Cargando…

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....

Descripción completa

Detalles Bibliográficos
Autores principales: 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
Formato: Online Artículo Texto
Lenguaje:English
Publicado: International Union of Crystallography 2023
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
_version_ 1785053897156460544
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
work_keys_str_mv AT roelsgaardmartin areactorfortimeresolvedxraystudiesofnucleationandgrowthduringsolvothermalsynthesis
AT kløvemagnus areactorfortimeresolvedxraystudiesofnucleationandgrowthduringsolvothermalsynthesis
AT christensenrasmus areactorfortimeresolvedxraystudiesofnucleationandgrowthduringsolvothermalsynthesis
AT bertelsenandreasd areactorfortimeresolvedxraystudiesofnucleationandgrowthduringsolvothermalsynthesis
AT brogenilsln areactorfortimeresolvedxraystudiesofnucleationandgrowthduringsolvothermalsynthesis
AT kantorinnokenty areactorfortimeresolvedxraystudiesofnucleationandgrowthduringsolvothermalsynthesis
AT sørensendanielrisskov areactorfortimeresolvedxraystudiesofnucleationandgrowthduringsolvothermalsynthesis
AT dippelannchristin areactorfortimeresolvedxraystudiesofnucleationandgrowthduringsolvothermalsynthesis
AT banerjeesoham areactorfortimeresolvedxraystudiesofnucleationandgrowthduringsolvothermalsynthesis
AT zimmermannmartinv areactorfortimeresolvedxraystudiesofnucleationandgrowthduringsolvothermalsynthesis
AT glaeveckephilipp areactorfortimeresolvedxraystudiesofnucleationandgrowthduringsolvothermalsynthesis
AT gutowskiolof areactorfortimeresolvedxraystudiesofnucleationandgrowthduringsolvothermalsynthesis
AT jørgensenmadsryvogel areactorfortimeresolvedxraystudiesofnucleationandgrowthduringsolvothermalsynthesis
AT iversenbobrummerstedt areactorfortimeresolvedxraystudiesofnucleationandgrowthduringsolvothermalsynthesis
AT roelsgaardmartin reactorfortimeresolvedxraystudiesofnucleationandgrowthduringsolvothermalsynthesis
AT kløvemagnus reactorfortimeresolvedxraystudiesofnucleationandgrowthduringsolvothermalsynthesis
AT christensenrasmus reactorfortimeresolvedxraystudiesofnucleationandgrowthduringsolvothermalsynthesis
AT bertelsenandreasd reactorfortimeresolvedxraystudiesofnucleationandgrowthduringsolvothermalsynthesis
AT brogenilsln reactorfortimeresolvedxraystudiesofnucleationandgrowthduringsolvothermalsynthesis
AT kantorinnokenty reactorfortimeresolvedxraystudiesofnucleationandgrowthduringsolvothermalsynthesis
AT sørensendanielrisskov reactorfortimeresolvedxraystudiesofnucleationandgrowthduringsolvothermalsynthesis
AT dippelannchristin reactorfortimeresolvedxraystudiesofnucleationandgrowthduringsolvothermalsynthesis
AT banerjeesoham reactorfortimeresolvedxraystudiesofnucleationandgrowthduringsolvothermalsynthesis
AT zimmermannmartinv reactorfortimeresolvedxraystudiesofnucleationandgrowthduringsolvothermalsynthesis
AT glaeveckephilipp reactorfortimeresolvedxraystudiesofnucleationandgrowthduringsolvothermalsynthesis
AT gutowskiolof reactorfortimeresolvedxraystudiesofnucleationandgrowthduringsolvothermalsynthesis
AT jørgensenmadsryvogel reactorfortimeresolvedxraystudiesofnucleationandgrowthduringsolvothermalsynthesis
AT iversenbobrummerstedt reactorfortimeresolvedxraystudiesofnucleationandgrowthduringsolvothermalsynthesis