SiC纤维增强Ti17合金复合材料轴向残余应力的拉曼光谱和X射线衍射法对比研究

准确测量和分析SiC纤维增强Ti合金复合材料(SiC_f/Ti)中残余应力状态对优化复合材料的成型工艺和理解其失效模式具有重要意义,但其残余应力的实验测量和分析仍是一个挑战.石墨C涂层作为SiC纤维与Ti17基体合金之间必需的扩散障涂层,承载了由纤维与基体之间热不匹配引入的残余应力.本文采用显微拉曼光谱法对比测量纤维表面C涂层在复合材料中和去掉基体无应力态下G峰的峰位,通过石墨C涂层应力态下峰位移动计算出SiCf/C/Ti17复合材料中SiC纤维受到～705.0 MPa的残余压应力.采用X射线衍射方法测量了不同方向上该复合材料中基体钛合金的晶面间距以获取其空间应变,根据三轴应力模型分析了复合材料中基体钛合金沿轴向方向的残余应力为～701.3 MPa的张应力,并通过线性弹性理论转化为SiC纤维的残余压应力为～759.4 MPa.两种测试方法都确定了SiC纤维在成型过程中受到残余压应力,且获得的应力值较为接近,都可以用于对SiC_f/Ti复合材料的残余应力测量.     

Fabrication of continuous fiber-reinforced thermoplastic composites with structural gradient from sheath-core type bicomponent fibers

Sheath-core type bicomponent fibers of polypropylene (PP) as a sheath component and thermotropic liquid crystalline polymer (TLCP) as a core component were prepared by the highspeed melt spinning process. Continuous fiber reinforced thermoplastic composites, in which TLCP acts as a reinforcing fiber and PP as a matrix polymer, were fabricated by the compression molding of these fibers. In the melt spinning, the attainable highest take-up velocity of TLCP was improved by co-processing with PP. Tensile modulus and strength of the TLCP component in the PP/TLCP bicomponent fibers increased with an increase in the take-up velocity. Comparison of wide-angle X-ray diffraction patterns of starting bicomponent fibers and fabricated composites indicated that the orientation relaxation of TLCP did not occur in the compression molding process. Accordingly, the tensile modulus and strength of the PP/TLCP composites were similar to those of the bicomponent fibers. Continuous fiber reinforced thermoplastic composites with various types of fiber content distributions were fabricated from the bicomponent fibers in which sheath-core composition was changed gradually in the spinning process. In the three-point bending test, the composites with two different types of symmetric structural gradients, one with higher TLCP fiber content near the surfaces than in the center and the other with higher TLCP content in the center than near the surfaces, exhibited different flexural moduli even though the overall TLCP contents were comparable. In the three-point bending test of a composite with asymmetric structural gradient, the yielding behavior and maximum flexural load varied depending on the direction of load application although the initial flexural moduli were similar.     

Temperature dependence of the stress transfer for thermal resistance polymer composites by X-ray diffraction

Temperature dependence of the stress transfer from the matrix resin to the incorporated fiber has been measured for poly(p-phenylene benzobisoxazole) (PBO) fiber/bismaleimide (BMI) resin composite by a novel X-ray diffraction method. At 120°C, stress transfer and tensile strength of the PBO/BMI composite are superior to that of the PBO/epoxy composite, due to the excellent thermal resistance and good mechanical property of BMI resins. The PBO/BMI composite possesses good adhesion and excellent mechanical properties at high temperature, which are suitable for thermal resistance applications.     

Short sisal fiber reinforced polypropylene composites: the role of interface modification on ultimate properties

Sisal fibers have been used for the reinforcement of polypropylene matrix. The compatibilization between the hydrophilic cellulose fiber and hydrophobic PP has been achieved through treatment of cellulose fibers with sodium hydroxide, isocyanates, maleic anhydride modified polypropylene (MAPP), benzyl chloride and by using permanganate. Various fiber treatments enhanced the tensile properties of the composites considerably, but to varying degrees. The SEM photomicrographs of fracture surfaces of the treated composites clearly indicated the extent of fiber–matrix interface adhesion, fiber pullout and fiber surface topography. Surface fibrillation is found to occur during alkali treatment which improves interfacial adhesion between the fiber and PP matrix. The grafting of the fibers by MAPP enhances the tensile strength of the resulting composite. It has been found that the urethane derivative of polypropylene glycol and cardanol treatments reduced the hydrophilic nature of sisal fiber and thereby enhanced the tensile properties of the sisal–PP composites, as evident from the SEM photomicrographs of the fracture surface. The IR spectrum of the urethane derivative of polypropylene glycol gave evidence for the existence of a urethane linkage. Benzoylation of the fiber improves the adhesion of the fiber to the PP matrix. The benzoylated fiber was analyzed by IR spectroscopy. Experimental results indicated a better compatibility between benzoylated fiber and PP. The observed enhancement in tensile properties of permanganate-treated composites at a low concentration is due to the permanganate-induced grafting of PP on to sisal fibers. Among the various treatments, MAPP treatment gave superior mechanical properties. Finally, experimental results of the mechanical properties of the composite have been compared with theoretical predictions.     

