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Syntheses and Studies of Some Graphite and Graphite Fluoride

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Syntheses and Studies of Some Graphite and Graphite Fluoride SYNTHESES AND STUDIES OF SOME GRAPHITE AND GRAPHITE FLUORIDE INTERCALATION COMPOUNDS BY JUN XIA B.Sc, Wuhan University, Hubei, China, 1982 A THESIS SUBMITTED IN PARTIAL FULFILLMENT OF THE REQUIREMENT FOR THE DEGREE OF MASTER OF SCIENCE IN THE FACULTY OF GRADUATE STUDIES (Department of Chemistry) We accept this thesis as conforming to the required standard THE UNIVERSITY OF BRITISH COLUMBIA © J. XIA, August 1990 In presenting this thesis in partial fulfillment of the requirements for an advanced degree at the University of British Columbia, I agree that the Library shall make it freely available for extensive copying of this thesis for scholarly purposes may be granted by the head of my department or by his or her representatives. It is understood that copying or publication of this thesis for financial gain shall not be allowed without my written remission. Department of chemistry The University of British Columbia Vancouver, B.C. Canada Date October 11,1991 ABSTRACT The oxidative intercalation of S2O6F2 into graphite ( SP-1 powder) in the gas phase has been studied. X-ray powder diffraction spectra shows that stage-1, stage-2 and stage-3 graphite fluorosulfates have been obtained. The compositions of these three compounds are C7.8SO3F, C15.5SO3F and C24S03F according to gravimetry with the repeat space distances of 7.8lA, 11.08A and 14.33A respectively. X-ray photoelectron spectroscopy (XPS) has been extensively used to study some graphite acceptor intercalation compounds. Two effects have been observed, charge transfer leads to higher binding energy and Fermi Level shift to the lower binding energy relative to that of graphite. Graphite fluoride intercalation compounds of S2O6F2, HSO3F and HSO3CF3 have been synthesized by direct reactions. X-ray powder diffraction, XPS, IR, Raman and microanalysis have been employed to study these compounds. The results show that: A. There are some graphite islands in graphite fluorides, CFX t when x<l. B. The islands can be intercalated by S206F2 to form stage-1 intercalation compounds and by HSO3F and HSO3CF3 to form higher stage intercalation compounds. C. The intercalates for the intercalants of S2O6F2, HS03F andHS03CF3 are SO3F-, HSO3F and HS03CF3 respectively. ii TABLE OF CONTENTS Page ABSTRACT ii LIST OF TABLES viii LIST OF FIGURES ix GLOSSARY xii ACKNOWLEDGEMENT xiv CHAPTER 1 INTRODUCTION 1 1.1 General Introduction 2 1.2 Graphite 3 1.3 Graphite Intercalation Compounds 7 1.3.1 Intercalation of Graphite 7 1.3.2 Staging Phenomenon 10 1.3.3 Donor Intercalation Compounds 14 1.3.4 Acceptor Intercalation Compounds 17 1.3.5 Neither Donor nor Acceptor Compounds 18 1.3.6 Covalent Graphite Compounds 19 1.3.7 Synthesis of Graphite Acceptor Intercalation Compounds 19 m 1.4 Graphite Fluoride 26 1.4.1 