Tensile creep behavior of SiCf/SiC ceramic matrix minicomposites

Single fiber-tow minicomposites represent the major load-bearing element of woven and laminate ceramic matrix composites (CMCs). To understand the effects of fiber type, fiber content, and matrix cracking on tensile creep in SiC_f/SiC CMCs, single-tow SiC_f/SiC minicomposites with different fiber types and contents were investigated. The minicomposites studied contained either Hi-Nicalon™ or Hi-Nicalon™ Type S SiC fibers with a boron nitride (BN) interphase and a chemical-vapor-infiltrated-silicon-carbide (CVI-SiC) matrix. Tensile creep was performed at 1200 °C in air. A bottom-up creep modeling approach was applied where creep parameters of the fibers and matrix were obtained separately at 1200 °C. Next, a theoretical model based on the rule of mixtures was derived to model the fiber and matrix creep-time-dependent stress redistribution. Fiber and matrix creep parameters, load transfer model results, and numerical modeling were used to construct a creep strain model to predict creep damage evolution of minicomposites with different fiber types and contents.     

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.     

Tensile behavior of ceramic matrix minicomposites with engineered interphases fabricated by chemical vapor infiltration

Ceramic matrix composites (CMCs) exhibit quasi-ductile behavior beyond the initial elastic region driven by a weak fiber-matrix interface that can be further engineered by introducing a finite thickness interphaseleading to enhanced strength and toughness. The current work explores the engineering of interphases in CMCs by a controlled variation of fabrication process parameters. C/BN/SiC minicomposite configurations have been fabricated by chemical vapor infiltration (CVI) with the intent of varying interphase thickness and constituent volume fractions by varying the interphase and matrix infiltration durations. The effect of processing durations on the resulting microstructure, tensile response, and damage mechanisms up to and during ultimate failure of CMC minicomposites have been investigated. The presented results highlight the significant influence of processing duration on the tensile and failure behavior of CMC minicomposites thereby providing an insight into the processing-microstructure-tensile response relationship in CMCs.     

Boron Modified Phenol Formaldehyde Derived C<Subscript>f</Subscript>/SiBOC Composites with Improved Mechanical Strength for High Temperature Applications

Ceramic matrix composites (CMCs) are potential thermo-structural materials for use in space applications. Fiber/matrix (F/M) interface plays a key role in determining the mechanical properties of CMCs. Present study focuses on the optimization of F/M volume ratio and the influence of Pyrocarbon (PyC) interphase coating on the mechanical properties of CMCs derived from precursor route. CMCs are fabricated using phenol formaldehyde (PF) resin and boron modified PF (BPF) resin as precursor slurries, 2D carbon fabric (Toray, T300 3K, 8H, satin weave) as reinforcement and PyC as interphase. The deposition of PyC interphase was done by chemical vapor infiltration on the carbon fabric followed by densification of the matrix using reaction bonded silicon carbide method. In CMCs prepared from PF resin, without interphase the flexural strength improves from 25 ± 3.9 MPa (fiber content-40) to 63 ± 9.9 MPa (fiber content-60) on increasing the fiber vol%. In the second part of the investigation, the effect of PyC interphase was studied using CMCs prepared from BPF resin with fiber volume ratio of 60 %. The CMCs with PyC interphase shows an improvement in flexural strength (102 ± 11.5 MPa) compared to that of CMCs prepared without interphase (38 ± 4.4 MPa). The fractography of CMCs with and without interphase was closely evaluated under a scanning electron microscope. CMCs without interphase show no fiber pull-out, indicating the strong fiber-matrix bonding. While CMCs with interphase show fiber pull-out phenomenon and hence fails in a ductile manner.     

Effects of interface bonding properties on cyclic tensile behavior of unidirectional C/Si3N4 and SiC/Si3N4 composites

In this paper, the effect of fiber/matrix interface bonding properties on the cyclic loading/unloading tensile stress?strain hysteresis loops of 2 different ceramic‐matrix composites (CMCs), ie, C/Si₃N₄ and SiC/Si₃N₄, has been investigated using micromechanical approach. The relationships between the damage mechanisms (ie, matrix multicracking saturation, fiber/matrix interface debonding and fibers failure), hysteresis dissipated energy and internal frictional damage parameter have been established. The damage evolution processes under cyclic loading/unloading tensile of C/Si₃N₄ and SiC/Si₃N₄ composites corresponding to different fiber/matrix interface bonding properties have been analyzed through damage models and interface frictional damage parameter. For the C/Si₃N₄ composite with the weakest fiber/matrix interface bonding, the composite possesses the lowest tensile strength and the highest failure strain; the hysteresis dissipated energy increases at low peak stress, and the stress?strain hysteresis loops correspond to the interface partially and completely debonding. However, for the SiC/Si₃N₄ composite with weak interface bonding, the composite possesses the highest tensile strength and intermediate failure strain; and the hysteresis dissipated energy increases faster and approaches to a higher value than that of composite with the strong interface bonding.     

