纳米SiO2改性炭纤维乳液上浆剂的性能评价

采用纳米SiO₂改性环氧树脂乳液上浆剂和未改性乳液上浆剂对聚丙烯腈(PAN)基炭纤维进行表面上浆。通过静置沉淀法和光学显微镜评价了两种乳液的稳定性。利用扫描电子显微镜(SEM)、 X射线能谱仪(EDS)、 原子力显微镜(AFM)和动态接触角测试仪(DCAA)研究了未上浆、 未改性和改性上浆炭纤维的表面性能, 并用单纤维碎裂法探讨了上浆剂对炭纤维与环氧树脂界面黏结的影响。结果表明: 未改性和经纳米SiO₂改性的两种乳液粒径较小, 稳定性较好, 而前者优于后者。上浆后, 炭纤维表面的粗糙度和表面能都增大, 而且最大值出现在改性乳液上浆炭纤维的表面。改性乳液上浆单纤维复合材料拥有最大的界面剪切强度(IFSS), 比未改性上浆的高出27.2%; 改性上浆炭纤维与基体的调和平均黏结功(W(h)_a )和几何平均黏结功(W(g)_a )也分别高出未改性上浆的12.7%和11.7%。      

碳纳米管改性乳液上浆剂对炭纤维复合材料界面性能的影响

采用碳纳米管改性环氧树脂乳液上浆剂和未改性上浆剂对聚丙烯腈(PAN)基炭纤维进行表面上浆。通过激光粒度仪研究两种乳液的稳定性。采用扫描电子显微镜(SEM)、X-射线光电子能谱仪(XPS)与原子力显微镜(AFM)研究未改性及改性上浆炭纤维的表面结构,并用HM410界面评价装置研究炭纤维复合材料的界面性能。结果表明,碳纳米管改性后,乳液稳定性得到提高。上浆后,炭纤维表面粗糙度增加73.1%,同时接触角减小11.9%,且炭纤维表面的含氧官能团含量增加45.96%。此外,改性炭纤维复合材料的界面性能得到明显改善。当碳纳米管在上浆剂中质量分数为0.75 w t%时,炭纤维单丝的界面剪切强度较之未改性炭纤维提高14.7%。     

纳米SiO2改性上浆剂对炭纤维复合材料界面性能的影响

利用单纤维碎裂法，三点短梁法，扫描电镜（SEM）和动态力学热分析（DMTA）研究了未上浆炭纤维、环氧树脂乳液上浆炭纤维和经纳米SiO2改性环氧树脂乳液上浆炭纤维增强树脂基复合材料（CFRP）的界面性能。结果表明：炭纤维经改性乳液上浆剂和未改性乳液上浆剂上浆后，与未上浆相比，其单纤维复合材料的界面剪切强度（IFSS）分别提高了79％和41％，复合材料的层间剪切强度（ILSS）分别提高了14％和9％。DMTA图谱显示经纳米SiO：改性上浆的CFRP其损耗角正切（tanδ）较未改性上浆的降低18％，玻璃化温度（Tg）高出5℃。说明上浆剂中添加纳米SiO2可使上浆后的CFRP界面黏结性得到显著增强。     

炭纤维特性与炭纤维/环氧树脂界面断裂能关联分析

采用基于WND(Wagner-Nairn-Detassis)能量模型的单丝断裂法,测试了5种国产炭纤维、2种国外炭纤维与航空结构用环氧树脂复合体系的界面断裂能,通过SEM,AFM,IR以及XPS等手段分析了7种炭纤维的表面物理化学特性,并研究了炭纤维特性与界面断裂能的关联。结果表明:对于所研究的炭纤维/环氧树脂体系,去除炭纤维表面上浆剂后界面断裂能下降,说明上浆剂可以在一定程度上提高界面的韧性。此外,实验范围内,纤维拉伸强度较高时,测得的界面断裂能较高,炭纤维表面粗糙度较高时,测得界面断裂能较高,说明纤维拉伸性能和表面粗糙度对界面韧性有重要影响,而与这两种因素相比,上浆剂的种类影响相对较小。研究结果为高性能国产炭纤维的研发和炭纤维/树脂匹配性的评价提供了重要的实验数据。     

