Surface modification of armos fibers with oxygen plasma treatment for improving interfacial adhesion with poly(phthalazinone ether sulfone ketone) resin

We introduce in this article oxygen plasma treatment as a convenient and effective method for the surface modification of Armos fibers. The effects of oxygen‐plasma‐treatment power on both the Armos fiber surface properties and Armos‐fiber‐reinforced poly(phthalazinone ether sulfone ketone) composite interfacial adhesion were investigated. The Armos fiber surface chemical composition, surface morphology and roughness, and surface wettability as a function of oxygen‐plasma‐treatment power were measured by X‐ray photoelectron spectroscopy, scanning electronic microscopy, atomic force microscopy, and dynamic contact angle analysis. The results show that oxygen plasma treatment introduced a lot of reactive functional groups onto the fiber surface, changed the surface morphology, increased the surface roughness, and enhanced the surface wettability. Additionally, the effect of the oxygen‐plasma‐treatment power on the composite interfacial adhesion was measured by interlaminar shear strength with a short‐beam bending test. Oxygen plasma treatment was an effective method for improving the composite interfacial properties by both chemical bonding and physical effects. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2011     

Surface modification of aramid fibers with γ‐ray radiation for improving interfacial bonding strength with epoxy resin

Co⁶⁰ γ‐ray radiation as a simple and convenient method for surface modification of Armos aramid fibers was introduced in this article. Two kinds of gas mediums, N₂ and air, were chosen to modify aramid fiber surface by γ‐ray irradiation. After fiber surface treatment, the interlaminar shear strength values of aramid/epoxy composites were enhanced by about 17.7 and 15.8%, respectively. Surface elements of aramid fibers were determined by XPS, the analysis of which showed that the ratio of oxygen/carbon was increased. The crystalline state of aramid fibers was determined by X‐ray diffraction instrument. The surface topography of fibers was analyzed by atomic force microscopy and scanning electron microscope. The degree of surface roughness and the wettability of fiber surface were both enhanced by γ‐ray radiation. The results indicated that γ‐ray irradiation technique, which is a suitable way of batch process for industrialization, can significantly improve the surface properties of aramid fibers reinforced epoxy resin matrix composites. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci 2007     

Interfacial studies on the surface modified aramid fiber reinforced epoxy composites

In this work, solutions of rare earth modifier (RES) and epoxy chloropropane (ECP) grafting modification method were used for the surface treatment of aramid fiber. The effect of chemical treatment on aramid fiber has been studied in a composite system. The surface characteristics of aramid fibers were characterized by Fourier transform infrared spectroscopy (FTIR). The interfacial properties of aramid/epoxy composites were investigated by means of the single fiber pull‐out tests. The mechanical properties of the aramid/epoxy composites were studied by interlaminar shear strength (ILSS). As a result, it was found that RES surface treatment is superior to ECP grafting treatment in promoting the interfacial adhesion between aramid fiber and epoxy matrix, resulting in the improved mechanical properties of the composites. Meanwhile, the tensile strengths of single fibers were almost not affected by RES treatment. This was probably due to the presence of reactive functional groups on the aramid fiber surface, leading to an increment of interfacial binding force between fibers and matrix in a composite system. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 102:4165–4170, 2006     

低温氨气等离子体对芳纶表面的改性

采用氨气等离子体对芳纶表面进行改性,用X-射线光电子能谱、场发射扫描电子显微镜、力学性能测试等手段对改性前后纤维表面的元素组成、形貌及其拉伸强度进行表征,并进一步通过微脱黏方法分析了等离子体处理条件对芳纶/环氧树脂复合材料界面黏结强度的影响。结果表明:芳纶经表面改性后,其表面极性官能团、表面粗糙度均有所增加,同时与环氧树脂基体的界面黏结强度明显增加。     

Surface ammonification of the mutual‐irradiated aramid fibers in 1,4‐dichlorobutane for improving interfacial properties with epoxy resin

The mutual irradiated aramid fibers in 1,4‐dichlorobutane was ammoniated by ammonia/alcohol solution, in an attempt to improve the interfacial properties between aramid fibers and epoxy matrix. Scanning electron microscopy (SEM), X‐ray photoelectron spectroscopy (XPS), dynamic contact angle analysis (DCA), interfacial shear strength (IFSS), and single fiber tensile testing were carried out to investigate the functionalization process of aramid fibers and the interfacial properties of the composites. Experimental results showed that the fiber surface elements content changed obviously as well as the roughness through the radiation and chemical reaction. The surface energy and IFSS of aramid fibers increased distinctly after the ammonification, respectively. The amino groups generated by ammonification enhanced the interfacial adhesion of composites effectively by participating in the epoxy resin curing. Moreover, benefited by the appropriate radiation, the tensile strength of aramid fibers was not affected at all. © 2017 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2017 , 134, 44924.     