Analysis of residual stresses in ternary electroconductive composites

Residual stresses in ceramic particle electroconductive composites were investigated by Raman microprobe spectroscopy and X-ray diffraction. The composites were ternary electroconductive ceramics in the system AlN+SiC+(ZrB₂,MoSi₂). Due to the poor definition of the reinforcing phase peaks, only the matrix residual stress could be evaluated by Raman spectroscopy, whilst the residual stress in the reinforcing phase was calculated by the equilibrium conditions. These calculated values were compared with those experimentally obtained by X-ray diffraction. The agreement between Raman and X-ray results was quite satisfactory. The values of residual stress calculated by the composite theory were in good agreement with those measured by Raman and X-ray diffraction for the MoSi₂-containing composite. For the ZrB₂-containing composite, the value calculated by the composite theory falls between the values measured by Raman and X-ray diffraction. PACS 81.05.Je; 87.64.Je; 87.64.Bx     

The Effects of Morphological Properties of Henequen Fiber Irradiated by EB on the Mechanical and Thermal Properties of Henequen Fiber/PP Composites

The aim of this study was to investigate the effects of electron beam (EB) irradiation on the morphological properties, crystallinity and surface area of henequen fiber and on the mechanical and thermal properties of henequen fiber reinforced polypropylene (PP) composites. The structure of henequen fiber was characterized by X-ray diffraction, mercury porosimetry and BET surface area analysis. The EB irradiation of 10 kGy led to the increasing of crystalline and surface pore area of henequen fiber, which contributed to the number of interlocking places with PP. From the results of tensile and impact strength tests, the highest value was observed for the composite reinforced with the henequen fiber treated with EB dose of 10 kGy, decreasing overall as EB dose increased. This tendency was also shown by coefficient of thermal expansion (CTE) measurements, but the value of CTE decreased until 50 kGy, meaning that a large total surface area can provide many interlocking places and so improve adhesion between fiber and matrix. Therefore, it can be concluded that the optimum pore surface area by 10 kGy irradiation contributes to successful mechanical interlocking between fiber and matrix and consequently enhances the mechanical and thermal properties of the composites.     

Interfacial interaction in carbon fiber/thermoplastic composites

This work was undertaken in order to increase the understanding of the mechanism responsible for fiber/matrix interaction in carbon fiber/thermoplastic composite. From results of previous study on carbon fiber/PEEK composite, which suggested that the formation of the fiber/ matrix interaction was primarily related to a chemisorption mechanism, a study was done of the conditions required to obtain efficient fiber/matrix interaction in PA-12 and PP/carbon fiber composites. The interest in studying carbon fiber composite based on PP and PA-12 was that these two matrices are very different in terms of reactivity, polyamide having many more reactive groups than polypropylene. As expected, due to the non-reactive chemical structure of the polypropylene, fiber/matrix interaction in carbon fiber/PP composite occurred only when the matrix was thermally degraded, i.e. when the composite was molded at high temperature or under long residence time at the melt temperature. For the carbon fiber/PA-12 composite, strong fiber/matrix interaction occurred readily at relatively low molding temperature, i.e. well before thermal degradation of the matrix. It was also found that the short beam shear strength in these composites seems to evolve with molding temperature, and a maximum interfacial strength was observed at a molding temperature corresponding to the thermal degradation of the matrix. This indicates that although matrix degradation often results in strong reduction in the composite performance, some matrix degradation can be beneficial in terms of interfacial mechanical properties. Finally, this work demonstrated that while the formation of fiber/matrix interaction seems to be primarily related to a chemisorption mechanism, the contribution of interphase crystallinity to the interfacial strength is not negligible. In fact, interfacial crystallinity was found to be essential to ensure optimum interfacial strength.     

