Treatment of multiple‐beam X‐ray diffraction in energy‐dependent measurements

During X‐ray diffraction experiments on single crystals, the diffracted beam intensities may be affected by multiple‐beam X‐ray diffraction (MBD). This effect is particularly frequent at higher X‐ray energies and for larger unit cells. The appearance of this so‐called Renninger effect often impairs the interpretation of diffracted intensities. This applies in particular to energy spectra analysed in resonant experiments, since during scans of the incident photon energy these conditions are necessarily met for specific X‐ray energies. This effect can be addressed by carefully avoiding multiple‐beam reflection conditions at a given X‐ray energy and a given position in reciprocal space. However, areas which are (nearly) free of MBD are not always available. This article presents a universal concept of data acquisition and post‐processing for resonant X‐ray diffraction experiments. Our concept facilitates the reliable determination of kinematic (MBD‐free) resonant diffraction intensities even at relatively high energies which, in turn, enables the study of higher absorption edges. This way, the applicability of resonant diffraction, e.g. to reveal the local atomic and electronic structure or chemical environment, is extended for a vast majority of crystalline materials. The potential of this approach compared with conventional data reduction is demonstrated by the measurements of the Ta L3 edge of well studied lithium tantalate LiTaO3. An approach to reliably extract the desired intensities and filter out multiple‐beam X‐ray diffraction, which often causes interference for high X‐ray energies and for large unit cells, is presented. Here, a universal concept of data acquisition and post‐processing for resonant X‐ray diffraction experiments is described, including the measurement of the energy‐dependent intensity at several azimuth angles and subsequently only considering the unaffected data points.