Optimizing the fiber push-out method to evaluate interfacial failure in SiC/BN/SiC ceramic matrix composites

The investigation of several parameters during fiber push-out micromechanical tests on the interfacial shear strength (ISS) of the BN interphase in SiC_f/SiC ceramic matrix composites (CMC) was undertaken to optimize experimental work. The SiC_f/SiC composites—candidate materials for jet engine components—were manufactured with varying fiber types and interlayer thicknesses. Experimental parameters explored included analyzing the effect of sample thickness on the success rate of micromechanical tests, the effect of fiber local environment whether at tow-level (intra-tow variability in ISS) or CMC architecture-level (inter-tow variability), the effect of nanoindenter flat-punch tip size, and the effect of the interphase thickness itself. Over 1000 fiber push-outs were performed and analyzed in this work—with data presented as cumulative distribution functions to compare and contrast samples. It was found that the ISS measured was strongly and statistically influenced by the underlying fiber roughness (interphase adherence), as well as its local fiber environment (e.g., number of nearest neighbors) only if the thickness of the interphase itself surpassed a threshold of 200 nm. Finally for thinner interphases, limited value was added to the CMC as the ISS measured was high and there was no effect from any local environment.     

Inspection of geometry influence and fiber orientation to characteristic value for short fiber reinforced ceramic matrix composite under bending load

For use of short fiber reinforced ceramics the knowledge of the influence of coupon geometry on the failure mode and the determined resistance in bending tests is necessary. In contrast to the continuous fiber reinforced ceramic matrix composites (CMC), for short fiber reinforced CMC there are only few studies and no standard on consideration of size effects. In the present work, the influence of coupon geometry and test conditions on the average value and distribution of flexural strength has been investigated. Two short fiber CMCs with different fiber length were examined under four point bending load. Moreover, the relationship between fiber orientation in the loaded area, failure location and measured flexural strength was investigated through high resolution X-ray computer tomography (μCT) and SEM. The presented outputs will be proposed to a future standard for bending test of short fiber reinforced CMC materials with different fiber length.     

羧甲基纤维素取代均一性的研究

羧甲基纤维素(钠盐,以下简称CMC)是一种重要的水溶性聚电解质。本文在传统溶媒法的基础上,采用乙醇作溶剂的两段加碱法新工艺制备CMC。研究表明,在低浴比(乙醇/纤维素=2.5—3.0)条件下,采用新工艺制得取代度约0.9,粘度(2％水溶液)为900—1000mPa·s,具有较高取代均一性和良好性能的CMC。用酶水解的方法,通过还原值测定,对CMC的取代基沿分子链的分布进行了表征;并对CMC的一些性能进行了测定,同时对其热稳定性进行了研究。     

Hybrid effect on mechanical properties of M40‐T300 carbon fiber reinforced Bisphenol A Dicyanate ester composites

Interply and intraply hybrid composites based on Bisphenol A Dicyanate ester (BADCy), high strength carbon fibers T300, and high modulus carbon fibers M40 were prepared by monofilament dip‐winding and press molding technique. The tensile, flexural, interlaminar shear properties and SEM analysis of the hybrid composites with different fiber content and fiber arrangement were investigated. The results indicated that the mechanical properties of intraply hybrid composites were mainly determined by fiber volume contents. When the ratio of fiber volume content was close to 1:1, the intraply hybrid composites possessed lowest tensile and flexural strength. The mechanical properties of interply hybrid composite mainly depended on the fiber arrangement, instead of the fiber volume contents. The hybrid composites using T300 fiber layout as outside layer possessed high flexural strength and low flexural modulus, which was close to that of T300/BADCy composites. The hybrid composites ([(M40)_x/(T300)_y]_S) using M40 fiber layout as outside layer and T300 fibers in the mid‐plane had high flexural modulus and interlaminar shear strength. POLYM. COMPOS., 2010. © 2010 Society of Plastics Engineers     

Interaction of fiber matrix bonding in SiC/SiC ceramic matrix composites

Non-oxide ceramic matrix composites (CMC) based on SiC fibers with SiC matrix were fabricated by polymer infiltration and pyrolysis (PIP) and characterized regarding their microstructural features and their mechanical properties. The fiber preform was made using winding technology. During the winding process, the SiC fiber roving was impregnated by a slurry containing SiC powder and sintering additives (Y₂O_3, Al₂O₃ and SiO₂). This already helped to achieve a partial matrix formation during the preform fabrication. In this way, the number of PIP cycles to achieve composites with less than 10% open porosity could be reduced significantly. Additionally, damage-tolerant properties of the composites were obtained by an optimal design of the matrix properties although only uncoated fibers were used. Finally, composites with a strength level of about 500 MPa and a damage-tolerant fracture behavior with about 0.4% strain to failure were obtained.     

