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Herein, we construct a p\u2013n junction photocathode composed of an atomic\u2010layer\u2010deposited ZnO\n                    <jats:sub>x<\/jats:sub>\n                    layer and black silicon (b\u2010Si) to regulate interfacial electron dynamics and reaction selectivity. Upon illumination, oxygen vacancies in the ZnO\n                    <jats:sub>x<\/jats:sub>\n                    surface serve as electron\u2010buffering sites that facilitate reversible charge storage and release, as confirmed by in situ Kelvin probe force microscopy. This modulation of electron chemical potential suppresses competing hydrogen evolution and over\u2010reduction pathways, while directing nitrogen\u2010centered intermediates toward selective hydroxylamine formation and subsequent C\u2500N coupling. The optimized photocathode delivers a photocurrent density of 38.6\u00a0mA cm\n                    <jats:sup>\u22122<\/jats:sup>\n                    with a Faradaic efficiency of 94.6% for cyclohexanone oxime production and a cyclohexanone\u2010to\u2010oxime selectivity of 99.9%. Mechanistic studies combining\n                    <jats:italic>operando<\/jats:italic>\n                    spectroscopy, density functional theory, and microkinetic analysis reveal that coverage\u2010dependent site competition governs surface site availability, thereby inhibiting the further reduction of hydroxylamine and promoting its desorption for solution\u2010phase coupling. Integration of the microkinetic model with the photovoltaic response establishes a quantitative design principle based on the matching between semiconductor photoresponse and interfacial catalytic kinetics, providing a general framework for selectivity control in photoelectrochemical systems.\n                  <\/jats:p>","DOI":"10.1002\/anie.8769472","type":"journal-article","created":{"date-parts":[[2026,9,25]],"date-time":"2026-09-25T06:27:29Z","timestamp":1790317649000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Regulating Surface Electron Dynamics Enables Selective C\u2500N Coupling in Photoelectrochemical Oxime Synthesis"],"prefix":"10.1002","author":[{"ORCID":"https:\/\/orcid.org\/0000-0003-3271-1758","authenticated-orcid":false,"given":"Zilong","family":"Li","sequence":"first","affiliation":[{"name":"School of Chemistry and Materials Science Hefei National Research Center for Physical Sciences at the 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