AbstractThis study uses synchrotron wide‐angle X‐ray diffraction (WAXD) and synchrotron small angle X‐ray scattering (SAXS) to carry out an in situ study of the pre‐oxidation process of polyacrylonitrile (PAN) fibers with two different preparation processes. Through analysis of 2D WAXD/SAXS data, this study divides the evolution of PAN fiber's crystal and microporous structures during pre‐oxidation into three and two stages, respectively. The evolution of PAN fiber's crystal structure during pre‐oxidation can be divided into three stages: 1) Initial stage: small‐sized crystals melt, crystal orientation decreases, and no cyclization reactions occur. 2) Intermediate stage: cyclization reactions happen in the amorphous region, leading to increased crystal size, crystal orientation, and crystallinity. 3) Final stage: cyclization reactions occur in the crystal region, resulting in reduced crystal size and orientation. The evolution of microporous structure can be divided into two stages: microporous shrinkage stage and microporous expansion stage. These features are analyzed using 2D WAXD/SAXS techniques. This study provides valuable references and guidance for the industrial production of PAN fibers by exploring the mechanism of the pre‐oxidation process in‐depth.
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