A refined method for estimating fiber and interfacial shear strength by using a single-fiber composite

In estimating interfacial shear strength from the fragmentation process of fibers in single-fiber composites, a problem arises as to the value of the fiber strength if the fiber strengths distribute widely and strongly depend on the fiber length. To overcome this problem, a refined analysis method for simultaneously estimating the fiber and the interfacial shear strength from the fragmentation process has been shown. Agreements between the values estimated with the proposed method and the results of the single-fiber tensile and the direct shear tests have been obtained. It has been shown that the estimation of the interfacial shear strength using the proposed method is insensitive to the matrix properties if the interfacial shear strength is unaltered by the matrix properties, and that the variations of the distribution parameters of the fiber strength is significantly smaller for the proposed method as compared with the single-fiber tensile tests. The results obtained by applying the proposed method to various carbon fibers have been shown.     

Interphase sizing temperature effect of LaRC PETI-5 on the dynamic mechanical thermal properties of carbon fiber/BMI composites

The dynamic mechanical thermal properties of carbon fiber-reinforced bismaleimide (BMI) composites processed using polyacrylonitrile(PAN)-based carbon fibers unsized and sized with LaRC PETI-5 amic acid oligomer as interphase material at 150°C, 250°C, and 350°C were investigated by means of dynamic mechanical thermal analysis. It was found that the storage modulus, loss modulus, tan δ and the peak temperature significantly depend on the sizing temperature as well as on the presence and absence of LaRC PETI-5 sizing interphase. The result showed that the carbon fiber/BMI composite sized at 150°C had the highest storage modulus at a measuring temperature of 250°C. The storage modulus decreased with increasing sizing temperature from 150°C to 350°C, being influenced by interdiffusion and co-reaction between the LaRC PETI-5 interphase and the BMI matrix resin. The present result is quite consistent with the interfacial result reported earlier in term of interfacial shear strength and interlaminar shear strength of carbon fiber/BMI composites. It is addressed that in the present composite system the sizing temperature of LaRC PETI-5 interphase critically influences not only the interfacial properties but also the dynamic mechanical thermal properties and its control is also important.     

Effect of processing temperature on the micro- and macro-interfacial properties of carbon fiber/epoxy composites

Three different temperature schemes were applied on carbon fiber/epoxy composite to elucidate the effect on interfacial shear strength (IFSS) and inter-laminar shear strength (ILSS). It showed that carbon fiber/epoxy IFSS was significantly influenced by the processing temperature, while ILSS was only slightly changed. Moreover, the mechanical properties revealed no necessary relationship between the micro- and macro-interfacial strengths with the properties of epoxy matrix. Among all the temperature schemes, Pro2 (the one-platform curing scheme with relatively rapid heating rate) produced highest IFSS and ILSS. Fourier transform infrared spectroscopy analysis demonstrated that the sizing agent can chemically react itself and also react with epoxy resin at temperature 180?°C. The resin rheological data showed that different temperature schemes can considerably impact diffusion behavior of the resin molecules. Hence, the highest interfacial strengths for Pro2 scheme were ascribed to large extent of chemical reactions and good inter-diffusion between components, at the interface region.     

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 matrix yield properties on fragmentation behavior of single fiber composites

Experimental and theoretical investigations have been conducted to study the dependence of fiber fragmentation behavior on matrix yielding properties. The cured Epikote 828 resins with two types of curing agents have almost similar elastic moduli, but different tensile yield strengths. The interfacial chemistry between fiber and epoxy resin is unchanged due to the same constituent of the epoxy resin. The experimental results indicate that the fragmentation behavior of the fibers embedded in the matrix is significantly different for the tested glass fiber treated by γ-glycidoxypropyltrimethoxysilane. The average fragment length decreased with increasing tensile yield strength of resin, which suggests that the interfacial shear strength determined in the fragmentation test should be different depending on the tensile yield strength of resin used. The important phenomenon observed is the transition of the micro-damage mode from matrix crack to interfacial debonding. An elastoplastic shear-lag model was used to calculate the shear stress and fiber tensile stress distributions considering different plastic behaviors of the matrices. The theoretical results indicate that the plastic behavior of the matrix has a large influence on stress transfer. Based on elastic and plastic properties of the matrix, the fiber fragmentation behavior in the matrix is predicted. Experimental and theoretical results are favorably compared.     

