Fiber/epoxy interfacial shear strength measured by the microdroplet test

In this study, we analyzed the interfacial shear strength between epoxy and carbon fibers, measured from microdroplet specimens adhered onto a single carbon fiber. Microdroplet specimens exhibited different results of the interfacial strength according to the range of embedded fiber lengths and the calculation methods. The shear stress distributions along the interface were calculated by using the finite element analysis of the droplet, sphere and cylinder model types. The stress analysis showed that a larger shear stress concentration arose along the interface for the droplet model than for the cylindrical one. A compensation factor for the conventional shear lag model is suggested to deduce the real interfacial shear strength on the basis of the average octahedral shear stress calculated from the distortional energy for a unit volume.     

A methodology to measure the interface shear strength by means of the fiber push-in test

A methodology is presented to measure the fiber/matrix interface shear strength in composites. The strategy is based on performing a fiber push-in test at the central fiber of highly-packed fiber clusters with hexagonal symmetry which are often found in unidirectional composites with a high volume fraction of fibers. The mechanics of this test was analyzed in detail by means of three-dimensional finite element simulations. In particular, the influence of different parameters (interface shear strength, toughness and friction as well as fiber longitudinal elastic modulus and curing stresses) on the critical load at the onset of debonding was established. From the results of the numerical simulations, a simple relationship between the critical load and the interface shear strength is proposed. The methodology was validated in an unidirectional C/epoxy composite and the advantages and limitations of the proposed methodology are indicated.     

Electrophoretic deposition of aramid nanofibers on carbon fibers for highly enhanced interfacial adhesion at low content

Here, an anodic electrophoretic deposition was adopted to facilitate the large-scale uniform coating of nano-fillers onto carbon fibers to enhance the interfacial properties between carbon fibers and epoxy matrix. As interface–reinforcing materials, aramid nanofibers were introduced because of their superior mechanical properties and epoxy matrix-friendly functional groups. Furthermore, aramid nanofibers can be readily coated on carbon fibers via electrophoretic deposition because they are negatively-charged in solution with high electrical mobility. Finally, aramid nanofiber-coated carbon fibers showed significantly improved interfacial properties such as higher surface free energy and interfacial shear strengths (39.7% and 34.9% increases, respectively) than those of a pristine carbon fiber despite a very small amount of embedding (0.025 wt% of aramid nanofibers in a carbon fiber), and the short beam strength of the laminated composite prepared with the aramid nanofiber-coated carbon fibers was also improved by 17.0% compared to a non-modified composite.     

Jute fibre/epoxy composites: Surface properties and interfacial adhesion

Jute fibres were surface treated in order to enhance the interfacial interaction between jute natural fibres and an epoxy matrix. The fibres are exposed to alkali treatment in combination with organosilane coupling agents and aqueous epoxy dispersions. The surface topography and surface energy influenced by the treatments were characterized. Single fibre pull-out tests combined with SEM and AFM characterization of the fracture surfaces were used to identify the interfacial strengths and to reveal the mechanisms of failure.     

Enhanced interfacial properties of domestic aramid fiber-12 via high energy gamma ray irradiation

The high energy irradiation was used to modify domestic aramid fiber-12 (DAF12) in epoxy chloropropane. The properties of the interphase between DAF12 and epoxy matrix systems were optimized. Scanning electron microscopy was employed to characterize the surface morphology of DAF12 and high energy irradiated fibers (HEI-DAF12) and composites de-bonding section. Atomic force microscopy showed the original smooth surface disappeared. Single fiber pull-out tests revealed that the interfacial shear strength of HEI-DAF12/epoxy composite was substantially improved by 45.17% after irradiation in 400 kGy dose. Dynamic contact angle analysis indicated the increased total surface free energy. The changes of elemental composition investigated via X-ray Photoelectron Spectrometer verified the increase polar groups on fiber surface caused by high energy irradiation.     

