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Flux Growth and Physical Properties of Rare Earth Aluminides and Tetrelides Xiaowei Ma

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Flux Growth and Physical Properties of Rare Earth Aluminides and Tetrelides Xiaowei Ma Florida State University Libraries Electronic Theses, Treatises and Dissertations The Graduate School 2013 Flux Growth and Physical Properties of Rare Earth Aluminides and Tetrelides Xiaowei Ma Follow this and additional works at the FSU Digital Library. For more information, please contact [email protected] FLORIDA STATE UNIVERSITY COLLEGE OF ARTS AND SCIENCES FLUX GROWTH AND PHYSICAL PROPERTIES OF RARE EARTH ALUMINIDES AND TETRELIDES By XIAOWEI MA A Dissertation submitted to the Department of Chemistry and Biochemistry in partial fulfillment of the requirements for the degree of Doctor of Philosophy Degree Awarded: Fall Semester, 2013 Xiaowei Ma defended this dissertation on September 24, 2013. The members of the supervisory committee were: Susan Latturner Professor Directing Dissertation David Lind University Representative Naresh Dalal Committee Member Michael Shatruk Committee Member The Graduate School has verified and approved the above-named committee members, and certifies that the Dissertation has been approved in accordance with university requirements. ii ACKNOWLEDGMENTS I would like to express my deepest gratitude to my advisor, Dr. Susan Latturner, for giving me the opportunity to join her group and leading me to the field of solid state chemistry. Without her excellent guidance, I would never have been able to finish my dissertation. Over the past five years, I really appreciate her kindly effort in directing me to obtain the research philosophy with warmhearted encouragement. She has been so generous to pass her broad knowledge and scientific attitude to me. She is not only a magnificent mentor but a good friend to provide personal support. I would also like to thank my committee members Dr. Shatruk, Dr. Dalal and Dr. Lind for their scientific guidance on my research. Dr. Shatruk always helped me to solve the hard problems especially concerning magnetic and electronic studies. Dr. Dalal and Dr. Lind also provided many important suggestions. I am also grateful to Dr. Lochner for kindly training me to use a lot of physical instruments. Additional thanks should be given to other members in Dr. Latturner's group, in particular, Dr. Whalen and Dr. Josiah, who provided their useful help at the beginning I joined the group. In addition, Dr. Chai, a postdoctoral associate in Dr. Shatruk's group, has taught me the electronic structure calculation. Finally, I want to thank my parents and my wife, Ling Wang, for their significant support during my graduate study. iii TABLE OF CONTENTS List of Tables ............................................................................................................................... viii List of Figures ..................................................................................................................................x Abstract ........................................................................................................................................ xvi 1. INTRODUCTION ...................................................................................................................1 1.1 Intermetallics and Their Applications ............................................................................1 1.2 Rare Earth Zintl Phases ..................................................................................................3 1.3 Flux Synthesis of Rare Earth Intermetallics ..................................................................4 1.4 Magnesium-based Binary Fluxes ...................................................................................5 2. EXPERIMENTAL TECHNIQUES ........................................................................................7 2.1 Synthesis Description.....................................................................................................7 2.2 Elemental Analysis ........................................................................................................8 2.3 Structure Determination .................................................................................................9 2.3.1 Powder and Single Crystal X-ray Diffraction ..................................................10 2.3.2 Single Crystal Neutron Diffraction ..................................................................11 2.4 Solid State 27Al and 29Si NMR.....................................................................................11 2.5 Thermal Analysis .........................................................................................................12 2.6 Magnetic Susceptibility ...............................................................................................12 2.7 Electrical Resistivity ....................................................................................................13 2.8 Heat Capacity ...............................................................................................................13 2.9 Electronic Structure Calculations ................................................................................14 3. SYNTHESIS AND PROPERTIES OF NEW MULTINARY SILICIDES R5(Mg/Al)5Fe4(Al/Si)18 (R=Gd, Dy, Y) GROWN IN Mg/Al FLUX ............................................15 3.1 Introduction ..................................................................................................................15 3.2 Experimental Procedure ...............................................................................................16 3.2.1 Synthesis ..........................................................................................................16 3.2.2 Elemental Analysis ..........................................................................................16 3.2.3 Powder and Single Crystal X-ray Diffraction ..................................................18 3.2.4 Single Crystal Neutron Diffraction ..................................................................18 3.2.5 Electronic Structure Calculations ....................................................................22 3.2.6 Magnetic Susceptibility ...................................................................................23 3.2.7 Solid State NMR Characterization...................................................................23 3.2.8 Electrical Resistivity ........................................................................................23 3.2.9 Heat Capacity ...................................................................................................23 3.3 Results and Discussion ................................................................................................24 3.3.1 Synthesis ..........................................................................................................24 3.3.2 Structure ...........................................................................................................25 3.3.3 Electronic Structure Calculations ....................................................................32 3.3.4 Magnetic Behavior ...........................................................................................36 3.3.5 Electrical Resistivity ........................................................................................39 3.4 Conclusion ...................................................................................................................41 iv 4. COMPETING PHASES, COMPLEX STRUCTURE, AND COMPLEMENTARY DIFFRACTION STUDIES OF R3FeAl4-xMgxTt2 INTERMETALLICS (R=Y, Dy, Er, Yb; Tt=Si OR Ge; x<0.5) ................................................................................................................................42 4.1 Introduction ..................................................................................................................42 4.2 Experimental Methods .................................................................................................43 4.2.1 Synthesis ..........................................................................................................43 4.2.2 Elemental Analysis ..........................................................................................44 4.2.3 X-ray Diffraction .............................................................................................45 4.2.4 Neutron Diffraction ..........................................................................................49 4.2.5 X-ray Photoelectron Spectroscopy ..................................................................50 4.2.6 Electronic Structure Calculations ....................................................................51 4.2.7 Magnetic Properties .........................................................................................51 4.3 Results and Discussion ................................................................................................52 4.3.1 Synthesis ..........................................................................................................52 4.3.2 Structure ...........................................................................................................55 4.3.3 Electronic Structure Calculations ....................................................................60 4.3.4 Magnetic Properties .........................................................................................63 4.4 Conclusion ...................................................................................................................67 5. Mg/Al FLUX GROWTH AND PROPERTIES OF M5+xMg18-xTt13 PHASES (M = Eu, Ba/Sr; Tt = Si, Ge) .........................................................................................................................68
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