Varfolomeeva Lydia A, Skvortsov Ivan Yu, Levin Ivan S, Shandryuk Georgiy A, Patsaev Timofey D, Kulichikhin Valery G
A. V. Topchiev Institute of Petrochemical Synthesis of Russian Academy of Sciences, Leninsky Av. 29, 119991 Moscow, Russia.
National Research Center "Kurchatov Institute", 1, Akademika Kurchatova pl., 123182 Moscow, Russia.
Polymers (Basel). 2023 Jun 5;15(11):2579. doi: 10.3390/polym15112579.
This study presents preparing and characterization of polyacrylonitrile (PAN) fibers containing various content of tetraethoxysilane (TEOS) incorporated via mutual spinning solution or emulsion using wet and mechanotropic spinning methods. It was shown that the presence of TEOS in dopes does not affect their rheological properties. The coagulation kinetics of complex PAN solution was investigated by optical methods on the solution drop. It was shown that during the interdiffusion process phase separation occurs and TEOS droplets form and move in the middle of the dope's drop. Mechanotropic spinning induces the TEOS droplets to move to the fiber periphery. The morphology and structure of the fibers obtained were investigated by scanning and transmission electron microscopy, as well as X-ray diffraction methods. It was shown that during fiber spinning stages the transformation of the TEOS drops into solid silica particles takes place as a result of hydrolytic polycondensation. This process can be characterized as the sol-gel synthesis. The formation of nano-sized (3-30 nm) silica particles proceeds without particles aggregation, but in a mode of the distribution gradient along the fiber cross-section leading to the accumulation of the silica particles either in the fiber center (wet spinning) or in the fiber periphery (mechanotropic spinning). The prepared composite fibers were carbonized and according to XRD analysis of carbon fibers, the clear peaks corresponding to SiC were observed. These findings indicate the useful role of TEOS as a precursor agent for both, silica in PAN fibers and silicon carbide in carbon fibers that has potential applications in some advanced materials with high thermal properties.
本研究介绍了通过互溶纺丝溶液或乳液,采用湿法和机械致动纺丝方法制备并表征含有不同含量四乙氧基硅烷(TEOS)的聚丙烯腈(PAN)纤维。结果表明,原液中TEOS的存在不影响其流变性能。通过光学方法对溶液滴进行研究,考察了复合PAN溶液的凝固动力学。结果表明,在互扩散过程中发生相分离,TEOS液滴形成并在原液滴的中部移动。机械致动纺丝促使TEOS液滴移至纤维周边。通过扫描电子显微镜、透射电子显微镜以及X射线衍射方法对所得纤维的形态和结构进行了研究。结果表明,在纤维纺丝阶段,由于水解缩聚作用,TEOS液滴转变为固态二氧化硅颗粒。该过程可表征为溶胶-凝胶合成。纳米级(3-30nm)二氧化硅颗粒的形成过程中无颗粒聚集现象,而是以沿纤维横截面分布梯度的方式进行,导致二氧化硅颗粒在纤维中心(湿法纺丝)或纤维周边(机械致动纺丝)积累。对制备的复合纤维进行碳化处理,根据碳纤维的XRD分析,观察到对应于SiC的清晰峰。这些发现表明TEOS作为PAN纤维中二氧化硅以及碳纤维中碳化硅的前驱剂具有重要作用,在一些具有高热性能的先进材料中具有潜在应用价值。