Failure micromechanisms in continuous carbon-fibre/epoxy-resin composites

This study is concerned with the influence of the strength of the fibre/matrix interface on the strength and failure process in uniaxial arrays of carbon fibres in an epoxy resin. A batch of high-strength carbon fibres has been supplied with several levels of an oxidative surface treatment to produce composites with various interface strengths. Tensile tests have been conducted on single fibres, on loose bundles and on tows impregnated with an epoxy resin. Further tests have been conducted to estimate the interface strength. A hybrid-tow test configuration has then been used to follow the sequence of failure within a single tow of the carbon fibre in a uniaxial composite. The results indicate that the fibre strength is affected only slightly by the surface treatment, the strength of impregnated tows is reduced, and their mode of failure and that of the hybrid tows is affected significantly.     

Some aspects of interface adhesion of electrolytically oxidized carbon fibres in an epoxy-resin matrix

A comprehensive investigation of the adhesion at the interface of a carbon fibre in an epoxy resin was made. The fibre surfaces were modified, to increase their adhesion to resin, by an electrolytic surface treatment which was applied at various current densities. Subsequent changes in the fibre properties relating to possible mechanical, physical and chemical contributions to adhesion were monitored. Tensile tests on single fibres indicated that the treatment altered the strengths of the fibres, which were found to have their highest values and to be least variable at an optimum adhesion level. A method was developed to estimate the strength of the fibres in the resin, this confirmed the single-fibre data. A novel method of labelling the acidic sites by producing adsorption isotherms was developed to identify surface functionality. Surface acidity correlated well with adhesion levels. Single-fibre pull-out tests, modelled using a new combination failure criterion and fragmentation tests, indicated that the optimum adhesion level for this fibre/resin system was achieved with an electrolytic treatment at 25 C m^–2. The principal effects of this treatment were considered to be due to chemical modification of the fibre surface coupled with the removal of a loosely adherent surface layer.     

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.     

The evaluation of the strength distribution of silicon carbide and alumina fibres by a multi-modal Weibull distribution

The strengh distributions of silicon carbide and alumina fibres have been evaluated by a multimodal Weibull distribution function. This treatment is based on the concept that the fracture of the fibre is determined by competition among the strength distributions of several kinds of the defect sub-population. Since those fibres were observed to have two types of fracture mode, the evaluation of a bi-modal Weibull distribution was performed in comparison with the single Weibull distribution usually employed. The accuracy of the fit for these two distributions was judged from maximum logarithm likelihoods and cumulative distribution curves. The result showed that the logarithm likelihood calculated using the bi-modal Weibull distribution function gave a larger value, as compared with those using the single Weibull distribution function. The curve predicted from the former function was also in good agreement with the data points. In addition, the strength distribution and the average value at a different gauge length were extrapolated from the Weibull parameters estimated at the original gauge length. In this case, also, the bi-modal Weibull distribution gave a more accurate prediction of the data points.     

Statistics of single‐fibre tensile strength incorporating spatial distribution of microcracks

The random distribution of single‐fibre tensile strength has been commonly characterized by the two‐parameter Weibull statistics. However, the calibrated Weibull model from one set of strength data at a given gauge length cannot accurately predicts the strength variation of the fibre at different gauge lengths. Instead of presuming the two‐parameter Weibull distribution or any other specific statistical distribution for the single‐fibre strength to begin with, this work proposes an approach to incorporating the appropriate spatial flaw distribution within a fibre and synchronizing multiple sets of tensile strength data to evaluate the single‐fibre strength distribution. The approach is examined and validated by published single‐fibre strength data sets of glass, ceramic and synthetic and natural carbon fibres. It is shown that the single‐fibre strength statistics does not necessarily always follow the two‐parameter Weibull distribution.     

