Interphase characterization of composites under fatigue loadings

The effect of glass-fiber epoxy interface in cross-ply reinforced composites on the fatigue behavior by using load-increasing fatigue test is studied throughout this paper. The damage as measured by stiffness reduction is more significant for the composites with poor bonded fibers as was found for EP sized ones, dependent from test conditions. The loss energy is shown to be a sensitive tool to characterize the nature of fiber–matrix adhesion. The loss energy for composites with poor adhesion between fiber and matrix results in significantly higher amounts of consumed energy during a single stress-strain loop than those composites containing well-bonded fibers.     

Damage monitor and life prediction of carbon fiber-reinforced ceramic-matrix composites at room and elevated temperatures using hysteresis dissipated energy-based damage parameter

In this paper, the damage monitor and life prediction of carbon fiber-reinforced ceramic-matrix composites (C/SiC CMCs) have been investigated using the hysteresis dissipated energy-based damage parameter. The evolution of the interface shear stress, hysteresis dissipated energy, hysteresis dissipated energy-based damage parameter and the broken fibers fraction vs. cycle number, the fatigue life S?N curves of unidirectional, cross-ply and 2.5D C/SiC composites at room temperature and 800 °C in air atmosphere have been analyzed. For unidirectional C/SiC, the hysteresis dissipated energy and hysteresis dissipated energy-based damage parameter first increase and then decrease with cycle number, and the fatigue limit stress decreases from 88% tensile strength at room temperature to 20% of the tensile strength at 800 °C in air atmosphere; for cross-ply C/SiC, the hysteresis dissipated energy and hysteresis dissipated energy-based damage parameter decrease with increasing applied cycles, and the fatigue limit stress decreases from 85% tensile strength at room temperature to 22% tensile strength at 800 °C in air; and for 2.5D C/SiC, the hysteresis dissipated energy and hysteresis dissipated energy-based damage parameter increases with cycle number, and the fatigue limit stress decreases from 70% tensile strength at room temperature to 25% tensile strength at 800 °C in air.     

Thermodynamics of deformation of micro composites

A thermodynamic evaluation, based on simultaneous measurements of the mechanical work and the concomitant heat of deformation in a stretching micro calorimeter, was performed on polycarbonate/carbon fibre (PC/CF) micro composites. Single fibre composite specimens containing sized and unsized CF were subjected to different thermal treatments. Thermodynamic effects of deformation were measured for both elastic and plastic deformation ranges. In the elastic/beginning of plastic deformation ranges the internal energies and heat effects of deformation of micro composites exceeded those of matrices. The highest internal energy and, in turn, the highest fibre/matrix adhesion, was found in the case of the quenched micro composites with sized fibers. Thermodynamic effects of deformation and calculated material constants of PC were in reasonable agreement with data in the literature.     

The effect of oxygen-plasma treatment on Kevlar fibers and the properties of Kevlar fibers/bismaleimide composites

The effect of oxygen-plasma treatment for Kevlar fibers on the interfacial adhesion and typical macro-properties of Kevlar fiber/bismaleimide composites was intensively studied. It is found that oxygen-plasma treatment significantly affects the interfacial adhesion by changing the chemistry and morphology of the surfaces of the fibers, and thus leading to improved interlaminar shear strength, water resistance and dielectric properties of the composites. However, the improvement is closely related to the treatment power and time. The best condition for treating Kevlar fiber is 70 W for 5 min. Oxygen-plasma treatment provides an effective technique for overcoming the poor interfacial adhesion of Kevlar fiber based composites, and thus showing great potential in fabricating high performance copper clad laminates.     

