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Electrogenerated reactive oxygen species (ROS) offer a promising route for pollutant degradation, yet the role of electrolyte cations in controlling ROS pathways remains poorly understood. Although singlet oxygen (\n                    <jats:sup>1<\/jats:sup>\n                    O\n                    <jats:sub>2<\/jats:sub>\n                    ) is more persistent and matrix\u2010tolerant than hydroxyl radicals (\u2022OH), whether cation\u2010induced changes in interfacial water structure govern ROS selectivity remains unclear. Here, using atomically dispersed Cu on Fe\n                    <jats:sub>2<\/jats:sub>\n                    O\n                    <jats:sub>3<\/jats:sub>\n                    \u2010carbon nanotubes (Cu\n                    <jats:sub>1<\/jats:sub>\n                    \/Fe\n                    <jats:sub>2<\/jats:sub>\n                    O\n                    <jats:sub>3<\/jats:sub>\n                    \u2010CNTs) as a dual\u2010ROS electrocatalyst, we show that alkali\u2010metal cations exert distinct effects on ROS generation. \u2022OH production follows the expected cation\u2010size\u2010dependent trend, whereas\n                    <jats:sup>1<\/jats:sup>\n                    O\n                    <jats:sub>2<\/jats:sub>\n                    generation exhibits an anomalous maximum in Na\n                    <jats:sup>+<\/jats:sup>\n                    \u2010containing electrolytes, leading to superior contaminant degradation. Quantitative ROS measurements, in situ electrochemical analysis, spectroscopy, and theoretical calculations show that this behavior is primarily governed by selective stabilization of the *OOH intermediate rather than enhanced O\n                    <jats:sub>2<\/jats:sub>\n                    adsorption. Na\n                    <jats:sup>+<\/jats:sup>\n                    promotes a highly interconnected interfacial hydrogen\u2010bond network that stabilizes *OOH and favors\n                    <jats:sup>1<\/jats:sup>\n                    O\n                    <jats:sub>2<\/jats:sub>\n                    formation. In natural seawater, this regulation enables &gt;98.2% contaminant removal within 8 h at an estimated energy demand of 0.779 kWh m\n                    <jats:sup>\u22123<\/jats:sup>\n                    . These findings identify electrolyte cations as important regulators of ROS selectivity and provide a basis for efficient saline\u2010water decontamination.\n                  <\/jats:p>","DOI":"10.1002\/anie.9670818","type":"journal-article","created":{"date-parts":[[2026,10,14]],"date-time":"2026-10-14T08:54:41Z","timestamp":1791968081000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Cation\u2010Mediated Interface Engineering Directs Electrogenerated Reactive Oxygen Species Pathways"],"prefix":"10.1002","author":[{"ORCID":"https:\/\/orcid.org\/0009-0007-3287-764X","authenticated-orcid":false,"given":"Xuelin","family":"Sheng","sequence":"first","affiliation":[{"name":"College of Chemistry Sichuan University  Chengdu China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Pengfei","family":"Wang","sequence":"additional","affiliation":[{"name":"Institute of Fundamental and Frontier Sciences University of Electronic Science and Technology of China  Chengdu China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Hongmei","family":"Li","sequence":"additional","affiliation":[{"name":"College of Chemistry Sichuan University  Chengdu China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Siyi","family":"Lin","sequence":"additional","affiliation":[{"name":"College of Materials Science and Engineering Sichuan University  Chengdu China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-4060-5912","authenticated-orcid":false,"given":"Baozhan","family":"Zheng","sequence":"additional","affiliation":[{"name":"College of Chemistry Sichuan University  Chengdu China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-0840-3931","authenticated-orcid":false,"given":"Zhaoyu","family":"Jin","sequence":"additional","affiliation":[{"name":"Institute of Fundamental and Frontier Sciences University of Electronic Science and Technology of China  Chengdu China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-3253-0749","authenticated-orcid":false,"given":"Guihua","family":"Yu","sequence":"additional","affiliation":[{"name":"Materials Science and Engineering Program and Walker Department of Mechanical Engineering The University of Texas at Austin  Austin Texas United States"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-9933-0357","authenticated-orcid":false,"given":"Panpan","family":"Li","sequence":"additional","affiliation":[{"name":"College of Materials Science and Engineering Sichuan University  Chengdu 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