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Study of Homogeneous Thermal Decomposition Of STUDY OF HOMOGENEOUS THERMAL DECOMPOSITION OF TRIETHYLGALLIUM, TRIETHYLALUMINUM WITH AMMONIA AND TUNGSTEN DIMETHYLHYDRAZIDO COMPLEX USING IN SITU RAMAN SPECTROSCOPY AND COMPUTATIONAL CHEMISTRY By JOOYOUNG LEE A DISSERTATION PRESENTED TO THE GRADUATESCHOOL OF THE UNIVERSITY OF FLORIDA IN PARTIAL FULFILLMENT OF THE REQUIREMENTS FOR THE DEGREE OF DOCTOR OF PHILOSOPHY UNIVERSITY OF FLORIDA 2011 1 © 2011Jooyoung Lee 2 To my parents, wife and son 3 ACKNOWLEDGMENTS First of all, I’d like to thank God. Whatever I do and however I do, He has been with me. I have been pleased to work with Dr. Anderson including all group members. Dr. Anderson always has kept his eyes on my research and has encouraged the progress. Due to his belief in my studies, I could finish my doctoral research. I have enjoyed discussion with group members and that always gives me good ideas and breakthroughs. The morning coffee with them refreshes my thinking and gives me energy to work efficiently. I feel five years in Gainesville is very short. My wife, Hankyung Seong, always has given encouragement and energy to my research and I’d like to dedicated this dissertation to her. My only son, Geon, has been everything to my family and I hope five years of Gainesville life would be his blessings from the heavenly God. 4 TABLE OF CONTENTS page ACKNOWLEDGMENTS .................................................................................................. 4 LIST OF TABLES ............................................................................................................ 8 LIST OF FIGURES ........................................................................................................ 10 LIST OF ABBREVIATIONS ........................................................................................... 15 ABSTRACT ................................................................................................................... 18 INTRODUCTION ........................................................................................................... 20 APPLICATIONS OF RAMAN SCATTERING TO GAS PHASE DECOMPOSITION REACTIONS ........................................................................................................... 24 Theoretical Background of Raman Scattering ........................................................ 25 Classical Theory of Raman Scattering ............................................................. 26 Selection Rule .................................................................................................. 27 Raman Scattering Intensity and Cross-section ................................................. 28 Signal-to-Noise ................................................................................................. 30 CVD Reactor with Raman Spectrometer ................................................................ 31 Reactor Setup .................................................................................................. 31 Characteristics of Spectroscopic System ......................................................... 32 Applications of Raman Scattering ........................................................................... 34 Gas Phase ........................................................................................................ 34 Temperature determination ........................................................................ 34 Concentration measurement ...................................................................... 39 Liquid Phase ..................................................................................................... 40 Solid Phase ...................................................................................................... 42 Summary ................................................................................................................ 47 COMPUTATIONAL CALCULATIONS ........................................................................... 59 Vibrational Frequency ............................................................................................. 61 Classical Approach ........................................................................................... 61 Quantum Mechanical Approach ....................................................................... 62 Potential Energy Surfaces ...................................................................................... 65 Thermodynamic Properties ..................................................................................... 66 Contribution from Translation ........................................................................... 66 Contribution from Electronic Motion ................................................................. 67 Contribution from Rotational Motion ................................................................. 67 Contribution from Vibration ............................................................................... 68 Kinetic Parameters ................................................................................................. 69 5 Theoretical Raman Intensity and Absolute Differential Raman Cross-section ........ 72 The Selection of Basis Set ...................................................................................... 74 REACTOR MODELING AND PARAMETER ESTIMATION .......................................... 83 Mathematical Description of CVD Reactor .............................................................. 84 Parameter Estimation ............................................................................................. 86 Solving Inverse Problem Using Optimization Algorithm .......................................... 91 Summary ................................................................................................................ 93 INVESTIGATION OF THE THERMAL DECOMPOSITION OF TRIETHYLGALLIUM USING IN SITU RAMAN SPECTROSCOPY AND DFT CALCULATIONS ........... 103 Overview ............................................................................................................... 103 Experimental and Theoretical Methods................................................................. 104 Results and Discussion......................................................................................... 109 TEGa Thermal Decomposition Experiments Using in situ Raman Spectroscopy . 113 The Comparison of DFT Calculation with Experimental Results ........................... 115 Concluding Remarks............................................................................................. 116 HOMOGENEOUS THERMAL DECOMPOSITION STUDIES OF TRIETHYLALUMINUM (TEAL): EFFECT OF NH3 ................................................ 127 Overview ............................................................................................................... 127 Experimental and Theoretical Methods................................................................. 128 Results and Discussion......................................................................................... 130 Homogeneous TEAl Thermal Decomposition Experiments ............................ 130 DFT Calculations ............................................................................................ 134 The Comparison of Experimental Results with DFT Calculations .................. 136 Concluding Remarks............................................................................................. 137 EXPERIMENTAL AND COMPUTATIONAL STUDIES OF THE HOMOGENEOUS THERMAL DECOMPOSITION OF THE TUNGSTEN DIMETHYLHYDRAZIDO COMPLEX CL4(CH3CN)W(NNME2) DURING DEPOSITION OF WNXCY THIN FILMS ................................................................................................................... 145 Overview ............................................................................................................... 145 Experimental and Theoretical Methods................................................................. 146 Results and Discussion......................................................................................... 148 Kinetics of Acetonitrile Dissociation from 1a ................................................... 148 Ion Cyclotron Resonance Experiments .......................................................... 148 In situ Raman Experiments ............................................................................ 149 DFT Calculations ............................................................................................ 151 Comparison of Experimental Results with DFT calculations .......................... 153 Concluding Remarks............................................................................................. 158 DESIGN, SIMULATION AND SETUP OF ULTRA HIGH VACUUM SYSTEM FOR SURFACE SCIENCE AND ITS APPLICATION .................................................... 171 6 Overview ............................................................................................................... 171 Characterization of Surface Kinetics in UHV ......................................................... 172 Temperature Programmed Desorption (TPD) ................................................ 172 Low Electron Energy Diffraction (LEED) ........................................................ 173 Auger Electron Spectroscopy (AES) .............................................................. 174 Attenuated Total Reflection Using FTIR Spectroscopy (ATR-FTIR) ............... 175 Current state of ATR-FTIR technique .....................................................
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