Comparisons of interface shear stress degradation rate between C/SiC and SiC/SiC ceramic-matrix composites under cyclic fatigue loading at room and elevated temperatures

The interface shear stress in C/SiC and SiC/SiC ceramic-matrix composites with different fiber preforms, i.e. unidirectional, cross-ply, 2D woven, 2.5D woven, and 3D braided, under cyclic fatigue loading at room and elevated temperatures have been estimated. An effective coefficient of the fiber volume fraction along the loading direction was introduced to describe the fiber preforms. Based on fiber slipping mechanisms, the hysteresis loops models considering different interface slip cases have been developed. Using the experimental fatigue hysteresis dissipated energy, the interface shear stress degradation rates of C/SiC and SiC/SiC composites with different fiber preforms at room and elevated temperatures have been obtained and compared. It was found that the interface shear stress degradation rate is the highest for 3D braided SiC/SiC at 1300 °C in air, and the lowest for 2D woven C/SiC at room temperature under cyclic fatigue loading.     

Study of impact properties and morphology of unidirectional bamboo strips–polyester composites: effect of mercerization

Composites were fabricated with alkali (10%, 15% and 20%) treated bamboo fibers incorporated to the extent of 50% (by volume) and polyester resin. Impact test was made on bamboo strips and composites samples. It was observed that the fracture energy undergoes an increase from untreated to alkali treated bamboo strips. Alkali treated bamboo fiber composites show higher fracture energy value than the untreated bamboo fiber composites. The phenomenal change was quite evident from scanning electron micrographs of the fractured surface. Considering the effects of all factors, the work of fracture shows maximum value in the case of 20% alkali treated bamboo strip composites. It was also observed that the rate of increase of work of fracture value is much higher in the case of composite samples than the bamboo sample. It was explained on the basis of synergism obtained by improved interfacial adhesion between fiber and matrix, and removal of hemicellulose from the bamboo itself, which was evident from the intermolecular H-bonding formation studied by FT-IR.     

A Fiber-Bundle Pull-out Test for Surface-Modified Glass Fibers in GF/Polyester Composite

The development of high-performance polymer composites is tightly bound with the functional surface modification of reinforcements. A new method, based on the principle of the fiber-bundle pull-out test, is proposed to analyze the interfacial properties between the long fibers in the form of a bundle and the polymer matrix. Specimen geometry and a test fixture were designed using finite element analysis. The method was verified for unsized and sized glass fibers embedded in polyester resin to demonstrate its applicability for a wide range of adhesion between fibers and the polymer matrix. The pull-out test can be used for a relative comparison of different surface modifications if the bundle geometry is unknown. The results of high reproducibility and sensitivity for interfacial properties make the method attractive.     

Elastomeric sizings for glass fibers and their role in fiber wetting and adhesion in resin transfer molded composites

Mold fill velocities of 0.067 cm³/s and 2.66 cm³/s were used to impregnate glass fiber preforms with different architectures and sizing types in two force-controlled resin transfer molding (RTM) fixtures. The fabrication of disk-shaped parts at high molding speed and high post-cure fill pressure was proven successful in reducing the amount of flow-induced defects for reinforcements with a random nonlayered structure. Investigations on the effect of fiber/matrix interface modification with controlled-thickness elastomeric films obtained by the admicellar polymerization technique were carried out to assess the structural integrity levels attained with these less expensive polymeric sizings. In particular, parts reinforced with fibers coated with a thin film of styrene-isoprene copolymer performed significantly better than the uncoated control samples in the tensile and flexural tests. For the same sizing type, the interlaminar shear strength was more than 30% higher than the desized composite and compared statistically to the adhesion level exhibited by commercially sized reinforcements. Greater data scatter and poorer adhesion performance was observed for those composites containing fibers with a thin polystyrene coat. We infer that beneficial effects of a nanometer-thick elastomer interlayer are more evident when extensive cooperative segmental motions take place, that is, when the surface glass transition temperature of the sizing is far below the room temperature. These results have implications for composite manufacture applications involving tailored interfaces with flexible sizings.     

