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Ultra-compact X-ray diffraction setup for sample characterization at ID20

29-10-2024

Researchers and engineers at the ESRF have developed an ultra-compact setup for in-situ X-ray diffraction at the inelastic X-ray scattering beamline ID20. This new configuration meets a growing demand for on-the-fly sample characterization, making it easier to navigate complex phase diagrams, particularly for samples under high pressure and/or high-temperature conditions.

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With the enhanced brilliance of the ESRF’s Extremely Brilliant Source, inelastic X-ray scattering (IXS) techniques are now able to explore increasingly complex samples in more advanced environments. However, unlike experimental techniques that are based on elastic scattering or photoelectric absorption, IXS experiments are still time-consuming, making on-the-fly sample-screening impractical. While X-ray diffraction (XRD) methods are commonly used for rapid sample characterization, the large area detectors required for fast XRD measurements are often not suitable due to the limited space available at ID20

To address this, a new compact XRD setup has been designed based on the Advacam Minipix pixelated area detector (Figure 1). This configuration enables the assessment of sample integrity and crystal structure, as well as complementary sample characterization, while performing non-resonant inelastic X-ray scattering (NIXS) and X-ray emission spectroscopy (XES) in both in-situ and ex-situ environments.
 

 

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Fig. 1: Technical drawing of the new miniXRD setup available at the large-solid-angle spectrometer at ID20. A small pixelated area detector translates across diffraction patterns, producing two-dimensional images by stitching together the detector’s captures.


The new miniXRD setup allows for quasi-simultaneous collection of X-ray diffraction patterns and low-Z absorption-edge measurements using X-ray Raman Scattering spectroscopy (Figure 2). It is compatible with in-situ environments, such as high-temperature cells, or diamond anvil cells that produce high-pressure conditions.

 

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Fig. 2:  a) Stitched miniXRD detector image obtained from the ambient temperature data shown in part (b). b) XRD data for CeO2 at ambient temperature and at T = 700C, following azimuthal integration, along with the results of Rietveld refinement at T = 700C (Small peaks around 2θ = 20, 21, and 49 are attributed to diffraction from the sample holder used).  c) Ce N4,5 excitation spectrum measured via X-ray Raman scattering spectroscopy at a momentum transfer of q = 9.3 Å−1.


X-ray diffraction is now available to users as a quick and straightforward technique for sample characterization, both before and during extended IXS experiments. This will enable faster sample screening and aid in navigating complex temperature/pressure phase diagrams for studies conducted at ID20.


Principal publication and authors
A miniature X-ray diffraction setup at ID20 of the European Synchrotron Radiation Facility, 
C.J. Sahle (a), M. Majkut (a), K. Ruotsalainen (a), F. Gerbon (a), N. Suomalainen (b), M.-C. Lagier (a), B. Detlefs (a), L. Claustre (a), A. Mirone (a), A. Longo (a,c), J. Synchrotron Radiat. 31, 6 (2024); https://doi.org/10.1107/S1600577524009147 
(a) ESRF
(b) Department of Physics, University of Helsinki, Helsinki (Finland)
(c) Istituto per lo Studio dei Materiali Nanostrutturati (ISMN)-CNR, UOS Palermo, Palermo (Italy)