Fiber–matrix adhesion from the single-fiber composite test: nucleation of interfacial debonding

The level of fiber–matrix interfacial adhesion in composites is traditionally evaluated by means of a stress-based parameter. Recently, it was suggested that an interfacial energy parameter might constitute a valid alternative. From an overview of the literature regarding the single-fiber composite fragmentation test, it appears that energy-based approaches have already been proposed in the past, but were either not successful, or not fully developed. Our recent energy balance scheme, proposed for the analysis of the initial interface debonding which occurs at fiber breaks during a fragmentation test, is presented and expanded here. The effects of thermal residual stress in the fiber, and of friction in the debonded area, are now incorporated in the energy balance model. We use a different shear-lag parameter proposed by Nayfeh, rather than the commonly used Cox parameter. New, extensive single-fiber fragmentation data regarding the interface crack initiation regime is presented, using sized and unsized E-glass fibers embedded in UV-curable or epoxy polymers. Some data for unsized carbon in epoxy is also presented. Fiber fragmentation is forced to take place entirely in the linear elastic region of the stress–strain curve, by means of pre-stressed single fibers. The importance of this procedure is discussed. Future work will focus on the interface crack propagation regime.     

Modelling and simulation of the mechanical behavior of ceramic matrix composites as shown by the example of SiC/SiC

Modelling of the mechanical behavior of unidirectionally fiber-reinforced ceramic matrix composites (CMC) is presented by the example of SiC/SiC. The starting point of the modelling is a substructure (elementary cell) which includes on a micromechanical scale the statistical properties of the fiber, matrix and fiber–matrix interface and their interactions. The substructure is chosen in such a way that a macrostructure representative of the whole structure can be modelled from a suitable number of substructures. The typical damage behavior of ceramic composites is modelled by taking fiber and matrix cracks into account. Cracks are inserted into the substructure by reducing the elastic coefficients of the material. The fracture criterion used is a surface represented by a spheroid in the principal stress space. The crack direction is determined by the criterion of the energy release rate. Interfacial behavior is simulated by consideration of fiber–matrix debonding and frictional sliding. The numerical evaluation of the model is accomplished by means of the finite element method (FEM). The effect of important parameters such as the fiber volume fraction or the fiber Weibull-shape parameter on the nonlinear behavior of the substructure is examined. Finally, a macrostructure is modelled to show the effects of these important parameters on the mechanical behavior of the whole structure.     

Influence of fiber/matrix interfacial adhesion on composite fracture behavior

A systematic study has been conducted to identify the effect of fiber/matrix interface strength on various composite properties. A new fiber treatment technique was developed to allow fibers to be treated and then made into prepregs and composites of acceptable quality. T500 carbon fibers were treated with release agent to establish the extreme case of poor fiber/matrix interface. Composite systems made of toughened epoxy R6376 and T500 fibers with and without such a treatment were subjected to a number of fracture and impact tests. For tests involving propagating pre-existing delamination cracks, such as double cantilever beam (DCB), end notched flexural (ENF) and crack lap shear (CLS) methods, the material properties were not appreciably affected by the release agent-treated fiber surfaces. For tests that had to initiate cracks in specimens without pre-introduced cracks, such as impact and edge delamination, the material variables and failure modes were highly sensitive to the fiber/matrix interface. The critical role of the fiber/matrix interface in crack initiation was demonstrated in this study.     

Feasibility study of a tungsten wire-reinforced tungsten matrix composite with ZrOx interfacial coatings

Brittleness problem imposes a severe restriction on the potential application of tungsten as high-temperature structural material. In this paper, a novel toughening method for tungsten is proposed based on reinforcement by tungsten wires. The underlying toughening mechanism is analogous to that of fiber-reinforced ceramic matrix composites. Strain energy is dissipated by debonding and frictional sliding at engineered fiber/matrix interfaces. To achieve maximum composite toughness fracture mechanical properties have to be optimized by interface coating. In this work, we evaluated six kinds of ZrO_x-based interface coatings. Interfacial parameters such as shear strength and fracture energy were determined by means of fiber push-out tests. The parameter values of the six coatings were comparable to each other and satisfied the criterion for crack deflection. Microscopic analysis showed that debonding occurred mostly between the W filament and the ZrO_x coating. Feasibility of interfacial crack deflection was also demonstrated by a three-point bending test.     