纳米SiO2改性乳液上浆剂对炭纤维抗拉强度的影响

利用Weibull统计分布分析了上浆对炭纤维单丝抗拉强度的影响。通过扫描电镜（SEM）观察和X射线能谱仪（EDS）分析了上浆前后炭纤维表面和截面的结构形貌及表面元素组成。结果表明：当纳米SiO2粒子与上浆树脂的质量比为0．5％时，上浆炭纤维单丝的抗拉强度最高，增幅达10．1％；Weibull参数m值最大，强度的分散性最小。EDS显示了改性上浆炭纤维表面Si元素含量增大。上浆炭纤维比未上浆的表面较均匀，纹理沟槽变浅；截面凹凸不平，呈现一定的韧性断裂特性。说明上浆剂中添加纳米SiO2粒子可以明显提高上浆炭纤维的强度。     

单丝拉伸断裂法探究上浆剂改性炭纤维与聚碳酸酯的界面黏结性

为了探究不同上浆剂对炭纤维/聚碳酸酯复合材料界面黏结性的影响,采用自制水性聚碳酸酯乳液、聚醋酸乙烯酯乳液、聚氨酯乳液与聚乙烯乳液等上浆剂对炭纤维进行表面改性。采用红外光谱(IR)和热重-质谱联用(TG-MS)仪分析上浆剂的化学结构;采用扫描电子显微镜(SEM)、X射线光电子能谱仪(XPS)与热重分析仪(TG)等研究上浆改性炭纤维的表面结构。为了量化地分析炭纤维与聚碳酸酯的界面剪切强度,采用单丝拉伸断裂法得到界面剪切强度。结果表明,水性聚氨酯乳液上浆改性后的炭纤维与聚碳酸酯的界面剪切强度最高(29.19 MPa),这是由于聚氨酯中含有较多的氨酯键,可与树脂形成较多的氢键。相对而言,水性自制乳液与聚醋酸乙烯酯乳液涂层后的炭纤维与聚碳酸酯之间只有物理吸附作用,因此界面黏结性略弱。     

聚酰亚胺改性炭纤维增强聚苯硫醚复合材料的制备及表征

以均苯四甲酸(PMDA)和4,4’二氨基二苯醚(ODA)为原料合成聚酰胺酸(PAA),并以此为上浆剂对炭纤维实施上浆处理,通过热酰亚胺化的方法在炭纤维表面形成聚酰亚胺(PI)上浆层,用于提高炭纤维/聚苯硫醚(CF/PPS)界面结合强度。通过扫描电子显微镜和X射线光电子能谱仪对PI上浆炭纤维表面进行分析,结果表明在炭纤维表面形成一层连续且均匀的PI涂层,且经PI处理后的炭纤维表面高活性碳含量比未处理炭纤维提高了9.72%。相比于未处理CF/PPS复合材料,PI上浆CF/PPS复合材料的层间剪切强度、压缩强度和压缩模量分别提高了26.39%、26.02%和19.64%。     

膨胀炭纤维增强柔性石墨复合材料力学性能研究

本工作制备了膨胀炭纤维增强柔性石墨复合材料。研究和比较了短切纤维的种类、含量对复合材料力学性能的影响。利用SEM等分析测试手段研究了膨胀炭纤维和柔性石墨基体的界面状况，并探讨了复合材料的断裂机理。结果表明，高温膨化处理后，膨胀炭纤维的表面形貌发生显著改变，膨胀炭纤维作为增强体参与膨胀石墨解理面的相互锁合，复合材料具有较高的抗拉强度。     

国产T800级炭纤维表面特性及其复合材料微观界面性能

采用扫描电镜(SEM)、原子力显微镜(AFM)、X射线光电子能谱(XPS)等测试方法表征了两种国产上浆/去浆T800级炭纤维的表面特性,并通过单丝断裂实验测试了单丝复合体系微观界面剪切强度(IFSS),在此基础上研究了炭纤维表面特性对单丝复合体系微观界面性能及其耐湿热性能的影响。结果表明:去浆后炭纤维表面含氧活性官能团含量降低,粗糙度增加,与基体树脂的界面结合强度增大;湿热环境对复合材料的微观界面性能影响显著,尤其是破坏了纤维/基体间的化学键合作用,但去湿后部分界面性能可恢复。     

