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Advantages and disadvantages of fast XRPD measurement by using image-plate and rotating anode source
|Giora Kimmel , Dmitry Mogilyanski|
Institutes for Applied Research, Ben Gurion University of the Negev, Beer-Sheva 84105, Israel
An image-plate detector performs simultaneous charge accumulation providing fast data collection. A high resolution Guinier image-plate camera was installed on a rotating anode source. This configuration enables fast measurement with high resolution. There are some differences between the Guinier image-plate camera (GIP) and the conventional Bragg-Brentano diffractometer (BBD). The GIP works in transmission mode with a constant focusing circle. The monochromator is attached to the source providing Kα1 radiation. There is no background cut. The range of the scattering angles 2θ is from 1 to 100°. The BBD works in back reflection mode with multiple focusing circles. The monochromator attached to the detector cuts Kβ and most of the background but without diminishing of Kα2. The range of the scattering angles 2θ is between 0.5 and 158°. In the standard measurement procedure there are also differences in the sample loading and measurement. In GIP a thin layer of powder is loaded and the illuminated area and depth are equal for the entire 2θ range. In BBD the sample is loaded in a cavity and the illuminated area and depth are changing throughout the 2θ range. As a final point, the counting principles in GIP and BBD are totally different. Data were collected from several samples in both GIP and BBD. Most of the samples were high quality powders of well known solids like LaB6, ZnO, α Al2O3, CeO2, NIST standards, WC. More complicated structures were studied such as monoclinic HfO2 and ZrO2. The crystal structure characteristics including cell parameters and atomic positions were compared. In addition, quantitative analysis was performed for mixtures of corundum and zirconia, in order to compare the results of relative phase amounts in both systems. The main tool for the data processing was the Rietveld method.
Presentation: Oral at 11th European Powder Diffraction Conference, Microsymposium 12, by Giora Kimmel
See On-line Journal of 11th European Powder Diffraction Conference
Submitted: 2008-04-21 19:31 Revised: 2009-06-07 00:48