Deformation micromechanics in model carbon fibre-reinforced composites

Raman spectroscopy has been used to study the deformation micromechanics of the single-fibre pull-out test for a carbon fibre/epoxy resin system using surface-treated and untreated versions of the same type of PAN-based fibre. It has been possible to determine the detailed strain distribution along embedded fibres and it has been found that it varies with the level of strain in the fibre outside the resin block. The variation of interfacial shear stress along the fibre/matrix interface has been determined using the balance of forces equilibrium and this has been compared with the single values of interfacial shear strength determined from conventional pull-out analyses. It has been demonstrated that it is possible to identify situations where the interface is well-bonded, partially debonded or fully debonded and also to follow the failure mechanisms in detail. It has been found that the level of interfacial adhesion is better for the surface-treated fibre and that, for the untreated fibre, interfacial failure takes place by the cohesive failure of a weakly-bonded surface skin that appears to be removed by the surface pretreatment process.     

Analysis of the fragmentation test for carbon-fibre/epoxy model composites by means of Raman spectroscopy

The interfaces between high-modulus PAN-(T50) and mesophase pitch-based (P55) carbon fibres and an epoxy matrix have been studied by using the conventional fragmentation test in conjunction with polarised-light optical microscopy. Raman spectroscopy has also been used to follow stress transfer from the matrix to the fibres for the same fragmentation geometries. The level of fibre/matrix adhesion and mechanisms by which the stress is transfered from the matrix to the fibres has been determined from both the stress birefringence patterns and strain-induced Raman band shifts in the fibres. The values of interfacial shear strength have been determined by means of both the conventional analysis and the Raman technique. It is found that the Raman method gives a much more detailed picture of stress transfer in the test specimens and that the two methods give somewhat different values of the interfacial shear strength. The values of interfacial shear stress have been discussed with respect to fibre surface energy, surface chemistry and surface morphology. It was found that the surface chemical functional groups appear to have no direct correlation with interfacial shear strength. Furthermore, it appears that mechanical interlocking due to surface roughness could contribute to the higher values of interfacial shear strength determined for the PAN-based fibre.     

Analysis of the single-fibre pull-out test by means of Raman spectroscopy: Part II. Micromechanics of deformation for an aramid/epoxy system

The single-fibre pull-out test has been analysed for Kevlar-49 fibres in a cold-cured epoxy resin by using both a conventional pull-out experiment and Raman spectroscopy. The interfacial shear strength (ISS) has been estimated from the pull-out force for fibres with a range of embedded lengths. Raman spectroscopy has been used to analyse the distribution of fibre strain in the pull-out test by mapping the variation of strain along an aramid fibre undergoing pull-out from the epoxy resin matrix. At low strains the behaviour follows elastic shear-lag analysis but, as the fibre strain is increased, debonding takes place at the fibre/matrix interface. It is found that this debond propagates along the interface until the entire fibre is debonded. The fibre is then pulled out of the resin matrix by a frictional pull-out process. It is shown that the conventional pull-out experiment produces only an apparent value of ISS and that through a partial-debonding model it is possible to use the interfacial parameters obtained from the Raman analysis to predict the data from the conventional test.     

Crack bridging and fibre pull-out in polyethylene fibre reinforced epoxy resins

An investigation has been undertaken of the stress distributions in high-performance polyethylene fibres bridging cracks in model epoxy composites. The axial fibre stress has been determined from stress-induced Raman band shifts and the effect of fibre surface treatment has been followed using untreated and plasma-treated polyethylene fibres. It is found that when the specimen is cracked, the fibres do not break and stress is transmitted from the matrix to the fibre across the fibre/matrix interface. A debond propagates along the fibre/matrix interface accompanied by friction along the debonded interface. The axial stress distributions in the fibres can be analysed using a partial-debonding model based upon shear-lag theory and it is found that the maximum interfacial shear stress at the bond/debond transition is a function of the debond length. The debonding process has been modelled successfully in terms of the interfacial fracture energy-based criterion developed by Hsueh for the propagation of a debond along a fibre/matrix interface accompanied by constant friction along the interface.     

New evaluation technique of interfacial properties in GFRP

A new method was proposed to evaluate the mechanical properties at the interface between the fibres and the matrix in composites using an embedded single fibre coupon test. A mechanical parameter at the interface (called the interfacial transmissibility, ) was derived from the fibre strength and the apparent stress of the fibre immediately before the first fracture of embedded fibre, _fa. This parameter indicated the degree of the mechanical transmission from the matrix to the fibre through the interface. This avoided some complicated problems such as the stress distribution along fibre fragments and the critical fragment state in a typical single-fibre test. This new method was tried to determine the -values for a fibre glass/epoxy resin with different amounts of a coupling agent at the interface. In order to measure the stress at the first fracture, the fracture process was monitored with a video camera during the single fibre test. The stress values at the first fracture for many coupons were analysed as a function of the three-parameter Weibull distribution. The resulting average stress and its coefficient of variation indicated that the reliability of the measurement for the stress at the first fracture was not less than that obtained by the usual single-fibre test. The change of interfacial transmissibility with amount of the coupling agent revealed the existence of an optimal interface.     