Strength and adhesion characteristics of elementary flax fibres with different surface treatments

It is known that the best flax fibres can compete in terms of mechanical properties with glass fibres. However, during the manufacturing process flax fibres are often damaged, and hence, the properties can be lowered. Furthermore, these properties change from batch to batch (depending on the time and place of harvest), which means that they are somewhat unpredictable. The most affected fibre property is strength, which can vary in very wide interval due to defects introduced by the manufacturing process. Therefore, there is a need for a simple but reliable testing procedure that allows the estimation of the strength of flax fibres, so called quality control. Regarding the final goal, that is the development of natural fibre composites, another crucial property is the fibre/matrix adhesion. The objective of this study is to investigate the possibility to use the single fibre fragmentation test to characterize strength distribution of flax fibres and to evaluate the adhesion. Untreated flax fibres and fibres coated by a special surface treatment are used. Fragmentation tests are performed on flax fibres embedded in thermoset, vinylester and polyester, resins. Results show that there is a definite improvement in interfacial strength when a fibre surface treatment is applied. Fibre strength distribution is obtained from SFFT and compared with limited results available from single flax fibre tests.     

Influence of temperature on fracture initiation in PET and PA66 fibres under cyclic loading

The fatigue of single thermoplastic fibres has been well documented to occur in a reproducible manner when they are subjected to certain cyclic loading conditions. The fatigue fracture morphologies of these fibres are very distinctive and differ markedly from other types of failure. This type of behaviour, which is clearly seen with the unambiguous tests on single fibres, must reflect behaviour of fibres in more complex structures which are subjected to cyclic loading. Only limited numbers of reports have, however, shown similar fracture morphologies with fibres extracted from fibre bundles embedded in a matrix material such as rubber. Usually the fractured ends of fibres taken from structures are seen to be shorter than those obtained in single fibre tests and also they show more complex and confused crack growth. The present study reveals that the low thermal conductivity of the fibres, exacerbated when they are embedded in a rubber matrix, leads to very high temperature rises, which is not the case in single fibre tests and under these conditions, crack initiation occurs across the fibre section instead of being restricted to the near surface region. Tests on single fibres at temperatures up to and beyond the glass transition temperature have shown how the fracture morphologies become modified. The fatigue process has been seen to become generalised throughout the fibre and failure occurs due to the coalescence of several cracks, some of which are initiated in the core of the fibre. In all cases, the cracks can be seen to have been initiated by solid inclusions in the fibres.     

Assessment of the tensile properties of coir,bamboo and jute fibre

Natural fibres are studied as alternatives for man-made fibres to reinforce composites while keeping the weight lower. The assessment of the value of some commonly available tropical fibres for the composite industry starts with the determination of the strength, E-modulus and strain to failure through single fibre tensile tests. The mean strength and standard deviation is calculated following the normal and Weibull distribution resulting in the questionable benefit of applying the Weibull distribution. Furthermore, a correction method assesses the real fibre elongation from the measured clamp displacement. This procedure seems to be useful for strong, brittle fibres to produce more reliable results for the E-modulus and strain to failure.     

The size effects on the mechanical behaviour of fibres

The size of a fibre affects its mechanical properties and thus is of theoretical and practical importance for studies of the rupturing process during loading of a fibrous structure. This paper investigates the overall effects of length on the mechanical behaviour of single fibres. Four types of fibres, ranging from brittle to highly extensible, were tested for their tensile properties at several different gauge lengths. Different from most previous studies where the focus has been on the gauge length effects on a single property such as fibre strength or breaking strain, this paper look comprehensively into the effects of length on all three of the most commonly studied mechanical properties, namely strength, breaking strain and initial modulus. Particular emphasis is placed on initial modulus and on the interactions between all three parameters. Influences of strain rate and fibre type on the size effects are also investigated. The effect of potential fibre slippage on experimental error is examined. An image analysis method is used to measure the real fibre elongation in comparison to the same fibre elongation obtained directly from an Instron tester. Finally, a statistical analysis is carried out using the experimental data to test the fitness of the Weibull theory to polymeric fibres. This was done as the Weibull model has been extensively utilized in examining fibre strength and breaking strain, although it is supposed to be valid only for the so-called classic fibres to which more extensible polymeric fibres do not belong. This revised version was published online in November 2006 with corrections to the Cover Date.     

Effect of hydrothermal ageing on bond strength

Changes in the fibre/resin interfacial zone due to hydrothermal ageing can be detected using the TRI microbond technique for measuring interfacial shear strength. The procedure involves exposing fibre/resin microdroplet assemblies to the specified environmental condition for a given time and comparing their interfacial shear strengths with those of unaged specimens. We have investigated the effect of hydrothermal exposure on Kevlar^® 49, AS4 carbon and E-glass fibres embedded in Epon 828 thermosetting resin and two thermoplastic resins (polyethylene and polycarbonate). For the fibres embedded in Epon 828 and polycarbonate resins, consistent and significant bond strength reductions (13–50%) were obtained after refluxing in water at 88°C. These reductions could be partially or completely reversed, depending on the fibre/resin system. In contrast, interfacial shear strengths for the same three fibres embedded in polyethylene resin were increased irreversibly by 36 to 46% upon exposure to water at 88°C for 24 h. Evaluation of these results suggests that the mechanisms of bond strength changes due to hydrothermal ageing may be different for various combinations of fibres and resins.     

