A method for the chemical anchoring of carbon nanotubes onto carbon fibre and its impact on the strength of carbon fibre composites

This article proposes an alternative way to use carbon nanotubes to improve the performance of carbon fibre-reinforced composites. A chemical process, based on esterification of surface groups, is used to anchor nanotubes onto carbon fibre surface. Anchored nanotubes form a network surrounding the carbon fibres. After CNT anchoring, the tow is impregnated with an epoxy resin and tensile tests are performed on this minicomposite sample. By enhancing matrix properties and fibre/matrix interface, the CNT network has a significant influence on the composite strength.     

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.     

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.     

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.     

Failure characteristics in carbon/epoxy composite tows

In this paper the failure mechanisms of unidirectional aligned carbon fibre/epoxy composites are investigated. Experimental results are presented for the strength of carbon/epoxy composite tows, as well as for single carbon fibres supplied in the sized and unsized condition. Laser Raman spectroscopy was used in this study to assess the effect of fibre breaks on the stress distribution within a composite. Fibre stress mapping of composite tows using laser Raman spectroscopy showed redistribution due to fibre failure and a value of the stress concentration factor, K_r, was obtained. The results were analysed using a Weibull distribution for the strength of the reinforcing fibres and composite.     

Investigation of the strength of surface-treated carbon fibres embedded in resin, by means of model composite tests

The strength of single fibres of carbon embedded in epoxy resin has been estimated by continuous monitoring of fragmentation tests on single embedded fibres. These fibres had previously been treated to enhance their adhesion to the resin, and the effect of this treatment on the fibre strength is studied. The data generated have been analysed by using an adapted Weibull model which includes the influence of the ‘ineffective’ length at each fibre break. Weibull parameters determined from this analysis have been compared with those from tests carried out on fibres in free air. Similar Weibull moduli are obtained and, although absolute values of strength differ, similar trends are observed and a peak in strength is observed at an intermediate level of treatment in both sets of results.     

Photoelastic study of the durability of interfacial bonding of carbon fibre-epoxy resin composites

The physical techniques of polarizing microscopy, including the quantitative measurements of small optical retardations, have been used to investigate elastic fields adjacent to short carbon fibres in epoxy resin composites. The elastic fields associated with shear stress distribution along the fibre-matrix interface have been employed to monitor the initiation of interface debonding during hot (100 °C) water uptake. By examining the development of stress birefringence during resin swelling in the resin adjacent to individual fibres, the differences in the durability of interfacial bonding and the fibre failure modes for differently coated fibres have been obtained. The results show that the state of self-stress in model composites, comprising a single carbon fibre in a film of epoxy resin, can, by immersion in hot distilled water, be enhanced to such an extent that the axial tension in the fibre can be sufficient to initiate fibre fracture. The results also show that, for fibres that have been given certain proprietary surface treatments, the fibre fractures by different failure modes.     

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.     

Tensile strength of glass fibres with carbon nanotube–epoxy nanocomposite coating

A study has been made of a concept of ‘healing’ coatings applied onto the brittle fibre surface to reduce the stress concentrations and thus to improve the reinforcing efficiency in a composite. Coatings made from neat epoxy and carbon nanotube (CNT) reinforced epoxy nanocomposite were applied onto the individual glass fibres as well as rovings. It is shown that the 0.3 wt.% CNT–epoxy nanocomposite coating gave rise to a significant increase in tensile strength of the single fibre for all gauge lengths, better than the neat epoxy coating. The results on glass fibre roving also indicated a clear beneficial effect of nanocomposite impregnation on tensile strength. The rovings impregnated with the CNT nanocomposite exhibited a more uniform strength distribution and higher strengths than those impregnated with the neat epoxy. The changes in prevailing failure mechanisms influenced by the epoxy and nanocomposite coatings have been identified.     

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.     

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.     

Fibre fragment distribution in a single-fibre composite tension test

Single fibre fragmentation tests are performed for brittle fibres with Weibull strength distribution and different surface treatments. The fragmentation process is modelled and closed-form expressions for break spacing distribution are obtained. The model accounts for the effect of finite fibre length on the initial fragmentation as well as for break interaction on the advanced fragmentation stage. It is assumed that the exclusion zone due to fibre–matrix interface failure and stress recovery in the fibre is linearly dependent on the applied load. This assumption is validated experimentally. The derived theoretical average fragment length dependence on applied load is used to determine the fibre strength distribution parameters and the effective interfacial shear stress for carbon/epoxy single fibre composites with different fibre surface treatment and for glass/vinylester single fibre composite. Fragment length distribution is predicted for several load levels. Predictions are in good agreement with experimental data.     

‘Bundle-debond’ technique for characterizing fibre/matrix interfacial adhesion

An experimental technique called bundle-debonding, has been developed for characterizing the interfacial adhesion of fibre bundles and matrix. The specimen is double-notched and contains a partially embedded fibre layer in between the notches. When a tensile load is applied at the specimen ends, the load transfer across the notch and between two pieces of matrix, occurs through the interface between a single layer of fibres and matrix. Kevlar-29 (Kelvar is a registered trademark of E.I. duPont de nemours) fibre tows were used in conjunction with a solid phenolic resin to fabricate the specimens. Experiments were conducted at various embedded lengths resulting in interfacial debond. A simple shear-lag analysis was carried out to determine the interfacial shear strength. The interfacial shear strength of Kevlar-29/phenolic resin has been determined to be 15 MPa. This technique is promising for application on several fibre/matrix systems, specially for fibres of extremely low nominal diameter, supplied as tows.     

