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.     

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。     

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．     

Three techniques of interfacial bond strength estimation from direct observation of crack initiation and propagation in polymer–fibre systems

Three techniques of bond strength determination in micromechanical tests—fibre strain profile analysis by means of Raman spectroscopy, “kink” force determination in a traditional pull-out test, and crack length monitoring in a microbond test—were used for investigation of interfacial debonding in epoxy–glass fibre and epoxy–aramid fibre systems. Crack propagation was characterised by local interfacial parameters—critical energy release rate, G_ic, and ultimate interfacial shear strength (IFSS), τ_ult. The comparison of the results showed good agreement both between different techniques and between stress-based and energy-based failure criteria. Sizing of glass fibres caused more pronounced variations in the IFSS than for aramid fibres due to different interfacial failure patterns. The strength of “real” epoxy–glass composites with sized and unsized fibres correlates well with the bond strength determined from the micromechanical tests.     

An evaluation of acoustic emission from fibre-reinforced composites

An analysis of acoustic emission (AE) from model composites consisting of a single aramid fibre and different epoxy matrix systems has been carried out to identify the source of acoustic emission. The AE activity was observed in a narrow range of strain when fibre fracture occurred, whereas in a relatively wide range of strain, debonding occurred at the fibre-matrix interface. Ion-etched fibres showed a good adhesion of the fibres to the matrix so as to produce fibre fracture in place of interfacial debonding. The total number of AE events has one to one correspondence with the number of broken fibres. The effect of surface treatment and matrix systems on the shear fracture strength between the fibre and matrix were described based on the critical length of the broken fibres using AE results.     

Evaluation of interface fracture energy for single-fibre composites

Raman and luminescence spectroscopy have been used for the first time to determine the interface fracture energy for single-fibre composites. By using the measured fibre stress distributions in single-fibre fragmentation composite specimens and a simple energy-balance scheme, the energy for the initiation of interfacial debonding has been estimated for carbon (T50) and α-alumina (PRD-166 and Nextel 610) fibres embedded in epoxy resins. It has been found that the interface fracture energy shows good sensitivity to changes in the level of fibre/matrix adhesion due to surface treatment and sizing of the fibres. It is also found that the values of interface fracture energy correlate well with measured values of interfacial shear strength determined for the same fibre/matrix systems.     

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.     

Axial compression fracture in carbon fibres

Axial compression fracture of carbon fibres was studied by embedding single fibres in epoxy resin and compressing the specimens parallel to the fibre axis. By careful optical monitoring of the fibre surface the earliest stages of fracture were identified leading to estimates of the fibre axial compression failure strengths. Compression strength decreases markedly from about 2.2 GN m^?2 for moderately oriented fibres to <1 GN m^?2 for highest modulus filaments. The trend towards decreasing compression strength with increasing anisotropy is explained on the basis of an increasing fibre microfibrillar nature. However fracture morphology studies show that the unduly rapid strength decrease results from an increasing degree of fibre outer layer ordering which accompanies increasing axial anisotropy in carbon fibres since cracking occurs first on the more highly aligned filament surfaces. It is suggested that fibre compression fracture changes from a shear to a microbuckling or kinking mode with increasing fibre anisotropy, where the latter initiates in individual, well-aligned but uncoupled microfibrils. The similarity of fine axial compression fractures in oriented carbon fibres to those found in elastica loop experiments is noted as are the possible implications which the low strain-to-failure in compression of very high modulus fibres might have for practical composites.     

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.     

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.     

Effect of fibre content and alkali treatment on mechanical properties of Roystonea regia-reinforced epoxy partially biodegradable composites

The present paper investigates the effect of fibre content and alkali treatment on tensile, flexural and impact properties of unidirectional Roystonea regia natural-fibre-reinforced epoxy composites which are partially biodegradable. The reinforcement Roystonea regia (royal palm) fibre was collected from the foliage of locally available royal palm tree through the process of water retting and mechanical extraction. The poor adhesion between fibre and matrix is commonly encountered problem in natural-fibre-reinforced composites. To overcome this problem, specific physical and chemical treatments were suggested for surface modification of fibres by investigators. Alkali treatment is one of the simple and effective surface modification techniques which is widely used in natural fibre composites. In the present study both untreated and alkali-treated fibres were used as reinforcement in Roystonea regia epoxy composites and the tensile, flexural and impact properties were determined at different fibre contents. The alkali treatment found to be effective in improving the tensile and flexural properties while the impact strength decreased.     