Introduction 26 1.4.2 Preparation and Characterization 27 1.4.3 Structure 29 1.4.4 Properties 34 1.4.5 Applications 36 1.4.6 Graphite Intercalation Compounds of Fluorine 38 1.5 Purpose of This Work 39 CHAPTER 2 EXPERIMENTAL 41 2.1 General Comments 42 2.2 Apparatus 42 2.2.1 Glass Vacuum Line 42 2.2.2 Dry Atmosphere Box 43 2.2.3 Reaction Vessels 43 2.3 Instrumentation 50 2.3.1 I.R. Spectroscopy 50 2.3.2 Raman Spectroscopy 50 2.3.3 X-ray Powder Diffractometry 50 IV 2.3.4 X-ray Photoelectron Spectroscopy 51 2.3.5 Elemental Analyses 51 2.4 Preparation and Purification of Reagents and Chemicals 52 2.4.1 Graphite 52 2.4.2 Graphite Fluoride 52 2.4.3 S206F2 52 2.4.4 HSO3F 53 2.4.5 HSO3CF3 56 2.4.6 KSO3F and KSO3CF3 56 2.5 Synthetic Reactions 57 2.5.1 Graphite Fluorosulfate 57 2.5.2 Ci2S03CF3 58 2.5.3 C14SO3FHSO3F 58 2.5.4 C8SbF6 59 2.5.5 (CFx)nS03F 59 2.5.6 (CFx)nHS03F and (CFx)nHS03CF3 59 CHAPTER 3 GRAPHITE FLUOROSULFATES 61 3.1 Introduction 62 V 3.2 Stage One Compounds 64 3.3 Stage Two Compounds 67 3.4 Stage Three Compounds 73 3.5 Conclusion 75 CHAPTER 4 XPS OF SOME ACCEPTOR GRAPHITE INTERCALATION COMPOUNDS 76 4.1 Introduction 77 4.2 Graphite Fluorosulfates 80 4.3 C12SO3CF3 89 4.4 CFX * 92 4.5 Other Graphite Acceptor Intercalation Compounds 97 4.6 Conclusion 101 CHAPTER 5 GRAPHITE FLUORIDE AND THEIR INTERCALATION COMPOUNDS 102 5.1 Graphite Fluorides 103 5.2 Graphite Fluoride-S206F2 Intercalation Compounds 109 5.3 Graphite Huoride-HSC^F Intercalation Compounds 119 5.4 Graphite Fluoride-HS03CF3 Intercalation Compound 133 vi 5.5 Conclusion 141 SUMMARY AND CONCLUSIONS 142 REFERENCES 143 vii LIST OF TABLES Table Page 1.1 Anisotropy Factor for Various Types of Graphite 8 1.2 Intercalate Sandwich Thickness Is for Several Graphite Intercalation Compounds 16 1.3 Resistivity of CFX 35 3.1 X-ray Diffraction Data of C7.8SO3F 66 3.2 X-ray Diffraction Data of C15SO3F 72 3.3 X-ray Diffraction Data of C24SO3F 74 4.1 Binding Energies of Elements in SO3F" for Different Compounds 88 4.2 Binding Energies of SO3CF3" in Some Compounds 90 4.3 Binding Energies of CFx's 95 4.4 Cis Electron Binding Energies of graphite and Acceptor GICs 97 5.1 Composition of CFX-S206F2 Compounds 110 5.2 X-ray Diffraction Data of (CFo.5)7.9S03F 113 5.3 F Is 1/2 Binding Energy of the Compounds 117 5.4 Composition of CFX-HS03F 120 5.5 X-ray Diffraction Data of (CFo.25)45.9HS03F 125 5.6 X-ray Diffraction Data of (CF0.33)25.6HSO3F 126 5.7 X-ray Diffraction Data of (CFo.5)i5.5HS03F 127 5.8 X-ray Diffraction Data of (CF0.83)23.lHSO3F 128 5.9 Composition of CFX-HS03CF3 Intercalation Compounds 134 viii LIST OF FIGURES Figures page 1.1 Molecular Structure of Hexagonal Graphite 4 1.2 Molecular Structure of Rhombohedral Graphite 6 1.3 Staging in Graphite Intercalation 11 1.4 The Daumas-Herold Model for Staging 13 1.5 Interchange of Domains of Stage-3 and Stage-4 Regions 15 as Might Occur During a Stage Transformation 1.6 Apparatus for the Electrochemical Synthesis of Intercalation Compounds 22 1.7 Absorption Derivatives