Enhanced surface free energy of polyimide fibers by alkali treatment and its interfacial adhesion behavior to epoxy resins

In this article, polyimide (PI) fibers were modified by alkali treatment, and PI fiber-reinforced epoxy composites were fabricated. The effects of different alkali treatment times on the surface properties of the PI fibers and the adhesion behaviors of PI fiber/epoxy composites were studied. The surface morphologies, chemical compositions, mechanical properties, and surface free energy of the PI fibers were characterized by atomic force microscopy, X-ray photoelectron spectroscopy, single-fiber tensile strength analysis, and dynamic contact angle analysis, respectively. The results show that alkali treatment plays an important role in the improvement of the surface free energy and the wettability of PI fibers. We also found that, after the 3 min, 30 °C, 20 wt% NaOH solution treatment, the fibers possessed good mechanical properties and surface activities, and the interlaminar shear strength of the composites increased to 64.52 MPa, indicating good interfacial adhesion properties.     

Cellulose-based biocomposites: comparison of different multiphasic systems

Biocomposites (biodegradable composites) are obtained by blending biodegradable polymers and fillers. Since the main components are biodegradable, the composite as a whole is also expected to be biodegradable. This paper presents various biocomposites that have been elaborated with cellulose or lignocellulose fibers from diverse sources, with different lignin contents. This paper is targeted on the analysis of 'fiber–matrix' interactions of two types of biocomposites based on agropolymer (plasticized wheat starch) and biopolyester (polybutylene adipate-co-terephthalate), named APB and BPB, respectively. Processing and main properties of both biocomposites are shown and compared. Polyolefin-based composite (PPC), which is known to present very poor 'fiber–matrix' interactions, is used as a reference. Through the Young's modulus, mechanical properties have shown that the reinforcement, by increasing fiber content, is much more significant for APB compared to BPB. The evolution of chains mobility, evidenced through shift of T _g values, according to the increase in fiber content and thence in interfacial area, have shown that the fiber–matrix interactions are higher for APB. BPB presents intermediate values, higher than PPC ones. These results are in agreement with the analysis of the composite morphologies performed by SEM on cryogenic fractures. Finally, by determining the theoretical works of adhesion and the interfacial tensions from contact angle measurements, it is shown that these parameters are partially able to predict the level of interaction between the fibers and the matrix. We could show that the perspectives of such work seem to be of importance to tailor new materials with a controlled end-use.     

Discontinuous basalt and glass fiber reinforced PP composites from textile prefabricates: effects of interfacial modification on the mechanical performance

Spun and blown basalt fibers and their PP matrix composites were investigated. The composites were manufactured by hot pressing technology from carded and needle punched prefabricate using PP fiber as matrix material. Glass and blown basalt fibers were treated with reaction product of maleic acid-anhydride and sunflower oil while spun basalt fibers had a surface coating of silane coupling agent. Fibers were investigated with tensile tests while composites were subjected to static and dynamic mechanical tests. The results show that blown basalt fibers have relatively poor mechanical properties, while spun basalt fibers are comparable with glass fibers regarding geometry and mechanical performance. The static and dynamic mechanical properties of glass and spun basalt fiber reinforced composites are similar and are higher than blown basalt fiber reinforced composites. Results were supported with SEM micrographs.     

Effect of transcrystallization in carbon fiber reinforced poly(p-phenylene sulfide) composites on the interfacial shear strength investigated with the single fiber pull-out test

The effect of transcrystallinity in carbon fiber reinforced poly(p-phenylene sulfide (PPS) composites on the apparent shear strength was investigated with the single fiber pull-out test. Transcrystalline zones around the reinforcing fibers do not seem to improve the adhesion level significantly. Neighbor fibers hinder the formation of the transcrystalline zone and a ductile fracture behavior can be observed. However, the apparent strength level is slightly higher for composites containing such reinforcing neighbor fibers compared with single fiber composite samples. During annealing a brittle interface can be formed in the multifiber composite yielding a higher level of the apparent shear strength.     

