Correlation of fiber pull-out strength and interfacial vibration damping techniques by micromechanical analysis

Adhesion between fiber and matrix in fiber-reinforced polymer composites plays an important role both in controlling mechanical properties and in the overall performance of composites. This suggests that analytical and experimental methods to characterize the interface can be used to predict the mechanical performance of the material. To this end, vibration damping techniques have been used as a non-destructive method to evaluate interfacial effects on composites. According to the theory of energy dissipation, the quality of the interfacial adhesion can be evaluated upon separating the predicted internal energy dissipation associated with perfect adhesion from the measured internal energy dissipation of a composite system; this enables the quantification of interfacial adhesion. A micromechanics-based model for evaluating the adhesion between fiber and matrix from the damping characteristic of a cantilever beam was developed that shows an inverse relationship between the damping contributed by the interface and its adhesion strength. A simple optical system was used to measure the damping factor of unidirectional fiber-reinforced-polymer composites. Cantilever beam specimens containing either a single glass fiber or three types of single metallic wires embedded in an epoxy resin matrix were tested. A correlation was found between the measured interfacial adhesion strength directly from microbond pull-out tests and the micromechanics-based calculations from vibration damping experiments.     

‘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.     

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.     

Investigation of the 12 orientations variants of nanoscale Al precipitates in eutectic Si of Al-7Si-0.6Mg alloy

Various orientations and diffraction patterns from nanoscale Al precipitates in eutectic Si were investigated by high-resolution transmission electron microscopy combined with transition matrix and stereographic projection.It was found that the Al precipitates had 12 variants,all orientation relationships can be expressed as:(001)Al//{111}Si,[110]Al//<110>Si.Further,a new diffraction pattern model from Al precipitates was established under[111]Si zone axis,which was in good agreement with the experiment data.The microstructure,adhesion strength and electronic structure of the interface between Al precipitate and Si matrix were studied by first-principles calculation and experimental observation.The results show that the covalent bonds are formed between interfacial Al and Si atoms,which play a key role in interfacial bind strength.Based on the Griffith fracture theory,the cracks tend to form and expand in the interior of Al precipitates firstly,and the interfaces can act as a protective layer to prevent crack propagation.Therefore,the nanoscale Al precipitates will improve the toughness of eutectic Si particles by releasing part of stress through lattice distortion.In addition,the stretched nanoscale Al precipitates can act as effective heterogeneous nucleation sites for high density deformation nanotwins in eutectic Si during deformation,which significantly improved the deformability of eutectic Si.     

A study of the mechanical properties of short natural-fiber reinforced composites

The degree of fiber–matrix adhesion and its effect on the mechanical reinforcement of short henequen fibers and a polyethylene matrix was studied. The surface treatments were: an alkali treatment, a silane coupling agent and the pre-impregnation process of the HDPE/xylene solution. The presence of Si–O–cellulose and Si–O–Si bonds on the lignocellulosic surface confirmed that the silane coupling agent was efficiently held on the fibres surface through both condensation with cellulose hydroxyl groups and self-condensation between silanol groups.

The fiber–matrix interface shear strength (IFSS) was used as an indicator of the fiber–matrix adhesion improvement, and also to determine a suitable value of fiber length in order to process the composite with relative ease. It was noticed that the IFSS observed for the different fiber surface treatments increased and such interface strength almost doubled only by changing the mechanical interaction and the chemical interactions between fiber and matrix.

HDPE-henequen fiber composite materials were prepared with a 20% v/v fiber content and the tensile, flexural and shear properties were studied. The comparison of tensile properties of the composites showed that the silane treatment and the matrix-resin pre-impregnation process of the fiber produced a significant increase in tensile strength, while the tensile modulus remained relatively unaffected. The increase in tensile strength was only possible when the henequen fibers were treated first with an alkaline solution. It was also shown that the silane treatment produced a significant increase in flexural strength while the flexural modulus also remained relatively unaffected. The shear properties of the composites also increased significantly, but, only when the henequen fibers were treated with the silane coupling agent. Scanning electron microscopy (SEM) studies of the composites failure surfaces also indicated that there is an improved adhesion between fiber and matrix. Examination of the failure surfaces also indicated differences in the interfacial failure mode. With increasing fiber–matrix adhesion the failure mode changed from interfacial failure and considerable fiber pull-out from the matrix for the untreated fiber to matrix yielding and fiber and matrix tearing for the alkaline, matrix-resin pre-impregnation and silane treated fibers.     