Influence of the fiber/matrix strength on the mechanical properties of a glass fiber/thermoplastic-matrix plain weave fabric composite

In this work, we analyze the influence of different fiber surface treatments on the mechanical properties of plain weave composites. The reinforcement is a glass fibers fabric and the matrix is an acrylic polymer. Until very recently, this thermoplastic polymer family was not used in composite industry. It is therefore necessary to study if the existing fiber surface treatments are suitable for acrylic resins or if new ones have to be found. At the macroscale, composite materials corresponding to different fiber surface treatments were characterized with: (i) monotonic in-plane shear tests and (ii) heat-build up fatigue measurements on specimens with ±45° fiber orientations with respect to the tensile force. At the mesoscale (fabric scale), the development of damage was experimentally analyzed from (i) 3-D DIC (Digital Image Correlation) full-field strain measurements with spatial resolution smaller than the textile repeating unit and (ii) X-ray microtomography. We show that the analyzed composite materials exhibit linear viscoelastic behavior until a given stress threshold above which damage develops in the material. It was also found that the application on the fibers of a coupling agent specifically developed for promoting the bond between glass fibers and acrylic resins improves the composite mechanical properties, in particular the fatigue properties.     

Evaluation of interfacial strength between fiber and matrix based on cohesive zone modeling

This paper presents a measurement technique of interfacial strength considering non-rigid bonding on a fiber/matrix interface modeled as a cohesive surface. By focusing on the stress concentration near a fiber crack obtained from a single-fiber fragmentation test, the stress contours in matrix observed by photoelasticity can be related to the interfacial strength by defining a characteristic length. An equation expressing the relationship between the characteristic length on the stress contour and the interfacial strength was derived, and validated using finite element analysis. The primary advantage of proposed measurement technique is that only a single fiber crack, which usually occurs within elastic deformation of matrix, is required for the evaluation of interfacial strength, whereas saturated fiber fragmentation is necessary in the conventional method. Herein, a sample application was demonstrated using a single carbon fiber and epoxy specimen, and an average interfacial strength of 23.8 MPa was successfully obtained.     

Fiber/matrix interfacial shear strength measured by a quasi-disk microbond specimen

A single fiber/quasi-disk microbond specimen was made for evaluating the interfacial shear strength of fiber-reinforced composites. A quasi-disk type microbond was formed with the insertion of a pin-holed Teflon film into a wetted liquid droplet epoxy resin that surrounded a single vertical carbon fiber. After finishing a curing process, the specimens were tested in comparison with conventional droplet microbond specimens. Test results for the quasi-disk type specimens showed more reliable shear strength data than those for the conventional ones. Their interfacial shear strength behaviors were in a good agreement with the hardness variation of the epoxy resin. Finite element analysis of droplet, quasi-disk and cylindrical pull-out tests showed that the stress concentration in the meniscus region for the quasi-disk type specimen was much less than that for droplet and very similar to that of the cylindrical one. This observation supported the reliability of experimental strength data measured in the quasi-disk type microbond test.     

Generation and analysis of FCG data using a single specimen and Kmax–ΔK testing matrix

A custom method to generate fatigue crack growth (FCG) data requires testing of multiple specimens at different load ratios, R, and the application of a load shedding procedure from pre-cracking level to threshold. In this paper, a novel method of testing has been investigated which utilizing a single specimen and a testing matrix in terms of K_max and ΔK values corresponding to predetermined R-ratios for which FCG data are recorded. Automatic K-controlled tests on 2324-T39 Al alloy were conducted using both increasing and decreasing ΔK procedures while K_max was kept constant. Results show that the increasing ΔK procedure gives less scatter than decreasing ΔK procedure. Also, fatigue crack growth curves near the threshold region obtained from increasing ΔK are above the curves obtained from decreasing ΔK procedure. These differences are explained by means of interaction between cyclic plastic zones and their effect on fatigue damage. The procedure with increasing ΔK demonstrated minimal interaction effects and hence it is recommended for efficient FCG data generation. The proposed procedure reduces testing time, the overall scatter associated with multiple samples and eliminates possible uncertainty linked to the load shedding procedure and its effects on threshold.     

