Ageing effect on microstructural and mechanical properties of mullite-ZrO2-TiO2 composites

The microstructural and mechanical properties of mullite-zirconia composites with TiO₂ (0.25 and 1.0 mol) additions have been studied, after ageing the samples over a wide temperature range (1000 to 1500° C) for long periods of time (100 to 200 h). In the sample with 0.25 mol TiO₂ addition, changes in mullite composition and in the solid state compatibility at temperatures below 1450° C were detected. In the sample containing 1 mol TiO₂, decomposition of Al₂TiO₅ occurs atT1200° C. Both compositions exhibit no increment in zirconia average grain size during ageing and, concomitantly, there is no strength degradation until higher temperatures (>1400° C) are reached, which become more drastic when Al₂Ti₅ is present.     

Simulation of fatigue performance of cross-ply composite laminates

The fatigue life of cross-ply composite laminates was evaluated using a statistical model. A modified shear-lag analysis was applied to describe the cycle-number-dependent stiffness reduction and consequent stress redistribution processes in the laminates resulted from both progressive transverse matrix cracking in transverse plies and local delamination at tips of transverse cracks. From the strength degradation behaviour and the static strength distribution of 0° plies as well as the fatigue behaviour of 90° plies, the fatigue life of cross-ply laminates with various types of lay-up can be simulated from the model. Predictions of fatigue performance are compared with experimental data for [0/90₂] _s , [02/90₂] _s and [0₂/90₄] _s graphite/epoxy cross-ply laminates: good agreements are obtained.     

The effect of thermal ageing on carbon fibre-reinforced polyetheretherketone (PEEK)

The morphological properties of carbon fibre-reinforced PEEK (APC-2) laminates subjected to long-term thermal ageing and cycling treatments have been studied using differential scanning calorimetry and wide-angle X-ray diffraction techniques. This work sought provided a structural explanation for measured changes in mechanical properties. Annealing at 120 ° had no effect but significant changes in crystal content and crystal perfection occurred at 250 ° and 310 °C. At 250 °C, for short ageing periods, both crystal growth and perfection processes were observed. For longer ageing periods, there was a multiple increase in capital perfection. Initial ageing at 310 °C caused rapid crystal growth, but further ageing resulted in a reduction in measured crystal contents due to thermal degradation.     

Monitoring quasi-static and cyclic fatigue damage in fibre-reinforced plastics by Poisson’s ratio evolution

Even if the extent of fatigue damage in fibre-reinforced plastics is limited, it can already affect the elastic properties. Therefore, the damage initiation and propagation in composite structures is monitored very carefully. Beside the use of nondestructive testing methods (ultrasonic inspection, optical fibre sensing), the follow-up of the degradation of engineering properties such as the stiffness is a common approach.In this paper, it is proved that the Poisson’s ratio can be used as a sensitive indicator of fatigue damage in fibre-reinforced plastics. Static tests, quasi-static cyclic tests and fatigue tests were performed on [0°/90°]_2s glass/epoxy laminates, and longitudinal and transverse strain were measured continuously. The evolution of the Poisson’s ratio ν_xy versus time and longitudinal strain ε_xx is studied. As the transverse strain measurement is crucial to monitor the degradation of the Poisson’s ratio, three techniques were applied to measure the transverse strain (strain gauges, mechanical extensometer and external optical fibre sensor).Finally, the technique has been applied to a totally different material: a carbon fabric thermoplastic composite. The results show a very similar degradation of the Poisson’s ratio, although no stiffness degradation can be observed during fatigue loading of this material.It is concluded that the degradation of the Poisson’s ratio can be a valuable indicator of fatigue damage, in combination with the stiffness degradation.     

