Journal of Synchrotron Radiation (Mar 2023)

Monitoring surface dynamics of electrodes during electrocatalysis using in situ synchrotron FTIR spectroscopy

  • Weiren Cheng,
  • Yanzhi Xu,
  • Chenyu Yang,
  • Hui Su,
  • Qinghua Liu

DOI
https://doi.org/10.1107/S1600577523000796
Journal volume & issue
Vol. 30, no. 2
pp. 340 – 346

Abstract

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Monitoring the surface dynamics of catalysts under working conditions is important for a deep understanding of the underlying electrochemical mechanisms towards efficient energy conversion and storage. Fourier transform infrared (FTIR) spectroscopy with high surface sensitivity has been considered as a powerful tool for detecting surface adsorbates, but it faces a great challenge when being adopted in surface dynamics investigations during electrocatalysis due to the complication and influence of aqueous environments. This work reports a well designed FTIR cell with tunable micrometre-scale water film over the surface of working electrodes and dual electrolyte/gas channels for in situ synchrotron FTIR tests. By coupling with a facile single-reflection infrared mode, a general in situ synchrotron radiation FTIR (SR-FTIR) spectroscopic method is developed for tracking the surface dynamics of catalysts during the electrocatalytic process. As an example, in situ formed key *OOH is clearly observed on the surface of commercial benchmark IrO2 catalysts during the electrochemical oxygen evolution process based on the developed in situ SR-FTIR spectroscopic method, which demonstrates its universality and feasibility in surface dynamics studies of electrocatalysts under working conditions.

Keywords