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Final Thesis BULK CRYSTAL GROWTH, CHARACTERIZATION AND THERMODYNAMIC ANALYSIS OF ALUMINUM NITRIDE AND RELATED NITRIDES by LI DU B.S., East China University of Science and Technology, 2004 AN ABSTRACT OF A DISSERTATION submitted in partial fulfillment of the requirements for the degree DOCTOR OF PHILOSOPHY Department of Chemical Engineering College of Engineering KANSAS STATE UNIVERSITY Manhattan, Kansas 2011 Abstract The sublimation recondensation crystal growth of aluminum nitride, titanium nitride, and yttrium nitride were explored experimentally and theoretically. Single crystals of these nitrides are potentially suitable as substrates for AlGaInN epitaxial layers, which are employed in ultraviolet optoelectronics including UV light-emitting diodes and laser diodes, and high power high frequency electronic device applications. A thermodynamic analysis was applied to the sublimation crystal growth of aluminum nitride to predict impurities transport (oxygen, carbon, and hydrogen) and to study the aspects of impurities incorporation for different growth conditions. A source purification procedure was established to minimize the impurity concentration and avoid degradation of the crystal’s properties. More than 98% of the oxygen, 99.9% of hydrogen and 90% of carbon originally in the source was removed. The AlN crystal growth process was explored in two ways: self-seeded growth with spontaneous nucleation directly on the crucible lid or foil, and seeded growth on SiC and AlN. The oxygen concentration was 2 ~ 4 x 10 18 cm -3, as measured by secondary ion mass spectroscopy in the crystals produced by self-seeded growth. Crystals grown from AlN seeds have visible grain size expansion. The initial AlN growth on SiC at a low temperature range (1400°C ~1600°C) was examined to understand the factors controlling nucleation. Crystals were obtained from c-plane on-axis and off-axis, Si-face and C-face, as well as m-plane SiC seeds. In all cases, crystal growth was fastest perpendicular to the c-axis. The growth rate dependence on temperature and pressure was determined for TiN and YN crystals, and their activation energies were 775.8±29.8kJ/mol and 467.1±21.7kJ/mol respectively. The orientation relationship of TiN (001) || W (001) with TiN [100] || W [110], a 45 o angle between TiN [100] and W [100], was seen for TiN crystals deposited on both (001) textured tungsten and randomly orientated tungsten. X- ray diffraction confirmed that the YN crystals were rock-salt structure, with a lattice constant of 4.88Å. Cubic yttria was detected in YN sample from the oxidation upon its exposed to air for limited time by XRD, while non-cubic yttria was detected in YN sample for exposures more than one hour by Raman spectra. BULK CRYSTAL GROWTH, CHARACTERIZATION AND THERMODYNAMIC ANALYSIS OF ALUMINUM NITRIDE AND RELATED NITRIDES by LI DU B.S., East China University of Science and Technology, 2004 A DISSERTATION submitted in partial fulfillment of the requirements for the degree DOCTOR OF PHILOSOPHY Department of Chemical Engineering College of Engineering KANSAS STATE UNIVERSITY Manhattan, Kansas 2011 Approved by: Major Professor James H. Edgar Copyright LI DU 2011 Abstract The sublimation recondensation crystal growth of aluminum nitride, titanium nitride, and yttrium nitride were explored experimentally and theoretically. Single crystals of these nitrides are potentially suitable as substrates for AlGaInN epitaxial layers, which are employed in ultraviolet optoelectronics including UV light-emitting diodes and laser diodes, and high power high frequency electronic device applications. A thermodynamic analysis was applied to the sublimation crystal growth of aluminum nitride to predict impurities transport (oxygen, carbon, and hydrogen) and to study the aspects of impurities incorporation for different growth conditions. A source purification procedure was established to minimize the impurity concentration and avoid degradation of the crystal’s properties. More than 98% of the oxygen, 99.9% of hydrogen and 90% of carbon originally in the source was removed. The AlN crystal growth process was explored in two ways: self-seeded growth with spontaneous nucleation directly on the crucible lid or foil, and seeded growth on SiC and AlN. The oxygen concentration was 2 ~ 4 x 10 18 cm -3, as measured by secondary ion mass spectroscopy in the crystals produced by self-seeded growth. Crystals grown from AlN seeds have visible grain size expansion. The initial AlN growth on SiC at a low temperature range (1400°C ~1600°C) was examined to understand the factors controlling nucleation. Crystals were obtained from c-plane on-axis and off-axis, Si-face and C-face, as well as m-plane SiC seeds. In all cases, crystal growth was fastest perpendicular to the c-axis. The growth rate dependence on temperature and pressure was determined for TiN and YN crystals, and their activation energies were 775.8±29.8kJ/mol and 467.1±21.7kJ/mol respectively. The orientation relationship of TiN (001) || W (001) with TiN [100] || W [110], a 45 o angle between TiN [100] and W [100], was seen for TiN crystals deposited on both (001) textured tungsten and randomly orientated tungsten. X- ray diffraction confirmed that the YN crystals were rock-salt structure, with a lattice constant of 4.88Å. Cubic yttria was detected in YN sample from the oxidation upon its exposed to air for limited time by XRD, while non-cubic yttria was detected in YN sample for exposures more than one hour by Raman spectra. Table of Contents List of Figures.................................................................................................................... ix List of Tables .................................................................................................................... xii Acknowledgements..........................................................................................................xiii Dedication........................................................................................................................ xiv Preface............................................................................................................................... xv CHAPTER 1 - Introduction............................................................................................. 1 1.1 Lighting Emitting Diodes and Laser Diodes ...................................................... 2 1.1.1 Background..................................................................................................... 2 1.1.2 History............................................................................................................. 2 1.1.3 Structure.......................................................................................................... 4 1.2 Why III-Nitrides.................................................................................................. 5 1.2.1 The demand for direct bandgap semiconductors ............................................ 5 1.2.2 The enormous variety of broad spectra wavelength ....................................... 7 1.3 Ultraviolet LEDs................................................................................................. 7 1.4 Research Overview............................................................................................. 9 1.5 References......................................................................................................... 11 CHAPTER 2 - Aluminum Nitride and Related Nitrides............................................... 13 2.1 Crystalline Structure of AlN, SiC and related nitrides ..................................... 13 2.1.1 Crystal Structure of AlN and related Nitrides............................................... 14 2.1.2 Crystal Structure of SiC................................................................................ 18 2.1.3 Crystal Structure of Related Transition Metal Nitrides ................................ 20 2.2 Material Properties............................................................................................ 23 2.2.1 Thermal Properties and Mechanical Properties ............................................ 23 2.2.2 Electronic and optical properties .................................................................. 24 2.3 History and Application of AlN........................................................................ 27 2.3.1 History........................................................................................................... 27 2.3.2 Application.................................................................................................... 28 2.4 Crystal Growth.................................................................................................. 29 vi 2.4.1 Physical Vapor Transport ............................................................................. 30 2.4.2 Bulk Crystal Growth of AlN by PVT ........................................................... 34 2.5 References......................................................................................................... 39 CHAPTER 3 - Experimental......................................................................................... 44 3.1 Equipment......................................................................................................... 44 3.2 Source Purification............................................................................................ 46 3.3 Metal Nitridation..............................................................................................
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