Effect of the preparation of cellulose pellets on the dispersion of cellulose fibers into polypropylene matrix during extrusion

Cellulose fibers are rarely used for the extrusion of composites because of the problems in feeding them into the extruder and in dispersing them properly. Pelletization made it possible to feed cellulose fibers into extruder, but it reduced dramatically the fiber length. The goal of this study was to optimize the pelletization process for extrusion applications. Bleached sulfite cellulose fibers were pelletized at different moisture contents and with the optional addition of carboxymethyl cellulose (CMC). The pellets were subsequently extruded with polypropylene matrix without compatibilizer. Fiber dispersion and fiber breakage during extrusion were investigated. Pre‐blending of polymer and fiber pellets and introduction of the fibers through a side extruder were compared. CMC acted as a processing aid during pelletization, resulting in lower fiber breakage but in compact and stiff pellets. Lower moisture content also increased the compactness of the pellets. The dispersability of the fibers during extrusion decreased with increased pellets' compactness. CMC created inter‐fiber bonds, decreasing further the fibers' dispersability. The fiber length in the composites was the same regardless of the pelletization parameters. Early introduction of the fibers improved fiber dispersion. Feeding through side extruder was more stable and more reliable than pre‐blending. © 2009 Wiley Periodicals, Inc. J Appl Polym Sci, 2010     

Fiber-reinforced ceramic matrix composites processed by a hybrid technique based on chemical vapor infiltration,slurry impregnation and spark plasma sintering

Fabrication of multidirectional continuous carbon and silicon carbide fiber reinforced ceramic matrix composites (CMC) by a new short time hybrid process was studied. This process is based, first, on the deposition of fiber interphase and coating by chemical vapor infiltration, next, on the introduction of silicon nitride powders into the fibrous preform by slurry impregnation and, finally, on the densification of the composite by liquid phase spark plasma sintering (LP-SPS). The homogeneous introduction of the ceramic charges into the multidirectional fiber preforms was realized by slurry impregnation from highly concentrated and well-dispersed aqueous colloid suspensions. The chemical degradation of the carbon fibers during the fabrication was prevented by adapting the sintering pressure cycle. The composites manufactured are dense. Microstructural analyses were conducted to explain the mechanical properties achieved. One main important result of this study is that LP-SPS can be used in some hybrid processes to densify fiber reinforced CMC.     

Mechanical characterization and fractography of glass fiber/polyamide (PA6) composites

The mechanical properties of the glass fiber reinforced Polyamide (PA6) composites made by prepreg tapes and commingled yarns were studied by in‐plane compression, short‐beam shear, and flexural tests. The composites were fabricated with different fiber volume contents (prepregs—47%, 55%, 60%, and commingled—48%, 48%, 49%, respectively) by using vacuum consolidation technique. To evaluate laminate quality in terms of fiber wet‐out at filament level, homogeneity of fiber/matrix distribution, and matrix/fiber bonding standard microscopic methods like optical microscopy and scanning electron microscopy (SEM) were used. Both commingled and prepreg glass fiber/PA6 composites (with V_f ∼ 48%) give mechanical properties such as compression strength (530–570 MPa), inter‐laminar shear strength (70–80 MPa), and transverse strength (80–90 MPa). By increasing small percentage in the fiber content show significant rise in compression strength, slight decrease in the ILSS and transverse strengths, whereas semipreg give very poor properties with the slight increase in fiber content. Overall comparison of mechanical properties indicates commingled glass fiber/PA6 composite shows much better performance compared with prepregs due to uniform distribution of fiber and matrix, better melt‐impregnation while processing, perfect alignment of glass fibers in the composite. This study proves again that the presence of voids and poor interface bonding between matrix/fiber leads to decrease in the mechanical properties. Fractographic characterization of post‐failure surfaces reveals information about the cause and sequence of failure. POLYM. COMPOS., 36:834–853, 2015. © 2014 Society of Plastics Engineers     

