Proceedings of Materials for Sustainable Development Conference (MAT-SUS) (NFM22)
DOI: https://doi.org/10.29363/nanoge.nfm.2022.031
Publication date: 11th July 2022
The electrocatalysis systems are very sensitive to electrode surface structure as well as the surface composition. A detail investigation of the nature of electrocatalysts is essential not only for the identification of reaction active sites or components, but also for the clarification of mechanism of electrocatalysts deactivation/activation, as the case of oxygen evolution reaction (OER)1-2. X-ray photoelectron spectroscopy (XPS) coupled with electrochemical methods is a powerful technique for this purpose. However, it is still quite challenging to combine the conventional electrochemical measurement under ambient conditions with XPS measurement under ultra-high vacuum (UHV) conditions. The in situ electrochemical XPS methods can overcome the shortness of sample change during the transfer as it is commonly encountered in ex situ studies3. However, due to presence of both electrolyte and vapor, synchrotron technique is usually required. In addition, the electrochemical signals are usually distorted by poor mass transfer. We have developed a quasi in situ XPS which consist of electrochemical treatment at ambient pressure, air free transfer from ambient pressure to UHV, and detection under UHV conditions. It has great advantages in: 1) acquiring electrochemical signal of good quality that can be directly compared with those in conventional cells; 2) avoiding oxidation of electrocatalysts due to air exposure; 3) collecting high intensity XPS signals by only commercial X-ray source. In this presentation, I will introduction the detailed setup, benchmark practice, and the application of a nearly in situ XPS on obtaining information on oxygen evolution reaction on Ru based catalysts.
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