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     

Studies on surface energetics of glass fabrics in an unsaturated polyester matrix system: Effect of sizing treatment on glass fabrics

The surfaces of glass fibers were sized by polyvinyl alcohol (PVA), polyester, and epoxy resin types in order to improve the mechanical interfacial properties of fibers in the unsaturated polyester matrix. The surface energetics of the glass fibers sized were investigated in terms of contact angle measurements using the wicking method based on the Washburn equation, with deionized water and diiodomethane as the wetting liquids. In addition, the mechanical behaviors of the composites were studied in the context of the interlaminar shear strength (ILSS), critical stress intensity factor (K_IC), and flexural measurements. Different evolutions of the London dispersive and specific (or polar) components of the surface free energy of glass fibers were observed after different sizing treatments. The experimental result of the total surface free energies calculated from the sum of their two components showed the highest value in the epoxy‐sized glass fibers. From the measurements of mechanical properties of composites, it was observed that the sizing treatment on fibers could improve the fiber–matrix interfacial adhesion, resulting in improved final mechanical behaviors, a result of the effect of the enhanced total surface free energy of glass fibers in a composite system. © 2001 John Wiley & Sons, Inc. J Appl Polym Sci 80: 1439–1445, 2001     

CF/纳米SiO_2改性树脂复合材料界面性能研究

本文以纳米SiO2改性树脂作为树脂基体,以连续碳纤维作为增强体制备复合材料,研究了纳米SiO2掺入树脂中百分含量对树脂基体与增强体之间的界面性能的影响。通过对树脂基体与增强体纤维浸润性、微脱粘、层间剪切强度和扫描电子显微镜,对复合材料界面性能测试和表征。结果表明,随着纳米SiO2含量的增加,常温下,基体树脂和增强体纤维浸润性能下降,单丝纤维与树脂微球的界面剪切强度和复合材料单向板层间剪切强度在某一含量范围均有所提高。     

Study on the interfacial properties of two‐dimensionally arranged glass fiber/epoxy resin model composites

The effect of interfiber distance on the interfacial properties in two dimensional multi‐E‐glass fiber/epoxy resin composites has been investigated using fragmentation test. In addition, the effect of the fiber surface treatment on the interfacial properties has been studied. We found that the interfacial shear strength decreased with the decreasing interfiber distance at the range of <50 μm and the extent of the decreasing was more serious as the increasing of the number of adjacent fiber. This is probably that the interface between the fiber and the resin was damaged by the breaking of adjacent fibers and the damage increased with minimizing the interfiber spacing and the number of adjacent fibers. We can guess that interfacial shear strength in real composites is much smaller than that of multifiber fragmentation sample with touched fiber. When the interfiber distance was >50 μm, the interfacial shear strengths were saturated regardless of fiber surface treatment and were in close agreement with those of the single fiber fragmentation test. Finally, the interfacial shear strength evaluated using two dimensional fragmentation tests are shown as real values in‐site regardless of fiber surface treatment, interfiber distance, and existing matrix cracks. © 2005 Wiley Periodicals, Inc. J Appl Polym Sci 99: 1541–1551, 2006     

The effect of silica (SiO2) nanoparticles and ammonia/ethylene plasma treatment on the interfacial and mechanical properties of carbon-fiber-reinforced epoxy composites

