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Study of Gas-Phase Reactions in Tio2 Production and Functionalised Thin Films Engd Thesis

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Study of Gas-Phase Reactions in Tio2 Production and Functionalised Thin Films Engd Thesis Study of Gas-Phase Reactions in TiO2 Production and Functionalised Thin Films EngD Thesis Ben Blackburn Supervisors Prof. Ivan Parkin Prof. Claire Carmalt Disclaimer I Ben Blackburn confirm that the work presented in this thesis is my own. Where information has been derived from other sources, I confirm that this has been indicated in the thesis. Signed: .................................................................................. Acknowledgements This project was funded by contributions from Huntsman Pigments, the EPSRC as well as the UCL EngDoc Center. I would like to thank Professors Ivan Parkin and Claire Carmalt for their guidance and support throughout this project, as well as Dr. Stephen Sutcliffe and Andrew Brown at Huntsman Pigments and Additives for providing and industrial insight to the work done. In addition thanks are owed to Dr. Jared Crane for his assistance in handling and analysis of TiCl4 samples and inorganic synthesis. Dr. Caroline Knapp, Dr. Peter Marchand, Dr. David Pugh for assistance in determining molecular structures using X-ray crystallography, Dr. Kristopher Page for assistance in procuring reagents, Dr. Steve Firth for instruction in Raman Spectrosocopy, Dr. Andreas Kafizas for assistance with X-ray diffraction analysis, Dr. Michael Parkes and Dr. Kirsty Karu for assistance mass spectroscopy, Dr. Michael Powell, Dr. Carlos Sotelo-Vazquez, Dr. Raul Quesada- Cabrera for their instruction in testing the thermochromic nature of thin films determining solar modulation and Dean Brett, Charalampos Drosos for their contributions to the deposition of thin films. This thesis is dedicated to Amy, whose love, friendship and patience has made the last four years easier in every possible way. iii Abstract Titanium dioxide (TiO2) is a pigment used in the whitening of millions of products from paint to foodstuffs. Produced via purification of ores using the Chloride Process, the mined TiO2 ore is chlorinated along with all of the impurities. The resulting TiCl4 is a liquid at room temperature and can be separated from its impurities using distillation. V2O5, an impurity present in this ore is converted to vanadium oxytrichloride (VOCl3) which is too similar in boiling point to TiCl4 to separate via distillation and instead is removed via addition of an oil, which preferably binds to VOCl3. This work, sponsored by Huntsman Pigments and Additives, seeks to better understand this reaction, as well as other aspects of the Chloride Process. This is achieved by analysing industrial samples as well as producing lab scale models for the process and investigating inorganic synthesis of analogous compounds [TiCl4{CH2(CO2CH(CH3)2}2] [1a], [(µ-O)(TiCl3{CH2(CO2CH(CH3)2}2)] [1b], [TiCl4{CH2(CO2CH(C6H5)}2] [2], [TiCl4{C2H4(CO2CH3)}2] [3], VOCl3+glycerol tribenzoate [4], [VOCl2(acac)] [5], [{VOCl2(CH2(CO2Et)2}4] [6] and [VOCl2{C2H4(CO2Et)2}]n [7] that were characterised via single crystal X-ray diffraction analysis (with the exception of 4) Alongside this study, multiple side projects were undertaken that sought to use some of the novel materials produced in materials synthesis, due to the useful nature of both TiO2 and VO2 in window coating applications, the abundance of oxygen in the products making them good contenders for metal oxide precursors. This included the deposition of TiO2 /SiO2 thin films for photocatalytic self cleaning applications, VO2 thin films for energy saving windows and VC/VN particles for mechanical hardening applications. In addition, a new system for the in-situ study of high temperature gas phase inorganic reactions via mass spectroscopy was developed and used to study the reactivity of gaseous TiCl4 and VOCl3, as well as several other species including vanadium chloride, titanium isopropoxide and butyltin trichloride considered to be of greater interest to the field of thin film deposition. iv Contents Disclaimer ii iii Acknowledgements iv Abstract v Contents x List Of Figures xviii List Of Tables xiv List Of Schemes xx List Of Abbreviations 1. Introduction 1 1.1. Project Overview 1 1.2. Titanium Dioxide 2 1.2.1. Structure and Phases 2 3 1.2.2. Uses of TiO2 1.3. Titanium Dioxide Production 6 1.3.1. The Sulfate Process 7 1.3.2. The Chloride Process 9 1.3.3 Issues with the Tioxide Production Process 14 1.4 Titanium(IV) Tetrachloride 16 2. Analysis