Tensile Creep Behavior and Thermal Stability of Orthogonal Three-Dimensional Woven TyrannoTM ZMI Fiber/Silicon-Titanium-Carbon-Oxygen Matrix Composites

This article presents experimental results for tensile creep behavior of orthogonal three-dimensional woven Tyranno™ ZMI fiber/Si-Ti-C-O ceramic matrix composites at 1300°–1450°C in air. The composite contained Tyranno ZMI (56% silicon, 1% zirconium, 34% carbon, and 9% oxygen) fibers with a BN coating layer to improve interface properties, and it exhibited excellent tensile properties at elevated temperature in air. For creep stresses between 60 and 140 MPa, the creep rate decreased continuously with time, with no apparent steady-state regime observed at 1300°–1450°C. Under the test conditions, the microstructure of the Tyranno ZMI fiber and Si-Ti-C-O matrix was unstable, resulting in weight loss and SiC grain growth. As a result, the viscosity of the fiber and matrix increased, because increased viscosity caused a creep rate that continuously decreased, which made steady-state creep impossible under these conditions.     

Infiltration and Pyrolysis of Polytitanocarbosilane in an Si-Ti-C-O Fabric/Mullite Porous Composite

Incorporating Si-Ti-C-O fabric into a mullite matrix is expected to increase the fracture energy of mullite ceramics. The present paper describes the processing of an Si-Ti-C-O fabric/mullite/polytitanocarbosilane composite. A polytitanocarbosilane (a precursor of Si-Ti-C-O fiber)/xylene solution was infiltrated into a laminated porous mullite composite with 35–37 vol% fabric and thermally decomposed to an amorphous solid at 1000°C, in an argon atmosphere, to decrease the porosity and residual stress induced by the difference in thermal and mechanical properties between the Si-Ti-C-O fabric and the mullite. The decrease in porosity of the composite with pyrolysis of the precursor polymer was analyzed theoretically, and those results were used to control the effective experimental parameters. The infiltration/pyrolysis process was repeated eight times to produce a composite of 90.4% theoretical density. The composite exhibited significant pseudoductility, with a fracture energy of 11.4 kJ/m² and a flexural strength of 290 MPa.     

Failure Modes of a Unidirectional Ultra-High-Modulus Carbon-Fiber Carbon-Matrix Composite

The objective of this study was to observe the effects of various microstructural features on the in situ , room-temperature tensile fracture behavior of an ultra-high-modulus, unidirectional carbon/carbon (C/C) composite as a function of processing heat-treatment temperature (HTT) over the range of 1100° to 2750°C. An in situ SEM flexural stage was used to observe the interactions between the advancing crack tip and the microstructural features in the frontal process zone. Following the lowest HTT of 1100°C, failure is dominated by the well-bonded brittle matrix; a tortuous crack path in the E130 fibers appears to contribute to a relatively high utilization of fiber strength in spite of this brittle-matrix failure. Approximate calculations of the interfacial shear stress that might be generated by matrix shrinkage during pyrolysis of the polymer to carbon were compared to approximations of crack-tip interfacial shear stresses (IFSS) using the Cook-Gordon approach. The results suggest that the strong bonding in the 1100°C HTT composite cannot be accounted for by friction alone, and, therefore, chemical bonding or some type of fiber-matrix mechanical interlocking must be involved. Higher HTTs lead to progressive weakening of the fiber-matrix interface, and, with heat treatment to 2150°C, multiple matrix cracking (MMC) is observed. Using the crack-spacing model of Aveston, Cooper, and Kelly (ACK), an IFSS of 1 MPa is estimated for the MMC case. Attempts to calculate the matrix failure strain using the ACK formulation led to a large overprediction of the failure strain, although a number of the parameters used in the calculation are known only very approximately. Heat treatments to 2400° and 2750°C led to longitudinal intramatrix cohesive failure; at 2750°C, this damage is extensive and results in composites with strength utilizations approaching those of dry fiber bundles.     

