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Point Defects in Lithium Gallate and Gallium Oxide

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Point Defects in Lithium Gallate and Gallium Oxide Air Force Institute of Technology AFIT Scholar Theses and Dissertations Student Graduate Works 8-23-2019 Point Defects in Lithium Gallate and Gallium Oxide Christopher A. Lenyk Follow this and additional works at: https://scholar.afit.edu/etd Part of the Nuclear Engineering Commons Recommended Citation Lenyk, Christopher A., "Point Defects in Lithium Gallate and Gallium Oxide" (2019). Theses and Dissertations. 2369. https://scholar.afit.edu/etd/2369 This Dissertation is brought to you for free and open access by the Student Graduate Works at AFIT Scholar. It has been accepted for inclusion in Theses and Dissertations by an authorized administrator of AFIT Scholar. For more information, please contact [email protected]. POINT DEFECTS IN LITHIUM GALLATE AND GALLIUM OXIDE DISSERTATION Christopher A. Lenyk, Lt Col, USAF AFIT-ENP-DS-19-S-023 DEPARTMENT OF THE AIR FORCE AIR UNIVERSITY AIR FORCE INSTITUTE OF TECHNOLOGY Wright-Patterson Air Force Base, Ohio DISTRIBUTION STATEMENT A. APPROVED FOR PUBLIC RELEASE; DISTRIBUTION UNLIMITED. The views expressed in this document are those of the author and do not reflect the official policy or position of the United States Air Force, the United States Department of Defense or the United States Government. This material is declared a work of the U.S. Government and is not subject to copyright protection in the United States. AFIT-ENP-DS-19-S-023 POINT DEFECTS IN LITHIUM GALLATE AND GALLIUM OXIDE DISSERTATION Presented to the Faculty Graduate School of Engineering and Management Air Force Institute of Technology Air University Air Education and Training Command in Partial Fulfillment of the Requirements for the Degree of Doctor of Philosophy in Nuclear Engineering Christopher A. Lenyk, B.S., M.S. Lt Col, USAF DISTRIBUTION STATEMENT A. APPROVED FOR PUBLIC RELEASE; DISTRIBUTION UNLIMITED. AFIT-ENP-DS-19-S-023 POINT DEFECTS IN LITHIUM GALLATE AND GALLIUM OXIDE DISSERTATION Christopher A. Lenyk, B.S., M.S. Lt Col, USAF Committee Membership: Nancy C. Giles, PhD Chair Maj Nicholas Herr, PhD Member Maj Tod Laurvick, PhD Member John W. McClory, PhD Member ADEDEJI B. BADIRU, PhD Dean, Graduate School of Engineering and Management AFIT-ENP-DS-19-S-023 Abstract Electron paramagnetic resonance (EPR), Fourier-Transform Infrared spectroscopy (FTIR), photoluminescence (PL), thermoluminescence (TL), and wavelength-dependent TL are used to identify and characterize point defects in lithium gallate and β-gallium oxide doped with Mg and Fe acceptor impurities single crystals. EPR investigations of − 2− LiGaO2 identify fundamental intrinsic cation defects lithium (VLi) and gallium (VGa) vacancies. The defects’ principle g values are found through angular dependence stud- ies and atomic-scale models for these new defects are proposed. Thermoluminescence measurements estimate the activation energy of lithium vacancies at Ea = 1.05 eV and gallium vacancies at Ea > 2 eV below the conduction band minimum. Mg and Fe doped β-Ga2O3 crystals are investigated with EPR and FTIR and concentrations of Ir4+ ions greater than 1 1018 cm3 are observed. The source of × the unintentional deep iridium donors is the crucible used to grow the crystal. In the Mg-doped crystals, the Ir4+ ions provide compensation for the singly ionized Mg acceptors contributing to the difficulties in producing p-type behavior in bulk single crystals. A large spin-orbit coupling causes Ir4+ ions to have a low-spin (5d5,S=1/2) ground state. The Ir4+ ions have an infrared absorption band representing a d d − transition within the t2g orbitals. 2+/3+ Using these same techniques the Fe level in Fe-doped β-Ga2O3 crystals is determined. With these noncontact spectroscopy methods, a value of 0.83 0.04 eV ± below the conduction band is obtained for this level. These results clearly establish that the E2 deep level observed in DLTS experiments is due to the thermal release of electrons from Fe2+ ions. iv AFIT-ENP-DS-19-S-023 Dedicated to my loving and unbelievably patient wife. Thank you for being by my side all these years. v Acknowledgements I wish to thank my faculty advisor, Dr. Nancy C. Giles, for her advice, encourage- ment, willingness to take on another student, and the opportunity to be a part of this exciting and fundamental field of research. I would like to thank Dr. Larry Hallibur- ton for the countless hours spent coaching me through the numerous experimental setups, explanations on the nuances of the physics, and for his insistence on critical thinking and always reminding me to be aware of any assumptions made during the exploration process. Also, I want to thank the members of my committee Majors Nicholas Herr and Tod Laurvick, and Dr. John McClory for agreeing to be part of the endeavor. Last, I want to thank Capt Elizabeth Scherrer for her support on EasySpin codes and posing many questions that made me rethink the way I was approaching my own data sets. Christopher A. Lenyk vi Table of Contents Page Abstract............................................ ...................iv Acknowledgements .................................... ..................vi ListofFigures...................................... .....................x ListofTables....................................... ...................xiii List of Abbreviations ................................. ..................xiv 1. Introduction..................................... ...................1 1.1 Overview and Motivation........................... ..............1 1.2 Previous Research on Ga2O3 ......................................2 1.3 Previous Research on LiGaO2 ....................................8 1.4 Organization of the Dissertation................... ................9 1.5 Research Support, Interest, and Limits .............. ..............10 2. Experimental Principles ........................... ..................11 2.1 Crystal Field Theory.............................. ..............11 2.1.1 The weak field approximation ...................... ........14 2.1.2 The intermediate field approximation .............. .........17 2.1.3 The strong field approximation .................... .........18 2.1.4 Pairing energies ............................... ...........18 2.1.5 Factors affecting magnitude of ∆ ................... ........19 2.2 Electron Paramagnetic Resonance (EPR) .............. ............20 2.3 Spin Hamiltonian.................................. .............25 2.3.1 Fine structure interactions: S D S...........................26 2.3.2 Hyperfine interactions: I A S...............................27· · 2.3.3 Nuclear quadrapole interactions:· · I Q I.......................28 · · 2.3.4 Nuclear Zeeman interactions: gnβnI B.......................29 2.4 ThegMatrix ......................................· ............29 2.5 Optical Spectroscopy ............................. ..............32 2.5.1 Photoluminescence and photoluminescence excitation ......................................... ......35 2.5.2 IR absorption due to a change in dipole moment........ ......35 2.6 Thermoluminescence (TL).......................... .............36 2.6.1 First order kinetics ............................ ...........40 2.6.2 Second order kinetics ........................... ..........44 2.6.3 General order kinetics.......................... ...........45 4+ 5 1 2.7 Ir d in a Strong Octahedral Field S= 2 .........................47 vii Page 3. ExperimentalSetup ................................ ................48 3.1 Electron Paramagnetic Resonance Spectrometer . .............48 3.1.1 EPRsamplecavity ............................... ........52 3.1.2 Phase sensitive detection ....................... ...........53 3.2 FTIR Spectrometer................................ .............55 3.3 Thermoluminescent Dosimeter Reader................ .............58 3.4 Wavelength-dependent TL.......................... .............59 4. Lithium and Gallium Vacancies in LiGaO2 .............................63 4.1 Abstract ......................................... .............63 4.2 Introduction.................................... ...............63 4.3 Experimental .................................... ..............65 0 4.4 Neutral Lithium Vacancy VLi ....................................66 2− 4.5 Doubly Ionized Gallium Vacancy VGa .............................74 4.6 Thermoluminescence Analysis....................... .............77 4.7 Summary ......................................... ............82 4+ 5. Ir ions in β-Ga2O3 An Unintentional Deep Donor .....................83 5.1 Abstract ......................................... .............83 5.2 Introduction.................................... ...............83 5.3 Experimental .................................... ..............85 5.4 EPRResults...................................... .............86 5.5 Infrared Absorption Results........................ ..............93 5.6 Effects of Above-Band-Gap Photons .................... ..........99 5.7 Conclusions..................................... ..............101 6. Deep Donors and Acceptors in β-Ga2O3 Crystals: Determination of the Fe2+/3+ Level by a Non-contact Method ...........104 6.1 Abstract ......................................... ............104 6.2 Introduction.................................... ..............104 6.3 Experimental .................................... .............105 6.4 Production and Thermal Decay of Fe2+ and Ir4+ Ions ..............108 6.5 Analysis of Thermal Decay Curves..................... ..........115 6.6 Luminescence Results............................. .............117 6.7 Summary ........................................
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