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Polyacrylonitrile (PAN) fiber modification can promote the stabilization efficiency and mechanical properties of the subsequent carbon fibers; however, it could cause damage to the fibers to some extent. In this article, the effects of NaIO4 treatment on the chemical and physical properties of PAN fibers were investigated. After NaIO4 modification, the cyclization reaction has partially occurred, owing to the FTIR revealed that the C≡N peak was weakened, but the C=N stretching vibration peak, the –N = C=O stretching vibration peak, the C=O stretching vibration absorption peak, and the short sequence conjugate C=N characteristic peak were enhanced simultaneously, indicating a successful cyclization and dehydrogenation reaction. Moreover, owing to more oxygen-containing functional groups successfully attached to the PAN fibers and the cyclization reaction taking place, the initial temperature, peak temperature, and heat release of cyclization decreased, which means a more efficient and safer stabilization process. X-ray diffraction (XRD) showed that the (100) crystal plane microcrystal size was the smallest at 40 °C of the modification temperature, whereas the (002) crystal plane microcrystal size was the largest at 60 °C. The modified stabilized PAN fibers presented lower crystallinity and a more aromatic structure compared with untreated fibers. Raman spectra revealed a significant increase in the intensity of the G peak after NaIO4 modification; the R-value decreased from 1.65 to 1.43, demonstrating a transformation of the sp3 hybrid carbon structure into a more graphite-like sp2 hybrid C=C structure. Meanwhile, scanning electron microscopy (SEM) images disclosed additional grooves and cracks on the fiber surface after modification. [ABSTRACT FROM AUTHOR]