Lange, Martin Alexander ; Krysiak, Yaşar ; Hartmann, Jens ; Dewald, Georg ; Cerretti, Giacomo ; Tahir, Muhammad Nawaz ; Panthöfer, Martin ; Barton, Bastian ; Reich, Tobias ; Zeier, Wolfgang G. ; Mondeshki, Mihail ; Kolb, Ute ; Tremel, Wolfgang (2024)
Solid State Fluorination on the Minute Scale: Synthesis of WO₃₋ₓFx with Photocatalytic Activity.
In: Advanced Functional Materials, 2020, 30 (13)
doi: 10.26083/tuprints-00016727
Artikel, Zweitveröffentlichung, Verlagsversion
 | Es ist eine neuere Version dieses Eintrags verfügbar. |
Kurzbeschreibung (Abstract)
Solid state reactions are notoriously slow, because the rate‐limiting step is diffusion of atoms or ions through reactant, intermediate, and product crystalline phases. This requires days or even weeks of high temperature treatment, consuming large amounts of energy. Metal oxides are particularly difficult to react, because they have high melting points. The study reports a high‐speed solid state fluorination of WO₃ with Teflon to the oxyfluorides WO₃₋ₓFx on a minute (<10 min) scale by spark plasma sintering, a technique that is used typically for a high‐speed consolidation of powders. Automated electron diffraction analysis reveals an orthorhombic ReO₃‐type structure of WO₃₋ₓFx with F atom disorder as demonstrated by ¹⁹F magic angle spinning nuclear magnetic resonance spectroscopy. The potential of this new approach is demonstrated by the following results. i) Mixed‐ valent tungsten oxide fluorides WO₃₋ₓFx with high F content (0 < x < 0.65) are obtained as metastable products in copious amounts within minutes. ii) The spark plasma sintering technique yields WO₃₋ₓFx nanoparticles with high photocatalytic activity, whereas the corresponding bulk phases obtained by conventional solid‐state (ampoule) reactions have no photocatalytic activity. iii) The catalytic activity is caused by the microstructure originating from the processing by spark plasma sintering.
| Typ des Eintrags: | Artikel |
|---|---|
| Erschienen: | 2024 |
| Autor(en): | Lange, Martin Alexander ; Krysiak, Yaşar ; Hartmann, Jens ; Dewald, Georg ; Cerretti, Giacomo ; Tahir, Muhammad Nawaz ; Panthöfer, Martin ; Barton, Bastian ; Reich, Tobias ; Zeier, Wolfgang G. ; Mondeshki, Mihail ; Kolb, Ute ; Tremel, Wolfgang |
| Art des Eintrags: | Zweitveröffentlichung |
| Titel: | Solid State Fluorination on the Minute Scale: Synthesis of WO₃₋ₓFx with Photocatalytic Activity |
| Sprache: | Englisch |
| Publikationsjahr: | 26 Januar 2024 |
| Ort: | Darmstadt |
| Publikationsdatum der Erstveröffentlichung: | 2020 |
| Ort der Erstveröffentlichung: | Weinheim |
| Verlag: | Wiley-VCH |
| Titel der Zeitschrift, Zeitung oder Schriftenreihe: | Advanced Functional Materials |
| Jahrgang/Volume einer Zeitschrift: | 30 |
| (Heft-)Nummer: | 13 |
| Kollation: | 13 Seiten |
| DOI: | 10.26083/tuprints-00016727 |
| URL / URN: | https://tuprints.ulb.tu-darmstadt.de/16727 |
| Zugehörige Links: | |
| Herkunft: | Zweitveröffentlichung DeepGreen |
| Kurzbeschreibung (Abstract): | Solid state reactions are notoriously slow, because the rate‐limiting step is diffusion of atoms or ions through reactant, intermediate, and product crystalline phases. This requires days or even weeks of high temperature treatment, consuming large amounts of energy. Metal oxides are particularly difficult to react, because they have high melting points. The study reports a high‐speed solid state fluorination of WO₃ with Teflon to the oxyfluorides WO₃₋ₓFx on a minute (<10 min) scale by spark plasma sintering, a technique that is used typically for a high‐speed consolidation of powders. Automated electron diffraction analysis reveals an orthorhombic ReO₃‐type structure of WO₃₋ₓFx with F atom disorder as demonstrated by ¹⁹F magic angle spinning nuclear magnetic resonance spectroscopy. The potential of this new approach is demonstrated by the following results. i) Mixed‐ valent tungsten oxide fluorides WO₃₋ₓFx with high F content (0 < x < 0.65) are obtained as metastable products in copious amounts within minutes. ii) The spark plasma sintering technique yields WO₃₋ₓFx nanoparticles with high photocatalytic activity, whereas the corresponding bulk phases obtained by conventional solid‐state (ampoule) reactions have no photocatalytic activity. iii) The catalytic activity is caused by the microstructure originating from the processing by spark plasma sintering. |
| Freie Schlagworte: | automated diffraction tomography, fluorination, photocatalysis, spark plasma synthesis, tungsten oxyfluoride |
| ID-Nummer: | 1909051 |
| Status: | Verlagsversion |
| URN: | urn:nbn:de:tuda-tuprints-167275 |
| Zusätzliche Informationen: | Dedicated with admiration to Prof. Arndt Simon on the occasion of his 80 birthday |
| Sachgruppe der Dewey Dezimalklassifikatin (DDC): | 500 Naturwissenschaften und Mathematik > 540 Chemie |
| Fachbereich(e)/-gebiet(e): | 11 Fachbereich Material- und Geowissenschaften 11 Fachbereich Material- und Geowissenschaften > Geowissenschaften 11 Fachbereich Material- und Geowissenschaften > Geowissenschaften > Fachgebiet Geomaterialwissenschaft |
| Hinterlegungsdatum: | 26 Jan 2024 14:08 |
| Letzte Änderung: | 29 Jan 2024 07:02 |
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| Suche nach Titel in: | TUfind oder in Google |
Verfügbare Versionen dieses Eintrags
- Solid State Fluorination on the Minute Scale: Synthesis of WO₃₋ₓFx with Photocatalytic Activity. (deposited 26 Jan 2024 14:08) [Gegenwärtig angezeigt]
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