沥青基炭纤维γ-射线改性对炭/ 炭复合材料力学性能的影响

为了提高沥青基炭纤维表面活性, 采用γ-射线辐照对沥青基炭纤维表面改性。用AFM、XPS 研究了γ-射线辐照改性后沥青基炭纤维表面结构的变化, 用浸润仪测定了改性前后沥青基炭纤维表面能的变化。研究了γ-射线辐照沥青基炭纤维对炭/ 炭复合材料力学性能的影响, 并用SEM 分析了炭/ 炭复合材料断口形貌。结果表明,γ-射线辐照使炭纤维表面含氧官能团和表面粗糙度增加, 提高了沥青基炭纤维的表面能; 降低了炭/ 炭复合材料孔隙率, 提高了炭/ 炭复合材料力学性能。     

Effect of nano-SiO2 modified emulsion sizing on the interfacial adhesion of carbon fibers reinforced composites

The influence of nano-SiO₂ modified epoxy emulsion sizing on the interfacial adhesion properties of carbon fibers reinforced composites was investigated. The interfacial interaction between carbon fibers and the matrix was characterized by X-ray photoelectron spectrometry (XPS), scanning electron microscopy (SEM) and three-point short-beam shear testing. The results showed that the amount of hydroxyl groups was slightly increased on the carbon fibers surface after treatment with nano-SiO₂ modified sizing. Compared to the unsized composites, the interlaminar shear strength (ILSS) values for the composites with unmodified sizing and nano-SiO₂ modified sizing were increased by 9% and 14%, respectively. The holes and carbon fibers pullout were not observed in their fracture sections. Surprisingly, the fracture section of the composites with nano-SiO₂ modified sizing was more compact and the fiber debonding was more difficult.     

Effects of emulsion sizing with nano-SiO<Subscript>2</Subscript> on interfacial properties of carbon fibers/epoxy composites

Nano-SiO₂ particles were used to modify epoxy emulsion sizing of carbon fibers to improve the interfacial properties of carbon fibers reinforced epoxy composites. The mechanical interfacial strength between fibers and matrix was investigated by the single fiber fragmentation test and the 3-point short beam shear test, respectively. Dynamic contact angle analysis (DCAA), X-ray photoelectron spectrometry (XPS) and atomic force microscopy (AFM) were performed on the carbon fibers with unmodified sizing and nano-SiO₂ modified sizing. The results indicated that modified sizing with nano-SiO₂ slightly increased the surface energy, the hydroxyl functional group and the surface roughness of carbon fibers compared to unmodified sizing, so that the interfacial shear strength (IFSS) of the single fiber composites and the interlaminar shear strength (ILSS) of composites were enhanced. SEM images of fracture sections of composites proved powerfully that the interfacial adhesion between fibers and matrix was improved after nano-SiO₂ modified emulsion sizing treatment.     

聚合物涂层对高模量碳纤维表面性能的影响

为改善碳纤维表面性能以及碳纤维/树脂复合材料的界面性能,对PAN基高模量碳纤维（HMCF）表面进行聚合物涂层处理。研究了不同潜伏性固化剂含量的聚合物涂层对HMCF表面以及碳纤维/树脂复合材料的界面性能的影响。IR分析表明,聚合物涂层与纤维或树脂基体发生了化学反应。扫描电镜和动态机械热分析的结果也说明,聚合物涂层能够提高...     

Surface and wettability property analysis of CCF300 carbon fibers with different sizing or without sizing

To analyze the role of sizing on carbon fibers and the mechanism of adhesion in CF/polymer matrix composites, scanning electronic microscopy (SEM), atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS), and dynamic contact angle analysis (DCAA) were selected to characterize the different properties between two types of sizings on carbon fiber CCF300. The results of surface roughness obtained from SEM and AFM images showed that the sizings smooth the surface of CCF300. In addition, the percentage of surface polar functional groups on sized CCF300 decreased slightly after sizing. In another hand, the total surface energy and the polar component of surface energy of the sized CCF300 decreased slightly compared to the unsized CCF300, and the J4 sizing has the more influence.     

