A novel microwave annealing system and a specific processing condition are proposed for the pre-oxidation of carbon fiber. The microwave annealing system consists of a TM-mode resonant cavity and a silicon carbide (SiC) susceptor. The TM-mode cavity enhances the electric field at the center. The SiC susceptor absorbs part of the microwave energy and converts it to heat. The enhanced fields and the SiC susceptor provide both nonthermal and thermal treatments for fibrous materials with various dielectric properties. Furthermore, a two-step microwave annealing process is used to oxidize polyacrylonitrile (PAN) fiber. The scanning electron microscopy (SEM) images, differential scanning calorimetry (DSC), and X-ray diffraction (XRD) results support the theory that the microwave annealing can achieve a high aromatic index of 66.39% in just 13 min, 9 times faster than the traditional processing time. The results of the Raman spectra also illustrate that the sheath-core factor of the microwave-heated specimen is closer to one than that of the conventional furnace-heated type, which agree with the images of the cross-section area.
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