Tensile Creep and Creep-Recovery Behavior of a SiC-Fiber─Si3N4-Matrix Composite

The tensile creep and creep-recovery behavior of a unidirectional SiC-fiber/Si₃N₄-matrix composite was investigated at 1200°C in air. A primary objective of the study was to determine how various sustained and cyclic creep loading histories would influence the creep rate, accumulated creep strain, and the amount of strain recovered upon specimen unloading. The key results obtained from the investigation can be summarized as follows: (1) A threshold stress of 60 MPa was identified, below which the creep rate of the composite was exceedingly low (∼10⁻¹² s⁻¹). (2) Periodic fiber fracture was identified as a fundamental damage mode for sustained tensile creep at stresses of 200 and 250 MPa. (3) Because of transient stress redistribution between the fibers and matrix, the creep life and failure mode at 250 MPa. were strongly influenced by the rate at which the initial creep stress was applied. (4) Very dramatic creep-strain recovery occurred during cyclic creep; for cyclic loading between stress limits of 200 and 2 MPa, 80% of the prior creep strain was recovered during 50-h-creep/ 50-h-unloading cycles and over 90% during 300-s-creep/ 300-s-unloading cycles. (5) Cyclic loading significantly lowered the duration of primary creep and overall creep-strain accumulation. The implications of the results for microstructural and component design are discussed.     

Tensile Creep and Creep-Strain Recovery Behavior of Silicon Carbide Fiber/Calcium Aluminosilicate Matrix Ceramic Composites

The tensile creep and creep strain recovery behavior of 0° and 0°/90° Nicalon-fiber/calcium aluminosilicate matrix composites was investigated at 1200°C in high-purity argon. For the 0° composite, the 100-h creep rate ranged from approximately 4.6 × 10⁻⁹ s⁻¹ at 60 MPa to 2.2 × 10⁻⁸ s⁻¹ at 200 MPa. At 60 MPa, the creep rate of the 0°/90° composite was approximately the same as that found for the 0° composite, even though the 0°/90° composite had only one-half the number of fibers in the loading direction. Upon unloading, the composites exhibited viscous strain recovery. For a loading history involving 100 h of creep at 60 MPa, followed by 100 h of recovery at 2 MPa, approximately 27% of the prior creep strain was recovered for the 0° composite and 49% for the 0°/90° composite. At low stresses (60 and 120 MPa), cavities formed in the matrix, but there was no significant fiber or matrix damage. For moderate stresses (200 MPa), periodic fiber rupture occurred. At high stresses (250 MPa), matrix fracture and rupture of the highly stressed bridging fibers limited the creep life to under 70 min.     

Oxidation-Induced Microstructural Change of Si-Ti-C-O Fibers

Two types of Si-Ti-C-O fibers STC(6HS) and STC(6H), with different C/Si molar ratios of 0.99 and 1.65, respectively, have been subjected to oxidation tests at high temperatures between 1000° and 1500°C. Both fibers showed different mass gain during the oxidation tests. In the unoxidized region, there was no change in the chemical composition. For STC(6HS), coarse ß-SiC grains were formed throughout the region, while the grain coarsening in STC(6H) was restricted to the vicinity of the film/fiber interface. In this paper, the influence of free carbon on the oxidation-induced microstructural change of Si-Ti-C-O fibers is discussed.     

Cyclic-Fatigue Behavior of SiC/SiC Composites at Room and High Temperatures

Tension-tension cyclic-fatigue tests of a two-dimensional-woven-SiC-fiber-SiC-matrix composite (SiC/SiC) prepared by chemical vapor infiltration (CVI) were conducted in air at room temperature and in argon at 1000°C. The cyclic-fatigue limit (10⁷ cycles) at room temperature was ∼160 MPa, which was ∼80% of the monotonic tensile strength of the composite. However, the fatigue limit at 1000°C was only 75 MPa, which was 30% of the tensile strength of the composite. No difference was observed in cyclic-fatigue life at room temperature and at 1000°C at stresses >180 MPa; however, cyclic-fatigue life decreased at 1000°C at stresses < 180 MPa. The fracture mode changed from fracture in 0° and 90° bundles at high stresses to fracture mainly in 0° bundles at low stresses. Fiber-pullout length at 1000°C was longer than that at room temperature, and, in cyclic fatigue, it was longer than that in monotonic tension. The decrease in the fatigue limit at 1000°C was concluded to be possibly attributed to creep of fibers and the reduction of the sliding resistance of the interface between the matrix and the fibers.     

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.     

