Fugitive Interfacial Carbon Coatings for Oxide/Oxide Composites

The effectiveness of fugitive interfacial carbon coatings in Nextel™ 720-based composites was investigated. Dense (>90%) matrix (calcium aluminosilicate, 0° and ±45°) composites and porous matrix (mullite/alumina, eight-harness satin fabric) composites were fabricated and tensile tested in two control conditions (uncoated or carbon-coated) and with the carbon removed (fugitive interface). Results indicated that carbon removal in dense matrix composites did not significantly change unidirectional composite strength, even after long-term exposure at 1000°C. For porous matrix composites, composite strength was independent of the fiber/matrix interface, even after exposure at 1150°C for 500 h in air.     

Toughened Oxide Composites Based on Porous Alumina-Platelet Interphases

A novel mechanism for debonding at a weak interphase in an all-oxide composite is introduced. This methodology involves the use of alumina platelets that have a diameter of 10–15 or 5–10 μm and a thickness of 1 μm. The platelets induce constrained sintering of the ceramic powder, which results in permanent porosity. For room-temperature properties, only minor additions (0–3 vol%) of matrix powder yield sufficiently weak debonding interphases. The platelets lie in random, three-dimensional orientations and provide a debonding mechanism that is independent of temperature, in chemically compatible matrixes. Laminated composites with two types of matrixes—mullite and alumina—have been fabricated with modified fibrous monoliths of alumina in a triple-layer "core/interphase/matrix" arrangement. In the laminated systems, the intimate mixing of strong versus tough microstructures has been tailored by alternating various matrix:interphase thickness ratios. Preliminary load–displacement curves clearly demonstrate characteristics of "graceful failure" and notable improvements in the work of fracture. Scanning electron microscopic observation of the crack paths confirms the viability of platelets for producing permanently porous, debondable interphases at elevated temperatures in air.     

Interfacial Characterization of Silicon Carbide Fiber/Lithia-Alumina-Silica Glass Matrix Composites

The development of the carbon-rich interphase in Nicalon SiC fiber/Li₂O-Al₂O₃–SiO₂ glass matrix composites was examined as a function of processing parameters with the use of high-resolution scanning electron microscopy and Auger electron spetroscopy. Specifically, hot-pressing temperatures (1000°, 1100°, and 1200°C) and times (15, 30, 60, and 240 min) were systematically varied in such a manner so as to fabricate dense composites suitable for evaluation of reaction kinetics. Carbon-rich interphase thickness, which ranged from 1400 to 5400 Å (140 to 540 nm), was observed to increase with either increasing times at constant temperature or increasing temperatures at constant time. The kinetics of formation of the carbon-rich interphase followed a diffusion-controlled model, with an activation energy of 25.4 kcal/mol.     

粗糙度对碳纤维/聚芳基乙炔复合材料界面性能的影响

采用二氧化碳超临界(scCO2)处理碳纤维(CF)表面的方法,研究了粗糙度对碳纤维/聚芳基乙炔(PAA)树脂复合材料界面性能的影响.处理前后的碳纤维通过XPS,AFM和表面能测量进行了表征.CF/PAA复合材料的界面力学性能通过层间剪切强度测试(ILSS)与断口形貌分析进行了评价.结果表明,scCO2处理前后碳纤维表面的化学组成基本上没有变化.随着碳纤维表面粗糙度的增加,CF/PAA复合材料的界面力学性能先增加后减小.其中粗糙度范围为30～45 nm的样品有最高的ILSS值,43.36MPa,比未处理的样品提高了44%.对复合材料的ILSS提高起主要作用的因素是碳纤维与PAA树脂的界面齿合作用.而齿合作用程度的不同主要是由于不同粗糙度而引起的碳纤维表面物理状态的不同.     