A nanoparticle dispersion is known to enhance the mechanical properties of a variety of polymers and resins. In this work, the effects of silica (SiO₂) nanoparticle loading (0–2 wt%) and ammonia/ethylene plasma-treated fibers on the interfacial and mechanical properties of carbon fiber–epoxy composites were characterized. Single fiber composite (SFC) tests were performed to determine the fiber/resin interfacial shear strength (IFSS). Tensile tests on pure epoxy resin specimens were also performed to quantify mechanical property changes with silica content. The results indicated that up to 2% SiO₂ nanoparticle loading had only a little effect on the mechanical properties. For untreated fibers, the IFSS was comparable for all epoxy resins. With ethylene/ammonia plasma treated fibers, specimens exhibited a substantial increase in IFSS by 2 to 3 times, independent of SiO₂ loading. The highest IFSS value obtained was 146 MPa for plasma-treated fibers. Interaction between the fiber sizing and plasma treatment may be a critical factor in this IFSS increase. The results suggest that the fiber/epoxy interface is not affected by the incorporation of up to 2% SiO₂ nanoparticles. Furthermore, the fiber surface modification through plasma treatment is an effective method to improve and control adhesion between fiber and resin.     

Improvement of interfacial interactions in CF/PEEK composites by an s-PSF/graphene oxide compound sizing agent

The interfacial interactions of carbon fiber (CF)-reinforced polymer composites is a key factor affecting the overall performance of the material. In this work, we prepared a sulfonated poly(ether sulfone)–graphene oxide mixed sizing agent to modify the interface of CF/PEEK composites and improve the interfacial properties between the PEEK matrix and CF. Results showed that the mechanical and interfacial properties of CF/PEEK composites are improved by the sizing agent. Specifically, the flexural strength, flexural modulus and interlaminar shear strength of the materials reached 847.29 MPa, 63.77 GPa, and 73.17 MPa, respectively. Scanning electron microscopy confirmed markedly improved adhesion between the resin matrix and fibers. This work provides a simple and effective method for the preparation of high-performance CF/PEEK composites, which can improve the performance of composites without degrading the mechanical property of pristine CF.     

Mechanical properties of carbon fiber composites modified with graphene oxide in the interphase

The surface topographies of carbon fibers treated by sizing agents with different graphene oxide (GO) content were investigated by scanning electron microscopy. The surface elements compositions of carbon fibers were determined by X‐ray photoelectron spectrometer. The interfacial properties of composites were studied by interfacial shear strength. The thermo‐mechanical properties of two typical specimens (CF‐G0 and CF‐G1 composites) were investigated by dynamic mechanical thermal analysis. The results showed the introduction of GO sheets on carbon fibers surfaces effectively improved the mechanical properties of carbon fibers/epoxy composites. POLYM. COMPOS., 38:2425–2432, 2017. © 2016 Society of Plastics Engineers     

Effect of quasi‐carbonization processing parameters on the mechanical properties of quasi‐carbon/phenolic composites

In this work, quasi‐carbon fabrics were produced by quasi‐carbonization processes conducted at and below 1200°C. Stabilized polyacrylonitrile (PAN) fabrics and quasi‐carbon fabrics were used as reinforcements of phenolic composites with a 50 wt %/50 wt % ratio of the fabric to the phenolic resin. The effect of the quasi‐carbonization process on the flexural properties, interfacial strength, and dynamic mechanical properties of quasi‐carbon/phenolic composites was investigated in terms of the flexural strength and modulus, interlaminar shear strength, and storage modulus. The results were also compared with those of a stabilized PAN fabric/phenolic composite. The flexural, interlaminar, and dynamic mechanical results were quite consistent with one another. On the basis of all the results, the quasi‐static and dynamic mechanical properties of quasi‐carbon/phenolic composites increased with the applied external tension and heat‐treatment temperature increasing and with the heating rate decreasing for the quasi‐carbonization process. This study shows that control of the processing parameters strongly influences not only the mechanical properties of quasi‐carbon/phenolic composites but also the interlaminar shear strength between the fibers and the matrix resin. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci, 2008     

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。     

Effects of novolac resin modification on mechanical properties of carbon fiber/epoxy composites

