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Probing the Interstellar Medium Using Laboratory Samples

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Probing the Interstellar Medium Using Laboratory Samples PROBING THE INTERSTELLAR MEDIUM USING LABORATORY SAMPLES A thesis submitted to the University of Manchester for the degree of Doctor of Philosophy in the Faculty of Engineering and Physical Sciences 2010 Ashley King School of Earth, Atmospheric and Environmental Sciences CONTENTS Contents 2 - 9 i. List of Figures 6 - 8 ii. List of Tables 9 Abstract 10 Declaration 11 Copyright Statement 12 Author 13 Acknowledgements 14 - 15 Dedication 16 Chapter 1: Introduction and Literature Review 17 - 56 1.1 INTRODUCTION 17 1.1.1 Stellar Environments 19 1.1.2 Interstellar Medium 20 1.1.3 Early Solar Nebula 20 1.2 STELLAR FORMATION AND EVOLUTION 22 1.2.1 H-burning 23 1.2.2 Red Giant Branch 24 1.2.3 Asymptotic Giant Branch 26 1.2.4 Novae and Supernovae 28 1.2.5 S- and R-process Nucleosynthesis 30 1.2.5.1 S-process 30 1.2.5.2 R-process 31 1.3 PRESOLAR GRAINS 33 1.3.1 Formation of Presolar Grains 33 1.3.2 Interstellar Processing 34 1.3.3 Discovery and Separation of Presolar Grains 35 1.3.4 Analysis of Presolar Grains 38 1.3.5 Presolar SiC 40 1.3.5.1 Noble Gases 40 1.3.5.2 C, N and Si 41 1.3.5.3 Trace Elements 45 1.3.5.4 Structure and Morphology 47 1.3.6 Presolar Graphite 48 1.3.7 Presolar Nanodiamonds 49 1.3.8 Presolar Silicates 50 1.3.9 Presolar Oxides 50 2 1.3.10 Presolar Silicon Nitride 51 1.4 CARBON IN THE SOLAR SYSTEM 52 1.5 THESIS AIMS AND OUTLINES 55 Chapter 2: Methodology and Analytical Techniques 57 - 78 2.1 TIME-OF-FLIGHT SECONDARY ION MASS SPECTROMETRY 57 2.1.1 Secondary Ion Mass Spectrometry 57 2.1.2 Primary Ion Gun 60 2.1.3 Mass Resolution 61 2.1.4 Isotopic Ratios 63 2.1.5 Elemental Abundances 65 2.1.6 Interstellar Dust Laser Explorer (IDLE3) 66 2.1.7 Depth-Profiling 67 2.1.8 Data Processing 69 2.2 NanoSIMS 71 2.3 ENVIRONMENTAL SCANNING ELECTRON MICROSCOPE (ESEM) 74 2.4 RAMAN SPECTROSCOPY 75 2.5 FOCUSED ION BEAM (FIB) AND TRANSMISSION ELECTRON MICROSCOPY (TEM) 77 Chapter 3: Determination of relative sensitivity factors during + + secondary ion sputtering of silicate glasses by Au , Au2 + and Au3 ions 79 - 95 3.1 INTRODUCTION 79 3.2 EXPERIMENTAL PROCEDURE 81 3.3 RESULTS 83 3.4 DISCUSSION 92 3.5 CONCLUSION 94 Chapter 4: Trace element depth-profiles in presolar silicon carbide grains 96 - 147 4.1 INTRODUCTION 97 4.2 EXPERIMENTAL PROCEDURE 100 4.2.1 Samples 100 4.2.2 Analytical Procedure 101 4.2.3 Mass Resolution 102 3 4.2.4 Element Quantification 104 4.2.5 Depth-Profiling Procedure 106 4.2.6 Limitations of Depth-Profiling 108 4.3 RESULTS 110 4.3.1 Isotopes 110 4.3.2 Average Grain Data 111 4.3.3 Depth-Profiles 113 4.3.3.1 Grain Surface 114 4.3.3.2 Below the Grain Surface 120 4.3.3.3 Flat Depth-Profiles 121 4.4 DISCUSSION 121 4.4.1 Average Abundance Patterns 121 4.4.2 Contamination 123 4.4.3 Condensation 125 4.4.4 Interstellar Medium 125 4.4.5 Profiles with Variations beneath the Grain Surface 126 4.4.6 Profiles with Variations from the Grain Surface 129 4.4.7 Flat Profiles 131 4.4.8 Implications 132 4.5 SUMMARY 133 4.6 ADDITIONAL DATA 134 4.6.1 A geometrical model to estimate the effects of primary ion beam mixing when there is a steep elemental abundance gradient between two layers in a grain 134 4.6.2 Trace element depth-profiles within individual presolar SiC grains 137 Chapter 5: Amorphous carbon grains in the Murchison meteorite 148 – 180 5.1 INTRODUCTION 149 5.2 EXPERIMENTAL PROCEDURE 152 5.2.1 Adapted Gentle Separation Procedure 152 5.2.2 Samples 154 5.2.3 TOFSIMS 155 5.2.4 NanoSIMS 157 5.2.5 Raman Spectroscopy 159 5.2.6 TEM 163 5.3 RESULTS 164 5.3.1 Grain Abundances, Sizes and Morphologies 164 5.3.2 Isotopic Ratios 165 5.3.3 Raman Spectroscopy 166 5.3.4 TEM 170 4 5.4 DISCUSSION 171 5.4.1 Contamination 171 5.4.2 Effects of SIMS and Raman Analyses 172 5.4.3 Amorphous Carbon 173 5.4.4 Origins of Amorphous Carbonaceous Grains 176 5.5 SUMMARY 179 Chapter 6: Summary and Future Work 181 - 187 6.1 ANALYTICAL DEVELOPMENTS 181 6.2 TRACE ELEMENTS IN PRESOLAR SiC 182 6.3 AMORPHOUS CARBONACEOUS GRAINS 183 6.4 DISCUSSION AND FUTURE WORK 185 References 188 - 210 5 Total Word Count: 48,006 i. List of Figures Chapter 1 Figure 1.1 Cartoon of the journey presolar grains take from parent star to the laboratory 19 Figure 1.2 Hertzsprung-Russell diagram of stellar evolution 24 Figure 1.3 Internal structure of a red