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.     

Effect of pyrocarbon interphase texture and thickness on tensile damage and fracture in T-700™ carbon fiber–reinforced silicon carbide minicomposites

In this paper, T-700™ carbon fiber–reinforced silicon carbide (C/SiC) minicomposites with pyrocarbon (PyC) interphase with different textural microstructure and thickness were fabricated using the chemical vapor infiltration method. The interface properties (i.e., textural microstructure, thickness, hardness, and modulus) were obtained through multiple testing methods (i.e., Raman spectroscopy, X-ray diffraction, scanning electron microscopy, and nanoindentation tests). Relationships between the deposition temperature and residence time with the texture type (i.e., low, medium, and high texture) were established. Uniaxial tensile experiments were conducted for C/SiC minicomposites with different PyC interphases to characterize the composite's internal damage evolution and fracture. Relationships between the composite's tensile nonlinear damage evolution, fracture strength and strain, PyC interphase texture, and thickness were established. The composite's tensile strength and fracture strain were the highest for the C/SiC minicomposite with medium-high texture PyC interphase. For the C/SiC minicomposite with the same texture interphase, the composite's tensile strength and fracture strain were affected by the coating thickness. The higher the thickness of the coating, the lower the composite's tensile strength and fracture strain.     

PyC interphase growth mechanism and control models of C/SiC composites

To better understand the pyrocarbon (PyC) interphase growth mechanism, a series of experiments was conducted on the PyC deposited on T-300™ and T-700™ carbon fibers by the chemical vapor infiltration (CVI) method. Nine groups of fabrication parameters were used to analyze the effects of deposition temperature, pressure, and residence time on the PyC interphase growth mechanism. Atomic force microscopy (AFM), scanning electron microscopy (SEM), high-resolution transmission electron microscopy (TEM), X-ray diffraction analysis (XRD), Raman spectroscopy, and nanoindentation tests were performed to characterize the microstructures of carbon fibers and PyC interphase. The PyC interphase growth mechanism was discussed, and the relationships between the fabrication parameters, R (C₂/C₆) value, texture type, and interphase thickness were established through numerical simulations. The hardness and modulus of PyC for T-300™ and T-700™ carbon fibers were measured. The tensile behaviors of C/SiC minicomposites with medium and high textures PyC interphases were analyzed. The C/SiC composite with the medium texture PyC interphase possessed the higher fracture strength and failure strain with a longer fiber pullout length at the fracture surface.     

Improvement of high-temperature stability of PIP SiCf/SiC material through in situ grown BNNTs

In this paper, the effect of in situ grown boron nitride nanotubes (BNNTs) and preparation temperature on mechanical behavior of PIP (Precursor Infiltration and Pyrolysis) SiC_f/SiC minicomposites under monotonic and compliance tensile is investigated. In situ BNNTs are grown on the surface of SiC fibers using ball milling–annealing process. Composite elastic modulus, tensile strength, fracture strain, tangent modulus, and loading/unloading inverse tangent modulus (ITM) are obtained and adopted to characterize the mechanical properties of the composites. Microstructures of in situ grown BNNTs and tensile fracture surfaces are observed under scanning electronic microscopic (SEM). For SiC_f/SiC minicomposites with BNNTs, the elastic modulus, tensile strength, and fracture strain are all lower than those of SiC_f/SiC minicomposites without BNNTs, mainly due to high preparation temperature and the oxidation of the PyC interphase during the annealing process. Tensile stress–strain curves of SiC_f/SiC minicomposites with and without BNNTs are predicted using the developed micromechanical constitutive model. The predicted results agreed with experimental data. This work will provide guidance for predicting the service life of SiC_f/SiC composite materials and may enable these materials to become a backbone for thermal structure systems in aerospace applications.     

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.     

Preparation and tensile behavior of SiCf/SiC mini composites containing different types and thicknesses of interphase

SiC fiber-reinforced SiC matrix (SiC_f/SiC) composites are promising materials for high-temperature structural applications. In this study, KD-II SiC fiber bundles with a C/Si ratio of approximately 1.25 and an oxygen amount of 2.53%, were used as reinforcement. PyC interphase, PyC-SiC co-deposition interphase I and II, with different thicknesses, and SiC matrix were deposited into the SiC fiber bundles by using chemical vapor infiltration (CVI) to form SiC_f/SiC mini composites. When the thickness of the interphase is approximately 1000 nm, the ultimate tensile stress and strain of SiC_f/SiC mini composites with PyC-SiC co-deposition interphase I can reach 1120.0 MPa and 0.72%, respectively, which are significantly higher than those of SiC_f/SiC mini composites with a PyC interphase (740.0 MPa, 0.87%) and PyC-SiC co-deposition interphase II (645.0 MPa, 0.54%). The effect of thicknesses and types of interphase on tensile fracture behavior of mini composites and then the fracture mechanism are discussed in detail.     