The epoxy resin matrix of carbon fiber (CF)‐reinforced epoxy composites was modified with novolac resin (NR) to improve the matrix‐dominated mechanical properties of composites. Flexural strength, interlaminar shear strength (ILSS), and impact strength were measured with unfilled, 7 wt% NR, 13 wt% NR, and 18 wt% NR filled to epoxy to identify the effect of adding NR on the mechanical properties of composites. The results showed that both interfacial and impact properties of composites were improved except for flexural property. The largest improvement in ILSS and impact strength were obtained with 13 wt% loading of NR. ILSS and impact strength were improved by 7.3% and 38.6%, respectively, compared with the composite without NR. The fracture and surface morphologies of the composite specimens were characterized by scanning electron microscopy. Intimate bonding of the fibers and the matrix was evident with the content of 7–13 wt% NR range. Decrease of crosslinking density and formation of NR transition layer were deduced with adding NR. POLYM. COMPOS., 2011. © 2010 Society of Plastics Engineers     

Improving the interfacial and flexural properties of carbon fiber–epoxy composites via the grafting of a hyperbranched aromatic polyamide onto a carbon fiber surface on the basis of solution polymerization

Hyperbranched aromatic polyamide (HBP) was grafted successfully onto carbon fibers (CFs) on the basis of solution polymerization to enhance the interfacial adhesion strength of CF-reinforced epoxy resin composites. The microstructure and interfacial properties of the CFs before and after decoration were researched. The results indicate that HBP was deposited uniformly onto the CFs with γ-aminopropyl triethoxysilane as the bridging agent. The active groups, roughness, and surface energy of the modified fiber [hyperbranched aromatic polyamide grafted carbon fiber (CF–HBP)] increased visibly in comparison with those of the untreated CFs. The CF–HBP composites revealed simultaneous remarkable enhancements (65.3, 34.3, and 84.8%) in their interfacial shear strength, flexural strength, and modulus, respectively; this was attributed to the improvement in the fiber–epoxy interface through enhanced chemical interactions, mechanical interlocking, and wettability. These agreed with the scanning electron microscopy observations from the fracture surface morphologies of the composites. © 2018 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2019 , 136, 47232.     

基于NOL环的高性能纤维与环氧树脂的匹配性研究

纤维与树脂的界面对复合材料的整体力学性能有着显著的影响。基于NOL环的宏观力学测试一般被用来反映复合材料的界面粘结性能,因此适用于评价纤维与树脂之间的宏观力学性能匹配性。为了探究高性能碳纤维T700SC、T800HB及高强玻璃纤维与环氧树脂的宏观力学性能匹配性,本研究首先根据GB/T 1458—2008国家标准制备NOL环试样,再借助NOL环的拉伸和层间剪切强度测试分析了高性能纤维与环氧树脂不同匹配组合宏观力学性能差异的原因,并寻找出最佳匹配组合。结果表明:玻璃纤维与环氧树脂的界面存在最佳的粘结强度,而且不同粘结强度导致拉伸强度和破坏机理不同,而碳纤维复合材料界面性能较差,容易分层破坏;T800HB与环氧树脂的宏观力学匹配性优于T700SC,环氧树脂力学性能、碳纤维的表面微观结构与性质以及环氧树脂与碳纤维之间的相互作用关系是影响界面粘结性能的根本原因。该研究在高性能纤维单向复合材料的材料选择与设计方面具有现实意义。     

Effects of silica surface treatment on the impregnation process of silica fiber/phenolics composites

Effects of silica surface treatment on the impregnation process of silica fiber/phenolics composites were studied. Micro‐Wilhelmy method was used to evaluate the surface characterization of silanized silica fibers. The interlaminar shear strength (ILSS) measurements and the void contents of the silica fiber/phenolics composites were also performed. The interactions occurring between silica fiber and the components of phenolic resin solution can affect the contact angle between silica fiber and phenolic solution and the dynamic adsorption behavior of phenolic resin onto silica fiber. There are competitive adsorptions to different extent for phenolic resin and solvent onto silica fibers. Silica fibers as reinforcement treated by silane‐coupling agent, such as γ‐aminopropyl‐triethoxysilane, γ‐glycidoxypropyl‐trimethoxysilane, trimethylchlorosilane, and γ‐methacryloxypropyl‐trimethoxysilane, influence the mechanical interfacial properties of silica fiber/phenolics composites and the uniformity of resin distribution. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci 2008     

