The modification before the stabilization process could tune the exothermic behavior and the structural evolution of PAN fibers during stabilization. In this study, we demonstrate that a rapid thermal pretreatment in nitrogen can effectively mitigate the exothermic behavior of PAN fibers, such as decreasing the initial temperature, broadening the exothermal peak, and decreasing the nominal heat release during heating the fibers in air. The color of fibers has shown gradual changes from white to light yellow, yellow and brown during thermal pretreatment in nitrogen with the increase of pretreating temperature and time. The differential scanning calorimetry (DSC), Fourier Transform Infrared Spectrometer (FTIR), X-ray diffraction (XRD), and Thermogravimetric Analysis (TG) characterization have been applied to analyze the thermal properties, chemical and physical structural difference between PAN, and thermally pretreated PAN fibers. The thermal pretreatment of PAN fibers in nitrogen could induce cyclization, dehydrogenation, and cross-linking reactions, in which the cyclization play an important role on improving the cyclization index of stabilized PAN fibers. Meanwhile, the pretreatment can result in noticeable changes of the aggregation structure of PAN fibers, as indicated by the increase of crystallinity and crystalline size. These structural modifications can benefit the main cyclization reaction during stabilization and enhance the carbon yield in resultant carbon fibers. The rapid thermal pretreatment in nitrogen could increase efficiency of modification on PAN fibers, and that could save much time and energy. It is beneficial to manufacture low-cost carbon fibers and to spread the applications of carbon fibers.

The radial structural heterogeneity of thermally-stabilized polyacrylonitrile (PAN) fiber is considered to be a limiting factor affecting the mechanical properties of the resulting carbon fibers. In this study, we demonstrate that a low-dose (60 kGy) γ-ray irradiation pretreatment can effectively mitigate the radial structural heterogeneity of PAN fibers after thermal stabilization. The characterization results indicate that low-dose γ-ray irradiation only affects the physical structure of PAN through decreasing its crystalline size and crystallinity, rather than inducing chemical cross-linking and/or intramolecular cyclization. It is proposed that an increased amorphous region in PAN fibers prompted by low-dose γ-ray irradiation can facilitate oxygen diffusion from skin to core during stabilization, which results in the increased structural homogeneity of stabilized PAN fibers.

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