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
{"title":"A reactor for time-resolved X-ray studies of nucleation and growth during solvothermal synthesis.","authors":"Martin Roelsgaard,&nbsp;Magnus Kløve,&nbsp;Rasmus Christensen,&nbsp;Andreas D Bertelsen,&nbsp;Nils L N Broge,&nbsp;Innokenty Kantor,&nbsp;Daniel Risskov Sørensen,&nbsp;Ann-Christin Dippel,&nbsp;Soham Banerjee,&nbsp;Martin V Zimmermann,&nbsp;Philipp Glaevecke,&nbsp;Olof Gutowski,&nbsp;Mads Ry Vogel Jørgensen,&nbsp;Bo Brummerstedt Iversen","doi":"10.1107/S1600576723002339","DOIUrl":null,"url":null,"abstract":"<p><p>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 <i>in situ</i> 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.</p>","PeriodicalId":14950,"journal":{"name":"Journal of Applied Crystallography","volume":"56 Pt 3","pages":"581-588"},"PeriodicalIF":6.1000,"publicationDate":"2023-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC10241040/pdf/","citationCount":"0","resultStr":null,"platform":"Semanticscholar","paperid":null,"PeriodicalName":"Journal of Applied Crystallography","FirstCategoryId":"88","ListUrlMain":"https://doi.org/10.1107/S1600576723002339","RegionNum":3,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q1","JCRName":"Biochemistry, Genetics and Molecular Biology","Score":null,"Total":0}
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

Abstract Image

Abstract Image

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。
求助全文
约1分钟内获得全文 求助全文
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.
×
引用
GB/T 7714-2015
复制
MLA
复制
APA
复制
导出至
BibTeX EndNote RefMan NoteFirst NoteExpress
×
提示
您的信息不完整,为了账户安全,请先补充。
现在去补充
×
提示
您因"违规操作"
具体请查看互助需知
我知道了
×
提示
确定
请完成安全验证×
copy
已复制链接
快去分享给好友吧!
我知道了
右上角分享
点击右上角分享
0
联系我们:info@booksci.cn Book学术提供免费学术资源搜索服务,方便国内外学者检索中英文文献。致力于提供最便捷和优质的服务体验。 Copyright © 2023 布克学术 All rights reserved.
京ICP备2023020795号-1
ghs 京公网安备 11010802042870号
Book学术文献互助
Book学术文献互助群
群 号:481959085
Book学术官方微信