Improvement of Interfacial Adhesion of Glass Fiber/Epoxy Composite by Using Plasma Polymerized Glass Fibers

This study intends to produce plasma polymer thin films of γ-glycidoxypropyltrimethoxysilane (γ-GPS) on glass fibers in order to improve interfacial adhesion of glass fiber-reinforced epoxy composites. A low frequency (LF) plasma generator was used for the plasma polymerization of γ-GPS on the surface of glass fibers at different plasma powers and exposure times. X-ray photoelectron spectroscopy (XPS) and SEM analyses of plasma polymerized glass fibers were conducted to obtain some information about surface properties of glass fibers. Interlaminar shear strength (ILSS) values and interfacial shear strength (IFSS) of composites reinforced with plasma polymerized glass fiber were evaluated. The ILSS and IFSS values of non-plasma polymerized glass fiber-reinforced epoxy composite were increased 110 and 53%, respectively, after plasma polymerization of γ-GPS at a plasma power of 60 W for 30 min. The improvement of interfacial adhesion was also confirmed by SEM observations of fractured surface of the composites.     

Graphite fiber-epoxy interphase modification by electrodeposition of poly(styrene-co-maleic anhydride) and its influence on composite properties

An electrodeposition technique has been used for the modification of the fiber-matrix interphase in graphite fiber-epoxy composites. A coating of poly(styrene-co-maleic anhydride) (SMA) polymer was electrodeposited from an aqueous solution on AU graphite fibers used as electrodes in an electrolytic cell. Different electrocoating parameters were initially used to establish the optimum conditions to achieve thin uniform coatings suitable for functioning as interphases in composites reinforced by the coated fibers. The interfacial shear strength (IFSS), evaluated by a single-fiber composite technique, showed that the SMA coating resulted in an improvement of about 50% in IFSS compared with the commercially treated fibers (AS). This was achieved without sacrificing impact strength. Evidence of good epoxy penetration into the coating was obtained by the use of electron microprobe line scans for bromine across the diameter of a filament in a single fiber composite-the bromine introduced through the use of a brominated epoxy resin. The observed improvement in the fiber-matrix interfacial shear strengths is dependent on the co-monomer ratio in electrodeposited SMA.     

Improvement of the interfacial adhesion between PBO fibers and PPESK matrices using plasma‐induced coating

This work deals with the plasma‐induced coating process on the surface of PBO fibers to obtain a strong interfacial adhesion between the poly(p‐phenylene benzobisoxazole) (PBO) fibers and the poly(phthalazinone ether sulfone ketone) (PPESK) matrices. The process consisted of four steps: (a) plasma preactivation of PBO fibers; (b) immersion in an epoxy resin solution; (c) drying and then soaking with the PPESK solution; (d) shaped by compression molding technique. The orthogonal experiments used in this study enable the determination of the significant experimental parameters that influence efficiency of the process by comparing the values of ILSS. The order of their influences was the concentration > power > treating time > treating pressure. The results of the interlaminar shear strength (ILSS) and water absorption showed that the ILSS of the composite increased by 56.5% after coating, meanwhile the water absorption declined to 0.32%. The changes of the surface chemical composition, the surface morphology, and the surface free energy of fibers were studied by FTIR spectroscopy, atomic force microscope (AFM), and dynamic contact angle analysis (DCAA), respectively. Fracture mechanism of the composite was examined by scanning electron microscope (SEM). The results indicated that plasma‐induced coating process was an efficient method to enhance the interfacial adhesion of PBO fibers and PPESK matrices. © 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2012     

炭纤维表面处理对CF／PMR—15复合材料力学性能的影响

研究了炭纤维表面不同处理方法对复合材料力学性能的影响,采用等离子体和等离子体接枝技术对炭纤维表面进行处理后,CF／PMR－15复合材料的界面剪切强度与层间剪切强度均有所提高,随着界面状态的改善,界面剪切强度提高的幅度比层间剪切强度提高的大,本文为指导炭纤维的表面处理,评价处理效果,进一步预报复合材料的宏观性能打下了基础。     

