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Here, we report the synthesis of bimetallic Cu\u2013Au metallic aerogels (MAs) via the freeze\u2013thaw method as efficient electrocatalysts for the electrochemical CO\n                    <jats:sub>2<\/jats:sub>\n                    reduction reaction (CO\n                    <jats:sub>2<\/jats:sub>\n                    RR). Electrochemical measurements reveal that Cu\u2013Au MAs exhibit remarkably high Faradaic efficiency for CO (FE\n                    <jats:sub>CO<\/jats:sub>\n                    ) over a broad potential window (\u22120.7 to \u22121.1\u2009V versus reversible hydrogen electrode (RHE)), with a peak FE\n                    <jats:sub>CO<\/jats:sub>\n                    of 86.4% at \u22120.8\u2009V\n                    <jats:sub>RHE<\/jats:sub>\n                    , outperforming monometallic Au MAs (81.5%) and Cu MAs (9.2%). Moreover, Cu\u2013Au MAs demonstrate excellent long\u2010term stability, showing negligible activity decay after 20\u2009h of continuous testing at \u22120.8\u2009V\n                    <jats:sub>RHE<\/jats:sub>\n                    . Mechanistic investigations indicate that the incorporation of Au sites in Cu\u2013Au MAs optimizes the electronic structure of Cu, accelerates electron transfer, and modulates the adsorption strength of CO\n                    <jats:sub>2<\/jats:sub>\n                    on the catalyst surface, thereby enhancing CO\n                    <jats:sub>2<\/jats:sub>\n                    RR performance. This study not only highlights the superior electrocatalytic performance of the bimetallic strategy for CO\n                    <jats:sub>2<\/jats:sub>\n                    conversion but also provides insights into the synergistic effect of bimetallic sites, paving the way for industrial\u2010scale CO\n                    <jats:sub>2<\/jats:sub>\n                    recycling and utilization.\n                  <\/jats:p>","DOI":"10.1002\/cphc.70474","type":"journal-article","created":{"date-parts":[[2026,6,30]],"date-time":"2026-06-30T01:16:06Z","timestamp":1782782166000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Synergistic Effect of Bimetallic Sites in Cu\u2013Au Metallic Aerogels for Carbon Dioxide Electroreduction"],"prefix":"10.1002","volume":"27","author":[{"given":"Minggang","family":"Ma","sequence":"first","affiliation":[{"name":"Key Laboratory of Synthetic and Biological Colloids Ministry of Education School of Chemical and Material Engineering Jiangnan University  Wuxi China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Liheng","family":"Guan","sequence":"additional","affiliation":[{"name":"Key Laboratory of Synthetic and Biological Colloids Ministry of Education School of Chemical and Material Engineering Jiangnan University  Wuxi China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Cun","family":"Chen","sequence":"additional","affiliation":[{"name":"Key Laboratory of Synthetic and Biological Colloids Ministry of Education School of Chemical and Material Engineering Jiangnan University  Wuxi China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Hanjun","family":"Li","sequence":"additional","affiliation":[{"name":"Key Laboratory of Synthetic and Biological Colloids Ministry of Education School of Chemical and Material Engineering Jiangnan University  Wuxi 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