2维C/SiC复合材料的拉伸损伤演变过程和微观结构特征

通过单向拉伸和分段式加载-卸载实验,研究了二维编织C/SiC复合材料的宏观力学特性和损伤的变化过程.用扫描电镜对样品进行微观结构分析,并监测了载荷作用下复合材料的声发射行为.结果表明:在拉伸应力低于50MPa时,复合材料的应力-应变为线弹性;随着应力的增加,材料模量减小,非弹性应变变大,复合材料的应力-应变行为表现为非线性直至断裂.复合材料的平均断裂强度和断裂应变分别为23426MPa和0.6%.拉伸破坏损伤表现为:基体开裂,横向纤维束开裂,界面层脱粘,纤维断裂,层间剥离和纤维束断裂.损伤累积后最终导致复合材料交叉编织节点处纤维束逐层断裂和拔出,形成斜口断裂和平口断裂.     

Multiple Cracking of Unidirectional and Cross-PlyCeramic Matrix Composites

This paper examines the multiple cracking behavior of unidirectional and cross-ply ceramic matrix composites. For unidirectional composites, a model of concentric cylinders with finite crack spacing and debonding length is introduced. Stresses in the fiber and matrix are found and then applied to predict the composite moduli. Using an energy balance method, critical stresses for matrix cracking initiation are predicted. Effects of interfacial shear stress, debonding length and bonding energy on the critical stress are studied. All the three composite systems examined show that the critical stress for the completely debonded case is lower than that for the perfectly bonded case. For cross-ply composites, an extensive study has been made for the transverse cracking in 90° plies and the matrix cracking in 0° plies. One transverse cracking and four matrix cracking modes are studied, and closed-form solutions of the critical stresses are obtained. The results indicate that the case of combined matrix and transverse crackings with associated fiber/matrix interfacial sliding in the 0° plies gives the lowest critical stress for matrix cracking. The theoretical predictions are compared with experimental data of SiC/CAS cross-ply composites; both results demonstrated that an increase in the transverse ply thickness reduces the critical stress for matrix cracking in the longitudinal plies. The effects of fiber volume fraction and fiber modulus on the critical stress have been quantified. Thermal residual stresses are included in the analysis.     

Micromechanical model of time-dependent damage and deformation behavior for an orthogonal 3D-woven SiC/SiC composite at elevated temperature in vacuum

This paper presents a micromechanical model to predict the time-dependent damage and deformation behavior of an orthogonal 3-D woven SiC fiber/BN interface/SiC matrix composite under constant tensile loading at elevated temperature in vacuum. In-situ observation under monotonic tensile loading at room temperature, load–unload tensile testing at 1200 °C in argon, and constant load tensile testing at 1200 °C in vacuum were conducted to investigate the effects of microscopic damage on deformation behavior. The experimentally obtained results led to production of a time-dependent nonlinear stress–strain response model for the orthogonal 3-D woven SiC/SiC. It was established using the linear viscoelastic model, micro-damage propagation model, and a shear-lag model. The predicted creep deformation was found to agree well with the experimentally obtained results.     

Thermal Cycling Damage Mechanisms of C/SiC Composites in Displacement Constraint and Oxidizing Atmosphere

A constraint stress of 62.5 MPa is created on a three-dimensional C/SiC composite specimen whose both ends are fixed when temperature is cycled between 900° and 1200°C. The cyclic stress results in a maximum damage strain of 0.06% within 50 cycles owing to coating and matrix cracking, fiber debonding, sliding, and breaking in the composite. This constrained specimen elongation also leads to a final compressive stress of 14 MPa on the composite through a decrease in the baseline constraint stress. Wet oxygen atmosphere at a high cyclic temperature, concomitant with stresses, can aggravate the damage situation by alternate oxidation between internal and external fibers in composites.     

Thermal Response and Oxidation of Tyranno™-Fiber-Reinforced Si-Ti-C-O Matrix Composites for a Thermal Protection System in High-Enthalpy Dissociated Air

The thermal response and oxidation of Tyranno™ Lox-M fiber-reinforced Si-Ti-C-O matrix composites in high-enthalpy dissociated air was investigated in an arc jet facility (an arc wind tunnel). The maximum surface temperature reached 1310–1670°C. Catalytic recombination of oxygen and nitrogen on the composite surface under dissociated air was not significant. Surface recession was insignificant below 1600°C surface temperatures and above 5 kPa of oxygen partial pressure at the stagnation point. Passive-to-active oxidation transition of the composite agreed with Balat's theory for monolithic silicon carbide. A glass sealant prevented active oxidation of the composite for short-time exposures.     

