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Herein, a series of non-fullerene acceptors (NFAs) with progressively reduced terminal fluorination were developed to systematically elucidate the role of terminal fluorination in molecular assembly and photovoltaic performance. Among them, the moderately fluorinated acceptor N3-3F delivered the highest power conversion efficiency (PCE) of 19.11%, achieving an optimal balance among open-circuit voltage (VOC), short-circuit current density (JSC) and fill factor (FF). By integrating in situ absorption spectroscopy with multiscale structural characterization and theoretical calculations, we demonstrate that moderate terminal defluorination regulates molecular assembly kinetics during film formation. The resulting optimized assembly process promotes ordered molecular packing and an optimized bulk-heterojunction morphology, thereby facilitating efficient charge generation and extraction while maintaining balanced charge transport. Theoretical calculations further reveal that the regulated assembly originates from an optimized intermolecular electrostatic environment established through moderate terminal fluorination. This work uncovers the molecular origin of assembly kinetics regulation by terminal fluorination, providing a fundamental insight into how intermolecular interactions govern morphology evolution in OSCs.<\/jats:p>","DOI":"10.1021\/acsami.6c16242","type":"journal-article","created":{"date-parts":[[2026,9,24]],"date-time":"2026-09-24T19:02:00Z","timestamp":1790276520000},"page":"53749-53758","source":"Crossref","is-referenced-by-count":0,"title":["Terminal Fluorination Regulates Molecular Assembly Kinetics toward Optimized Bulk-Heterojunction Morphology"],"prefix":"10.1021","volume":"18","author":[{"given":"Shanshan","family":"Qin","sequence":"first","affiliation":[{"name":"Fujian Normal University , , ,","place":["Fuzhou, China, 350117"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Fengzhi","family":"Wang","sequence":"additional","affiliation":[{"name":"Fujian Normal University , , ,","place":["Fuzhou, China, 350117"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Zhenyu","family":"Chen","sequence":"additional","affiliation":[{"name":"Fujian Normal University , , ,","place":["Fuzhou, China, 350117"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Yongchao","family":"Hu","sequence":"additional","affiliation":[{"name":"Fujian Normal University , , ,","place":["Fuzhou, China, 350117"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Jinrong","family":"Shi","sequence":"additional","affiliation":[{"name":"Fujian Normal University , , ,","place":["Fuzhou, China, 350117"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Pengfei","family":"Ding","sequence":"additional","affiliation":[{"name":"Ningbo Institute of Materials Technology & Engineering, Chinese Academy of Sciences , , ,","place":["Ningbo, China, 315201"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-3583-7578","authenticated-orcid":true,"given":"Lizhi","family":"Jiang","sequence":"additional","affiliation":[{"name":"Fujian Normal University , , ,","place":["Fuzhou, China, 350117"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Tao","family":"Zhang","sequence":"additional","affiliation":[{"name":"Fujian Normal University , , ,","place":["Fuzhou, China, 350117"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Kangqiao","family":"Ma","sequence":"additional","affiliation":[{"name":"Fujian Normal University , , ,","place":["Fuzhou, China, 350117"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-1011-7977","authenticated-orcid":true,"given":"Kang","family":"Wang","sequence":"additional","affiliation":[{"name":"Fujian Normal University , , ,","place":["Fuzhou, China, 350117"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0009-0008-5530-514X","authenticated-orcid":true,"given":"Deping","family":"Qian","sequence":"additional","affiliation":[{"name":"Fujian Normal University , , ,","place":["Fuzhou, China, 350117"]}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"316","published-online":{"date-parts":[[2026,9,24]]},"reference":[{"issue":"28","key":"2026100705072017300_cit1","doi-asserted-by":"publisher","DOI":"10.1002\/adma.202500352","article-title":"Organic Solar Cell with Efficiency of 20.49% Enabled by Solid Additive and Non-Halogenated Solvent","volume":"37","author":"Liu","year":"2025","journal-title":"Adv. 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