The relationship between sensitisation and small punch test behaviour in a high-nitrogen austenitic stainless steel at cryogenic temperatures

Austenitic stainless components used in nuclear fusion reactors must be capable of maintaining reasonable mechanical properties to thermal ageing caused by welding and in‐service. Recently, high‐nitrogen (High‐N) austenitic stainless steels (SS) are receiving increased attention because of their strength advantages, but they have been found to be susceptible to dichromium nitride (Cr₂N) precipitation during thermal exposure at 823–1073 K. The susceptibility to sensitisation at thermal ageing temperature for high‐N austenitic SS is examined using the single‐loop electrochemical potentiokinetic reactivation (EPR) test. High‐N SS were found to be susceptible to sensitisation caused by grain boundary precipitation of Cr₂N, with the degree of sensitisation increasing systematically with ageing time and temperature. In particular, it was found that the precipitates, which effected sensitisation, were changed from carbides (M₂₃C₆) to nitrides (Cr₂N) with increasing ageing time and temperature. The deterioration of mechanical properties associated with thermal ageing in high‐N SS was investigated by a small punch (SP) test using miniature specimens at cryogenic temperatures. Results indicated that the degradation of mechanical properties in this alloy was caused by a decrease of cohesive strength resulting from carbides (Cr₂₃C₆) and nitrides (Cr₂N) precipitated in grain boundaries.     

The effect of temperature on fatigue damage of FRP composites

The present study intends to investigate the effect of temperature on cumulative fatigue damage (D) of laminated fibre-reinforced polymer (FRP) composites. The effect of temperature on fatigue damage is formulated based on Ramkrishnan–Jayaraman and Varvani-Farahani–Shirazi residual stiffness fatigue damage models. The models are further developed to assess the fatigue damage of FRP composites at various temperatures (T). This task is fulfilled by formulating the temperature dependency of Young’s modulus (E) and ultimate tensile strength (σ_ult) as the inputs of the models. Temperature-dependant parameters of Young’s modulus and ultimate tensile strength are found to be in good agreement with the experimentally obtained data when used for unidirectional, cross-ply and quasi-isotropic FRP laminates. The proposed fatigue damage model is evaluated using six sets of fatigue damage data. The proposed temperature-dependent model was also found promising to predict the fatigue damage of unidirectional (UD) and orthogonal woven FRP composites at different temperatures.     

The effect of formulated molecular weight on temperature resistance and mechanical properties in polyimide based composites

This experimental study examines the role of formulated molecular weight between crosslink sites on the temperature resistance and mechanical properties of composites based on a polyimide containing a diphenyl thioether unit (PTI). The composites are fabricated by in situ polymerization of monomer reactants (PMR) using three monomeric ingredients: bis(3,4-dicarboxyphenyl) sulfide dianhydride (TDPA); 4,4-methylene dianiline (MDA); and the monomethyl ester of norbornene anhydride (NE). By changing monomeric molar ratio, three formulations are prepared, in which formulated molecular weight between crosslink sites varies from 1487 to 3446 g mol^–1. Unidirectional composite laminates from each formulation and T300 carbon fibres are compression moulded and cut into a series of test specimens. By measuring the glass transition temperature (T _g), Mode I interlaminar fracture toughness (G _IC) and other mechanical properties at room and elevated temperatures, the influences of formulated molecular weight on the temperature resistance and mechanical properties of PTI-based composites are investigated.     

Fatigue life prediction of carbon/epoxy laminates by stochastic numerical simulation

A three dimensional (3D) finite element model is developed to predict the progressive fatigue damage and the life of a plain carbon/epoxy laminate (AS4/3501-6) based on the longitudinal, transverse and in-plane shear fatigue characteristic. The model takes into account stress analysis, fatigue failure analysis, random distribution and material property degradation. Different cross- and angle-ply laminates including [0₈], [90₈], [0/90₂]_s, [0/90₄]_s, [0₂/90₂]_s, [30₁₆], [45/−45]_2s with the available experimental data are considered for the fatigue life simulation. In order to consider the random distribution of the laminate’s properties from element to element in the model, the laminate’s stiffness, and strength are randomly generated using a Gaussian distribution function. Sudden and gradual material properties degradation are considered during the fatigue simulation. The progressive fatigue damage and failure analysis is implemented in ABAQUS through user subroutines UMAT (user-defined material) and USDFLD (user-defined field variables). The predicted fatigue life of the simulation for different laminates is in good agreement with the experimental results.     