Effect of surface treatment upon the pull-out behaviour of aramid fibres from epoxy resins

A detailed study has been undertaken of the pull-out behaviour of aramid fibres with different surface characteristics from blocks of an epoxy resin matrix. The fibres employed had either no surface treatment (HM), a standard surface finish (HMF) or had been treated with a special epoxy-based adhesion-activating finish (HMA). The point-to-point variation of axial fibre strain along the fibres both inside and outside of the resin matrix has been determined from stress-induced Raman band shifts. This has enabled the distribution of interfacial shear stress along the fibre/matrix interface to be determined and, in combination with scanning electron microscope analysis of the specimens following pull-out testing, the failure mechanisms to be elucidated. It is found that pull out of the HM fibre takes place by a debond propagating along the fibre/matrix interface at a low level of interfacial shear stress. The HMF fibre showed better adhesion to the epoxy matrix with pull out occurring in a complex manner through both separation of the fibre skin and failure at the fibre/finish interface. No evidence of debonding was found for the HMA fibre and failure occurred by fracture of the fibre at the point where it entered the resin block.     

Fracture mechanisms in glass-reinforced plastics

Model glass fibre/polyester resin composites have been made in the form of double cantilever beams and the effect of a small number of fibres on quasi-static crack propagation has been studied by simultaneous plotting of load/deflection curves, measurements of crack length, and observation of the progress of fibre/resin debonding and fibre pull-out. By varying the condition of the fibre surface and the arrangement of the fibres to a limited extent and carrying out subsidiary experiments on single-fibre samples of identical character it has been possible to make direct measurements of all of the important parameters required for an analysis of the macroscopic behaviour in terms of established models of fibre/matrix interaction. Agreement between experimental and calculated fracture energies for these model composites is not highly satisfactory, but it seems clear that the fracture energy of grp is likely to be determined very largely by work done against friction between fibres and matrix after the debonding process has occurred. This conclusion opposes the currently-held view which attributes the largeγ _F values of grp to the fibre/resin debonding mechanism.     

Investigation of morphology-dependent fracture behaviour with the single-fibre pull-out test

In this study attempts are made to answer the question of how the morphology, and especially the transcrystallinity, influences the fibre/matrix adhesion in carbon-fibre/poly(phenylene sulphide) composites. Therefore, single-fibre pull-out measurements are performed with samples containing high-modulus (HM) and high-strength (HS) fibres that had been subjected to different thermal treatments. Transcrystallinity leads to a prevailing brittle fracture process in the interface and to higher values of the apparent shear strength. Samples with HS fibres and high crystallinity show an unexpected ductile fracture behaviour at a high apparent shear strength level.     

Effect of water on the mechanical adhesion of the glass/epoxy interface

In recent years, the quality of the fibre/matrix bonding in polymer composites has been quantified by means of a single mechanical parameter, the interfacial shear strength, based on measurements made using micromechanical techniques. It has gradually appeared, however, that this parameter is both ambiguous in terms of its physical meaning and, at the same time, difficult to measure reliably in many cases. Moreover, different micromechanical techniques yield differing values of the interfacial shear strength. Finally, it has been suggested in a few studies that it may not be the critical factor governing fibre/matrix debonding. In this paper an energy balance approach is proposed, by which the degree of fibre/matrix bonding is now quantified by means of the interfacial energy, as a function of the fibre geometrical and mechanical characteristics, the stress transfer length and the debonding length. The validity of the approach is discussed in the case of the single-fibre composite test, in which progressive fragmentation of a single brittle fibre in a more ductile polymeric matrix takes place, using data for E-glass fibres embedded in epoxy, both in the dry state and in the presence of hot distilled water.     

Shear strength and fracture toughness of carbon fibre/epoxy interface: effect of surface treatment

Textile-reinforced composites have become increasingly attractive as protection materials for various applications, including sports. In such applications it is crucial to maintain both strong adhesion at fibre–matrix interface and high interfacial fracture toughness, which influence mechanical performance of composites as well as their energy-absorption capacity. Surface treatment of reinforcing fibres has been widely used to achieve satisfactory fibre–matrix adhesion. However, most studies till date focused on the overall composite performance rather than on the interface properties of a single fibre/epoxy system. In this study, carbon fibres were treated by mixed acids for different durations, and resulting adhesion strength at the interface between them and epoxy resin as well as their tensile strength were measured in a microbond and microtensile tests, respectively. The interfacial fracture toughness was also analysed. The results show that after an optimum 15–30 min surface treatment, both interfacial shear strength and fracture toughness of the interface were improved alongside with an increased tensile strength of single fibre. However, a prolonged surface treatment resulted in a reduction of both fibre tensile strength and fracture toughness of the interface due to induced surface damage.     

