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NiFe oxyhydroxide is one of the most promising oxygen evolution reaction(OER) catalysts for renewable hydrogen production, and deciphering the identityand reactivity of the oxygen intermediates on its surface is a key challengebut is critical to understanding the OER mechanism as well as designingwater-splitting catalysts with higher efficiencies. Here, we screened andutilized in situ reactive probes that can selectively target specific oxygenintermediates with high rates to investigate the OER intermediates and pathwayon NiFe oxyhydroxide. Most importantly, the oxygen atom transfer (OAT) probes(e.g. 4-(Diphenylphosphino) benzoic acid) could efficiently inhibit the OERkinetics by scavenging the OER intermediates, exhibiting lower OER currents,larger Tafel slopes and larger kinetic isotope effect values, while probes withother reactivities demonstrated much smaller effects. Combining the OATreactivity with electrochemical kinetic and operando Raman spectroscopictechniques, we identified a resting Fe=O intermediate in the Ni-O scaffold anda rate-limiting O-O chemical coupling step between a Fe=O moiety and a vicinalbridging O. DFT calculation further revealed a longer Fe=O bond formed on thesurface and a large kinetic energy barrier of the O-O chemical step,corroborating the experimental results. These results point to a new directionof liberating lattice O and expediting O-O coupling for optimizing NiFe-basedOER electrocatalyst.

Recognition of Surface Oxygen Intermediates on NiFe Oxyhydroxide Oxygen-evolving Catalysts by Homogeneous Oxidation Reactivity