Publication date: 15th December 2025
Accurately distinguishing oxygen evolution reaction (OER) currents from anodic metal dissolution is essential for accurately evaluating metal electrocatalysts, as both processes often overlap in the transpassive potential region.[1, 2] This study explored multi-principal element alloys (MPEAs) as a pathway toward sustainable electrocatalysis by reducing reliance on noble and critical metals. CrCoNi and CrMnFeCoNi alloys are used as model systems to understand how complex compositions behave when OER and dissolution occur simultaneously, providing a benchmark for designing Co-reduced/free variants within the FeCrNi MPEA family.
To quantitatively separate these pathways, we employ an integrated operando approach: tip-substrate voltammetry in scanning electrochemical microscopy (TSV-SECM) for spatially resolved O2 detection, ICP-MS and UV-Vis spectroscopy for dissolution quantification and chromium speciation, and in-situ electrochemical AFM (EC-AFM) to identify the onset of corrosion and track nanoscale surface evolution. Converting dissolution data into electrochemical charge enables a precise attribution of transpassive currents to either OER or metal dissolution. To further assessmass-transport effects, MPEAs were examined using rotating disk electrode (RDE) methods. Controlled hydrodynamics separate kinetic from diffusion-limited regimes and reveal how dissolution rates, passive-film behavior, and OER activity respond under flow conditions.
Overall, this methodology provides a robust platform for reliably distinguishing catalytic OER performance from corrosion processes while guiding the design of next-generation electrocatalysts that minimize or eliminate Co and other critical and noble metals. Extending these insights to FeCrNi-based systems offers new opportunities for sustainable, high-performance materials capable of operating under technologically relevant anodic conditions.
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