The effective interfacial shear strength of carbon nanotube fibers in an epoxy matrix characterized by a microdroplet test

The tensile properties of continuous carbon nanotube (CNT) fibers spun from a CNT carpet consisting of mainly double- and triple-walled tubes, and their interfacial properties in an epoxy matrix, are investigated by single fiber tensile tests and microdroplet tests, respectively. The average CNT fiber strength, modulus and strain to failure are 1.2 ± 0.3 GPa, 43.3 ± 7.4 GPa and 2.7 ± 0.5%, respectively. A detailed study of strength distribution of CNT fiber has been carried out. Statistical analysis shows that the CNT fiber strength is less scattered than those of MWCNTs as well as commercial carbon and glass fibers without surface treatment. The effective CNT fiber/epoxy interfacial shear strength is 14.4 MPa. Unlike traditional fiber-reinforced composites, the interfacial shear sliding occurs along the interface between regions with and without resin infiltration in the CNT fiber. Guidelines for microdroplet experiments are established through probability analysis of variables basic to specimen design.     

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.     

淀粉纳米晶对玻璃纤维的表面改性研究

采用自制的淀粉纳米晶(SNC)对玻璃纤维进行表面处理,增加其与环氧树脂基体的界面剪切强度(IFSS)。研究了处理方式、处理时间、SNC乙醇分散液浓度、热处理温度等工艺参数对SNC在玻璃纤维表面沉积情况的影响,以及对改性玻璃纤维与环氧树脂的界面性能的影响规律。采用扫描电子显微镜、单纤维强力仪对处理前后玻璃纤维进行表征,并采用微脱粘法测试玻璃纤维与环氧树脂的界面粘结情况。结果表明,当重力静置处理时间24 h,SNC乙醇分散液浓度为1 g/100 m L时,SNC在玻璃纤维表面均匀沉积,且能显著提高玻璃纤维与环氧树脂的IFSS,为27.29 MPa,较未处理的纤维增加29.3%。150℃热处理4 h后,X射线光电子能谱结果显示SNC与玻璃纤维形成化学键合,进一步增加纤维与环氧树脂的界面粘结,IFSS值达到32.30 MPa,较未处理的纤维增加53%,且纤维的拉伸强度得到较好的维持。     

微脱黏法在碳纤维/环氧树脂界面性能评价中的应用

利用微脱黏法测定碳纤维/环氧树脂复合材料的界面剪切强度,并分析了造成测试结果分散的影响因素.结果表明:在脱黏过程中,最大脱黏力随碳纤维埋人环氧树脂内长度的增加而线性递增,当埋人长度超过一定值后最大脱黏力趋于稳定:碳纤维与环氧树脂间的接触角对复合材料界面剪切强度有一定影响,接触角越大,界面剪切强度越高;测试结果的分散性与树脂微球的半月板区域、钳口区等因素有关;未经表面处理的碳纤维增强环氧树脂复合材料的界面剪切强度仪为39.4 MPa,低于处理后的复合材料(60.6 MPa).     

Experimental evaluation of the interfacial properties of carbon nanotube coated carbon fiber reinforced hybrid composites

A floating catalyst chemical vapor deposition (CVD) unit was utilized to grow CNT onto the surface of carbon fiber (CF). The surface morphology of the resultant fibers, CNT population density and alignment pattern were found to be depended on the CNT growth temperature, growth time, and atmospheric conditions within the CVD chamber. In contrast to the neat‐CF reinforced composites, improved interfacial shear strength (IFSS) between CF and matrix were obtained when the surface of CF was coated by CNT. Particularly, CF treatment condition for CNT‐coating with 700°C reaction temperature and 30 min reaction time has shown a considerable increase in IFSS approximately of 45% over that of the untreated fiber from which it was processed. The proper justification of fiber–matrix adhesion featured by composite interfacial properties was explained through IFSS. POLYM. COMPOS., 36:1941–1950, 2015. © 2014 Society of Plastics Engineers     

Improvement of interfacial properties of carbon fiber‐reinforced poly(phthalazinone ether ketone) composites by introducing carbon nanotube to the interphase

