EXAFS Experiments at High Pressure with Small Samples
Abstract
X-ray absorption spectroscopy has been used to study alkali halides at high pressures, using a pressure cell with either diamond or boron carbide X-ray transparent anvils, and having a free X-ray beam path to those anvils. Sample pressures were determined both by ruby fluorescence and by EXAFS analytic methods. Methods of obtaining pressure from EXAFS data are explored, and a portable apparatus for the ruby fluorescence pressure determination is described. It is found that diamond diffraction events are significant in dealing with EXAFS spectra, and apparatus is built to facilitate gathering useful data in the presence of diffraction. A technique of deconvolution and filtering of these diffraction events is performed and analyzed. A software environment that facilitates this analysis is built, documented, and expanded to perform other tasks. A small crystal of YBa_2Cu_3O _{7-x} is positioned and aligned, and its EXAFS angular dependence is probed with polarized X-rays. Analysis of the EXAFS indicates that the crystal is a pseudomorph, containing many twinned domains which make the external a axis and b axis indeterminate, though the c axis is well defined. A new piston tip design for pressure generation with boron carbide components is built and tested in EXAFS experimentation. Because the experimental result may be compromised if the boron carbide thickness is not correctly chosen for the pressure and X-ray energy of interest, a simulation of the experimental conditions is constructed so that the adequacy of X-ray flux can be determined in advance of an experiment.
- Publication:
-
Ph.D. Thesis
- Pub Date:
- 1994
- Bibcode:
- 1994PhDT.......133W
- Keywords:
-
- HIGH PRESSURES;
- Physics: Condensed Matter; Physics: Radiation