for 19F NMR in Graphite Fluorides 30 1.8 Possible Layer Structures for Poly( carbon monofluoride) 32 1.9 Bond Lengths and c-axis Length of (C2F)n 33 2.1 One Part Reactor and One Part Storage Vessel 44 2.2 Two Part Reaction Vessels 46 2.3 One Part Two Chamber Reactor 47 2.4 S2O6F2 Addition Trap 49 2.5 Reactor for Deintercalation Studies 49 2.6 Apparatus for the Preparation of S206F2 54 2.7 Fluorosulfuric Acid Distillation Apparatus 55 3.1 X-ray Powder Diffraction Spectra of Graphite and C7SO3F 65 3.2 X-ray Powder Diffraction Spectrum of C7.8SO3F 66 ix 3.3 XPS Spectra of C7.8S03F 68 3.4 X-ray Powder Diffraction Spectra of C7SO3F After Exposing to Moist Air and Water 69 3.5 X-ray Powder Diffraction Spectrum of C12.5SO3F 70 3.6 X-ray Powder Diffraction Spectrum of C15.5SO3F 72 3.7 X-ray Powder Diffraction Spectrum of C24SO3F 74 4.1 Density of Occupied and Empty State in the Materials and the Definition of the Fermi Level Ep and the Work Function <|>s 79 4.2 XPS Spectra of Graphite and C7S03F 82 4.3 Two Effects on Chemical Shift of Cis Electron Binding Energy, Fermi Level Motion and Electrostatic Attraction 83 4.4 XPS Spectra of C7SO3F-AU 85 4.5 XPS Spectra of KS03F and C7S03F 87 4.6 Structural Model of C7SO3F 88 4.7 XPS Spectrum of C12SO3CF3 90 4.8 Electrostatic Effect and Fermi Level Motion in XPS of Ci2S03CF3 91 4.9 XPS Spectra of CF0.5 93 4.10 XPS Spectra of CF1.0 94 4.11 XPS Spectra of CF2 96 4.12 XPS Spectra of Ci4S03HS03F 98 4.13 XPS Spectra of C8SbF6 99 4.14 XPS Spectra of CgAsF6 100 X 5.1 IR Spectra of Graphite Fluorides 104 5.2 X-ray Powder Diffraction Spectra of CFX 105 5.3 XPS Spectra of CFX 108 5.4 X-ray powder Diffraction Spectra of CFX-S206F2 111 5.5 XPS Spectra of CFX-S206F2 Intercalation Compounds 114 5.6 XPS Spectra of (CF0.83)l6.lSO3F and KSO3F 116 5.7 XPS Spectra of Residue of (CF0.83)i6.lSO3F 118 5.8 Intercalation Amounts of S206F2 and HSO3F into CFX 122 5.9 X-ray Powder Diffraction Spectra of CFx-HS03F 123 5.10 XPS Spectra of (CF0.83)23.lHSO3F 130 5.11 X-ray Powder Diffraction Spectrum of Residue of (CFo.83)23. iHS03F Deintercalation Compound 131 5.12 XPS Spectrum of Residue of (CF0.83)23.lHSO3F 131 5.13 Raman Spectrum of Collected Volatile of (CF0.5)i5.5HSO3F 132 5.14 IR Spectrum of (CFo.5)l7.75HS03CF3 135 5.15 X-ray Powder Diffraction Spectra of CFX-HS03CF3 Intercalation Compounds 137 5.16 XPS Spectra of (CF0.83)2l.78HSO3CF3 140 xi GLOSSARY 1. ACCEPTOR INTERCALATION COMPOUND: Compounds formed from electron acceptor intercalants in oxidative intercalation 2. BOUNDING LAYERS: The carbon layers adjacent to an intercalate layer 3. DEINTERCALATION: The process that occurs at elevated temperatures which produces the initial intercalants as well as other volatile decomposition products 4. DONOR INTERCALATION COMPOUND: Compounds formed from electron donor intercalants in reductive intercalation 5. INTERCALANT: The bulk reagent that provides atoms, molecules or ions for intercalation 6.
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