of Samples from Industrial TiO₂ Production 19 19 2.1. NMR study of Industrial TiCl4 Samples 19 2.1.1. Experimental 2.1.1.1. Making an NMR sample 19 2.1.1.2. Distilling Titanium Chloride Samples 21 22 2.1.2. Results and Discussion 2.1.2.1. Initial Study 22 24 2.1.2.2. Comparison of Recent and Older TiCl4 Samples 2.1.2.3. Lab-distilled Primary Titanium Tetrachloride Samples 26 2.1.2.3a. The First 20 ml of Distillate 26 2.1.2.3b. The Second 60 ml of Distillate 26 2.1.2.3c. The Third 20 ml of Distillate 29 2.1.2.4. Investigation of Aging in Distilled Fractions 30 2.1.3. Conclusion 32 v 35 2.2. Analysis of the Black Precipitate in the Tetra Samples 2.2.1. Experimental 36 2.2.2. Results and Discussion 37 2.2.2.1. NMR spectroscopy 37 2.2.2.2. Toluene Washings 37 2.2.2.3. Mass Spectroscopy 38 2.2.2.4. Infrared Spectroscopy 39 2.2.2.5. Energy dispersive X-ray Spectroscopy 41 2.2.2.6. X-ray Photoelectron Spectroscopy 43 2.2.3. Conclusion 44 3. Reaction of Titanium Chloride and Vanadium Oxytrichloride 47 with Diester and Triester Molecules as Analogues for Oil 47 3.1. Introduction 50 3.2. Experimental 3.2.1. Synthesis of tetrachloro(diisopropyl malonate)-titanium(IV) [1] 50 3.2.2. Synthesis of tetrachloro(dibenzyl malonate)-titanium(IV) [2] 51 3.2.3. Synthesis of tetrachloro(diethyl succinate)-titanium(IV) [3] 51 3.2.4. Synthesis of complex of titanium(IV) chloride with glycerol tribenzoate [4] 52 3.2.5. Synthesis of dichloro(oxo)(2, 4-Pentanedione) vanadium(V) [5] 53 3.2.6. Synthesis of dichloro(oxo)(diethyl malonate) vanadium(V) [6] 53 3.2.7. Synthesis of VOCl3 Bis-isopropyl malonate Complex [7] 54 54 3.2.8. Synthesis of dichloro(oxo)(diethyl succinate) vanadium(V) [8] 54 3.2.9. Synthesis Of Glycerol tribenzoate VOCl3 [9] 3.2.10. Crystallography 55 56 3.3. Results and Discussion 3.3.1. Interaction of TiCl4 with Diester Ligands 56 3.3.1.1. Tetrachloro(diisopropyl malonate)-titanium(IV) [1a] 57 3.3.1.2. Bis-trichloro-µ-oxo-(diisopropyl malonate)-titanium(IV) [1b] 61 3.3.1.3. Tetrachloro(dibenzyl malonate)-titanium(IV) [2] 63 3.3.1.4. Tetrachloro(diethyl succinate) titanium(IV) [3] 66 69 3.3.2. Interaction of TiCl4 with Triglyceride Analogue Glycerol Tribenzoate [4] 73 3.3.3. Interaction of Glycerol Tribenzoate and Diesters With VOCl3 74 3.3.3.1. Dichloro(oxo) (2,4-Pentanedione) vanadium(V) [5] 78 3.3.3.2. Dichloro(oxo) (diethyl malonate) vanadium(V) [6] 83 3.3.3.3. Dichloro(oxo)(diethyl succinate) vanadium (V) [7] 88 3.3.3.4. Reaction of VOCl3 with Other Species 91 3.4. Conclusion vi 4. Vanadium Removal Flow System 93 93 4.1. Introduction 95 4.2. Experimental 4.2.1. Soya Bean Oil Experiments 98 4.2.2. Analysis of Naphthenic Oils 99 101 4.3. Results and Discussion 4.3.1. Soya Bean Oil Analysis 101 101 4.3.1.1. TiCl4 + Soya Oil 107 4.3.1.2. VOCl3 + Soya Oil 108 4.3.1.3. TiCl4 + 1000 ppm VOCl3 + Soya Oil 109 4.3.1.4. TiCl4 + 40,000 ppm VOCl3 + Soya Oil 4.3.2. Naphthenic Oil Analysis 110 4.3.2.1. NMR of the Naphthenic Oils 112 4.3.2.2. Flow Cell Experiments 113 4.3.2.3. NMR Experiments with Flavex 977s 116 4.4. Conclusion 118 5. Using Mass Spectrometry to Study Gas Phase Reactions in 120 Chemical Vapour Deposition 120 5.1. Introduction 5.1.1. Atmospheric Pressure CVD 120 5.1.2. Using Mass Spectrometry to Study CVD 124 5.1.3. Mass Spectrometry 126 5.2. Experimental 130 5.2.1. Preliminary Experiments 134 5.2.1.1. Toluene Test Run 134 5.2.1.2. Purge Flow Test 135 5.2.2. Precursor Deposition 136 5.2.2.1. Ethyl Acetate 139 5.2.2.2. Titanium (IV) Tetrachloride 139 5.2.2.3. Vanadium (V) Oxytrichloride 140 5.2.2.4. Titanium(IV) Isopropoxide 141 5.2.2.5. Butyltin (IV) Trichloride 141 5.2.2.6. Vanadium(IV) Chloride 142 5.3. Results and Discussion 143 5.3.1. Ethyl Acetate 143 5.3.2. Titanium Tetrachloride 145 5.3.2.1. Mass Spectra Analysis 145 5.3.2.2 Thin Film Analysis 148 i) X-ray diffraction 148 ii) Scanning Electron Microscopy 148 vii 5.3.3. Vanadium Oxytrichloride 150 5.3.3.1. Mass Spectra Analysis 150 5.3.3.2 Thin Film Analysis 152 i) X-ray Diffraction 152 ii) Scanning Electron Microscopy 155 5.3.4. Butyltin Trichloride 157 5.3.4.1. Mass Spectra Analysis 157 5.3.4.2 Thin Film Analysis 160 i) X-ray Diffraction 160 ii) Scanning Electron Microscopy 161 5.3.5. Titanium Isopropoxide 162 5.3.5.1. Mass Spectrometry Analysis 163 5.3.5.2. Thin Film Analysis 167 i) X-ray Diffraction 167 ii) Scanning Electron Microscopy 168 5.3.6. Vanadium Tetrachloride 169 5.3.6.1. Mass Spectrometry Analysis 170 5.3.6.2. Thin Film Analysis 174 i) X-ray Diffraction 174 ii) X-ray Photoelectron Spectroscopy 175 iii) Scanning Electron Microscopy 177 5.4.
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