T800H碳纤维表面特性及T800H/BA9918复合材料湿热性能研究

为了研究T800H碳纤维的表面特性及其与BA9918树脂的界面匹配性,分别采用SEM、AFM、XPS和TGA对T800H碳纤维表面形貌、表面化学特性以及碳纤维上浆剂热稳定性进行表征,测试了T800H/BA9918复合材料湿热处理前后0°压缩强度、90°拉伸强度和层间剪切强度,并得到了其在湿热处理前后的开孔压缩和冲击后压缩性能.测试发现T800H碳纤维表面有明显的沟槽,有利于表面机械啮合作用;T800H/BA9918复合材料经29 J能量冲击后压缩强度为314 MPa;在130℃湿态环境下其0°压缩强度和层间剪切强度保持率高于58%,开孔压缩强度保持率高于60%.试验结果证明T800H碳纤维与BA9918树脂具有良好的界面匹配性,T800H/BA9918复合材料具有优异的耐湿热性能.     

UHMWPE 纤维表面处理及其复合材料性能

对超高分子量聚乙烯(U HMWPE) 纤维进行了铬酸液相氧化和上胶剂表面涂覆的复合表面处理, 并对U HMWPE 纤维表面处理前后与几种不同结构的环氧树脂基体制备的复合材料进行界面性能研究。结果表明: 树脂种类对复合材料界面性能略有影响, 但层间剪切强度都较低。对纤维进行单纯的液相氧化和表面涂覆均可以提高复合材料的界面性能, 但液相氧化处理时间过长会使纤维强度降低; 而液相氧化2涂覆的复合处理则具有协同效应, 在不降低纤维强度的同时大幅度提高复合材料的层间剪切强度, 是一种有效的表面处理方法。      

新型水性上浆剂对碳纤维及其复合材料界面性能的影响

使用新型水性上浆剂O3PPA对碳纤维表面进行改性处理,使用聚己内酰胺树脂为基体制备碳纤维/聚己内酰胺树脂复合材料,使用X射线光电子能谱仪(XPS)、扫描电镜(SEM)、纤维强伸度仪(XQ-1A)、万能材料试验机等手段表征改性后的碳纤维和碳纤维/聚己内酰胺树脂复合材料。结果表明,O3PPA的最佳上浆质量分数和吸附量分别为1%和5 mg/g。经O3PPA处理的碳纤维单丝的断裂强度提高了12%,碳纤维短丝在聚己内酰胺树脂中的分散性明显提高。而经O3PPA处理的碳纤维/聚己内酰胺树脂复合材料,其弯曲强度和层间剪切强度比未处理分别提高了35%和46%。     

Surface State of Carbon Fibers Modified by Electrochemical Oxidation

Surface of polyacrylonitrile (PAN)-based carbon fibers was modified by electrochemical oxidation. The modification effect on carbon fibers surface was explored using atomic force microscopy (AFM), X-ray photoelectron spectroscopy (XPS) and X-ray diffraction (XRD). Results showed that on the modified surface of carbon fibers, the carbon contents decreased by 9.7% and the oxygen and nitrogen contents increased by 53.8% and 7.5 times, respectively. The surface roughness and the hydroxyl and carbonyl contents also increased. The surface orientation index was reduced by 1.5% which decreased tensile strength of carbon fibers by 8.1%, and the microcrystalline dimension also decreased which increased the active sites of carbon fiber surface by 78%. The physical and chemical properties of carbon fibers surface were modified through the electrochemical oxidative method, which improved the cohesiveness between the fibers and resin matrix and increased the interlaminar shear strength (ILSS) of carbon fibers reinforc     

Determination of nano-roughness of carbon fibers by atomic force microscopy

We present a novel approach to determine the surface roughness on varying scales using atomic force microscopy data. The key factor is to find a suitable background correction for the desired scale. Using the example of the surface of sized and unsized high-tenacity carbon fibers, we present an easy method to find backgrounds for widely varying scales and to evaluate respective topography and surface roughness with the same lateral resolution as the microscope itself. The analysis is done by subtracting a tunable background from the respective height data. By choosing an appropriate background to investigate the surface topography of a carbon fiber on a nm-scale, only small nano-structures with a width of around 20 nm remain after the background subtraction. Evaluating the mean roughness R _a of these nano-structures, sized carbon fibers show an overall value of around 0.1 nm while unsized carbon fibers a value of around 0.4 nm. Total background corrected height analysis shows an even distribution of these nano-structures along the fibrils of the unsized fibers, whereas for the sized fibers the nano-structures are not present. The presented method allows analysis and visualization of the distribution of nano-structures on a carbon fiber surface for the first time. This feature is used to visualize the distribution of the sizing and can further be used to investigate the influence of different production parameters on the fiber topography or to evaluate the contribution of mechanical interlocking to the interfacial strength.