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Although LiClO4 has been employed in such systems, its role beyond a lithium-ion source has not been systematically investigated. Here, we report a two-component electrolyte consisting of 1 M LiClO4 and 0.3 M BF3-THF (1-0.3PTHF) that enables the in situ formation of poly(tetrahydrofuran) (PTHF) with substantially reduced initiator loading. The incorporation of LiClO4 not only provides mobile Li+ ions but also facilitates polymerization. Possible ionic interactions between LiClO4 species and growing polymer chains may contribute to the improvement. The 1-0.3PTHF exhibited a narrow mass distribution (\u0110 = 1.23) and a low degree of crystallinity (4.7%) compared to commercial PTHF (\u0110 = 3.25) and the PTHF polymerized without LiClO4. The in situ 1-0.3PTHF delivered a bulk ionic conductivity of 2.75 \u00d7 10\u22123 S cm\u22121, an electrochemical window of 5.06 V, and stable lithium plating\/stripping up to 3 mA cm\u22122, suggesting its promise as a GPE. Post-mortem XPS confirms the coexistence of B-containing species and LiCl within the SEI. Full cell tests demonstrated the preliminary feasibility of the 1-0.3PTHF GPE with LFP, LCO, and NCM cathodes. This work highlights the multifunctional role of LiClO4 in in situ polymerized PTHF. The resulting 1-0.3PTHF electrolyte simultaneously regulates polymerization, enhances ionic conduction, and promotes protective SEI formation. These findings broaden the role of lithium salts beyond lithium-ion sources to polymerization modulators in in situ polymerized GPEs.<\/jats:p>","DOI":"10.3390\/polym18192379","type":"journal-article","created":{"date-parts":[[2026,9,29]],"date-time":"2026-09-29T16:33:12Z","timestamp":1790699592000},"page":"2379","update-policy":"https:\/\/doi.org\/10.3390\/mdpi_crossmark_policy","source":"Crossref","is-referenced-by-count":0,"title":["Multifunctional LiClO4 for Polymerization Regulation, Ionic Conduction, and Interphase Formation in In Situ Poly(tetrahydrofuran) Gel Polymer Electrolytes"],"prefix":"10.3390","volume":"18","author":[{"given":"Si-Han","family":"Peng","sequence":"first","affiliation":[{"name":"Department of Chemical and Materials Engineering, Chang Gung University, Guishan District, Taoyuan City 333, Taiwan"}],"role":[{"vocabulary":"crossref","role":"author"},{"role":"conceptualization","vocabulary":"credit"},{"role":"methodology","vocabulary":"credit"},{"role":"validation","vocabulary":"credit"},{"role":"formal-analysis","vocabulary":"credit"},{"role":"investigation","vocabulary":"credit"},{"role":"data-curation","vocabulary":"credit"},{"role":"writing-original-draft","vocabulary":"credit"},{"role":"visualization","vocabulary":"credit"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-3939-8736","authenticated-orcid":false,"given":"Wei-Fan","family":"Kuan","sequence":"additional","affiliation":[{"name":"Center for Sustainability and Energy Technologies, Department of Chemical and Materials Engineering, Chang Gung University, Guishan District, Taoyuan City 333, Taiwan"}],"role":[{"vocabulary":"crossref","role":"author"},{"role":"resources","vocabulary":"credit"},{"role":"formal-analysis","vocabulary":"credit"},{"role":"writing-review-editing","vocabulary":"credit"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-1950-8093","authenticated-orcid":false,"given":"Shingjiang Jessie","family":"Lue","sequence":"additional","affiliation":[{"name":"Department of Chemical and Materials Engineering, Chang Gung University, Guishan District, Taoyuan City 333, Taiwan"},{"name":"Department of Safety, Health and Environmental Engineering, Ming-Chi University of Technology, Taishan District, New Taipei City 243, Taiwan"}],"role":[{"vocabulary":"crossref","role":"author"},{"role":"funding-acquisition","vocabulary":"credit"},{"role":"supervision","vocabulary":"credit"},{"role":"project-administration","vocabulary":"credit"},{"role":"writing-review-editing","vocabulary":"credit"},{"role":"formal-analysis","vocabulary":"credit"}]}],"member":"1968","published-online":{"date-parts":[[2026,9,29]]},"reference":[{"key":"ref_1","doi-asserted-by":"crossref","first-page":"10087","DOI":"10.1021\/acs.chemrev.1c00978","article-title":"Freestanding metal\u2013organic frameworks and their derivatives: An emerging platform for electrochemical energy storage and conversion","volume":"122","author":"He","year":"2022","journal-title":"Chem. 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