Longcheng Zhang, Yuan Liu, Ling Li, Xiaoning Li, Pengfei Song, Ting Chen, Qian Wu, Justin Zhu Yeow Seow, Kai Tang, Shirong Sun, Xia Guo, Zhichuan Xu
Manipulating the selectivity-determining step in the hydrogenation of nitrogen-containing intermediates is critical to achieving high ammonia selectivity in electrocatalytic nitrate reduction. Here, we propose a molecular interface engineering strategy that functionalized with thiol-anchored aromatic ligands to regulate the interfacial binding affinity and activation of key nitrogen-containing intermediates on silver nanocube surfaces. By systematically varying the electronic properties of the substituents, we identify 4-(methylthio)benzaldehyde as the most effective ligand, increasing the ammonia Faradaic efficiency from 50.8% to 98.9% and achieving a yield rate of 14,366.1 μg h–1 cmgeo–2 at –0.63 V versus reversible hydrogen electrode. In situ electrochemical characterizations combined with theoretical simulations further reveal that 4-(methylthio)benzaldehyde modification promotes the activation of weakly hydrogen-bonded water molecules and accelerates the hydrogenation of *HNO intermediates. This targeted modulation of interfacial binding affinity offers an effective strategy for selectivity control in electrocatalytic nitrate reduction. The enhanced performance is further validated in a membrane electrode assembly electrolyser, underscoring the practical viability of this molecular design strategy for selective nitrate conversion. Controlling reaction selectivity in complex multistep electrochemical transformations remains a major challenge. Here, the authors report that molecular interface engineering on silver electrodes enables precise regulation of key reaction intermediates for efficient ammonia electrosynthesis.