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Novel poly(vinyl alcohol) (PVA) nanofibers were prepared through the heterogeneous saponification of poly(vinyl acetate) (PVAc) nanofibers for the first time. To prepare the saponified PVA nanofibers, the effects of the alkali solution concentration and temperature were studied. It was found that the degree of saponification depended on the temperature and alkali solution concentration. Field emission scanning electron microscopy was utilized to characterize the morphology and properties of mats of the saponified PVA nanofibers, and unusual wrinkled and wound fibers were found. The conversion of PVAc nanofibers to PVA nanofibers was measured using proton nuclear magnetic resonance spectrometry, X-ray diffraction measurements, and Fourier transform infrared spectroscopy.