Shear Strength as a Function of Test Rate for SiCf/BSAS Ceramic Matrix Composite at Elevated Temperature

Both interlaminar and in-plane shear strengths of a unidirectional Hi-Nicalon™-fiber-reinforced barium strontium aluminosilicate (SiC_f/BSAS) composite were determined at 1100°C in air as a function of test rate using double-notch shear test specimens. The composite exhibited a significant effect of test rate on shear strength, regardless of orientation. The shear strength degraded by about 50% as the test rate decreased from 3.3 × 10⁻¹ to 3.3 × 10⁻⁵ mm/s. The rate dependency of shear strength was similar to that observed for ultimate tensile strength at 1100°C for the two-dimensional (2-D) SiC_f/BSAS composite, in which tensile strength decreased by about 60% when the test rate varied from 5 to 0.005 MPa/s. A phenomenological, power-law slow crack growth model is proposed and formulated to account for the rate dependency of shear strength of the composite. The proposed model has been validated with additional results of both constant stress-rate and constant stress testing in shear at 1100°C using a 2-D Nicalon-fiber-reinforced crossply magnesium aluminosilicate (SiC_f/MAS-5) ceramic matrix composite.     

Mechanical Properties of Two Plain-Woven Chemical Vapor Infiltrated Silicon Carbide-Matrix Composites

The elastic and inelastic properties of a chemical vapor infiltrated (CVI) SiC matrix reinforced with either plain-woven carbon fibers (C/SiC) or SiC fibers (SiC/SiC) have been investigated. It has been investigated whether the mechanics of a plain weave can be described using the theory of a cross-ply laminate, because it enables a simple mechanics approach to the nonlinear mechanical behavior. The influences of interphase, fiber anisotropy, and porosity are included. The approach results in a reduction of the composite system to a fiber/matrix system with an interface. The tensile behavior is described by five damage stages. C/SiC can be modeled using one damage stage and a constant damage parameter. The tensile behavior of SiC/SiC undergoes four damage stages. Stiffness reduction due to transverse cracks in the transverse bundles is very different from cross-ply behavior. Compressive failure is initiated by interlaminar cracks between the fiber bundles. The crack path is dictated by the bundle waviness. For SiC/SiC, the compressive behavior is mostly linear to failure. C/SiC exhibits initial nonlinear behavior because of residual crack openings. Above the point where the cracks close, the compressive behavior is linear. Global compressive failure is characterized by a major crack oriented at a certain angle to the axial loading. In shear, the matrix cracks orientate in the principal tensile stress direction (i.e., 45° to the fiber direction) with very high crack densities before failure, but only SiC/SiC shows significant degradation in shear modulus. Hysteresis is observed during unloading/reloading sequences and increasing permanent strain.     

Damage development during flexural loading of a 5-directional braided C/C-SiC composite,characterized by X-ray tomography and digital volume correlation

In situ observations of damage development within 3-dimensional 5-directional braided carbon fiber reinforced carbon and silicon carbide (C/C-SiC) ceramic composites, fabricated by gaseous silicon infiltration (GSI) and precursor infiltration pyrolysis (PIP), have been obtained using laboratory X-ray computed tomography during in situ flexural tests. The GSI composite has a denser structure than that fabricated by PIP, but contains initial defects within the fiber bundles. The GSI composite ultimately failed due to fracture across the fiber bundles, while failure of the higher strength PIP composite propagated along the interface between the fiber bundle and matrix with a greater degree of fiber pullout. These differences arise from the higher process temperature and greater degree of matrix-fiber reaction of GSI compared to PIP. Digital volume correlation (DVC), applied to the tomographs, measured the 3-dimensional deformations and hence the specimen curvature. This demonstrated the significant reduction in elastic modulus caused by the development of internal cracking with tensile strain in both materials.     

Creep and Stress–Strain Behavior after Creep for SiC Fiber Reinforced, Melt-Infiltrated SiC Matrix Composites

Silicon carbide fiber (Hi-Nicalon Type S, Nippon Carbon) reinforced silicon carbide matrix composites containing melt-infiltrated silicon were subjected to creep at 1315°C at three different stress conditions. For the specimens that did not rupture after 100 h of tensile creep, fast-fracture experiments were performed immediately following the creep test at the creep temperature (1315°C) or after cooling to room temperature. All specimens demonstrated excellent creep resistance and compared well to the creep behavior published in the literature on similar composite systems. Tensile results on the after-creep specimens showed that the matrix cracking stress actually increased, which is attributed to stress redistribution between composite constituents during tensile creep.     

