Environmental aging of high-performance polymeric composites: Effects on durability

The effect of sub-T_g environmental aging on the durability of two high-performance polymeric composites has been investigated. The material systems under study were a thermoplastic-toughened cyanate ester resin (Fiberite 954-2) and a semicrystalline thermoplastic resin (Fiberite ITX), and their respective carbonfiber composites, IM8/954-2 and IM8/ITX. Specimens were aged for periods of up to 9 months in environmental chambers at 150 °C and in one of three different gas environments: nitrogen, a reduced air pressure of 13·8 kPa (2psi air) or atmospheric ambient air (14·7psi air). The glass transition temperatures, T_g, of the two resin systems were monitored as a function of aging time and environment. The changes in T_g showed effects of both physical aging and chemical degradation; the latter appeared to be sensitive to the oxygen concentration in the aging environment. Flexure tests were performed on 8-ply unidirectional (90 °) IM8/954-2 and IM8/ITX composites, aged up to 6 months in the three gas environments at 150 °C. The samples showed a 30–40% loss in the bending strength after aging. These strength reductions were sensitive to the oxygen concentrations in the aging environment. Stress/strain tests were also conducted on the same composites to measure the ultimate properties of the materials before and after aging in the three different environments at 150 °C. The results showed a decrease of 40–60% in the ultimate strain to failure with aging. The modulus of both composite systems on the other hand increased by up to 20 % after aging for 6 months, possibly as a consequence of the physical aging phenomena. In both systems greatest reduction in ‘useful’ mechanical properties occurred in the ambient air environment, while the least reduction occurred in nitrogen. Weight loss in the plain resin and composite samples was monitored as a function of aging time and environment. Typically, all of the samples showed 1–2 % weight loss after 9 months of aging at 150 °C, and the composite samples lost much more weight (on a polymer basis) than unreinforced resin specimens over the same aging period. The weight loss data as well as all the above-mentioned observations were indicative of an oxidation process in the composites.     

High strain rate compressional behavior of stitched and unstitched composite laminates with radial constraint

This paper is concerned with the high strain rate compressional behaviour of glass/epoxy (Hy-E 9134B, Fiberite, USA) composite laminates with or without stitching reinforcement by untwisted Kevlar-49 threads (1140 denier). The split Hopkinson pressure bar (SHPB) apparatus is used in performing the high strain rate tests. Test data are analyzed in a manner similar to that reported by Hauser Exp. Mech., 6 (1966) 395. Specimens are tested at strain rates up to 10⁴ s⁻¹. Unidirectional laminated parallelepiped samples are impacted along their fiber direction. Their high velocity compressive ductility is observed. Both [0°]₂₄ and [(0°/90°)₆]_S glass/epoxy circular specimens with disc diameters of 10 and 50·8 mm are transversely impacted by an input bar in order to study their high strain rate behavior. Moreover, two sets of stitched circular specimens with disc diameters of 10 and 50·8 mm are also examined. The effect of strain rate and radial constraint on the dynamic properties of stitched and unstitched GFRP laminated specimens and their associated damage patterns are described.     

复合材料开孔层板压缩渐进损伤试验

为研究碳纤维增强树脂基复合材料开孔层板在压缩加载过程中的损伤起始、演化方式和损伤特点,采用微距拍摄、逐级加载超声C扫描、X光扫描和扫描电子显微镜观测4种观测手段对国产CCF300/5228A[45/0/-45/90]4s、[452/02/-452/902]2s、[454/04/-454/904]s3种铺层方式的开孔层板进行了压缩试验研究。对压缩载荷作用下开孔层板的损伤起始和损伤演化进行了观察和对比。对试验中观测到的纤维微屈曲、纤维挤出、孔边开裂和分层扩展等现象之间的关系进行了分析和说明。试验结果表明:压缩载荷下45°和90°铺层相邻位置为层板易分层位置,含45°和90°铺层相邻位置的开孔层板渐进损伤过程较为明显:开孔层板在压缩载荷下较早出现损伤,损伤的起始和演化缓解了孔边应力集中,促使压缩应变能在孔边逐步释放,推迟开孔层板压缩破坏的发生,提高层板压缩承载能力。研究结果可为材料结构损伤容限设计提供依据。     

An investigation of graphite PEEK composite under compression with a centrally located circular discontinuity

