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Development of Zinc Nitride Materials for Semiconductor Applications Development of Zinc Nitride Materials for Semiconductor Applications By: Aristotelis Trapalis A thesis submitted in partial fulfilment of the requirements for the degree of Doctor of Philosophy The University of Sheffield Faculty of Engineering Department of Electronic and Electrical Engineering November 2018 to my friends and family· σας ευχαριστώ Table of Contents Acknowledgements ............................................................................................ iii Abstract ................................................................................................................ v Introduction ....................................................................................... 1 1.1. Semiconductor materials and devices .................................................................. 1 1.2. Zinc Nitride and Zn-IV-Nitrides ............................................................................. 2 1.3. Thesis outline ....................................................................................................... 4 1.4. Bibliography ......................................................................................................... 5 Literature Review of Zinc Nitride ..................................................... 7 2.1. Crystal structure ................................................................................................... 7 2.2. Charge transport properties .................................................................................. 9 2.3. Bandgap and refractive index ............................................................................. 11 2.4. Chemical synthesis approaches ......................................................................... 14 2.5. Physical vapour deposition ................................................................................. 18 2.6. Roadmap for applications ................................................................................... 21 2.7. Summary ............................................................................................................ 23 2.8. Bibliography ....................................................................................................... 23 Experimental Techniques and Methodologies ............................. 27 3.1. Physical vapour deposition techniques ............................................................... 27 3.2. Characterisation techniques ............................................................................... 33 3.3. Bibliography ....................................................................................................... 46 Zinc Nitride Grown by Sputtering ................................................. 49 4.1. Sputtering process ............................................................................................. 49 4.2. Surface morphology and film composition .......................................................... 52 4.3. Crystal structure ................................................................................................. 55 4.4. Charge transport properties ................................................................................ 57 4.5. Absorption coefficient and refractive index ......................................................... 59 4.6. Photoluminescence ............................................................................................ 63 4.7. Summary ............................................................................................................ 68 4.8. Bibliography ....................................................................................................... 69 Zinc Nitride Grown by Molecular Beam Epitaxy .......................... 73 5.1. Molecular Beam Epitaxy of Zinc Nitride .............................................................. 73 5.2. Growth process parameters ............................................................................... 73 5.3. Effect of experimental parameters on the growth rate ........................................ 77 5.4. Morphology and crystal structure ........................................................................ 85 5.5. Charge transport properties ................................................................................ 91 5.6. Optical bandgap and Burstein-Moss shift ........................................................... 95 5.7. Summary ............................................................................................................ 99 i 5.8. Bibliography ..................................................................................................... 100 Aluminium Zinc Nitride Grown by Sputtering ............................ 103 6.1. Bandgap tuning in Zinc Nitride materials .......................................................... 103 6.2. Compositional analysis of a II-III-V alloy ........................................................... 104 6.3. Crystal structure and morphology ..................................................................... 107 6.4. Absorption coefficient and refractive index ....................................................... 108 6.5. Charge transport properties .............................................................................. 112 6.6. Summary .......................................................................................................... 114 6.7. Bibliography ..................................................................................................... 114 On thermal annealing and the stability of Zinc Nitride .............. 117 7.1. Ex-situ thermal annealing of Zinc Nitride .......................................................... 117 7.2. Ambient stability of annealed samples .............................................................. 117 7.3. Crystal structure ............................................................................................... 122 7.4. Optical bandgap ............................................................................................... 123 7.5. Summary .......................................................................................................... 125 7.6. Bibliography ..................................................................................................... 126 Zinc Nitride Nanoparticles by Gas Phase Aggregation ............. 127 8.1. Zinc Nitride nanoparticles ................................................................................. 127 8.2. In-situ process monitoring ................................................................................ 127 8.3. Deposition rate and process stability ................................................................ 129 8.4. Nanoparticle deposition with and without nitrogen plasma ................................ 130 8.5. Summary .......................................................................................................... 133 8.6. Bibliography ..................................................................................................... 134 Conclusions and Further Work ................................................... 135 9.1. Conclusions ...................................................................................................... 135 9.2. Further work ..................................................................................................... 137 9.3. Bibliography ..................................................................................................... 140 ii Acknowledgements Throughout my PhD studies, I have been fortunate to work with people who helped me cope with the difficulties of studying for a PhD, and without whom this task would have been much more difficult. I would like to express my gratitude above all to Prof. Jon Heffernan, Dr. Ian Farrer, Dr. Alistair Kean, and Dr. Jonathan Sharman who played a critical role in guiding this project and my development as a student. I would also like to thank the research staff in the National Epitaxy Facility in the University of Sheffield who have helped introduce me (and many other students) to the facilities, despite their own busy schedules. This includes Dr. Kenneth Kennedy, Dr. Paul Fry, and Mr. Saurabh Kumar. Last but not least, I would like to thank friends, family, and fellow PhD students with whom I have shared my frustrations and difficulties over this period, and who have helped make my time in Sheffield enjoyable. This research was co-funded by the EPSRC (Engineering and Physical Sciences Research Council) and Johnson Matthey PLC. The financial support by these parties is highly appreciated. Some of the results and discussion presented in this work have produced the following publications: 1. “Structural, electrical and optical characterization of as grown and oxidized zinc nitride thin films”, A. Trapalis, J. Heffernan, I. Farrer, J. Sharman, and A. Kean, Journal of Applied Physics, 120, 205102 (2016) 2. “Temperature dependence of the bandgap of zinc nitride observed in photoluminescence measurements”, A. Trapalis, I. Farrer, K. Kennedy, A. Kean, J. Sharman, and J. Heffernan, Applied Physics Letters 111, 122105 (2017). iii Abstract Zn3N2 has recently attracted research interest as a candidate for use in earth-abundant semiconductor devices. However, Zn3N2 is in a group of semiconductor materials that have not been studied extensively in past literature. As a result, this study is focused on the fundamental properties of Zn3N2 from a materials science point of view, with an emphasis
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