In-situ tensile damage and fracture behavior of PIP SiC/SiC minicomposites at room temperature

In-situ tensile damage and fracture behavior of original SiC fiber bundles, processed and uncoated SiC fiber bundles, SiC fiber bundle with PyC interphase, SiC/SiC minicomposites without/with PyC interphase are analyzed. Relationships between load-displacement curves, stress-strain curves, and micro damage mechanisms are established. A micromechanical approach is developed to predict the stress-strain curves of SiC/SiC minicomposites for different damage stages. Experimental tensile stress-strain curves of two different SiC fiber reinforced SiC matrix without/with interphase are predicted. Evolution of composite’s tangent modulus, interface debonding fraction, and broken fiber fraction with increasing applied stress is analyzed. For the BX™ and Cansas-3303™ SiC/SiC minicomposite with interphase, the composite’s tangent modulus decreased with applied stress especially approaching tensile fracture; the interface debonding fraction increased with applied stress, and the composite’s tensile fracture occurred with partial interface debonding; and the broken fiber fraction increased with applied stress, and most of fiber’s failure occurred approaching final tensile fracture.     

Modeling creep behavior in ceramic matrix composites

In this work, a three-dimensional viscoplasticity formulation with progressive damage is developed and used to investigate the complex time-dependent constituent load transfer and progressive damage behavior in ceramic matrix composites (CMCs) subjected to creep. The viscoplasticity formulation is based on Hill's orthotropic plastic potential, an associative flow rule, and the Norton-Bailey creep power law with Arrhenius temperature dependence. A fracture mechanics-informed isotropic matrix damage model is used to account for CMC brittle matrix damage initiation and propagation, in which two scalar damage variables capture the effects of matrix porosity as well as matrix property degradation due to matrix crack initiation and propagation. The Curtin progressive fiber damage model is utilized to simulate progressive fiber failure. The creep-damage formulation is subsequently implemented as a constitutive model in the generalized method of cells (GMC) micromechanics formulation to simulate time-dependent deformation and material damage under creep loading conditions. The developed framework is used to simulate creep of single fiber SiC/SiC microcomposites. Simulation results are in excellent agreement with experimental and numerical data available in the literature.     

Matrix cracking onset stress and strain as a function of temperature,and characterisation of damage modes in SiCf/SiC ceramic matrix composites via acoustic emission

The complex damage mechanisms that accumulate within SiC_f/SiC ceramic matrix composites (CMCs) subject to thermal and mechanical stress are being investigated in anticipation of the material’s introduction into high performance gas turbine engines. Acoustic emission (AE) is recognised as a leading non-destructive evaluation (NDE) tool to this end, and was used in this study to determine the so-called matrix cracking onset stress under tensile load as a function of temperature up to a maximum of 1100 °C. Onset stress was interpreted using three traditional measurements based on AE energy characteristics during monotonic tests to failure. Pattern recognition (PR) analysis was performed on the AE data, revealing a specific cluster of signals that correlated closely with the initial matrix cracking region of the stress-strain curve. Taken in isolation, the onset stress of this activity was significantly lower than the conventional value. PR results were investigated further, and isolated clusters were linked to damage modes anticipated at other specific regions of the stress history. A secondary series of experiments was performed on specimens representing the individual constituents of the CMC (single-phase SiC flexural bars, Hi-Nicalon? fibre bundles and SiC_f/SiC mini-composites) in attempts to further validate the corresponding AE signal characteristics. Matrix cracking and interphase debonding/sliding damage modes could be identified consistently, while fibre breaks remained difficult to isolate under the current experimental conditions.     