This article aims to improve interfacial properties of carbon fiber‐reinforced poly(phthalazinone ether ketone) (PPEK) composites by means of preparing carbon nanotube (CNT)/carbon fiber hybrid fiber. XPS was used to characterize the chemical structure of unsized carbon fiber and SEM was used to observe the surface topography of carbon fibers. Specific area measurement, dynamic contact angle, and interfacial shear strength (IFSS) testing were performed to examine the effect of CNT on the interfacial properties of carbon fiber/PPEK composites. By the introduction of CNT to the interphase of carbon fiber‐reinforced PPEK composites, an enhancement of IFSS by 55.52% was achieved. Meanwhile, the interfacial fracture topography was also observed and the reinforcing mechanism was discussed. POLYM. COMPOS., 36:26–33, 2015. © 2014 Society of Plastics Engineers     

Effect of silane coupling agents on basalt fiber–epoxidized vegetable oil matrix composite materials analyzed by the single fiber fragmentation technique

The fiber–matrix interfacial shear strength (IFSS) of biobased epoxy composites reinforced with basalt fiber was investigated by the fragmentation method. Basalt fibers were modified with four different silanes, (3‐aminopropyl)trimethoxysilane, [3‐(2‐aminoethylamino)propyl]‐trimethoxysilane, trimethoxy[2‐(7‐oxabicyclo[4.1.0]hept‐3‐yl)ethyl]silane and (3‐glycidyloxypropyl)trimethoxysilane to improve the adhesion between the basalt fiber and the resin. The analysis of the fiber tensile strength results was performed in terms of statistical parameters. The tensile strength of silane‐treated basalt fiber is higher than the tensile strength of the untreated basalt fiber; this behavior may be due to flaw healing effect on the defected fiber surfaces. The IFSS results on the composites confirm that the interaction between the fiber modified with coupling agents and the bio‐based epoxy resin was much stronger than that with the untreated basalt fiber. POLYM. COMPOS., 36:1205–1212, 2015. © 2014 Society of Plastics Engineers     

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.     

Nanoscale toughening of carbon fiber‐reinforced epoxy composites through different surface treatments

Interests in improving poor interfacial adhesion in carbon fiber‐reinforced polymer (CFRP) composites has always been a hotspot. In this work, four physicochemical surface treatments for enhancing fiber/matrix adhesion are conducted on carbon fibers (CFs) including acid oxidation, sizing coating, silane coupling, and graphene oxide (GO) deposition. The surface characteristics of CFs are investigated by Fourier transform infrared spectroscopy, X‐ray photoelectron spectroscopy, atomic force microscopy, scanning electron microscopy, interfacial shear strength, and interlaminar shear strength. The results showed that GO deposition can remarkably promote fiber/matrix bonding due to improved surface reactivity and irregularity. In comparison, epoxy sizing and acid oxidation afford enhancement of IFSS owing to effective molecular chemical contact and interlocking forces between the fiber and the matrix. Besides, limited covalent bonds between silane coupling and epoxy matrix cannot make up for the negative effects of excessive smoothness of modified CFs, endowing them inferior mechanical properties. Based on these results, three micro‐strengthening mechanisms are proposed to broadly categorize the interphase micro‐configuration of CFRP composite, namely, “Etching” “Coating”, and “Grafting” modifications, demonstrating that proper treatments should be chosen for combining optimum interfacial properties in CFRP composites. POLYM. ENG. SCI., 59:625–632, 2019. © 2018 Society of Plastics Engineers     

Effect of Halloysite Nanotube Incorporation in Epoxy Resin and Carbon Fiber Ethylene/Ammonia Plasma Treatment on Their Interfacial Property

Abstract

Effects of halloysite nanotube (HNT) loading of up to 2% in epoxy resin on its mechanical properties were characterized. The interfacial property of the resin with carbon fiber nanocomposite was also studied. Single fiber composite (SFC) technique was used to characterize the carbon fiber/epoxy resin interfacial shear stress. Carbon fibers were also coated with ammonia/ethylene plasma polymer to obtain a thin coating of the polymer with amine groups that could react with the epoxy and thus improve the interfacial property. The results indicated that the Young’s modulus of HNT containing nanocomposites increased slightly up to a loading of 0.25% after which it started to decrease. The tensile strength, however, steadily decreased with increasing of HNT loading although the fracture strain did not change significantly. This might be related to the nanotube shape, size and clustering. The interfacial shear strength (IFSS) was also increased slightly with HNT loading. The ethylene/ammonia plasma polymer coated fibers exhibited significantly higher IFSS by over 150%, independent of the HNT loading. The highest IFSS obtained was almost 79 MPa for plasma treated fibers. The results suggest that the carbon fiber/epoxy interface is not affected by the incorporation of up to 1.5% of HNT. Furthermore, the fiber surface modification through plasma polymerization is an effective method to improve and control the IFSS.     

