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abstracts
With the recent advances in x-ray area detectors, high quality diffuse scattering became readily available. This allows to investigate local order in single crystals and provides invaluable information about real structures of disordered crystals, e.g. stacking probabilities, or structural dynamics. Recently, a new method called Three Dimensional Difference Pair Distribution Function (3D-ΔPDF) analysis was introduced [1]. It provides direct access to the short range order correlations and allows to investigate the diffuse scattering of both static and dynamic origin in a unified fashion . The method is similar to the powder PDF, but availability of three dimensional diffraction data provides several key differences. Firstly, it allows elimination of Bragg peaks and refinement of diffuse scattering alone which conveniently separates the investigation of average structure from investigation of ordering. Secondly, due to reduced overlap of PDF signals, the correlation coefficients at very long interatomic vectors become accessible. The 3D-ΔPDF analysis can be performed in the newly developed program Yell [2]. The program supports all types of correlations and contains a fast FFT-based method for diffuse scattering calculation, and the constraints of arbitrary arithmetic expressions.
abstracts
The use of 2D position and energy sensitive hybrid pixel Pilatus detectors allows performing energy-dispersive analysis of Bragg reflections [1]. This significantly improves the classical Laue experiments enabling the unique determination of the crystal lattice and resolving the higher order harmonics. It allows quantitative crystal structure determination using the Laue method without having any priory information about the crystal [2]. Such energy-dispersive Laue diffraction (EDLD) experiments can be performed with a white X-ray beam either from a synchrotron source or from conventional X-ray tubes. The second approach looks less profitable due to its lower irradiation intensity, but this can be compensated considering the better control of white beam spectra by applying different voltage/current settings during the tube operation. Thus, one can efficiently combine the primary beam and XRD measurements using the same Pilatus detector. This allows the implementation of the energy resolved (color Laue) method for any conventional XRD diffractometer equipped with a Pilatus detection system. In the present work EDLD experiments with a conventional X-ray tube were combined with corresponding primary beam measurements using a 300K Pilatus detector tuned for operation within an energy range of 4-25 keV at energy resolution <0.12 keV. Such a combination simplifies several data correction procedures (the spectral intensity distribution, the sample absorption etc.) significantly. Following our developed intensity correction protocols the structure refinement of a reference quartz sample could be achieved with R-factor <0.10. Possible applications of this method (e.g. quantitative XRD studies with stationary crystals) and the details for its further development will be discussed.
