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.     

Plasma surface modification of advanced organic fibres: Part V Effects on the mechanical properties of aramid/phenolic composites

Aramid fibres have been treated in ammonia and oxygen plasma to enhance adhesion to resole phenolic resins. The plasma treatments resulted in significant improvements in interlaminar shear strength (ILSS) and flexural strength of composites made from these materials. Composites containing aramid fibres with epoxide groups reacted on to the ammonia plasma-treated fibre surface also showed further improvements in ILSS and flexural strength. Scanning electron and optical microscopic observations were used to examine the microscopic basis for these results, which have been compared with those obtained previously for aramid/epoxy and aramid/vinyl ester composites. For composites containing oxygen and ammonia plasma-treated fibres, the enhanced ILSS and flexural strength are attributed to improved wetting of the surface-treated aramid fibres by the phenolic resin. However, for those containing fibres with reacted epoxide groups on the ammonia plasma-treated fibre surfaces, the enhanced composite properties may be due to covalent chemical interfacial bonding between the epoxide groups and the phenolic resin. Effects of catalyst levels and cure cycle on the ILSS of composites laminated with untreated fabric has also been examined and optimum values have been determined. The catalyst concentration has an influence on the phase-separated water domain density in the matrix which in turn, affects the available fibre/matrix bonding area and hence the composite ILSS and flexural strength. This revised version was published online in November 2006 with corrections to the Cover Date.     

Atmospheric plasma fluorination as a means to improve the mechanical properties of short-carbon fibre reinforced poly (vinylidene fluoride)

The impact of fluorination of carbon fibres on the properties of short fibre reinforced polyvinylidene fluoride (PVDF) composites was studied. As received and continuously atmospheric plasma fluorinated (APF) carbon fibres were cut to an average fibre length of 2 mm. Short fibre composites (SFC) containing 5, 10 and 15 wt.% carbon fibres were manufactured using a twin-screw mixer. Test specimens were produced by injection moulding. The mechanical properties of the SFC were studied using tensile and compression testing. As expected, the incorporation of short-carbon fibres into PVDF led to an increase in strength and stiffness. The tensile strength and Young’s modulus of the SFC containing APF-treated carbon fibres increased by up to 17% and 190%, respectively. Furthermore, the compressive strength and modulus of the SFC containing APF-treated carbon fibres also increased by 19% and 35%, respectively. APF of carbon fibres results only in a marginal increase in the bulk matrix crystallinity of PVDF as determined by DSC. Scanning electron micrographs of fracture surfaces from tensile tested specimens exhibited a typical brittle failure mode with low fibre loading fraction. Despite the presence of up to 5% of voids and visible resin rich regions at fracture surface, SFC containing APF-treated fibres suggest better bonding at the fibre/matrix interface which led to the much enhanced mechanical properties.     

X-ray photoelectron spectroscopic studies of carbon fibre surfaces

Carbon fibres were anodically surface treated by passing them continuously through an electrochemical bath, thus simulating a possible industrial surface-treatment process. Composites were made from these fibres with an epoxy resin and their interlaminar shear strength (ILSS) tested. The surfaces of the fibres were examined by X-ray photoelectron spectroscopy after treatment. Both golvanostatic and potentiostatic cell control led to treated fibres that produced composites with high interlaminar shear strengths (80 to 90 MPa). The effect of potential, reaction time, electrolyte and subsequent heating of the fibres in a vacuum on the ILSS of the composites is reported. The rise in ILSS with surface treatment is not dependent upon the O-1 s: C-1 s ratios or the amount of carboxyl functionality present on the surface. This suppors the view that mechanical keying of the resin to the fibre surface plays an important role in forming the fibre-resin bond.     

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.     

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.     