The influence of hydrothermal conditioning on the Mode-I,thermal and flexural properties of Carbon/Benzoxazine composites with a thermoplastic toughening interlayer

Carbon/Benzoxazine laminates with and without non-woven thermoplastic fibrous polyamide (PA) veils at the interlaminar regions were manufactured using Vacuum Assisted Resin Transfer Moulding (VARTM). The effect of the interlaminar thermoplastic veils on the Mode-I strain energy release rate (G_IC), flexural stiffness, glass transition temperature (T_g) and water absorption behaviour was determined using two commercially available Benzoxazine resins. Despite an increase in the maximum moisture content, the veils greatly enhanced G_IC by an increase in fibre bridging of PA fibres, with concurrent reductions in flexural stiffness. Water ingress resulted in large reductions in the T_g, although no significant change was observed due to the PA interlayers. Fibre bridging and fibre pull-out were the main mechanisms by which the veils assisted in resisting delamination. The presence of the water was observed to degrade mechanical properties due to a reduction in fibre/matrix interfacial strength, molecular degradation and plasticisation of the matrix.     

Processing and characterization of carbon fibre-reinforced polynaphthoxazine composite

In order to attain a high-temperature resistant composite with good performance as well as processability, a polynaphthoxazine composite with 60% by volume of carbon fibre has been successfully developed. The naphthoxazine monomer was modified to obtain lower melting point and higher solubility for improved processability. The density and void content of this composite were measured at room temperature. TheT _g and the activation enthalpy of the glass transition process were measured by dynamic mechanical analysis, and the effect of cure temperature on theT _g of the composite was studied. The thermal characteristics of this composite were studied in terms of the weight loss after isothermal ageing, the decomposition temperature from thermogravimetric analysis, and the change in dynamic storage moduli at high temperatures. Flexural and interlaminar shear tests were performed to evaluate the mechanical properties of this composite. A good balance between strength and toughness of this composite was achieved. A very high char yield of 90% was gained after carbonization in a nitrogen atmosphere. This polynaphthoxazine composite compares favourably with thebismaleimide composites in terms of mechanical properties and thermal stabilities.     

Preliminary results on thermo-oxidative ageing of multi-hole carbon/epoxy composites

During their service life, fibre-reinforced polymers are subjected to the influences of numerous ageing factors such as temperature, pressure, oxygen or moisture, which generally result in a decrease of the composite properties. This study deals with the combined actions of two damaging parameters, temperature and oxygen. Thermo-oxidation is analysed in an original way by ageing in air plain and multi-hole laminates for 9000 h. Since perforated panels have a greater surface exposed to the oxidative environment, the degradation due to oxygen is increased, thus allowing a better understanding of thermo-oxidation mechanisms. Characterisation of the aged composite includes FTIR, microscopy, weight loss measurements, DMA, compression and SBS tests. Thermo-oxidative ageing leads to oxidation and cracking of the laminates surfaces, weight loss and decrease of both compression and SBS failure strengths. The glass transition temperature remains constant. Degradation is more important for the multi-hole panels and results in a greater decrease of the physical and mechanical properties for these laminates.     

中温固化高强度环氧基体及其复合材料性能研究

本文对曾用于直升机复合材料旋翼桨叶的高强度环氧树脂基体及其复合材料性能进行了深入的研究工作。测定了单向玻璃纤维复合材料的九个工程常数和动态模量随着温度升高(20～80℃)的变化。从桨叶取样的测试数据看,Y—2复合材料的某些力学性能均优于国外同类的BO—105桨叶用复合材料。湿热老化试验表明,Y—2复合材料在45℃和90±5%湿度情况下经过3000小时老化后其强度与模量下降不到10%。对树脂基体,除了一些常规的力学性能外,还测定了四种谱图和改进了它的阻燃性能。     

Effect of underfill on bending fatigue behavior of chip scale package

This study evaluated the mechanical behavior of chip scale packages (CSPs) with the underfills using the four-point bending test. The bending fatigue durability in the CSP increased with increasing glass transition temperature (T _g ) of the underfill. The mechanical fatigue cracks occurred in the region between the (Ni,Cu)₃Sn₄ layer and the solder region near the upper substrate and the solder region of the CSP with the underfill which had the higher T _g . However, these cracks occurred in the region between the (Ni,Cu)₃Sn₄ layer and the Ni₃P layer near the bottom substrate and the solder region of the CSP with the underfill which had the lower T _g .     