Interfacial interaction in carbon fiber/thermoplastic composites

This work was undertaken in order to increase the understanding of the mechanism responsible for fiber/matrix interaction in carbon fiber/thermoplastic composite. From results of previous study on carbon fiber/PEEK composite, which suggested that the formation of the fiber/ matrix interaction was primarily related to a chemisorption mechanism, a study was done of the conditions required to obtain efficient fiber/matrix interaction in PA-12 and PP/carbon fiber composites. The interest in studying carbon fiber composite based on PP and PA-12 was that these two matrices are very different in terms of reactivity, polyamide having many more reactive groups than polypropylene. As expected, due to the non-reactive chemical structure of the polypropylene, fiber/matrix interaction in carbon fiber/PP composite occurred only when the matrix was thermally degraded, i.e. when the composite was molded at high temperature or under long residence time at the melt temperature. For the carbon fiber/PA-12 composite, strong fiber/matrix interaction occurred readily at relatively low molding temperature, i.e. well before thermal degradation of the matrix. It was also found that the short beam shear strength in these composites seems to evolve with molding temperature, and a maximum interfacial strength was observed at a molding temperature corresponding to the thermal degradation of the matrix. This indicates that although matrix degradation often results in strong reduction in the composite performance, some matrix degradation can be beneficial in terms of interfacial mechanical properties. Finally, this work demonstrated that while the formation of fiber/matrix interaction seems to be primarily related to a chemisorption mechanism, the contribution of interphase crystallinity to the interfacial strength is not negligible. In fact, interfacial crystallinity was found to be essential to ensure optimum interfacial strength.     

Preparation of vertically aligned carbon nanotube arrays grown onto carbon fiber fabric and evaluating its wettability on effect of composite

Vertically aligned carbon nanotube (CNT) arrays have been grown onto the carbon fiber fabric using a catalytic chemical vapor deposition (CCVD) method. The as-synthesized CNT arrays are about 20 μm in height, and the nanotube has a mean inner and outer diameter of 2.6 nm, 5.5 nm, respectively. The CNT-grafted carbon fabric shows a hydrophobic property with a contact angle over 145°, and the single CNT-grafted carbon fiber shows a sharp increase of dynamic contact angle in de-ionized water from original 71.70° to about 103°, but a little increase does in diiodomethane or E-51 epoxy resin. However, the total surface energy of carbon nanotube-grafted carbon fiber is almost as same as that of as-received carbon fiber. After CNTs growth, single fiber tensile tests indicated a slight tensile strength degradation within 10% for all different lengths of fibers, while the fiber modulus has not been significantly damaged. Compared with the as-received carbon fibers, a nearly 110% increase of interfacial shear strength (IFSS) from 65 to 135 MPa has been identified by single fiber pull-out tests for the micro-droplet composite, which is reinforced by as-received carbon fiber or CNT-grafted carbon fiber.     

Enhancing the interfacial strength of glass/epoxy composites using ZnO nanowires

This paper investigated the application of ZnO nanowires (ZnO NW) to enhance the interfacial strength of glass/epoxy composites. ZnO NW were grown on glass fibers by hydrothermal method, tensile properties of bare and ZnO NW coated fibers were measured by single fiber tensile testing, wettability of fiber with resin was studied by contact angle measurements and finally the interfacial strength and mechanisms were determined by single fiber fragmentation testing of glass/epoxy composites. The surface coverage of ZnO NW on glass fibers was fairly uniform without formation of major clusters. The coating of ZnO NW slightly reduced the tensile strength and improved the tensile modulus of fibers. Wettability tests showed reduction in contact angles for ZnO NW coated fibers because of enhanced wetting and infiltration of epoxy resin into nanowires. In fragmentation testing of microcomposites, smaller and concentrated interfacial debonding zones for ZnO NW coated fibers indicated good stress transfer and strong interfacial adhesion. A new form of crossed and closely spaced stress patterns were observed for nanowires of high aspect ratios. The interfacial strength of ZnO NW coated fibers increased by at least 109% and by 430% on average, which was attributed to the increased surface area and mechanical interlocking provided by ZnO NW.     

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.     

Maintenance of highly interfacial shear strength by diblock copolymer between carbon fiber and epoxy resin in hostile environment

The environmental resistance properties of carbon fiber (CF), with various surface modifications, reinforcing epoxy resin composites have been studied by a microbond test. The results of cooling–heating cycling between ?40 and 95?°C indicate that the introduction of the flexible poly(n-butyl acrylate) (PnBA) blocks into the interface can effectively decrease the interfacial degradation rate, induced by interfacial thermal stress. After 50 cooling–heating cycles, the interfacial shear strength between CF and epoxy resin was still as high as 32.69?±?2.13?MPa. The results of hygrothermal treatment by immersing the composites in hot water show that assembly morphology of the diblock copolymer hydroxyl-terminated poly(n-butyl acrylate-b-glycidyl methacrylate) (OH-PnBA-b-GMA) at the interface can decrease the interfacial water absorption and thus increase the hygrothermal resistance of the composite. Besides, the length of PnBA block in the diblock copolymer influenced the interfacial properties of the composite in a hygrothermal environment.     