Interfacial properties and initial step of the water sorption in unidirectional unsaturated polyester/vegetable fiber composites

In this work the interfacial properties of polyester/vegetable fiber composites were analyzed by flexural testing. The compressive/tensile (σ) and shear (τ) stresses were determined for each composite in function of the span-to-depth ratio (λ). The general behavior of the composites was similar to that of composites reinforced with DuPont Kevlar fiber, i.e., a maximum σ stress value is obtained. Flexural test validity for determining the Young's and shear moduli, E₁₁ and G₁₂, was ascertained. The Young's modulus agreed with that expected from the rule of mixtures for the composites with lowest fiber content. Short beam tests were performed on the composites. The shear stress value was improved by means of the matrix modification. Moisture sorption experiments and dynamic mechanical analysis were also performed on the natural fiber composites in the first Fickian step. Water sorption at 50% RH and 90% RH can be satisfactorily described by using a diffusional model. Water diffusion on parallelepiped samples shows a positive deviation from the Fickian behavior. Fiber capillary flow occurs through the fiber and the debonded matrix/fiber interphase during the initial Fickian step.     

TEM thin foil preparation for ceramic composites with multilayered matrix

A method for preparing thin foils for transmission electron microscopy (TEM) has been developed in the field of ceramic matrix composites (CMC). These composites belong to the last generation. They are developed for high temperature applications in oxidative environment (1350 °C). They possess a self-healing capability. Their design is based on a multilayered matrix. A refinement of the regular ion-milling technique was necessary to thin the samples and to proceed to a full observation of the inner matrix of the composite by TEM. In a regular CMC, the matrix is homogeneous and thereafter it has not to be fully inspected from the fiber to the surface. This sampling technique unable to thin the complete sequence of the different layers in the vicinity of large pores where the ion-milling technique is known to be very difficult. High resolution TEM as well as electron energy loss spectroscopy can be managed anywhere in the core sequence of the matrix.     

CMC jackets for metallic pipes – A novel approach to prevent the creep deformation of thermo-mechanically loaded metals

Steel materials suffer extensive creep by the application at temperatures of about 700?°C and pressures about 350?bar in a power plant environment. The presented concept overwraps a steel pipe with a ceramic matrix composite (CMC) jacket in order to support the steel pipe and provide high temperature strength. Finite Element simulations show the influence of the wall thickness of CMC jacket and the coefficient of thermal expansion (CTE) on circumferential stresses within the hybrid metal ceramic pipe. Suitable fiber and matrix materials were studied, composites fabricated and mechanical properties determined. Finally, a prototype was designed in order to confirm the feasibility of the concept. The lifetime of a pure steel pipe was increased by more than four-fold by the additional CMC jacket.     

In-Plane Cracking Behavior and Ultimate Strength for 2D Woven and Braided Melt-Infiltrated SiC/SiC Composites Tensile Loaded in Off-Axis Fiber Directions

The tensile mechanical properties of ceramic matrix composites (CMC) in directions off the primary axes of the reinforcing fibers are important for the architectural design of CMC components that are subjected to multiaxial stress states. In this study, two-dimensional (2D)-woven melt-infiltrated (MI) SiC/SiC composite panels with balanced fiber content in the 0° and 90° directions were tensile loaded in-plane in the 0° direction and at 45° to this direction. In addition, a 2D triaxially braided MI SiC/SiC composite panel with a higher fiber content in the ±67° bias directions compared with the axial direction was tensile loaded perpendicular to the axial direction tows (i.e., 23° from the bias fibers). Stress–strain behavior, acoustic emission, and optical microscopy were used to quantify stress-dependent matrix cracking and ultimate strength in the panels. It was observed that both off-axis-loaded panels displayed higher composite onset stresses for through-thickness matrix cracking than the 2D-woven 0/90 panels loaded in the primary 0° direction. These improvements for off-axis cracking strength can in part be attributed to higher effective fiber fractions in the loading direction, which in turn reduces internal stresses on weak regions in the architecture, e.g., minicomposite tows oriented normal to the loading direction and/or critical flaws in the matrix for a given composite stress. Both off-axis-oriented panels also showed relatively good ultimate tensile strength when compared with other off-axis-oriented composites in the literature, both on an absolute strength basis as well as when normalized by the average fiber strength within the composites. Initial implications are discussed for constituent and architecture design to improve the directional cracking of SiC/SiC CMC components with MI matrices.     

