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Cesium-Based Colloidal Halide Perovskite Nanocrystal CESIUM-BASED COLLOIDAL HALIDE PEROVSKITE NANOCRYSTAL: STABILITY AND LEAD-FREE DESIGN BY CHANG LU A Dissertation Submitted to the Graduate Faculty of Wake Forest University Graduate School of Arts and Sciences in Partial Fulfillment of the Requirements for the Degree of DOCTOR OF PHILOSOPHY Chemistry August 2019 Winston-Salem, North Carolina Copyright Chang Lu 2019 Approved By: Scott M. Geyer, Ph.D., Advisor Michael D. Gross, Ph.D., Chair Elham Ghadiri, Ph.D. Paul B. Jones, Ph.D. Akbar Salam, Ph.D. Acknowledgements Time flies very fast. I can still remember the very first day I spent at Salem Hall, I was nervous, not very comfortable speaking English and I just barely passed the Organic Placement Exam. Now, when I look at this thesis, my PhD is close to an end. While I am writing these acknowledgement words, I find myself thinking back on these five incredible years I have had here at WFU, as well as in Winston-Salem. I would not have such a positive experience and scientific contribution here without many people I have met along the journey. Therefore, I would like to thank the following people for shaping the past years into a truly incredible memory in my life. I would like to thank Dr. Geyer first. What I have learnt from you are not just experience and QD or ALD techniques, it is the positive and attentive attitude to zero in on a specific area, a specific question. When I was an undergraduate, there was always someone you can seek for help, and I am really used to this learning mode. However, being a PhD student is different, nobody can teach you everything. I have to confront the problems and issues by myself. What you have shown me was if I am not familiar with this software/theory/technique/setup/system, etc, face it and learn/solve it. This is simple but sometimes not very easy for me to do. Moreover, working under you is quite enjoyable, I can report any flash on my mind and ask for unconditional chemical or equipment support from you. Thanks for all the patience and encouragements you have given to me. Special thanks go to my committee, Dr. Gross and Dr. Salam, I am thankful to all the discussion with you, your engineering and quantum mechanical perspectives truly broaden my horizon with the perovskite projects I have been working on. II I would also like to thank my colleagues in our lab: Hui, Dominique, Xiao and Alex. My work at WFU could not be possible without the helpful discussion and assistance from many of you. I really enjoy the thought sharing and look forward to pumping out more publications with you in the future. Throughout the years here at WFU, there are also a lot of internal and external collaborators and staff members who have helped me. Being involved in collaborative projects, I had the chance to work with extraordinary scientists, students and professors. In this regard, I would love to thank: the Carroll lab (Prof. David Carroll, Corey, Chaochao, Wenxiao, Junwei and Kateryna); the Jurchescu lab (Prof. Oana Jurchescu, Andrew and Peter); the Donati lab (Prof. George Donati, Charles, Jake); Dr. Day, Dr. Wright, Dr. KB Ucer, Dr. Brown-Harding, Dr. Tracy, and etc. Last but not least, I would like to thank my family, although I am thousands of miles away from you, but I can always feel you are with me and you are close to me. Chang Lu July 2019 III Table of Contents List of Figures ________________________________________________________________ VI List of Tables ________________________________________________________________ X List of Abbreviations __________________________________________________________ XI Abstract ____________________________________________________________________ XIII Chapter 1 Introduction _______________________________________________________ 1 1.1 Semiconductor and Its Impact _______________________________________________ 1 1.2 Fundamentals of Semiconductor Nanocrystals ___________________________________ 3 1.3 Synthetical Approach for Colloidal Nanocrystal: The Hot-Injection Method __________ 16 1.4 Cesium Lead Halide Perovskites ____________________________________________ 24 1.5 Current Obstacles of Lead Halide Perovskite: Instability and Lead Toxicity __________ 30 1.6 Common Characterization Techniques ________________________________________ 36 1.7 The Outline of This Dissertation and The Scope of Phd Projects ___________________ 39 Chapter 2 The Hidden Role of Oleic Acid in Cs-Oleate Reagent for Perovskite Nanocrystal Synthesis ___________________________________________________________________ 56 2.1 Introduction _____________________________________________________________ 57 2.2 Experimental Sections ____________________________________________________ 59 2.3 Results and Discussion ____________________________________________________ 