Analysis of single-fiber pull-out from composites by using stress birefringence

During a fiber pull-out test, it is desirable to analyze the stress profiles along the embedded fiber directly within the same time scale as the normal pull-out tests. In the present study, the axial tensile stress profiles of the fiber in a model composite are measured during the single-fiber pull-out tests by using stress birefringence of the fiber. It is concluded from the analysis of the measured stress profiles that an effective radius of matrix, i.e. a radius defining the region of the matrix where the major deformation takes place, is not constant but is an increasing function of the interfacial shear stress. By incorporating the variable values of the effective radius of matrix into the shear-lag model, the axial tensile and the interfacial shear stress profiles are calculated. To accurately estimate the interfacial shear strength, the stress distribution along the embedded fiber and the variability of the effective radius of matrix should be taken into account instead of calculating the interfacial shear strength simply from the pull-out stress and the embedded length.     

Surface and core modification of carbon fibers

Thermal and thermochemical treatments with amines have been shown to improve both the mechanical strengths of carbon fibers and their interfacial bonding forces with polymer matrix. In this report, the wettabilities of the surface-treated carbon fibers were studied by dynamic contact angles with epoxy resin. Two mechanisms occur during the fiber modification processes, namely, the fiber core restructuring and surface etching. The former occurs at elevated temperature and increases the fiber strength significantly. When surface reaction occurs, the number of surface oxides increases to improve the surface wettabilities, which may be observed by the decreased dynamic contact angles. Accompanying the etch-cleaning effects, the fiber strength would also increase initially. Deeper penetration of amine would destroy the graphite crystallinity on fiber surfaces and lower the fiber strength.     

Correlation of the mechanical properties to the fiber–matrix adhesion of Nextel 312™ fiber/BN/Blackglas™ composites

Boron nitride (BN)-coated aluminoborosilicate (Nextel? 312) fibers, produced via ammonia nitridation, along with 'as-received' and 'desized' fibers, were composited in a silicon oxycarbide (Blackglas?) matrix. The mechanical properties, failure properties, and fiber–matrix interfacial chemistry of the composite were investigated. BN treated fiber composites show a 90% improvement in flexural strength and substantial increases in shear strength (short beam shear and Iosipescu) over the 'as-received' fiber composite. The composite fabricated with 'desized' fibers underwent spontaneous delamination during pyrolization, precluding mechanical testing. X-ray photoelectron spectroscopy of the starting materials and of composite fracture surfaces combined with scanning electron microscopy and energy dispersive X-ray spectroscopy indicate that the locus of failure of the BN-coated fiber composite occurs at the matrix/BN coating interface.     

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.     

Interface end theory and re-evaluation in interfacial strength test methods

The experimental results of fragmentation, micro-indentation, pull-out and microdebond tests often exhibit large discrepancies. Since all specimens of the four test methods all have interface ends, the singularity theory of the interface end should be used to evaluate the exactness of the test methods. The eigenvalues of the specimens for the micro-indentation test, pull-out test and microdebond test are calculated and investigated. The results show that the stress singularity of the interface end depends on the Dundurs' parameters and the wedge angles. The interfacial shear strength (IFSS) obtained from the tests loses its rationality if the stress is singular at the interface end. In further analysis, for a carbon fiber-epoxy resin composite, it is found that the microdebond test gives the most reliable IFSS results, if the wedge angle of the resin droplet is less than 40°; the results from the pull-out test are dubious, due to the stress singularity at the interface end. In the micro-indentation test, there is a critical matrix stiffness value for a given fiber, above which the stress at the interface end will be non-singular. The fragmentation test assumes the interfacial shear stress on the fiber fragment of critical length is the IFSS. If debonding does not occur at the interface end, then apparently, the interfacial shear stress on the fiber fragment of critical length is less than the true value of IFSS.     