The effect of atmospheric‐pressure air plasma discharge power on adhesive properties of aramid fibers

After exposure to the atmospheric‐pressure air plasma at different discharge powers, the adhesion characteristics of Twaron aramid fibers were investigated. For the 12 s‐300 W plasma treatment, the interlaminar shear strength of Twaron fiber reinforced thermoplastic poly(phthalazinone ether sulfone ketone) was increased from 46.0 to 61.7 MPa by 34.1%, and the diffusion of water molecule into the resulting composites was proved to be effectively prevented. These results showed that surface adhesive properties of the plasma‐treated aramid fibers were improved. At the power level of 300 W, X‐ray photoelectron spectroscopy analysis revealed the increases in concentrations of oxygen and nitrogen polar groups on the fiber surface, and atomic force microscopy observations led to the conclusion that the fiber surface morphology was changed and the surface roughness was greatly increased. These new polar and irregular surface structures accounted for the better adhesion between the fiber and the matrix, while due to the reasonability of this discharge power level applied to the surface modification, the measured fiber tensile strength only decreased by 2.0%. POLYM. COMPOS., 37:620–626, 2016. © 2014 Society of Plastics Engineers     

DBD等离子体改性芳纶表面的动态工艺研究

采用介质阻挡放电(DBD)空气等离子体,选择不同放电强度及处理时间对芳纶表面进行连续动态处理。通过扫描电镜以及光电子能谱仪对处理前后芳纶表面进行表征。结果表明,经DBD等离子体处理后的芳纶表面粗糙度有较大提高,浸润性显著提高,且纤维表面C元素质量分数下降超过5%,0元素质量分数约上升8%;芳纶表面的粗糙度、浸润性及含氧基团含量均随放电强度和处理时间的增加而提高。     

介质阻挡放电等离子体处理芳纶的表面性能研究

采用介质阻挡放电(DBD)装置对芳纶1414表面进行改性处理,探讨低温等离子体处理对纤维表面性能的影响。结果表明:经过DBD等离子体处理后,芳纶1414纤维表面粗糙程度加剧,粘结性能和浸润性能有了明显的改善;当DBD等离子体处理功率为200～300 W,时间为60 s,氩气流量为2～3 L/min时,芳纶1414的界面剪切强度从处理前的11.9 MPa上升到14.2 MPa,接触角由处理前的85.0°下降到了60.6°。     

芳纶纤维增强树脂基复合材料的界面粘结性能研究

为了改善芳纶纤维增强树脂基复合材料的界面粘结性能,从树脂基体入手,依据相似相容原理和芳纶的结构特点,合成出新型热固性树脂(AFR–T)用作芳纶复合材料的基体,以未经表面处理的芳纶作增强材料,采用热压成型法制备了AFR–T/芳纶纤维复合材料,并通过测定溶度参数、接触角、线膨胀系数、层间剪切强度(ILSS)和横向拉伸强度等方法研究了复合材料的界面粘结性能。结果表明,AFR–T树脂浇注体与芳纶的溶度参数相近,AFR–T树脂溶液在芳纶纸表面的接触角为36.9°,小于环氧树脂(EP)溶液与芳纶纸的接触角(53.2°),说明AFR–T树脂对芳纶的浸润性优于EP;AFR–T/芳纶纤维复合材料的ILSS和横向拉伸强度为73.0 MPa和25.3 MPa,分别比EP/芳纶纤维复合材料提高了25.9%和32.5%,这表明AFR–T树脂与芳纶纤维之间的浸润性和界面粘结性能较好。     

空气等离子体处理芳纶纤维及其与天然橡胶/乳聚丁苯橡胶的黏合性能

考察了空气等离子体处理对芳纶纤维表面结构形态的影响,研究了空气等离子体和间苯二酚-甲醛-胶乳(RFL)浸胶处理芳纶纤维与天然橡胶(NR)/乳聚丁苯橡胶(ESBR)的黏合性能,并对经处理的芳纶纤维与NR/ESBR体系的界面层作了动态力学分析。结果表明,芳纶纤维经空气等离子体处理后,表面粗糙度增大,表面积增加,结晶度减小,但处理功率过大、处理时间过长时,芳纶纤维的表面又变得比较光滑、结晶度又呈增大趋势。随着等离子体处理时间的延长,芳纶纤维与NR/ESBR的黏合性能增强,但处理时间过长时,芳纶纤维与NR/ESBR的黏合性能下降;等离子体处理芳纶纤维经RFL进一步浸胶处理后,芳纶纤维与NR/ESBR的黏合性能大幅度提高。芳纶纤维与NR/ESBR的界面存在介于高模量芳纶纤维和低模量橡胶之间的过渡层。     