Study on long fiber–reinforced thermoplastic composites prepared by in situ solid‐state polycondensation

Long glass fiber–reinforced thermoplastic composites were prepared by a new process, in situ solid‐state polycondensation (INSITU SSP). In this process reinforcing continuous fibers were impregnated by the oligomer of PET melt, and then the impregnated continuous fibers were cut to a desired length (designated prepreg); finally, the prepreg was in situ polymerized in the solid state to form the high molecular weight matrix. SEM, FTIR spectra, short‐beam shear stress test, flexural strength test, impact strength test, and the intrinsic viscosity measurement were used to investigate the wetting and interfacial adhesion, the mechanical properties of the composite, and the molecular weight of matrix resin in the composite. The results showed that the molecular weight of PET in the matrix resin and mechanical properties could be adjusted by controlling the SSP time and that the high level of interfacial adhesion between reinforcing fibers and matrix resin could be achieved by this novel INSITU SSP process, which are attributed to the good wetting of reinforcing fibers with low molecular weight oligomer melt as the impregnation fluid, the in situ formation of chemical grafting of oligomer chains onto the reinforcing fiber surface, and the in situ formation of the high molecular weight PET chains in the interphase regions. © 2004 Wiley Periodicals, Inc. J Appl Polym Sci 91:3959–3965, 2004     

Adhesion and Hydrolytic Stability of the Interface Between High-Modulus Polyethylene Fibers and Acrylic Resins

The effects of oxyen plasma treatment on the surface chemistry of Spectra 1000® high modulus polyethylene fibers and on the mechanical properties of fiber-reinforced composites of the fibers in a Bis-GMA based acrylic resin have been studied. X-ray photoelectron spectroscopy and diffuse reflectance FTIR spectroscopy have been used to show that the majority of oxygen on the fiber surface exists mostly in the form of ether and/or epoxy linkages, with carbonyl-, carboxylic- and ester-containing compounds accounting for less than 10 percent of the total. While the untreated and plasma-treated fibers have similar chemical compositions, the surfaces of the plasma-treated fibers are more polar and the oxygen is chemically bonded instead of being merely physisorbed. The interfacial shear strength between the fibers and the acrylic resin is increased by a factor of 2.3 by the plasma treatment indicating the presence of a weak boundary layer on the surface of the untreated fibers. The hydrolytic stability of the composite interfaces was investigated for fibers sized with several Bis-GMA-based adhesives. Maximum stability was attained by sizing with Bis-GMA containing a peroxide catalyst or an amine accelerator. The flexural properties of composites utilizing plasma-treated and untreated fibers were compared in three-point bending. The ultimate bending loads for composites using treated fibers were much higher than those for composites with untreated fibers, but only a fraction of that for glass or Kevlar®-reinforced materials.     

芳纶纤维/AFR树脂复合材料界面粘结性能的研究

为了改善芳纶纤维复合材料的界面粘结性能,合成了一种新型树脂(AFR)作为基体,以未经任何表面处理的芳纶纤维作增强材料,制备了芳纶纤维/AFR复合材料。采用测定表面能、接触角、层间剪切强度、横向拉伸性能和扫描电镜观察形貌等方法,从宏观和微观等方面研究了芳纶纤维/AFR复合材料的界面粘结性能。结果表明,AFR树脂与芳纶纤维有相近的表面能,AFR树脂溶液与芳纶纤维的接触角为42.8°,而环氧树脂(EP)与芳纶纤维的接触角为68°,说明AFR树脂对芳纶纤维的润湿性优于EP树脂;芳纶/AFR复合材料的层间剪切强度、横向拉伸强度和纵向拉伸强度分别为74.64MPa、25.34MPa和2256MPa,比芳纶/EP复合材料的相应强度分别提高了28.7%、32.5%和13.4%,其复合材料破坏面的形貌也说明芳纶纤维与AFR树脂之间的界面粘结性能较好。     

