Study of the interlaminar shear strength of unidirectional high-modulus polyethylene fibre composites

The interlaminar shear strength of a unidirectional high-modulus polyethylene fibre-epoxy resin composite, measured using a short-beam bend test, increases when the fibre has been plasma treated but decreases with increasing fibre content or increasing filament diameter. Attempts have been made to explain these observations. From observation of the sample failure and the bending load/deflection curves, it was found that there are two possible failure modes dependent on fibre type, fibre volume fraction and fibre plasma treatment. These are (1) brittle failure of the resin and (2) failure at the fibre/resin surface. The present results appear to be consistent with the interlaminar shear strength data obtained from high-modulus polyethylene fibre samples made by the hot compaction process developed at Leeds.     

纤维表面处理对CF/PAA复合材料界面性能的影响

采用多结构形态倍半硅氧烷（VMS—SSO）涂层结合等离子活化纤维表面的方法对碳纤维（CF）改性，研究了纤维表面处理对碳纤维／聚芳基乙炔复合材料界面性能的影响．结果表明，等离子活化前后纤维表面涂层处理使材料的ILSS分别提高25％和45％，在碳纤维与树脂之间引入了过渡层．等离子活化纤维在碳纤维与涂层间通过VMS-SSO引入了化学键连接．含活性官能团的多形态倍半硅氧烷涂层在等离子活化纤维前后处理碳纤维，都能提高复合材料的界面性能．但是效果不同．其原因是，碳纤维与树脂间相互作用的不同，前者主要是过渡层效应，后者在碳纤维与树脂间引入了化学键．     

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.     

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.     

Plasma surface modification of advanced organic fibres

Aramid and extended-chain polyethylene fibres have been treated in ammonia and oxygen plasmas in order to enhance adhesion to vinylester resins and thereby improve fibre/resin interfacial properties in composites made from these materials. For both aramid/vinylester and extended-chain polyethylene/vinylester composites, the plasma treatments result in significant improvements in interlaminar shear strength and flexural strength. Extended-chain polyethylene/vinylester composites also exhibit increased flexural modulus. Scanning electron and optical microscopic observations have been used to examine the microscopic basis for these results, which are compared with results previously obtained for aramid/epoxy and extended-chain polyethylene/epoxy composites. It is concluded that the increased interlaminar shear and flexural properties of vinylester matrix composites are due to improved wetting of the surface-treated fibres by the vinylester resin, rather than covalent chemical bonding.     

Influence of titanium carbide on the interlaminar shear strength of carbon fibre laminate composites

The potential use of carbon fibre laminate composites is limited by the weak out-of-plane properties, especially delamination resistance. The effect of incorporating titanium carbide to the mesophase pitch matrix precursor of carbon fibre laminate composites on interlaminar shear strength is studied both on carbonised and graphitised composites. The presence of titanium carbide modifies the optical texture of the matrix from domains to mosaics in those parts with higher concentrations and it contributes to an increase of fibre/matrix bonding. This fact produces an increase of the interlaminar shear strength of the material and changes the fracture mode.     

The mechanical properties of oxyfluorinated hybrids of glass fibre and polypropylene fibre

The mechanical properties of a low-cost system comprising orthophthalic polyester resin reinforced with hybrids of glass and polypropylene fibres were investigated. The fibres were oxyfluorinated to overcome the poor surface adhesion properties of polypropylene. Interlaminar shear tests, Izod-type impact tests and tensile tests were considered. It would be expected that increasing polypropylene fibre content corresponds with a decrease in mechanical properties due to the poor properties of polypropylene. Oxyfluorinated laminates containing approximately 25% and 50% polypropylene in the warp direction were, however, found to exhibit significant improvements in interlaminar shear strength, in peak shear stress under impact loading as well as in impact resistance over untreated glass fibre laminates. Scanning electron microscope images show that the reason for this improvement is that the interfacial bond between the polypropylene fibres and the resin is strengthened to such an extent that failure occurs within the polypropylene fibres rather than at the interface.     