炭纤维增强水泥复合材料的制备及力学性能研究

 本文采用羧甲基纤维素钠(Sodium Carbonxymethyl Cellulose， CMC)与硅微粉(Fine Silica Fumes， SF) 作为复合分散剂对PAN基炭纤维进行协同分散来制备炭纤维增强水泥复合材料(Carbon Fiber Reinforced Cement Composites， CFRCC)，研究了炭纤维用量、分散剂配比及水灰比对其强度的影响。试验结果表明，此法对纤维具 有良好的分散效果。经过对各个掺量进行优选发现，在炭纤维为水泥掺量的1%，CMC和SF的分别为0.05%和15%，水 灰比为0.30～0.32时效果最好，所得CFRCC 7d（7天）的抗折和抗压强度分别提高了31.22%和41.25%。     

酵母菌发泡PVAL/CMC多孔复合材料的制备

采用微生物发泡法,将酵母菌作为微生物发泡剂,结合循环冷冻–解冻法制备聚乙烯醇(PVAL)/羧甲基纤维素(CMC)多孔复合材料。通过单因素试验探讨了酵母菌与葡萄糖比例(Y/G)、发泡时间、发泡温度和CMC与PVAL比例(CMC/PVAL)对发泡效果的影响,采用L9(34)正交试验进一步优化了发泡条件,通过傅立叶变换红外光谱和扫描电子显微镜(SEM)表征了PVAL/CMC多孔复合材料的结构。结果表明,当Y/G比例为2.8/1、发泡温度为31℃、发泡时间为60 min、CMC/PVAL比例为0.7/1时,PVAL/CMC多孔复合材料发泡效果最佳,其中CMC/PVAL比例为主要影响因素,此外,Y/G比例对发泡效果的影响也较为显著。SEM照片显示,以酵母菌为发泡剂制备的PVAL/CMC多孔复合材料具有较高的孔隙率,大孔平均孔径在180μm左右,小孔平均孔径在15μm左右,呈现大孔套小孔的开孔结构。     

Laser-supported joining of SiC-fiber/SiCN ceramic matrix composites fabricated by precursor infiltration

SiC-fiber/SiCN ceramic matrix composites were manufactured by means of polymer infiltration and pyrolysis. The fiber preform was made by slurry infiltration and winding using a computer-controlled winding module. Multiple infiltration steps using a Si–C–N precursor were included to increase the density. The influence of the sintering conditions on the microstructure of the CMC was demonstrated.Pipe sections made of the CMC materials were joined using a laser-supported heating technology with an Y–Al–Si–O glass–ceramic filler. The thermal response of the CMC components was controlled by the anisotropic thermal conductivity. Fast heating by laser beam was achieved for elements rotating in the direction of the fiber winding. SEM micrographs of the joints showed the good wettability of the CMC by the glass–ceramic filler. Nearly defect-free joints were obtained using a nitrogen process atmosphere. The laser-supported technology was shown to be promising for the joining of CMC components.     

原位微纤增强复合材料的结构与性能

采用熔融挤出——热拉伸——牵引拉伸制备了HDPE/PA6原位成纤增强复合材料,通过SEM分析了分散相PA6含量对其在基体中的形态及分布的影响;讨论了两种加工方式条件下分散相PA6含量对复合材料拉伸性能和冲击韧性的影响以及加工方式对复合体系力学性能的影响。结果表明：在原位成纤增强复合材料中存在直径为2～5 μm的纤维,当HDPE/PA6质量比为85/15时,微纤直径约为3 μm,此时,与普通共混复合材料相比,原位成纤增强复合材料的拉伸强度提高了6.9%,拉伸模量提高了14.8%,冲击强度提高10.03%。     

Mechanical properties of glass/flax hybrid composites based on a novel modified soybean oil matrix material