The failure characteristic of graphite polyetheretherketone (Gr/PEEK) under compression with a centrally located circular discontinuity was investigated through experimentation and a nonlinear ply-by-ply finite element technique. The stacking sequence of the laminates investigated were: [0 °₁₆], [90 °₁₆], [±45 °]_4S [0 °/90 °]_4S, and [0 °/ ± 45 0°/90 °]_2S. In the experimentation, [90 °]₁₆, [0 °/90 °]_4S, and [0 °/ ±45 °/90 °]_2S laminates, as well as three of the [0 °]₁₆, failed due to a crack that was normal to the loading direction and initiated from the edge of the hole progressing to the outer edges of the specimen. The [±45 °]_4S specimens failed to support the load due to an internal crack that originated from the hole's edge and then traveled at an angle of about 42% to the direction of loading. The finite element method used to analytically model the failure of Gr/PEEK accurately modeled the response of the specimens tested experimentally.     

铺层方式对CFRP-Al单搭接接头胶接性能的影响

使用热压罐制备[45/-45]_4s、[0/90]_4s和[0/45/-45/90]_2s三种铺层方式的CFRP层合板,然后在室温下与Al胶接制备出单搭接试样。使用电子万能试验机、数字图像相关法(DIC)和扫描电子显微镜(SEM)等手段测量胶接接头的拉伸载荷-位移曲线和应变分布并观察断口形貌。基于试验数据分析不同铺层方式下CFRP-Al单搭接接头的拉伸性能,研究了铺层方式对CFRP-Al单搭接接头胶接性能的影响和铺层方式胶接接头的破坏机制。结果表明,在拉伸过程中[45/-45]_4s试样出现塑性变形阶段其拉伸位移最大,而[0/45/-45/90]_2s和[0/90]_4s试样的拉伸位移较小且发生了脆性断裂。铺层方式从[45/-45]_4s到[0/45/-45/90]_2s再到[0/90]_4s,试样的极限载荷和纤维束断裂数量增加、层间剪切力减小、应变集中程度和分层破坏程度降低。     

Fatigue damage mechanics of composite materials Part III: Prediction of post-fatigue strength

A damage-based model for post-fatigue notch strength is presented. The model is an extension of a method developed previously to predict the notch strength of laminated composites. A simple finite element representation of the notch tip damage zone is used to obtain the localized damage-modified stress distribution. A uniaxial tensile stress failure criterion is applied to the 0° plies from which the laminate strength is evaluated. In conjunction with the fatigue damage growth law described in Part II, residual strength is calculated as a function of the applied loading conditions, specimen geometry and lay-up for (90/0)_s, (90/0)_2s and (90₂/0₂)_s T300/914C carbon-fibre/epoxy laminates subjected to tension-tension fatigue cycling.     

聚酰亚胺树脂基MT300/KH420复合材料高温力学性能(Ⅱ)——弯曲性能

从宏、微观的角度研究了碳纤维增强聚酰亚胺树脂基MT300/KH420复合材料的高温力学性能,重点揭示了MT300/KH420复合材料[0°]14和[±45°/0°/90°/+45°/0°2]s层合板在常温~500℃的弯曲性能变化规律。研究表明:MT300/KH420复合材料高温力学性能优异,[0°]14层合板在420℃的弯曲强度保持在51%以上,弯曲模量在500℃以内变化很小。[0°]14层合板在常温下断口粗糙,且贯穿厚度,表现为脆性破坏;随温度升高,树脂流动性增强,呈现出黏弹效应,破坏逐渐集中在加载点处,在500℃,部分树脂热解,纤维束脱离基体并氧化。[±45°/0°/90°/+45°/0°2]s层合板高温弯曲性能较为稳定,主要破坏为上、下表面沿45°方向开裂,并伴有层间分离,在500℃出现严重分层破坏;相比于受基体控制的层合板弯曲性能,温度对受纤维控制的层合板弯曲性能影响较小。     