Toughening of carbon fiber-reinforced epoxy polymer composites utilizing fiber surface treatment and sizing

Toughening of fiber-reinforced epoxy composites while maintaining other mechanical properties represents a significant challenge. This paper presents an approach of enhancing the toughness of a DGEBA/mPDA-based carbon fiber-reinforced epoxy composite, without significantly reducing the static-mechanical properties such as flexural properties and glass transition temperature. The impact of combining an UV-ozone fiber surface treatment with an aromatic and aliphatic epoxy fiber sizing on composite toughness is investigated. Carbon fiber-epoxy adhesion was increased as measured by the single fiber interfacial shear test. The Mode I composite fracture toughness was enhanced by 23% for the UV-ozone fiber surface treatment alone. With the addition of an aromatic and aliphatic fiber sizing, the composite fracture toughness was further increased to 50% and 84% respectively over the as-received, unsized fiber. The increased fiber/matrix adhesion also improved the transverse flexural strength.     

Effect of fibre/matrix adhesion on residual strength of notched composite laminates

Effects of fibre/matrix adhesion and residual strength of notched polymer matrix composite laminates (PMCLs) and fibre reinforced metal laminates (FRMLs) were investigated. Two different levels of adhesion between fibre and matrix were achieved by using the same carbon fibres with or without surface treatments. After conducting short-beam shear and transverse tension tests for fibre/matrix interface characterisation, residual strength tests were performed for PMCLs and FRMLs containing a circular hole/sharp notch for the two composite systems. It was found that laminates with poor interfacial adhesion between fibre and matrix exhibit higher residual strength than those with strong fibre/matrix adhesion. Major failure mechanisms and modes in two composite systems were studied using SEM fractography. The effective crack growth model (ECGM) was also applied to simulate the residual strength and damage growth of notched composite laminates with different fibre/matrix adhesion. Predictions from the ECGM were well correlated with experimental data.     

Controlling fracture toughness of matrix for ductile fiber reinforced cementitious composites

An experimental study was carried out to find material parameters for making fiber reinforced cementitious composites (FRCC) more ductile. One of the dominant factors to control the ductility might be hidden in fracture property of matrix as well as the interface property between fiber and matrix. Therefore this study varied air content and water-binder ratio as the parameters to change the fracture property of matrix and experimentally examined their influence on the ductility of FRCC by three-point bend test with notched beams. As a result, it is concluded that fracture toughness of the matrix could be one of key parameters to control the ductility of FRCC. In case of a polyethylene fiber used in this study, the optimum value of the fracture toughness (critical strain energy release rate): G_IC of the matrix was obtained to be 7.5-8.0 N/m.     

Investigation of fiber/matrix adhesion: test speed and specimen shape effects in the cylinder test

The cylinder test, developed from the microdroplet test, was adapted to assess the interfacial adhesion strength between fiber and matrix. The sensitivity of cylinder test to pull-out speed and specimen geometry was measured. It was established that the effect of test speed can be described as a superposition of two opposite, simultaneous effects which have been modeled mathematically by fitting two parameter Weibull curves on the measured data. Effects of the cylinder size and its geometrical relation on the measured strength values have been analyzed by finite element method. It was concluded that the geometry has a direct influence on the stress formation. Based on the results achieved, recommendations were given on how to perform the novel single fiber cylinder test.     

Interfacial strength and fracture energy of individual carbon nanofibers in epoxy matrix as a function of surface conditions