In the Affordable Composites from Renewable Resources (ACRES) program at the University of Delaware, soybean oil and other plant triglycerides have been made amenable to polymerization using a broad range of chemical routes. The resultant polymers range in properties from soft rubbers to hard thermosets for composite applications. In this paper we present an investigation of the mechanical properties of glass/flax hybrid composites based on these thermoset matrix materials. Composites with different glass/flax ratios and different fiber arrangements were made using a modified soybean oil matrix material. The fiber arrangement was varied to make symmetric and unsymmetric composites. The latter were tested in different modes in flexural tests and drop weight impact tests. The mechanical properties of the composites were found to depend upon the glass/flax ratio and the arrangement of fibers in the composite. On proper selection of the arrangement of fibers in the composite, the glass fibers and flax fibers were found to act synergistically resulting in an improved flexural and impact performance. POLYM. COMPOS., 26:407–416, 2005. © 2005 Society of Plastics Engineers     

Effects of poly(dimethyl siloxane) on the water absorption and natural degradation of poly(lactic acid)/oil‐palm empty‐fruit‐bunch fiber biocomposites

Composites were fabricated with poly(lactic acid) and oil‐palm empty‐fruit‐bunch (EFB) fibers with extrusion; this was followed by an injection‐molding technique. Before compounding, the surface of the fiber was modified through ultrasound and poly(dimethyl siloxane) (PDMS). The influences of the ultrasound and PDMS on the water absorption and biodegradability of the composites were investigated. Additionally, the composites were buried under soil for 6 months, and their biodegradability was assessed through different characterization techniques, such as tensile testing and weight loss and diffussability measurement. The changes on the surface of the fibers due to treatment were examined by scanning electron microscopy analysis, and the influences on the biodegradability of the composites were observed. Functional group analysis and possible changes before and after degradation were also examined by a Fourier transform infrared spectrophotometric technique. The results analyses revealed that the treatment of fibers improved the density of the fibers and reduced the water uptake of the composites. The overall weight loss due to soil burial testing was found to be maximum for the untreated‐fiber‐based composites (6.8%), whereas the ultrasound‐ and silane‐treated composites showed the minimum value of weight loss (3.7%). The deterioration of the tensile strength due to degradation was found to be at a maximum for the untreated‐fiber‐based composite (27%), whereas the ultrasound‐ and silane‐treated‐fiber‐based composites showed a minimum value of 8%. © 2015 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2015 , 132, 42784.     

Organic–inorganic interface enhancement for boosting mechanical and tribological performances of carbon fiber reinforced composites

The limitation in the poor interface would severely affect the further development and application of carbon fiber reinforced composites (CFRP). Unique organic–inorganic hybrid architectures of MOF-5-NH₂ and carboxymethyl cellulose (CMC) were established on the fiber/matrix interphase for promoting mechanical and tribological performances of the composites. The existence of above interfacial reinforced structure was in favor of generating abundant micromechanical interaction sites for enhancing mechanical interlocking. Meanwhile, high-density chemical crosslinking networks played a positive role in elevating interfacial adhesion, further relieving stress concentration and hindering crack propagation. The tensile strength of CFRP-2, CFRP-3, CFRP-4, and CFRP-5 exhibited a significant rising of 27.18%, 30.64%, 27.75%, and 36.88%, respectively. The friction coefficient of MOF-5-NH₂/CMC modified sample increased from 0.0953 to 0.1219, while the drop in the wear rate of the composites achieved 68.51%. This work provides an effective method for achieving the structure–function integrated design of composite materials according to the organic–inorganic interface enhancement of MOF-5-NH₂/CMC.     

The effects of fiber orientation on failure behaviors of 2D C/SiC torque tube

Different failure behaviors were observed in the 2D C/SiC torque tubes which were fabricated by chemical vapor infiltration (CVI) with different fiber orientations (0°/90° and ±45°). CT test was implemented to characterize the density heterogeneity of the ceramic matrix composite (CMC) torque tubes. With the density value measured by Archimedes drainage method, FEM software was implemented to simulate the stress distribution of the ceramic matrix composite torque tubes and calculate the failure stress. Torsional tests were conducted using special attachments to a universal material test machine. Different torsional behaviors of CMC torque tubes with two different fiber orientations were presented in the stress-strain curves. The fracture morphologies were observed by SEM, and the predominant factors of failure were analyzed. CMC torque tubes with fiber orientation of ±45° have a higher torque capacity and modulus. In failure analysis, we found that ±45° fiber orientation CMC torque tubes have reasonable fracture morphologies.