Roelsgaard Martin, Kløve Magnus, Christensen Rasmus, Bertelsen Andreas D, Broge Nils L N, Kantor Innokenty, Sørensen Daniel Risskov, Dippel Ann-Christin, Banerjee Soham, Zimmermann Martin V, Glaevecke Philipp, Gutowski Olof, Jørgensen Mads Ry Vogel, Iversen Bo Brummerstedt
Department of Chemistry and iNANO, Aarhus University, Langelandsgade 140, 8000 Aarhus C, Denmark.
MAX IV Laboratory, Lund University, 224 84 Lund, Sweden.
J Appl Crystallogr. 2023 Apr 13;56(Pt 3):581-588. doi: 10.1107/S1600576723002339. eCollection 2023 Jun 1.
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 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.
了解水热和溶剂热条件下纳米晶体的成核和生长机制是定制功能纳米材料的关键。高能和高通量同步辐射非常适合通过粉末X射线衍射和实时X射线全散射进行表征。在这项工作中采用了不同版本的间歇式细胞反应器，利用内径为0.7 mm的聚酰亚胺涂层熔融石英管的坚固性，因为它们可以承受高达250 bar的压力和高达723 K的温度数小时。本文报道了在PETRA III的P21.1光束线和MAX IV的DanMAX光束线上可供普通用户使用的装置的最新进展，以研究溶剂热合成中的成核和生长现象。结果表明，在4 ms的时间尺度上可以获得适用于倒易空间Rietveld精修和正空间对分布函数精修的数据。
