WAXS/SAXS,SAXS二维全谱拟合研究PAN基炭纤维预氧化、炭化过程中微观结构演变

李小芸; 田丰; 高学平; 边风刚; 李秀宏; 王劼

doi:10.1016/S1872-5805(17)60110-0

WAXS/SAXS,SAXS二维全谱拟合研究PAN基炭纤维预氧化、炭化过程中微观结构演变

doi: 10.1016/S1872-5805(17)60110-0

1.
中国科学院上海应用物理研究所, 上海 201204;
2.
山东大学材料科学与工程学院, 山东省碳纤维工程技术研究中心, 山东济南 250061

基金项目: 东华大学纤维材料改性国家重点实验室开放课题（LK1506）；国家自然科学青年基金（11305249）；973项目（2011CB606104，2011CB605604）.

详细信息

作者简介:
李小芸,助理研究员.E-mail:lixiaoyun@sinap.ac.cn

通讯作者:
李秀宏.E-mail:lixiuhong@sinap.ac.cn;王劼.E-mail:wangjie@sinap.ac.cn

中图分类号: TQ342⁺.74
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- 被引次数: 0
出版历程
- 收稿日期: 2017-01-18
- 录用日期: 2017-04-26
- 修回日期: 2017-04-08
- 刊出日期: 2017-04-28

WAXD/SAXS study and 2D fitting (SAXS) of the microstructural evolution of PAN-based carbon fibers during the pre-oxidation and carbonization process

1.
Shanghai Synchrotron Radiation Facility, Shanghai Institute of Applied Physics, Chinese Academy of Sciences, Shanghai 201204, China;
2.
Carbon Fiber Engineering Research Center, School of Material Science and Engineering, Shandong University, Ji'nan 250061, China

Funds: State Key Laboratory for Modification of Chemical Fibers and Polymer Materials in Donghua University (LK1506); National Natural Science Foundation of China (11305249); National Basic Research Program of China (2011CB606104, 2011CB605604).

摘要

摘要: 利用广角（WAXD）和小角散射（SAXS）的方法，对PAN基炭纤维制备过程不同阶段纤维的微晶和微孔进行研究。WAXD结果表明，在炭化过程中，微晶尺寸变大，并沿着纤维轴方向取向。SAXS结果表明，制备过程过，新微孔进一步形成，微孔逐渐沿纤维轴排列，微孔的平均长度增大。基于传统分析方法，确立微孔为具有择优取向的圆柱状，其尺寸大小成log正态函数分布的散射模型，对二维散射图进行全谱拟合分析。将此方法运用于炭纤维，得出该模型可以准确描述微孔的相关特征。
- 广角散射 /
- 小角散射 /
- 炭纤维 /
- 微孔 /
- 模型拟合
Abstract: Microstructural evolution in polyacrylonitrile (PAN) fibers at different temperatures during pre-oxidation and carbonization under stretching was studied by synchrotron wide-angle X-ray diffraction (WAXD) and small-angle X-ray scattering (SAXS). Microvoids were characterized by the classical SAXS method, and were compared with simulation results obtained by fitting 2D SAXS patterns to a model based on a dilute system of cylindrical microvoids randomly distributed and preferentially orientated along the fiber axis and having a log-normal size distribution. The WAXD results showed that the crystal size, d-spacing and preferred orientation decreased during pre-oxidation, and increased during carbonization. A diffraction peak for PAN fibers at 2θ=13.6° disappeared during the final stage of pre-oxidation, meanwhile a new peak at 2θ=23.6° appeared, whose intensity increased during carbonization, indicating the formation of the graphite structure. The average length of the microvoids increased, and new microvoids were formed, which became oriented along the fiber axis as the fiber manufacturing process proceeded. The length of microvoids from simulation results is consistent with that from the classical method, indicating that the model is valid to describe the microvoid structure of fibers.
- Wide-angle X-ray scattering /
- Small-angle X-ray scattering /
- Carbon fiber /
- Microvoids /
- Direct model fitting

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