Effect of oxygen plasma treatment of PPTA and PBO fibers on the interfacial properties of single fiber/epoxy composites studied by Raman spectroscopy

The interfacial micromechanics of single poly(p-phenylene terephthalamide (PPTA) and poly(p-phenylene benzobisoxazole (PBO) fibers embedded in an epoxy resin has been investigated by determining the interfacial shear stress distributions along the fiber length. The effects of an oxygen plasma treatment on the interfacial shear stress of the fiber-epoxy systems are analyzed. Raman spectroscopy was used to map the stress distributions along the fiber when the composite is subjected to a small axial tensile strain (3.5% for PPTA and 2.5% for PBO). The quality of the interface or adhesion was improved after the surface treatment, supporting the ability of plasma oxidation to enhance the adhesion of high-performance fibers to epoxy resins. The tensile behavior of fiber-reinforced systems was different in each case. PPTA reinforcements underwent fragmentation, likely by fiber microfailure, whereas debonding or bridging is the most probable fragmentation mechanism in the case of PBO.     

Interfacial strength and fracture energy of individual carbon nanofibers in epoxy matrix as a function of surface conditions

The interfacial shear strength (IFSS) and fracture energy of individual carbon nanofibers embedded in epoxy were obtained for different surface conditions and treatments by novel, MEMS-based, nanoscale fiber pull-out experiments. As-grown vapor grown carbon nanofibers (VGCNFs) with turbostratic surface and 5 nm peak-to-valley surface roughness exhibited high IFSS and interfacial fracture energy, averaging 106 ± 29 MPa and 1.9 ± 0.9 J/m², respectively. Subsequent high temperature heat treatment and graphitization resulted in drastically reduced IFSS of 66 ± 10 MPa and interfacial fracture energy of 0.65 ± 0.14 J/m². The smaller IFSS values and the reduced standard deviation were due to significant reduction of the fiber surface roughness to 1–2 nm, as well as a decrease in surface defect density during conversion of turbostratic and amorphous carbon to highly ordered graphitic carbon. For both grades of VGCNFs failure was adhesive with clear nanofiber surfaces after debonding. Oxidative functionalization of high temperature heat-treated VGCNFs resulted in much higher IFSS of 189 ± 15 MPa and interfacial fracture energy of 3.3 ± 1.0 J/m². The debond surfaces of functionalized nanofibers had signs of matrix residue and/or shearing of the outer graphitic layer of the VGCNFs, namely the failure mode was a combination of cohesive matrix and/or cohesive fiber failure which contributed to the high IFSS. For all three grades of VGCNFs the IFSS was independent of fiber length and diameter. The findings of this experimental study emphasized the critical role of nanofiber surface morphology and chemistry in determining the shear strength and fracture energy of nanofiber interfaces, and shed light to prior composite-level strength and fracture toughness measurements.     

Macroscopic analysis of interfacial properties of flax/PLLA biocomposites

This study presents results from a study of the mechanical behaviour of flax reinforced Poly(l-Lactic Acid) (PLLA) under in-plane shear and mode I interlaminar fracture testing. Slow cooling of the unreinforced polymer has been shown to develop crystalline structure, causing improvement in matrix strength and modulus but a drop in toughness. The in-plane shear properties of the composite also drop for the slowest cooling rate, the best combination of in-plane shear performance and delamination resistance is noted for an intermediate cooling rate, (15.5 °C/min). The values of G_Ic obtained at this cooling rate are higher than those for equivalent glass/polyester composites. These macro-scale results have been correlated with microdroplet interface debonding and matrix characterization measurements from a previous study. The composite performance is dominated by the matrix rather than the interface.     

