Crystalline γ-FeO(OH) dominantly possessing ─OH terminals (𝛾-FeO(OH)), polycrystalline γ-FeO(OH) containing multiple ─O, ─OH, and Fe terminals (𝛾-FeO(OH)), and α-FeO majorly containing ─O surface terminals are used as electrocatalysts to study the effect of surface terminals on electrocatalytic nitrate reduction reaction (eNORR) selectivity and stabilization of reaction intermediates. Brunauer-Emmett-Teller analysis and electrochemically determined surface area suggest a high active surface area of 117.79 m g (ECSA: 0.211 cm) for 𝛾-FeO(OH) maximizing the surface accessibility for nitrate adsorption and exhibiting selective eNORR to NH at pH 7 with a yield rate 18.326 mg h cm, >85% Faradaic efficiency (FE), and at least nine-times catalyst-recyclability. N- and D-labeling combined with in situ IR and Raman studies validate the adsorption of nitrate ions on the ─OH terminals of 𝛾-FeO(OH) and the generation of nitrite and hydroxyl amine as eNORR intermediates. A kinetic isotope effect (KIE) value of 2.1 indicates HO as the proton source and proton-coupled electron transfer as the rate-limiting step. The rotating-ring disk electrochemical (RRDE) study and subsequent Koutecký-Levich analysis reveal the electron-transfer rate constant (k) for the 2e- reduction of nitrate to nitrite is 5.7 × 10 cm s. This study provides direct evidence of the hydroxyl amine formation as the dominant pathway of eNORR on γ-FeO(OH).
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