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.     

Role of fibre surface—matrix combination in carbon fibre reinforced epoxy composites

The effect of surface treatment of carbon fibres with concentrated as well as dilute nitric acid on the mechanical properties of carbon fibres has been reported. The role of the fibre—matrix interface in carbon fibre reinforced epoxy resin composites has been studied. Composites have been made both with untreated and surface treated carbon fibres and epoxy resin Araldite LY556 with different hardeners. Mechanical properties as well as fracture behaviour of these composites suggest that it is the physical interlocking between the fibres and the matrix, along with some chemical bonding between the two, and not the pure chemical bonding which yield better composites.     

The structure of the interface in carbon fibre composites by scanning Auger microscopy

Scanning Auger microscopy (SAM) has been used to study the fibre/matrix interface of composite materials. This novel application of Auger spectroscopy enables further understanding of the mechanism of failure in composites when applied to carbon fibre-reinforced epoxy material. Initial work was carried out on carbon fibres prior to their incorporation into the resin matrix. Auger spectroscopy can be used to detect the presence of thin polymeric layers on the carbon fibres if a suitable, matrix-specific element is chosen to form the scanning Auger image. Two composite materials have been investigated. They differ from each other by the fracture mechanisms. In the case of unidirectional continuous fibre composites, a high volume fraction of conducting carbon fibres makes Auger analysis possible although the failure surface is predominantly polymer residues. For short-fibre composites the technique is more difficult considering the low volume fraction of fibres, but Auger spectroscopy enables the identification of microfailure mechanism and of the effect of fibre surface treatment on the failure mode.     

Effects of fibre/matrix adhesion on carbon-fibre-reinforced metal laminates—I.: Residual strength

The role of interfacial adhesion between fibre and matrix on the residual strength behaviour of carbon-fibre-reinforced metal laminates (FRMLs) has been investigated. Differences in fibre/matrix adhesion were achieved by using treated and untreated carbon fibres in an epoxy resin system. Mechanical characterisation tests were conducted on bulk composite specimens to determine various properties such as interlaminar shear strength (ILSS) and transverse tension strength which clearly illustrate the difference in fibre/matrix interfacial adhesion. Scanning electron microscopy confirmed the difference in fracture surfaces, the untreated fibre composites showing interfacial failure while the treated fibre composites showed matrix failure. No clear differences were found for the mechanical properties such as tensile strength and Young's modulus of the FRMLs despite the differences in the bulk composite properties. A reduction of 7·5% in the apparent value of the ILSS was identified for the untreated fibre laminates by both three-point and five-point bend tests. Residual strength and blunt notch tests showed remarkable increases in strength for the untreated fibre specimens over the treated ones. Increases of up to 20% and 14% were found for specimens with a circular hole and saw cut, respectively. The increase in strength is attributed to the promotion of fibre/matrix splitting and large delamination zones in the untreated fibre specimens owing to the weak fibre/matrix interface.     

The influence of fibre surface properties on the mode of failure in carbon-fibre/epoxy composites

A series of mechanical tests have been performed on composites consisting of high-strength carbon fibres in an amine-cured epoxy resin. A comparison has been made between composites containing untreated, commercially treated (electrochemically), and plasma treated fibres. While both treatments improve interfacial adhesion, the manner in which the composite fails is totally different. In composites that contain electrochemically treated fibres failure is, in most cases, matrix dominated, whereas interfacial failure always occurs in samples made from plasma-treated fibres. This behaviour can be explained in terms of the nature of the fibre surface after each type of 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.     

Bolted Joints in Three Axially Braided Carbon Fibre/Epoxy Textile Composites with Moulded-in and Drilled Fastener Holes

Experimental behaviour of bolted joints in triaxial braided (0°/±45°) carbon fibre/epoxy composite laminates with drilled and moulded-in fastener holes has been investigated in this paper. Braided laminates were manufactured by vacuum infusion process using 12 K T700S carbon fibres (for bias and axial tows) and Araldite LY-564 epoxy resin. Moulded-in fastener holes were formed using guide pins which were inserted in the braided structure prior to the vacuum infusion process. The damage mechanism of the specimens was investigated using ultrasonic C-Scan technique. The specimens were dimensioned to obtain a bearing mode of failure. The bearing strength of the specimens with moulded-in hole was reduced in comparison to the specimens with drilled hole, due to the increased fibre misalignment angle following the pin insertion procedure. An improvement on the bearing strength of moulded-in hole specimens might be developed if the specimen dimensions would be prepared for a net-tension mode of failure where the fibre misalignment would not have an effect as significant as in the case of bearing failure mode, but this mode should be avoided since it leads to sudden catastrophic failures.