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A reactor for time-resolved X-ray studies of nucleation and growth during solvothermal synthesis
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....
Autores principales: | , , , , , , , , , , , , , |
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Formato: | Online Artículo Texto |
Lenguaje: | English |
Publicado: |
International Union of Crystallography
2023
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Materias: | |
Acceso en línea: | https://www.ncbi.nlm.nih.gov/pmc/articles/PMC10241040/ https://www.ncbi.nlm.nih.gov/pubmed/37284256 http://dx.doi.org/10.1107/S1600576723002339 |
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author | 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 |
author_facet | 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 |
author_sort | Roelsgaard, Martin |
collection | PubMed |
description | 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. |
format | Online Article Text |
id | pubmed-10241040 |
institution | National Center for Biotechnology Information |
language | English |
publishDate | 2023 |
publisher | International Union of Crystallography |
record_format | MEDLINE/PubMed |
spelling | pubmed-102410402023-06-06 A reactor for time-resolved X-ray studies of nucleation and growth during solvothermal synthesis 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 J Appl Crystallogr Research Papers 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. International Union of Crystallography 2023-04-13 /pmc/articles/PMC10241040/ /pubmed/37284256 http://dx.doi.org/10.1107/S1600576723002339 Text en © Martin Roelsgaard et al. 2023 https://creativecommons.org/licenses/by/4.0/This is an open-access article distributed under the terms of the Creative Commons Attribution (CC-BY) Licence, which permits unrestricted use, distribution, and reproduction in any medium, provided the original authors and source are cited. |
spellingShingle | Research Papers 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 A reactor for time-resolved X-ray studies of nucleation and growth during solvothermal synthesis |
title | A reactor for time-resolved X-ray studies of nucleation and growth during solvothermal synthesis |
title_full | A reactor for time-resolved X-ray studies of nucleation and growth during solvothermal synthesis |
title_fullStr | A reactor for time-resolved X-ray studies of nucleation and growth during solvothermal synthesis |
title_full_unstemmed | A reactor for time-resolved X-ray studies of nucleation and growth during solvothermal synthesis |
title_short | A reactor for time-resolved X-ray studies of nucleation and growth during solvothermal synthesis |
title_sort | reactor for time-resolved x-ray studies of nucleation and growth during solvothermal synthesis |
topic | Research Papers |
url | https://www.ncbi.nlm.nih.gov/pmc/articles/PMC10241040/ https://www.ncbi.nlm.nih.gov/pubmed/37284256 http://dx.doi.org/10.1107/S1600576723002339 |
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