Evaluation of interfacial properties and microfailure mechanisms in single fiber‐reinforced epoxy composites at low temperature

In this preliminary study, micromechanical techniques were used to compare the interfacial properties of both carbon and glass fiber composites with two structurally different epoxy matrices (YD‐114 and YDF‐175) at ambient and relatively low temperatures (25°C and −10°C). Tensile modulus of elasticity for both epoxies was higher at lower temperature. Although both fibers exhibited more bimodality at lower temperature than at ambient temperature, glass fiber composites exhibited a statistically greater improvement in tensile strength. This may be attributed to differences in inherent flaws and rigidity. A decrement in stress was observed for YDF‐175 epoxy composites under cyclic loadings at both temperatures, which was attributed to lower interfacial shear strength (IFSS). In contrast to the IFSS of conventional YD‐114 epoxy composites, the IFSS of both the carbon and glass fibers/YDF‐175 epoxy composites studied was higher at the lower temperature. The microfailure pattern observed in microdroplet pullout tests was consistent with the other IFSS results. POLYM. COMPOS., 2012. © 2011 Society of Plastics Engineers     

热处理温度对PBO纤维性能的影响

PBO纤维因其具有高强度、高模量、高耐热性以及高化学稳定性等性能而被公认为目前综合性能最好的有机纤维。对自制的初生PBO纤维分别在500℃、550℃、600℃、650℃和700℃进行高温热处理,并对处理后纤维的力学性能、耐热性能、表面形貌以及界面性能进行测试。结果表明,500℃下热处理后PBO纤维拉伸强度最大为4.72GPa,随着热处理温度升高,纤维的力学性能下降;600℃下热处理后PBO纤维的初始分解温度最高为641.3℃;随着热处理温度的提高,PBO纤维的表面粗糙度在增加,同时其界面剪切强度(IFSS)也随着温度的升高而增大。     

Surface modification of PBO fibers by argon plasma and argon plasma combined with coupling agents

The methods of argon plasma and argon plasma combined with coupling agents were employed to modify the poly[1,4‐phenylene‐cis‐benzobisoxazole] (PBO) fiber surface. The interfacial shearing strength (IFSS) of PBO fibers/epoxy resin was measured by the single fiber pull‐out test. The surface chemical structure and surface composition of PBO fibers were determined by FTIR and X‐ray photoelectron spectroscopy respectively. The morphology of the fiber surface was investigated by scanning electron microscopy and the specific surface area of the fibers was calculated by B.E.T. equation. Furthermore, the wettability of PBO fibers was confirmed by the droplet profile analysis method. The results showed that the elemental composition ratio of the fiber surface changed after the modification. The IFSS increased by 42 and 78% when the fibers were treated by argon plasma and argon plasma combined with the coupling agents, respectively. Meanwhile, the specific surface areas of the treated fibers were improved. In addition, compared with the modification of argon plasma, the modification of argon plasma combined with the coupling agents inhibited the attenuation phenomena of the IFSS and the wettability. © 2006 Wiley Periodicals, Inc. J Appl Polym Sci 102: 1428–1435, 2006     

The interfacial strength and fracture characteristics of ethanol and polymer modified carbon nanotube fibers in their epoxy composites

Carbon nanotube (CNT) fibers spun from CNT arrays were used as the reinforcement for epoxy composites, and the interfacial shear strength (IFSS) and fracture behavior were investigated by a single fiber fragmentation test. The IFSS between the CNT fiber and matrix strongly depended on the types of liquid introduced within the fiber. The IFSS of ethanol infiltrated CNT fiber/epoxy varied from 8.32 to 26.64 MPa among different spinning conditions. When long-molecule chain or cross-linked polymers were introduced, besides the increased fiber strength, the adhesion between the polymer modified fiber and the epoxy matrix was also significantly improved. Above all, the IFSS can be up to 120.32 MPa for a polyimide modified CNT fiber, one order of magnitude higher than that of ethanol infiltrated CNT fiber composites, and higher than those of typical carbon fiber/epoxy composites (e.g. 60–90 MPa). Moreover, the composite IFSS is proportional to the tensile strength and modulus of the CNT fiber, and decreases with increasing fiber diameter. The results demonstrate that the interfacial strength of the CNT fiber/epoxy can be significantly tuned by controlling the fiber structure and introducing polymer to optimize the tube–tube interactions within the fiber.     