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     

Improving delamination resistance of carbon fiber reinforced polymeric composite by interface engineering using carbonaceous nanofillers through electrophoretic deposition: An assessment at different in-service temperatures

In this article, modification of carbon fiber surface by carbon based nanofillers (multi-walled carbon nanotubes [CNT], carbon nanofibers, and multi-layered graphene) has been achieved by electrophoretic deposition technique to improve its interfacial bonding with epoxy matrix, with a target to improve the mechanical performance of carbon fiber reinforced polymer composites. Flexural and short beam shear properties of the composites were studied at extreme temperature conditions; in-situ cryo, room and elevated temperature (−196, 30, and 120°C respectively). Laminate reinforced with CNT grafted carbon fibers exhibited highest delamination resistance with maximum improvement in flexural strength as well as in inter-laminar shear strength (ILSS) among all the carbon fiber reinforced epoxy (CE) composites at all in-situ temperatures. CNT modified CE composite showed increment of 9% in flexural strength and 17.43% in ILSS when compared to that of unmodified CE composite at room temperature (30°C). Thermomechanical properties were investigated using dynamic mechanical analysis. Fractography was also carried out to study different modes of failure of the composites.     

Physical interactions at carbon nanotube-polymer interface

Mechanical properties of carbon nanotube (CNT) reinforced polystyrene rod and CNT reinforced epoxy thin film were studied and the CNT-polymer interface in these composites was examined. Transmission and scanning electron microscopy examinations of CNT/polystyrene (PS) and CNT/epoxy composite showed that these polymers adhered well to CNT at the nanometer scale. Molecular mechanics simulations and elasticity calculations were used to quantify some of the important interfacial characteristics that critically control the performance of a composite material. In the absence of chemical bonding between CNT and the matrix, it is found that the non-bond interactions, consist of electrostatic and van der Waals forces, result in CNT-polymer interfacial shear stress (at 0 K) of about 138 and 186 MPa, respectively, for CNT/epoxy and CNT/PS. The high interfacial shear stress calculated, about an order of magnitude higher than micro fiber reinforced composites, is believed attributed to intimate contact between the two solid phases at the molecular scale. Simulations and calculations also showed that local non-uniformity of CNT and mismatch of the coefficients of thermal expansions between CNT and polymer matrix also promote the stress transfer ability between the two.     

Effects of surface modification on rheological and mechanical properties of CNT/epoxy composites

Despite superior properties of carbon nanotubes (CNTs), physical properties of the CNT/epoxy composites are not improved significantly because interfacial bonding between the CNTs and the polymer matrix is weak. CNTs were treated by an acidic solution to remove impurities and modified subsequently by amine treatment or plasma oxidation to improve interfacial bonding and dispersion of nanotubes in the epoxy matrix. The functional groups on the surface of treated CNTs were investigated by X-ray photoelectron spectroscopy. The surface modified CNTs were embedded in the epoxy resin by ultra-sonication and the cured nanotube containing composites were characterized by field emission scanning electron microscopy. Rheological properties of nanotube containing epoxy resin and mechanical properties of the modified CNT/epoxy composites were improved because the modification of CNTs improved dispersion and interaction between the CNT and the epoxy resin.     

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     

Mechanical properties of carbon fiber composites modified with nano-SiO2 in the interphase

