In situ solid-state NMR and XRD investigations of structural transformations in crystalline porous solids

In-situ measurement techniques have significantly gained in importance during the last decades, as they have the potential to reveal detailed and realistic insights into chemical reactions. Also for complex processes in solid phases as adsorption or structural transformations in-situ investigations...

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Tác giả chính: Paula, Carolin
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Được phát hành: FAU University Press 2026
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author Paula, Carolin
author_browse Paula, Carolin
author_facet Paula, Carolin
author_sort Paula, Carolin
collection Directory of Open Access Books
description In-situ measurement techniques have significantly gained in importance during the last decades, as they have the potential to reveal detailed and realistic insights into chemical reactions. Also for complex processes in solid phases as adsorption or structural transformations in-situ investigations are the method of choice to receive information at molecular level. In this work a novel designed 4.0 mm wide-bore probe is presented that enables in-situ solid-state NMR measurements under continuous flow conditions and at elevated temperature while the rotor is spinning at the magic angle. The special feature of the probe is a very fast, selective and uniform heating of the sample in the rotor which is realized by lasers. The operation and working principle of the probe is demonstrated with oberservations of structural transformations in porous crystalline solids. In combination with in-situ XRD studies the application of the probe allowed for new insights into the recrystallization kinetics and mechanism of VPI-5 to AlPO4-8 and the breathing behaviour of MOFs with MIL-53 type topolgy.
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spelling doab-20.500.12854ir-1707722026-01-07T05:09:04Z In situ solid-state NMR and XRD investigations of structural transformations in crystalline porous solids Paula, Carolin In-Situ MAS NMR spectroscopy MIL-53 solid-solid transformation crystalline porous solids VPI-5 In-situ X-ray diffractometry breathing behaviour thema EDItEUR::P Mathematics and Science::PN Chemistry::PNF Analytical chemistry::PNFS Spectrum analysis, spectrochemistry, mass spectrometry thema EDItEUR::M Medicine and Nursing::MF Pre-clinical medicine: basic sciences::MFG Physiology::MFGV Biomechanics, human kinetics thema EDItEUR::P Mathematics and Science::PN Chemistry In-situ measurement techniques have significantly gained in importance during the last decades, as they have the potential to reveal detailed and realistic insights into chemical reactions. Also for complex processes in solid phases as adsorption or structural transformations in-situ investigations are the method of choice to receive information at molecular level. In this work a novel designed 4.0 mm wide-bore probe is presented that enables in-situ solid-state NMR measurements under continuous flow conditions and at elevated temperature while the rotor is spinning at the magic angle. The special feature of the probe is a very fast, selective and uniform heating of the sample in the rotor which is realized by lasers. The operation and working principle of the probe is demonstrated with oberservations of structural transformations in porous crystalline solids. In combination with in-situ XRD studies the application of the probe allowed for new insights into the recrystallization kinetics and mechanism of VPI-5 to AlPO4-8 and the breathing behaviour of MOFs with MIL-53 type topolgy. 2026-01-07T05:09:03Z 2026-01-07T05:09:03Z 2026-01-06T13:12:20Z 2021 book ONIX_20260106T140303_9783961474509_40 https://library.oapen.org/handle/20.500.12657/109613 9783961474509 9783961474493 https://directory.doabooks.org/handle/20.500.12854/170772 eng open access image/jpeg Attribution 4.0 International https://library.oapen.org/bitstream/20.500.12657/109613/1/9783961474509.pdf FAU University Press 10.25593/978-3-96147-450-9 10.25593/978-3-96147-450-9 2c600dea-eece-4066-87be-da335e323fdb 9783961474509 9783961474493 AG Universitätsverlage 209 Erlangen open access
spellingShingle In-Situ MAS NMR spectroscopy
MIL-53
solid-solid transformation
crystalline porous solids
VPI-5
In-situ X-ray diffractometry
breathing behaviour
thema EDItEUR::P Mathematics and Science::PN Chemistry::PNF Analytical chemistry::PNFS Spectrum analysis, spectrochemistry, mass spectrometry
thema EDItEUR::M Medicine and Nursing::MF Pre-clinical medicine: basic sciences::MFG Physiology::MFGV Biomechanics, human kinetics
thema EDItEUR::P Mathematics and Science::PN Chemistry
Paula, Carolin
In situ solid-state NMR and XRD investigations of structural transformations in crystalline porous solids
title In situ solid-state NMR and XRD investigations of structural transformations in crystalline porous solids
title_full In situ solid-state NMR and XRD investigations of structural transformations in crystalline porous solids
title_fullStr In situ solid-state NMR and XRD investigations of structural transformations in crystalline porous solids
title_full_unstemmed In situ solid-state NMR and XRD investigations of structural transformations in crystalline porous solids
title_short In situ solid-state NMR and XRD investigations of structural transformations in crystalline porous solids
title_sort in situ solid state nmr and xrd investigations of structural transformations in crystalline porous solids
topic In-Situ MAS NMR spectroscopy
MIL-53
solid-solid transformation
crystalline porous solids
VPI-5
In-situ X-ray diffractometry
breathing behaviour
thema EDItEUR::P Mathematics and Science::PN Chemistry::PNF Analytical chemistry::PNFS Spectrum analysis, spectrochemistry, mass spectrometry
thema EDItEUR::M Medicine and Nursing::MF Pre-clinical medicine: basic sciences::MFG Physiology::MFGV Biomechanics, human kinetics
thema EDItEUR::P Mathematics and Science::PN Chemistry
topic_facet In-Situ MAS NMR spectroscopy
MIL-53
solid-solid transformation
crystalline porous solids
VPI-5
In-situ X-ray diffractometry
breathing behaviour
thema EDItEUR::P Mathematics and Science::PN Chemistry::PNF Analytical chemistry::PNFS Spectrum analysis, spectrochemistry, mass spectrometry
thema EDItEUR::M Medicine and Nursing::MF Pre-clinical medicine: basic sciences::MFG Physiology::MFGV Biomechanics, human kinetics
thema EDItEUR::P Mathematics and Science::PN Chemistry
url ONIX_20260106T140303_9783961474509_40
work_keys_str_mv AT paulacarolin insitusolidstatenmrandxrdinvestigationsofstructuraltransformationsincrystallineporoussolids