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However, these harsh conditions pose significant challenges, including intensified hydrogen evolution reaction (HER). Herein, guided by density functional theory (DFT) calculations, the Ni\u2010N\n                    <jats:sub>4<\/jats:sub>\n                    \u2010O\/Ni clusters are identified as active sites that can simultaneously promote *COOH formation and suppress HER. Based on this insight, a molecular\u2010crosslinking strategy is developed to construct a Ni\n                    <jats:sub>X<\/jats:sub>\n                    @NiN\n                    <jats:sub>4<\/jats:sub>\n                    \u2010O catalyst with high\u2010density Ni\u2010N\n                    <jats:sub>4<\/jats:sub>\n                    \u2010O\/Ni clusters. The resulting catalyst achieves a high CO Faradaic efficiency (FE\n                    <jats:sub>CO<\/jats:sub>\n                    ) of 93.6% at an industrial\u2010level current density of 1 A cm\n                    <jats:sup>\u22122<\/jats:sup>\n                    in strongly acidic media (0.25\u00a0\n                    <jats:sc>m<\/jats:sc>\n                    K\n                    <jats:sub>2<\/jats:sub>\n                    SO\n                    <jats:sub>4<\/jats:sub>\n                    , pH = 1). Even in dilute sulfuric acid (pH = 2) without K\n                    <jats:sup>+<\/jats:sup>\n                    , it retains a FE\n                    <jats:sub>CO<\/jats:sub>\n                    of 70.9%. Notably, the catalyst also exhibits remarkable performance in a pure\u2010water\u2010fed membrane electrode assembly (MEA) system using both cation and anion exchange membranes (CEM and AEM), with FE\n                    <jats:sub>CO<\/jats:sub>\n                    values of 92.7% and 94.8%, respectively.\n                  <\/jats:p>","DOI":"10.1002\/smll.202511758","type":"journal-article","created":{"date-parts":[[2025,11,29]],"date-time":"2025-11-29T18:56:08Z","timestamp":1764442568000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":2,"title":["Molecularly Crosslinked Dense Ni\u2010N\n                    <sub>4<\/sub>\n                    \u2010O\/Ni Clusters for Scalable CO\n                    <sub>2<\/sub>\n                    Electroreduction in Acidic and Alkali\u2010Metal\u2010Free Media"],"prefix":"10.1002","volume":"22","author":[{"given":"Jiaji","family":"Zhang","sequence":"first","affiliation":[{"name":"Key Laboratory of Biomass Chemical Engineering of Ministry of Education College of Chemical and Biological Engineering Zhejiang University  Hangzhou 310058 China"},{"name":"Zhejiang Key Laboratory of Green Biomanufacturing of Functional Sugar Alcohols Institute of Zhejiang University\u2010Quzhou  99 Zheda Road Quzhou 324000 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Gaobo","family":"Lin","sequence":"additional","affiliation":[{"name":"Key Laboratory of Biomass Chemical Engineering of Ministry of Education College of Chemical and Biological Engineering Zhejiang University  Hangzhou 310058 China"},{"name":"Zhejiang Key Laboratory of Green Biomanufacturing of Functional Sugar Alcohols Institute of Zhejiang University\u2010Quzhou  99 Zheda Road Quzhou 324000 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Can","family":"Yu","sequence":"additional","affiliation":[{"name":"National Synchrotron Radiation Laboratory University of Science and Technology of China  Hefei Anhui 230026 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Weitao","family":"Ji","sequence":"additional","affiliation":[{"name":"Key Laboratory of Biomass Chemical Engineering of Ministry of Education College of Chemical and Biological Engineering Zhejiang University  Hangzhou 310058 China"},{"name":"Zhejiang Key Laboratory of Green Biomanufacturing of Functional Sugar Alcohols Institute of Zhejiang University\u2010Quzhou  99 Zheda Road Quzhou 324000 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Jie","family":"Zhu","sequence":"additional","affiliation":[{"name":"Key Laboratory of Biomass Chemical Engineering of Ministry of Education College of Chemical and Biological Engineering Zhejiang University  Hangzhou 310058 China"},{"name":"Zhejiang Key Laboratory of Green Biomanufacturing of Functional Sugar Alcohols Institute of Zhejiang University\u2010Quzhou  99 Zheda Road Quzhou 324000 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