A Fluoropolymer Coating on Carbon Fibers Improves Their Adhesive Interaction with PTFE Matrix

Carbon fibers were treated in a HF glow discharge in tetrafluoroethylene and octafluorocyclobutane in order to improve their adhesion to poly(tetrafluoroethylene) matrix. As the result of the plasma treatment, a thin (20–140 nm) fluoropolymer coating was deposited onto the fiber surface. The structure of this coating was studied by means of IR spectroscopy, XPS, AFM and SEM techniques. The coating material appeared to be similar to PTFE in its chemical composition but distinguished by branched, partially crosslinked, amorphous structure and included unsaturated chemical bonds. The coating thickness of 70 nm was sufficient to effectively screen the field of molecular forces of the initial substrate, thus, decreasing the surface energy of the fibers and improving their compatibility with the PTFE matrix. The adhesive strength in the PTFE–carbon fiber systems, measured by means of the microbond test, more than doubled upon the plasma treatment (the local interfacial shear strength increased from 10.7 to 29.7 MPa, apparent IFSS from 4.3 to 7.8 MPa), and the interfacial frictional stress increased by 70%. The new composite material consisting of 20% short coated carbon fibers in the PTFE matrix showed better mechanical, thermal and tribological characteristics as compared with the composite reinforced with untreated fibers.     

Effect of the molecular weight of sizing agent on the surface of carbon fibres and interface of its composites

The influence of different molecular weight sizing agent on the performances of carbon fibres and carbon fibres composites were studied. Three different kinds of molecular weight sizing were used. Surface composition of the fibres modified with aqueous sizing and topographies of carbon fibres surface were characterized by X-ray photoelectron spectroscopy (XPS), atomic force microscopy (AFM) and scanning electron microscope (SEM). The interlaminar shear strength and hygrothermal ageing test have been used to study the effect of fibres coatings on the adhesion of surface. The results of the study indicate that the molecular weight of sizing agent has an important influence to the carbon fibres and carbon fibres composites. The high and low molecular weight sizing agent decreased the interfacial shear strengths and hygrothermal ageing of carbon fibres composite. The moderate molecular weight of sizing agent showed an improvement of the interfacial adhesion and hygrothermal ageing.     

Interphase formation and fiber matrix adhesion in carbon fiber reinforced epoxy resin: influence of carbon fiber surface chemistry

The chemistry and morphology of the carbon fiber surface are important parameters which govern the properties of the interfacial region and the adhesion between carbon fibers and polymeric matrix in carbon fiber reinforced polymers. In the presented paper the surface chemistry of the fibers is varied while the surface morphology is left unchanged. We analyze chemical functionality and morphology of carbon fiber surfaces showing different degrees of activation, together with the adhesion of these fibers to an epoxy matrix and the width of the interfacial region between fiber and matrix. An increase of the oxygen and nitrogen concentration of the fiber surface, in particular in form of carboxyl functional groups, results in a significant increase of interfacial shear strength. Also the width of the interphase, as determined by scanning force microscopy in nanomechanical mode, depends on the activation degree of the carbon fibers. However, no direct correlation between interphase width, surface chemistry and fiber matrix adhesion is found, suggesting no direct influence of interphase width on adhesion properties.     

Improvement of surface wettability and interfacial adhesion of poly-(p-phenylene terephthalamide) by incorporation of the polyamide benzimidazole segment

In order to investigate the effect of the polyamide benzimidazole group on the surface wettability and interfacial adhesion of fiber/matrix composites, surface features of two kinds of aramid fibers, poly (p-phenylene terephthalamide) fiber (Kevlar-49) and poly-(polyamide benzimidazole-co-p-phenylene terephthalamide) (DAFIII), have been analyzed by X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM) and contact angle analysis (CAA) system, respectively.The results show that with the incorporation of the polyamide benzimidazole segment, more polar functional groups exist on DAFIII surface. The contact angles of water and diiodomethane on DAFIII surface get smaller. The surface free energy of DAFIII increases to 36.5 mJ/m², which is 2.3% higher than that of Kevlar-49. In addition, DAFIII has a larger rough surface compared with that of Kevlar-49 due to different spinning processes. The interfacial shear strength (IFSS) of DAFIII/matrix composite is 25.7% higher than that of Kevlar-49/matrix composite, in agreement with the observed results from surface feature tests. SEM micrographs of failed micro-droplet specimens reveal a strong correlation between the fracture features and the observed test data.     

Improved mechanical properties of carbon fiber reinforced PTFE composites by growing graphene oxide on carbon fiber surface

The mechanical properties of carbon fiber reinforced polymer composites depend upon fiber-matrix interfacial properties. To improve the mechanical properties of ?bers/PTFE composites without sacri?cing tensile strength of ?bers, graphene oxide (GO) was introduced onto the surface of CFs by chemical vapour deposition (CVD). This hybrid coating increased the wettability and surface roughness of carbon fibers, which led to improved affinity between the carbon fibers and PTFE matrix. The resulting hybrid-coated carbon fiber-reinforced composites showed an enhancement in the short beam strength compared to un-coated carbon fiber composites. Meanwhile, a signi?cant increase of interlaminar shear strength (ILSS), interface shear strength tests (IFSS) and impact property were achieved in the 5-min-modi?ed CFs.