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While artificial solid\u2010electrolyte interphases offer a protective strategy, most designs are limited to single\u2010ion regulation and fail to orchestrate the complex, dual\u2010ion (Li\n                    <jats:sup>+<\/jats:sup>\n                    and anion) chemistry at the molecular level. Here, we report a rationally designed polymeric artificial interphase of poly\u2010fluorotoluene\u2010triglycoldimercaptan (PFT) featuring rigid fluorinated benzene rings and flexible sulfur\u2010oxygen chains for synergistic dual\u2010ion regulation. The flexible segments enable gradient Li\n                    <jats:sup>+<\/jats:sup>\n                    coordination with differential binding energies, lowering desolvation barrier and facilitating uniform Li\n                    <jats:sup>+<\/jats:sup>\n                    transport, whereas the rigid electron\u2010deficient fluorinated rings trap TFSI\n                    <jats:sup>\u2212<\/jats:sup>\n                    anions via anion\u2010\u03c0 interactions. This dual modulation directs the in\u2010situ formation of a robust, LiF\u2010Li\n                    <jats:sub>2<\/jats:sub>\n                    S\u2010rich inorganic composite SEI, as validated by calculations and spectroscopy. The PFT\u2010based Li anodes exhibit exceptional stability, with symmetric cells operating over 4000 h at 1 mA cm\n                    <jats:sup>\u22122<\/jats:sup>\n                    , 1 mAh cm\n                    <jats:sup>\u22122<\/jats:sup>\n                    . A high\u2010loading LiFePO\n                    <jats:sub>4<\/jats:sub>\n                    full cell retains 80% capacity after 1000 cycles at 5 C, and an NCM811 pouch cell retains 85% capacity after 160 cycles at 0.5 C, demonstrating practical viability. This work establishes a molecular design principle for dual\u2010ion regulation via a polyinterface for high\u2010performance Li metal batteries.\n                  <\/jats:p>","DOI":"10.1002\/adma.74068","type":"journal-article","created":{"date-parts":[[2026,7,14]],"date-time":"2026-07-14T11:56:02Z","timestamp":1784030162000},"update-policy":"https:\/\/doi.org\/10.1002\/crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["A Rigid\u2010Flexible Polyinterface Enabling Molecular\u2010Level Dual\u2010Ion Regulation for Ultrastable Lithium Metal Batteries"],"prefix":"10.1002","volume":"38","author":[{"given":"Gaochuang","family":"He","sequence":"first","affiliation":[{"name":"School of Chemical Engineering and Light Industry Guangdong University of Technology  Guangzhou China"},{"name":"Dongguan Institute of Materials Science and Technology Chinese Academy of Sciences Dongguan China"},{"name":"Songshan Lake Materials Laboratory Dongguan 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