Linking Diffraction Techniques with XRF and XAS Spectroscopy at the German CRG Beamline ROBL / ESRF

The recent upgrade of the Rossendorf Beamline at ESRF allows simultaneous collection of diffraction and spectroscopy (XRF and XANES). A 6-circle Huber diffractometer (XRD-1) with Eulerian cradle geometry is used for high-resolution powder diffraction and surface diffraction. The powder diffraction module uses an Eiger CdTe 500k detector, the surface diffraction module is equipped with a Pilatus Si 100k detector. PXRD data suitable for Rietveld refinement can be collected between 10 and 31 keV in an 2θ angular range of 0-65°. The Bragg reflexes in PXRD are extracted by radial integration using a modified pyFAI code. Diffraction measurements can be combined with XRF and XAS spectroscopy using a single-element Si drift detector (Vortex X90 CUBE, 1mm SDD, 25 mm Be window) with a FalconX1 processor.

The second diffractometer (XRD-2) consists of a heavy optical bench with an exchangeable goniometer and a Pilatus3 X 2M detector. It is used for single crystal diffraction and in situ or operando powder diffraction. Devices for non-ambient sample conditions are a hot-air blower (RT-1100K), a heating chamber (RT-1470K), and a LN2 cryostream (90-400K). This diffractometer is controlled with the Pylatus software. The single crystal data extraction is performed with CrysAlisPro. The Si drift detector can be placed in different positions to combine diffraction with XRF and XAS measurements.