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 [1] for simultaneous in situ Raman/ experiments, to take full advantage of the complementarities of the two techniques in investigating solid-state transformations at non-ambient conditions. The invaluable added value of the proposed experiment is the perfect synchronization of the two probes with the reaction coordinate and the elimination of possible bias caused by different sample holders and conditioning modes used in “in situ but separate” approaches. 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 thermal swelling of stearate-hydrotalcite nanocomposites, iii) the photoinduced 2+2 cyclization of (E)-furylidenoxindole. 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.

[1] E. Boccaleri, F. Carniato, G. Croce, D. Viterbo, W. van Beek, H. Emerich and M. Milanesio, In situ simultaneous Raman/high-resolution X-ray powder diffraction study of transformations occurring in materials at non-ambient conditions, J. Appl. Cryst., 2007, 40, 684-693.

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