The performance of carbon fibers-reinforced composites is dependent to a great extent on the properties of fiber–matrix interface. To improve the interfacial properties in carbon fibers/epoxy composites, nano-SiO₂ particles were introduced to the surface of carbon fibers by sizing treatment. Atomic force microscope (AFM) results showed that nano-SiO₂ particles had been introduced on the surface of carbon fibers and increase the surface roughness of carbon fibers. X-ray photoelectron spectroscopy (XPS) showed that nano-SiO₂ particles increased the content of oxygen-containing groups on carbon fibers surface. Single fiber pull-out test (IFSS) and short-beam bending test (ILSS) results showed that the IFSS and ILSS of carbon fibers/epoxy composites could obtain 30.8 and 10.6% improvement compared with the composites without nano-SiO₂, respectively, when the nano-SiO₂ content was 1 wt % in sizing agents. Impact test of carbon fibers/epoxy composites treated by nano-SiO₂ containing sizing showed higher absorption energy than that of carbon fibers/epoxy composites treated by sizing agent without nano-SiO₂. Scanning electron microscopy (SEM) of impact fracture surface showed that the interfacial adhesion between fibers and matrix was improved after nano-SiO₂-modified sizing treatment. Dynamic mechanical thermal analysis (DMTA) showed that the introduction of nano-SiO₂ to carbon fibers surface effectively improved the storage modulus of carbon fibers/epoxy.     

Effect of annealing and silylation on the strength of melt-spun Ni–Mn–Ga fibres and their adhesion to epoxy

Single crystals of ferromagnetic Ni–Mn–Ga shape memory alloys show magnetic-field and stress induced twinning, leading to shape memory. Adaptive composites can thus be produced by embedding single crystalline particles or bamboo-structured Ni–Mn–Ga fibres into a polymer matrix. To guarantee a durable performance of these composites, adhesion between reinforcement phase and matrix should be quantified and optimised. The influence of annealing and surface treatment with an aminosilane of melt-spun Ni–Mn–Ga fibres on their strength and adhesion to an epoxy matrix was investigated using single fibre tension and fragmentation tests. Annealing of the melt-spun Ni–Mn–Ga fibres changed the surface from a “pimpled” to a smooth microstructure. This resulted in a reduced adhesion of the annealed fibres in comparison to the as-spun fibres embedded in an epoxy matrix. As-spun fibres exhibited an interfacial shear strength (IFSS) comparable to the shear strength of the epoxy matrix so that the silylation did not change the adhesion significantly. For the annealed fibres, the silane treatment improved the IFSS by 67%. Furthermore, the silylation increased the fracture strength of the Ni–Mn–Ga fibres due to surface flaw healing or forming of a protective surface coating.     

The properties of dry-spun carbon nanotube fibers and their interfacial shear strength in an epoxy composite

Continuous fibers composed of carbon nanotubes have been adopted as reinforcements for polymeric composites. This paper presents several fundamental studies relevant to the mechanical behavior of CNT fibers, including fiber tensile behavior; in situ SEM observation of fiber deformation mechanisms; and fiber modulus, ultimate strength and fracture strain measurements. A modified Weibull strength distribution model that takes into account the flaw density variation with fiber diameter has been adopted for the statistical strength analysis. The interfacial shear strength between the carbon nanotube fiber and the epoxy matrix has been measured using fragmentation tests of single-fiber composites.     

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.     

Microstructure and mechanical properties of quasi-isotropic chopped fiber-reinforced PyC–SiC matrix composite prepared by novel nondamaging method

In this work, quasi-isotropic chopped carbon fiber-reinforced pyrolytic carbon and silicon carbide matrix (C_f/C–SiC) composites and chopped silicon carbide fiber-reinforced silicon carbide matrix (SiC_f/SiC) composites were prepared via novel nondamaging method, namely airlaid process combined with chemical vapor infiltration. Both composites exhibit random fiber distribution and homogeneous pore size. Young's modulus of highly textured pyrolytic carbon (PyC) matrix is 23.01 ± 1.43 GPa, and that of SiC matrix composed of columnar crystals is 305.8 ± 9.49 GPa in C_f/C–SiC composites. Tensile strength and interlaminar shear strength of C_f/C–SiC composites are 52.56 ± 4.81 and 98.16 ± 24.62 MPa, respectively, which are both higher than those of SiC_f/SiC composites because of appropriate interfacial shear strength and introduction of low-modulus and highly textured PyC matrix. Excellent mechanical properties of C_f/C–SiC composites, particularly regarding interlaminar shear strength, are due to their quasi-isotropic structure, interfacial debonding, interfacial sliding, and crack deflection. In addition to the occurrence of crack deflection at the fiber/matrix interface, crack deflection in C_f/C–SiC composites takes also place at the interface between PyC–SiC composite matrix and the interlamination of multilayered PyC matrix. Outstanding mechanical properties of as-prepared C_f/C–SiC composites render them potential candidates for application as thermal structure materials under complex stress conditions.