Effect of emulsifier content of sizing agent on the surface of carbon fibres and interface of its composites

In this work, carbon fibres were sized with different emulsifier content sizing agent in order to improve the performances of carbon fibres and the interface of carbon fibres composites. The surface characteristic changing after modification was investigated by scanning electron microscopy (SEM), atomic force microscopy (AFM). Wetting and surface energy along with contact angles were determined by the dynamic contact angle analysis test (DCAT). At the same time, the single fibre strengths and weibull distributions were also studied in order to understand the effect of the emulsifier content of sizing agent on the carbon fibres. The interfacial shear strength and hygrothermal ageing of the composites were measured which showed a different enhancement, respectively. The results revealed that sizing agent E-3 showed better interface adhesion between fibres and matrix and sizing agent E-2 sized carbon fibre has better ageing resistant properties.     

Interlaminar interface in carbon fiber polymer-matrix composites,studied by contact electrical resistivity measurement

The interlaminar interface in carbon fiber (continuous) epoxy-matrix composites was studied by measuring the contact electrical resistivity of this interface. The contact resistivity was found to decrease with increasing curing pressure and to be higher for unidirectional than crossply composites. The lower the contact resistivity, the greater was the extent of direct contact between fibers of adjacent laminae. The activation energy for electrical conduction in the through-thickness direction was found to increase with increasing curing pressure and to be lower for unidirectional than crossply composites. The higher the activation energy, the greater the residual interlaminar stress.     

The friction and wear properties of divinylbenzene-grafted UHMWPE fiber-filled serpentine/PTFE composite

Divinylbenzene-grafted Ultra-high-molecular-weight polyethylene (UHMWPE) fibers were used to reinforce the Polytetrafluoroethylene (PTFE) composite and the friction and wear behaviors of UHMWPE/PTFE composite were studied on the ring-block machine under vacuum condition. The worn surfaces of specimens were investigated using scanning electron microscopy and energy dispersive spectroscopy (EDS). The results showed that the friction coefficient and temperature of UHMWPE/PTFE composites with surface-treated UHMWPE fiber were apparently lower than that with untreated one. In conclusion, the surface treatment favored the improvement of the higher interface strength and so had good effect on improving the tribological properties of the composites. The dominant wear mechanisms were adhesion wear, plastic deformation, brittle facture, and spalling. The EDS analysis of the worn surface indicated the trend of the tribochemical reaction of the Fe related to the transfer of the PTFE.     

Micromechanical Behavior of Carbon Nanotube-Covered SiC Fibers in Polymer Matrix Composites

The incorporation of nanotube-covered fibers in continuous fiber/epoxy composites has been shown to influence the mechanical, electrical, and thermal properties of the composite. Increased interlaminar shear stress, flexural strength and modulus have been reported in such composites over composites containing bare fibers. In this study, the microstructure and interfacial shear strength (ISS) of continuous silicon carbide fiber/epoxy composites with and without nanotubes grown from the SiC fiber surface were investigated with micro-Raman spectroscopy (MRS) and microscopy. The fibers with nanotubes grown from the surface were found to have a reduced ISS compared with the bare fibers. Electron microscopy showed good wetting of epoxy in the nanotube forests, but poor attachment of the nanotube forests to the fibers. These results suggest that the mechanism leading to improvements in bulk composite properties is not due to an improvement in the fiber/matrix ISS.     

Fiber-matrix adhesion mechanism of pitch-based carbon fiber composites

The fiber-matrix adhesion mechanism in high modulus pitch-based carbon fiber-epoxy matrix composites has been studied. The surface morphology and chemistry of the carbon fibers were examined by microscopic (SEM, STM), thermodynamic and spectroscopic (XPS, Raman) techniques. The interlaminar shear strength and transverse tensile strength of the composites made from surface-treated and untreated fibers were also obtained. In the microscopic analysis, there was no difference in the surface roughness between the surface-treated and untreated fibers. In the thermodynamic and spectroscopic analyses, surface treatment of the carbon fibers increased the amount of surface oxygen. The results indicated that the major role of the surface treatment on the carbon fiber-epoxy resin adhesion is not the mechanical interlocking effect by the surface roughness. The formation of surface oxygen-containing functional groups is assumed to account for the increase in fiber-matrix interfacial adhesion.     