Effects of residual stress and interfacial frictional shear stress on interfacial debonding at notch-tip in two-dimensional unidirectional composite

A calculation method based on the shear lag approach was presented to get an approximate estimate of influences of residual stresses and frictional shear stress at the debonded interface on the interfacial debonding behavior at the notch-tip along fiber direction in two-dimensional unidirectional double-edge-notched composites. With this method, the energy release rate for initiation and growth of debonding as a function of composite stress were calculated for some examples. The calculation results showed in outline how much the tensile and compressive residual stresses in the matrix and fiber along fiber direction, respectively, act to hasten the initiation and growth of the debonding when the final cut element in the notch is matrix, while they act to retard them when the final cut element is fiber, and how much the frictional shear stress at the debonded interface reduces the growth rate of the debonding.     

New Insight into the Interfacial Enhancement of Polypropylene Glass Fiber Composites via a Compatibilizer: The Role of Injection Screw Temperature

Polypropylene (PP)glass fiber (GF) composites modified by maleic anhydride-grafted polypropylene (MAH-g-PP) were prepared and the thermal influence on the interfacial properties was characterized and discussed. The results showed that the migration of MAH-g-PP from the PP matrix onto the GF surface was a thermally activated process. To be more specific, with the increasing processing temperature, more MAH-g-PP migrated onto the interface region to bridge PP matrix and GF together and promote the interfacial interaction, resulting in more efficient applied load transfer to GF through the interface. Accordingly, the mechanical properties of PPGF composites were improved with increasing processing temperature. Moreover, based on the content of MAH-g-PP on the surface of the GF and the mobility of MAH-g-PP in the PPGF composites, a temperature-dependent mechanism for the enhanced interface was proposed. We suggest this study not only provides a guide to adjust processing parameters to prepare high-performance PPGF composite, but also would be applicable for other immiscible systems.     

Laser bending of AISI 304 steel sheets: Thermal stress analysis

Laser induced bending of steel sheet is carried out and thermal stress developed in the heated region is examined. Temperature and stress fields are predicted using the finite element model. The microstructural changes in the melted region are investigated through scanning electron microscope, energy dispersive spectroscopy and X-ray diffraction. The residual stress developed at the surface vicinity of the laser treated region is measured using the X-ray diffraction technique, which is then compared with its counterpart predicted from the simulations. It is found that the residual stress at the surface vicinity is compressive and the prediction of the residual stress agrees well with that obtained from the X-ray diffraction technique. In addition, surface temperature predictions are in good agreement with the thermocouple data. The laser treated region is free from major cracks and large cavities.     

Thermal and Structural Behaviors of Polypropylene Nanocomposites Reinforced with Single-Walled Carbon Nanotubes by Melt Processing Method

In this work, polypropylene (PP) matrix reinforced with several single-walled carbon nanotubes (SWNTs) concentrations were prepared by a melt-mixing method. The effect of SWNTs on the thermal degradation behavior of polypropylene was studied by thermal gravimetric analysis. The results revealed that adding the SWNTs into the PP can increase the decomposition temperature. The results obtained from differential scanning calorimetry showed that incorporating SWNTs reduced the crystallinity but increased the crystallization temperature of the PP. The mechanical measurements showed that the tensile modulus of the nanocomposite was greatly enhanced to 882 MPa, compared to 485 MPa for pristine PP. For wide-angle X-ray diffraction tests, two cooling methods were used. The addition of SWNTs to the polymer in slow-cooled samples resulted in partial crystallization in the γ -form, while SWNTs had no effect in water-cooled samples, the sample crystallizing in the α -form. Scanning electron microscopy observations on the fracture surface of the nanocomposites showed the dispersion of the SWNTs in the nanocomposites.     

Structure and Mechanical Properties of Melt Intercalated Po1lypropylene–Organomontmorillonite Nanocomposites

The preparation and properties of polymer nanocomposites, obtained by melt-compounding of polypropylene (PP) and organomontmorillonite (OMMT) modified by different alkyl ammonium salts, are described. A copolymer of maleic anhydride and PP was used as a compatibilizing additive. Nanocomposites with OMMT content of 1, 5 and 10 wt% were prepared and tested. The influence of OMMT content on the tensile stress–strain curves, elastic modulus, yield and tensile strength, and ultimate elongation of the nanocomposites is determined. The results of measuring the microhardness and impact strength of polymer nanocomposites are presented. Long-term creep tests were performed to predict the long-term deformation behavior of nanocomposites. The crystallinity of nanocomposites was analyzed by means of differential scanning calorimetry and optical microscopy, while the structural features were studied by X-ray diffraction and scanning electron microscopy methods.     