Enhanced microwave‐absorbing property of precursor infiltration and pyrolysis derived SiCf/SiC composites at X band: Role of carbon‐rich interphase

Ceramic matrix composites (CMCs) can be microwave‐absorbent when endowing the composite constituents with proper dielectric properties. In this work, we report a new method to enhance the microwave‐absorbing property of CMCs by in situ fabrication of a carbon‐rich interphase at the fiber/matrix interface. This was achieved in a SiC fiber reinforced SiC matrix (SiCf/SiC) composite fabricated by precursor infiltration and pyrolysis (PIP). We found that as the PIP temperature increased from 800 to 1000°C, the microwave‐absorbing property of the SiCf/SiC composite was significantly enhanced at X band, which also surpassed those of the SiC fiber and monolithic SiC ceramic fabricated at the same temperature. The dominant mechanism was studied by decoupling the effect of individual SiC fibers, SiC matrix, and fiber/matrix interface. The results showed that the SiC fiber and SiC matrix were barely microwave‐absorbent, due to their low dielectric losses. The microwave‐absorbing mechanism was finally ascribed to the fiber/matrix interface, which was carbon‐rich, containing Si and O elements. The interphase showed a conductivity that was superior to that of the fiber and the matrix, and mainly dominated the dielectric property of the overall composite. The results highlight the role of carbon‐rich interphase on the microwave‐absorbing property of CMCs.     

陶瓷基复合材料疲劳损伤模拟与界面优化设计

本文从界面损伤模拟出发研究了陶瓷基复合材料(CMCs)的抗疲劳设计方法.以CMCs微观结构演变为切入点,在微观尺度建立复合材料各组分损伤机制的物理模型,然后集成到细观尺度的有限元分析之中,从而建立CMCs疲劳损伤的数值模拟方法,并对界面相组成、结构等因素影响疲劳性能的作用机制进行探究,以实现界面的抗疲劳设计.通过多尺度...     

A synergistic model of stress and oxidation induced damage and failure in silicon carbide-based ceramic matrix composites

A micromechanics-based modeling approach that allows for the simultaneous consideration of deformation, damage, and oxidation associated with each constituent of silicon carbide (SiC)-based ceramic matrix composites (CMC), including the fiber, fiber coating, and matrix, is described. Chemical kinetics models from the literature are combined with a progressive damage model. Rupture predictions of unnotched and notched stress-hold (creep) specimens are compared with experimental measurements from a SiC/SiC CMC to assess the efficacy of the modeling approach. Techniques of improving creep rupture life are explored using the model.     

SiC/SiC mini-composites with multilayer ZrSiO4 interphase: Room-temperature properties and toughening mechanism

SiC/SiC mini-composites reinforced with SiC fibers coated with different numbers of ZrSiO₄ sublayers prepared via a non-hydrolytic sol-gel process were fabricated. The tensile strength and work of fracture of the prepared SiC/SiC mini-composites were determined, and the relationship between their mechanical properties and fracture morphologies was discussed. The toughening mechanism and the variation tendency of their mechanical properties were further elaborated by analyzing the interfacial debonding morphologies of the SiC/SiC mini-composites with 1 and 4 layers of ZrSiO₄ interphase as well as the results of prior studies. A relatively rare phenomenon—the delamination of the multilayer ZrSiO₄ interphase in the SiC/SiC mini-composites but not on the SiC fibers—was observed, which clearly demonstrated the weak bonding between the ZrSiO₄ sublayers in the SiC/SiC mini-composites. The ZrSiO₄ sublayer delamination mechanism was then explained based on the high-magnification morphologies found in and beside the ZrSiO₄ interphase.     

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.     

Effect of interface types on the heat-resistance of Cansas-II SiCf /SiC composites

The heat-resistance of the Cansas-II SiC/CVI-SiC mini-composites with a PyC and BN interface was studied in detail. The interfacial shear strength of the SiC/PyC/SiC mini-composites decreased from 15 MPa to 3 MPa after the heat treatment at 1500 °C for 50 h, while that of the SiC/BN/SiC mini-composites decreased from 248 MPa to 1 MPa, which could be mainly attributed to the improvement of the crystallization degree of the interface and the decomposition of the matrix. Aside from the above reasons, the larger declined fraction of the interfacial shear strength of the SiC/BN/SiC mini-composites might also be related to the gaps in the BN interface induced by the volatilization of B₂O₃·SiO₂ phase, leading to a significant larger declined fraction of the tensile strength of the SiC/BN/SiC mini-composites due to the obvious expansion of the critical flaws on the fiber surface. Therefore, compared with the CVI BN interface, the CVI PyC interface has better heat-resistance at high temperatures up to 1500 °C due to the fewer impurities in PyC.     