Development of aligned-hemp yarn-reinforced green composites with soy protein resin: Effect of pH on mechanical and interfacial properties

Unidirectional hemp yarn-reinforced green composites were fabricated with soy protein concentrate (SPC) resin processed at various pH values. To preserve the yarn alignment during the fabrication of green composites, hemp yarn was wound onto a metal frame with slight tension and precured SPC resin was applied to the yarns. Effects of pH values on the tensile properties of the SPC resin and hemp yarn/SPC resin interfacial shear strength (IFSS) were investigated. Increasing pH of the SPC resin from 7 to 12 decreased its fracture stress and Young’s modulus from 13.1 MPa and 357.5 MPa to 8.1 MPa and 156.2 MPa, respectively. At the same time fracture strain and moisture content increased from 31.5% and 15.65% to 53·4% and 19.30%, respectively, indicating resin plasticization. However, hemp yarn/SPC resin IFSS increased from 17.7 MPa at pH 7 up to 28.0 MPa at pH 10, after which it decreased. The fracture toughness of the composites increased up to pH of 10 but further increase in pH reduced the toughness. SEM photomicrographs showed fracture surfaces of hemp yarn-reinforced green composites that indicated better resin/fiber interaction at pH of 10 than 7 or 12.     

Feasibility study of a tungsten wire-reinforced tungsten matrix composite with ZrOx interfacial coatings

Brittleness problem imposes a severe restriction on the potential application of tungsten as high-temperature structural material. In this paper, a novel toughening method for tungsten is proposed based on reinforcement by tungsten wires. The underlying toughening mechanism is analogous to that of fiber-reinforced ceramic matrix composites. Strain energy is dissipated by debonding and frictional sliding at engineered fiber/matrix interfaces. To achieve maximum composite toughness fracture mechanical properties have to be optimized by interface coating. In this work, we evaluated six kinds of ZrO_x-based interface coatings. Interfacial parameters such as shear strength and fracture energy were determined by means of fiber push-out tests. The parameter values of the six coatings were comparable to each other and satisfied the criterion for crack deflection. Microscopic analysis showed that debonding occurred mostly between the W filament and the ZrO_x coating. Feasibility of interfacial crack deflection was also demonstrated by a three-point bending test.     

Influence of ultrasonic treatment on the characteristics of epoxy resin and the interfacial property of its carbon fiber composites

To enhance the interfacial property between a carbon fiber and epoxy matrix, an ultrasonic technique was used to treat the resin liquid and the impregnated fibers respectively. The effects of the treatments on the characteristics of the resin system and the fiber surface, as well as fiber/matrix interfacial bonding strength, were analyzed and discussed. The results indicated ultrasonic treatments significantly decreased the viscosity and surface tension of the resin system, and increased the wettability and the oxygen content of the fiber surface due to the ultrasonic cavitation effects. Microbond tests revealed much more increase of interfacial shear strength when the ultrasound was applied to the impregnated fibers, and combination failures of interface and matrix layer were observed from the pulled-out fiber surface.     

Effect of γ-ray irradiation grafting on the carbon fibers and interfacial adhesion of epoxy composites

A special technique using γ-ray irradiation-induced graft-polymerization was applied to carbon fibers. Epoxy resin and chloroepoxy propane reacted with carbon fibers by a co-irradiation grafting method and acrylic acid was graft-polymerized onto the fiber surface via a pre-irradiation grafting method. The roughness, amount of containing-oxygen functional groups and surface energy were all found to increase significantly after irradiation grafting. Gamma-ray irradiation grafting improved marginally the tensile strength of carbon fibers, which was evaluated by statistical analysis using the Weibull distribution. The interlaminar shear strength of treated carbon fiber/epoxy was enhanced by at least 17.5%, compared with that of untreated carbon fiber/epoxy. The mechanisms of irradiation grafting are proposed by radical reactions. The γ-ray co-irradiation grafting and pre-irradiation grafting are both an effective method for modifying the physicochemical properties of carbon fibers and improving the interfacial adhesion of composites.     