Surface modification and adhesion mechanisms in woodfiber-polypropylene composites

The interfacial adhesion between wood fiber and thermoplastic matrix polymer plays an important role in determining the performance of wood-polymer composites. The objectives of this research were to elucidate the interaction between the anhydride groups of maleated polypropylene (MAPP) and hydroxyl groups of wood fiber, and to clarify the mechanisms responsible for the interfacial adhesion between wood fiber and polypropylene matrix. The modification techniques used were bulk treatment in a thermokinetic reactive processor and solution coating in xylene. FT-IR was used to identify the nature of bonds between wood fiber and MAPP. IGC and wood veneer pull-out test was used to estimate the interfacial adhesion. Mechanical properties of injection molded woodfiber-polypropylene composites were also determined and compared with the results of esterification reaction and interfacial adhesion tests. Confocal Microscopy was employed to observe the morphology at the wood fiber-polypropylene interface, and the dispersion and orientation of wood fiber in the polypropylene matrix, respectively. The effectiveness of MAPP to improve the mechanical properties (particularly the tensile strength) of the composites was attributed to the compatibilization effect which is accomplished by reducing the total wood fiber surface free energy, improving the polymer matrix impregnation, improving fiber dispersion, improving fiber orientation, and enhancing the interfacial adhesion through mechanical interlocking. There was no conclusive evidence of the effects of ester links on the mechanical properties of the composites.     

Multi-scale investigation of microstructure,fiber pullout behavior,and mechanical properties of ultra-high performance concrete with nano-CaCO3 particles

The mechanical properties of a fiber-reinforced concrete are closely related to the properties of the matrix, fiber, and fiber-matrix interface. The fiber-matrix bond property is mainly governed by the adhesion between the fiber and surrounding cement materials, as well as the strength of materials at the interfacial transition zone. In this paper, the effect of nano-CaCO₃ content, varying between 0 and 6.4%, by mass of cementitious materials, on microstructure development, fiber-matrix interfacial bond properties, and mechanical properties of ultra-high performance concrete (UHPC) reinforced with 2% steel fibers were investigated. The bond properties, including bond strength and pullout energy, were evaluated. Mercury intrusion porosimetry (MIP), backscattered electron microscopy (BSEM), optical microscopy, and micro-hardness testing were used to characterize the microstructure of matrix and/or interfacial transition zone (ITZ) around an embedded steel fiber. Test results indicated that the incorporation of 3.2% nano-CaCO₃ significantly improved the fiber-matrix bond properties and the flexural properties of UHPC. This was attributed to densification and strength enhancement of ITZ as observed from micro-structural analyses. Beyond the nano-CaCO₃ content of 3.2%, the fiber bond and mechanical properties of UHPC decreased due to increased porosity associated with agglomeration of the nano-CaCO₃.     

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.     

玻璃包覆Co68Fe4.5Si13.5B14非晶微丝的力学性能

以玻璃包覆Co68Fe4.5Si13.5B14非晶微丝为研究对象,对经氢氟酸溶液腐蚀不同时间的微丝和不同直径的原丝进行了力学性能评价和断口形貌分析。结果表明,玻璃包覆非晶微丝的断裂过程是弹性变形。外径为28μm、内径为8.8μm的微丝经氢氟酸溶液腐蚀,刚去掉玻璃包覆层时裸丝的抗拉强度最大,可达到3545MPa,应变量为1.96%;若微丝经酸液腐蚀仍存在玻璃层,当腐蚀时间为40s时,抗拉强度和延伸率达到该阶段的最大值,分别为724MPa和1.3%;同时玻璃包覆Co68Fe4.5Si13.5B14非晶微丝具有尺寸效应,微丝的抗拉强度随直径的减小而增大。     

A new method to normalize the effect of matrix properties on the value of interfacial shear strength obtained from the fragmentation test

A new method, based on tensile yield strength and strain, has been developed to normalize the effect of matrix properties on the critical fibre length and the interfacial shear strength obtained from the fragmentation test. It is argued that the conventional data normalization technique which employs elastic properties of the matrix, is fundamentally flawed because the model employed to calculate interfacial shear strength assumes perfect plasticity. Single embedded fibre fragmentation in a range of epoxy resins with differing mechanical properties has been used to validate the new method. Stoichiometric quantities of the current agent were used to keep the same interfacial chemistry. The proposed method provides more consistent interfacial shear strength data than existing theories. Furthermore, this normalization technique can also be used to predict the interfacial shear strength of glass fibres embedded in a range of support resins, such as vinyl ester or epoxy resins. For these cases, a thin layer of the phenolic resin was used on the glass fibre to keep the interface chemistry the same. This revised version was published online in November 2006 with corrections to the Cover Date.     

