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Herein, a high\u2010density Ga\u2500Y dual\u2010atom catalyst is developed with loading up to 14.1 wt.% of Ga and Y supported on N, P\u2010co\u2010doped carbon substrate (Ga\/Y\u2010CNP) for urea electrosynthesis. The catalyst facilitates efficient C\u2500N coupling through co\u2010reduction of CO\n                    <jats:sub>2<\/jats:sub>\n                    and NO\n                    <jats:sub>3<\/jats:sub>\n                    <jats:sup>\u2212<\/jats:sup>\n                    , resulting in a high urea yield rate of 41.9 mmol h\n                    <jats:sup>\u22121<\/jats:sup>\n                    g\n                    <jats:sup>\u22121<\/jats:sup>\n                    and a Faradaic efficiency of 22.1% at \u22121.4 V versus the reversible hydrogen electrode. In situ spectroscopy and theoretical calculations\u00a0reveal that the superior performance is attributed to the cross\u2010tuning between adjacent pair Ga\u2500Y sites, which can mutually optimize their electronic states for facilitating CO\n                    <jats:sub>2<\/jats:sub>\n                    reduction to *CO at Ga sites and promoting NO\n                    <jats:sub>3<\/jats:sub>\n                    <jats:sup>\u2212<\/jats:sup>\n                    conversion to hydroxylamine (*NH\n                    <jats:sub>2<\/jats:sub>\n                    OH) at Y sites, followed by spontaneous coupling of *CO and *NH\n                    <jats:sub>2<\/jats:sub>\n                    OH intermediates at Ga\u2500Y sites to form C\u2500N bonds. This work offers a pioneering strategy to manipulate C\u2500N coupling pathways by cross\u2010tuning active sites to produce high\u2010value\u2010added chemicals.\n                  <\/jats:p>","DOI":"10.1002\/adma.202420593","type":"journal-article","created":{"date-parts":[[2025,3,11]],"date-time":"2025-03-11T18:46:16Z","timestamp":1741718776000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":53,"title":["Electrosynthesis of Urea on High\u2010Density Ga\u2500Y Dual\u2010Atom Catalyst via Cross\u2010Tuning"],"prefix":"10.1002","volume":"37","author":[{"given":"Dechao","family":"Chen","sequence":"first","affiliation":[{"name":"State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter Chinese Academy of Sciences  Fuzhou 350002 China"},{"name":"Fujian Science &amp; Technology Innovation Laboratory for Optoelectronic Information of China  Fuzhou Fujian 350108 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Yimeng","family":"Cai","sequence":"additional","affiliation":[{"name":"State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter Chinese Academy of Sciences  Fuzhou 350002 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Yi","family":"Xiao","sequence":"additional","affiliation":[{"name":"State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter Chinese Academy of Sciences  Fuzhou 350002 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Chengqiang","family":"Wang","sequence":"additional","affiliation":[{"name":"State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter Chinese Academy of Sciences  Fuzhou 350002 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Physics Tamkang University  New Taipei City 251301 Taiwan"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Chi\u2010Feng","family":"Lee","sequence":"additional","affiliation":[{"name":"Department of Physics Tamkang University  New Taipei City 251301 Taiwan"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Linjie","family":"Zhang","sequence":"additional","affiliation":[{"name":"State Key Laboratory of Structural Chemistry Fujian Institute of Research on the Structure of Matter Chinese Academy of Sciences  Fuzhou 350002 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Hirofumi","family":"Ishii","sequence":"additional","affiliation":[{"name":"National Synchrotron Radiation Research Center  Hsinchu 30076 Taiwan"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Yu\u2010Cheng","family":"Shao","sequence":"additional","affiliation":[{"name":"National Synchrotron Radiation Research Center  Hsinchu 30076 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