| Summary: | The low temperature carbonization process is an important stage to realize the structural transition from the organic cyclized structure of PAN based pre-oxidized fiber to the inorganic pseudo-graphite structure of the ultimate carbon fiber. In the present paper, the evolution mechanism of cyclized structure and aggregation structure of PAN stabilized fiber during low temperature carbonization was studied by means of TGA, ^13 C-NMR, XRD, XPS and Raman. The results indicated that when the heat-treated temperature was lower than 450 °C, the mainly chemical reactions were the dehydrogenation and pyrolysis reactions in acyclic linear molecular chain or partial cyclized structure. At this stage, the growth of cyclized structure was not obvious. While the original ordered structure was destroyed gradually and the internal stress increased significantly. It induced the cyclized structure to be further oriented. When the temperature was higher than 450 °C, the polycondensation and reconstruction in aromatic heterocyclic structure was more important. The early aromatic heterocycles had many different structural scales, poor homogeneity and many defects in the heterocycles. At this stage, a new pseudo-graphite crystalline structure gradually formed and the d-spacing of graphite layer decreased slightly and crystallites size increased slowly with the increase of heat-treated temperature. When the temperature was higher than 550 °C, the pseudo-graphite base structure gradually formed. The d-spacing were further reduced slightly, and the crystallites size increased slowly. A new ordered basis structure was gradually developed into carbon fiber.
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