The role of sizing resins in carbon fibre-reinforced polyethersulfone (PES)

The role of sizing resin in carbon fibre-reinforced polyethersulfone has been studied using surface-treated Type A carbon fibre sized with different polymeric coatings. To investigate their influence on the adhesion of the carbon fibre to the matrix, the single embedded filament fragmentation test was used. Sized carbon fibres showed a higher interfacial shear strength than the unsized ones. Analysis by time-of-flight secondary ion mass spectrometry suggests that this arises from a strong interaction between sizing resin, the fibre and the matrix.     

The effect of fibre sizing on fibres and bundle strength in hybrid glass carbon fibre composites

Tests have been carried out on single carbon fibres supplied in the sized and unsized conditions, as well as impregnated tows and tows in a glass–carbon fibre hybrid composite of the same fibre. The results were analysed using a Weibull distribution for the strengths of the reinforcing fibres and composites. The tensile strength of the single fibres appeared to be unaffected by the sizing of the filaments. In the case of the impregnated tows, an increase in characteristic strength of 7% was observed for the unsized fibres. The strength of the impregnated tows in hybrid composites was seen to be 15% higher than those tested in air. This can be attributed to the “hybrid effect”. This revised version was published online in November 2006 with corrections to the Cover Date.     

Statistical fracture of E-glass fibres using a bundle tensile test and acoustic emission monitoring

Mechanical strength studies have been carried out on fibre bundles used in composite manufacturing. The variability in mechanical properties of glass fibres has been studied using bundles of about 2000 filaments. The fibre strength distributions were analysed using the survival probability-applied strain (S–ε) curve, in relation with various experimental conditions. We also examine the effect of lubricant’s viscosity on the fracture behaviour of E-glass fibre bundles. Acoustic emission (AE) was monitored during the bundle tensile tests in order to verify that individual filament failures are statistically independent. On tensile tests with lubricated bundles of E-glass fibres, it is shown that each individual fibre break can be detected using AE. Hence, AE monitoring of a lubricated bundle of E-glass fibres provides a convenient and relatively quick method to obtain the Weibull parameters of strength distribution.     

Weibull analysis of strength-length relationships in single Nicalon SiC fibres

Nicalon SiC fibre is naturally brittle and offers high-temperature application in fibrous composites. Due to the randomly distributed flaws along the fibre, the statistical variability in single-fibre strength is obvious. In this paper, the effect of heat-cleaning procedures on Nicalon fibres has been investigated, and the statistical strength and variability of single Nicalon fibres have been characterized in tension and compared. Experimental results show that the strengths of single Nicalon fibres among the three types of heat-cleaning procedures are less than that of as-received unsized fibres by 22–30%. In addition, both the failure load and the failure stress of the fibres, for a given gauge length (50 mm) and yarn cross-section, can be well fitted to a two-parameter Weibull distribution. The effect of gauge length over the range from 10–175 mm, holding the strain rate constant, was also studied. The logarithmic strength-length plots show that the strength of single Nicalon fibres follows the weakest-link rule.     