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.     

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。     

国产T800碳纤维/双马来酰亚胺复合材料的界面及力学性能

分别采用日本东丽T800H和国产T800碳纤维作为增强体,采用热压罐工艺制备双马来酰亚胺树脂基复合材料。研究了2种碳纤维的表面物理和化学状态,复合材料的微观界面性能及力学性能。结果表明:国产T800碳纤维表面沟槽分布较多,表面粗糙度较高,有利于与树脂基体形成更好的物理结合作用。同时,国产T800碳纤维表面具有较多的含氧官能团,有利于与基体树脂形成更好的化学结合作用。因此,国产T800碳纤维的界面剪切强度较T800H碳纤维高约27%。国产T800/HT-280复合材料的力学性能均普遍高于T800H/HT-280复合材料,其中,90°拉伸强度高约25%,面内剪切强度、弯曲强度高约12%,层间剪切强度高约7%。      

Investigation on adhesion, interphases, and failure behaviour of cyclic butylene terephthalate (CBT)/glass fiber composites

Interphases exist in hybrid materials and significantly influence their mechanical performance. To find a bridge between the microscopic and macroscopic mechanical properties, this work investigates the microscopic nature of glass fiber surfaces and glass/CBT interphases in terms of topography, fractography, and adhesion properties. The variations in glass fiber surface properties result from the different sizings. Using the single fiber pull-out test, AFM, and ζ potential tests, it is shown that the interfacial bond strengths in CBT resin composites can vary depending on the kind of sizing formulation and properties. The greatest adhesion strength is achieved by aminosilane sizings with epoxy resin film former. The surface roughness of the fibers can be varied by sizings with different content and ζ potential values, which has no significant contribution to interphase adhesion strength from ‘mechanical interlocking’. For the systems with film formers, cohesive failure occurs and similar values of both interfacial adhesion strength, τ_d, and fracture energy release rate, G_ic, are obtained, in which τ_d approaches the shear yield strength of CBT matrix. A further enhancement of interfacial adhesion is limited by the mechanical properties and the non-homogeneous microstructure of CBT resin due to the less-than-perfect CBT polymerization.     

The interfacial properties of aramid/epoxy model composites

Many attempts have been made to measure, evaluate and improve the level of interfacial adhesion in aramid/epoxy composites. Different surface treatments have been developed in order to promote chemical bonding between the fibre and the matrix but it is found that most of the surface treatments developed have shown little or no improvement in the level of interfacial adhesion. The interfacial properties of a model composite are often determined by measuring the interfacial shear strength using micromechanical test methods that employ different loading configurations. However, the values of interfacial shear strength determined using different test methods are found to be dependent upon the variation of localized stress in the samples due to the different loading configurations and often give different results. Using Raman spectroscopy it is shown that the strain-dependent shift of the 1610 cm^–1 aramid Raman band can be used to determine the point-to-point variation of axial fibre strain along aramid fibres embedded in epoxy resin matrices from which the interfacial properties can be derived. The interfacial properties of aramid/epoxy model composites have been determined using Raman spectroscopy where the properties of the fibre, including different surface treatments, and the matrix have been changed systematically. The results are reviewed here and compared to those obtained using conventional micromechanical test methods. It is also demonstrated that the Raman technique can be used to characterize the interfacial properties of aramid/epoxy model composites deformed using different micromechanical test methods. In this way the interfacial properties can be determined at different loading levels enabling the progressive failure of the fibre/matrix interface to be monitored and defined accurately.     