RETRACTED ARTICLE: Surface modification of aramid fibers with novel chemical approach

Friedel–Crafts Reaction as a simple and convenient approach to the surface modification of aramid fiber was introduced in this paper. Epoxy chloropropane was chosen as the treatment reagent to modify aramid fibers surface via Graft reaction. After the modification, the interfacial properties of aramid/epoxy composites were investigated by the single fiber pull-out test (SFP), and the mechanical properties of aramid fibers were investigated by the tensile strength test. The results showed that the interfacial shear strength (IFSS) value of aramid/epoxy composites was enhanced by about 50%, and the tensile strength of aramid fibers had no obvious damage. The crystalline state of aramid fibers was determined by X-ray diffraction instrument (XRD), and the results showed that there were not any distinct crystal type varieties. The surface elements of aramid fibers were determined by X-ray photoelectron spectroscopy (XPS), the analysis of which showed that the oxygen/carbon ratio of aramid fiber surface increased obviously. The possible changes of the chemical structure of aramid fibers were investigated via Fourier transform infrared spectrum (FTIR), and the analysis of which showed that the epoxy functional groups were grafted into the molecule structure of aramid fibers. The surface morphology of aramid fibers was analyzed by Scanning electron microscope (SEM), and the SEM results showed that the physical structure of aramid fibers was not etched or damaged obviously. The surface energy of aramid fibers was investigated via the dynamic capillary method, and the results showed that the surface energy was enhanced by 31.5%, and then the wettability degree of aramid fiber surface was enhanced obviously too. All of the results indicated that this novel chemical modification approach not only can improve the interfacial bonding strength of aramid/epoxy composites remarkably, but also have no negative influence on the intrinsic tensile strength of aramid fibers.     

Effect of ultrasound on wettability between aramid fibers and epoxy resin

Good wetting of reinforced fiber by resin was a main factor in the improvement of the interface adhesion of their composites. Ultrasound with a frequency of 20 kHz was used to improve the wettability between aramid fibers and epoxy resin during the winding process of the composites. The effects of ultrasound on the viscosity and surface tension of epoxy resin and on the surface characteristics of aramid fibers were investigated. The wettability of aramid fibers and treated epoxy resin under different conditions and of aramid fibers and epoxy resin under ultrasonic online treatment were compared. The results indicated that the main action of ultrasound was to force epoxy resin to impregnate aramid fibers, in addition to the influence of ultrasound on the properties of epoxy resin and aramid fibers. The results of microdebond testing showed that the interfacial shear strength (IFSS) of aramid/epoxy composites could be 26% higher than that of untreated composites because of the improved wettability between aramid fibers and epoxy resin subjected to ultrasonic online treatment. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci, 2006     

低温等离子体改性芳纶1414的研究

对芳纶1414进行低温等离子体表面改性以改善其构成复合材料时的界面黏结性能。设计正交试验,得到低温等离子体处理芳纶1414的最佳条件为放电功率100 W,处理时间300 s,放电压强20 Pa。采用电子单纤维强力机、纤维摩擦因数测定仪、纤维接触角测量仪、扫描电子显微镜和傅里叶变换红外光谱仪对改性前后的芳纶1414进行性能表征。结果表明:经过低温等离子体改性的芳纶1414的断裂强力较原样下降了6.3%,静摩擦因数上升了15.7%,表面接触角减小了36.8%,纤维表面出现微小均匀的凹槽,增大了比表面积,引入了自由基团,增大了表面反应活性,从而改善了与树脂基体复合时的黏结强度。     

介质阻挡放电在芳纶表面改性中的应用

综述了介质阻挡放电应用于芳纶表面改性研究的最新进展;介绍了介质阻挡放电的机理、特点以及国内主要的介质阻挡放电等离子体的设备;阐述了介质阻挡放电对芳纶亲水性能和粘结性能等表面性能的改善。指出芳纶等离子体表面改性的时间效应限制了其广泛应用,应进一步加强纤维表面等离子体改性的机理研究。     

磷酸酯偶联剂改性芳纶纤维增强聚丙烯复合材料的性能研究

采用磷酸酯偶联剂对芳纶纤维表面进行接枝改性,研究了实验条件和纤维含量对芳纶纤维增强聚丙烯(PP)复合材料力学性能的影响,并用电子扫描显微镜观察了PP复合材料的微观形态结构。结果表明:磷酸酯偶联剂成功接枝到芳纶纤维表面上,使芳纶纤维和PP的界面黏结性能得以明显改善。芳纶纤维可以显著地提高PP复合材料的力学性能当,其含量为20%时复,合材料的综合性能最优。     