giant branch star 25 Figure 1.4 Internal structure of an asymptotic giant branch star 27 Figure 1.5 Onion shell model of nucleosynthesis in massive stars 29 Figure 1.6 S-process pathways in the Kr-Rb-Sr region of the chart of the nuclides 30 Figure 1.7 S- and R-process pathways on the chart of the nuclides 32 Figure 1.8 Flow-diagram of the Chicago procedure used to extract presolar SiC grains from meteorites 37 Figure 1.9 Noble gas components measured in bulk presolar SiC samples 41 Figure 1.10 12C/13C versus 14N/15N in presolar SiC grains 42 Figure 1.11 Silicon three-isotope plot for presolar SiC grains 43 Figure 1.12 Example SEM images of presolar graphite grains of onion and cauliflower morphologies 49 Figure 1.13 Oxygen isotopic compositions of presolar oxide grains 51 Chapter 2 Figure 2.1 Schematic diagram of a TOFSIMS instrument 58 Figure 2.2 Energy spread of atomic secondary ions released during sputtering with a primary ion beam 59 Figure 2.3 Schematic diagram of the TOFSIMS primary ion gun and optics 60 Figure 2.4 Sketch of IDLE3 TOFSIMS instrument 67 Figure 2.5 Schematic diagram of the co-axial design of the NanoSIMS 72 Figure 2.6 Typical Raman carbon spectra from IOM in primitive meteorites, amorphous carbon and terrestrial coal 76 Chapter 3 Figure 3.1 Practical secondary ion yields for Na, Mg, Al, Si, K, Ca, Ti, + V, Cr, Mn and Fe when analyzing silicate glass with Au2 and + + Au3 relative to Au primary ions 84 Figure 3.2 RSFs obtained in silicate glasses using a delayed relative to normal secondary ion extraction technique, versus element mass 92 Figure 3.3 Comparison of RSFs for Li, B, O, Na, Mg, Al, Si, K, Ca, Ti, V, Cr, Mn, Fe, Rb, Sr, Cs and Ba in silicate glasses when analyzing with Au+ and Ga+ primary ions 93 Chapter 4 6 Figure 4.1 Comparison of RSFs for Al, Ca and Fe obtained from silicate glasses and SiC using Au+ primary ions 105 Figure 4.2 Trace element depth-profile through a Murchison matrix silicate grain 107 Figure 4.3 Silicon three-isotope plot of analyzed SiC grains 111 Figure 4.4 Average abundances of Mg, Fe, Ca, Al, Ti and V relative to Si and CI abundances in analyzed SiC grains, and comparison to data from other studies using TOFSIMS and DC-SIMS 112 Figure 4.5 Representative trace element depth-profiles in analyzed SiC grains showing abundance variations either from or below the grain surfaces, or displaying no variation 119 Figure 4.6 SRIM calculations simulating the implantation of Li, B, Al, Ca and Ti ions into a 1μm SiC grain at a velocity of 1000kms-1 128 Additional Data Figure 4a.1 Set-up of geometrical model used to show the effects of primary ion beam mixing between layers of differing elemental abundance 134 Figure 4a.2 Results of geometrical model used to show the effects of primary ion beam mixing between layers of differing elemental abundance 136 Figure 4a.3 Trace element depth-profile for grain AK-MM2-G-1 137 Figure 4a.4 Trace element depth-profile for grain AK-MM2-G-2 138 Figure 4a.5 Trace element depth-profile for grain AK-MM2-M-1 139 Figure 4a.6 Trace element depth-profile for grain AK-MM2-N-1 140 Figure 4a.7 Trace element depth-profile for grain AK-MM2-delta-1 141 Figure 4a.8 Trace element depth-profile for grain AK-MM2-delta-2 142 Figure 4a.9 Trace element depth-profile for grain AK-MM2-5-1 143 Figure 4a.10 Trace element depth-profile for grain AK-KJG-D-1 144 Figure 4a.11 Trace element depth-profile for grain AK-KJG-D-2 145 Figure 4a.12 Trace element depth-profile for grain AK-KJG-M-1 146 Figure 4a.13 Trace element depth-profile for grain AK-KJG-6-1 147 Chapter 5 Figure 5.1 Final size and density fractions from the gentle separation procedure adapted for presolar graphite 153 Figure 5.2 ESEM images of carbonaceous grains of “Flake”, “Elongated” and “Blocky” morphologies 155 Figure 5.3 Comparison of Raman carbon spectra from a terrestrial graphite grain, Allende IOM, and analyzed carbonaceous grains B4a-W-1 and B4b-7-1 162 Figure 5.4 Raman carbon D-band characteristics of analyzed carbonaceous grains compared to IOM, IDPs and cometary samples 169 Figure 5.5 Raman carbon G-band characteristics of analyzed carbonaceous grains compared to IOM, IDPs and 7 cometary samples 170 Figure 5.6 TEM images and SAED patterns from analyzed carbonaceous grains B4a-X-1, B4a-Q-1and C4a-D-1 171 Figure 5.7 Comparison of Raman carbon G-band characteristics of analyzed carbonaceous grains and irradiated terrestrial soot 175 8 ii.
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