Kevlar缝线表面处理对炭纤维/双马来酰亚胺树脂缝合复合材料界面性能的影响

为了改善Kevlar缝线缝合复合材料的耐湿热性能, 采用化学接枝烯丙基的方法对Kevlar缝合线进行表面改性处理。通过力学测试、 扫描电子显微镜(SEM)、 光电子能谱分析(XPS)对表面改性的纤维进行表征。实验结果表明, 化学处理的Kevlar缝线表面变得粗糙, 缝线表面氧元素的含量提高23%, 在合适的处理条件下, 缝线的拉伸强度降低很小。同时通过测试干、 湿态下炭纤维/双马来酰亚胺树脂缝合复合材料层压板的层间剪切强度, 研究了化学表面处理的Kevlar缝线对缝合炭纤维/双马来酰亚胺树脂复合材料界面性能的影响。测试结果显示, 表面处理后Kevlar缝线缝合的复合材料的吸湿率降低约52%, 湿态层间剪切强度保持率提高15%。      

The effect of surface treatment on the interfacial properties in carbon fibre/epoxy matrix composites

Carbon fibres with different degrees of surface oxidation, as well as epoxy-sized fibres, were used to prepare epoxy composites in order to compare the effects of the fibres surface chemistry on the interfacial properties. X-ray photoelectron spectroscopy, water vapour adsorption measurements and contact angle examination were applied to characterize the carbon fibre surfaces. A correlation was found between the content of primary adsorption sites on the fibre surface and interlaminar shear strength (ILSS) of the composites. Higher values of ILSS obtained for the oxidized fibres containing composites are proposed to be due to the higher concentration of carboxylic groups created on the oxidized fibres surface and to the creation of chemical bonds at the fibre/epoxy matrix interface. Enthalpy of cure, reaction peak temperature and glass transition temperature of the composites were determined by differential scanning calorimetry.     

Investigation of damage mechanism of flax fibre LPET commingled composites by acoustic emission

Tensile failure and fracture behaviour of parallel laid twisted flax fibre reinforced low melting polyethylene terephthalate (LPET) composites were investigated. The tensile failure results of the model specimens were compared with AE results in terms of amplitude, energy and counts. The failure results of the flax fibre LPET composites exhibited mainly matrix crack initiation as a brittle failure for low, medium and high fibre contents. Since the composites at high fibre contents have higher porosity content, they show higher strain to failure, higher variation in the tensile results and have different appearances on their fracture surfaces than those of the composites at low and medium fibre contents.     

Investigation of the effect of surface modifications on the mechanical properties of basalt fibre reinforced polymer composites

Unsaturated polyester-based polymer composites were developed by reinforcing basalt fabric into an unsaturated polyester matrix using the hand layup technique at room temperature. This study describes basalt fibre reinforced unsaturated polyester composites both with and without acid and alkali treatments of the fabrics. The objective of this investigation was to study the effect of surface modifications (NaOH & H₂SO₄) on mechanical properties, including tensile, shear and impact strengths. Variations in mechanical properties such as the tensile strength, the inter-laminar shear strength and the impact strength of various specimens were calculated using a computer-assisted universal testing machine and an Izod Impact testing machine. Scanning Electron Microscope (SEM) observations of the fracture surface of the composites showed surface modifications to the fibre and improved fibre–matrix adhesion. The result of the investigation shows that the mechanical properties of basalt fibre reinforced composites are superior to glass fibre reinforced composites. This work confirms the applicability of basalt fibre as a reinforcing agent in polymer composites.     

Shear strength of polymers and fibre composites: 2. carbon/epoxy pultrusions

Pultrusions were made with carbon fibres and an epoxy resin. Three different curing agents were used, so that the matrices were resins with different glass transition temperatures. The composites were tested for shear strength at different temperatures, so that the effect of the resin shear strength on composite shear strength could be observed, with a fixed fibre architecture. It was found that the composite was always much stronger than the resin both for the 0 and 90° fracture modes. The 90° fracture surfaces contained many broken fibres, and shear hackles were observed in the resin-rich regions. These suggested that shear failure (rather than tensile failure) took place in the Iosipescu test for the 90° specimens. It was concluded that the fibre architecture played a dominant role in the composite shear strength, with interphase effects being involved also.     