Carbon nanotubes grafting PBO fiber: A study on the interfacial properties of epoxy composites

To improve the interfacial performance of poly[p‐phenylene benzobisoxazole] (PBO) fiber and epoxy resin, a modified multiwalled carbon nanotubes (MWCNTs‐Ecp) were used to achieve this purpose through grafting onto PBO fiber surface using a gamma ray radiation method. Experimental results indicated that the equilibrium wetting rate and equilibrium adsorption amount of the modified PBO fiber for epoxy resin and acetone were all higher than that of as received PBO fiber. The interfacial shear strength (IFSS) of single fiber composite increased from 31.4 to 77.5 MPa after modification. The fracture models of composites are changed from pure interfacial failure to combination failure of interface and resin interlayer. POLYM. COMPOS., 2012. © 2012 Society of Plastics Engineers     

Structures and properties of HMPBO fibers treated by oxygen plasma/polyhedral oligomeric silsesquioxane

The surface of high modulus poly(p‐phenylene‐2,6‐benzobisoxazole) (HMPBO) fibers were treated by the combination method of oxygen plasma/polyhedral oligomeric silsesquioxane (POSS). The chemical compositions and surface morphologies of HMPBO fibers were characterized by Fourier transform infrared, X‐ray photoelectron spectroscopy, thermogravimetric analyzer, and scanning electron microscopy. The interfacial shearing strength (IFSS) of the HMPBO/cyanate ester (HMPBO/CE) micro‐composites was measured by single fiber pull out test. Results showed that the POSS was grafted on the surface of HMPBO fibers, and the grafting amount was about 0.82 wt%. After the treatment, the HMPBO fibers became coarser and the diameter was also increased. Compared with that of pure HMPBO/CE micro‐composites, the IFSS of treated HMPBO/CE micro‐composites was increased by 20.7%. POLYM. COMPOS., 34:2026–2030, 2013. © 2013 Society of Plastics Engineers     

Effect of solubility and miscibility on the adhesion behavior of polymer‐coated carbon fibers with vinyl ester resins

Interfacial shear strength (IFSS) of carbon fibers with vinyl ester resin was investigated as a function of the structure of the polymer coating on carbon fibers via microdroplet tests. For coating carbon fibers, high‐performance polymers such as poly(arylene ether phosphine oxide) (PEPO), Udel® P‐1700, and Ultem® 1000, water‐soluble poly(hydroxy ether ethanol amine) (PHEA), water‐dispersed carboxy‐modified poly(hydroxy ether) (C‐PHE), and water‐insoluble poly(hydroxy ether) (PHE) were utilized. Adhesion of polymers to carbon fibers was also evaluated and the failure surface of the fibers was analyzed by SEM to understand the adhesion mechanism. Diffusion between polymers and vinyl ester resins was investigated and the solubility parameters of the polymers were calculated, with the results being correlated to the IFSS. A highly enhanced IFSS was obtained with PEPO coating, while marginally improved IFSS resulted from PHE, Udel®, and C‐PHE coatings. However, PHEA and Ultem® coatings showed no improvement. Such results were attributed to the extent of solubility and/or miscibility of polymer coatings in vinyl ester resin, with better solubility and miscibility leading to a higher IFSS. © 2000 John Wiley & Sons, Inc. J Appl Polym Sci 79: 1042–1053, 2001     

Preparation and characterization of the modulus intermediate layer in carbon fiber/epoxy composites by depositing sepiolites