Effects of fibre surface silanisation on silica fibre/phenolics composites produced by resin transfer moulding process

Abstract

The effects of fibre surface silanisation on silica fibre/phenolics composites produced by the resin transfer moulding (RTM) solution impregnation route were investigated. Diffuse reflectance infrared Fourier transform (DRIFT) spectroscopy and micro-Wilhelmy method were used to evaluate the surface properties of silanised silica fibre. The interlaminar shear strength (ILSS) measurements and morphological observations of the silica fibre/phenolics composites were also performed. The interactions occurring between silica fibre and the components of phenolic resin solution affect the dynamic adsorption behaviour of phenolic resin onto fibre reinforcement. The competitive adsorption of ethanol as solvent onto silica fibre suppresses that of phenolic resin. Fibre surface silanisation by γ-aminopropyl-triethoxysilane (γ-APS), γ-glycidoxypropyl-trimethoxysilane (γ-GPS) and γ-methacryloxypropyl-trimethoxysilane (γ-MPS) leads to the improvement of mechanical interfacial properties of silica fibre/phenolics composites on one hand and decreases the inhomogeneities of resin distribution and mechanical interfacial properties at different regions of the RTM product on the other hand.     

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.     

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.     

Mechanical properties of E-glass fibre reinforced nylon 6/6 resin composites

The tensile strength, tensile modulus, compressive strength, interlaminar shear strength and residual tensile strength of E-glass fibre reinforced nylon 6/6 resin composite with the variation of fibre volume fraction are characterized. The results are in line with the required limits of theoretical values.     

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.     

Preparation and properties of Fibre–Metal Laminates based on carbon fibre reinforced PMR polyimide

A novel Fibre–Metal Laminates (FMLs) based on carbon fibre reinforced PMR polyimide were prepared using a hot press process in this paper. Pre-treatment on the titanium surface were conducted prior to laminating. Scanning Electron Microscope (SEM) were used to observe the morphologies of the titanium and the cross-sections of the FMLs. SEM results showed that micro-roughness structures were formed on the titanium surface after anodization. This structure enhanced the interlaminar bond strength between titanium and polyimide. Flexural and Interlaminar shear (ILSS) tests showed that the FMLs possess excellent flexural and interlaminar properties at both room temperature and elevated temperature. Thermostability tests proved that the FMLs based on carbon fibre reinforced PMR polyimide offered excellent thermal properties. It is shown that no delamination appears between titanium layer and the fibre-reinforced polyimide layer after 1000 times thermal shock.     

Comparison of the mechanical and physical properties of a carbon fibre epoxy composite manufactured by resin transfer moulding using conventional and microwave heating

Microwave processing holds great potential for improving current composite manufacturing techniques, substantially reducing cure cycle times, energy requirements and operational costs. In this paper, microwave heating was incorporated into the resin transfer moulding technique. Through the use of microwave heating, a 50% cure cycle time reduction was achieved. The mechanical and physical properties of the produced carbon fibre/epoxy composites were compared to those manufactured by conventional resin transfer moulding. Mechanical testing showed similar values of flexural moduli and flexural strength for the two types of composites after normalisation of the corresponding data to a common fibre volume fraction. A 9% increase of the interlaminar shear strength (ILSS) was observed for the microwave cured composites. This enhancement in ILSS is attributed to a lowering of resin viscosity in the initial stage of the curing process, which was also confirmed via scanning electron microscopy by means of improved fibre wetting and less fibre pull-out. Furthermore, both types of composites yielded minimal void content (<2%). Dynamic mechanical thermal analysis revealed comparable glass transition temperatures for composites produced by both methods. A 15 °C shift in the position of the β-transition peak was observed between thermally and microwave cured composites, suggesting an alteration in the cross-linking path followed.     

Synergy of matrix and fibre modification on adhesion between carbon fibres and poly(vinylidene fluoride)

Interfacial properties between carbon fibres and poly(vinylidene fluoride) (PVDF) were tuned by modifying both constituents. Atmospheric plasma fluorination (APF) was utilised to tailor the surface composition of carbon fibres, which resulted in an incorporation of up to 3.7 at.% of fluorine functionalities in to the fibre surfaces. The PVDF matrix was modified by blending pure PVDF with maleic anhydride (MAH) grafted PVDF. Both fibre and matrix modifications act in synergy with improvements of up to 50% in the apparent interfacial shear strength (IFSS) above the level of pure fibre or matrix modification. Modification of both constituents led to the formation of various interactions at the fibre/matrix interface namely dispersive and polar (H-bonds) between (modified) PVDF and the fluorine as well as oxygen functionalities on the fibre surfaces. The apparent IFSS between the modified fibres and matrix reaches a maximum of 42 MPa, which is almost the tensile strength of the pure PVDF. The improvements in apparent IFSS in single fibre model composites for both fibre and matrix modifications translated to a seven times improvement in the interlaminar shear strength of unidirectional 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.     

