The following chapters present three peer reviewed publications having CSD as main topic or FXD-CSD is used as core method to derive the FXD-CSD of the samples under investigation. At present, the manuscript underlying Chapter 2 is in print. It was submitted at 5th of May 2018, reviewed positive at 25th of May 2018 and was accepted at the 23rd of July 2018.
Chapter 2: “A fast X-ray diffraction-based method for a determination of crystal size distributions (FXD-CSD)”, accepted for publication in the Journal of Applied Crystallography, constitutes the main part of this thesis and provides a comprehensive description of the method. Starting with an overview of other methods used to derive CSDs or mean crystal sizes, including non-X-ray diffraction-based approaches, all theoretical aspects and applied intensity corrections are presented. The fundamental functionality and the application range of FXD-CSD is shown by presenting the analysis and results of five samples.
The measurements are carried out with the diffractometer setup described in Section 1.5 using a molybdenum X-ray tube. Most valuable here are the results of four corundum crystal size fractions.
These samples have been specifically prepared (Chapter 2, Section 2.4) for this purpose and their CSD was determined in advance. This allowed their utilization both as a reference material and as a sample to crosscheck the obtained results.
For this publication the fxd-csd software, written by me, was used. This is including the data reduction, data evaluation and the CSD determination. The samples were produced, prepared and measured by me. My contribution to the manuscript preparation comprises drafting, figure preparation and partially the literature search. The final preparation and proofreading were carried out with the aid of Prof. Dr.
W.F. Kuhs and PD Dr. Helmut Klein.
Chapter 3: “Determination of crystal size distributions in alumina ceramics by a novel X-ray diffraction procedure”, published in 2017 the Journal of the American Ceramic Society, presents an application example, investigating the microstructure of a polycrystalline material. Again, the diffractometer setup described in Section 1.5 with a molybdenum X-ray tube was used. Here we were able to analyze the microstructural evolution of four alumina substrates with different time spans of sintering. The CSD of all samples was determined and good evidence for abnormal grain growth was found.
My contributions to this publication are the sample preparation, the diffraction measurements, the data analysis (using the fxd-csd software), the figure preparation and the drafting of the manuscript.
The samples were provided by PD. Dr. Helmut Klein. Finalizing the manuscript was done with the input and correction of my supervisors Prof. Dr. W.F. Kuhs and PD. Dr. Helmut Klein.
Chapter 4: The publication, “Time Resolved Coarsening of Clathrate Crystals: The Case of Gas Hydrates”, published 2016 in the Journal Crystal Growth & Design, constitutes a fundamental research paper. FXD-CSD is the core method used to determine the CSD evolution of gas hydrates. The analyzed data was collected at the European Synchrotron Research Facility (ESRF) in Grenoble, France. The obtained results show the coarsening and the CSD evolution over time and it is shown that they are in accordance with X-ray tomography data of comparable samples.
1-20 The presented data was analyzed with a preliminary version of fxd-csd, which was used by Marwen Chaouachi for the data reduction and to calculate the diffraction geometry dependent intensity corrections. The data evaluation and intensity scaling were done manually by Marwen. I was attending the beam times and as part of the crew assisting Marwen carrying out the measurements. I was involved in writing the manuscript by drafting the data reduction section.
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