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In this work, we report the preparation of high-purity perfluorosulfonated ionomer (Nafion) nanofibers (NFs) via solution blow spinning (SBS). Fiber formation in solution jet spinning is strongly dependent on the structure of the spinning solution. Upon adding a small amount of poly(ethyleneoxide) (PEO) as a spinning aid to Nafion dispersion, most of the highly ordered Nafion aggregate disappeared, allowing the stable production of bead-free and smooth high-purity NFs (Nafion/PEO = 99/1) by SBS. The microstructure of the blowspun Nafion NFs differed from that of electrospun NFs. In the blowspun NFs, incomplete microphase separation between hydrophilic (ionic) and hydrophobic domains was observed, but the crystallization of CF₂−CF₂ chains was enhanced owing to the high extensional strain rate and rapid solidification during SBS. These findings provide fundamental information for the preparation and characterization of blowspun Nafion NFs.