Publication date: 15th December 2025
Nitrate contamination and the mechanistic complexity of nitrate electroreduction motivate direct, time‑resolved observation of surface intermediates that control selectivity. Nitrate electroreduction (NO3RR) is the electrochemical conversion of dissolved nitrate into less harmful or value-added nitrogen products (e.g., nitrite, N2, NH4+/NH3), offering a remediation route that transforms a persistent pollutant into benign or useful species while enabling integration with renewable electricity.[1] Understanding NO3RR is also critical for emerging reactions such as electrochemical urea synthesis, because nitrate‑derived adsorbates and their binding geometries determine opportunities for C–N bond formation.[2] Silver is an ideal model platform to benchmark nitrogenous adsorbates because it stabilizes key nitrogenous intermediates while providing strong plasmonic enhancement for in-situ surface‑enhanced Raman spectroscopy (SERS).[3]
In-situ time‑resolved SERS (TR-SERS) was used to follow adsorbate dynamics on roughened Ag during potential sweeps, with spectra synchronized to cyclic voltammetry to directly link spectroscopic events to electrochemical features. TR‑SERS results reveal potential‑dependent Raman bands assigned to interfacial species: Ag–O stretch, aqueous NO3– symmetric stretch, NO3– antisymmetric stretch ν3, adsorbed NO2–, and two nitrate adsorption bands attributed to bidentate and bridge coordination, respectively.[4]. Our observations establish a direct, time‑resolved correlation between applied potential, adsorption geometry, and the spectroscopic precursor state for nitrite formation on Ag, demonstrating TR‑SERS as a powerful operando approach for probing dynamic adsorbate behaviour relevant to NO3RR and C–N coupling chemistry.
Financial support from EU project ICONIC (No. 101115204) is gratefully acknowledged.
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