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Optimization of Molybdenum Electrodes for Glass Melting

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Optimization of Molybdenum Electrodes for Glass Melting Optimization of Molybdenum Electrodes for Glass Melting by WenDi Liu A Dissertation Submitted to the Faculty of WORCESTER POLYTECHNIC INSTITUTE In partial fulfillment of the requirements of the Degree of Doctor of Philosophy in Materials Science and Engineering April 2015 APPROVED: _______________________________ Dr. Diran Apelian, Advisor Alcoa-Howmet Professor of Engineering _______________________________ Dr. Richard D. Sisson Jr. Director of Manufacturing and Materials Engineering George F. Fuller Professor ABSTRACT The U.S. glass industry is a $28 billion enterprise and millions of tons of glasses are melted each day by different heating techniques, such as conventional oil fired furnaces or via electrical heating. The share of electrical heating is bound to rise steadily because it is cleaner and more energy efficient. Due to this situation molybdenum will play a significant role in electrical glass melting, since it is the most frequently used electrode material to deliver the electricity into the glass melts. Although it has a high melting point, high electrical and thermal conductivity and a low coefficient of expansion, molybdenum electrodes fail because of lack of sustainability during the glass melting process. Melt reaction with electrodes is the fundamental barrier to higher melting temperatures. Glass manufacturers have suggested that the need for better performance of molybdenum electrodes will see a rapid advancement in the use of electric heating system in the U.S. This work first focused on post-mortem analysis on used molybdenum electrodes with and without the current load in order to establish failure mechanisms for molybdenum during glass melting. It was determined that service life of molybdenum electrodes are limited by poor oxidation and corrosion resistance of molybdenum with redox reactions. Various studies have shown that the failure mode for molybdenum electrodes is a complex phenomenon. It depends on chemical composition of the electrode, current density and frequency, and chemical composition of the glass melt, specifically polyvalent ions that may be present in the melt. In this work, the MoSiB coating was validated as a promising protection for molybdenum from oxidation attack. Several molybdenum and molybdenum based-alloy electrodes were tested in different molten glasses in the remelter furnace to optimize the structural characteristics that are needed in Mo electrodes. Moreover, the quantitative data and fundamental knowledge gained in this work is being applied for molybdenum electrode production to extend its service life and also improve its quality. I ACKNOWLEDGMENTS First and foremost I want to express my sincere gratitude to my advisor, Professor Diran Apelian for his outstanding guidance, enthusiasm, and patience during my research and study. As my mentor, he has not only advised me to think out of the box in my thesis, but also inspired me to have a big picture perspective in my career path. My heartily thanks go to my thesis committee members Professor Richard D. Sisson Jr., Professor Jianyu Liang, Assistant Professor Yan Wang, Mr. Paul Aimone, Dr. Francois Dary and Dr. Marc Abouaf for their encouragement, critical comments and stimulating questions. My PhD project was financially supported by H.C. Starck, Inc. I would also like to thank my supervisor, Mr. Paul Aimone for his absolute help and continuous support. His input has been invaluable to this project and is gratefully acknowledged. The hospitality of H.C. Starck during my internship is very much appreciated. Special thanks go to Anne Coyle, Joao Depina, and Eileen Ricigliano for their assistance and collaboration. I had the opportunity and pleasure to visit Professor Perepezko and his research group at University of Wisconsin–Madison; I thank him for sharing his knowledge with me. I am also grateful to Tom Loretz from CES, Inc. for his support and assistance on the construction and operation of the remelter furnace. My friends and colleagues at WPI and at H.C. Starck made my PhD years an enjoyable experience and a wonderful journey. Dr. Boquan Li deserves a special thank for his assistance in experiments and invaluable discussions. I would also like to take the opportunity to thank Dr. Libo Wang, Patrick Hogan and Yang Mei for their support. I also greatly appreciate our department secretary, Rita Shilansky and MPI staff Carol Garofoli, Renée Brodeur and Maureen Plunkett for their constant assistance. Your support facilitated my work in all aspects. Finally, I owe my deepest gratitude to my parents, Hanhua Liu and Fengfang Zhang and my wife, Xiaochen Liu who supported me throughout these years and her constant faith in me. Thank you for standing beside me all these times; this work would not have been done without your love and belief. II TABLE OF CONTENTS ABSTRACT ....................................................................................................................................................... I ACKNOWLEDGMENTS ................................................................................................................................... II TABLE OF CONTENTS .................................................................................................................................... III 1. Introduction .......................................................................................................................................... 5 1.1. Glass .............................................................................................................................................. 5 1.2. Glass Melting ................................................................................................................................. 5 1.3. Molybdenum Electrodes ............................................................................................................... 6 1.3.1. Oxidation Resistance ............................................................................................................. 7 1.3.2. Corrosion Resistance ............................................................................................................. 7 1.4. Solution Pathways to Improve GME Performance ....................................................................... 9 2. Objectives ........................................................................................................................................... 10 3. Failure Mechanisms in Molybdenum (Mo) Electrodes ....................................................................... 11 3.1. Background ................................................................................................................................. 11 3.2. Examination Results and Discussions ......................................................................................... 11 3.2.1. Commercial Electrodes from Glass Industry ....................................................................... 11 3.2.2. Molybdenum Electrodes Tested in the Laboratory Furnace .............................................. 20 3.3. Conclusions ................................................................................................................................. 23 4. Hypothesis for the Failure of Molybdenum Electrodes Used in Melting Glass .................................. 25 5. Approach and Experimental Procedure.............................................................................................. 29 5.1. Oxidation Resistant Coating Development ................................................................................. 29 5.2. Oxidation Tests on the Coated Molybdenum ............................................................................. 31 5.3. Comparison Corrosion Tests ....................................................................................................... 33 5.3.1. Build-up of the remelter furnace ........................................................................................ 33 5.3.2. The Choice of Glass Melts ................................................................................................... 35 5.3.3. Corrosion Tests on Glass Melting Electrodes ...................................................................... 36 6. Results ................................................................................................................................................. 39 6.1. Oxidation Behavior of Coated Molybdenum .............................................................................. 39 6.1.1. Oxidation Resistant Mo-Si-B-Based Coating ....................................................................... 39 III 6.1.2. Oxidation Behavior of Coated Pure Molybdenum Samples ............................................... 52 6.1.3. The scale-up of the MoSiB Coating for Glass Melting Electrode (GME) ............................. 56 6.2. Corrosion of GMEs ...................................................................................................................... 58 6.2.1. The Corrosion Tests on Pure Molybdenum Electrodes ...................................................... 58 6.2.2. The Comparison Corrosion Tests on Molybdenum and Molybdenum-based Alloy Electrodes ........................................................................................................................................... 68 7. Discussion ..........................................................................................................................................
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