62 2.4 Conclusion _____________________________________________________________ 74 Chapter 3 Enhanced Structural Stability of Colloidal α-CsPbI3 NCs in Solution Phase with Trioctylphosphine ___________________________________________________________ 81 3.1 Introduction _____________________________________________________________ 82 3.2 Experimental Sections ____________________________________________________ 84 3.3 Results and Discussion ____________________________________________________ 86 3.4 Conclusion _____________________________________________________________ 94 Chapter 4 Ligand-Mediated Water Resistance Stability Enhancement for CsPbBr3 Perovskite Nanocrystals _____________________________________________________ 100 4.1 Introduction ____________________________________________________________ 100 4.2 Experimental Sections ___________________________________________________ 102 4.3 Results and Discussion ___________________________________________________ 106 4.4 Conclusion ____________________________________________________________ 112 Chapter 5 The Synthesis of Pb-Free Perovskites: Vacancy-Ordered Double Perovskite Cs2SnI6 and Perovskite Alternative Cs3Bi2Br9 ___________________________________ 117 5.1 Introduction ____________________________________________________________ 117 IV 5.2 Experimental Sections ___________________________________________________ 121 5.3 Results and Discussion ___________________________________________________ 123 5.4 Conclusion ____________________________________________________________ 132 Chapter 6 Synthesis Of Lead-Free Cs3Sb2Br9 Perovskite Nanocrystals with Enhanced Activity in Photocatalytic CO2 Reduction Reaction _______________________________ 139 6.1 Introduction ____________________________________________________________ 140 6.2 Experimental Sections ___________________________________________________ 141 6.3 Results and Discussion ___________________________________________________ 145 6.4 Conclusion ____________________________________________________________ 152 Chapter 7 Summary and Outlook ____________________________________________ 157 7.1 Summary ______________________________________________________________ 157 7.2 Future Perspective_______________________________________________________ 160 Appendix A Supporting Information for Chapter 2 ______________________________ 162 A.1 Extra Control Experiments for Soluble CsOL Preparation _______________________ 162 A.2 Pure CsOL Powders Synthesis and NMR Characterization _______________________ 163 A.3 Precursor Characterization ________________________________________________ 168 A.4 Electrostatic Potential Calculation for Cs Butanoate ____________________________ 170 Appendix B Supporting Information for Chapter 6 ______________________________ 172 B.1 Additional Morphological Characterization for Cs3Sb2Br9 NCs ___________________ 172 B.2 XPS of Cs3Sb2Br9 and CsPbBr3 NCs ________________________________________ 173 B.3 DFT Calculations for Band Structure and Reaction Pathway _____________________ 176 B.4 Characterizations of CsPbBr3 And Cs3Sb2Br9 NCs _____________________________ 182 B.5 Transient Absorption ____________________________________________________ 183 Appendix C Materials Characterizations ______________________________________ 186 Appendix D Copyright Documents ____________________________________________ 189 Curriculum Vitae ___________________________________________________________ 191 V List of Figures Figure 1.1 A band diagram for a light emitting diode device. The injection of electron and hole from cathode and anode will result in the recombination of electron and hole in the semiconductor layer, which in turn will emit light. ___________________________ 2 Figure 1.2 Shapes of the 1s orbital (red), the 2p orbitals (yellow), the 3d orbitals (blue) and the 4f orbitals (green). ______________________________________________________ 5 Figure 1.3 (a) Construction of MOs from two AOs; (b) Energy diagram for MOs constructed from AOs. __________________________________________________________ 7 Figure 1.4 The bonding and antibonding orbitals in MAPbI3. ____________________________ 7 Figure 1.5 Evolution of atomic-molecular levels into bands and the formation of valence and conduction bands by overlapping s and p orbitals in a semiconductor. EF is the Fermi energy. _____________________________________________________________ 8 Figure 1.6 Band diagrams for conductor, semiconductor and insulator. ____________________ 9 Figure 1.7 The band structure evolution with respect of the size of a semiconductor system. Bulk, NC (from tens of atoms to a few hundred of atoms) and molecule (few atoms) band diagrams. __________________________________________________________ 10 Figure 1.8 The Brus calculation for the
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