Three-Dimensional Microstructure Characterization of Surface-Crystallized Glass Ceramics

Autor: Busch, Richard
Jazyk: angličtina
Rok vydání: 2023
Předmět:
Druh dokumentu: Text<br />Doctoral Thesis
Popis: Die dreidimensionale Mikrostruktur, welche bei der Oberflächenkristallisation von Glaskeramiken entsteht, wird mittels einer neuartigen Methode zur Präparation von abgesenkten Probenoberflächen untersucht. Diese Initialkantensektionierungsmethode, welche auf der Erzeugung von Scharten in der Probenoberfläche und anschließender Glanzwinkelionenstrahlerosion basiert, erlaubt das rapide Freilegen von großflächigen Schichten in wohldefinierten Tiefen unterhalb der ursprünglichen Probenoberfläche. In dieser Dissertation werden mehrere Variationen der Technik durch Kombination von Laserablation, Ionenbreit- sowie Ionenfeinstrahlerosion untersucht und miteinander verglichen. Die in Bezug auf Schnittgeometrie und Probengüte relevanten, experimentellen Parameter werden bestimmt und bewertet. Ein Modell zur Beschreibung der zeitlichen Evolution der Probengeometrie während des Erosionsvorgangs wird auf Grundlage von Simulationen und analytischen Näherungen aufgestellt und mit experimentellen Ergebnissen verglichen. Schließlich wird die Initialkantensektionierungsmethode mit Elektronenrückstreubeugung kombiniert um Wachstumseffekte bei der Oberflächenkristallisation von Diopsid- und Ba2TiSi2O8-Fresnoitglaskeramiken zu untersuchen.:1 Introduction 1.1 Motivation 1.2 Aims and Objectives 2 Literature Review 2.1 Sample Preparation for Electron Backscatter Diffraction Studies 2.2 Serial Sectioning Methods 2.3 Microstructure Characterization of Glass Ceramics using EBSD 2.4 Interim Conclusion 3 Theory 3.1 Erosion of a Surface Under Ion Bombardment 3.1.1 Sputtering 3.1.2 Kinetic Theory of Surface Evolution 3.1.3 Numerical Simulation of Surface Erosion 3.1.4 Erosion of a Surface With Initial Notches 3.2 Electron Backscatter Diffraction 3.2.1 Measurement Principle 3.2.2 Representation of Orientations and Texture 4 Methods and Materials 4.1 Sample Preparation and Processing 4.2 Surface Metrology 4.3 Microstructure Analysis 4.4 Materials 5 Erosion of Surfaces With Initial Notches 5.1 Evaluation of Surface Processing Methods 5.1.1 Notch Creation 5.1.2 Terrace Formation by Glancing-Angle Ion Beam Erosion 5.2 Surface Properties in the Terrace Region 5.2.1 Terrace Roughness 5.2.2 Ion Beam Induced Amorphization 5.3 Evolution of Surface Geometry 5.3.1 Linear Model 5.3.2 Simulations 5.3.3 Experimental Results 5.4 Discussion 5.4.1 Sample Processing 5.4.2 Sample Quality 5.4.3 Kinetic Model of Surface Evolution 6 Depth-Resolved Microstructure Characterization Using Initial Notches 6.1 Diopside 6.2 Ba2TiSi2O8 fresnoite (BTS) 6.3 Discussion 6.3.1 Methodological Aspects of Initial Notch Sectioning 6.3.2 Microstructure Analysis on Surface-Crystallized Glass Ceramics 7 Summary and Outlook
Three-dimensional microstructures resulting from surface crystallization of glass ceramics are studied using a novel sample sectioning method. Based on the creation of notches on the sample surface and subsequent glancing-angle ion beam erosion, initial notch sectioning enables the rapid excavation of large subsurface layers at well-defined depths. In this thesis, several variations of this technique using different combinations of laser ablation, broad and focused ion beam erosion are realized and compared to each other. Relevant parameters controlling the section geometry and quality are determined. A model of the surface evolution kinetics is developed using simulations and analytical estimates, which is compared to experimental results. Finally, initial notch sectioning in combination with electron backscatter diffraction is applied to elucidate growth phenomena in the surface crystallization of diopside and Ba2TiSi2O8 fresnoite glass ceramics.:1 Introduction 1.1 Motivation 1.2 Aims and Objectives 2 Literature Review 2.1 Sample Preparation for Electron Backscatter Diffraction Studies 2.2 Serial Sectioning Methods 2.3 Microstructure Characterization of Glass Ceramics using EBSD 2.4 Interim Conclusion 3 Theory 3.1 Erosion of a Surface Under Ion Bombardment 3.1.1 Sputtering 3.1.2 Kinetic Theory of Surface Evolution 3.1.3 Numerical Simulation of Surface Erosion 3.1.4 Erosion of a Surface With Initial Notches 3.2 Electron Backscatter Diffraction 3.2.1 Measurement Principle 3.2.2 Representation of Orientations and Texture 4 Methods and Materials 4.1 Sample Preparation and Processing 4.2 Surface Metrology 4.3 Microstructure Analysis 4.4 Materials 5 Erosion of Surfaces With Initial Notches 5.1 Evaluation of Surface Processing Methods 5.1.1 Notch Creation 5.1.2 Terrace Formation by Glancing-Angle Ion Beam Erosion 5.2 Surface Properties in the Terrace Region 5.2.1 Terrace Roughness 5.2.2 Ion Beam Induced Amorphization 5.3 Evolution of Surface Geometry 5.3.1 Linear Model 5.3.2 Simulations 5.3.3 Experimental Results 5.4 Discussion 5.4.1 Sample Processing 5.4.2 Sample Quality 5.4.3 Kinetic Model of Surface Evolution 6 Depth-Resolved Microstructure Characterization Using Initial Notches 6.1 Diopside 6.2 Ba2TiSi2O8 fresnoite (BTS) 6.3 Discussion 6.3.1 Methodological Aspects of Initial Notch Sectioning 6.3.2 Microstructure Analysis on Surface-Crystallized Glass Ceramics 7 Summary and Outlook
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