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This study systematically compares this traditional method with a proton donor-coupled deprotonation (PCD) strategy. While both preserve the core chemical structure of PPTA fibers, the PCD approach, by incorporating a proton donor, dramatically alters the reaction kinetics and nanofibrillation pathway. Comprehensive characterization confirms that it accelerates exfoliation from days to 4 h, yielding a highly transparent dispersion. Crucially, the synthesis pathway dictates the final nanomorphology: conventional ANFs form rigid networks with larger pores (\u223c44 nm), whereas PCD-derived ANFs are more interconnected and pliable, self-assembling into denser membranes with finer pores (\u223c9 nm). This structural divergence translates to superior integrated mechanical performance, with PCD-ANF membranes exhibiting a remarkable balance of high tensile strength (115.14 MPa) and good ductility (19.27%), alongside fully retained inherent flame retardancy. This work establishes fundamental structureproperty relationships, demonstrating that the choice of nanofibrillation mechanism is a powerful tool for tailoring nanoscale architecture in advanced functional materials.<\/jats:p>","DOI":"10.1021\/acsami.6c16767","type":"journal-article","created":{"date-parts":[[2026,9,28]],"date-time":"2026-09-28T18:02:48Z","timestamp":1790618568000},"page":"53879-53894","source":"Crossref","is-referenced-by-count":0,"title":["A Comparative Study: Unveiling the Nanomorphology Evolution and Fibrillation Pathways in Deprotonation vs Proton-Coupled Deprotonation for High-Efficiency Aramid Nanofiber Synthesis"],"prefix":"10.1021","volume":"18","author":[{"ORCID":"https:\/\/orcid.org\/0000-0002-8204-7413","authenticated-orcid":true,"given":"Weiwei","family":"Li","sequence":"first","affiliation":[{"name":"Shangluo University , , ,","place":["Shangluo, China, 726000"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Jinxue","family":"Lei","sequence":"additional","affiliation":[{"name":"Shangluo University , , ,","place":["Shangluo, China, 726000"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Hongli","family":"Mi","sequence":"additional","affiliation":[{"name":"Shangluo University , , ,","place":["Shangluo, China, 726000"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Ting","family":"Chen","sequence":"additional","affiliation":[{"name":"Shangluo University , , ,","place":["Shangluo, China, 726000"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"given":"Xuan","family":"Li","sequence":"additional","affiliation":[{"name":"Shangluo University , , ,","place":["Shangluo, China, 726000"]}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-9267-6061","authenticated-orcid":true,"given":"Meiyun","family":"Zhang","sequence":"additional","affiliation":[{"name":"Shaanxi University of Science & Technology , , ,","place":["Xi\u2019an, China, 710021"]}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"316","published-online":{"date-parts":[[2026,9,28]]},"reference":[{"key":"2026100915081908700_cit1","doi-asserted-by":"publisher","first-page":"168","DOI":"10.1007\/s40820-022-00919-0","article-title":"Self Exfoliation of Flake Graphite for Bioinspired Compositing with Aramid Nanofiber toward Integration of Mechanical and Thermoconductive Properties","volume":"14","author":"Huang","year":"2022","journal-title":"Nano Micro Lett."},{"key":"2026100915081908700_cit2","doi-asserted-by":"publisher","first-page":"10359","DOI":"10.1039\/d3ta07473k","article-title":"Electromagnetic interference shielding performance of lightweight aramid nanofiber\/graphene composite aerogels","volume":"12","author":"Luo","year":"2024","journal-title":"J. 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