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

Martin Roelsgaard, Magnus Kløve, Rasmus Christensen, Andreas D. Bertelsen, Nils L. N. Broge, Innokenty Kantor, Daniel Risskov Sørensen, Ann-Christin Dippel, Soham Banerjee, Martin V Zimmermann, Philipp Glaevecke, Olof Gutowski, Mads Ry Vogel Jørgensen*, Bo Brummerstedt Iversen*

*Corresponding author for this work

Research output: Contribution to journal/Conference contribution in journal/Contribution to newspaperJournal articleResearchpeer-review

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.

Original languageEnglish
JournalJournal of Applied Crystallography
Volume56
Issue3
Pages (from-to)581-588
Number of pages8
ISSN0021-8898
DOIs
Publication statusPublished - Jun 2023

Keywords

  • in situ X-ray scattering
  • powder X-ray diffraction
  • small-angle scattering
  • solvothermal chemistry
  • total scattering

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