Interfacial Sliding Friction in Silicon Carbide–Borosilicate Glass Composites: A Comparison of Pullout and Pushout Tests

Interfacial sliding friction stress (τ_f) was assessed using both pushout and pullout tests on SiC-borosilicate glass composite specimens. Single-filament composite specimens were fabricated by heating to 950°C in argon borosilicate glass rods with fine-diameter (250-μm) capillary in which SiC filaments were inserted. The composite specimens prepared in this manner showed only frictional bonding. The maximum frictional sliding loads for pushout and the initial frictional sliding loads in pullout were measured as functions of the embedded length of the filament in the glass rods. The nonlinear variations of the frictional loads were analyzed using shear-lag models that include corrections for the effects of Poisson expansion or contraction on the sliding friction stress. It is shown that under identical conditions of composite fabrication the two tests give nearly identical properties for the interfaces. Pushout tests on hotpressed bulk composite specimens, however, showed both chemical bonding and a higher sliding friction stress relative to the single-filament capillary specimens. The presence of compressive residual stress on the filaments was independently confirmed by evidence of stress-induced birefringence.     

Effectiveness of Monazite Coatings in Oxide/Oxide Composites after Long-Term Exposure at High Temperature

The effectiveness of monazite (LaPO₄) in providing an oxidation-resistant weak fiber/matrix interface was evaluated in a fiber roving/thin coating/ceramic-matrix composite with >20% fiber volume fraction. Nextel™ 610/monazite/alumina composites were fabricated and tensile tested after isothermal exposures of up to 1000 h. Some strength loss was seen after short-term exposures (1100°–1200°C/5–250 h); however, no further loss was observed after 1000 h at 1200°C. Conversely, control samples containing uncoated fiber displayed >70% strength losses after only 5 h at 1200°C. Fiber pullout was seen in monazite-containing samples even after 1000 h at 1200°C. Debonding was predominantly in the coating or at either the fiber/coating or coating/matrix interface. Push-out testing confirmed the weakness of the monazite coating interface.     

Influence of Residual Stresses, Interface Roughness, and Fiber Coatings on Interfacial Properties in Ceramic Composites

Fiber pushout tests are performed on zircon-matrix composites especially fabricated with a variety of silicon carbide reinforcing fibers and fiber coatings in order to create samples with different interfacial properties, surface roughness, and possibly in different states of residual stress to demonstrate their role on the interfacial and mechanical properties of fiber-reinforced composites. The data obtained from fiber pushout tests are analyzed using linear, shear-lag, and progressive debonding models to extract important interfacial properties, residual stresses, and surface roughness. The nature and magnitude of residual stresses in composites are independently characterized by measuring the coefficient of thermal expansion of the fiber, the matrix, and the composite for comparison with similar values measured using the fiber pushout tests. These results are then compared for self-consistency among different ways of analyzing data and with independently measured and calculated values. The results have shown that independent and complementary methods of data acquisition and analysis are required to fully understand interfacial properties in ceramic composites. In particular, independent measures of the coefficient of thermal expansion, residual stresses, and surface roughness are required to confidently interpret interfacial properties obtained by different analytical approaches and then relate them to the overall mechanical response of composites. It is also shown that composites with optimum mechanical response can be created by suitably engineering the interface using multiple fiber coatings.     

Interface Debonding and Fiber Cracking in Brittle Matrix Composites

Analyses of debonding along interfaces and of the kinking of interface cracks into a fiber have been used to define the role of debonding in fiber-reinforced, brittle matrix composites. The results reveal that, for fibers aligned with the tensile stress axis, debonding requires an interface fracture energy, Γ_i, less than about one-fourth that for the fiber, Γ_f. Further-more, once this condition is satisfied, it is shown that fiber failure does not normally occur by deflection of the debond through the fiber. Instead, fiber failure is governed by weakest-link statistics. The debonding of fibers inclined to the stress axis occurs more readily, such that debonds at acutely inclined fibers can deflect into the fiber, whereupon the failure of fibers is dominated by their toughness.     

氧化物纤维/氧化物陶瓷基复合材料研究概述

氧化物纤维，氧化物陶瓷基复合材料可以在高温氧化环境下长时间工作，是最有发展潜力的高温结构陶瓷材料之一。决定氧化物纤维，氧化物陶瓷基复合材料性能最主要的2个因素是氧化物纤维的性能和界面材料的组成与结构。笔者介绍了氧化物纤维和界面材料的发展，以及界面材料涂覆方法，并探讨了氧化物纤维，氧化物陶瓷基复合材料的发展趋势。     

Measurement of Fiber/Matrix Interfacial Shear Stress at Elevated Temperatures

An apparatus for measurement of the fiber/matrix interfacial shear stress at temperatures up to 1100° is described. Equipment was used to measure interfacial properties as a function of temperature in two ceramic-matrix composites and one metal-matrix composite. In the composites where the thermal expansion of the matrix was higher than that of the fiber, the interfacial shear stress decreased with temperature. The opposite trend was observed in a system with low matrix thermal expansion. The change of the interfacial shear stress with temperature of all the composites studied can be fully explained by considering the fiber/matrix expansion differences.     

