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Design and Development of Group 13 Precursors for Improved Vapour Deposition of Metal Nitride Thin Films

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Design and Development of Group 13 Precursors for Improved Vapour Deposition of Metal Nitride Thin Films Design and development of group 13 precursors for improved vapour deposition of metal nitride thin films by Sydney Cristina Buttera A thesis submitted to the Faculty of Graduate and Postdoctoral Affairs in partial fulfillment of the requirements for the degree of Doctor of Philosophy in Chemistry CARLETON UNIVERSITY Ottawa, Ontario © 2020 Sydney Cristina Buttera This thesis is dedicated to my parents, Claudia and Rob Buttera. i Abstract Vapour phase deposition techniques such as atomic layer deposition (ALD) and chemical vapour deposition (CVD) are important for the deposition of thin films for a wide range of applications. Metal oxides and metal nitrides, particularly, can be used as passivation layers and dielectrics, and due to their use in increasingly small microelectronic devices, their deposition must be precise, conformal, and of high purity. It is non-trivial to deposit pure materials without impurities by ALD; several factors including temperature, exposures, and precursor(s) must be considered. This work examines how precursor design can reduce impurities in deposited films. An initial thermal study of an indium tris(guanidinate) precursor by high-resolution NMR (HR-NMR) and thermogravimetric analysis (TGA) demonstrated its thermal instability as a function of long-term heating, following which simpler group 13 precursors were synthesized and studied. Both Al(NMe2)3 and Ga(NMe2)3 were designed due to their lack of metal-carbon bonds and were used to deposit metal oxide and metal nitride films, respectively, with very low impurities by ALD. Methylamines were studied computationally in comparison to ammonia as a possible replacement for a nitrogen co-reagent, though CVD experiments confirmed their favoured reactivity in the gas phase as opposed to at the surface. Other bidentate group 13 ligands were also studied where a new In(III) triazenide produced pure, epitaxial indium nitride by ALD, and MeNacNac ligands Me were used to develop novel Al precursors including Al( NacNac)(NMe2)2 and Me r,Me Al( NacNac)( NacNac). Ultimately, a simple AlH2(NMe2) precursor was designed due to its metal-nitrogen bonds and the addition of the hydride ligand to maintain a reducing atmosphere during depositions and resist AlN film oxidation. Pure aluminum nitride films were deposited by ALD using this precursor and ammonia plasma as a co-reagent. Generally, this work emphasizes the importance of smart precursor design to produce pure, high-quality group 13 nitride thin films. It demonstrates the value in developing new ALD precursors, but doing so in a methodical and logical way. This methodology could be extended to other metal centres to develop a variety of precursors and ALD process that will deposit pure, impurity-free, and high-quality films in a cost- and time-efficient manner. ii Preface This preface provides full bibliographical details for each article included in this thesis, as well as whether the article is reproduced in whole or in part. Use of copyrighted material is likewise acknowledged here. When citing material from this thesis, please cite the article relevant to the chapter, if the chapter is based on a publication. Pursuant to the Integrated Thesis policy of Carleton University, the supervisor (Seán T. Barry) and the “student” (Sydney C. Buttera) confirm that the student was fully involved in setting up and conducting the research, obtaining data and analyzing results, as well as preparing and writing the material presented in the co-authored articles(s) integrated in the thesis. Additionally, the supervisor confirms the information provided by the student in this preface. Chapter 2 Buttera, S. C.; Rönnby, K.; Pedersen, H.; Ojamäe, L.; Barry, S. T. Thermal Study of an Indium Trisguanidinate as a Possible Indium Nitride Precursor. J. Vac. Sci. Technol. A Vacuum, Surfaces, Film. 2018, 36 (1), 01A101. https://doi.org/10.1116/1.5002634 This article is wholly reproduced and edited for formatting and clarity of presentation. Sydney C. Buttera performed all experimentation for this publication outside of the modelling, which was performed by Karl Rönnby and Lars Ojamäe. The publication was written by Seán T. Barry. Chapter 3 Part I – Buttera, S. C.; Mandia, D. J.; Barry, S. T. Tris(Dimethylamido)Aluminum(III): An Overlooked Atomic Layer Deposition Precursor. J. Vac. Sci. Technol. A Vacuum, Surfaces, Film. 2017, 35 (1), 01B128. https://doi.org/10.1116/1.4972469. iii This article is wholly reproduced and edited for formatting and clarity of presentation. Sydney C. Buttera performed all experimentation for this publication including precursor design and synthesis, thermogravimetric analysis, and thin film deposition. David J. Mandia performed X-ray photoelectron spectroscopy measurements and their analyses, as well as assisted with manuscript preparation. This publication was written by Sydney C. Buttera. Part II – Rouf, P.; O’Brien, N. J.; Buttera, S. C.; Martinovic, I.; Bakhit, B.; Martinsson, E.; Palisaitis, J.; Hsu, C.