橡胶改性对硼纤维/环氧单向复合材料力学性能的影响

对环氧树脂进行液体丁腈橡胶改性, 并采用缠绕无纬布层压成型工艺制备了硼纤维/环氧单向复合材料。测试了环氧树脂液体丁腈橡胶改性前后硼纤维/环氧单向复合材料的力学性能, 研究了硼纤维/环氧单向复合材料的纵向拉伸破坏模式。结果表明, 基体中的10%液体丁腈橡胶使硼纤维/环氧单向复合材料的拉伸强度、 弯曲强度、 层间剪切强度和断裂延伸率分别提高了18.42%、 13.39%、 28.45%和43.40%, 但其拉伸和弯曲模量稍有下降。基体中含10%液体丁腈橡胶的硼纤维/环氧单向复合材料的纵向拉伸破坏模式为界面层的内聚破坏和脱黏破坏共存的混合破坏。      

Effect of Co60 gamma ray irradiation for carbon fibre on interfacial properties in epoxy resin composites

Abstract

In order to improve the interfacial adhesion between carbon fibre and resin matrix in composite materials, it is necessary to treat the surface of the carbon fibre. In this paper, γ-ray irradiation technique was used to modify polyacrylonitrile based carbon fibre. Laser Raman spectrum and X-ray photoelectron spectroscopy were used to investigate and analyse the structure and chemical composition near the surface of the carbon fibre. The influence of irradiation parameters on the interlaminar shear strength (ILSS) of carbon fibre reinforced epoxy composite materials and the bundle tension strength of carbon fibre was studied. The interfacial adhesion behaviour of composites was characterised using torsional braid analysis. The results show that after irradiation the ILSS of the composite was increased by 20%, while the glass transition peak of the specimen, determined from torsional braid analysis, shifts towards a higher temperature compared with an unirradiated specimen. The value of the glass transition temperature T _g is increased from 416.8 to 424.3 K. After irradiation there was no apparent change in the bundle tensile strength of carbon fibre. Investigations indicate that after irradiation the decrease of microcrystal size, the increase of surface free energy of carbon fibre surface and the active chemical function group formed from unsaturated carbon atoms improve the interface adhesion between the carbon fibre and the matrix in the composites.     

Plasma surface modification of advanced organic fibres

A marked improvement in the interlaminar shear strength and flexural strength of aramid/ epoxy composites is observed when the fibres are pretreated in an ammonia or ammonia/ nitrogen gaseous discharge (plasma) to introduce amine groups on to the fibre surface. Scanning electron and optical microscopic observations are used to examine the microscopic basis for these results. Scanning electron micrographs of shear fracture surfaces show clean fibre/matrix separation in composites made from untreated fibres, indicative of weak interfacial bonding. In contrast, shear fracture surfaces of composites containing plasma-treated fibres exhibit clear evidence of fibre fibrillation and matrix cracking, suggesting stronger interfacial bonding. Optical microscopic examination of flexure specimens shows that enhanced strength results mainly from reduced compressive fibre buckling and debonding, due to an increase in fibre/matrix interfacial bond strength. This increase is not accompanied by any significant change in the interlaminar fracture energy or flexural modulus of the composites, but there is an appreciable loss in transverse ballistic impact properties. These results are also examined in terms of the observed increase in fibre/matrix interfacial strength.     

Effects of moisture on the mechanical properties of glass fibre reinforced vinylester resin composites

Glass fibre reinforced vinylester resin composites incorporating varying amounts of fibres (63.5, 55.75, 48.48, 38.63 and 27.48 wt%) were characterized for their mechanical properties both as prepared and after treatment with boiling water for 2, 4, 6, 8 and 24 h. Weights of the samples were found to increase to a saturation at about 8 h with boiling water treatment. In keeping with the composite principle, the mechanical properties improved with fibre loading. However, the properties were relatively inferior when treated with boiling water for longer hours attributing to ingress of moisture by capillary action through the interface between the fibre and the resin matrix. Considering the rates of moisture absorption and correlating with the mechanical properties, it was observed that the deteriorating effects were predominant up to 4 h treatment with boiling water. Estimation of defect concentrations for 63.5 wt% of nascent fibre reinforced composites as well as those composites treated with boiling water for 24 h were 56.93% and 64.16% respectively. Similarly, 27.48 wt% nascent fibre reinforced composites and those composites with boiling water treatment showed the estimation of defect concentrations of 39.94% and 50.55% respectively. SEM study of the fractured surfaces showed heavy fibre pull-out in the tensile zone whilst shear fracture of the fibre bundles was predominant at the compressive zone of the samples tested for flexural strength properties.     

