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.     

Influence of Interface Characteristics on the Mechanical Properties of Hi-Nicalon type-S or Tyranno-SA3 Fiber-Reinforced SiC/SiC Minicomposites

The tensile behavior of CVI SiC/SiC composites with Hi-Nicalon type-S (Hi-NicalonS) or Tyranno-SA3 (SA3) fibers was investigated using minicomposite test specimens. Minicomposites contain a single tow. The mechanical behavior was correlated with microstructural features including tow failure strength and interface characteristics. The Hi-NicalonS fiber-reinforced minicomposites exhibited a conventional damage-tolerant response, comparable to that observed on composites reinforced by untreated Nicalon or Hi-Nicalon fibers and possessing weak fiber/matrix interfaces. The SA3 fiber-reinforced minicomposites exhibited larger interfacial shear stresses and erratic behavior depending on the fiber PyC coating thickness. Differences in the mechanical behavior were related to differences in the fiber surface roughness.     

Properties of Multilayered Interphases in SiC/SiC Chemical-Vapor-Infiltrated Composites with "Weak" and "Strong" Interfaces

The interfacial properties of SiC/SiC composites with interphases that consist of (C-SiC) sequences deposited on the fibers have been determined by single-fiber push-out tests. The matrix has been reinforced with either as-received or treated Nicalon fibers. The measured interfacial properties are correlated with the fiber-coatingbond strength and the number of interlayers. For the composites reinforced with as-received (weakly bonded) fibers, interfacial characteristics are extracted from the nonlinear portion of the stress-displacement curve by fitting Hsueh's push-out model. The interfacial characteristics are controlled by the carbon layer adjacent to the fiber. The resistance to interface crack growth and fiber sliding increases as the number of (C-SiC) sequences increases. For the composites reinforced with treated (strongly bonded) fibers, the push-out curves exhibit an uncommon upward curvature, which reflects different modes of interphase cracking and a contribution of fiber roughness.     

Ultrasonic Characterization of Oxidation Mechanisms in Nicalon/C/SiC Composites

The nonbrittle fracture of composites consisting of ex polycarbosilane SiC (Nicalon) fibers in a SiC matrix prepared by chemical vapor infiltration is strongly dependent on the presence of a pyrocarbon layer at the fiber/matrix interface (Nicalon/C/SiC composites). The mechanical properties of such materials are known to be influenced by oxidation reactions. Elastic modulus measurements, using ultrasonic wave propagation in the "long bar" mode, have been used to show the influence of the environmental parameters temperature, atmosphere, and pressure on the mechanical behavior of bidirectional Nicalon/C/SiC. In situ , measurements of elastic modulus performed in parallel with thermogravimetric analysis allow examination of oxidation mechanisms which affect interfacial properties. Results showed the modulus to be affected by two interfacial oxidation mechanisms: (1) oxidation of pyrocarbon coating and (2) closure of the resulting interphase gap by silica formation.     

Effect of Carbon and Silicon Carbide/Carbon Interlayers on the Mechanical Behavior of Tyranno-SA-Fiber-Reinforced Silicon Carbide-Matrix Composites

Several CVI-SiC/SiC composites were fabricated and the mechanical properties were investigated using unloading–reloading tensile tests. The composites were reinforced with a new Tyranno-SA fiber (2-D, plain-woven). Various carbon and SiC/C layers were deposited as fiber/matrix interlayers by the isothermal CVI process. The Tyranno-SA/SiC composites exhibited high proportional limit stress (∼120 MPa) and relatively small strain-to-failure. The tensile stress/strain curves exhibited features corresponding to strong interfacial shear and sliding resistance, and indicated failures of all the composites before matrix-cracking saturation was achieved. Fiber/matrix debonding and relatively short fiber pullouts were observed on the fracture surfaces. The ultimate tensile strength displayed an increasing trend with increasing carbon layer thickness up to 100 nm. Further improvement of the mechanical properties of Tyranno-SA/SiC composites is expected with more suitable interlayer structures.     

