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Materials containing disordered moieties and/or amorphous or liquid-like phases or showing surface- or defect-related phenomena constitute a problem for their characterization using X-ray powder diffraction (XRPD), and Raman spectroscopy can provide useful complementary information. We have designed and realized a novel experimental set-up for simultaneous in situ Raman/
The set-up was developed by the Swiss-Norwegian Beamline at the European Synchrotron Radiation Facility in Grenoble and tested on three solid-state transformations: i) the kinetics of the solid-state synthesis of the charge-transfer complex fluorene:TCNQ, ii) the structure and the thermally-induced modifications of hydrotalcite-based nanocomposites, iii) the decarboxilation process of layered Zirconium phosphonates. The reported experiments demonstrated that, even though the simultaneous Raman/XRPD experiment is more challenging than the separated ones, high-resolution XRPD and Raman data could be collected. A gas blower allows studies from RT to 700K and 100K can be reached using a nitrogen cryostream. The experimental setup flexibility allows the addition of ancillary devices, such as the UV-lamp used to study photoreactivity.
The scheme of the Raman/XRPD experimental setup
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