The Effects of Surface and Pore Characteristics of Natural Fiber on Interfacial Adhesion of Henequen Fiber/PP Biocomposites

The pore characteristics and morphological changes of henequen fiber after electron beam (EB) irradiation were studied, and their effects on interfacial adhesion between henequen fiber and polypropylene (PP) matrix of biocomposites were investigated. The surface morphologies of the fibers exposed to various EB irradiation doses were observed with an atomic force microscope (AFM). The porosity and pore distribution of fibers were characterized by mercury porosimetry and nonfreezing bound water (NFW) was measured by differential scanning calorimeter (DSC). Henequen fiber-reinforced polypropylene biocomposites were manufactured by the compression molding method and interlaminar shear strength (ILSS) was analyzed to examine the interfacial adhesion between henequen fiber and the PP matrix of the biocomposites. The AFM images indicated that pectin, waxy materials and impurities were removed from the surfaces of the henequen fibers during EB irradiation, resulting in changes of the surface morphology and characteristics of the fibers. When pectin, waxy compounds and impurities were removed, small pores of 1–0.01 μm were produced, and total surface area and porosity were increased. The increase in total surface area and porosity induced better adhesion between fiber and polymer which was confirmed by ILSS tests. However, the excessive creation of small pore size gives a negative effect on the tensile strength of henequen fiber. The best interfacial adhesion between henequen fiber and PP was obtained for the biocomposite reinforced with the henequen fiber treated with 10 kGy, which has the highest surface area and optimum pore diameter for interlocking between henequen fiber and polypropylene.     

Tensile performance of packaged optical fibers

The tensile testing of packaged optical fibers involves the measurement of elastic strains in the range 2-10%. Under these conditions slippage at the tensile grips can produce erroneous results when a nonextensometric method of measurement (e.g., in positive production testing) is used. Slippage of packaged silica fibers (polypropylene/silicone resin-coated silica fibers) observed when using standard pneumatic parallel-faced jaws has been eliminated by using 50-mm-diameter pulley grips with suitable clamps to hold the fiber ends. With this arrangement clean fiber failures are obtained within the gauge length. A correction factor has been estimated for the measured strain values by a theoretical analysis of the measured tension/extension curves for the composite polypropylene/silicone resin-coated fibers. Statistical data have also been obtained for polypropylene-(PP) coated lead silicate fibers and PP-coated “plastic clad” silica fibers. In the latter case, true failure had been obscured by the onset of fiber slippage within the PP jacket.     

Structural modifications of silicon-implanted GaAs induced by the athermal annealing technique

We have used high-resolution X-ray diffraction and Raman spectroscopy to investigate structural modifications inside and outside the focal region of Si-implanted GaAs samples that have been irradiated at high power by a focused short-pulse laser. Si atoms implanted into the GaAs matrix generate exciton-induced local lattice expansion, resulting in a satellite on the lower-angle side of the Bragg peak. After the laser pulse irradiation, surface features inside and outside the focal spot suggest the presence of Bernard convection cells, indicating that a rapid melting and re-crystallization has taken place. Moreover, the laser irradiation induces a compressive strain inside the focal spot, since the satellite appears on the higher-angle side of the Bragg peak. The stress maximizes at the center of the focal spot and extends far outside the irradiated area (approximately 2.5-mm away from the bulls eye), suggesting the propagation of a laser-induced mechanical wave. The maximum compressive stress inside the focal spot corresponds to 2.7 GPa. Raman spectra inside the focal spot resemble that of pristine GaAs, indicating that rapid melting has introduced significant heterogeneity, with zones of high and low Si concentration. X-ray measurements indicate that areas inside the focal spot and annealed areas outside of the focal spot contain overtones of a minor tetragonal distortion of the lattice, consistent with the observed relaxation of Raman selection rules when compared with the parent zinc-blende structure. PACS 61.72.Vv; 62.50.+p; 71.55.Eq; 79.20.Ds; 81.05.Ea     

