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DEVELOPMENT of a DYNAMIC ATOM PROBE by Rita Kirchhofer

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DEVELOPMENT of a DYNAMIC ATOM PROBE by Rita Kirchhofer DEVELOPMENT OF A DYNAMIC ATOM PROBE By Rita Kirchhofer A thesis submitted to the Faculty and the Board of Trustees of the Colorado School of Mines in partial fulfillment of the requirements for the degree of Doctor of Philosophy (Materials Science). Golden, Colorado Date ______________ Signed: _____________________________ Rita Kirchhofer Signed: _____________________________ Dr. Brian P. Gorman Thesis Advisor Golden, Colorado Date ______________ Signed: _____________________________ Dr. Brian P. Gorman Associate Professor and Director of the Interdisciplinary Materials Science Program ii ABSTRACT Near atomic scale characterization can be achieved using probe tomography (APT) and cross- correlative transmission electron microscopy (TEM). However, pre-APT information about the specimen geometry and structure is necessary to produce accurate 3-D reconstructions and single atom identification. To solve these issues, a combined scanning TEM and APT system is being engineered and constructed, and this instrument has been termed a Dynamic Atom Probe (DyAP). The main goal of the development program is to demonstrate an electron imaging and diffraction system with sub-nanosecond temporal resolution, combined with atom probe tomography analysis with atomic scale resolution and chemical sensitivity in ppm. Three goals were identified to meet the objectives of the program: 1. Develop new methodology for analysis of oxides in the atom probe. 2. Attain a fundamental understanding of thermal transport in APT specimens under laser pulsed irradiation. 3. Develop and implement hardware for the DyAP, and carry out validation of dynamic experiments. Investigation of the behavior of oxides was performed by analyzing CeO2, (Pb,Zr)TiO3, and ZnMgO:Ga film on c-oriented -Al2O3. A study of the impact of laser pulse energy and specimen base temperature on mass resolution, measurement of stoichiometry, multiple detector hits, and evaporation mechanisms were investigated. It was determined that laser pulse energy has effects on inhomogeneous heating of the specimen, formation of neutrals acompanied by loss of detection, and preferential evaporation of ionic species. A dynamic atom probe experiment was demonstrated using the ZnMgO:Ga on -Al2O3. Laser pulsing in the atom probe was used to induce a phase transformation, given by the formation of spinel at the interface. APT results were correlated with TEM selected area diffraction patterns to confirm the transformation followed by APT analysis. The development program is funded by the National Science Foundation (NSF) through the Major Research Instrumentation program (MRI) award Number 1040456. iii TABLE OF CONTENTS ABSTRACT ................................................................................................................................................. iii LIST OF FIGURES .................................................................................................................................... vii LIST OF TABLES ...................................................................................................................................... xv ABBREVIATIONS ................................................................................................................................... xvi SYMBOLS ................................................................................................................................................ xvii ACKNOWLEDGEMENTS ..................................................................................................................... xviii CHAPTER 1: GENERAL INTRODUCTION ........................................................................................... 1 1.1 Introduction ............................................................................................................ 1 1.2 Research Objectives ............................................................................................... 2 1.3 Dissertation Organization ...................................................................................... 2 1.3.1 List of Publications ................................................................................... 3 CHAPTER 2: BACKGROUND ................................................................................................................ 4 2.1 Techniques for Characterization at the Nanometer Scale ...................................... 4 2.1.1 Transmission Electron Microscopy and Crystallography ......................... 5 2.1.2 Materials Characterization Using Atom Probe Tomography ................... 7 2.2 Previous Work on Characterization of Oxides via Atom Probe Tomography and Cross-Correlative Transmission Electron Microscopy ................................. 13 2.3 Thermal Conductivity of Insulating Materials ..................................................... 15 2.3.1 Effects at the Nanometric Scale .............................................................. 17 CHAPTER 3: EXPERIMENTAL DESIGN AND METHODS .............................................................. 19 3.1 Experimental Design ............................................................................................ 19 3.1.1 Analyzed Materials ................................................................................. 20 3.1.2 Modeling the Laser Induced Temperature Changes in Atom Probe Specimens ............................................................................................... 20 3.1.3 The Dynamic Atom Probe Experiment .................................................. 25 3.2 Experimental Methods ......................................................................................... 27 3.2.1 Specimen Preparation ............................................................................. 27 3.2.2 Cross-correlative Transmission Electron Microscopy and Atom Probe Tomography ................................................................................. 27 3.3 Development of Atom Probe Experiments on Oxides ......................................... 30 3.3.1 Laser Absorption .................................................................................... 30 3.3.2 Instrumental Variables in the Atom Probe.............................................. 31 3.3.3 Effects on the Mass Spectrum ................................................................ 31 iv CHAPTER 4: THERMAL EFFECTS ON MASS AND SPATIAL RESOLUTION DURING LASER PULSE ATOM PROBE TOMOGRAPHY OF CERIUM OXIDE ..................... 38 4.1 Abstract ................................................................................................................ 38 4.2 Introduction .......................................................................................................... 38 4.3 Experimental Set Up ............................................................................................ 39 4.4 Results and Discussion ........................................................................................ 41 4.4.1 Laser Energy and Temperature Effects on Mass Resolving Power ........ 41 4.4.2 Cluster and Multiple Hits ........................................................................ 45 4.4.3 Composition Analysis ............................................................................. 46 4.5 Conclusions .......................................................................................................... 50 4.6 Acknowledgements .............................................................................................. 51 CHAPTER 5: QUANTIFYING COMPOSITIONAL HOMOGENEITY IN Pb(Zr,Ti)O3 USING ATOM PROBE TOMOGRAPHY .................................................................................... 52 5.1 Section Title ......................................................................................................... 52 5.2 Introduction .......................................................................................................... 52 5.3 Experimental Procedure ....................................................................................... 54 5.4 Results .................................................................................................................. 58 5.5 Discussion ............................................................................................................ 68 5.5.1 Stoichiometry Measurements from APT ................................................ 69 5.5.2 Cation Spatial Clustering ........................................................................ 70 5.6 Atom Probe Analysis of Bulk PLZT 12/70/30 and PNZT 2.4/52/48 .................. 72 5.7 Summary .............................................................................................................. 77 5.8 Acknowledgements .............................................................................................. 78 CHAPTER 6: DEVELOPMENT OF A DYNAMIC ATOM PROBE .................................................... 79 6.1 Abstract ................................................................................................................ 79 6.2 Introduction .......................................................................................................... 79 6.3 Hardware Development: Components and their Applications ............................ 81 6.3.1 Chamber and Atom Probe....................................................................... 81 6.3.2 Electron Column ..................................................................................... 82 6.3.3 Detectors
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