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全谱拟合法研究聚丙烯腈基碳纤维形成过程中晶态结构演变
引用本文:张彩红,盛毅,田红,徐耀,吕春祥,吴忠华.全谱拟合法研究聚丙烯腈基碳纤维形成过程中晶态结构演变[J].物理学报,2011,60(3):36101-036101.
作者姓名:张彩红  盛毅  田红  徐耀  吕春祥  吴忠华
作者单位:(1)中国科学院高能物理所同步辐射实验室,北京 100049; (2)中国科学院山西煤炭化学研究所,中国科学院炭材料重点实验室,太原 030001
基金项目:国家自然科学基金(批准号:10835008)资助的课题.
摘    要:通过全谱拟合法对碳纤维制备过程中不同阶段纤维的XRD谱图进行处理,得到不同阶段纤维的微观结构参数,研究了聚丙烯腈(PAN)基碳纤维制备过程中晶态结构的演变.全谱拟合法基于晶体衍射的严格物理理论,拟合目标为整个衍射谱,并不是个别衍射峰,所得结果具有更高的可信度.研究结果表明:PAN原丝中的高分子链沿纤维轴高度取向,表观晶粒尺寸为6.5 nm左右;经过预氧化处理,纤维中的有序结构遭到破坏,表观晶粒尺寸锐减.纤维中逐渐形成梯形结构并沿纤维轴取向,从而形成新的有序结构;经过碳化处理后,环状梯形结构转变为碳的层状结 关键词: 碳纤维 晶体结构 XRD 全谱拟合法

关 键 词:碳纤维  晶体结构  XRD  全谱拟合法
收稿时间:2010-03-24

The evolution of crystalline structure in the preparation of PAN-based carbon fibers studied by whole powder pattern fitting
Zhang Cai-Hong,Sheng Yi,Tian Hong,Xu Yao,Lü Chun-Xiang,Wu Zhong-Hua.The evolution of crystalline structure in the preparation of PAN-based carbon fibers studied by whole powder pattern fitting[J].Acta Physica Sinica,2011,60(3):36101-036101.
Authors:Zhang Cai-Hong  Sheng Yi  Tian Hong  Xu Yao  Lü Chun-Xiang  Wu Zhong-Hua
Institution:Key Laboratory of carbon Materials, Institute of Coal Chemistry, Chinese Academy of Sciences, Taiyuan 030001, China;Key Laboratory of carbon Materials, Institute of Coal Chemistry, Chinese Academy of Sciences, Taiyuan 030001, China;Key Laboratory of carbon Materials, Institute of Coal Chemistry, Chinese Academy of Sciences, Taiyuan 030001, China;Key Laboratory of carbon Materials, Institute of Coal Chemistry, Chinese Academy of Sciences, Taiyuan 030001, China;Key Laboratory of carbon Materials, Institute of Coal Chemistry, Chinese Academy of Sciences, Taiyuan 030001, China;Laboratory of Synchrotron Radiation, Institute of High Energy Physics, Chinese Academy of Sciences, Beijing 100049, China
Abstract:Based on the Rietveld theory and Maud software, the evolution of crystalline structure of PAN-based carbon fibers was studied by investigating the different stages in the preparation of carbon fibers. The microstructure parameters of PAN fibers, oxidative fibers, and carbon fibers, including cell parameters, apparent crystal grain sizes, textural structure and micro-strain, were obtained from the named whole powder pattern fitting method for XRD result. Based on rigorus theory of crystallography, the whole powder pattern fitting treats the whole XRD powder diffraction pattern rather than individual diffraction peaks, resulting in higher credibility and precision. The results indicated that polymer chains were arranged along the axis of PAN fiber and the apparent crystallite size was about 6.4 nm. After pre-oxidation, the originally ordered structure in PAN fiber was damaged and new less-ordered cyclic ladder structure was formed in the pre-oxidized PAN fibers, while the apparent crystallite size of fiber decreased obviously. With the carbonization process, the cyclic ladder structure of per-oxidized fibers transferred into layer structure similar to that of graphite. The layers were oriented along the axis of carbonized fiber that contributed to the X-ray diffraction, which comprised the apparent crystallite grains. As the carbonization temperature increased, size of the layer structure in the direction perpendicular to fiber axis increased clearly, the preferential orientation was enhanced and the layer structure became much more ordered.
Keywords:carbon fiber  crystalline structure  XRD  whole powder pattern fitting method
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