Li Yang, Luo Zhu, Yang Le, Li Xiaolong, Xiang Kun
Department of Polymer Material and Engineering, College of Materials and Metallurgy, Guizhou University, Guiyang 550025, China.
School of Materials Science and Metallurgy Engineering, Guizhou Institute of Technology, Guiyang 550003, China.
Polymers (Basel). 2019 Apr 17;11(4):700. doi: 10.3390/polym11040700.
The outstanding diffusivity and permeability of supercritical carbon dioxide (scCO) are extremely beneficial for grafting reaction. In this work, aramid fibers (AF) are modified in scCO by glycidyl-polyhedral oliomeric silsesquioxane (POSS) with 2-ethyl-4-methylimidazole (2E4MZ) on the basis of cleaning with acetone. The surface morphology and chemical structure of the modified AF were measured and characterized by Fourier transform infrared spectroscopy (FTIR), X-ray photoelectron spectroscopy (XPS), Scanning electron microscope (SEM), Thermogravimetric (TG), and Atomic force microscope (AFM). The interfacial shear strength (IFSS) was measured by a micro-bond pull-out test, then the modified AF/EP composites were prepared and the interlaminar shear strength (ILSS) was characterized. Research has shown that some of the glycidyl-POSS molecular chains permeated into the surface of the fiber and grafted onto the surface of the AF after modification, and the other glycidyl-POSS self-assembled on the surface of the fiber. XPS indicated the introduction of C-O and -COO-, which confirmed the existence of chemical reactions between AF and glycidyl-POSS. AFM and SEM images revealed that 2E4MZ, not only promoted the grafting reaction of glycidyl-POSS, but also intensified the self-assembly of glycidyl-POSS, both of which increased the roughness of the fiber. A monofilament tensile test and micro-bond pull-out test showed that there was a negative effect on the tensile strength after scCO processing. The tensile strength of modified AF, with glycidyl-POSS, increased the highest strength of 25.7 cN dtex, which was 8% higher than that of pristine AF. The improvement of ILS roughness and the polar chemical groups produced in grafting reaction. These results indicated that AF, treated in scCO, with glycidyl-POSS, which is a suitable way of fiber modification, can significantly improve the surface adhesion of AF reinforced composites.
超临界二氧化碳(scCO₂)出色的扩散率和渗透率对接枝反应极为有利。在本工作中,芳纶纤维(AF)在经丙酮清洗后,于scCO₂中用缩水甘油基-多面体低聚倍半硅氧烷(POSS)和2-乙基-4-甲基咪唑(2E4MZ)进行改性。通过傅里叶变换红外光谱(FTIR)、X射线光电子能谱(XPS)、扫描电子显微镜(SEM)、热重分析(TG)和原子力显微镜(AFM)对改性AF的表面形貌和化学结构进行了测量与表征。通过微粘结拔出试验测量界面剪切强度(IFSS),随后制备改性AF/EP复合材料并表征层间剪切强度(ILSS)。研究表明,部分缩水甘油基-POSS分子链渗透到纤维表面并在改性后接枝到AF表面,另一部分缩水甘油基-POSS在纤维表面自组装。XPS表明引入了C-O和-COO-,证实了AF与缩水甘油基-POSS之间存在化学反应。AFM和SEM图像显示,2E4MZ不仅促进了缩水甘油基-POSS的接枝反应,还强化了缩水甘油基-POSS的自组装,二者均增加了纤维的粗糙度。单丝拉伸试验和微粘结拔出试验表明,scCO₂处理后对拉伸强度有负面影响。含缩水甘油基-POSS的改性AF的拉伸强度最高提高了25.7 cN dtex,比原始AF高8%。ILSS粗糙度的提高以及接枝反应中产生的极性化学基团。这些结果表明,在scCO₂中用缩水甘油基-POSS处理AF是一种合适的纤维改性方式,可显著提高AF增强复合材料的表面附着力。