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In this study, hypercrosslinked polystyrene nanoparticles prepared using formaldehyde dimethyl acetal, denoted as PS-FDA, were introduced as porous structure-regulating fillers to tune the microstructural evolution of polyimide-derived CMS membranes. By adjusting the filler loading and pyrolysis temperature, the resulting HCMS membranes achieved excellent gas separation performance. The optimized 5-PS-FDA\/PI-600 HCMS membrane exhibited the best overall performance, giving CO2 and H2 permeabilities of 16,050.92 and 18,810.15 Barrer, corresponding to approximately 152% and 139% increases over the pristine PI-600 HCMS membrane, respectively. At the same time, this membrane retained CO2\/N2, CO2\/CH4, H2\/N2, and H2\/CH4 selectivities of 28.15, 37.40, 32.99, and 43.85, respectively, surpassing the 2019 and 2015 Robeson upper bounds. Diffusivity\/solubility analysis further indicated that the permeability enhancement was mainly associated with improved diffusional transport rather than increased gas sorption. Pressure-dependent permeation measurements and a 7-day physical aging test further showed that the optimized HCMS membrane preserved its molecular-sieving characteristics under the tested conditions. These results demonstrate that hypercrosslinked porous nanofillers can effectively regulate the pore-structure evolution of PI-derived HCMS membranes and offer a feasible approach for developing stable, highly permeable carbon membranes.<\/jats:p>","DOI":"10.1021\/acsami.6c10540","type":"journal-article","created":{"date-parts":[[2026,8,4]],"date-time":"2026-08-04T13:13:29Z","timestamp":1785849209000},"page":"42664-42675","source":"Crossref","is-referenced-by-count":0,"title":["Pore-Structure Regulation of Hybrid Carbon Molecular Sieve Membranes by Hypercrosslinked Porous Nanofillers for High-Performance CO2 and H2 Separation"],"prefix":"10.1021","volume":"18","author":[{"given":"Jiaxue","family":"Li","sequence":"first","affiliation":[{"name":"Sichuan University , , ,","place":["Chengdu, China, 610065"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Xinyu","family":"Wang","sequence":"additional","affiliation":[{"name":"Sichuan University , , ,","place":["Chengdu, China, 610065"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Min","family":"Deng","sequence":"additional","affiliation":[{"name":"Sichuan University , , ,","place":["Chengdu, China, 610065"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Jia","family":"Song","sequence":"additional","affiliation":[{"name":"Sichuan University , , ,","place":["Chengdu, China, 610065"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-8515-6770","authenticated-orcid":true,"given":"Junfeng","family":"Zheng","sequence":"additional","affiliation":[{"name":"Sichuan University , , ,","place":["Chengdu, China, 610065"]},{"name":"National Engineering Research Centre for Flue Gas Desulfurization , ,","place":["Chengdu, China, 610065"]},{"name":"Carbon Neutral Technology Innovation Center of Sichuan , ,","place":["Chengdu, China, 610065"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-2743-758X","authenticated-orcid":true,"given":"Lu","family":"Yao","sequence":"additional","affiliation":[{"name":"Sichuan University , , ,","place":["Chengdu, China, 610065"]},{"name":"National Engineering Research Centre for Flue Gas Desulfurization , ,","place":["Chengdu, China, 610065"]},{"name":"Carbon Neutral Technology Innovation Center of Sichuan , ,","place":["Chengdu, China, 610065"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-3367-244X","authenticated-orcid":true,"given":"Lin","family":"Yang","sequence":"additional","affiliation":[{"name":"Sichuan University , , ,","place":["Chengdu, China, 610065"]},{"name":"National Engineering Research Centre for Flue Gas Desulfurization , ,","place":["Chengdu, China, 610065"]},{"name":"Carbon Neutral Technology Innovation Center of Sichuan , ,","place":["Chengdu, China, 610065"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-1327-7159","authenticated-orcid":true,"given":"Wenju","family":"Jiang","sequence":"additional","affiliation":[{"name":"Sichuan University , , ,","place":["Chengdu, China, 610065"]},{"name":"National Engineering Research Centre for Flue Gas Desulfurization , ,","place":["Chengdu, China, 610065"]},{"name":"Carbon Neutral Technology Innovation Center of Sichuan , ,","place":["Chengdu, China, 610065"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-3558-5403","authenticated-orcid":true,"given":"Zhongde","family":"Dai","sequence":"additional","affiliation":[{"name":"Sichuan University , , ,","place":["Chengdu, China, 610065"]},{"name":"National Engineering Research Centre for Flue Gas Desulfurization , ,","place":["Chengdu, China, 610065"]},{"name":"Carbon Neutral Technology Innovation Center of Sichuan , ,","place":["Chengdu, China, 610065"]}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"316","published-online":{"date-parts":[[2026,7,28]]},"reference":[{"issue":"26","key":"2026081200072487000_cit1","doi-asserted-by":"publisher","first-page":"32906","DOI":"10.1021\/acsami.4c06914","article-title":"Metal-Organic-Frameworks Based Mixed-Matrix Membranes for CO2 Separation: An Applicable-Conceptual Approach","volume":"16","author":"Mohsenpour Tehrani","year":"2024","journal-title":"ACS Appl. 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