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Surface and Interface Characterization of 2D Materials: Transition Metal Dichalcogenide and Black Phosphorous

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Surface and Interface Characterization of 2D Materials: Transition Metal Dichalcogenide and Black Phosphorous SURFACE AND INTERFACE CHARACTERIZATION OF 2D MATERIALS: TRANSITION METAL DICHALCOGENIDE AND BLACK PHOSPHOROUS by Hui Zhu APPROVED BY SUPERVISORY COMMITTEE: ___________________________________________ Dr. Robert M. Wallace, Chair ___________________________________________ Dr. Christopher L. Hinkle ___________________________________________ Dr. Jiyoung Kim ___________________________________________ Dr. Kyeongjae Cho Copyright 2017 Hui Zhu All Rights Reserved Dedicated to my husband and my parents SURFACE AND INTERFACE CHARACTERIZATION OF 2D MATERIALS: TRANSITION METAL DICHALCOGENIDE AND BLACK PHOSPHOROUS by HUI ZHU, BS, MS DISSERTATION Presented to the Faculty of The University of Texas at Dallas in Partial Fulfillment of the Requirements for the Degree of DOCTOR OF PHILOSOPHY IN MATERIALS SCIENCE AND ENGINEERING THE UNIVERSITY OF TEXAS AT DALLAS December 2017 ACKNOWLEDGMENTS First of all, I’d like to thank my supervisor, Dr. Robert M. Wallace, for his continuous and tremendous support of my master’s and Ph.D. research, for his patience, motivation, and immense knowledge. His diligent working attitude and enthusiasm for science establish a great standard of learning for every researcher in our group, including me. An open, friendly, and positive working environment is created, and it is my pleasure to work and study there. I would also like to acknowledge my committee professors, Dr. Jiyoung Kim, Dr. Kyeongjae Cho, and Dr. Christopher L. Hinkle for their stimulating instruction and the supportive research environment they provided. Grateful appreciation is also delivered to my colleague Mr. Qingxiao Wang and his supervisor Dr. Moon J. Kim for their extensive STEM collaborations included in this work. My acknowledgment to all my colleagues working together on 2D materials at UTD, including postdoctoral researchers: Dr. Stephen McDonnell, who now is an assistant professor at the University of Virginia, Dr. Xiaoye Qin, Dr. Rafik Addou, Dr. Lanxia Cheng, Dr. Antonio Lucero, and Dr. Lee Walsh; my fellow colleagues: Angelica Azcatl, Christopher Smyth, Christopher Cormier, Ava Khosravi, Ruoyu Yue, Chenxi Zhang, Yifan Nie, Jeong-Bong Lee, and Arul Vignerswar Ravichandran. It’s my great pleasure to work with them. Special gratitude goes out to our technician staff: Tommy Bennett, Dave Stimson, Billy Raulston, and Richard Arthur Mills Jr. for their unfailing support and laboratory maintenance. Especially, I want to thank my dear husband, Xiaoye, who has accompanied me on my Ph.D. journey and provided selfless support and constant encouragement. I am also grateful to all our family members and friends. They are always there for me. October 2017 v SURFACE AND INTERFACE CHARACTERIZATION OF 2D MATERIALS: TRANSITION METAL DICHALCOGENIDE AND BLACK PHOSPHOROUS Hui Zhu, PhD The University of Texas at Dallas, 2017 ABSTRACT Supervising Professor: Robert M. Wallace Transition metal dichalcogenides (TMDs) and black phosphorous (black-P) are representative two dimensional (2D) materials with versatile electronic, optical, physical, and chemical properties that can be manipulated for novel electronic and optoelectronic device applications in nanoscale science and technology. However, many challenges remain associated with the nature of defects, crystal synthesis, thickness control, chemical stabilities, doping strategies, and Schottky contacts. This dissertation focuses on the surface and interface understanding of 2D materials to propose desired attributes and surface engineering to overcome those challenges. In particular, the interfacial qualities between the atomic layer deposited Al2O3 and black-P, MoTe2, or WTe2 are investigated by in situ X-ray photoelectron spectroscopy to lower the interfacial damage possibility. Then the chemical and structural properties of MoS2 under remote O2 plasma and thermal treatments are studied to propose a two-step atomic layer etching method. Also, the thermal and structural properties of MoTe2 are investigated to avoid thermal damage as well as explore possible phase engineering applications. vi TABLE OF CONTENTS Acknowledgments............................................................................................................................v Abstract .......................................................................................................................................... vi List of Figures ................................................................................................................................ xi List of Tables ............................................................................................................................. xviii CHAPTER 1 INTRODUCTION ...................................................................................................1 1.1 2D materials for the next generation of nanoelectronics .........................................1 1.2 Transition metal dichalcogenides overview.............................................................4 1.3 Black phosphorous overview ...................................................................................8 1.4 Challenges and Research Motivation of this work ................................................10 1.5 Outline of this work ...............................................................................................13 1.6 References ..............................................................................................................15 CHAPTER 2 EXPERIMENTAL METHODS.............................................................................21 2.1 In situ UHV systems ..............................................................................................21 2.1.1 X-Ray Photoelectron Spectroscopy (XPS) ................................................22 2.1.2 Scanning Tunneling Microscopy (STM)....................................................27 2.1.3 Atomic Layer Deposition (ALD) ...............................................................30 2.2 Ex situ characterization techniques ........................................................................31 2.2.1 Raman Spectroscopy ..............................................................................................31 2.2.2 Scanning Transmission Electron Microscopy (STEM) .........................................34 2.3 References ..............................................................................................................36 CHAPTER 3 AL2O3 ON BLACK PHOSPHORUS BY HALF CYCLE ATOMIC LAYER DEPOSITION ...............................................................................................................................38 3.1 Preface....................................................................................................................38 vii 3.2 Introduction ............................................................................................................39 3.3 Experimental Section .............................................................................................41 3.4 Results and Discussion ..........................................................................................44 3.5 Conclusions ............................................................................................................52 3.6 References ..............................................................................................................53 CHAPTER 4 REMOTE PLASMA OXIDATION AND ATOMIC LAYER ETCHING OF MOS2………….............................................................................................................................57 4.1 Preface....................................................................................................................57 4.2 Introduction ............................................................................................................58 4.3 Experimental Section .............................................................................................60 4.4 Results and discussion ...........................................................................................62 4.4.1 The effect of plasma exposure time on the oxidation of MoS2 ..................62 4.4.2 The impact of substrate temperature on the oxidation of MoS2 .................67 4.4.3 Atomic layer etching by thermal annealing ...............................................71 4.5 Conclusions ............................................................................................................76 4.6 References ..............................................................................................................77 CHAPTER 5 DEFECTS AND SURFACE STRUCTURAL STABILITY OF MOTE2 UNDER VACUUM ANNEALING .............................................................................................................82 5.1 Preface....................................................................................................................82 5.2 Introduction ............................................................................................................83 5.3 Experimental Section .............................................................................................85 5.4 Results and Discussion ..........................................................................................87 5.4.1 Intrinsic crystal qualities induced by excess of Te .....................................87 5.4.2 Surface dissociation and development of Te vacancies .............................94 5.4.3 Passivation of MoTe2 with monolayer graphene
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