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Application of near-ambient pressure X-ray photoelectron spectroscopy (NAP-XPS) in an in-situ analysis of the stability of the surface-supported metal-organic framework HKUST-1 in water, methanol and pyridine atmospheres

  • Surface-supported metal-organic frameworks HKUST-1 (Hong Kong University of Science and Technology) were used as a model system for a development of a near ambient pressure (NAP) XPS based approach to investigate interaction with atmospheres of water, methanol or pyridine at pressures ranging from 1 to 4 mbar. The films were grown on a gold substrate functionalized with a COOH-terminated self-assembled monolayer using liquidphase epitaxy in a step-by-step fashion. Measurement protocols were developed and optimised for different gases in order to obtain spectra of similar quality in terms of signal intensity, noise and shape. Peak shapes were found to depend on the efficiency of charge compensation. Reference measurements in argon proved to be a useful strategy not only for the evaluation of the Cu(II)-fraction in pristine samples, but also to identify the contributions by the respective gas atmosphere to the C 1s and O 1s photoelectron spectra. Reduced copper was found during theSurface-supported metal-organic frameworks HKUST-1 (Hong Kong University of Science and Technology) were used as a model system for a development of a near ambient pressure (NAP) XPS based approach to investigate interaction with atmospheres of water, methanol or pyridine at pressures ranging from 1 to 4 mbar. The films were grown on a gold substrate functionalized with a COOH-terminated self-assembled monolayer using liquidphase epitaxy in a step-by-step fashion. Measurement protocols were developed and optimised for different gases in order to obtain spectra of similar quality in terms of signal intensity, noise and shape. Peak shapes were found to depend on the efficiency of charge compensation. Reference measurements in argon proved to be a useful strategy not only for the evaluation of the Cu(II)-fraction in pristine samples, but also to identify the contributions by the respective gas atmosphere to the C 1s and O 1s photoelectron spectra. Reduced copper was found during the exposition of HKUST-1 to water vapour and pyridine, but this effect was not observed in case of methanol. Additionally, it was established that there are no changes in relative Cu(II) percentage with increasing exposure time. This indicates that saturation was reached already at the lowest time of gas exposure. A detailed elucidation of the mechanism of Cu(II) reduction to Cu(I) in HKUST-1 mediated by water and pyridine is part of ongoing work and not in the scope of the present paper.zeige mehrzeige weniger

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Autor*innen:Marit Kjaervik, P. M. Dietrich, A. Thissen, Jörg RadnikORCiD, A. Nefedov, C. Natzeck, C. Wöll, Wolfgang UngerORCiD
Dokumenttyp:Zeitschriftenartikel
Veröffentlichungsform:Verlagsliteratur
Sprache:Englisch
Titel des übergeordneten Werkes (Englisch):Journal of Electron Spectroscopy and Related Phenomena
Jahr der Erstveröffentlichung:2021
Organisationseinheit der BAM:6 Materialchemie
6 Materialchemie / 6.1 Oberflächen- und Dünnschichtanalyse
Verlag:Elsevier B.V.
Verlagsort:Amsterdam, Netherlands
Ausgabe/Heft:247
Erste Seite:147042
DDC-Klassifikation:Naturwissenschaften und Mathematik / Chemie / Analytische Chemie
Freie Schlagwörter:HKUST-1; Interaction with atmospheres; Metal-organic frameworks; Near-ambient pressure X-ray photoelectron spectroscopy; Water
Themenfelder/Aktivitätsfelder der BAM:Chemie und Prozesstechnik
DOI:10.1016/j.elspec.2020.147042
ISSN:0368-2048
Verfügbarkeit des Dokuments:Datei im Netzwerk der BAM verfügbar ("Closed Access")
Datum der Freischaltung:10.02.2021
Referierte Publikation:Ja
Datum der Eintragung als referierte Publikation:10.05.2021
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