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在梯度升温和恒温两种模式下,对聚丙烯腈(PAN)纤维进行了热氧稳定化处理,借助FTIR、核磁共振碳谱(13 C-NMR)、元素分析(EA)、DSC、X-射线能谱(EDS)、密度等多种表征手段系统研究了不同温度下热氧稳定化纤维皮-芯结构的形成机制和氧元素的扩散速率。研究结果表明:氧化反应速率小于氧的扩散速率时,PAN纤维横截面外层与芯部差别较大,将出现皮-芯形貌结构特征;热氧稳定化纤维皮-芯结构的产生不但与温度有关,而且与升温模式密切相关;EDS表征方法可以有效地量化不同温度下,热氧稳定化纤维径向氧元素的扩散速率,同时可直观显示出氧在纤维截面不同区域的结合速率。
The polyacrylonitrile (PAN) fibers were thermally oxidized and stabilized by FTIR, 13 C-NMR, EA, DSC, and X- Ray diffraction (EDS), density and other characterization methods were used to systematically study the formation mechanism of the skin-core structure of thermo-oxidized stabilized fibers and the oxygen diffusion rate. The results show that when the oxidation rate is lower than the diffusion rate of oxygen, the outer layer of the cross-section of PAN fiber is different from the core, and the skin-core morphology will appear. The thermal-oxygen stabilized fiber skin- Temperature, but also closely related to the heating mode. The EDS characterization method can effectively quantify the diffusion rate of oxygen in the radial direction of the thermostable oxygen stabilized fibers at different temperatures, and at the same time, can visually indicate the binding rate of oxygen in different regions of the fiber cross section.