Interphase characterization in epoxy resin/carbon fibre composites

In this paper, interphase properties of carbon fibre/epoxy resin single-fibre model and unidirectional (UD) composites are reported. To study the contribution of the carbon fibre surface chemistry and morphology and of the resin itself to the overall properties of the composites, untreated, oxidized and sized fibres are used with bi- and tetrafunctional, diglycidylether of Bisphenol A, DGEBA and tetraglycidyl 4,4'-diaminodiphenylmethane, TGDDM-based resins, cured with amine and anhydride hardeners. Adsorption measurements and single fibre contact angle experiments, as well as the pull-out test were applied to characterize the surface of carbon fibre and the interfacial shear strength with different matrices. It was shown that the presence of the size on the surface can drastically affect the wettability as well as the starting rate of the cure reaction of epoxide in the vicinity of the fibre surface, as revealed by FTIR microscopy. Different elastic-plastic behavior of model composites before debonding is found for untreated, oxidized and sized fibres, due to the various interphase structures formed. Both micro-and macromechanical properties of the composites are found to be significantly affected by the matrix properties. The role of the surface treatment of fibers becomes especially important in high performance resin systems.     

Effect of chemical modifications of the pineapple leaf fiber surfaces on the interfacial and mechanical properties of laminated biocomposites

Natural fiber reinforced renewable resource based laminated composites were prepared from biodegradable poly(lactic acid) (PLA) and untreated or surface-treated pineapple leaf fibers (PALF) by compression molding using the film stacking method. The objective of this study was to determine the effects of surface treatment of PALF on the performance of the fiber-reinforced composites. X-ray photoelectron spectroscopy (XPS) and Fourier transform infrared spectroscopy (FTIR) were used to aid in the analysis. The mechanical properties of the PLA laminated composites were improved significantly after chemical treatment. It was found that both silane- and alkali-treated fiber reinforced composites offered superior mechanical properties compared to untreated fiber reinforced composites. The effects of temperature on the viscoelastic properties of composites were studied by dynamic mechanical analysis (DMA). From the DMA results, incorporation of the PALF fibers resulted in a considerable increase of the storage modulus (stiffness) values. The heat defection temperature (HDT) of the PALF fiber reinforced PLA laminated composites was significantly higher than the HDT of the neat PLA resin. The differential scanning calorimeter (DSC) results suggest that surface treatment of PALF affects the crystallization properties of the PLA matrix. Additionally, scanning electron microscopy (SEM) was used to investigate the distribution of PLA within the fiber network. SEM photographs of fiber surface and fracture surfaces of composites clearly indicated the extent of fiber–matrix interface adhesion. It was found that the interfacial properties between the reinforcing PALF fibers and the surrounding matrix of the laminated composite are very important to the performance of the composite materials and PALF fibers are good candidates for the reinforcement fiber of high performance laminated biodegradable biocomposites.     

Surface Modification of Ultrahigh-molecular-weight Polyethylene Fibers with Coupling Agent during Extraction Process

Ultrahigh molecular weight polyethylene (UHMWPE) fibers were treated with a coupling agent following the extraction of gel fibers, resulting in modified fibers after subsequent ultra-drawing. The structure and morphology of the modified UHMWPE fibers were characterized and their surface wetting, interfacial adhesion, and mechanical properties were investigated. It was found that the coupling agent was absorbed into the UHMWPE fiber and trapped on the fiber surface. Compared with unmodified UHMWPE fibers, the modified fibers had smaller contact angle, higher crystallinity, and smaller crystal size. The interfacial adhesion and mechanical properties of UHMWPE fibers were significantly improved with increasing coupling agent concentration and gradually reached a plateau value. After treatment with 1.5 wt% solution of a silane coupling agent (γ -aminopropyl triethoxysilane, SCA-KH-550), the interfacial shear strength of the UHMWPE-fiber/epoxy composites was increased by 108% and the tensile strength and modulus of modified UHMWPE fibers were increased by 11% and 37% respectively.