Fatigue of three advanced SiC/SiC ceramic matrix composites at 1200°C in air and in steam

High‐temperature mechanical properties and tension‐tension fatigue behavior of three advanced SiC/SiC composites are discussed. The effects of steam on high‐temperature fatigue performance of the ceramic‐matrix composites are evaluated. The three composites consist of a SiC matrix reinforced with laminated, woven SiC (Hi‐Nicalon?) fibers. Composite 1 was processed by chemical vapor infiltration (CVI) of SiC into the Hi‐Nicalon? fiber preforms coated with boron nitride (BN) fiber coating. Composite 2 had an oxidation inhibited matrix consisting of alternating layers of silicon carbide and boron carbide and was also processed by CVI. Fiber preforms had pyrolytic carbon fiber coating with boron carbon overlay applied. Composite 3 had a melt‐infiltrated (MI) matrix consolidated by combining CVI‐SiC with SiC particulate slurry and molten silicon infiltration. Fiber preforms had a CVI BN fiber coating applied. Tensile stress‐strain behavior of the three composites was investigated and the tensile properties measured at 1200°C. Tension‐tension fatigue behavior was studied for fatigue stresses ranging from 80 to 160 MPa in air and from 60 to 140 MPa in steam. Fatigue run‐out was defined as 2 × 10⁵ cycles. Presence of steam significantly degraded the fatigue performance of the CVI SiC/SiC composite 1 and of the MI SiC/SiC composite 3, but had little influence on the fatigue performance of the SiC/SiC composite 2 with the oxidation inhibited matrix. The retained tensile properties of all specimens that achieved fatigue run‐out were characterized. Composite microstructure, as well as damage and failure mechanisms were investigated.     

Fabrication and Properties of Ceramic Composites with a Boron Nitride Matrix

Boron nitride (BN) matrix composites reinforced by a number of different ceramic fibers have been prepared using a low-viscosity, borazine oligomer which converts in very high yield to a stable BN matrix when heated to 1200°C. Fibers including Nicalon (SiC), FP (A1₂O₃), Sumica and Nextel 440 (Al₂O₃-SiO₂) were evaluated. The Nicalon/BN and Sumica/BN composites displayed good flexural strengths of 380 and 420 MPa, respectively, and modulus values in both cases of 80 GPa. On the other hand, FP/BN and Nextel/BN composites exhibited very brittle behavior. Nicalon fiber with a carbon coating as a buffer barrier improved the strength by 30%, with a large amount of fiber pullout from the BN matrix. In all cases except for Nicalon, the composites showed low dielectric constant and loss.     

Effective Fiber Properties to Incorporate Coating Thermoelastic Effects in Fiber/Matrix Composite Models

A method to incorporate the thermoelastic effects of fiber coatings into models of fiber/matrix composites was deter-mined. The coated fiber was replaced by an "effective" transversely isotropic fiber so that the properties of this effective fiber could be used in composite models. This ap-proach was used to determine the magnitude of errors re-sulting from neglect of the coatings in modeling fiber/matrix debonding and sliding and in reduction of data from real composites. The effects of carbon and BN coatings in the Nicalon/SiC system were found to be significant. It was found that significant errors could be expected from fitting models to experimental data if the compliance and coeffi-cient of thermal expansion of the coatings were ignored, even when the coatings were thin. Wide use of the approach required revision of composite models to allow inclusion of a transversely isotropic fiber. Such a revision was de-rived for a popular model of matrix cracking stress, and significant effects again were found to result from neglect of coatings.     

Elastic Properties of Laminated Calcium Aluminosilicate/Silicon Carbide Composites Determined by Resonant Ultrasound Spectroscopy

The elastic properties of unidirectional and 0°/90° crossply Nicalon-SiC-fiber-reinforced calcium aluminosilicate (CAS/SiC) ceramic-matrix composites have been measured using a resonant ultrasound spectroscopy (RUS) technique. This approach has allowed the nondestructive determination of the complete set of independent second-order elastic stiffness constants of these ceramic composites. These stiffness data have been used to obtain the orientation dependence of Young's modulus and the shear modulus. The results are in reasonably good agreement with the limited experimental data obtained from mechanical testing. The RUS measurements reveal that the unidirectional CAS/SiC composite is well modeled by transverse isotropic symmetry, indicating relatively isotropic fiber spacing in the transverse plane. The analysis indicates that the overall elastic anisotropy is also small for unidirectional and 0°/90° laminated CAS ceramic-matrix composites, a result that can be attributed to the relatively low modulus ratio of the Nicalon SiC fiber to the CAS matrix and to the moderate fiber volume fraction.     

三维碳化硅纤维增强碳化硅基复合材料的研究

采用结构为(PyC/SiC)n的多层复合模式的界面层,依次用化学气相渗透法和先驱体转化法相结合的增密工艺制备出三维Nicalon-SiCf/SiC陶瓷基复合材料.所研制的材料具有较高的强度,而且表现出优异的韧性和类金属材料非灾难性断裂特征.复合材料的主要性能指标为:体积密度2.42 g/cm3,弯曲强度530 MPa.     

