Zitieren Sie bitte immer diesen URN: urn:nbn:de:kobv:b43-567659
Dispersive x-ray absorption spectroscopy for time-resolved in situ monitoring of mechanochemical reactions
- X-ray absorption spectroscopy (XAS) provides a unique, atom-specific tool to probe the electronic structure of solids. By surmounting long-held limitations of powder-based XAS using a dynamically averaged powder in a Resonant Acoustic Mixer (RAM), we demonstrate how time-resolved in situ (TRIS) XAS provides unprecedented detail of mechanochemical synthesis. The use of a custom-designed dispersive XAS (DXAS) setup allows us to increase the time resolution over existing fluorescence measurements from ∼15 min to 2 s for a complete absorption spectrum. Hence, we here establish TRIS-XAS as a viable method for studying mechanochemical reactions and sampling reaction kinetics. The generality of our approach is demonstrated through RAM-induced (i) bottom-up Au nanoparticle mechanosynthesis and (ii) the synthesis of a prototypical metal organic framework, ZIF-8. Moreover, we demonstrate that our approach also works with the addition of a stainless steel milling ball, opening the door to usingX-ray absorption spectroscopy (XAS) provides a unique, atom-specific tool to probe the electronic structure of solids. By surmounting long-held limitations of powder-based XAS using a dynamically averaged powder in a Resonant Acoustic Mixer (RAM), we demonstrate how time-resolved in situ (TRIS) XAS provides unprecedented detail of mechanochemical synthesis. The use of a custom-designed dispersive XAS (DXAS) setup allows us to increase the time resolution over existing fluorescence measurements from ∼15 min to 2 s for a complete absorption spectrum. Hence, we here establish TRIS-XAS as a viable method for studying mechanochemical reactions and sampling reaction kinetics. The generality of our approach is demonstrated through RAM-induced (i) bottom-up Au nanoparticle mechanosynthesis and (ii) the synthesis of a prototypical metal organic framework, ZIF-8. Moreover, we demonstrate that our approach also works with the addition of a stainless steel milling ball, opening the door to using TRIS-DXAS for following conventional ball milling reactions. We expect that our TRIS-DXAS approach will become an essential part of the mechanochemical tool box.…
Autor*innen: | Ana de Oliveira Guilherme BuzanichORCiD, Cafer Tufan CakirORCiD, Martin RadtkeORCiD, M. Bilal Haider, Franziska EmmerlingORCiD, P. F. M. Oliveira, Adam A. L. Michalchuk |
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Dokumenttyp: | Zeitschriftenartikel |
Veröffentlichungsform: | Verlagsliteratur |
Sprache: | Englisch |
Titel des übergeordneten Werkes (Englisch): | Journal of chemical physics |
Jahr der Erstveröffentlichung: | 2022 |
Organisationseinheit der BAM: | 6 Materialchemie |
6 Materialchemie / 6.0 Abteilungsleitung und andere | |
6 Materialchemie / 6.3 Strukturanalytik | |
Veröffentlichende Institution: | Bundesanstalt für Materialforschung und -prüfung (BAM) |
Verlag: | American Institute of Physics |
Verlagsort: | Melville, NY |
Jahrgang/Band: | 157 |
Ausgabe/Heft: | 21 |
Aufsatznummer: | 214202 |
Erste Seite: | 1 |
Letzte Seite: | 12 |
DDC-Klassifikation: | Naturwissenschaften und Mathematik / Chemie / Analytische Chemie |
Technik, Medizin, angewandte Wissenschaften / Ingenieurwissenschaften / Ingenieurwissenschaften und zugeordnete Tätigkeiten | |
Freie Schlagwörter: | Dipsersive XAS; In situ studies; Mechanochemistry; Time-resolved |
Themenfelder/Aktivitätsfelder der BAM: | Chemie und Prozesstechnik |
Material | |
DOI: | 10.1063/5.0130673 |
URN: | urn:nbn:de:kobv:b43-567659 |
ISSN: | 1089-7690 |
Verfügbarkeit des Dokuments: | Datei für die Öffentlichkeit verfügbar ("Open Access") |
Lizenz (Deutsch): | Creative Commons - CC BY - Namensnennung 4.0 International |
Datum der Freischaltung: | 02.01.2023 |
Referierte Publikation: | Ja |
Datum der Eintragung als referierte Publikation: | 02.01.2023 |
Paper des Monats: | Ja |
Schriftenreihen ohne Nummerierung: | Wissenschaftliche Artikel der BAM |