Plasma surface modification of advanced organic fibres

The interlaminar shear strength, interlaminar fracture energy, flexural strength and modulus of extended-chain polyethylene/epoxy composites are improved substantially when the fibres are pretreated in an ammonia plasma to introduce amine groups on to the fibre surface. These property changes are examined in terms of the microscopic properties of the fibre/matrix interface. Fracture surface micrographs show clean interfacial tensile and shear fracture in composites made from untreated fibres, indicative of a weak interfacial bond. In contrast, fracture surfaces of composites made from ammonia plasma-treated fibres exhibit fibre fibrillation and internal shear failure as well as matrix cracking, suggesting stronger fibre/matrix bonding, in accord with the observed increase in interlaminar fracture energy and shear strength. Failure of flexural test specimens occurs exclusively in compression, and the enhanced flexural strength and modulus of composites containing plasma-treated fibres result mainly from reduced compressive fibre buckling and debonding due to stronger interfacial bonding. Fibre treatment by ammonia plasma also causes an appreciable loss in the transverse ballistic impact properties of the composite, in accord with a higher fibre/matrix interfacial bond strength.     

Thermomechanical behaviour of interfacial region in carbon fibre/epoxy composites

A study of the thermomechanical stability of the fibre-matrix interphase in carbon/epoxy composites has been carried out. The thermodynamic work of adhesion has been evaluated at room temperature by wetting measurements. The interfacial shear stress transfer level τ for sized and desized carbon fibre has been measured as a function of temperature by means of a single-fibre fragmentation test. As the test temperature increased τ values were found to decrease, with values being higher for the desized carbon fibre. The dependence of interfacial shear stress transfer on bulk matrix mechanical properties (modulus and shear strength) has also been discussed. Dynamic mechanical measurements performed on single-bundle composites confirmed the better thermomechanical stability of the desized fibre interphase.     

Interfacial failure in poly(p-phenylene benzobisoxazole) (PBO)/epoxy single fibre pull-out specimens

The pull-out behaviour of poly(p-phenylene benzobisoxazole) fibres from an epoxy resin has been shown to follow that predicted by the elastic stress transfer shear-lag model at low applied strains, but at higher matrix strains a partial debonding model was more suitable. Debonding of the fibre/matrix interface led to interfacial failure where only friction resisted fibre extraction. Raman spectroscopy was able to quantify this level of friction and together with in situ optical microscopy proved an excellent method for the close monitoring of the frictional pull-out process. The effect of fibre surface treatment was also studied. The interfacial shear stress values from the heat-treated and corona-treated fibres showed only small differences. The failure processes were examined further using scanning electron microscopy and clean fibre pull-out was observed with the heat-treated fibre whereas fracture of the free fibre occurred with the corona-treated fibre.     

电晕处理对高性能PBO纤维的表面性能及其界面粘接性能的影响

对高性能PBO纤维表面进行了电晕处理,优化了其处理工艺。用XPS,FT-IR和SEM研究了处理前后纤维表面化学结构及物理结构的变化,通过单丝拔出试验和短梁剪切试验评价了PBO纤维与树脂基体的微宏观界面粘接性能。结果表明:经电晕处理后,PBO纤维表面含氧量增多,表面浸润性得到改善,单丝拔出的PBO-环氧界面剪切强度(IFSS)提高了25.6 ％,但短梁剪切强度(ILSS)的提高不明显。     

Effects of fibre volume fraction on the stress transfer in fibre pull-out tests

The elastic stress transfer taking place across the fibre/matrix interface is analysed for the fibre pull-out test by means of both micromechanics and finite element (FE) analyses. A special focus has been placed on how fibre volume fraction, V_f, affects the interface shear stress fields in the model composites containing both single and multiple fibres. In a so-called ‘three-cylinder model’, where a fibre, a matrix and a composite medium are coaxially located, the constraint imposed on the central fibre due to the surrounding fibres is properly evaluated. It is shown in the FE analysis that the differences in stress distributions between the composite models containing single and multiple fibres become increasingly prominent with increasing V_f. The principal effect of the presence of surrounding fibres in the multiple-fibre composite model is to suppress effectively the development of stress concentration near the embedded fibre end and thus eliminate the possibility of debond initiation from this region for all V_f considered. This is in sharp contrast to the single-fibre composite model, in which the interfacial debond can propagate from the embedded end if V_f is larger than a critical value. These findings are essentially consistent with the results from micromechanics analysis on the same specimen geometry. The implications of the results for the practical fibre pull-out test as a means of measuring the interface properties are discussed.     