碳化硅纤维热处理对单向碳化硅纤维增强磷酸铝基复合材料性能的影响

用不同条件热处理的碳化硅纤维制备了单向连续碳化硅纤维增强磷酸铝基复合材料.研究了碳化硅纤维热处理的温度、时间及热处理方法对制成的复合材料性能的影响.测试了复合材料的断裂强度,相对介电常数和介电损耗.通过扫描电镜分析复合材料的微观形貌,并使用电子探针对碳化硅纤维/磷酸铝基体界面进行了微区元素分析.结果表明:碳化硅纤维热处理降低了复合材料的介电常数和介电损耗;纤维/基体界面之间未发生任何化学反应.由于热处理使纤维/基体形成了强结合界面,大大降低了复合材料的力学性能.快速热处理方式直接降低纤维的自身强度.     

模压压力对SiC/SiC复合材料力学性能及力学行为的影响

采用热模压辅助聚合物先驱体浸渍裂解工艺制备了国产近化学计量比SiC纤维增强SiC陶瓷基复合材料,通过阿基米德排水法和SEM技术对SiC/SiC复合材料致密化过程进行表征,采用弯曲强度、拉伸强度和断裂韧性对SiC/SiC复合材料力学性能和力学行为进行评价。研究表明,热模压压力是影响材料结构和性能的重要因素,热模压在提升材料致密度的同时,亦造成纤维的损伤。随着热模压压力的增加,SiC/SiC复合材料力学性能先增加后降低。热模压压力适中时,致密度增加因素占优,材料力学性能较为优异;热模压压力较大时候,热模压操作对纤维性能的损伤因素逐渐凸显,基体致密化和纤维损伤两种作用机制相当。     

Mechanical Characterization of Si–C(O) Fiber/SiC (CVI) Matrix Composites witrTa BN–Interphase

The mechanical behavior of three CVT-processed 2D woven SiC/BN/SiC composite materials with different initial BN interphase thicknesses has been investigated by means of tensile and impact tests. The results have established the efficiency of a BN interphase in promoting a nonlinear/non–catastrophic tensile behavior and high impact resistance. The effect of the initial BN interphase thickness on the resulting mechanical behavior has also been demonstrated. Characterization of the fiber/matrix interfacial zones by AES and TEM has revealed the presence of a SiO₂/C double layer at the BN/fiber interface, which might result from a decomposition undergone by the Si–C(O) Nicalon fiber during processing. It has been suggested that the influence of the initial BN interphase thickness on the mechanical properties of the composites results from both changes occurring in the composition and morphology of the interfacial zones and modifications of the interfacial forces due to accommodation of the radial residual clamping stress.     

Consequence of Intermittent Exposure to Moisture and Salt Fog on the High-Temperature Fatigue Durability of Several Ceramic-Matrix Composites

Fatigue behavior of four ceramic-matrix composites (CMCs) was documented at 1000°C, and a fifth composite was documented at 1200°C. Additional fatigue specimens were cycled for set blocks of cycles, removed from the fatigue machine, and exposed in a cyclic corrosion tester for 24 h with a fog of deionized water and a fog of deionized water containing 0.05 wt% NaCl. BN-fiber-coated Nicalon™/SiNC and Nicalon/Al₂O₃ experienced a pronounced decrease in fatigue life (∼86%) with salt fog exposure. Nicalon/C experienced rapid loss of the SiC exterior seal coat and a 30% decrease in life with salt fog exposure. Nextel610/AS and Nextel720/Al₂O₃ demonstrated no loss in fatigue performance or retained strength with water or salt fog exposure. Changes to the constituents of Nicalon/SiNC were evaluated to determine if they influenced moisture sensitivity. BN fiber coatings, BN or BN/SiC, alternate matrix prepreg, and matrix filler type had no influence on improving moisture resistance. Direct exposure to moisture fog produced accelerated rates of degradation in the BN fiber coating and greatly decreased fatigue durability.     

Microstructural Stability of Nicalon at 1000deg;C in Air after Exposure to Salt (NaCl) Water

When either uncoated or BN-coated Nicalon fibers are exposed to water saturated with NaCl before being annealed in air at 1000^deg;C, accelerated degradation of the structure of the fiber occurs. The fiber surface oxidizes to tridymite instead of vitreous silica, and the crystallites of SiC in Nicalon begin to grow. These findings suggest that prior exposure to salt water may cause appreciable debit in the mechanical strength of Nicalon fibers with time at 1000^deg;C in air .     