Preparation of SiC/SiC Composites by Hot Pressing, Using Tyranno-SA Fiber as Reinforcement

The development of advanced Tyranno SA SiC fiber with a near-stoichiometric composition and a well-crystallized microstructure has made it possible to prepare SiC/SiC composites even under harsh conditions. To assess the reinforcing effectiveness of Tyranno SA fiber at high temperature under pressure, unidirectional SiC/SiC composites were prepared by hot pressing, using pyrolytic carbon (PyC)-coated Tyranno SA fiber as a reinforcement and nanopowder SiC with sintering additives for matrix formation. The effects of sintering conditions on the microstructural evolution and mechanical properties of the composites were characterized. As the sintering temperature increased (from 1720° to 1780°C) and the sintering pressure increased (from 15 to 20 MPa), the density of the composites gradually increased. Simultaneously, the elastic modulus, the proportional limit stress, and the strength, under both bend and tensile tests, also improved. At lower temperature and/or pressure, long fiber pullout was a predominant fracture behavior, indicating relatively weak fiber/matrix bonding. However, at high temperature and/or pressure, short fiber pullout became a main fracture characteristic, indicating relatively strong fiber/matrix bonding. These phenomena were also confirmed by the characteristics of the hysteresis loops derived from the stress–strain curves produced by a tensile test with unloading–reloading cycles. In the present investigation, the reinforcement of Tyranno SA fiber is effective for providing noncatastrophic fracture behavior to composites.     

Tensile and Fatigue Behavior of Silicon Carbide Fiber-Reinforced Aluminosilicate Glass

The onset of damage accumulation in ceramic-matrix composites occurs as matrix microcracking and fiber/matrix debonding. Tension tests were used to determine the stress and strain levels to first initiate microcracking in both unidirectional and cross-ply laminates of silicon carbide fiber-reinforced aluminosilicate glass. Tension–tension fatigue tests were then conducted at stress levels below and above the matrix cracking stress level. At stress levels below matrix microcracking, no loss in stiffness occurred. At stresses above matrix cracking, the elastic modulus of the unidirectional specimens exhibited a gradual decrease during the first 10 000 cycles, and then stabilized. However, the cross-ply material sustained most of the damage on the first loading cycle. It is shown that fatigue life can be related to nonlinear stress–strain behavior of the 0° plies, and that the cyclic strain limit was approximately 0.3%.     

Microstructure and tensile behavior of (BN/SiC)n coated SiC fibers and SiC/SiC minicomposites

Interphase plays an important role in the mechanical behavior of SiC/SiC ceramic-matrix composites (CMCs). In this paper, the microstructure and tensile behavior of multilayered (BN/SiC)_n coated SiC fiber and SiC/SiC minicomposites were investigated. The surface roughness of the original SiC fiber and SiC fiber deposited with multilayered (BN/SiC), (BN/SiC)₂, and (BN/SiC)₄ (BN/SiC)₈ interphase was analyzed through the scanning electronic microscope (SEM) and atomic force microscope (AFM) and X-ray diffraction (XRD) analysis. Monotonic tensile experiments were conducted for original SiC fiber, SiC fiber with different multilayered (BN/SiC)_n interfaces, and SiC/SiC minicomposites. Considering multiple damage mechanisms, e.g., matrix cracking, interface debonding, and fibers failure, a damage-based micromechanical constitutive model was developed to predict the tensile stress-strain response curves. Multiple damage parameters (e.g., matrix cracking stress, saturation matrix crack stress, tensile strength and failure strain, and composite’s tangent modulus) were used to characterize the tensile damage behavior in SiC/SiC minicomposites. Effects of multilayered interphase on the interface shear stress, fiber characteristic strength, tensile damage and fracture behavior, and strength distribution in SiC/SiC minicomposites were analyzed. The deposited multilayered (BN/SiC)_n interphase protected the SiC fiber and increased the interface shear stress, fiber characteristic strength, leading to the higher matrix cracking stress, saturation matrix cracking stress, tensile strength and fracture strain.