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.     

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.     

Role of matrix modification on interlaminar shear strength of glass fibre/epoxy composites

Interlaminar shear properties of fibre reinforced polymer composites are important in many structural applications. Matrix modification is an effective way to improve the composite interlaminar shear properties. In this paper, diglycidyl ether of bisphenol-F/diethyl toluene diamine system is used as the starting epoxy matrix. Multi-walled carbon nanotubes (MWCNTs) and reactive aliphatic diluent named n-butyl glycidyl ether (BGE) are employed to modify the epoxy matrix. Unmodified and modified epoxy resins are used for fabricating glass fibre reinforced composites by a hot-press process. The interlaminar shear strength (ILSS) of the glass fibre reinforced composites is investigated and the results indicate that introduction of MWCNT and BGE obviously enhances the ILSS. In particular, the simultaneous addition of 0.5 wt.% MWCNTs and 10 phr BGE leads to the 25.4% increase in the ILSS for the glass fibre reinforced composite. The fracture surfaces of the fibre reinforced composites are examined by scanning electron microscopy and the micrographs are employed to explain the ILSS results.     

Influence of fibre surface oxidation treatment on mechanical interfacial properties of carbon fibre/ polyarylacetylene composites

Abstract

In the present work, the mechanical interfacial properties of carbon fibre (CF) reinforced polyarylacetylene (PAA) resin composites were modified through the surface oxidation treatment of carbon fibres by ozone. Both X-ray photoelectron spectroscopy (XPS) and Fourier transform infrared (FTIR) spectroscopy showed that oxidation treatment could increase the amount of elemental oxygen on the fibre surface markedly by introducing more oxygen groups. Atomic force microscopy (AFM) images indicated that weak surface regions of fibres had been etched and removed, and the degree of fibre surface roughness was increased. The interlaminar shear strength (ILSS) and the interfacial shear strength (IFSS) of CF/PAA composites were both improved notably (no less than 50%). It could be concluded that an improvement of fibre surface chemical activity, better wettability of resin on the carbon fibre surface, and stronger mechanical joining between fibres and resin all resulted in the modification of interfacial properties of carbon fibre reinforced PAA composites. The influences of temperature, ozone concentration, and treatment time on the oxidation results were studied, and optimal treatment parameters determined.     

Mechanical performance of carbon fibre-reinforced composites based on stitched preforms

A comparative assessment of the influence of pure assembly seams based on a thin (11 tex) polyester yarn in a zigzag geometry on the resulting mechanical performance of a non-crimped fabric (NCF) carbon fibre-reinforced epoxy composite manufactured by vacuum-assisted resin transfer moulding is presented. This study was aimed at generating a solid foundation regarding the overall performance level of stitched NCF composites and at identifying critical property changes. The comprehensive evaluation of the mechanical composite properties includes static as well as dynamic tests of the in-plane properties as well as a characterisation of the interlaminar properties such as apparent interlaminar shear strength (ILSS) and compression after impact (CAI). It is demonstrated that mechanical properties such as the tensile and compression stiffness and CAI strength are not degraded by the chosen stitching parameters, whereas the tensile and compression strength, ILSS as well as the tensile fatigue behaviour are reduced as a result of pronounced localised fibre ondulations. A direct comparison to properties of a commonly used 5H satin woven fabric composite verifies that the overall performance of these particular stitched NCF composites must be enhanced with regard to the identified key criteria to meet the level required for aircraft applications and in order to maintain the performance advantage of NCF composites as compared to standard woven fabrics in general. Promising approaches include the use of different yarn materials based on soluble thermoplastics and/or modified stitching parameters.