Fragmentation in alumina fibre reinforced epoxy model composites monitored using fluorescence spectroscopy

It has been found that well-defined fluorescence R₁ and R₂ lines can be obtained from PRD-166 alumina-zirconia fibres and that the fluorescence R lines shift with applied stress. They are found to shift to higher wavenumber when subjected to tensile deformation and to lower wavenumber in compression. The stress-sensitive fluorescence R₂ line has been used to map the distribution of stress along PRD-166 fibres embedded in an epoxy resin matrix cured under different conditions. It has been shown that the distributions of stress along the PRD-166 fibres at different levels of matrix strain are consistent with those predicted by conventional shear-lag analysis. The interfacial shear stress has been derived from the point-to-point variation of stress along the fibre. The fluorescence technique has also been used to map the stress distribution along a PRD-166 fragment in an epoxy matrix during a single-fibre fragmentation test where it is found that debonded regions propagate along the fibre fragments during loading, after initial fragmentation has occurred.     

Effect of humidity during manufacturing on the interfacial strength of non-pre-dried flax fibre/unsaturated polyester composites

The influence of moisture content in the environment during manufacture of a novel cobalt-free UP matrix reinforced with flax fibres, on the fibre–matrix adhesion was studied. Flax surface energy was experimentally determined by measuring contact angles on technical fibres, using the Wilhelmy technique and the acid–base theory. The mechanical strength of the interface under different humidity conditions was characterized by the critical local value of interfacial shear stress, τ_d, at the moment of crack initiation, which was assessed by single-fibre pull-out tests. Differential scanning calorimetry and X-ray photoelectron spectroscopy analysis gave further insight into the topic. The results suggest that the effect of humidity during manufacturing on the composite interface might be limited. However, longitudinal composite strength decreased somewhat for composites produced in humid conditions, showing that there is some detrimental effect of high levels of moisture during cure on the fibre mechanical performance, likely caused by some fibre degradation.     

Deterministic method for predicting the strength distribution of a fibre bundle

Owing to the non-strain hardening plastic behaviour of the aluminium matrix and the weak fibre/matrix interface, it has been shown that the strength of a carbon fibre-reinforced aluminium matrix composite made by diffusion bonding of prepreg layers can be derived from the corresponding fibre bundle strength. Application of Coleman's model to predict bundle strength leads to the conclusion that the composite must break when 15% of the fibres are broken. This greatly overestimates the experimental composite strength. Overestimations made by using the Coleman model are due to some implicit assumptions which are not valid in the case under consideration and which may consequently not describe our material. A new approach is proposed for the calculation of the strength distribution of a fibre bundle, based on the same fracture mechanism (fibres fracture progressively until the catastrophic fracture) but without restrictive assumptions. The real interpolated experimental fibre strength distribution (and not the Weibull distribution) is taken into account to predict bundle strength. The proposed method clearly shows the limit of strength prediction, in term of bundle size (number of fibres and gauge length). The risk of making predictions following the Weibull distribution out of the range of the observations (through single-fibre tensile tests) is demonstrated.     

Interface and fracture of carbon fibre reinforced Al-7 wt% Si alloy

The interface structure in an aluminium-7 wt% silicon alloy reinforced with carbon fibres has been investigated using analytical electron microscopy. Crystals of aluminium carbide (Al₄C₃) have been identified in interface regions and their structure and growth are discussed. Mechanical properties of the composite have been measured and fracture behaviour studied using acoustic emission analysis in parallel with microstructural examination. The results indicated that the aluminium carbide interfacial reaction had produced a strong fibre matrix bond, but reduced the fibre strength and embrittled the matrix. Consequently, whole fibre bundles failed in a brittle manner in the longitudinal direction with limited pull-out of individual fibres. The findings are discussed in relation to the method used to manufacture the composite.     

Evaluation of interfacial properties between carbon fibres and semicrystalline thermoplastic matrices in single-fibre composites

The interfacial properties between pitch-based carbon fibre and semicrystalline thermoplastic matrices have been investigated by using the fragmentation test on single-fibre composites. For this purpose, fibres with seven different degrees of surface oxidation were prepared. From the fragmentation test, it was found that oxidization of carbon fibre reduces the fibre fragment length. Further, the length is also influenced by the nature of resin used as matrix. The morphology of crystallites formed on the fibres has been studied. Based on these results, the interfacial properties of carbon fibre and thermoplastic resins are discussed.