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

Author:

Roelsgaard MartinORCID,Kløve MagnusORCID,Christensen Rasmus,Bertelsen Andreas D.,Broge Nils L. N.,Kantor InnokentyORCID,Sørensen Daniel Risskov,Dippel Ann-ChristinORCID,Banerjee SohamORCID,Zimmermann Martin V.,Glaevecke Philipp,Gutowski Olof,Jørgensen Mads Ry VogelORCID,Iversen Bo BrummerstedtORCID

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.

Funder

Villum Fonden

Vetenskapsrådet

VINNOVA

Svenska Forskningsrådet Formas

Publisher

International Union of Crystallography (IUCr)

Subject

General Biochemistry, Genetics and Molecular Biology

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