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Probing Surface Changes in Fe–Ni Oxide Nanocatalysts with a ToF-SIMS-Coupled Electrochemistry Setup and Principal Component Analysis
- Understanding catalyst surface dynamics under operating conditions is essential for improving electrocatalytic performance. Here, we present a novel approach combining electrochemical treatment with contamination-free transfer to Time-of-Flight Secondary Ion Mass Spectrometry (ToF-SIMS), followed by principal component analysis (PCA), to probe surface and interfacial changes in Ni–Fe oxide nanoparticles stabilized by polyvinylpyrrolidone (PVP) during the oxygen evolution reaction (OER). The surface analysis at three distinct treatment stages revealed distinct chemical fingerprints across pristine nanoparticles, after exposure to 1 M KOH electrolyte, and after cyclic voltammetry treatment. The results highlight a progressive transition from ligand-rich to ligand-depleted interfaces, with PVP-related fragments dominant in the early stages and metal- and electrolyte-derived species emerging after activation. Complementary ToF-SIMS analysis of electrolyte deposited on Si wafers after eachUnderstanding catalyst surface dynamics under operating conditions is essential for improving electrocatalytic performance. Here, we present a novel approach combining electrochemical treatment with contamination-free transfer to Time-of-Flight Secondary Ion Mass Spectrometry (ToF-SIMS), followed by principal component analysis (PCA), to probe surface and interfacial changes in Ni–Fe oxide nanoparticles stabilized by polyvinylpyrrolidone (PVP) during the oxygen evolution reaction (OER). The surface analysis at three distinct treatment stages revealed distinct chemical fingerprints across pristine nanoparticles, after exposure to 1 M KOH electrolyte, and after cyclic voltammetry treatment. The results highlight a progressive transition from ligand-rich to ligand-depleted interfaces, with PVP-related fragments dominant in the early stages and metal- and electrolyte-derived species emerging after activation. Complementary ToF-SIMS analysis of electrolyte deposited on Si wafers after each treatment step confirms the concurrent leaching of PVP and Fe–Ni-based fragments during OER. These findings underscore the dynamic nature of catalyst–electrolyte interfaces and demonstrate a robust strategy for monitoring surface-sensitive chemical changes associated with the nanoparticles, especially during the initial cycles of the OER.…


| Autor*innen: | Heydar Habibimarkani, Jörg RadnikORCiD, Vasile-Dan HodoroabaORCiD, Elisabeth John |
|---|---|
| Dokumenttyp: | Zeitschriftenartikel |
| Veröffentlichungsform: | Verlagsliteratur |
| Sprache: | Englisch |
| Titel des übergeordneten Werkes (Englisch): | Analytical Chemistry |
| Jahr der Erstveröffentlichung: | 2025 |
| Organisationseinheit der BAM: | 6 Materialchemie |
| 6 Materialchemie / 6.1 Oberflächen- und Dünnschichtanalyse | |
| Veröffentlichende Institution: | Bundesanstalt für Materialforschung und -prüfung (BAM) |
| Verlag: | American Chemical Society (ACS) |
| Aufsatznummer: | acs.analchem.5c03894 |
| Erste Seite: | 1 |
| Letzte Seite: | 8 |
| DDC-Klassifikation: | Technik, Medizin, angewandte Wissenschaften / Ingenieurwissenschaften / Ingenieurwissenschaften und zugeordnete Tätigkeiten |
| Technik, Medizin, angewandte Wissenschaften / Ingenieurwissenschaften / Angewandte Physik | |
| Freie Schlagwörter: | Electrochemistry; Fe-Ni oxide; Nanocatalysts; OER; PCA (principal component analysis); ToF-SIMS |
| Themenfelder/Aktivitätsfelder der BAM: | Energie |
| Energie / Elektrische Energiespeicher und -umwandlung | |
| Material | |
| Material / Advanced Materials | |
| DOI: | 10.1021/acs.analchem.5c03894 |
| URN: | urn:nbn:de:kobv:b43-652667 |
| ISSN: | 0003-2700 |
| Verfügbarkeit des Dokuments: | Datei für die Öffentlichkeit verfügbar ("Open Access") |
| Lizenz (Deutsch): | Creative Commons - CC BY - Namensnennung 4.0 International |
| Datum der Freischaltung: | 05.01.2026 |
| Referierte Publikation: | Ja |
| Datum der Eintragung als referierte Publikation: | 05.01.2026 |
| Schriftenreihen ohne Nummerierung: | Wissenschaftliche Artikel der BAM |


