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The University of Chicago Next Generation Synthetic THE UNIVERSITY OF CHICAGO NEXT GENERATION SYNTHETIC ROUTES TO COLLOIDAL III-V QUANTUM DOTS A DISSERTATION SUBMITTED TO THE FACULTY OF THE DIVISION OF THE PHYSICAL SCIENCES IN CANDIDACY FOR THE DEGREE OF DOCTOR OF PHILOSOPHY DEPARTMENT OF CHEMISTRY BY VISHWAS SRIVASTAVA CHICAGO, ILLINOIS AUGUST 2018 TABLE OF CONTENTS List of Figures ................................................................................................................... vii List of Tables ................................................................................................................... xiv Acknowledgments..............................................................................................................xv Abstract ........................................................................................................................... xvii CHAPTER 1: An Introduction to colloidal semiconductor nanocrystals ....................1 CHAPTER 2: Aminoarsines as arsenic precursors for the synthesis of metal arsenide nanocrystals ......................................................................................................................14 2.1 Introduction .................................................................................................................14 2.2 DIBAL-H mediated synthesis of InAs Nanocrystals ..................................................16 2.3 Effect of DIBAL-H concentration and temperature on NC size .................................18 2.4 Structural Characterization of InAs NCs ....................................................................21 2.5 Synthesis of InAs/CdSe core-shell NCs for NIR emission ..........................................24 2.6 Aminoarsines as general arsenic precursors: Synthesis of Cd3As2 NCs ......................25 2.7 Conclusions ..................................................................................................................28 2.8 References ....................................................................................................................28 ii CHAPTER 3: Role of reducing agents in Aminoarsines based synthesis of InAs Quantum Dots: Search for an optimal reducing agent ..................................................................31 3.1 Introduction .................................................................................................................31 3.2 Control of Precursor conversion kinetics in nanocrystal synthesis ............................33 3.3 Comparison of InAs QDs synthesized using different reducing agents .....................34 3.4 Monodisperse InAs QDs synthesized using DMEA-AlH3 complex ...........................38 3.5 Amorphous InAs clusters as growth precursors for InAs QDs....................................43 3.6 Tunable Near IR emission from InAs QDs..................................................................44 3.7 Conclusions ..................................................................................................................45 3.8 References ....................................................................................................................46 CHAPTER 4: Colloidal GaAs Nanocrystals .................................................................48 4.1 Introduction .................................................................................................................48 4.1.1 Prior attempts on synthesis of colloidal GaAs .........................................................48 4.1.2 Unusual Optical Properties of GaAs NCs ................................................................49 4.1.3 A Novel synthetic approach to GaAs NCs ...............................................................50 4.2 Superhydride mediated synthesis of GaAs NCs ..........................................................51 4.2.1 General Considerations .............................................................................................51 4.2.2 Optimized synthesis of GaAs NCs ...........................................................................51 4.3 Surface treatment of GaAs NCs ...................................................................................54 iii 4.4 Size selective precipitation to achieve monodisperse GaAs population ......................56 4.5 Absorption Spectroscopy of GaAs NCs ......................................................................60 4.5.1 Steady state Absorption spectra and Extinction Coefficients ...................................60 4.5.2 Transient Absorption Studies ....................................................................................62 4.6 Characterization of disorder in GaAs NCs ..................................................................63 4.6.1 Raman Spectrum shows amorphous characteristics .................................................63 4.6.2 EXAFS Studies point to imbalanced stoichiometry .................................................64 4.6.3 EPR Spectroscopy shows Ga vacancies ...................................................................66 4.7 Conclusions ..................................................................................................................67 4.8 References ....................................................................................................................68 CHAPTER 5: Molten salts as solvents for the processing of colloidal nanomaterials ...................................................................................................................72 5.1 Introduction .................................................................................................................72 5.2 Choice of molten salts and Ionic liquids and their NC dispersions ............................74 5.3 SAXS studies on NCs in molten salts and Ionic liquids .............................................76 5.4 Chemical binding between nanocrystals and molten salts ...........................................83 5.5 PDF studies on nanocrystal/molten salt dispersions ....................................................84 5.6 Conclusions and potential applications of NC dispersions in molten salts .................87 iv 5.7 References ....................................................................................................................88 CHAPTER 6: Curing structural defects in colloidal GaAs NCs via molten salt annealing ...........................................................................................................................91 6.1 Introduction .................................................................................................................91 6.2 High temperature annealing of GaAs films ................................................................93 6.3 Dispersion of colloidal GaAs NCs in molten salts .....................................................95 6.4 Molten Salt annealed GaAs NCs: Structural Properties ..............................................96 6.5 Molten salt annealed GaAs NCs: Optical Properties .................................................100 6.6 Conclusions ...............................................................................................................103 6.7 References ..................................................................................................................103 CHAPTER 7: Cation exchange reactions in molten salts: Synthesis of Luminescent In1- xGaxP and In1-xGaxAs Quantum Dots ..........................................................................105 7.1 Introduction ...............................................................................................................105 7.2 Experimental methodology for cation exchange reactions in molten salts ...............107 7.2.1 Ligand exchange on Inp and InAs QDs .................................................................108 7.2.2 Dispersion of InP and InAs QDs in Molten salt and cation exchange into In1-xGaxP and In1-xGaxAs QDs .......................................................................................................109 7.3 Structural properties of Ternary In1-xGaxP and In1-xGaxAs QDs ..............................110 7.4 Morpholological characterization of ternary In1-xGaxP and In1-xGaxAs QDs ...........114 v 7.5 Optical properties of ternary In1-xGaxP and In1-xGaxAs QDs ....................................120 7.5.1 Optical properties of ternary In1-xGaxP QDs ..........................................................120 7.5.2 ZnS shell growth on In1-xGaxP QDs .......................................................................124 7.5.3 High temperature luminescence of In1-xGaxP/ZnS QDs ........................................128 7.5.4 Optical properties of ternary In1-xGaxAs QDs and its core-shells ..........................130 7.6 Conclusions ...............................................................................................................133 7.7 References ..................................................................................................................134 APPENDIX A: Characterization Techniques and Analysis ......................................138 APPENDIX B: Synthesis of Nanocrystals based on reported protocols ...................142 APPENDIX C: Synthesis of AsH3 ................................................................................144 vi List of Figures 1.1 Dependence of the band gap on the nanocrystal diameter for InP and CdSe ................5 1.2 Changes in the electronic structure of GaAs upon quantum
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