Interfacial Bonding and Friction in Silicon Carbide [Filament]-Reinforced Ceramic- and Glass-Matrix Composites

Interfacial shear strength and interfacial sliding friction stress were assessed in unidirectional SiC-filament-reinforced reaction-bonded silicon nitride (RBSN) and borosilicate glass composites and 0/90 cross-ply reinforced borosilicate glass composite using a fiber pushout test technique. The interface debonding load and the maximum sliding friction load were measured for varying lengths of the embedded fibers by continuously monitoring the load during debonding and pushout of single fibers in finite-thickness specimens. The dependences of the debonding load and the maximum sliding friction load on the initial embedded lengths of the fibers were in agreement with nonlinear shear-lag models. An iterative regression procedure was used to evaluate the interfacial properties, shear debond strength (T _d ), and sliding friction stress (T _f ), from the embedded fiber length dependences of the debonding load and the maximum frictional sliding load, respectively. The shear-lag model and the analysis of sliding friction permit explicity evaluation of a coefficient of sliding friction (μ) and a residual compressive stress on the interface (σ₀). The cross-ply composite showed a significantly higher coefficient of interfacial friction as compared to the unidirectional composites.     

Porous Yttrium Aluminum Garnet Fiber Coatings for Oxide Composites

A porous oxide fiber coating was investigated for Nextel^™ 610 fibers in an alumina matrix. Polymeric-solution-derived yttrium aluminum garnet (YAG, Y₃Al₅O₁₂) with a fugitive carbon phase was used to develop the porous fiber coating. Ultimate tensile strengths of tows and minicomposites following heat treatments in argon and/or air were used to evaluate the effect of the porous fiber coating. The porous YAG fiber coatings did not reduce the strength of the tows when heated in argon, and they degraded tow strength by only ∼20% after heating in air at 1200°C for 100 h. Minicomposites containing porous YAG-coated fibers were nearly twice as strong as those containing uncoated fibers. However, after heating at 1200°C for 100 h, the porous YAG coatings densified to >90%, at which point they were ineffective at protecting the fibers, resulting in identical strengths for minicomposites with and without a fiber coating.     

Ceramic Composites with Multilayer Interface Coatings

Silicon carbide matrix composites have been fabricated from either ceramic-grade Nicalon^TM or Hi-Nicalon^TM fibers coated with an interface material consisting of six alternating carbon and silicon carbide layers. Initial efforts involved the use of chemical vapor infiltration to produce minicomposites (single tows of fibers). In subsequent work, forced-flow thermal-gradient chemical vapor infiltration was used to produce a single composite plate with a multilayer interface from ceramic-grade Nicalon fabric and two plates from Hi-Nicalon fabric, one with a single carbon layer and one with a multilayer interface. Tensile testing of the minicomposites and of specimens cut from the plates revealed typical composite behavior and strengths for the as-processed samples. Exposure of tensile specimens to 950°C air for 100 h resulted in large losses in strength and strain tolerance regardless of the interface coating. The results demonstrate that forced-flow thermal-gradient chemical vapor infiltration can be used to prepare multilayer interface material. The results also verified that relatively thick (>100 nm) single or multiple carbon layers are susceptible to oxidation that causes the loss of composite properties.     

Influence of Interfacial Shear Stress on First-Matrix Cracking Stress in Ceramic-Matrix Composites

The first-matrix cracking stress and fiber-matrix interfacial shear stress were measured in zircon-matrix composites uniaxially reinforced with either uncoated or BN-coated silicon carbide filaments to study the role of intentional changes in interfacial shear stress on first-matrix cracking stress. The first-matrix cracking stress was measured by mechanical tests performed in either tension or flexure, and the filament-matrix interfacial shear stress was measured by a fiber pushout test. The first-matrix cracking stress was independent of the measured interfacial shear stress and did not conform to the predictions of a number of energy-based micromechanics models. In contrast, the first-matrix cracking stress showed a good correlation with the first-matrix cracking strain, which is hypothesized to be a more realistic criterion for first-matrix cracking in this class of filament-reinforced ceramic-matrix composites.     