Effect of moisture absorption on the micromechanical behavior of carbon fiber/epoxy matrix composites

Carbon fiber/epoxy material in the form of a single fiber unidirectional composite was subjected to controlled humidity environments. Moisture uptake in polymer composites has significant effects on the mechanical properties of the matrix as well as on the final performance of the composite material. Diminishing of the mechanical properties of the matrix is attributed to a decrease of its glass transition temperature (T _g). The quality of the fiber–matrix interphase was assessed using the single fiber fragmentation test and the fiber-fragment length, considered as an indicator of interfacial quality. In order to measure the fiber fragment lengths and indentify failure mechanism at the interface optical observation and acoustic emission technique were used. The speed of propagation of an acoustic wave in the material was also determined. A comparison is made of interfacial shear strength values determined by acoustic emission and optical techniques. Excellent agreement between the two techniques was obtained. By means of a micromechanical model, it was possible to determine from the fragmentation lengths a measure of the interfacial shear strength between the fiber and the matrix. The role of moisture uptake swelling of the matrix on the residual stresses is considered to be important when considering the effect deterioration of interfacial shear properties. Both the contribution of the radial stresses and the mechanical component of fiber–matrix adhesion are seen to decrease rapidly for higher moisture contents in the matrix and/or interface.     

玻璃纤维增强HDPE的性能及界面研究

通过扫描电镜观察、红外光谱分析及材料力学性能试验等方法考察了不同界面粘结形式下玻璃纤维增强HDPE的力学性能及其与界面粘结性的关系。结果表明,复合过程中加入的界面反应性试剂及其与HDPE接枝而形成的接枝物可与玻纤表面及其硅烷发生化学作用或交(?),从而显著提高复合材料的界面粘结强度及其力学性能。     

Preparation and characterization of carbon nanotube/polyetherimide nanocomposite films

Multi-walled carbon nanotube (MWCNT)/polyetherimide (PEI) nanocomposite films have been prepared by casting and imidization. A homogeneous dispersion of MWCNTs throughout the PEI matrix is observed by scanning electron microscopy of fracture surfaces, which shows not only a fine dispersion of MWCNTs but also strong interfacial adhesion with the matrix, as evidenced by the presence of many broken but strongly embedded carbon nanotubes (CNTs) in the matrix and by the absence of debonding of CNTs from the matrix. Differential scanning calorimetry and dynamic mechanical analysis show that the glass transition temperature of PEI increases by about 10 °C by the addition of 1 wt% MWCNTs. Mechanical testing shows that for the addition of 1 wt% MWCNTs, the elastic moduli of the nanocomposites are significantly improved by about 250% while the tensile strength is comparable to that of the matrix. This improvement is due to the strong interfacial interaction between the MWCNTs and the PEI matrix which favors stress transfer from the polymer to the CNTs.     

Grafting Low Contents of Branched Polyethylenimine onto Carbon Fibers to Effectively Improve Their Interfacial Shear Strength with an Epoxy Matrix

The mechanical properties of carbon fiber (CF) reinforced composites are greatly dependent on the interfacial strength between the CFs and matrix. To improve the interfacial adhesion of carbon fiber/epoxy composites, branched polyethylenimine (PEI) is grafted onto the CFs treated in a mixed acid at optimized process time. The chemical compositions and bonds of functionalized CFs are characterized by thermal gravimetric analysis, Fourier‐transform infrared, and X‐ray photoelectron spectroscopy. The surface structures and morphologies of various CFs are analyzed by Raman spectroscopy and scanning electron microscopy, respectively. Microbond test is adopted to evaluate the interfacial shear strength (IFSS) between the CFs and epoxy matrix. The results show that the CFs modified by low molecular weight PEI are better than those modified by high molecular weight PEI. The IFSS of PEI modified CFs can reach a maximum of 107.2 ± 14.3 MPa at a low functionalization degree compared with 78.1 ± 11.6 MPa of unmodified CFs. The branched structure and high density of active amine groups on the PEI chains are responsible for the improved interfacial strength.     

Preparation and properties of polypropylene composites reinforced with wheat and flax straw fibres: Part II Analysis of composite microstructure and mechanical properties

The microstructure and mechanical properties of polypropylene composites containing flax and wheat straw fibres are discussed. Particular emphasis has been given to determining the nature and consequences of fibre damage induced during melt-processing operations, fibre orientation occurring in mouldings, and possible interfacial adhesion between the matrix and fibres. Compared to unfilled polypropylene, addition of flax and wheat straw caused a significant increase in tensile modulus, particularly, in the case of flax fibres, which also gave higher tensile yield strength and Charpy toughness, despite a lack of interfacial bonding. Tensile strength was increased further through inclusion of 5% by weight of maleic anhydride-modified polypropylene, which was shown to promote adhesion between fibres and matrix. This revised version was published online in November 2006 with corrections to the Cover Date.