TY - JOUR
T1 - A reactor for time-resolved X-ray studies of nucleation and growth during solvothermal synthesis
AU - Roelsgaard, Martin
AU - Kløve, Magnus
AU - Christensen, Rasmus
AU - Bertelsen, Andreas D.
AU - Broge, Nils L. N.
AU - Kantor, Innokenty
AU - Sørensen, Daniel Risskov
AU - Dippel, Ann-Christin
AU - Banerjee, Soham
AU - Zimmermann, Martin V.
AU - Glaevecke, Philipp
AU - Gutowski, Olof
AU - Jørgensen, Mads Ry Vogel
AU - Iversen, Bo Brummerstedt
PY - 2023
Y1 - 2023
N2 - 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.
AB - 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.
KW - In situ X-ray scattering
KW - Powder X-ray diffraction
KW - Small-angle scattering
KW - Solvothermal chemistry
KW - Total scattering
U2 - 10.1107/S1600576723002339
DO - 10.1107/S1600576723002339
M3 - Journal article
C2 - 37284256
SN - 0021-8898
VL - 56
SP - 581
EP - 588
JO - Journal of Applied Crystallography
JF - Journal of Applied Crystallography
IS - Pt 3
ER -