Analysis of thermal fatigue behaviour of brittle structural materials

The effect of the level of maximum temperature (T _max), the temperature range (T) and the mode of convective heat transfer on the thermal fatigue resistance of brittle structural materials is analysed. Expressions are derived for the number of thermal cycles to failure in terms of the appropriate mechanical and thermal properties, crack growth parameter, T andT _max. For simultaneous changes inT _max and T commonly used in practice, the change in thermal fatigue life is governed by both the thermal stress intensity exponent (n) and the activation energy (Q) for subcritical crack growth, in contrast to the results of other studies. For constantT _max but variable T, thermal fatigue life is affected byn only, whereas, for constant T but variableT _max, the value ofQ alone governs changes in fatigue-life. Heat transfer by natural or forced convection will result in differences in thermal fatigue resistance. Recommendations are made for the design and analysis of thermal fatigue experiments. Figures-of-merit for the selection of materials with high thermal fatigue resistance are presented.     

Hygrothermal effects on the shear properties of carbon fiber/epoxy composites

The environmental factors, such as humidity and temperature, can limit the applications of composites by deteriorating the mechanical properties over a period of time. Environmental factors play an important role during the manufacture step and during composite’s life cycle. The degradation of composites due to environmental effects is mainly caused by chemical and/or physical damages in the polymer matrix, loss of adhesion at the fiber/matrix interface, and/or reduction of fiber strength and stiffness. Composite’s degradation can be measure by shear tests because shear failure is a matrix dominated property. In this work, the influence of moisture in shear properties of carbon fiber/epoxy composites (laminates [0/0]_s and [0/90]_s) have been investigated. The interlaminar shear strength (ILSS) was measured by using the short beam shear test, and Iosipescu shear strength and modulus (G ₁₂) have been determinated by using the Iosipescu test. Results for laminates [0/0]_s and [0/90]_s, after hygrothermal conditioning, exhibited a reduction of 21% and 18% on the interlaminar shear strenght, respectively, when compared to the unconditioned samples. Shear modulus follows the same trend. A reduction of 14.1 and 17.6% was found for [0/0]_s and [0/90]_s, respectively, when compared to the unconditioned samples. Microstructural observations of the fracture surfaces by optical and scanning electron microscopies showed typical damage mechanisms for laminates [0/0]_s and [0/90]_s.     

Mechanical properties of nylon 6 subjected to photodegradation

The degradation of mechanical properties in nylon 6 films due to both oxidative and non-oxidative photodegradation is studied. It is shown that in a non-oxygen environment the rate of degradation is enhanced with rising temperature due to increases in quantum yield. Experimental results obtained on specimens exposed to natural weathering are found to be difficult to relate to those obtained by accelerated ageing. It is proposed and proven that the specific energy absorption in a tensile test (W _p) is an effective parameter for characterizing photodegradation in nylon.     

Prediction of initiation of transverse cracks in cross-ply CFRP laminates under fatigue loading by fatigue properties of unidirectional CFRP in 90° direction

A fatigue life to the initiation of transverse cracks in cross-ply carbon fiber-reinforced plastic (CFRP) laminates has been predicted using properties of the fatigue strength of unidirectional CFRP in the 90° direction. In the experiments, unidirectional [90]₁₂ laminates were used to obtain a plot of maximum stress versus number of cycles to breaking, and two types of cross-ply laminates of [0/90₄]_S and [0/90₆]_S were used to evaluate the initiation and multiplication of transverse cracks under fatigue loading. Transverse cracks were studied by optical microscopy and soft X-ray photography. Analytical and experimental results showed good agreement, and the fatigue life for transverse crack initiation in cross-ply laminates was predicted successfully from the fatigue strength properties of the unidirectional CFRP in the 90° direction. The prediction results showed a conservative fatigue life than the experimental results.     