典型螺栓连接CFRP薄壁C型柱轴压失效行为:试验及数值模拟

为了研究典型螺栓连接碳纤维增强树脂复合材料(CFRP)薄壁C型柱的轴压失效模式及吸能特性,进行了5组不同铺层方式C型柱的准静态轴压试验,即[0/90]_4s、[±45]_4s、[±45/90₂/0₄]_s、[±45/90/0₂/90/0₂]_s、[90/±45/0]_2s,获得其失效形貌及载荷-位移曲线。采用Lavadèze单层壳单元模型、Puck-Yamada失效准则、层间胶粘单元及螺栓模型,建立C型柱层合壳模型进行轴压仿真,并与试验失效形貌、载荷-位移曲线及吸能特性评估指标进行对比分析。结果表明:0°、±45°、90°纤维可以显著影响C型柱轴压失效模式及吸能特性。在轴压载荷下,±45°纤维铺设C型柱发生局部屈曲失效模式,吸能特性差。±45°纤维铺设在外部,0°和90°纤维交替铺设在内部的C型柱,其轴压失效过程平稳,吸能特性好。与C型柱轴压试验结果相比,层合壳模型获得的整体变形和局部失效形貌吻合较好,载荷-位移曲线变化趋势和吸能特性评价指标基本一致。研究结果对CFRP薄壁C型柱吸能设计具有一定的指导意义。      

Determination of fracture energy and tensile cohesive strength in Mode I delamination of angle-ply laminated composites

The energy release rate in delamination of angle-ply laminated double cantilever composite beam specimens was calculated using the compliance equation, and interlaminar cohesive strengths were obtained. Instead of the traditional approach of a beam on an elastic foundation, a second-order shear-thickness deformation beam theory (SSTDBT) was considered. The equilibrium equations were obtained using the principle of minimum total potential energy and the system of ordinary differential equations were solved analytically. The problem was solved for [0°]₆ , [±30°]₅, and [±45°]₅ laminates with mid-plane delaminations and the results were verified using experimental evidence available in the literature.     

Interfacial debonding in laminated titanium matrix composites

The results of an experimental program in which multiaxial loads were applied to [0₄] and [±45]_s silicon carbide/titanium (SiC/Ti) tubes are reviewed showing that stress coupling, matrix viscoplasticity (including room temperature creep) and fiber/matrix interfacial damage all contribute to nonlinear response and permanent strains in titanium matrix composites (TMC). A micromechanical model that explicitly considers the aforementioned phenomena is presented herein. The model assumes a periodic microstructure and uses finite elements to analyze a representative volume element. The composite is assumed to be in a state of generalized plane strain making it possible to discretize only a generic transverse plane while still being able to apply three-dimensional loading through appropriate boundary conditions. The response of laminated composites is predicted by incorporating the micromechanical results into nonlinear lamination theory. Predictions are presented to show the influence of the model parameters on the effective composite response of unidirectional [0₄] and angle-ply [±45]_s TMC laminates.     

The relation between compressive strength of carbon/epoxy fabrics and micro-tow geometry with various bias angles

In this paper compressive tests of carbon/epoxy (plain weave, 3k) fabric composites were performed to investigate the relation between compressive strength and various bias angles and shear angles. Compressive properties such as chord modulus and maximum strength of the fabric composite materials are essential to analyze the drape behaviour and estimate the quality of the final products. Various specimens with different bias and shear angles which were fabricated by using autoclave de-gassing moulding process were prepared to estimate the strength and chord modulus with respect to the bias and shear angle variations. The stacking sequences of the compressive test specimens are [0]_10T, [15]_10T, [30]_10T and [45]_10T for bias specimens and [±37]_10T, [±32]_10T, [±28]_10T, [±22]_10T for sheared specimens. Micro-tow structures were observed to correlate the fabric compressive strength with crimp angle. Anti-buckling rig was involved to prevent specimens from buckling during the compressive tests. The compressive test was performed with 1.3 mm/min strain rates. Compressive test results were compared with calculation results. Facture modes which were classified in two different modes were analyzed using microscopic observation.     

Studies on drilling of glass/epoxy laminates using coated high-speed steel drills

Drilling studies were conducted on glass/epoxy composite laminates having two different lay-ups [(0/90)_4s and (0/±45/90)_2s]. Normal drills (2 flute with cone angle of 118°) made of high-speed steel (HSS), TiN-coated HSS, and TiC-coated HSS were used. Drilling parameters were optimized in terms of least thrust and torque. Parameters studied were thrust, torque, tool wear, form deviation, acoustic emission peak, and root mean square (RMS) of acoustic energy. It was observed that coated HSS drills perform little better than uncoated HSS for small number of holes, while their performance is inferior to uncoated HSS for larger number of holes. This is mainly due to peeling or chipping of the coating from base material (HSS). Also, the performance of TiN-coated HSS drill was observed to be better than TiC-coated HSS.     

