Proceedings of MATSUS23 & Sustainable Technology Forum València (STECH23) (MATSUS23)
DOI: https://doi.org/10.29363/nanoge.matsus.2023.126
Publication date: 22nd December 2022
Operando characterization techniques are indispensable for understanding the catalysts evolution during operation. Electrochemical liquid-phase transmission electron microscopy (ec-LPTEM) grants the capability of real-time imaging of electrochemically-induced processes in liquid media. Herein, we describe the advancements of ec-LPTEM towards studying the solid-liquid-gas interfacial processes occurring on Co-based oxide oxygen evolving catalysts. By performing real-time measurements, we can associate the potential-dependent variation of the local contrast to the effects that precede the electrocatalytic reaction such as electrowetting and redox-induced reactions. Further, through optimization of the microcell, we report on the direct probing of the evolution of molecular oxygen by operando electron energy loss spectroscopy (EELS). Similar experiments on IrO2 particles indicate the capability to separate the contribution of different components in the EEL spectra, providing qualitative maps of O2 and liquid electrolyte. Our work on catalytic particles exemplifies the crucial role that surface sensitive and electrochemical microcell TEM techniques can play in detailing the mechanism of electrocatalytic processes and can provide a new characterization framework aiding development of novel design routes for targeted nanocatalyst preparation.
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