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UCLA UCLA Electronic Theses and Dissertations UCLA UCLA Electronic Theses and Dissertations Title Tetrides and Pnictides for Fast-Ion Conductors, Phosphor-Hosts, Structural Materials and Improved Thermoelectrics Permalink https://escholarship.org/uc/item/9068g8b2 Author Hick, Sandra Marie Publication Date 2013 Supplemental Material https://escholarship.org/uc/item/9068g8b2#supplemental Peer reviewed|Thesis/dissertation eScholarship.org Powered by the California Digital Library University of California UNIVERSITY OF CALIFORNIA Los Angeles Tetrides and Pnictides for Fast-Ion Conductors, Phosphor-Hosts, Structural Materials and Improved Thermoelectrics A dissertation submitted in partial satisfaction of the requirements for the degree Doctor of Philosophy in Chemistry by Sandra Marie Hick 2013 ABSTRACT OF THE DISSERTATION Tetrides and Pnictides for Fast-Ion Conductors, Phosphor-Hosts, Structural Materials and Improved Thermoelectrics by Sandra Marie Hick Doctor of Philosophy in Chemistry University of California, Los Angeles, 2013 Professor Richard B. Kaner, Chair New routes to solid states materials are needed for discovery and the realization of improved reactions. By utilizing reactive approaches such as solid-state metathesis, pyrolysis, and nitride fluxes new routes to hard materials, phosphor hosts, and fast ion conductors were developed. The fast ion conductor lithium silicon nitride, Li2SiN2, was produced in a metathesis reaction between silicon chloride, SiCl4 and lithium nitride, Li3N, initiated in a conventional microwave oven. The Li2SiN2 produced had a conductivity of 2.70 x 10-3 S/cm at 500 °C. Colorless millimeter-sized crystals of Ca16Si17N34 were synthesized at high temperatures from a flux generated in situ from reaction intermediates. The ii compound was found to crystallize in the cubic space group F-43m (a = 14.8882 Å). The powder X-ray diffraction pattern of Ca16Si17N34 matches that of a phase identified as cubic CaSiN2 in the 1960s but never structurally characterized. In contrast to the 2+ orthorhombic phase of CaSiN2, in which Ca sits in octahedral sites, this cubic phase has Ca2+ in cubic sites that makes it an interesting host for new phosphors and gives rise to unique crystal field splitting. A carbon-free silazane was formed by reacting metallic silicon in a melt of sodium amide; pyrolysis of this material offers a convenient route to Si3N4. The use of oxides for solid-state metathesis reactions was investigated for the formation of ternary silicon nitrides for phosphor hosts. Red, green, and blue phosphors were rapidly produced using rare earth oxides dopants. Solid-state metathesis reactions were investigated for the production of nano-scale B4C and ZrC. The addition of a refractory, hard material significantly improves the mechanical properties of existing thermoelectric materials. iii The dissertation of Sandra Marie Hick is approved. M. Frederick Hawthorne Bruce S. Dunn Richard B. Kaner, Committee Chair University of California, Los Angeles 2013 iv Dedication This work is dedicated to the memories of Glenn and Cindie Blair, Grandma Delores, Grandpa Orville, and my dear friend Susannah. For my husband, Richard. Thank you for believing in me. v Table of Contents ABSTRACT OF THE DISSERTATION ............................... ii Dedication ................................................................................ v List of Tables ........................................................................ xviii Acknowledgements ................................................................ xix Vita ............................................................................ xxii Publications and Presentations ............................................................................. xxiv Chapter 1: Introduction to Alternative Solid-State Synthesis ................................................................................ 1 References ................................................................................................................. 3 Chapter 2: Microwave Initiated Solid-State Metathesis Routes to Li2SiN2 ................................................... 7 Summary ................................................................................................................... 7 Introduction ............................................................................................................... 7 Experimental ............................................................................................................. 9 Reagents ................................................................................................................ 9 Synthesis ................................................................................................................ 9 vi Characterization ................................................................................................. 11 Results and Discussion ........................................................................................... 12 Conclusions ............................................................................................................. 19 Acknowledgments ................................................................................................... 19 References ............................................................................................................... 20 Chapter 3: Synthesis and Crystal Structure of Cubic Ca16Si17N34 ............................................................ 24 Summary ................................................................................................................. 24 Introduction ............................................................................................................. 24 Reagents .............................................................................................................. 26 Single Crystal Synthesis ...................................................................................... 26 Powder Synthesis ................................................................................................ 27 Refractive Index .................................................................................................. 28 Characterization ................................................................................................. 28 Results ..................................................................................................................... 29 Discussion ............................................................................................................... 33 Conclusions ............................................................................................................. 37 Acknowledgements ................................................................................................. 38 Supporting Information ........................................................................................... 38 References ............................................................................................................... 38 vii Chapter 4: Synthesis of Si3N4 via a Polysilazane Intermediate ........................................................ 42 Introduction ............................................................................................................. 42 Experimental ........................................................................................................... 47 Chemicals ............................................................................................................ 47 Method ................................................................................................................ 47 Characterization ................................................................................................. 51 Results ..................................................................................................................... 51 Discussion ............................................................................................................... 54 Conclusions ............................................................................................................. 58 References ............................................................................................................... 58 Chapter 5: Luminescence in Ternary Silicon Nitrides ....... 63 Introduction ............................................................................................................. 63 Experimental ........................................................................................................... 65 Chemicals ............................................................................................................ 65 Synthesis .............................................................................................................. 66 LiSi2N3 Phosphor Synthesis ................................................................................. 66 MgSiN2 Phosphor Synthesis ................................................................................ 67 XRD Analysis ...................................................................................................... 67 Luminescence ...................................................................................................... 68 Results and Discussion ........................................................................................... 68 viii Fluorescence ....................................................................................................... 70 Conclusions
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