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Conventional filler-functionalized polyimide (PI) composites can provide strong electromagnetic attenuation, but their limited foamability under supercritical carbon dioxide (scCO2) restricts porous structure formation and thus impairs impedance matching. To address these limitations, this study proposes an intrinsic molecular modification strategy based on a chain segment design. Furthermore, by combining synergistic dielectric-magnetic loss from nanofillers with a double-layer heterogeneous architecture, a PI-based electromagnetic shielding nanocomposite with strong microwave absorption performance and low-reflection characteristics was constructed. Bisphenol A dianhydride (BPADA) was used as the dianhydride monomer, and a series of PI copolymers with tunable chain segment compositions were prepared through the reaction of BPADA with mixed aromatic diisocyanate (MDI) and aliphatic diisocyanate (HDI), followed by thermal imidization\/cyclization. The changes in molecular chain mobility, scCO2 foaming behavior, and cellular structure associated with the nominal HDI feed fraction were systematically investigated. The results showed that increasing the nominal HDI feed fraction was associated with an improved rigid-flexible balance of the PI backbone, enhanced segmental mobility, a broader foaming window, and the formation of PI foams with uniform and compact cellular structures. CNT@Fe3O4 nanofillers with both dielectric and magnetic loss capabilities were further introduced to improve the intrinsic electromagnetic loss of the composite foams. The calculated microwave absorption results showed that, after pore structure regulation, the PI\/CNT@Fe3O4 nanocomposite foam exhibited markedly enhanced microwave absorption in the X-band. At a porosity of 46 vol %, the minimum reflection loss reached \u221238 dB at a thickness of 2 mm. A double-layer heterogeneous structure comprising a CNT@Fe3O4-containing porous absorbing layer and a CNT-containing dense reflecting layer was then constructed to exploit impedance gradient transition, dielectric-magnetic synergistic loss, and multiple reflection\/reabsorption processes. The optimized sample showed an average absorption coefficient of 0.92 in the X-band and a maximum A\/R ratio of 332, indicating pronounced high absorption and low reflection characteristics. This study provides a new strategy for designing and fabricating lightweight, high-performance PI-based electromagnetic protection materials with an absorption-dominated shielding behavior.<\/jats:p>","DOI":"10.1021\/acsomega.6c06706","type":"journal-article","created":{"date-parts":[[2026,9,21]],"date-time":"2026-09-21T07:01:55Z","timestamp":1789974115000},"page":"59784-59795","source":"Crossref","is-referenced-by-count":0,"title":["Supercritical CO2 Foaming of Molecular\nChain-Modified Polyimide for High-Performance Electromagnetic Wave\nAbsorption"],"prefix":"10.1021","volume":"11","author":[{"given":"Jiaozhu","family":"Wu","sequence":"first","affiliation":[{"name":"Sichuan University , , ,","place":["Chengdu, PR China, 610065"]},{"name":"Jiangsu JITRI Advanced Polymer Materials Research Institute , ,","place":["Nanjing, PR China, 211800"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Jiaxi","family":"Zhang","sequence":"additional","affiliation":[{"name":"Sichuan University , , ,","place":["Chengdu, PR China, 610065"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Xutao","family":"Zhang","sequence":"additional","affiliation":[{"name":"Sichuan University , , ,","place":["Chengdu, PR China, 610065"]},{"name":"Zigong Zhongtiansheng New Material Technology Co., Ltd. , ,","place":["Zigong, PR China, 643030"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Haoyu","family":"Ma","sequence":"additional","affiliation":[{"name":"Sichuan University , , ,","place":["Chengdu, PR China, 610065"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Jie","family":"He","sequence":"additional","affiliation":[{"name":"Sichuan University , , ,","place":["Chengdu, PR China, 610065"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-9479-4141","authenticated-orcid":true,"given":"Qiang","family":"Liu","sequence":"additional","affiliation":[{"name":"China Academy of Engineering Physics , , ,","place":["Mianyang, PR China, 621900"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Guangxian","family":"Li","sequence":"additional","affiliation":[{"name":"Sichuan University , , ,","place":["Chengdu, PR China, 610065"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0009-0005-9209-5581","authenticated-orcid":true,"given":"Pengjian","family":"Gong","sequence":"additional","affiliation":[{"name":"Sichuan University , , ,","place":["Chengdu, PR China, 610065"]}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"316","published-online":{"date-parts":[[2026,9,21]]},"reference":[{"key":"2026100610502706500_cit1","doi-asserted-by":"publisher","first-page":"152257","DOI":"10.1016\/j.cej.2024.152257","article-title":"Multi-scale\ncollaboration of polyimide-based composite foams for multi-spectrum\ncompatible stealth in acoustic, microwave and infrared bands","volume":"492","author":"Zhang","year":"2024","journal-title":"Chem. 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Mater."},{"issue":"20","key":"2026100610502706500_cit6","doi-asserted-by":"publisher","DOI":"10.1002\/smll.202514802","article-title":"Multiscale structural\nengineering in electromagnetic wave absorption materials: From atomic\ndefects to macroscopic structures","volume":"22","author":"Ning","year":"2026","journal-title":"Small"},{"key":"2026100610502706500_cit7","doi-asserted-by":"publisher","first-page":"2091","DOI":"10.1039\/D5TC02882E","article-title":"Materials\nengineering in microwave absorbers: recent advances and prognosis","volume":"14","author":"Shehbaz","year":"2026","journal-title":"J. Mater. Chem. 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Hybrid Mater."},{"issue":"3","key":"2026100610502706500_cit21","doi-asserted-by":"publisher","DOI":"10.1002\/inf2.70087","article-title":"A strategy\nfor modulation of permittivity in manganese doping to induce lattice\ndistortion","volume":"8","author":"Xu","year":"2026","journal-title":"InfoMat"},{"issue":"28","key":"2026100610502706500_cit22","doi-asserted-by":"publisher","first-page":"22613","DOI":"10.1039\/D5TA02068A","article-title":"Hierarchically\nporous polyimide\/graphene aerogels with superior compressibility and\nelectromagnetic interference shielding performance","volume":"13","author":"Zhao","year":"2025","journal-title":"J. Mater. Chem. 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