Multiple Cracking and Tensile Behavior for an Orthogonal 3-D Woven Si-Ti-C-O Fiber/Si-Ti-C-O Matrix Composite

This paper presents experimental results for the multiple microcracking and tensile behavior of an orthogonal 3-D woven Si-Ti-C-O fiber (Tyranno™ Lox-M)/Si-Ti-C-O matrix composite with a nanoscale carbon fiber/matrix interphase and processed using a polymer impregnation and pyrolysis route. Based on microscopic observations and unidirectional tensile tests, it is revealed that the inelastic tensile stress/strain behavior is governed by matrix cracking in transverse (90°) fiber bundles between 65 and 180 MPa, matrix cracking in longitudinal (0°) fiber bundles between 180 and 300 MPa, and fiber fragmentation above 300 MPa. A methodology for estimation of unidirectional tensile behavior in orthogonal 3-D composites has been established by the use and modification of existing theory. A good correlation was obtained between the predicted and measured composite strain using this procedure.     

Unified tensile model for unidirectional ceramic matrix composites with degraded fibers and interface

In order to overcome the roughness of the previously proposed micromechanical model [Acta Mech. Sin. (2011) 382], an enhanced multiscale analytical model was thus developed based on the rule of mixture, shear-lag theory and statistical approach to forecast the load carrying capacity of the prestressed ceramic matrix composites (CMCs) subjected to high-temperature oxidation. For comprehensive characterization of the mechanical degradation mechanisms, the oxidation induced fiber necking (or embrittlement) and fiber-matrix interface weakening were both taken into account. The suggested model was then applied to 2D-C/SiC composites. The influences of interface friction resistance, interface recession length, fiber necking factor and oxidation duration upon the residual mechanical property were investigated. Parametric analysis demonstrates that the modified formulations are much more reasonable than the previous model. The predicted residual tensile modulus and strength for the 2D-C/SiC composite agree well with the experimental data and furthermore the microscopic damage mechanisms were correlated properly with the macroscopic fracture morphologies.     

Effect of strain rate on the tensile properties of mini-SiC/SiC composites

SiC/SiC composites are the ideal candidates for hot-end components in aerospace and other high-tech fields. In recent years, as one type of material with simple structures, mini-composites have been widely used to study or initially verify the properties of ceramic matrix composites (CMC). Nevertheless, attentions were rarely paid on the influence of strain rate on the mechanical properties of mini-composites. In this study, based on mini-SiC/SiC composites, we investigated the effect of the strain rate on their tensile strength, initial tensile modulus, Weibull modulus, and fracture work. Furthermore, the underlying mechanisms were discussed and the exact constitutive model of the as-prepared mini-SiC/SiC composites was constructed according to the Michaelis-Menten and generalized linear models. This work can fill the gaps in the CMC research in some degree and provide a preliminary theoretical basis for the formulation of tensile properties test standards of mini-composites.     

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.     

In Situ Reacted Rare-Earth Hexaaluminate Interphases

A novel in situ reaction between a ceria-doped zirconia interphase coating on Saphikon fibers and an outer alumina coating has resulted in the formation of oriented hexaaluminate platelets which can act as a low fracture energy interface barrier for crack deflection in oxide-oxide ceramic-matrix composites (CMCs). The reaction proceeds only in reducing environments where the reduction of the cerium and zirconium ions to their 3+ valent state causes a destabilization phenomenon consistent with previously reported findings. The diffusion of the cerium from the zirconia into solid solution with the alumina can stabilize the layered hexaaluminate structure. Preferred orientational growth of the hexaaluminate parallel to the coating interface was observed which is the required orientation for enhanced debonding at the fiber/matrix interface in long-fiber-reinforced CMCs.     

Measuring Interphase Recession by Fiber Push-In Testing

A novel technique for measuring interphase recession in ceramic-matrix composites (CMCs) due to oxidation is described. The technique involves fiber push-in testing and analysis of the load–displacement curves. Fiber push-in tests were conducted on carbon-coated Hi-Nicalon SiC fibers in a CVI SiC matrix, where the carbon interphase had recessed due to oxidation. Estimates of interphase recession distances from analysis of fiber push-in tests are in reasonable agreement with measurements made by optical microscopy. Besides measuring the recession distance, the fiber push-in test can be used to investigate environmental effects on fiber bridging.