Aufbau einer Röntgenkleinwinkelstreuanlage und Untersuchung von ZrO 2 -Solen und weiterer Systeme [article]

Björn A. Schmid, Universität Stuttgart, Universität Stuttgart
2005
In the sol-gel-process for the manufactering of zirconia-fibres a so called particel-sol is obtained as intermediate product. The properties of the final fibres are strongly influenced by the structure of these particles. So the characterization of these intermediates is of great interest and can be carried out by small angle X-ray scattering (SAXS) The set-up of the SAXS equipment of the Kratky-type, as well as the adjustment and calibration of the collimating system and the position sensitive
more » ... position sensitive detector is described. As reference substances for calibration silver stearate and octadecanol-1 were used. Other useful substances are e.g. liquid crystals like DODAB (dioctadecyldimethylammoniumbromide) or porous silicates. For the later samples the preparation is described. To evaluate the measurements several computer programms are available freely. Different programms which were based on different mathematical theories and routines have been tested and compared. Some were either not well described or not applicable for the problems in the present case. Only the programm flood by Krauthäuser, which is well described, available as source code, and as compiled programm for different computer systems, was useful for discussing and interpreting the measured X-ray diffraction patterns. However none of the above mentioned programms was appropiate for a complete data evaluation of the measured curves. Therefore a new computer programm was developed, that mainly deals with the deconvolution process of the measured scattering intensities. The programm was tested with theoretical scattering curves, that were calculated from ideal, spherical particles and smeared with the experimental beam profile. Additionally it was tested with in the literature well characterized systems like the mentioned liquid crystals of DODAB and the porous silicates. Finally samples of ZrO2 sols were prepared under various conditions and characterized with small angle X-ray scattering and other methods. In summary the first particles produced in [...]
doi:10.18419/opus-791 fatcat:647opit53rdz7fraz3t4s7vygu