Washington University in St. Louis Washington University Open Scholarship Arts & Sciences Electronic Theses and Dissertations Arts & Sciences Spring 5-15-2017 Stellar and Interstellar Origins of Meteoritic Nanodiamonds Josiah Lewis Washington University in St. Louis Follow this and additional works at: https://openscholarship.wustl.edu/art_sci_etds Part of the Astrophysics and Astronomy Commons, and the Physics Commons Recommended Citation Lewis, Josiah, "Stellar and Interstellar Origins of Meteoritic Nanodiamonds" (2017). Arts & Sciences Electronic Theses and Dissertations. 1123. https://openscholarship.wustl.edu/art_sci_etds/1123 This Dissertation is brought to you for free and open access by the Arts & Sciences at Washington University Open Scholarship. It has been accepted for inclusion in Arts & Sciences Electronic Theses and Dissertations by an authorized administrator of Washington University Open Scholarship. For more information, please contact [email protected]. WASHINGTON UNIVERSITY IN ST. LOUIS Department of Physics Dissertation Examination Committee: Ryan Ogliore, Chair Christine Floss, Co-Chair Erik Henriksen Dieter Isheim Martin Israel Rita Parai Stellar and Interstellar Origins of Meteoritic Nanodiamonds by Josiah Benjamin Lewis A dissertation presented to The Graduate School of Washington University in partial fulfillment of the requirements for the degree of Doctor of Philosophy May 2017 St. Louis, Missouri © 2017, Josiah Benjamin Lewis Table of Contents List of Figures ................................................................................................................................ vi List of Tables ............................................................................................................................. xxiii Acknowledgments...................................................................................................................... xxiv Abstract ...................................................................................................................................... xxix Chapter 1: Introduction ................................................................................................................... 1 1.1 Presolar grains .................................................................................................................. 1 1.2 Nanodiamonds .................................................................................................................. 7 1.2.1 Stellar Evolution and the Nucleosynthesis of Carbon ......................................................... 12 1.2.2 Type II Supernovae ............................................................................................................. 14 1.2.3 Other Presolar Source Candidates ....................................................................................... 16 1.2.4 Evidence for Solar System Formation of Nanodiamonds ................................................... 17 1.2.5 Experimental Considerations .............................................................................................. 18 1.3 Outline of the Following Chapters ................................................................................. 19 1.4 References ...................................................................................................................... 20 Chapter 2: Experimental and Analysis Methods .......................................................................... 25 2.1 Materials ......................................................................................................................... 27 2.2 NanoSIMS ...................................................................................................................... 28 2.3 Atom-probe Tomography ............................................................................................... 29 2.3.1 Multilayer Preparation ........................................................................................................ 29 2.3.2 Focused Ion Beam Liftout of Multilayers ........................................................................... 31 2.3.3 Micropost Preparation on Prefabricated Arrays .................................................................. 38 2.3.4 Micropost Preparation on Electropolished Cu Half-grids ................................................... 39 2.3.5 Focused Ion Beam Sharpening of Microtips ....................................................................... 40 2.3.6 Transmission Electron Microscopy..................................................................................... 43 2.3.7 Atom-probe Data Collection ............................................................................................... 44 2.3.8 Atom-probe Data Reduction ............................................................................................... 51 2.4 References ...................................................................................................................... 57 Chapter 3: Origin of Nanodiamonds from Allende Constrained by Statistical Analysis of C Isotopes from Small Clusters of Acid Residue by NanoSIMS ..................................................... 60 ii 3.1 Introduction .................................................................................................................... 60 3.2 Methods .......................................................................................................................... 66 3.2.1 Samples ............................................................................................................................... 66 3.2.2 Data Collection ................................................................................................................... 67 3.3 Data Reduction ............................................................................................................... 74 3.3.1 Bulk Ratio Analysis ............................................................................................................ 75 3.3.2 Broadening Analysis ........................................................................................................... 77 3.3.3 Outlier Analysis .................................................................................................................. 80 3.3.4 Detection Limit Calculation ................................................................................................ 82 3.4 Results ............................................................................................................................ 83 3.4.1 Bulk 12C/13C Ratio ............................................................................................................... 83 3.4.2 Outlier Ratios ...................................................................................................................... 84 3.4.3 Broadening of Ratio Distributions ...................................................................................... 93 3.4.4 Silicon-containing Materials in the Allende Residue .......................................................... 95 3.4.5 Detection Limits .................................................................................................................. 96 3.5 Discussion ...................................................................................................................... 98 3.5.1 12C/13C Ratio of the Nanodiamond Residues ...................................................................... 98 3.5.2 Implications of Gaussian Broadening ................................................................................. 99 3.5.3 Source of 12C/13C Outliers ................................................................................................. 100 3.6 Summary ...................................................................................................................... 103 3.7 Acknowledgements ...................................................................................................... 104 3.8 References .................................................................................................................... 105 Chapter 4: Atom-Probe Analyses of Nanodiamonds from Allende ........................................... 109 4.1 Introduction .................................................................................................................. 109 4.2 Analytical method: Atom-probe Tomography ............................................................. 113 4.3 Samples ........................................................................................................................ 117 4.4 Sample Preparation Methods ....................................................................................... 117 4.4.1 Chicago Methods .............................................................................................................. 117 4.4.2 St. Louis Method ............................................................................................................... 119 4.5 Data Processing ............................................................................................................ 121 4.5.1 Uncertainties on Carbon Isotope Peak Ratios ................................................................... 121 4.6 Results and Discussion ................................................................................................. 129 iii 4.6.1 Mass Spectra and Tomographic Reconstructions ............................................................