Crack Deflection in Composites with Very Thin Interlayers

Composites with very thin second-phase interlayers were made by painting zirconia tapes with a slurry that contained alumina and a fugitive polymer. Warm uniaxial pressing was used to produce microstructures that contained either straight or wavy interlayers. Through the use of the fugitive polymer and a carefully selected sintering temperature, porosity was introduced into the second phase. Samples that were tested in bending displayed high strengths (540–580 MPa), whereas examination of polished and fractured test bars revealed crack deflection at weak interlayers.     

Interfacial Mechanical Characterization of Nicalon SiC Fiber/Alumina-Based Composites

Interfacial mechanical properties of both Nicalon SiC/aluminum borate and Nicalon SiC/aluminum phosphate with various fiber coatings and heat treatments were evaluated using a commercially-available indenter to induce fiber sliding during load cycling experiments. Varying degrees of sliding due to different coating materials were found. The interfacial characteristics including the shear, the residual axial fiber, and debond stresses were estimated by matching the experimental stress-displacement curves with curves predicted from an existing model. The elastic modulus and hardness of the interphase/interface in ceramic matrix composites were also evaluated. These results provided important insights into the ultimate mechanical performance of fiber-reinforced ceramic-matrix composites.     

Interfacial Mechanical Characterization of Nicalon SiC Fiber/Alumina-Based Composites

Interfacial mechanical properties of both Nicalon SiC/aluminum borate and Nicalon SiC/aluminum phosphate with various fiber coatings and heat treatments were evaluated using a commercially-available indenter to induce fiber sliding during load cycling experiments. Varying degrees of sliding due to different coating materials were found. The interfacial characteristics including the shear, the residual axial fiber, and debond stresses were estimated by matching the experimental stress-displacement curves with curves predicted from an existing model. The elastic modulus and hardness of the interphase/interface in ceramic matrix composites were also evaluated. These results provided important insights into the ultimate mechanical performance of fiber-reinforced ceramic-matrix composites.     

Effect of the Fiber Size on the Physicochemical and Mechanical Properties of Composites of Epoxy and Date Palm Tree Fibers

Lignocellulosic fibers from date palm trees were employed to reinforce an epoxy matrix. Two fiber sizes were used, with the length and diameter in the range of 20–30 and 1.5–3 mm, respectively, for the so‐called long fibers, and in the range of 5–15 and 0.25–0.75 mm, respectively, for the so‐called short fibers. The morphologies of the resulting composites, as well as their thermal, mechanical, and water sorption properties were evaluated. Strong interactions between both components and etherification reactions may occur between the hydroxyl groups of the fibers and the epoxy groups of the epoxy‐amine reactive mixture. These effects are emphasized when decreasing the size of the fibers.

     

Characterization of Interfacial Properties in Fiber-Reinforced Cementitious Composites

For calculating interface properties from pullout tests, a simple theoretical model is proposed. The model enables calculating of the following material parameters: the parameter of shear stiffness of the fiber–matrix boundary layer, the shear bond strength, the frictional bond strength and the specific interfacial fracture energy. These parameters can be determined from the slope of the load-slip curve, the maximum pullout load and the corresponding slip value. Slip-controlled, multiple-fiber pullout tests were conducted in a closed-loop test system. The effects of embedment length of fibers on the model-predicted material parameters were examined. The model predictions were satisfactorily compared with some previously published test data.     

Effect of Interfacial Roughness on the Frictional Stress Measured Using Pushout Tests

A fiber which is partially pushed out of a surrounding matrix and subsequently pushed in the opposite direction exhibits a substantial decrease in sliding friction as it passes through its original position (its "origin"). This is manifest by a decrease in the load required to push the fiber. It is suggested that interfacial roughness causes this phenomenon and that the decrease in load (friction) is associated with the fiber seating back into its original position. The period of the drop has been correlated with the spatial extent of the interfacial surface roughness, and the magnitude of the drop (referred to hereafter as the seating drop) has been correlated with the amplitude of the interfacial roughness. Observation of the seating drop allows separation of the friction associated with interfacial irregularities from that resulting primarily from residual stresses at the interface. Implications for composite design and use are discussed. The effect of abrasion at the sliding interface is also addressed.