Bearing strength of carbon epoxy laminates under static and dynamic loading

An experimental study has been carried out to investigate both the static and dynamic bearing strengths of a pinned-joint carbon epoxy composite plate with [0°/45°/−45°/90°]_S and [90°/45°/−45°/0°]_S stacking configurations. The static and dynamic experiments have been carried out according to the ASTM D953 standards and ASTM STP 749, respectively [ASTM D 953-D, Standard Test method for Bearing Strength of Plastics, ASTM Designation. 342; Joining of Composite Materials, ASTM STP 749, American Society for Testing and Materials (1981) 131]. The ratio of the edge distance to the pin diameter (E/D), and that of the width to the pin diameter (W/D) of the specimens were varied to obtain the static bearing strength and the S–N fatigue curve. The experiments show that the static bearing strengths reach their upper limit when E/D and W/D ratios are equal to or greater than 4 for both [0°/45°/−45°/90°]_S and [90°/45°/−45°/0°]_S stacking sequences. The fatigue strength, on the other hand, reduces by up to 65% as E/D and W/D ratios increase for both stacking configurations.     

Sintering of Fused Mullite Based Particulate Composites Containing Zirconia

2r0₂ and its modified versions containing MgO and Y₂0₃ were selected as particulate reinforcement in order to achieve better mechanical properties in fused mullite. Particulate composites containing up to 25 vol% Zr0₂ and its modifications were pressed to 65% relative density at 350 MPa followed by sintering at 1650°C and 1700°C for one hour. Studies were conducted on fracture toughness, transverse rupture strength, dielectric constant, microstructure, fractography and thermal shock resistance. Composites sintered at 1700°C were found superior in properties than those sintered at 1650°C.     

Ionic Conductivity and Mechanical Properties of Post-HIPed Cubic Zirconia/Alumina Composites

8 mol.% yttria-doped cubic zirconia (8Y-CSZ)/AI₂O₃ composites containing 0-30 vol.% Al₂O₃ particles were fabricated by sintering, followed by hot isostatic pressing (post-HIPing). All composites were densified to at least 99·5% of the theoretical density by post-HIPing. The bending strength of composites sintered at 1500°C in air was independent of A1₂O₃ content, but a significant improvement in the bending strength was achieved by the post-HIPing technique. The bending strength and the fracture toughness of the HIPed composites increased with increasing A1₂O₃ content. Ionic conductivity of the composites was evaluated and the total, lattice, and grain boundary conductivities slightly decreased with increasing A1₂O₃ content. The HIPed composites containing up to 20 vol.% A1₂0₃ appear to be suitable candidate materials as electrolyte for solid oxygen fuel cell.     

Low temperature metal oxide film deposition and reaction kinetics in supercritical carbon dioxide

An effective method is developed for low temperature metal oxide deposition through thermal decomposition of metal diketonates in supercritical carbon dioxide (scCO₂) solvent. The rates of Al(acac)₃ (Aluminum acetyl acetonate) and Ga(acac)₃ (Gallium acetyl acetonate) thermal decomposition in scCO₂ to form conformal Al₂O₃ and Ga₂O₃ thin films on planar surfaces were investigated. The thermal decomposition reaction of Al(acac)₃ and Ga(acac)₃ was found to be initialized at  150 °C and 160 °C respectively in scCO₂ solvent, compared to  250 °C and 360 °C in analogous vacuum-based processes. By measuring the temperature dependence of the growth rates of metal oxide thin films, the apparent activation energy for the thermal decomposition of Al(acac)₃ in scCO₂ is found to be 68 ± 6 kJ/mol, in comparison with 80–100 kJ/mol observed for the corresponding vacuum-based thermal decomposition reaction. The enhanced thermal decomposition rate in scCO₂ is ascribed to the high density solvent which effectively reduces the energy of the polar transition states in the reaction pathway. Preliminary results of thin film deposition of other metal oxides including ZrO_x, FeO_x, Co₂O₃, Cr₂O₃, HfO_x from thermal decomposition of metal diketonates or fluorinated diketonates in scCO₂ are also presented.     

Thermal and mechanical fatigue analysis of CFRP laminates

[0°/90°]_s and [±45°]_s CFRP laminated plates were analysed using a finite element formulation for their fatigue behaviour. A fatigue criterion which is based on the laminate interlaminar stresses and the basic lamina fatigue parameters was used. Thermal effects were included in the formulation. In particular, initial thermal stresses resulting from the curing of the laminate were also included in the analysis. The results showed that both laminates had predicted S-N behaviour similar to that from experiments of past investigators. Also, the fatigue behaviour for the [±45°]_s laminate between room temperature and the curing temperature were found to be the same. However, in the case of the [0°/90°]_s laminate the fatigue strength at high temperatures was found to be lower than that at low temperatures.     