Fiber/matrix interfacial shear strength measured by a quasi-disk microbond specimen

A single fiber/quasi-disk microbond specimen was made for evaluating the interfacial shear strength of fiber-reinforced composites. A quasi-disk type microbond was formed with the insertion of a pin-holed Teflon film into a wetted liquid droplet epoxy resin that surrounded a single vertical carbon fiber. After finishing a curing process, the specimens were tested in comparison with conventional droplet microbond specimens. Test results for the quasi-disk type specimens showed more reliable shear strength data than those for the conventional ones. Their interfacial shear strength behaviors were in a good agreement with the hardness variation of the epoxy resin. Finite element analysis of droplet, quasi-disk and cylindrical pull-out tests showed that the stress concentration in the meniscus region for the quasi-disk type specimen was much less than that for droplet and very similar to that of the cylindrical one. This observation supported the reliability of experimental strength data measured in the quasi-disk type microbond test.     

Tailored interyarn friction in aramid fabrics through morphology control of surface grown ZnO nanowires

Para-aramid fibers, such as Kevlar, have been the most common material used for ballistic applications by providing a variety of energy absorption mechanisms to dissipate a projectile’s momentum. One important mechanism is interyarn friction, which can be controlled through surface treatment of the fibers. It was recently shown that the growth of ZnO nanowires on the surface of the fibers could increase the interyarn friction, producing 10.85 times higher peak load and 22.70 times higher energy absorption compared to neat fabrics. Here, it is demonstrated that variation of the morphology of the nanowires produces a drastic change in the pullout behavior with low aspect ratio nanowires producing the largest increase in pullout force. While weight of the modified fabrics increased only 20% compared to the bare ones, tensile test results show that the growth of ZnO nanowires enhances both tensile strength and elastic modulus of the fabrics by 13% and 10%, respectively. A comprehensive post-test micrograph analysis is performed to reveal possible enhancement mechanisms of modified aramid fabrics with different nanowire morphologies.     

Grafting of nano-TiO2 onto flax fibers and the enhancement of the mechanical properties of the flax fiber and flax fiber/epoxy composite

In this article, a flax fiber yarn was grafted with nanometer sized TiO₂, and the effects on the tensile and bonding properties of the single fibers and unidirectional fiber reinforced epoxy plates were studied. The flax fiber yarn was grafted with nanometer sized TiO₂ through immersion in nano-TiO₂/KH560 suspensions under sonification. The measured grafting content of the nano-TiO₂ ranged from 0.89 wt.% to 7.14 wt.%, dependent on the suspension concentration. With the optimized nano-TiO₂ grafting content (∼2.34 wt.%), the tensile strength of the flax fibers and the interfacial shear strength to an epoxy resin were enhanced by 23.1% and 40.5%, respectively. The formation of Si–O–Ti and C–O–Si bonds and the presence of the nano-TiO₂ particles on the fiber surfaces contributed to the property enhancements. Unidirectional flax fiber reinforced epoxy composite (V_f = 35.4%) plates prepared manually showed significantly enhanced flexural properties with the grafting of nano-TiO₂.     

The role of interfacial interactions on the glass-transition and viscoelastic properties of silica/polystyrene nanocomposite

Filler surface properties and polymer-filler interactions have dominate influence on viscoelastic behavior of polymeric matrix composites. When the filler-filler spacing is on the order of the polymeric matrix molecular size, fillers may agglomerate through direct short-range interactions, also by overlapping of interfacial layers of neighboring fillers. In this work the effect of interfacial layer on the viscoelastic properties of silica/polystyrene composite was investigated.The Si/Ps nanocomposites were prepared by solution mixing method, and dynamic rheometry was employed to determine the viscoelastic behavior in the melt state. Experimental results show that, addition of silica nanoparticles to polystyrene matrix would increase the glass-transition temperature of polymer. This increasing will be accelerated by presence of nanoparticles with more filler-polymer adhesion energy, because of more interfacial layer volume fraction. It is helpful in evaluating the volume fraction and equivalent thickness of interfacial layer in polymer nanocomposites. Likewise it is shown that, the dynamic moduli of nanocomposite is enhanced associated with the increase in the glass-transition temperature. This study implies that the main source of increment in both dynamic modulus and glass-transition temperature of polymer nanocomposites is the presence of the immobilized interfacial layer and the secondary filler network.     

