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  Understanding Anomalous Gas-Phase Peak Shifts in Dip-and-Pull Ambient Pressure XPS Experiments

Teschner, D., Plescher, J., Piccinin, S., Jones, T. E., Hammud, A., Schmidt, F., et al. (2024). Understanding Anomalous Gas-Phase Peak Shifts in Dip-and-Pull Ambient Pressure XPS Experiments. The Journal of Physical Chemistry C, 128(17), 7096-7105. doi:10.1021/acs.jpcc.4c00113.

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teschner-et-al-2024-understanding-anomalous-gas-phase-peak-shifts-in-dip-and-pull-ambient-pressure-xps-experiments.pdf (Verlagsversion), 4MB
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 Urheber:
Teschner, Detre1, Autor                 
Plescher, Julius2, Autor           
Piccinin, Simone, Autor
Jones, Travis E., Autor
Hammud, Adnan1, Autor                 
Schmidt, Franz1, Autor                 
Knop-Gericke, Axel1, Autor           
Bluhm, Hendrik1, Autor                 
Shavorskiy, Andrey, Autor
Affiliations:
1Inorganic Chemistry, Fritz Haber Institute, Max Planck Society, ou_24023              
2Physical Chemistry, Fritz Haber Institute, Max Planck Society, ou_634546              

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 Zusammenfassung: Dip-and-pull ambient pressure X-ray photoelectron spectroscopy (AP-XPS) holds promise to uncover elementary processes of (photo)electrochemistry. We show, however, that the sample for such experiments should preferably be nonporous and the potential on the surface homogeneous. We carried out dip-and-pull AP-XPS experiments on a hematite thin film sample under the photoelectrochemical oxygen evolution reaction (OER) and find unexpected O 1s core level shifts. Upon electrochemical biasing under simulated solar light illumination, the gas-phase water peak shifted more than the electrolyte peak. To uncover the origin of the unexpected larger shift of the gas-phase peak, we performed electrostatic simulations using COMSOL, to map the potential field in the relevant volume between the sample and the first aperture of the XPS spectrometer. A number of geometric models were considered. We find that when the potential on the sample surface is inhomogeneous, e.g., with ionically isolated electrolyte patches, the gas-phase peak of the spectrum can shift more than the peak due to the electrolyte film. This suggests that at the measured sample position, the local potential was not as set by the potentiostat. Despite this, we find reversible consumption and replenishment of hydroxide in the spectra, which, due to OH being the reactant of the OER in alkaline electrolyte, makes sense chemically. We propose that this is linked to OH diffusion across the measured sample position, driven by the potential dependent consumption and replenishment of OH at the nearby well-connected surface regions.

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Sprache(n): eng - English
 Datum: 2024-04-092024-01-062024-04-102024-04-222024-05-02
 Publikationsstatus: Erschienen
 Seiten: 10
 Ort, Verlag, Ausgabe: -
 Inhaltsverzeichnis: -
 Art der Begutachtung: Expertenbegutachtung
 Identifikatoren: DOI: 10.1021/acs.jpcc.4c00113
 Art des Abschluß: -

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Titel: The Journal of Physical Chemistry C
  Kurztitel : J. Phys. Chem. C
Genre der Quelle: Zeitschrift
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Ort, Verlag, Ausgabe: Washington, D.C. : American Chemical Society
Seiten: 10 Band / Heft: 128 (17) Artikelnummer: - Start- / Endseite: 7096 - 7105 Identifikator: ISSN: 1932-7447
CoNE: https://pure.mpg.de/cone/journals/resource/954926947766