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However, their industrial\u2010scale application in membrane electrode assemblies (MEAs) is limited by inadequate Faraday efficiency (FE) and long\u2010term stability. Herein, we propose a rational mesoporous engineering approach for Ni\u2010NC catalysts via a two\u2010step space\u2010confinement pyrolysis strategy. Through cryo CO\u2010pulse chemisorption, real\u2010time observations of CO\n                    <jats:sub>2<\/jats:sub>\n                    gas bubble diffusion, and finite element simulations, we demonstrate that the mesoporous structured Ni\u2010NC (meso\u2010Ni\u2010NC) exhibits significantly enhanced active site accessibility and mass transport capabilities compared to microporous structured Ni\u2010NC (micro\u2010Ni\u2010NC). More importantly, the mesoporous engineering enhances the internal gas\u2010holding capacity of the catalytic layer, effectively mitigating flooding and salt deposition and thus enhancing the catalyst's long\u2010term stability. Consequently, meso\u2010Ni\u2010NC achieves an industrially relevant CO partial current density of 291.8\u00a0mA cm\n                    <jats:sup>\u22122<\/jats:sup>\n                    at 97.3% CO Faradaic efficiency (FE\n                    <jats:sub>CO<\/jats:sub>\n                    ), along with stable operation for 136 h at 100\u00a0mA cm\n                    <jats:sup>\u22122<\/jats:sup>\n                    while maintaining FE\n                    <jats:sub>CO<\/jats:sub>\n                    exceeding 90% in an MEA, outperforming those of micro\u2010Ni\u2010NC and representing an advancement over existing state\u2010of\u2010the\u2010art Ni\u2010based single\u2010atom catalysts. This work highlights the critical role of pore structure in determining the performance of industry\u2010level electrocatalytic CO\n                    <jats:sub>2<\/jats:sub>\n                    reduction.\n                  <\/jats:p>","DOI":"10.1002\/anie.202523859","type":"journal-article","created":{"date-parts":[[2026,1,12]],"date-time":"2026-01-12T14:40:26Z","timestamp":1768228826000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":29,"title":["Mesoporous Engineering of Single\u2010Atom Catalyst for Industry\u2010Level Electrocatalytic CO\n                    <sub>2<\/sub>\n                    Reduction in Membrane Electrode Assemblies"],"prefix":"10.1002","volume":"65","author":[{"given":"Zhanshuai","family":"Ma","sequence":"first","affiliation":[{"name":"State Key Laboratory of Chemical Resource Engineering Beijing University of Chemical Technology  Beijing 100029 China"},{"name":"Shanghai Synchrotron Radiation 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China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Xingjiang","family":"Liu","sequence":"additional","affiliation":[{"name":"College of Chemistry Zhengzhou University  Zhengzhou 450001 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Chengjin","family":"Chen","sequence":"additional","affiliation":[{"name":"Shanghai Synchrotron Radiation Facility Zhangjiang Laboratory Shanghai Advanced Research Institute Chinese Academy of Sciences  Shanghai 201204 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Songqi","family":"Gu","sequence":"additional","affiliation":[{"name":"Shanghai Synchrotron Radiation Facility Zhangjiang Laboratory Shanghai Advanced Research Institute Chinese Academy of Sciences  Shanghai 201204 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Yuying","family":"Huang","sequence":"additional","affiliation":[{"name":"Shanghai Synchrotron Radiation Facility Zhangjiang Laboratory Shanghai Advanced Research Institute Chinese Academy of Sciences  Shanghai 201204 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Chunhui","family":"Li","sequence":"additional","affiliation":[{"name":"College of Chemistry Zhengzhou University  Zhengzhou 450001 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Yu","family":"Wang","sequence":"additional","affiliation":[{"name":"Shanghai Synchrotron Radiation Facility Zhangjiang Laboratory Shanghai Advanced Research Institute Chinese Academy of Sciences  Shanghai 201204 China"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-7455-6314","authenticated-orcid":false,"given":"Junfeng","family":"Liu","sequence":"additional","affiliation":[{"name":"State Key Laboratory of Chemical Resource Engineering Beijing University of Chemical Technology  Beijing 100029 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