Inter-Atomic Synergy on Single-Atom Alloy Promotes Cyclohexanone Oxime Electrosynthesis.

Zhai, Panlong; Wang, Chen; Sheng, Guan; Ye, Chao; Hou, Jungang; Gu, Qinfen; Ling, Tao; Zhu, Ye et al. · Adv Mater · 2026

basic_science · Level V

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Abstract

The electrosynthesis of cyclohexanone oxime from cyclohexanone and nitrogenous feedstock driven by renewable electricity presents a sustainable alternative to energy-intensive and hazardous industrial processes. However, achieving high activity and selectivity is challenged by the over-reduction of key intermediates and the lack of effective sites for C─N coupling. Herein, we report a Fe<sub>1</sub>Bi single-atom alloy (Fe<sub>1</sub>Bi SAA) featuring Fe-Bi atomic interfaces that collaborate for the one-pot electrosynthesis of cyclohexanone oxime. The Fe<sub>1</sub>Bi SAA achieves a remarkable Faradaic efficiency of 70.9% and a yield rate of 0.94 mmol cm<sup>-2</sup> h<sup>-1</sup> for cyclohexanone oxime. Combined in situ electrochemical spectroscopic measurements and density functional theory calculations reveal an atomic-scale synergistic mechanism: dispersed Fe sites adsorb and activate cyclohexanone, while adjacent Bi sites selectively reduce nitrite to the key hydroxylamine intermediate. The techno-economic analysis based on flow electrolyzer operation confirms the potential economic viability of the electrosynthesis of cyclohexanone oxime. This work provides profound atomic-level insight into cooperative catalysis for C─N coupling reactions toward the electrosynthesis of value-added organonitrogen compounds.