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Flux Synthesis of Zintl Phases and Feas Related Intermetallics Josiah Mathieu

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Flux Synthesis of Zintl Phases and Feas Related Intermetallics Josiah Mathieu Florida State University Libraries Electronic Theses, Treatises and Dissertations The Graduate School 2013 Flux Synthesis of Zintl Phases and FeAs Related Intermetallics Josiah Mathieu Follow this and additional works at the FSU Digital Library. For more information, please contact [email protected] THE FLORIDA STATE UNIVERSITY COLLEGE OF ARTS AND SCIENCES FLUX SYNTHESIS OF ZINTL PHASES AND FeAs RELATED INTERMETALLICS By JOSIAH MATHIEU 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 Josiah Mathieu defended this dissertation on August 13th, 2013 The members of the supervisory committee were: Susan Latturner Professor Directing Dissertation Eric Hellstrom University Representative Naresh Dalal Committee Member Oliver Steinbock 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 ACKNOWLEDGEMENTS I would like to thank Dr. Latturner for the opportunity to work in her lab and pursue my interests in solid state chemistry. It has been everything I hoped if not more. I also appreciate the opportunity to have made a small contribution to the field of superconductivity, which is where my interest in the solid state came from originally. I would also like to thank Dr. Evan Benbow and Dr. Milorad Stojanovic for the numerous consultations about my work, as well as the time they spent training me on all the instrumentation necessary for it. Lastly, I would like to thank the rest of the Latturner group for their support. iii TABLE OF CONTENTS List of Tables ................................................................................................................................. vi List of Figures ............................................................................................................................... vii Abstract .......................................................................................................................................... ix 1. INTRODUCTION: METAL FLUX SYNTHESIS AND ZINTL PHASES ...........................1 2. THEORETICAL AND TECHNICAL BACKGROUND FOR CHARACTERIZATION TECHNIQUES OF SOLID STATE MATERIALS USED IN THIS WORK ........................7 2.1 Scanning Electron Microscopy and Energy Dispersive Spectroscopy ..........................7 2.2 X-ray Diffraction ...........................................................................................................9 2.3 Heat Capacity Measurements and Thermal Excitation Processes in Solids ................12 2.4 Electrical Measurements ..............................................................................................18 2.5 Magnetic Measurements ..............................................................................................21 2.6 Nuclear Magnetic Resonance Spectroscopy ................................................................26 3. FLUX GROWTH AND ELECTRONIC PROPERTIES OF Ba2In5Pn5 (Pn = P, As): ZINTL PHASES EXHIBITING METALLIC BEHAVIOR ...........................38 3.1 Introduction ..................................................................................................................38 3.2 Experimental Section ...................................................................................................39 3.2.1 Synthesis ..........................................................................................................39 3.2.2 Structure Refinements ......................................................................................40 3.2.3 Differential Scanning Calorimetry–Thermogravimetric Analysis...................42 3.2.4 Resistivity Measurements ................................................................................43 3.2.5 Nuclear Magnetic Resonance ..........................................................................43 3.2.6 Electronic Structure Calculations ....................................................................44 3.3 Results and Discussion ................................................................................................44 3.3.1 Synthesis ..........................................................................................................44 3.3.2 Structure ..........................................................................................................45 3.3.3 Transport Properties .........................................................................................49 3.3.4 NMR Studies ....................................................................................................50 3.3.5 Electronic Structure Calculations ....................................................................52 3.4 Conclusion ...................................................................................................................53 4. ZINTL PHASE AS DOPANT SOURCE IN THE FLUX SYNTHESIS OF Ba1-XKXFe2As2 TYPE SUPERCONDUCTORS ..................................................................55 4.1 Introduction .................................................................................................................55 4.2 Experimental Procedure ...............................................................................................59 4.2.1 Synthesis ..........................................................................................................59 4.2.2 Elemental Analysis ..........................................................................................59 4.2.3 Crystallographic Characterization of Ba1-x-yKxSnyFe2As2 Phases ...................60 iv 4.2.4 Magnetic Susceptibility Measurements ...........................................................61 4.3 Results and Discussion ................................................................................................62 4.3.1 Structure Determination ...................................................................................62 4.3.2 Magnetic Susceptibility Measurements ...........................................................64 4.4 Conclusion ...................................................................................................................64 5. FLUX GROWTH AND PHYSICAL PROPERTIES OF A/Ni/Sb PHASES (A = Eu OR Sr) ..........................................................................................................................................66 5.1 Introduction ..................................................................................................................66 5.2 Experimental Procedure ...............................................................................................67 5.2.1 Synthesis ..........................................................................................................67 5.2.2 Elemental Analysis ..........................................................................................67 5.2.3 Structure Refinements ......................................................................................68 5.3 Discussion ....................................................................................................................71 5.3.1 Synthesis and Crystal Growth ..........................................................................71 5.3.2 Structure ...........................................................................................................72 5.3.3 Magnetic Properties .........................................................................................75 5.4 Conclusions ..................................................................................................................79 6. FUTURE WORK ..................................................................................................................80 7. REFERNCES ........................................................................................................................81 8. BIOGRAPHICAL SKETCH .................................................................................................87 v LIST OF TABLES 3.1. Crystallographic Data for Ba2In5Pn5 Phases ........................................................................41 3.2 Atomic Positions for the Ba2In5Pn5 Phases .........................................................................42 3.3. Selected Bond Lengths (Å) ....................................................................................................48 4.1. Reaction ratios and product stoichiometries, unit cells, and superconducting transition temperatures for Ba1-x-yKxSnyFe2As2 phases. ........................................................................61 4.2. Atomic positions and occupancies for Ba0.598(6)K0.381(1)Sn0.044(5)Fe2A2. .................................61 5.1. Crystallographic data for A/Ni/Sb phases...............................................................................69 5.2 Atom positions for EuNi1.78Sb2 ...............................................................................................69 5.3 Atom positions for SrNi1.78Sb2................................................................................................70 5.4 Atom positions for EuNi2Sb2 ..................................................................................................70 5.5 Atom positions for Eu2Sb5Ni7 .................................................................................................70 5.6 Selected bond
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