Predicted Effects of Interfacial Roughness on the Behavior of Selected Ceramic Composites

Potential effects of interfacial roughness in ceramic composites were studied using a model that included the progressively increasing contribution of roughness with relative fiber/matrix displacement during debonding of the fiber/matrix interface. A parametric approach was used to study interfacial roughness in conjunction with other parameters such as the strength, radius, and volume fraction of the fiber. The progressive roughness contribution during initial fiber/matrix sliding caused a high effective coefficient of friction, as well as an increased clamping stress, which led to rapidly changing friction with increasing debond length. Calculated effects implied a potentially significant contribution to the behavior of real composite systems and the necessity for explicit consideration in the interpretation of experimental data to understand composite behavior correctly. In a tension test, the Poisson's contraction of the fiber may negate the effects of roughness, allowing an "effective constant shear stress" (tau) approximation. This was evaluated using a piecewise linear approximation to the progressive roughness model in an analysis of composite stress-strain behavior; for the Nicalon/SiC system, the effective tau value was lower than the values that would be obtained from fiber pushout tests and/or matrix crack spacings.     

Mechanical and three‐body abrasive wear behaviour of SiC filled glass‐epoxy composites

Fiber/filler reinforced polymer composites are known to possess high strength and attractive wear resistance in dry sliding conditions. How these composites perform in abrasive wear situations needs a proper understanding. Hence, in this research article the mechanical and three‐body abrasive wear behaviour of E‐glass fabric reinforced epoxy (G‐E) and silicon carbide filled E‐glass fabric reinforced epoxy (SiC‐G‐E) composites are investigated. The mechanical properties were evaluated using Universal testing machine. Three‐body abrasive wear tests are conducted using rubber wheel abrasion tester wherein two different loads and four varying abrading distances are employed. The results showed that the wear volume loss is increased with increase in abrading distance and the specific wear rate decreased with increase in abrading distance/load. However, the presence of SiC particulate fillers in the G‐E composites showed a promising trend. The worn surface features, when examined through scanning electron microscopy, show higher levels of broken glass fiber in G‐E system compared to SiC‐ filled G‐E composites. POLYM. COMPOS., 2008. © 2008 Society of Plastics Engineers     

Effect of a Boron Nitride Interphase That Debonds between the Interphase and the Matrix in SiC/SiC Composites

Typically, the debonding and sliding interface enabling fiber pullout for SiC-fiber-reinforced SiC-matrix composites with BN-based interphases occurs between the fiber and the interphase. Recently, composites have been fabricated where interface debonding and sliding occur between the BN interphase and the matrix. This results in two major improvements in mechanical properties. First, significantly higher failure strains were attained due to the lower interfacial shear strength with no loss in ultimate strength properties of the composites. Second, significantly longer stress-rupture times at higher stresses were observed in air at 815°3C. In addition, no loss in mechanical properties was observed for composites that did not possess a thin carbon layer between the fiber and the interphase when subjected to burner-rig exposure. Two primary factors were hypothesized for the occurrence of debonding and sliding between the BN interphase and the SiC matrix: a weaker interface at the BN/matrix interface than the fiber/BN interface and a residual tensile/shear stress-state at the BN/matrix interface of melt-infiltrated composites. Also, the occurrence of outside debonding was believed to occur during composite fabrication, i.e., on cooldown after molten silicon infiltration.     

Strength Distribution of Reinforcing Fibers in a Nicalon Fiber/Chemically Vapor Infiltrated Silicon Carbide Matrix Composite

The strength distribution of fibers within a two-dimensional laminate ceramic/ceramic composite consisting of an eight harness satin weave of Nicalon continuous fibers within a chemically vapor infiltrated SiC matrix was determined from analysis of the fracture mirrors of the fibers. Comparison of the fiber strengths and the Weibull moduli with those for Nicalon fibers prior to incorporation into composites suggests that possible fiber damage may occur either during the weaving or during another stage of the composite manufacture. Observations also indicate that it is the higher-strength fibers which experience the greatest extent of fiber pullout and thus make a larger contribution to the overall composite toughness than do the weaker fibers.     

Interface Properties in High-Strength Nicalon/C/SiC Composites, As Determined by Rough Surface Analysis of Fiber Push-Out Tests

Fiber push-out curves generated on high-strength, treated-fiber Nicalon/C/SiC composites indicate behavior that is distinctly different from other composites. These composites have been analyzed using a model that explicitly includes two sets of debond-crack-surface topographies that correspond to two stages of crack propagation. The model successfully duplicates the observed unusual push-out load-deflection behavior by adjusting interfacial toughness and topographical parameters to fit the experimental data. Although the topographical parameters of the debonding cracks are largely unconfirmed, the fitted values are consistent with observations and expectations. This analysis has determined interfacial fracture energies that are unusually high for composites with acceptable mechanical behavior but are consistent with measurements on bulk pyrocarbons. The analysis provides a unifying rationalization of the apparent inconsistencies in results reported for such materials.