An important aspect in development of multi‐scale reinforced composites is their mass production which can be easily realized. In this article, the sepiolites (Si12O30Mg8(OH)4(OH2)4·8H2O) are directly deposited onto the surface of JH‐T800 carbon fibers for the first time with no need for removal of the commercial sizing agent. The sepiolites adhering to the carbon fibers are uniformly distributed with random orientation, and participated in the formation of high modulus intermediate layer encompassing the carbon fiber. After the deposition of sepiolites, the interfacial shear strengths (IFSS) of the carbon fiber/epoxy composites are significantly improved as shown in single‐fiber composite fragmentation tests. Compared to the commercial carbon fiber composites, the sepiolite‐deposited fiber composites also exhibit obvious improvement in the interlaminar shear strength and flexural strength. As a new kind of multi‐scale reinforcement with industrial application value, the sepiolite‐deposited carbon fibers can further raise the level of mechanical properties of the existing carbon fiber reinforced composites. © 2016 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2016 , 133, 43955.     

Temperature effect on graphene‐filled interface between glass–carbon hybrid fibers and epoxy resin characterized by fiber‐bundle pull‐out test

The overall mechanical performance of glass–carbon hybrid fibers reinforced epoxy composites depends heavily upon fiber–matrix interfacial properties and the service temperatures. Fiber‐bundle pull‐out tests of glass (GF) and/or carbon fiber (CF) reinforced epoxy composites were carried out at room and elevated temperatures. Graphene nanoplatelets were added in the interfacial region to investigate their influence on the interfacial shear strength (IFSS). Results show that IFSS of specimens with fiber‐bundle number ratio of GF:CF = 1:2 is the largest among the hybrid composites, and a positive hybridization effect is found at elevated temperatures. IFSS of all the specimens decreases with the increasing of test temperatures, while the toughness shows a contrary tendency. As verified by scanning electron microscopy observations, graphene nanoplatelets on fiber surface could enhance the IFSS of pure glass/carbon and hybrid fibers reinforced epoxy composites at higher temperatures significantly. © 2018 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2018 , 135, 46263.     

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.     

Electrostatic deposition of silica nanoparticles between E‐glass fibers and an epoxy resin

The achievement of optimum adhesion between a thermoset and an inorganic material is an important goal for the composites and coatings industries. There is a growing interest in the use of structural surface modifiers, such as nanotubes, nanoparticles, and whiskers, to improve this adhesion. Here, a method for electrostatically depositing poly(ethylene imine)‐functionalized silica nanoparticles onto E‐glass fibers was developed. The deposition of 26‐nm functionalized particles onto glycidyloxypropyltrimethoxysilane (GPS)‐functionalized E‐glass fibers and then their embedding in a resin of diglycidyl ether of bisphenol A and m‐phenylene diamine increased the interfacial shear strength (IFSS) 35% over that of bare fibers and 8% over that of GPS‐functionalized fibers. IFSS was highly dependent on the particle size; the 16‐nm functionalized particles had little effect on the IFSS. When the particles size was increased to 71 and 100 nm, this led to increasingly poor IFSS values, whereas the 26‐nm particles produced the best results. Similar results were seen with the transverse flexural strength of the unidirectional composites. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 41516.     

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.     

Influence of oxygen plasma treatment on interfacial properties of poly(p‐phenylene benzobisoxazole) fiber‐reinforced poly(phthalazinone ether sulfone ketone) composite

The influence of oxygen plasma treatment on both surface properties of poly(p‐phenylene benzobisoxazole) (PBO) fibers and interfacial properties of PBO fiber reinforced poly(phthalazinone ether sulfone ketone) (PPESK) composite were investigated. Surface chemical composition, surface roughness, and surface morphologies of PBO fibers were analyzed by X‐ray photoelectron spectroscopy (XPS), Atomic force microscopy (AFM), and scanning electron microscopy (SEM), respectively. Surface free energy of the fibers was characterized by dynamic contact angle analysis (DCAA). The interlaminar shear strength (ILSS) and water absorption of PBO fiber‐reinforced PPESK composite were measured. Fracture mechanisms of the composite were examined by SEM. The results indicated that oxygen plasma treatment significantly improved the interfacial adhesion of PBO fiber‐reinforced PPESK composite by introducing some polar or oxygen‐containing groups to PBO fiber surfaces and by fiber surface roughening. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2009     