Effect of low-temperature-plasma surface treatment on the adhesion of ultra-high-molecular-weight-polyethylene fibres

The poor adhesion of ultra-high-molecular-weight polyethylene (UHMW-PE) fibres to epoxy resin (due to characteristics of their surface structure) makes it difficult to develop light composite materials with good mechanical properties. In our experiments a low-temperature plasma was applied to treat the surfaces of the fibres. The results showed that the surface energy of the treated fibres was increased greatly so that the fibres could be wetted very well by resin, which was an essential prerequisite in improving the adhesion of the fibre/epoxy resin systems; and the results also showed that the pull-out adhesion strength of the treated fibres to resin was increased significantly by about 10 times. This paper discusses the mechanism of the improvement of the adhesion. Two reasons for improvement are that: varieties of polaroxygen-containing groups are produced in the non-polar surface layer, forming chemical bonds; and plasma-etched pits spread all over the surface of the fibres into which the resin penetrates to form a mechanical interlock between fibre and resin. A synthetic analysis and discussion of these two factors and of non-polar interactions influencing the adhesion is given, and a preliminary relationship between them is presented.     

Pulped Phormium tenax leaf fibres as reinforcement for epoxy composites

Leaf fibres from Phormium tenax (harakeke, New Zealand flax) were pulped at 170 °C with NaOH and anthraquinone. The pulp was wet laid to form mats, which were used to reinforce epoxy composites. The flexural modulus was almost as high as that measured for epoxy reinforced with glass chopped strand mat at the same weight fraction. The flexural strength was two-thirds that of the glass-reinforced composite. Failure was abrupt. SEM images showed torn fragments of fibre cell walls protruding from the fracture surface, indicating strong interfacial bonding. Good mechanical performance was attributed to the rarity of kink bands in the individual fibre cells, along with wrinkled cell-wall surfaces that enhanced the area of the fibre–matrix interface.     

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.     

The potential of using date palm fibres as reinforcement for polymeric composites

Interfacial adhesion of natural fibres as reinforcement for fibre polymeric composites is the key parameter in designing composites. In the current study, interfacial adhesion of date palm fibre with epoxy matrix is experimentally investigated using single fibre pull out technique. The influence of NaOH treatment concentrations (0–9%), fibre embedded length and fibre diameter on the interfacial adhesion property was considered in this study. Scanning Electron Microscopy (SEM) was used to observe the surface morphology and damage feature on the fibre and bonding area before and after conducting the experiments. The results revealed that 6% concentration of NaOH is the optimum solution for treating the date palm fibre to maintain high interfacial adhesion and strength with epoxy matrix. The embedded length of the fibre controlled the interfacial adhesion property, where 10 mm embedded length was the optimum fibre length.     

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.     

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.     

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.     

Effect of anodic oxidation of coal tar pitch-based carbon fibre on adhesion in epoxy matrix: Part 2. Comparative study of three alkaline solutions

Anodic oxidation of coal tar pitch-based carbon fibre was performed in various alkaline solutions, such as NaOH, NaHCO₃ and Na₂CO₃, to examine the effect of various kinds of electrolytes on the surface chemical nature of treated fibres and the adhesive strength between treated fibres and epoxy resin. Evaluation of the oxygen concentration and surface functional groups of the carbon fibre surface was conducted by X-ray photoelectron spectroscopy (XPS). A fragmentation test was adopted for evaluation of the adhesive strength between the carbon fibre and epoxy matrix. As a result, it was shown that the highest O_1S/C_1S value was obtained in NaOH aqueous solution, and the highest interfacial shear strength (IFSS) was also obtained from the carbon fibre oxidized in NaOH solution. It was recognized that the IFSS values increase with increasing of O_1S/C_1S in every solution at the initial stage of oxidation below 1.0 × 10⁻³ C mm⁻². However, above this level of electrical charge in NaOH solution, decreasing IFSS values may occur, regardless of an increasing O_1S/C_1S value. SEM analysis inferred that in the case of the fibre treated in NaOH solution, grooves on the carbon fibre surfaces had become deeper over 1.0 × 10⁻³ C mm⁻². Presumably, the amorphous part of the carbon fibres could be oxidized intensively, and the remaining graphite layer become very thin and easy to break when a shear stress is loaded on its interface.     

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.