Formation of a carbon fiber/polyhedral oligomeric silsesquioxane/carbon nanotube hybrid reinforcement and its effect on the interfacial properties of carbon fiber/epoxy composites

A carbon fiber/polyhedral oligomeric silsesquioxane/carbon nanotube (CF–POSS–CNT) hybrid reinforcement was prepared by grafting CNTs onto the carbon fiber surface using octaglycidyldimethylsilyl POSS as the linkage in an attempt to improve the interfacial properties between carbon fibers and an epoxy matrix. X-ray photoelectron spectroscopy, scanning electron microscopy, dynamic contact angle analysis and single fiber tensile testing were performed to characterize the hybrid reinforcements. Interlaminar shear strength (ILSS), impact toughness, dynamic mechanical analysis and force modulation atomic force microscopy were carried out to investigate the interfacial properties of the composites. Experimental results show that POSS and CNTs are grafted uniformly on the fiber surface and significantly increase the fiber surface roughness. The polar functional groups and surface energy of carbon fibers are obviously increased after the modification. Single fiber tensile testing results demonstrate that the functionalization does not lead to any discernable decrease in the fiber tensile strength. Mechanical property test results indicate the ILSS and impact toughness are enhanced. The storage modulus and service temperature increase by 11 GPa and 17 °C, respectively. POSS and CNTs effectively enhance the interfacial adhesion of the composites by improving resin wettability, increasing chemical bonding and mechanical interlocking.     

Influence of surface treatment of carbon fibers on interfacial adhesion strength and mechanical properties of PLA‐based composites

In the present study C/PLA composites with different fiber surface conditions (untreated and with nitric acid oxidation for 4 h and 8 h) were prepared to determine the influence of surface treatment on the interfacial adhesion strength and mechanical properties of the composites. A chemical reaction at the fiber–matrix interfaces was confirmed by XPS studies. Nitric acid treatment was found to improve the amount of oxygen‐containing functional groups (particularly the carboxylic group, —COOH) on carbon fiber surfaces and to increase the surface roughness because of the formation of longitudinal crevices. The treated composites exhibited stronger interface adhesion and better mechanical properties in comparison to their untreated counterparts. There was a greater percentage of improvement in interfacial adhesion strength than in the mechanical properties. The strengthened interfaces and improved mechanical performance have been mainly attributed to the greater extent of the chemical reaction between the PLA matrix and the carbon fibers. The increased surface roughness also has had a slight contribution. © 2001 John Wiley & Sons, Inc. J Appl Polym Sci 80: 367–376, 2001     

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     

Surface modification of polyimide fibers by novel alkaline–solvent hydrolysis to form high‐performance fiber‐reinforced composites

We modified polyimide (PI) fibers by a novel hydrolysis approach and fabricated PI‐fiber‐reinforced novolac resin (NR) composites with enhanced mechanical properties. We first used an alkaline–solvent mixture containing potassium hydroxide liquor and dimethylacetamide (DMAc) for the surface modification of the PI fibers. The results indicate that the surface roughness and structure of the PI fibers were controlled by the hydrolysis time and the content of DMAc. With the optimized hydrolysis conditions, the tensile modulus of modified PI fibers improved 15% without compromises in the fracture stress, fracture strain, or thermal stability. The interfacial shear strength between the modified PI fibers and NR increased 57%; this indicated a highly enhanced interfacial adhesion. Finally, the tensile and flexural strengths of the composites increased 72 and 53%, respectively. This research provides an effective method for the surface modification of PI fibers and expands their applications for high‐performance composites. © 2018 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2018 , 135, 46595.