermic Reduction ......................................................................... - 20 - 1.3.2. During Carbothermic Reduction ......................................................................... - 22 - 1.3.3. After Carbothermic Reduction ............................................................................ - 26 - 1.4. Scope and Structure of this Thesis ............................................................................. - 26 - 1.4.1. Process Description ............................................................................................. - 27 - 1.4.2. Process Development .......................................................................................... - 27 - 2. Characterization Methods .................................................................................................. - 29 - 2.1. Quartz Section Preparation ......................................................................................... - 29 - 2.2. Microscopy ................................................................................................................. - 30 - 2.2.1. Optical Microscopy ............................................................................................. - 30 - 2.2.2. Scanning Electron Microscopy ........................................................................... - 30 - 2.2.3. Electron Probe Micro-Analyzer .......................................................................... - 31 - 2.2.4. Synchrotron Based X-ray Fluorescence.............................................................. - 31 - 2.3. Spectroscopy .............................................................................................................. - 34 - 2.3.1. X-Ray Near Edge Absorption Structure ............................................................. - 34 - 2.3.2. Fourier Transform Infrared Spectroscopy .......................................................... - 35 - - 7 - 2.4. X-ray Diffraction ........................................................................................................ - 35 - 2.5. Bulk Concentration Analysis ..................................................................................... - 36 - 2.5.1. Inductively Coupled Plasma Mass Spectrometry ............................................... - 36 - 2.5.2. Glow Discharge Mass Spectrometry .................................................................. - 37 - 3. Before Carbothermic Reduction: Raw Feedstock Materials ............................................. - 39 - 3.1. Raw Feedstock Materials
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