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

IF 6.1 3区 材料科学 Q1 Biochemistry, Genetics and Molecular Biology
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
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引用次数: 0

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.

Abstract Image

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用于溶剂热合成过程中成核和生长的时间分辨x射线研究的反应器。
了解纳米晶体在水热和溶剂热条件下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是粉末x射线衍射和x射线全散射实时表征的理想选择。不同版本的间歇式电池反应器被用于这项工作,利用聚酰亚胺涂层熔融石英管的坚固性,内径为0.7毫米,因为它们可以承受高达250巴的压力和高达723 K的温度几个小时。这里报告了PETRA III的P21.1束线和MAX IV的DanMAX束线上可供一般用户使用的原位装置的最新进展,用于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,可以得到适合于往向空间Rietveld细化和直接空间对分布函数细化的数据。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
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来源期刊
CiteScore
10.00
自引率
3.30%
发文量
178
审稿时长
4.7 months
期刊介绍: Many research topics in condensed matter research, materials science and the life sciences make use of crystallographic methods to study crystalline and non-crystalline matter with neutrons, X-rays and electrons. Articles published in the Journal of Applied Crystallography focus on these methods and their use in identifying structural and diffusion-controlled phase transformations, structure-property relationships, structural changes of defects, interfaces and surfaces, etc. Developments of instrumentation and crystallographic apparatus, theory and interpretation, numerical analysis and other related subjects are also covered. The journal is the primary place where crystallographic computer program information is published.
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