Enhancement of ablative and interfacial bonding properties of EPDM composites by incorporating epoxy phenolic resin

Effects of epoxy phenolic resin (EPR) on ablative and interfacial bonding properties of EPDM composites were evaluated. Ablative properties of EPDM composites were enhanced by two folds with incorporating 10 phr EPR. This significant enhancement was attributed to positive effect of EPR on thermal stability and thermal insulating properties of EPDM composites as well as formation of compact char layer onto composites. Furthermore, interfacial shear strength of EPDM composites with carbon fiber/epoxy (CF/EP) composites was increased by 55.6% with incorporating 10 phr EPR, due to interfacial chemical reaction of epoxide groups of EPR molecule from EPDM composites with amine group of hardener from CF/EP composites.     

Tailoring of the interfacial properties of polymeric single fibre-reinforced epoxy composites by non-oxidative plasma treatments

The interfacial properties of epoxy composites reinforced with a single, plasma-treated fibre of either poly(p-phenyleneterephthalamide) (PPTA) or poly(p-phenylenebenzobisoxazole) (PBO) have been investigated with a focus on evaluating the effect of two non-oxidative (He and N₂) microwave plasma treatments on interfacial adhesion properties. Tensile testing of single filaments revealed that their tensile strength does not diminish with the plasma treatments, despite the fact that their surface properties have been both physically and chemically modified. Interfacial characterisation by Raman spectroscopy indicated that the quality of adhesion was substantially enhanced following exposure of the fibres to microwave plasma treatment in either pure helium or pure nitrogen flows for just one minute. Such improvement was higher than that attained when O₂ was used for blowing the plasma, under the same operational conditions. Moreover, no swelling effect was observed by AFM after exposure of the He or N₂ plasma-treated fibres to ambient conditions for as much as 24 h.     

Characterization of fibre/matrix interfaces in carbon/carbon composites

The present paper proposes an approach to characterizing fibre/matrix (F/M) interface in carbon/carbon (C/C) composites with respect to both modes of loading that may be expected: opening or shearing. Push-out and tensile tests were used. The former tests involve the shearing mode whereas the latter ones involve the opening one. Push-out tests use a diamond indenter to load the fibres. The interface sliding shear stress was obtained from the load-fibre displacement curve. The tensile tests were conducted on specimens having fibres oriented at 90° with respect to loading direction in order to preferentially open the interfaces. Interface opening strength was extracted from the composite tensile stress–strain behaviour. The specimens were examined under load and after ultimate failure by optical microscopy (OM). The mechanical properties of the F/M interfaces were then discussed.     

Assessment of interfacial bonding between polymer threads and epoxy resin by transverse fibre bundle (TFB) tests

Two experimental approaches were employed to assess the fibre/matrix adhesion between polymer threads and epoxy resin by transverse fibre bundle (TFB) tests. The first approach was to measure interfacial bonding strength of the fibre/matrix interface in dog-bone-shaped tensile specimens by applying normal stress until failure, simulating the Mode I failure mode. The second approach was to determine the fibre/epoxy interfacial bonding strength in shear (simulating the Mode II failure mode) by means of a V-notched beam shear testing method, i.e. a modified Iosipescu test. In both methods, polymer threads were transversely incorporated in the middle section of the specimens. It was found that both methods were simple, reliable, and sensitive to changes in the fibre/matrix adhesion conditions, though interpretation of the test results was somewhat complex. The two experimental approaches were able to produce consistent results and can thus be adopted as alternative methods for determining the interfacial bonding properties between fibres and matrix in composite systems where conventional micro-mechanical or macro-mechanical testing methods cannot be used.