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Combined Dilatometry and Mass Spectrometry of Sintering And COMBINED DILATOMETRY AND MASS SPECTROMETRY OF SINTERING AND EVOLVED GASES OF BARIUM TITANATE AND ZIRCONIUM DIBORIDE WITH SINTERING ADDITIVES _______________________________________ A Thesis presented to the Faculty of the Graduate School University of Missouri _______________________________________ In Partial Fulfillment Of the Requirements for the Degree Master of Science _______________________________________ by MURRAY MOSS Dr. Stephen J. Lombardo, Thesis Supervisor DECEMBER 2012 The undersigned, Appointed by the Dean of the Graduate School, have examined the thesis entitled COMBINED DILATOMETRY AND MASS SPECTROMETRY OF SINTERING AND EVOLVED GASES OF BARIUM TITANATE AND ZIRCONIUM DIBORIDE WITH SINTERING ADDITIVES Presented by Murray Moss A candidate for the degree of Master of Science And hereby certify that in their opinion it is worth of acceptance. Dr. Stephen J. Lombardo _____________________________________________ Dr. David Retzloff _____________________________________________ Dr. Alan Whittington _____________________________________________ ACKNOWLEDGEMENTS I would like to first thank Dr. Stephen J. Lombardo for giving me the opportunity to work in his lab and for all the time he has spent with me on this project. Dr. Lombardo has been all that a teacher and mentor should be: an invaluable source of knowledge, one which motivates and challenges you to grow, all the while showing enormous patience. I really appreciate all you have done for me and wish you success in the future. Secondly, I would like to thank the GAANN (Graduate Assistantship in Areas of National Need) Fellowship for financial support for both myself and the lab, and for the opportunity to meet other professionals by attending conferences. I would also like to thank my Thesis Committee members Dr. Retzloff and Dr. Whittington for their time and input in the process of finishing this thesis. I also would not have been able to finish this without the help of the staff from the Chemical Engineering Department, specifically Rita Preckshot and Jennifer Keyzer-Andre, and the Engineering Technical Services electrician Rich Oberto. A big thank you is also necessary to fellow graduate assistants Matt Schurwanz, Brandon Abeln, Ki-Yong Lee, Mojtaba Asadirad, and Jun Oh, and all of the previous graduate assistants who have worked for Dr. Lombardo and set the foundation for this work, especially Kai Feng, Chang Soo Kim, and Jeong Woo Yun. Finally I would like to thank my beautiful wife Danielle for all of her love and dedication during my work. Our families have also been very supportive, for which I am very grateful. ii TABLE OF CONTENTS ACKNOWLEDGEMENTS ................................................................................................ ii LIST OF FIGURES ........................................................................................................... vi LIST OF TABLES ...............................................................................................................x ABSTRACT ...................................................................................................................... xii CHAPTERS 1. INTRODUCTION ................................................................................................1 1.1 General Background .......................................................................................2 1.2 Analysis Techniques .......................................................................................6 1.3 Motivation, Objective, and Thesis Organization ............................................8 1.4 References .....................................................................................................11 2. EXPERIMENTAL AND SYSTEM DETAILS ..................................................15 2.1 Introduction ...................................................................................................16 2.1.1 System Overview .................................................................................16 2.2 System Details ..............................................................................................17 2.2.1 Coolant Flow Paths ..............................................................................17 2.2.2 Gas Flow Paths ....................................................................................18 2.2.3 Dilatometer ..........................................................................................20 2.2.4 Furnace .................................................................................................21 2.2.5 Mass Spectrometer ...............................................................................26 2.3 Improvements ...............................................................................................27 2.4 Procedure ......................................................................................................28 2.5 References .....................................................................................................33 iii 3. EVOLVED GAS ANALYSIS OF BARIUM TITANATE, BARIUM CARBONATE, AND BARIUM SULFATE, WITH BACKGROUND CHEMISTRY OF THE CDMS .................................................................34 3.1 Introduction ...................................................................................................35 3.2 Experimental .................................................................................................37 3.3 Results ...........................................................................................................40 3.3.1 Inert Conditioning Heating Cycle ........................................................40 3.3.2 Background Heating Cycle ..................................................................44 3.3.3 Barium Sulfate .....................................................................................46 3.3.4 Barium Carbonate ................................................................................50 3.3.5 Barium Titanate Heated at 14°C/min ...................................................53 3.3.6 Barium Titanate Heated at 8°C/min .....................................................61 3.3.7 Barium Titanate Heated at 20°C/min ...................................................64 3.3.8 Loose Barium Titanate Heated at 14°C/min ........................................66 3.4 Discussion .....................................................................................................69 3.5 Conclusions ...................................................................................................70 3.6 References .....................................................................................................72 4. HIGH TEMPERATURE CHEMISTRY OF ZIRCONIUM DIBORIDE AND SINTERING ADDITIVES ........................................................................74 4.1 Introduction ...................................................................................................75 4.2 Experimental .................................................................................................78 4.3 Results ...........................................................................................................80 4.3.1 Boron Oxide .........................................................................................80 4.3.2 Boron Nitride Spray .............................................................................82 4.3.3 Zirconium Diboride .............................................................................86 iv 4.3.4 Boron Carbide ......................................................................................91 4.3.5 Silicon Carbide.....................................................................................93 4.3.6 Zirconium Oxide ..................................................................................95 4.4 Discussion .....................................................................................................98 4.5 Conclusions ...................................................................................................99 4.6 References ...................................................................................................100 5. HIGH TEMPERATURE CHEMISTRY DURING THE HEATING OF MIXTURES OF ULTRA-HIGH TEMPERATURE MATERIALS .......103 5.1 Introduction .................................................................................................104 5.2 Experimental ...............................................................................................107 5.3 Results .........................................................................................................110 5.3.1 Phenolic Resin ...................................................................................110 5.3.2 ZrO2-B4C............................................................................................114 5.3.3 ZrB2-B4C-PR......................................................................................118 5.3.4 ZrB2-SiC-B4C-PR-B-D-S ..................................................................121 5.3.5 ZrB2-5-ZrSi2 .......................................................................................125 5.3.6 ZrB2-10-ZrSi2 .....................................................................................128 5.3.7 ZrB2-20-ZrSi2 .....................................................................................129 5.4 Discussion ...................................................................................................132 5.5 Conclusions
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