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PreprintCC BY-NC-NDChemRxiv

A substrate-versatile operando electrochemical cell for X-ray absorption spectroscopy

  • Javier Villalobos1,2
  • Joaquin Morales-Santelices1,3
  • Dulce M. Morales1,4
  • Denis Antipin1
  • Omeshwari Yadorao Bisen1
  • Giacomo Zuliani1
  • Marcel Risch1,5
5 affiliations
  1. 1Helmholtz–Zentrum Berlin für Materialien und Energie GmbH, Hahn-Meitner Platz 1, Berlin, Germany, 14109
  2. 2Bundesanstalt für Materialforschung und -prüfung (BAM, Unter den Eichen 87, Berlin, Germany, 12205
  3. 3Institut für Solarenergieforschung GmbH, Am Ohrberg 1, Emmerthal, Germany, 31860
  4. 4Engineering and Technology institute Groningen (ENTEG, University of Groningen, Nijenborgh 3, Groningen, AG, Netherlands, 9747
  5. 5Freie Universität Berlin, Arnimalle 14, Berlin, 14195
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Abstract

Operando characterization techniques allow the understanding of electrochemical energy materials under operating conditions, which is essential to design high-performance electrocatalysts. Here, we present a novel operando electrochemical cell designed for X-ray absorption spectroscopy (XAS), enabling the simultaneous acquisition of electrochemical data, real-time oxygen detection, and XAS spectra on X-ray opaque electrodes. The incident X-ray beam reaches the sample through the electrolyte rather than through the substrate in contrast to the majority of other cells. This configuration removes constraints related to substrate transparency and thickness, thereby broadening the range of compatible electrode materials and samples that can be analyzed. The cell was commissioned using a well-characterized CoOx catalyst for the oxygen evolution reaction in alkaline media. Reversible shifts in the Co K-edge position were observed under applied potential steps, directly correlating electronic structure changes with electrochemical activity and oxygen production. The modular and adaptable design provides a versatile platform for advanced spectroelectrochemical investigations and can be extended to a wide range of electrochemical systems and complementary spectroscopic techniques.

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Cite

BibTeXRIS
BibTeX
@misc{villalobos2026substrateversatile,
  title = {{A substrate-versatile operando electrochemical cell for X-ray absorption spectroscopy}},
  author = {Javier Villalobos and Joaquin Morales-Santelices and Dulce M. Morales and Denis Antipin and Omeshwari Yadorao Bisen and Giacomo Zuliani and Marcel Risch},
  howpublished = {ChemRxiv},
  year = {2026},
  month = oct,
  doi = {10.26434/chemrxiv.15010804/v1},
  url = {https://chemrxiv.org/doi/full/10.26434/chemrxiv.15010804/v1},
  note = {CC BY-NC-ND},
}
RIS
TY  - UNPB
TI  - A substrate-versatile operando electrochemical cell for X-ray absorption spectroscopy
AU  - Javier Villalobos
AU  - Joaquin Morales-Santelices
AU  - Dulce M. Morales
AU  - Denis Antipin
AU  - Omeshwari Yadorao Bisen
AU  - Giacomo Zuliani
AU  - Marcel Risch
PY  - 2026
DA  - 2026/10/21
PB  - ChemRxiv
DO  - 10.26434/chemrxiv.15010804/v1
UR  - https://chemrxiv.org/doi/full/10.26434/chemrxiv.15010804/v1
AB  - Operando characterization techniques allow the understanding of electrochemical energy materials under operating conditions, which is essential to design high-performance electrocatalysts. Here, we present a novel operando electrochemical cell designed for X-ray absorption spectroscopy (XAS), enabling the simultaneous acquisition of electrochemical data, real-time oxygen detection, and XAS spectra on X-ray opaque electrodes. The incident X-ray beam reaches the sample through the electrolyte rather than through the substrate in contrast to the majority of other cells. This configuration removes constraints related to substrate transparency and thickness, thereby broadening the range of compatible electrode materials and samples that can be analyzed. The cell was commissioned using a well-characterized CoOx catalyst for the oxygen evolution reaction in alkaline media. Reversible shifts in the Co K-edge position were observed under applied potential steps, directly correlating electronic structure changes with electrochemical activity and oxygen production. The modular and adaptable design provides a versatile platform for advanced spectroelectrochemical investigations and can be extended to a wide range of electrochemical systems and complementary spectroscopic techniques.
ER  -