Hi-Nicalon/SiC Minicomposites with (Pyrocarbon/SiC)n Nanoscale Multilayered Interphases

SiC/SiC minicomposites that comprise different pyrocarbon/silicon carbide ((PyC/SiC) _n ) multilayered interphases and a tow of SiC fibers (Hi-Nicalon) have been prepared via pressure-pulsed chemical vapor infiltration. Pyrocarbon and SiC were deposited from propane and a CH₃SiCl₃/H₂ mixture, respectively. The microstructure of the interphases has been investigated using transmission electron microscopy. The mechanical tensile behavior of the minicomposites at room temperature exhibits the classical features of tough composites, regardless of the characteristics of the (PyC/SiC) sequences. The interfacial shear stress has been determined from the width of hysteresis loops upon unloading/reloading and from the crack-spacing distance at saturation. All the experimental data indicate that the strength of the fiber/interphase interfaces is rather weak (∼50 MPa).     

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.     

Relationships between the accumulative damage and dielectric properties of woven BN-coated Hi-Nicalon™ SiC fibre-reinforced SiC matrix composites

The accumulative damage behaviour of BN-coated Hi-Nicalon™ SiC fibre-reinforced SiC matrix composite was examined under tensile cyclic loading at room and elevated temperatures. The accumulative damage occurring during the cyclic loading was quantitatively characterised using the damage parameter obtained by the hysteresis loop curves. The damage parameter increased with increasing applied stress beyond the matrix cracking stress, and it subsequently retained a nearly constant value until just before fracture. Moreover, the dielectric constant, dielectric loss and loss tangent of the composite were measured before and after the fracture in the frequency range 1–1000 MHz. The dielectric properties had similar frequency dependency before and after the fracture. However, the dielectric constant, dielectric loss and loss tangent were lower in the post-fractured specimens than in the pristine ones. The reduction of the dielectric properties was associated with the accumulative damage stored in the specimens. In addition, the relationships between the dielectric properties and the damage parameter were described in detail.     

Effect of multiple loading sequence on time-dependent stress rupture of fiber-reinforced ceramic-matrix composites

In this paper, the effect of multiple loading sequence on time-dependent stress rupture of fiber-reinforced ceramic-matrix composites (CMCs) at intermediate temperatures in oxidative environment is investigated. Considering multiple damage mechanisms, a micromechanical constitutive model for time-dependent stress rupture is developed to determine damage evolution of matrix crack spacing, interface debonding and oxidation length, and fiber failure probability under single and multiple loading sequences. The relationships between multiple loading sequence, composite strain evolution, time, matrix cracking, interface debonding and oxidation, and fiber fracture are established. The effects of fiber volume, matrix crack spacing, interface shear stress in the slip and oxidation region, and environment temperature on the stress/time-dependent strain, interface debonding and oxidation fraction, and fiber broken fraction of SiC/SiC composite are analyzed. The experimental stress rupture of SiC/SiC composite under single and multiple loading sequences at 950°C in air atmosphere is predicted. Compared with single loading stress, multiple loading sequence affects the interface debonding and oxidation fraction in the debonding region, leading to the higher fiber broken fraction and shorter stress-rupture lifetime.     

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.     

Interfacial optimization of SiC nanocomposites reinforced by SiC nanowires with high volume fraction

High volume fraction SiC nanowires-reinforced SiC composites (SiCNWs/SiC) were prepared by hybrid process of chemical vapor infiltration and polymer impregnation/pyrolysis in this research. SiCNWs networks are first to be made promising a high volume fraction (20 vol%), and the pyrolytic carbon (PyC) interphase with 5 nm is designed on SiCNWs surface to optimize the bonding condition between SiCNWs and SiC matrix. Nanoindentation shows a modulus of 494 ± 14 GPa of SiCNWs/SiC composites without interphase comparing to the one with PyC interphase of 452 ± 13 GPa. However, the 3-point bending test shows a higher strength of the composite with PyC interphase (273 ± 32 MPa) comparing with the one without interphase (240 ± 38 MPa). The fracture surface is observed under SEM, which shows a longer SiCNWs pullout of the composite with PyC interphase. The energy dissipation during the 3-point bending test is calculated by the length of nanowire pull-out, it demonstrates that the SiCNWs with PyC interphase possess better performance for toughening composite. Further characterization proves that the PyC interphase can give SiCNWs/SiC composites higher fracture toughness (4.49 ± 0.44 MPa·m^1/2) than the composites without interphase (3.66 ± 0.28 MPa·m^1/2).     

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.     

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.     

Influence of Strong Fiber/Coating Interfaces on the Mechanical Behavior and Lifetime of Hi-Nicalon/(PyC/SiC)n/SiC Minicomposites

Hi-Nicalon fiber-reinforced silicon carbide matrix minicomposites (Hi-Nicalon/SiC) with nanoscale multilayered (PyC/SiC) _n fiber coatings (also referred to as interphases) have been manufactured via pressure pulse chemical vapor infiltration (P-CVI). Fiber/coating interfaces were strengthened by using treated fibers. The microstructures of the interphases as well as the propagation and deflection of cracks in the interfacial region were investigated by SEM and TEM. Interfacial shear stress was estimated using various methods based on either the width of hysteresis loops on unloading–reloading, crack spacing, or fitting of the force–deformation curve using a micromechanics-based model. Tensile behavior at room temperature and lifetime in static fatigue in air at 700°C were related to the interphase/interface characteristics.     