Verhalten laserschockverfestigter und festgewalzter Randschichten der Ti‐Legierung Ti‐6Al‐4V bei schwingender Beanspruchung unter erhöhten Temperaturen

Residual stress stability and near‐surface microstructures in high temperature fatigued mechanically surface treated Ti‐6Al‐4V It is well known that mechanical surface treatments, such as deep rolling, shot peening and laser shock peening, can significantly improve the fatigue behavior of highly‐stressed metallic components. Deep rolling is particularly attractive since it is possible to generate, near the surface, deep compressive residual stresses and work hardened layers while retaining a relatively smooth surface finish. In the present investigation, the effect of deep rolling on the low‐cycle and high‐cycle fatigue behavior of a Ti‐6Al‐4V alloy is examined, with particular emphasis on the thermal and mechanical stability of the residual stress states and the near‐surface microstructures. Preliminary results on laser shock peened Ti‐6Al‐4V are also presented for comparison. Particular emphasis is devoted to the question of whether such surface treatments are effective for improving the fatigue properties at elevated temperatures up to ～450 °C, i.e., at an homologous temperature of ～0.4 T/T_m (where T_m is the melting temperature). Based on cyclic deformation and stress/life (S/N) fatigue behavior, together with the X‐ray diffraction and in situ transmission electron microscopy observations of the microstructure, it was found that deep rolling can be quite effective in retarding the initiation and initial propagation of fatigue cracks in Ti‐6Al‐4V at such higher temperatures, despite the almost complete relaxation of the near‐surface residual stresses. In the absence of such stresses, it is shown that the near‐surface microstructures, which in Ti‐6Al‐4V consist of a layer of work hardened nanoscale grains, play a critical role in the enhancement of fatigue life by mechanical surface treatment.     

Mechanical and thermal behavior of non-crimp glass fiber reinforced layered clay/epoxy nanocomposites

Mechanical and thermal properties of non-crimp glass fiber reinforced clay/epoxy nanocomposites were investigated. Clay/epoxy nanocomposite systems were prepared to use as the matrix material for composite laminates. X-ray diffraction results obtained from natural and modified clays indicated that intergallery spacing of the layered clay increases with surface treatment. Tensile tests indicated that clay loading has minor effect on the tensile properties. Flexural properties of laminates were improved by clay addition due to the improved interface between glass fibers and epoxy. Differential scanning calorimetry (DSC) results showed that the modified clay particles affected the glass transition temperatures (T_g) of the nanocomposites. Incorporation of surface treated clay particles increased the dynamic mechanical properties of nanocomposite laminates. It was found that the flame resistance of composites was improved significantly by clay addition into the epoxy matrix.     

Fatigue life prediction of composite laminates by FEA simulation method

This paper is to simulate the fatigue damage evolution in composite laminates and predict fatigue life of the laminates with different lay-up sequences on the basis of the fatigue characteristics of longitudinal, transverse and in-plane shear directions by finite element analysis (FEA) method. In FEA model, considering the scatter of the material’s properties, each element was assigned with different material’s properties. The stress analysis was carried out in MSC Patran/Nastran, and a modified Hashin’s failure criterion was applied to predict the failure of the elements. A new stiffness degradation model was proposed and applied in the simulation and then a strength degradation model was deduced, which is coupled with the presented stiffness degradation model. The reduced or discounted elastic constants were determined based on the failure mechanism of the laminates and the restrictive conditions of orthotropic property. The fatigue behavior and fatigue life of six kinds of E-glass/epoxy composite laminates with different lay-up sequences were experimentally studied, and the S–N curves and stiffness degradation models in longitudinal, transverse and in-plane shear direction were obtained. These fatigue data were adopted in the simulation to simulate fatigue behavior and estimate life of the laminates. The simulation results, including the fatigue life predicted and the residual stiffness, were coincident with the experimental results well except for the quasi-isotropic laminate for the lack of consideration of the out-of-plane fatigue character in the simulation.