等离子体处理对芳纶性能的影响

芳纶作为增强材料在复合材料中有广泛的应用,其界面性能是影响其复合材料界面粘结性能的重要因素。分别采用H2、空气低温等离子体对芳纶表面进行了处理。研究了等离子体表面改性后芳纶性能的变化。结果表明:经低温等离子体处理后纤维表面张力增大,由46.0mN·m-1增加到63.2mN·m-1;表面极性增强,极性分数由58.0%提高到69.9%,而纤维单丝断裂强度未有明显变化。     

Interfacial behavior of high performance organic fibers

The surface and interfacial properties of different high performance fibers of current interest have been analyzed. The pyridobisimidazole fiber M5 shows a markedly higher polar contribution to its surface free energy than the rest of the organic fibers under study. Interfacial shear strength (IFSS) values measured by means of the microdroplet test indicate that M5 fiber has an IFSS that doubles that of the Kevlar fibers, in agreement with the observed results from surface free energy tests. Armos fiber, a para-aramid material that incorporates imidazole functional groups, shows an average IFSS 30-35% higher than the Kevlar fibers. SEM micrographs of failed microdroplet specimens show different failure mechanisms for the Kevlar KM2, Armos and M5 fibers. The KM2 specimens fail due to complete detachment of surface fibrils from the bulk of the fiber, while Armos specimens fail by the combined effect of microfibrillation on the fiber surface coupled with adhesive failure. In contrast, M5 microdroplet specimens exhibit failure surfaces consisting of partial matrix yielding during droplet debonding, indicative of the high level of interfacial bonding to the surface and higher levels of hydrogen bonding within the fiber that suppress microfibrillation. The higher polar character of the M5 surface can lead to the presence of an interphase region with different mechanical properties from the bulk matrix.     

Effect of rare earth elements surface treatment on tensile properties of aramid fiber‐reinforced epoxy composites

Solutions of rare earth modifier (RES) and epoxy chloropropane (ECP) grafting modification method were used for the surface treatment of aramid fiber. Tensile properties of both the aramid/epoxy composites and single fibers were tested. The effects of RES concentration on tensile properties of aramid/epoxy composites were investigated in detail to explore an optimum amount of rare earth elements in solution for modifying aramid fiber. The fracture surface morphologies of tensile specimens were observed and analyzed with the aid of SEM. The experimental results show that rare earth treatment is superior to ECP grafting treatment in promoting interfacial adhesion between the aramid fiber and epoxy matrix. Meanwhile, the tensile strengths of single fibers were almost not affected by RES treatment. The optimum performance is obtained when the content of rare earth elements is 0.5 wt %. © 2004 Wiley Periodicals, Inc. J Appl Polym Sci 92: 1037–1041, 2004     

Argon low‐temperature plasma modification of chopped aramid fiber and its effect on paper performance of aramid sheets

Chopped aramid fiber was modified by an argon low‐temperature plasma treatment to enhance the interfacial strength of aramid paper. The water contact angle of the aramid fiber and the tensile strength, tearing strength, and evenness of the aramid sheets were investigated under different conditions, and the parameters of the argon low‐temperature plasma modification, like gas pressure, discharge power, and discharge time, were optimized. The chemical structure and surface morphology of the fiber after plasma modification were characterized by X‐ray photoelectron spectroscopy, atomic force microscopy, and scanning electron microscopy. The strengthening mechanism of aramid paper by low‐temperature plasma modification was also studied. It was found that the argon low‐temperature plasma treatment introduced some new polar groups onto the fiber surface and increased the fiber surface wettability and roughness. © 2017 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2017 , 134, 45215.     

Influence of oxygen plasma treatment parameters on the properties of carbon fiber

This study is focused on the impact of oxygen plasma treatment on properties of carbon fibers and interfacial adhesion behavior between the carbon fibers and epoxy resin. The influences of the main parameters of plasma treatment process, including duration, power, and flow rate of oxygen gas were studied in detail using interlaminar shear strength (ILSS) of carbon fiber composites. The ILSS of composites made of carbon fibers treated by oxygen plasma for 1 min, at power of 125 W, and oxygen flow rate of 100 sccm presented a maximum increase of 28% compared to composites made of untreated carbon fibers. Furthermore, carbon fibers were characterized by scanning electron microscopy (SEM), tensile strength test, attenuated total reflectance Fourier transform infrared (ATR-FTIR), and Raman spectroscopy analyses. It was found that the concentration of reactive functional groups on the fiber surface was increased after the plasma modification, as well the surface roughness, which finally improved the interfacial adhesion between carbon fibers and epoxy resin. However, high power and long exposure times could partly damage the surface of carbon fibers and decrease the tensile strength of filaments and ILSS of treated fiber composites.