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Operando Characterization of Porous Nickel Foam Water Splitting Electrodes Using Near-Ambient Pressure X-ray Photoelectron Spectroscopy

Chalil Oglou, Ramadan ; Frederiksen, Morten Linding ; Sun, Zhaozong ; Ceccato, Marcel ; Shavorskiy, Andrey LU and Lauritsen, Jeppe Vang (2025) In Journal of Physical Chemistry Letters 16(14). p.3597-3605
Abstract

This study presents a practical approach for characterizing industrial water-splitting nickel foam electrodes under both cathodic and anodic conditions by employing synchrotron radiation near-ambient pressure X-ray photoelectron spectroscopy (NAP-XPS). The in situ studies reveal quantitatively reduced and oxidized Ni species on the electrode surface by recording the Ni 2p3/2 signals after cycling the potential in cathodic and anodic regions, respectively. Operando studies demonstrate that a stable electrolyte film forms, allowing the probing of the solid/liquid interface under applied potentials. We attribute this stability to capillary forces within the porous structure of the foam, which enables the monitoring of surface... (More)

This study presents a practical approach for characterizing industrial water-splitting nickel foam electrodes under both cathodic and anodic conditions by employing synchrotron radiation near-ambient pressure X-ray photoelectron spectroscopy (NAP-XPS). The in situ studies reveal quantitatively reduced and oxidized Ni species on the electrode surface by recording the Ni 2p3/2 signals after cycling the potential in cathodic and anodic regions, respectively. Operando studies demonstrate that a stable electrolyte film forms, allowing the probing of the solid/liquid interface under applied potentials. We attribute this stability to capillary forces within the porous structure of the foam, which enables the monitoring of surface deprotonation under anodic potentials and surface protonation under cathodic potentials. Given that the most common industrial alkaline water electrolyzer electrodes are based on nickel foams similar to the samples measured in this study, the demonstrated method offers a valuable approach for fundamental NAP-XPS examination directly on industrially employed electrodes.

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author
; ; ; ; and
organization
publishing date
type
Contribution to journal
publication status
published
subject
in
Journal of Physical Chemistry Letters
volume
16
issue
14
pages
9 pages
publisher
The American Chemical Society (ACS)
external identifiers
  • scopus:105002148563
  • pmid:40178296
ISSN
1948-7185
DOI
10.1021/acs.jpclett.4c03362
language
English
LU publication?
yes
id
317894df-5ab1-4d2c-a49d-f72db94e52ac
date added to LUP
2025-08-15 14:40:25
date last changed
2025-08-15 16:05:46
@article{317894df-5ab1-4d2c-a49d-f72db94e52ac,
  abstract     = {{<p>This study presents a practical approach for characterizing industrial water-splitting nickel foam electrodes under both cathodic and anodic conditions by employing synchrotron radiation near-ambient pressure X-ray photoelectron spectroscopy (NAP-XPS). The in situ studies reveal quantitatively reduced and oxidized Ni species on the electrode surface by recording the Ni 2p<sub>3/2</sub> signals after cycling the potential in cathodic and anodic regions, respectively. Operando studies demonstrate that a stable electrolyte film forms, allowing the probing of the solid/liquid interface under applied potentials. We attribute this stability to capillary forces within the porous structure of the foam, which enables the monitoring of surface deprotonation under anodic potentials and surface protonation under cathodic potentials. Given that the most common industrial alkaline water electrolyzer electrodes are based on nickel foams similar to the samples measured in this study, the demonstrated method offers a valuable approach for fundamental NAP-XPS examination directly on industrially employed electrodes.</p>}},
  author       = {{Chalil Oglou, Ramadan and Frederiksen, Morten Linding and Sun, Zhaozong and Ceccato, Marcel and Shavorskiy, Andrey and Lauritsen, Jeppe Vang}},
  issn         = {{1948-7185}},
  language     = {{eng}},
  number       = {{14}},
  pages        = {{3597--3605}},
  publisher    = {{The American Chemical Society (ACS)}},
  series       = {{Journal of Physical Chemistry Letters}},
  title        = {{Operando Characterization of Porous Nickel Foam Water Splitting Electrodes Using Near-Ambient Pressure X-ray Photoelectron Spectroscopy}},
  url          = {{http://dx.doi.org/10.1021/acs.jpclett.4c03362}},
  doi          = {{10.1021/acs.jpclett.4c03362}},
  volume       = {{16}},
  year         = {{2025}},
}