Combining a nine-crystal multi-analyser stage with a two-dimensional detector for high-resolution powder X-ray diffraction

Abstract

The high‐resolution powder diffraction beamline at ESRF (ID22), built with a dual‐undulator source on the 6 GeV storage ring, combines a wide continuous range of incident energy (6–80 keV) with high brightness, offering the possibility to carry out high‐flux high‐resolution powder diffraction measurements. In routine operation, a bank of nine scintillation detectors is scanned vertically to measure the diffracted intensity versus 2gθ, each detector being preceded by an Si 111 analyser crystal. Although the current detector system has operated successfully for the past 20 years, recent developments in detector technology could be exploited to improve the overall performance. With this in mind, as a test, a two‐dimensional Pilatus3 X CdTe 300 K‐W pixel detector has been mounted on the arm of the diffractometer, replacing the nine scintillator detectors. At each nominal 2gθ value, a two‐dimensional image is recorded showing nine distinct regions corresponding to the diffraction signals passing via each of the analyser crystals. This arrangement offers new flexibility in terms of data handling and processing, with the possibility to optimize both peak shape and statistics, to remove parasitic effects, and to gain spatial resolution information. Combining the high efficiency of a hybrid photon‐counting area detector with the high angular resolution given by analyser crystals is an effective approach to improving the overall performance of high‐resolution powder diffraction.

Full reciprocal-space mapping up to 2000 K under controlled atmosphere: the multipurpose QMAX furnace

“…Nowadays, it is clear that in situ or operando X-ray scattering setups have to be built using a 2D, or at least a 1D, positionsensitive detector. Although a lot of work is currently being done to obtain high angular resolution using 2D positionsensitive detectors [see for example Dejoie et al (2018)], under reflection geometry the resolution remains directly linked to the beam size. We demonstrate that, as a result of the high flux provided by the synchrotron radiation source and in spite of the use of a highly collimated parallel primary X-ray beam, high-resolution XRD patterns can be recorded on a timescale of seconds and full 3D RSMs can be obtained in a few minutes.…”

Applications of X-ray Powder Diffraction in Protein Crystallography and Drug Screening

“…However, advances in instrumentation as well as the development of powerful crystallographic software have significantly facilitated the collection of high-resolution diffraction data and have made XRPD particularly useful for the extraction of structural information. For example, ID22 experimental station at ESRF provides the possibility of using a two-dimensional detector in combination with crystal analyzers in order to retrieve high-resolution powder diffraction patterns [183], while, employing the Mythen II detector of MS-X04SA at SLS [157] and following a strategy which combines vertical focus of the beam on the detector instead of the sample and data collection at multiple detector positions, dataset's angular resolution capabilities have been expanded.…”

ROBL-II at ESRF: a synchrotron toolbox for actinide research

“…While the highest resolution in powder diffraction can be achieved with secondary analyzer crystals (Dejoie et al, 2018;Hodeau et al, 1998), we refrained from this approach, since installation and alignement of the analyzer crystals turned out to be too time consuming for user operation with experiments changing typically from week to week. Instead, as a compromise between short installation time and reasonable resolution, we developed a module for the small Pilatus 100k detector also used for surface diffraction, with a sampledetector distance of 800 mm (Fig.…”