Enhanced interfacial adhesion via interfacial crystallization between sisal fiber and isotactic polypropylene: direct evidence from single‐fiber fragmentation testing

Bioresource natural sisal fiber (SF) was used to prepare single fiber‐reinforced isotactic polypropylene (iPP) composites. Three kinds of interfacial crystalline morphologies, spherulites, medium nuclei density transcrystallinity (MD‐TC) and high nuclei density transcrystallinity (HD‐TC), were obtained in the single fiber‐reinforced composites by implementing quiescent or dynamic shear‐enhanced crystallization and by modulating the compatibility interaction between SF and iPP. The development of interfacial shear strength (IFSS) during the interfacial crystallization process was demonstrated for the first time using a combination of single‐fiber fragmentation testing and optical microscope observation. A close correlation between IFSS and morphological characteristics of interfacial crystallization was well elucidated. The increases in IFSS were very different for spherulitic, MD‐TC and HD‐TC morphologies. The highest IFSS obtained was 28 MPa, after the formation of HD‐TC, which was about 62% of the tensile strength of neat iPP (45 MPa). These results offer powerful and direct evidence that interfacial crystallization could play an important role in the enhancement of interfacial adhesion of real SF/iPP composites. © 2013 Society of Chemical Industry     

The influence of the interphase on composite properties: Poly(ethylene-co-acrylic acid) and poly(methyl vinyl ether-co-maleic anhydride) electrodeposited on graphite fibers

The electrodeposition of saturated copolymers onto carbon fibers is investigated, focusing particular attention on improvement of shear and impact properties of the corresponding composites. Carbon fibers are electrocoated with poly(ethylene-co-acrylic acid) and poly(methyl vinyl ether-co-maleic anhydride) from aqueous media, and fabricated into epoxy composites. The results of interlaminar shear strength (ILSS) tests, initially employed to assess fibermatrix adhesion, are vitiated by the occurrence of mixed-mode failure. Interfacial shear strength (IFSS) is hence evaluated by stressing single-fiber composite specimens to obtain ultimate aspect ratios of the fiber fragments. The data are combined with fiber strengths by a recently developed statistical theory (1) to yield a distribution for IFSS. Both copolymer interphases improve fiber-matrix bonding to an extent greater even than that obtained with commercial fiber surface treatment. Good fiber-matrix adhesion is further apparent from SEM studies of fractured ILSS test specimens. A key to this improved adhesion is the interpenetration of matrix resin and interphase polymer, revealed by electron microprobe analysis (2). Notched Izod impact strength is also increased over uncoated-fiber composites. These copolymer interphases behave as deformable interlayers, absorbing impact energy and blunting the growing crack tip. Further energy is absorbed in deflecting the crack through a more tortuous path. Simultaneous improvements in impact and shear strengths are thus obtained, which may be further enhanced by optimizing the electrodeposition parameters and the coating thickness. The influence of the interphase on composite properties is better understood from this study, paving the way for refinement in interphase design.     

Improvement of interfacial shear strengths of polybenzobisoxazole fiber/epoxy resin composite by n‐TiO2 coating

Smooth polybenzobisoxazole (PBO) fiber has limited interfacial interaction with resin matrix. In this article, nano‐TiO₂ coating on PBO fiber is applied to improve the interfacial adhesion between PBO fiber and epoxy resin. The test results suggest that the PBO fiber had good interaction with epoxy resin matrix after its treatment with n‐TiO₂ sol. Nano TiO₂ particle embedded onto PBO fiber surface, acting as a chock, which made fiber implanted into the resin better. This greatly improved the shear strengths (IFSS) of PBO fiber/epoxy resin composite. It has been found that a 56% increase in interfacial IFSS has achieved without sacrificing mechanical properties of fiber. © 2012 Wiley Periodicals, Inc. J. Appl. Polym. Sci., 2013