-W.; Pedersen, H. Epitaxial GaN Using Ga(NMe2)3 and NH3 Plasma by Atomic Layer Deposition. J. Mater. Chem. C 2020, 3, 1101–1134. https://doi.org/10.1039/D0TC02085K. This article is wholly reproduced and edited for formatting and clarity of presentation. Sydney C. Buttera performed and analyzed all thermal characterization of the precursor, including calculation of the 1 Torr temperature, by thermogravimetric analysis and differential scanning calorimetry. Polla Rouf performed the majority of the precursor synthesis and perform SEM, XPS, and XRD measurements. Nathan J. O’Brien aided with synthesis and Erik Martinsson performed absorption measurements. Babak Bakhit performed ERBA/RBS while Ivan Martinovic, Justinas Palisaitis, and Chih-Wei Hsu collected TEMs. This publication was written by Polla Rouf. Chapter 4 Rönnby, K.; Buttera, S. C.; Rouf, P.; Barry, S. T.; Ojamäe, L.; Pedersen, H. Methylamines as Nitrogen Precursors in Chemical Vapor Deposition of Gallium Nitride. J. Phys. Chem. C 2019, 123 (11), 6701–6710. https://doi.org/10.1021/acs.jpcc.9b00482. This article is wholly reproduced and edited for formatting and clarity of presentation. Sydney C. Buttera designed and performed all chemical vapour deposition experiments and collected all optical microscopy images. Computational experiments were performed by Karl Rönnby and Lars Ojamäe. Polla Rouf performed grazing-incidence X-ray diffraction experiments on thin films. This publication was largely written by Karl Rönnby while all other collaborators contributed for sections of the publication that pertained to their experiments. iv Chapter 5 Part I – O’Brien, N. J.; Rouf, P.; Samii, R.; Ronnby, K.; Buttera, S. C.; Hsu, C.- W.; Ivanov, I. G.; Kessler, V.; Ojamäe, L.; Pedersen, H. In-Situ Activation of an Indium(III) Triazenide Precursor for Epitaxial Growth of Indium Nitride by Atomic Layer Deposition. Chem. Mater. 2020. https://doi.org/10.1021/acs.chemmater.9b05171. This article is wholly reproduced and edited for formatting and clarity of presentation. Sydney C. Buttera performed all thermolysis experiments, including thermogravimetric analysis and differential scanning calorimetry, as well as their analyses and calculation of the 1 Torr temperature of all precursors. Nathan J. O’Brien developed and Rouzbeh Samii developed and characterized the precursor while Polla Rouf performed deposition experiments and their associated characterizations (XPS, SEM, XRR). Karl Rönnby and Lars Ojamäe performed DFT calculations related to the thermal decomposition of precursors. Chih-Wei Hsu characterized the films electronically, Ivan Ivanov performed Raman spectroscopy, and Vadim Kessler performed XRD. This publication was written by Nathan J. O’Brien with the aid of other contributors related to their experiments and measurements. Part II – Buttera, S. C.; Masuda, J. D.; Barry, S. T. Novel Aluminum MeNacNac Compounds as Possible Precursors for Atomic Layer Deposition. Manuscript in progress. This article is a manuscript in progress. Sydney C. Buttera performed all syntheses, thermal characterizations by thermogravimetric analysis, and NMR boilup experiments. Jason C. Masuda collected solid state molecular structures by single crystal X-ray diffraction. This manuscript was written by Sydney C. Buttera. Chapter 6 Buttera, S. C.; Rouf, P.; Deminskyi, P.; Pedersen, H.; Barry, S. T. A Low Cost, High Efficiency TMA-replacement for the Deposition of Pure Aluminum Nitride by Atomic Layer Deposition. Manuscript in progress. This article is a manuscript in progress. Sydney C. Buttera designed the precursor, performed and analyzed thermogravimetric analysis including the collection of the 1 Torr temperature, and designed and performed all ALD experiments. Polla Rouf v and Petro Deminskyi collected and analyzed all GIXRD data. Polla Rouf calculated AlN stress and strain and collected/analyzed XPS data. SEM data was collected by Petro Deminskyi. This manuscript was written by Sydney C. Buttera. vi Acknowledgements Writing this thesis and looking back on all this work is the greatest representation of the fact that I could have never done this on my own. I am eternally grateful to every single person who contributed to this work, taught me along the way, or was there as sometimes much-needed and always much-appreciated support. Firstly, I have to acknowledge my supervisor Dr. Seán T. Barry. Seán, without your trust in me as a post-first year student and incalculable support over the following eight years through to my PhD studies, this thesis would not exist. Your encouragement
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