A reactor for time-resolved X-ray studies of nucleation and growth during solvothermal synthesis

J Appl Crystallogr. 2023 Apr 13;56(Pt 3):581-588. doi: 10.1107/S1600576723002339. eCollection 2023 Jun 1.

Abstract

Understanding the nucleation and growth mechanisms of nanocrystals under hydro- and solvothermal conditions is key to tailoring functional nanomaterials. High-energy and high-flux synchrotron radiation is ideal for characterization by powder X-ray diffraction and X-ray total scattering in real time. Different versions of batch-type cell reactors have been employed in this work, exploiting the robustness of polyimide-coated fused quartz tubes with an inner diameter of 0.7 mm, as they can withstand pressures up to 250 bar and temperatures up to 723 K for several hours. Reported here are recent developments of the in situ setups available for general users on the P21.1 beamline at PETRA III and the DanMAX beamline at MAX IV to study nucleation and growth phenomena in solvothermal synthesis. It is shown that data suitable for both reciprocal-space Rietveld refinement and direct-space pair distribution function refinement can be obtained on a timescale of 4 ms.

Keywords: in situ X-ray scattering; powder X-ray diffraction; small-angle scattering; solvothermal chemistry; total scattering.

Grants and funding

Research conducted at MAX IV is supported by the Swedish Research Council under contract 2018-07152, the Swedish Governmental Agency for Innovation Systems under contract 2018-04969 and Formas under contract 2019-02496. DanMAX is funded by the NUFI (grant No. 4059-00009B). The work was supported by the Villum Foundation. We thank the Danish Agency for Science, Technology and Innovation for funding the instrument centre DanScatt.