Stress transfer efficiency in model composites under dynamic loading

The micromechanics of tension–tension fatigue loading in model single-fibre composite geometries is investigated in this paper. In an attempt to emulate the conditions encountered in full carbon fibre composites, the fibres were prestrained prior to the curing process to ensure that they were free of high residual compressive stresses as a result of resin shrinkage. The resulting specimens were grouped into two categories depending on the level of the initial fibre prestrain (case A low, case B high). The cyclic load is designed to be well below the endurance fatigue limit of the polymer matrix (∼0.6%), and to have a frequency low enough to avoid unwanted thermal post curing. Throughout the preparation procedure, as well as during fatigue loading, the fibre stress (strain) was constantly monitored by means of laser Raman spectroscopy. The fibre axial stress distributions at each fatigue step were converted to interfacial shear stress (ISS) distributions, from which important parameters such as the maximum ISS the system can accommodate, the transfer length for efficient stress built-up and the length required for the attainment of maximum ISS were obtained. The results showed that, up to 2×10⁶ loading cycles, the main parameters which affected the stress transfer efficiency at the interface were the fibre fracture process itself and the viscoelastic behaviour of the matrix material. Received: 7 November 2001 / Accepted: 22 March 2002 / Published online: 5 July 2002     

ZrO2薄膜残余应力实验研究

采用ZYGO MarkⅢ-GPI数字波面干涉仪对电子束蒸发方法制备的ZrO2薄膜中的残余应力进行了研究,讨论了沉积温度、沉积速率等工艺参量对ZrO2薄膜残余应力的影响。实验结果表明：随着沉积温度及沉积速率的升高,ZrO2薄膜中残余应力状态由张应力变为压应力,且压应力值随着沉积温度升高而增大。同时用X射线衍射技术测量分析了不同沉积条件下ZrO2薄膜的微结构组织,探讨了ZrO2薄膜微结构与其应力的对应关系。     

The Preparation and Study on Ultrahigh Molecular Weight Polypropylene Gel‐spun Fibers

A novel polypropylene (PP) fiber was prepared by using gel spinning/crystallization from dilute solutions of ultrahigh molecular weight isotactic polypropylene (i‐UHMWPP), and subsequently drawing at various temperatures. The influence of drawing temperature on the properties of the resulted fibers was investigated. We found that the draw‐ability and mechanical as well as crystallization properties of the fibers obtained were dramatically improved with increasing drawing temperature. When the drawing temperature is below the α‐crystal relaxation temperature of PP, which was measured by wide‐angle X‐ray diffraction (WAXD) analysis as 100–120°C, the fibers are characterized by lower crystallinity and smaller crystals with less perfection, resulting in brittle fracture and subsequently poor mechanical durability. With drawing at temperatures above the α‐crystal relaxation temperature of PP, a novel UHMWPP fiber with Young's modulus of 27 GPa and tensile strength of 1.3 GPa was obtained. Higher crystallinity and larger crystals with better perfection and orientation were observed in this fiber.     

Effect of Compatibilizer Content on the Shear and Extensional Rheology of Polypropylene/Clay Nanocomposites

The shear and extensional rheology of polypropylene (PP)/organoclay nanocomposites in the presence of various maleic anhydride grafted polypropylene (PP-g-MA) compatibilizer concentrations were investigated. The PP nanocomposites were prepared via direct melt intercalation in an internal mixer. The structures of the nanocomposites were characterized by X-ray diffraction (XRD) and scanning electron microscopy. It was found that both the compatibilized and uncompatibilized nanocomposites could form an intercalated structure. However, the organoclay particles can disperse well only in the compatibilized systems. The linear viscoelastic properties, including the storage modulus G′ and complex viscosity η* were very sensitive to the microstructure of the nanocomposites. The extensional viscosities of PP nanocomposites were enhanced under a low deformation rate with increasing compatibilizer content and displayed a lack of superposition for different strain rates. It was proposed that the lack of superposition might originate from the formation of a three-dimensional organoclay network, which decreased in its complexity and strength as the deformation rate increased.     

Modification of nano-kenaf surface with maleic anhydride grafted polypropylene upon improved mechanical properties of polypropylene composite

The surface of nano-kenaf fiber is modified with maleic anhydride grafted polypropylene (MA-g-PP) and added into PP and the mechanical properties and the flow property of the composite are investigated. The addition of MA-g-PP in nano-kenaf/PP composite increases the tensile strength, the elongation%, and the impact strength (I.S.), while it decreases the flow property (melt flow index) compared to without MA-g-PP composite (nano-kenaf/PP). The scanning electron microscope photograph shows it also increases interfacial adhesion between nano-kenaf and PP matrix. Regardless of MA-g-PP, nano-kenaf fibers shows better adhesion with PP compared to micron-kenaf fibers. Addition of MA-g-PP further improved interfacial adhesion between nano-kenaf surface and PP matrix compared to without MA-g-PP nano-kenaf compound. The addition of MA-g-PP apparently improves the interfacial adhesion between nano-kenaf surface and PP by formation of 3-dimensional network structure.