Surface modification of an aramid fibre treated in a low-temperature microwave plasma

The surface modification of an aramid fibre treated in a low-temperature microwave (mw) plasma was investigated. Three different plasma gases, oxygen, argon and ammonia, were used to achieve different surface modifications during fibre treatment. The modification of the fibre surface was analysed with electron spectroscopy and electron microscopy. The influence of the surface modification on the fibre-matrix interaction was inspected by measuring the interlamellar shear strength of the composites and the pull-out strength of a fibre bundle in model composites. The process gas and thus the kind of plasma has no significant influence on the fibre modification resulting from plasma treatment. It was shown that a fibre cleaning with subsequent surface ablation is the dominate modification process during mw plasma treatment, independent of the process gas. The degree of surface cleaning and removal of a contamination layer strongly depended on the treatment range. No incorporation of oxygen or nitrogen containing functional groups was observed. This was explained with the composition of the process gas. The improvements of the composite properties demonstrate the advantage of the mw plasma treatment as a fast, environmentprotected, cost-efficient process for fibre modification.     

Strength and fracture toughness of carbon fibre polyester composites

Fracturing of carbon fibre/polyester composites has been studied by means of mechanical testing and scanning electron microscopy. Carbon fibres were surface-treated in several ways so as to vary the interlaminar shear strength of the composites, and the effect of this variation on the work of fracture was determined by means of Charpy V-notch impact tests and slow three-point bend tests on notched specimens of triangular cross-section. The effect of moisture on the fracture toughness was also studied by measuring toughness and interlaminar shear strength after exposure to steam. Improvement of the fibre/resin bond results, as expected, in an increase in the brittleness of composites and it appears that a purely mechanical bond, such as might be obtained by acid-etching the fibre surface, is less proof against deterioration in humid atmospheres than a chemical bond, such as can be obtained by the use of coupling agents. Estimates of the magnitude of various contributions to the fracture toughness show that in carbon-fibre-reinforced resins the effect of increasing the stiffness or load-bearing ability of the matrix and the work done against friction in pulling broken fibres out of the matrix contribute approximately one fifth and four fifths, respectively, of the total work of fracture.     

Mixed resin and carbon fibres surface treatment for preparation of carbon fibres composites with good interfacial bonding strength

The objective of this work is to improve the interlaminar shear strength of composites by mixing epoxy resin and modifying carbon fibres. The effect of mixed resin matrix’s structure on carbon fibres composites was studied. Anodic oxidation treatment was used to modify the surface of carbon fibres. The tensile strength of multifilament and interlaminar shear strength of composites were investigated respectively. The morphologies of untreated and treated carbon fibres were characterized by scanning electron microscope and X-ray photoelectron spectroscopy. Surface analysis indicates that the amount of carbon fibres chemisorbed oxygen-containing groups, active carbon atom, the surface roughness, and wetting ability increases after treatment. The tensile strength of carbon fibres decreased little after treatment by anodic oxidation. The results show that the treated carbon fibres composites could possess excellent interfacial properties with mixed resins, and interlaminar shear strength of the composites is up to 85.41 MPa. The mechanism of mixed resins and treated carbon fibres to improve the interfacial property of composites is obtained.     

电晕处理对超高分子量聚乙烯纤维表面性能的影响

对超高分子量聚乙烯（UHMWPE）纤维表面进行了电晕处理，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UHMWPE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，UHMWPE纤维表面含氧量增多，含氧基团数量与种类增加，表面浸润性得到改善，纤维与基体的界面粘结强度（Ts）提高幅度可达535％，短梁剪切强度TNOL提高了40％以上．