Effects of HF treatments on tensile strength of Hi-Nicalon fibres

Tensile strengths of as-received Hi-Nicalon fibres and those having a dual BN–SiC surface coating, deposited by chemical vapour deposition, have been measured at room temperature. These fibres were also treated with HF for 24 h followed by tensile strength measurements. Strengths of uncoated and BN–SiC coated Hi-Nicalon fibres extracted from celsian matrix composites, by dissolving away the matrix in HF for 24 h, were also determined. The average tensile strength of uncoated Hi-Nicalon was 3.19±0.73 GPa with a Weibull modulus of 5.41. The Hi-Nicalon–BN–SiC fibres showed an average strength of 3.04±0.53 GPa and Weibull modulus of 6.66. After HF treatment, the average strengths of the uncoated and BN–SiC coated Hi-Nicalon fibres were 2.69±0.67 and 2.80±0.53 GPa and the Weibull moduli were 4.93 and 5.96, respectively. The BN–SiC coated fibres extracted from the celsian matrix composite exhibited a strength of 2.38±0.40 GPa and a Weibull modulus of 7.15. The strength of the uncoated Hi-Nicalon fibres in the composite was so severely degraded that they disintegrated into small fragments during extraction with HF. The uncoated fibres probably undergo mechanical surface damage during hot pressing of the composites. Also, the BN layer on the coated fibres acts as a compliant layer, which protects the fibres from mechanical damage during composite processing. The elemental composition and thickness of the fibre coatings were determined using scanning Auger analysis. Microstructural analyses of the fibres and the coatings were done by scanning electron microscopy and transmission electron microscopy. Stengths of fibres calculated using average and measured fibre diameters were in good agreement. Thus, the strengths of fibres can be evaluated using an average fibre diameter instead of the measured diameter of each filament. © 1998 Kluwer Academic Publishers     

SWNT composite coatings as a strain sensor on glass fibres in model epoxy composites

The preparation of a model glass-fibre/epoxy composite with single-walled carbon nanotubes (SWNTs) incorporated as a strain sensor on the fibre surface is described. A micromechanical study of stress transfer at the fibre–matrix interface followed using Raman spectroscopy properties is reported. The SWNTs were distributed along the fibre surface either by dispersing them in an amino-silane coupling agent or coating with an epoxy resin solution containing the SWNTs. The point-by-point mapping of the fibre strain in single fibre fragmentation tests has been undertaken for the first time using SWNTs on the fibres and the interfacial shear stress distribution along the fibre length was determined using the embedded SWNTs. The behaviour was found to be consistent with the classical shear-lag model. The effects of SWNT type and preparation procedure on the sensitivity of the technique were evaluated and optimized from single fibre deformation tests.     

Characterisation of carbon fibres recycled from carbon fibre/epoxy resin composites using supercritical n-propanol

Three different PAN based carbon fibres (Toray T600S, T700S and Tenax STS5631) were recycled from epoxy resin/carbon fibre composites using supercritical n-propanol. The recycled carbon fibres were characterised using single fibre tensile tests, SEM, XPS and micro-droplet test. The tensile strength and modulus of the recycled carbon fibre was very similar to the corresponding as-received carbon fibres. However, the surface oxygen concentration decreased significantly, which caused a reduction of the interfacial shear strength with epoxy resin.     

Effect of viscous flow on the thermal residual stresses in a monofilament SiC/borosilicate glass composite

Residual strains of SiC (SCS-6) single fibres embedded between borosilicate slides were measured by comparing their post-fabricated in situ lengths with their original lengths as a function of processing temperature and load in an open die. If cooled without load the residual strains agreed with the values one would expect if the stress-free temperature was taken to be the strain point of the glass. However, if cooled under load, the residual strains were found to be significantly enhanced, and increased linearly with the applied load, but were insensitive to processing temperature. A hydrodynamic model, where glass flow normal to the vertically applied pressure entrains the embedded fibres and results in the enhanced residual strains, is proposed. The implications of these results in calculating thermal residual stresses in viscous media are discussed. At higher applied loads, the fibre edges broke into smaller fragments. The fragment length distribution was measured and analysed using Weibull statistics. Heat treatment of the fibres at 1600 °C for 4 h in vacuum, resulted in approximately a 50% decrease in their strength and critical length as compared to the as-received fibres. The Weibull moduli, however, were not affected by the heat treatment.     

Experimental determination of the true epoxy resin strength using micro-scaled specimens

In fibre reinforced composite materials, the matrix is the continuous phase, but the inter-fibre distance is rather small. The strength and the capability of plastic deformation is controlled by the matrix physics properties as well as by the acting stress state and the stressed volume. A new method is explained to produce fibres from epoxy resin. The single fibre strength was measured according to the standard test method for single fibre tests. The measured strength data of these thin epoxy resin fibres is close (60%) to the theoretical strength. The mechanism of fracture was identified by fractographic studies as cohesive failure initiated at pre-existing voids or void nucleation and growth. Before final rupture, the fibres showed necking and plastic deformation, which is a surprising behaviour for a brittle epoxy resin.