The design of zirconium and hafnium germanate interphase in SiCf/SiC composites

Unidirectional SiC_f/SiC minicomposites with SiC matrix derived by polymer-impregnation pyrolysis (PIP), reinforced with SiC fibers coated with zirconium or hafnium germanate were fabricated. Microdebonding indentation tests for SiC_f/SiC composites with one- and multilayered germanate interphase were performed. Interfacial shear stress depending on the number of germanate interfacial layers and morphology was determined. The microstructure of the minicomposites and indented fracture surfaces were studied by scanning electron microscopy (SEM). It was stated that an increase in the number of interfacial coatings leads to a decrease in the interfacial frictional stress in SiC_f/SiC minicomposites with germanate interphases. The key factor of interphase weakening is the formation of a weak interlayer bonding within the interphase but not germanate layered crystal structure itself. Thus, bonding at the fiber/matrix boundary could be regulated by the number of layers of ZrGeO₄ or HfGeO₄ in the interphase zone.     

The improvement of mechanical properties of SiC/SiC composites by in situ introducing vertically aligned carbon nanotubes on the PyC interface

In order to improve the mechanical properties, vertically aligned carbon nanotubes (VACNTs) were in situ introduced on the pyrocarbon (PyC) interfaces of the multilayer preform via chemical vapor deposition (CVD) process under tailored parameters. Chemical vapor infiltration (CVI) process was then employed to densify the multilayer preform to acquire SiC/SiC composites. The results show that the growth of VACNTs on PyC interface is highly dependent to the deposition temperature, time and constituent of gas during CVD process. The preferred orientation and high graphitization of VACNTs were obtained when temperature is 800?℃ and C₂H₄/H₂ ratio is 1:3. The bending strength and fracture toughness of SiC/SiC composites with PyC and PyC-VACNTs interfaces were compared. Compared to the SiC/SiC composite with PyC interface, the bending strength and fracture toughness increase 1.298 and 1.359 times, respectively after the introduction of PyC-VACNTs interface to the SiC/SiC composites. It is also demonstrated that the modification of PyC interface with VACNTs enhances the mechanical properties of SiC/SiC composites due to the occurrence of more fiber pull-outs, interfacial debonding, crack branching and deflection     

Mechanical property degradation of high crystalline SiC fiber–reinforced SiC matrix composite neutron irradiated to ∼100 displacements per atom

For the development of silicon carbide (SiC) materials for next-generation nuclear structural applications, degradation of material properties under intense neutron irradiation is a critical feasibility issue. This study evaluated the mechanical properties and microstructure of a chemical vapor infiltrated SiC matrix composite, reinforced with a multi-layer SiC/pyrolytic carbon–coated Hi-Nicalon^TM Type S SiC fiber, following neutron irradiation at 319 and 629?°C to ～100 displacements per atom. Both the proportional limit stress and ultimate flexural strength were significantly degraded as a result of irradiation at both temperatures. After irradiation at 319?°C, the quasi-ductile fracture behavior of the nonirradiated composite became brittle, a result that was explained by a loss of functionality of the fiber/matrix interface associated with the disappearance of the interphase due to irradiation. The specimens irradiated at 629?°C showed increased apparent failure strain because the fiber/matrix interphase was weakened by irradiation-induced partial debonding.     

Increasing the strength and toughness of a carbon fiber/silicon carbide composite by heat treatment

The effect of heat treatment on the strengthening and toughening of a carbon fiber/silicon carbide composite (C/SiC) with a thin pyrolytic carbon (PyC) interphase was investigated. Tensile strength and modulus were measured using tensile tests, and toughness was obtained by calculating the area under the stress–strain curves. Results show that with increasing heat treatment temperature both the strength and toughness of the C/SiC composite increased, but the modulus decreased. After heat treatment at 1900 °C the tensile strength and toughness increased by a maximum of 42% and 252%, respectively, and the modulus decreased by 48%. X-ray diffraction analysis and microstructural observation confirmed that the heat treatment mainly increased the graphitization of the amorphous PyC interphase, and this was responsible for the property changes observed because it decreased the interfacial sliding resistance associated with long fiber pull-out, relieved the thermal residual stress and lower stress concentrations on the fibers to uniformly share the load for improving the strength and toughness.     

Evaluation of SiC/SiC minicomposites with yttrium disilicate fiber coating

Hi‐Nicalon‐S/α‐Y₂Si₂O₇/SiC minicomposites were formed by polymer infiltration pyrolysis (PIP) and characterized by TEM, SEM fractography, tensile testing, and fiber push‐in testing. All minicomposites with α‐Y₂Si₂O₇ fiber coatings had strengths significantly higher than the control samples without fiber coatings. Extensive fiber pullout with debonding at the coating‐fiber interface or within the coating itself was observed in minicomposites with Y₂Si₂O₇ fiber coatings, but no debonding was observed in minicomposites without fiber coatings. Debond energies of 4.5 ± 3, 4.6 ± 3 J/m² and average sliding stresses of 91 ± 40, 94 ± 40 MPa were measured by fiber push‐in tests.