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

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  • Martin Roelsgaard, Lund University
  • ,
  • Magnus Kløve
  • Rasmus Christensen
  • ,
  • Andreas D. Bertelsen
  • Nils L. N. Broge
  • ,
  • Innokenty Kantor, MAX IV Laboratory, Danmarks Tekniske Universitet
  • ,
  • Daniel Risskov Sørensen, Lund University
  • ,
  • Ann-Christin Dippel
  • Soham Banerjee, Helmholtz-Gemeinschaft Deutscher Forschungszentren
  • ,
  • Martin V Zimmermann, Helmholtz-Gemeinschaft Deutscher Forschungszentren
  • ,
  • Philipp Glaevecke, Helmholtz-Gemeinschaft Deutscher Forschungszentren
  • ,
  • Olof Gutowski, Helmholtz-Gemeinschaft Deutscher Forschungszentren
  • ,
  • Mads Ry Vogel Jørgensen
  • Bo Brummerstedt Iversen

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.

TidsskriftJournal of Applied Crystallography
Sider (fra-til)581-588
Antal sider8
StatusUdgivet - jun. 2023

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