Microstructure and creep properties of a cast intermetallic Ti–46Al–2W–0.5Si alloy for gas turbine applications

The microstructure and creep properties including minimum creep rate, time to 1% creep deformation and creep fracture time of a cast TiAl-based alloy with nominal chemical composition Ti–46Al–2W–0.5Si (at.%) were investigated. The creep specimens were prepared from investment-cast plate and two large turbine blades. Constant load creep tests were performed in air at applied stresses ranging from 150 to 400 MPa in the temperature range 973–1073 K. The microstructure of the specimens is characterised by optical, scanning and transmission electron microscopy before and after creep deformation. The minimum creep rate is found to depend strongly on the applied stress and temperature. The power law stress exponent of minimum creep rate is n = 7.3 and the apparent activation energy for creep is Q_a = 427 ± 14 kJ/mol. The initial microstructure of the creep specimen is unstable. The ₂(Ti₃Al)-phase transforms to γ(TiAl)-phase and needle-like B2-precipitates during long-term creep testing at all testing temperatures. At lower applied stresses, the creep specimens fail by the growth and coalescence of cavities and small cracks formed along the γ/₂ interfaces. At the highest applied stresses, the specimens fail by nucleation and propagation of cracks.     

Pyrolytic Trifluoromethylation of [76]-, [78]-, [84]-, and Aza[60]Fullerenes with Silver Trifluoroacetate; Evidence for Coordination of Fullerenes to Silver

Pyrolytic trifluoromethylation of [76], [78], [84], and aza[60]fullerenes with silver trifluoroacetate at 300°C results in extensive polyaddition of up to 18, 18, 20 and 20 CF₃ groups, respectively. In contrast to trifluoromethylation of [60]- and [70]fullerenes that give a full range of derivatives ranging upwards from C_n(CF₃)₂, [76]-, [78]-, and [84]-fullerenes only give C_n(CF₃)_6-18 derivatives, largely in the 10-12 CF₃ range; reaction with [76]fullerene is accompanied by formation of C₆₀(CF₃)₆ attributed to cage fragmentation. For aza[60]fullerene the hexa-addition level dominates, in contrast to its other reactions which give predominantly penta-addition products. All the compounds showed peaks at 1256±2 and 1180-1190 cm^-1, due to the CF₃ group, and peaks in this region are shown also by the soluble extract obtained on trifluoromethylation of nanotubes. As in trifluoromethylation of [60]- and [70]-fullerenes, the products obtained initially are involatile, attributed to formation os silver complexes; these are decomposed on subsequent solution in toluene. Mixed isomeric trifluoromethylated C₆₀F₈ derivatives viz. C₆₀F₇CF₃, C₆₀F₆(FG₃)₂, C₆₀F₅(CF₃)₃ and C₆₀F₄(CF₃)₄, and C₆₀F₄CF₃CF₂CF₃ (a C₆₀F₆ derivative) have been isolated from fluorination of [60]fullerene with MnF₃/K₂NilF₆ at 510°C.     

铺层顺序对复合材料薄壁圆管轴向压溃吸能特性的影响研究

采用仿真和试验相结合的方法探讨复合材料薄壁圆管在准静态轴向压缩载荷下的失效吸能特性和吸能机理。首先,建立复合材料薄壁圆管"层合壳"有限元模型,通过显式动力学方法求解其在准静态轴向载荷下的压溃失效力学行为。仿真与试验结果在圆管轴向压溃变形过程、初始峰值载荷、平均压溃载荷及比吸能等主要吸能参数上具有很好的一致性,验证了"层合壳"复合材料圆管有限元模型和建模方法的有效性。其次,采用解析模型与仿真分析方法分别对[0/90]_3s、[0/90/0₂/90₂]_s、[0₃/90₃]_s三种不同铺层顺序的复合材料圆管的屈曲载荷与吸能特性进行了对比,进一步分析了铺层顺序对圆管失效吸能特性的影响。研究表明,0°与90°铺层交替程度对复合材料圆管的吸能特性影响较大,保证纤维失效方式在结构宏观失效中占主导地位能够提高材料失效吸收能量。