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Here, we demonstrate that engineering the local chemical microenvironment is as critical as tuning intrinsic catalytic activity. Inspired by the functional orchestration of cyanobacterial carboxysomes, we report a biomimetic interface that integrates carbonic anhydrase within copper phosphate nanoflowers to establish a reaction\u2013diffusion nanoreactor. Hyperspectral micro-FTIR imaging reveals a spatially localized and quantitatively enhanced CO2-associated signal at the biohybrid interface, consistent with the formation of an interfacial CO2 reservoir sustained by enzymatic bicarbonate dehydration. This interfacial CO2 enrichment directly translates into enhanced carbon utilization, manifested by higher conversion rates and improved selectivity toward carbon-derived reduction products relative to the enzyme-free control. Real-time online electrochemical mass spectrometry confirms a shift in selectivity toward carbon-derived products under conditions where conventional electrodes are transport-limited. This work establishes that shifting the focus from material-bound kinetics to interface-driven carbon management is also a strategy for advancing electrosynthesis.<\/jats:p>","DOI":"10.1021\/jacs.6c12039","type":"journal-article","created":{"date-parts":[[2026,9,3]],"date-time":"2026-09-03T02:53:49Z","timestamp":1788404029000},"page":"39054-39066","source":"Crossref","is-referenced-by-count":0,"title":["Decoupling CO2 Availability from Bulk Solubility\nvia Biohybrid Reaction\u2013Diffusion Nanoconfinement"],"prefix":"10.1021","volume":"148","author":[{"ORCID":"https:\/\/orcid.org\/0000-0001-8897-187X","authenticated-orcid":true,"given":"Fhysme\u0301lia F.","family":"Albuquerque","sequence":"first","affiliation":[{"name":"University of Sa\u0303o Paulo (USP) , , ,","place":["Sa\u0303o Carlos, Brazil, 13560-970"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Artur C.","family":"Souza","sequence":"additional","affiliation":[{"name":"University of Sa\u0303o Paulo (USP) , , ,","place":["Sa\u0303o Carlos, Brazil, 13560-970"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0009-0004-2391-2982","authenticated-orcid":true,"given":"Matheus","family":"S Corsino","sequence":"additional","affiliation":[{"name":"University of Sa\u0303o Paulo (USP) , , ,","place":["Sa\u0303o Carlos, Brazil, 13560-970"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Lucas D.","family":"Paquini","sequence":"additional","affiliation":[{"name":"University of Sa\u0303o Paulo (USP) , , ,","place":["Sa\u0303o Carlos, Brazil, 13560-970"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-8696-5978","authenticated-orcid":true,"given":"Graziela C.","family":"Sedenho","sequence":"additional","affiliation":[{"name":"University of Sa\u0303o Paulo (USP) , , ,","place":["Sa\u0303o Carlos, Brazil, 13560-970"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0001-8126-4398","authenticated-orcid":true,"given":"Rafael N. 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