The interfacial shear strength (IFSS) and fracture energy of individual carbon nanofibers embedded in epoxy were obtained for different surface conditions and treatments by novel, MEMS-based, nanoscale fiber pull-out experiments. As-grown vapor grown carbon nanofibers (VGCNFs) with turbostratic surface and 5 nm peak-to-valley surface roughness exhibited high IFSS and interfacial fracture energy, averaging 106 ± 29 MPa and 1.9 ± 0.9 J/m², respectively. Subsequent high temperature heat treatment and graphitization resulted in drastically reduced IFSS of 66 ± 10 MPa and interfacial fracture energy of 0.65 ± 0.14 J/m². The smaller IFSS values and the reduced standard deviation were due to significant reduction of the fiber surface roughness to 1–2 nm, as well as a decrease in surface defect density during conversion of turbostratic and amorphous carbon to highly ordered graphitic carbon. For both grades of VGCNFs failure was adhesive with clear nanofiber surfaces after debonding. Oxidative functionalization of high temperature heat-treated VGCNFs resulted in much higher IFSS of 189 ± 15 MPa and interfacial fracture energy of 3.3 ± 1.0 J/m². The debond surfaces of functionalized nanofibers had signs of matrix residue and/or shearing of the outer graphitic layer of the VGCNFs, namely the failure mode was a combination of cohesive matrix and/or cohesive fiber failure which contributed to the high IFSS. For all three grades of VGCNFs the IFSS was independent of fiber length and diameter. The findings of this experimental study emphasized the critical role of nanofiber surface morphology and chemistry in determining the shear strength and fracture energy of nanofiber interfaces, and shed light to prior composite-level strength and fracture toughness measurements.     

单丝断裂双树脂法研究碳纤维/环氧树脂界面粘结性能

建立了单丝断裂双树脂体系法,利用外层树脂的韧性使包埋于内层脆性树脂中的纤维单丝断裂达到饱和,解决了断裂伸长率较低的树脂基体采用传统的单丝断裂法无法测得界面剪切强度的问题.分别采用界面剪切强度和界面断裂能作为表征参量,考察了干态及湿热条件下两种T300级和两种T800级碳纤维/环氧树脂的界面性能,并与单丝断裂单树脂体系的界面性能进行比较.结果表明:单丝断裂双树脂体系与单树脂体系在表征碳纤维/环氧树脂的界面性能上定性规律一致;双树脂体系界面断裂能和界面剪切强度均可评价界面的耐湿热性能,且二者得到的变化规律一致;湿热处理后界面粘结性能均呈下降趋势,国外碳纤维体系的界面耐湿热性能明显优于国产碳纤维体系.     

Improvement of the bonding interface in hybrid fiber/particle preform reinforced Al matrix composite

The bonding interface between the reinforcement and the matrix alloy in hybrid AZS fiber/SiC particle preform based aluminum metal matrix composites (Al MMCs) has been investigated as a function of reinforced particle size and the binder content. It is observed that high binder and large particle will result in a poor bonding interface. This has deleterious effects on the mechanical properties of the cast MMCs. Estimation of the binder thickness indicates that there exists a critical particle size above which the particles are not appropriate to be used in fabricating the hybrid fiber/particle preform based MMCs.     

单丝断裂双树脂法研究碳纤维/环氧树脂界面粘结性能

建立了单丝断裂双树脂体系法, 利用外层树脂的韧性使包埋于内层脆性树脂中的纤维单丝断裂达到饱和, 解决了断裂伸长率较低的树脂基体采用传统的单丝断裂法无法测得界面剪切强度的问题。分别采用界面剪切强度和界面断裂能作为表征参量, 考察了干态及湿热条件下两种T300级和两种T800级碳纤维/环氧树脂的界面性能, 并与单丝断裂单树脂体系的界面性能进行比较。结果表明: 单丝断裂双树脂体系与单树脂体系在表征碳纤维/环氧树脂的界面性能上定性规律一致; 双树脂体系界面断裂能和界面剪切强度均可评价界面的耐湿热性能, 且二者得到的变化规律一致; 湿热处理后界面粘结性能均呈下降趋势, 国外碳纤维体系的界面耐湿热性能明显优于国产碳纤维体系。     

Role of controlled debonding along fiber/matrix interfaces in the strength and toughness of metal matrix composites

In metal matrix composites toughness is derived primarily from the plastic work of rupture of ductile matrix ligaments between the fractured fibers and from the plastic work of simple shear separation along steps connecting major fracture terraces. In the optimization of tensile strength in the longitudinal and transverse directions together with the respective works of fracture the most important factor is the control of the extent of debonding along interfaces between the fibers and the matrix, which develops locally in the course of deformation in a continuously changing mix of modes. In Al alloy matrix composites reinforced with Al₂O₃ fibers an effective means of controlling the key interface fracture toughness is through coarsening of Al₂Cu intermetallic interface precipitates which prescribe a ductile fracture separation layer. A combined experimental approach and micromechanical modeling, utilizing a specially tailored novel tension/shear: traction/separation law provides the means for further optimization of overall behavior. This revised version was published online in July 2006 with corrections to the Cover Date.     

