A miniature X-ray diffraction setup on ID20 at the European Synchrotron Radiation Facility

Abstract

We describe an ultra-compact setup for in situ X-ray diffraction on the inelastic X-ray scattering beamline ID20 at the European Synchrotron Radiation Facility. The main motivation for the design and construction of this setup is the increasing demand for on-the-fly sample characterization, as well as ease of navigation through a sample's phase diagram, for example subjected to high-pressure and/or high-temperature conditions. We provide technical details and demonstrate the performance of the setup.

Keywords: X-ray diffraction; inelastic X-ray scattering; radiation damage; sample characterization.

Figure 1

Three-dimensional renderings of the miniXRD setup installed in (a) the vertical and (b) the horizontal scanning configuration. (c) Photograph of the setup installed within the large-solid-angle spectrometer on ID20 at the ESRF. (d) Direct beam positions (vertical and horizontal) on the detector versus vertical detector translation, including linear fits. Along the scan direction, the slope of the linear fit suggests a pixel size of 0.055 mm per pixel, in perfect agreement with the hardware specifications.

Figure 2

Raw data after azimuthal integration and results of our Rietveld refinement of a mixed WO₃–Al₂O₃ polycrystalline powder sample measured using (a) the miniXRD setup and (b) a Pilatus 300Kw large-area detector.

Figure 3

Simultaneously taken XRD and XRS data of a polycrystalline CeO₂ sample in pellet form. (a) Stitched miniXRD detector image from the ambient temperature data shown in panel (b). (b) XRD data for CeO₂ at ambient temperature (RT) and T = 700°C after azimuthal integration and the result of a Rietveld refinement at T = 700°C. (The small peaks around 2θ = 20°, 21° and 49° are due to diffraction from the sample holder used.) (c) Ce N_4,5 excitation spectra measured using X-ray Raman scattering spectroscopy at a momentum transfer of q = 9.3 Å⁻¹.