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Operando x-ray absorption spectroscopy unveils light-driven redox dynamics at the semiconductor/cocatalyst interface.

Raffaello Mazzaro1,2, Alberto Piccioni1,2, Marco Salvi1

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We uncovered light-induced changes in cobalt-iron oxide (CoFeOₓ) cocatalysts during solar water splitting. Operando X-ray techniques revealed a new interfacial state and distinct photocatalytic cycles, crucial for efficient solar energy conversion.

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Area of Science:

  • Materials Science
  • Electrochemistry
  • Photocatalysis

Background:

  • Cobalt-based mixed oxides are key oxygen evolution reaction (OER) catalysts.
  • Their function as photoelectrochemical cocatalysts under irradiation is not well understood.
  • Operando studies are needed to probe irradiation-induced structural changes.

Purpose of the Study:

  • To investigate the redox dynamics of cobalt-iron oxide (CoFeOₓ) cocatalysts in semiconductor photoanodes.
  • To understand the role of interfacial structure and light in modulating catalytic activity for solar water splitting.
  • To elucidate charge transfer mechanisms at the semiconductor/cocatalyst interface.

Main Methods:

  • Utilized operando X-ray absorption spectroscopy (XAS) combined with fixed-energy X-ray absorption voltammetry (FEXRAV).
  • Probed cobalt oxidation states at the semiconductor/cocatalyst interface under both dark and illuminated conditions.
  • Analyzed element-selective changes to understand interfacial charge transfer.

Main Results:

  • Discovered a novel interfacial cobalt state influencing catalytic activity.
  • Observed light-induced reduction in cobalt oxidation state and a cathodic shift in redox potentials.
  • Identified a photocatalytic cycle distinct from the dark-state electrocatalysis, showing light's impact on rate-determining steps.

Conclusions:

  • Interface structure plays a critical role in tuning the catalytic activity of CoFeOₓ cocatalysts.
  • Light significantly modulates the catalytic behavior and redox potentials of the cocatalyst.
  • Operando X-ray techniques are powerful tools for understanding interfacial charge transfer and designing efficient photoelectrochemical systems for solar water splitting.