The effect of surface modifications on sisal fiber properties and sisal/poly (lactic acid) interface adhesion

The main aims of this work were to study the effect of surface modifications on sisal fiber properties as well as on fiber/poly (lactic acid) (PLA) interface adhesion. For this purpose, alkali, silane and combination of both treatments were applied to sisal fiber. The effects of treatments on fiber thermal stability, fiber wettability, morphology, tensile properties and on fiber/PLA interfacial shear strength (IFSS) were studied. After treatments IFSS values improved at least 120%, however, tensile strength of sisal fibers decreased. Alkali treatment removed some non-cellulosic components (hemicelluloses, lignin) as confirmed by Fourier transform infrared spectroscopy (FTIR) and thermogravimetric analysis (TGA). The removal of non-cellulosic materials led to fibrillated and rough morphology as observed by optical microscopy (OM). FTIR spectrum of silane treated fibers showed a band related to silane amino group and contact angle measurements confirmed that fibers became more hydrophobic. All treatments used improved fiber/PLA adhesion.     

Mode-I fracture toughness testing of thick section FRP composites using the ESE(T) specimen

Experimental and numerical analyses are performed to determine the translayer mode-I fracture toughness of a thick-section fiber reinforced polymeric composite using the eccentrically loaded, single-edge-notch tension, ESE(T) specimen. Finite element analyses using the virtual crack closure technique were performed to assess the effect of material orthotropy on the mode-I stress intensity factors in the ESE(T) specimen. The stress intensity factors for the proposed ESE(T) geometry, are calculated as a function of the material orthotropic parameters. The formula is validated for a class of thick composite materials. The thick composite tested in this study is a pultruded composite material that consists of roving and continuous filament mat layers with E-glass fiber and polyester matrix materials. Data reduction from the fracture tests was performed using two methods based on existing metallic and composite ASTM [ASTM E 1922, Standard Test Method for Translaminar Fracture Toughness of Laminated Polymer Matrix Composites, Annual Book of ASTM Standards, 1997; ASTM E 399, Standard Test Method for Plane-Strain Fracture Toughness of Metallic Materials, Annual Book of ASTM Standards, 1997] fracture testing standards. Criteria for assessing test validity and for determining the critical load used in calculating the fracture toughness were examined. Crack growth measurements were performed to determine the amount of stable crack growth before reaching critical load. The load versus notch mouth opening displacement, for different crack length to width ratios is affected by material orthotropy, nonlinearity, and stable crack propagation. The mode-I translayer fracture toughness and response during crack growth is reported for ESE(T) specimen with roving layers oriented both, transverse and parallel to the loading direction.     

Control of strength anisotropy of metal matrix fiber composites

Summary This paper examines theoretically the stress distribution around fiber breaks in a unidirectional reinforced metal matrix composite, subjected to axial loading when plastic yielding of the matrix is allowed to occur. The composites considered have a ductile interphase, bonding the matrix to the fiber. The likelihood of failure of a fiber adjacent to the existing broken fiber is considered. Detailed and systematic results are given for composites with a wide range of fiber volume fractions, Young's modulus of the fibers and the matrix, interphase properties and Weibull modulus for the strength of the fibers. The objective is the optimization of these material and geometric variables to ensure global load sharing among the fibers in the longitudinal direction, which will give the composite good longitudinal strength. Calculations are carried out for transverse loading of the composite to determine the effect of the ductile interphase on the yield strength. Characteristics of the ductile interphase are determined that will provide good longitudinal strength through global load sharing and a relatively high yield strength in the direction transverse to the fibers. This, in turn, will allow control of the strength anisotropy of uniaxially reinforced metal matrix composites.