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.     

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.     

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.     

Preparation of SiC/SiC composites with high toughness by reaction of the SiCP+C double-cladding layer with liquid silicon

SiC/SiC composites prepared by liquid silicon infiltration (LSI) have the advantages of high densification, matrix cracking stress and ultimate tensile strength, but the toughness is usually insufficient. Relieving the residual microstress in fiber and interphase, dissipating crack propagation energy, and improving the crystallization degree of interphase can effectively increase the toughness of the composites. In this work, a special SiC particles and C (SiC_P +C) double-cladding layer is designed and prepared via the infiltration of SiC_P slurry and chemical vapor infiltration (CVI) of C in the porous SiC/SiC composites prepared by CVI. After LSI, the SiC generated by the reaction of C with molten Si combines with the SiC_P to form a layered structure matrix, which can effectually relieve residual microstress in fiber and interphase and dissipate crack propagation energy. The crystallization degree of BN interphase is increased under the effects of C-Si reaction exotherm. The as-received SiC/SiC composites possess a density of 2.64 g/cm³ and a porosity of 6.1%. The flexural strength of the SiC/SiC composites with layered structure matrix and highly crystalline BN interphase is 577 MPa, and the fracture toughness reaches up to 37 MPa·m^1/2. The microstructure and properties of four groups of SiC/SiC composites prepared by different processes are also investigated and compared to demonstrate the effectiveness of the SiC_P +C double-cladding layer design, which offers a strategy for developing the SiC/SiC composites with high performance.     

SiC/SiC minicomposites with structure-graded BN interphases

BN interphases in SiC/SiC minicomposites were produced by infiltration of fibre tows from BF₃–NH₃–H₂ gaseous system. During interphase one-step processing, the tow travels through a reactor containing a succession of different hot areas. By TEM characterization, the BN interphases were found to be made of a structural gradient: from isotropic to highly anisotropic. The very first coating is poorly organised and allows to protect the fibre from a further chemical attack by the reactant mixture. The minicomposites were tensile tested at room temperature with unloading-reloading cycles. The BN interphases act as mechanical fuses; the fibre/matrix bonding intensity ranges from weak to rather strong depending on the tow travelling rate during interphase infiltration. The specimen lifetimes at 700°C under a constant tensile loading were measured in dry and moist air. Compared to a pyrocarbon reference interphase, the BN interphases significantly improve the oxidation resistance of the SiC/SiC minicomposites.     

SiC/SiC mini-composites with yttrium disilicate fiber coatings: Oxidation in steam

Solutions of YPO₄ were used to precipitate YPO₄ on pre-oxidized Hi-Nicalon-S SiC fibers. Tows of the coated fibers were then infiltrated with a preceramic polymer loaded with SiC particles to form mini-composites. During pyrolysis of the matrix, SiO₂ and YPO₄ on the fibers reacted and formed a Y₂Si₂O₇ fiber matrix interphase. Mini-composites were exposed to steam at 1000 °C for 10, 50, and 100 h, tensile tested, and the effect of oxidation in steam on the functionality of the Y₂Si₂O₇ fiber coating was investigated. The minicomposites oxidized at 1000 °C for 10 h retained 100 % of their unoxidized strength, and those oxidized for 50 and 100 h retained 92 % and 90 % of unoxidized strength, respectively. Strength retention and fiber pullout in both unoxidized and oxidized minicomposites suggests that the Y₂Si₂O₇ interphase was effective in maintaining a weak fiber-matrix interface.     

The mechanical,thermophysical and electromagnetic properties of UD SiCf/SiC composites in different directions

Unidirectional (UD) silicon carbide (SiC) fiber-reinforced SiC matrix (UD SiC_f/SiC) composites with CVI BN interphase were fabricated by polymer infiltration-pyrolysis (PIP) process. The effects of the anisotropic distribution of SiC fibers on the mechanical properties, thermophysical properties and electromagnetic properties of UD SiC_f/SiC composites in different directions were studied. In the direction parallel to the axial direction of SiC fibers, SiC fibers bear the load and BN interphase ensures the interface debonding, so the flexural strength and the fracture toughness of the UD SiC_f/SiC composites are 813.0 ± 32.4 MPa and 26.1 ± 2.9 MPa·m^1/2, respectively. In the direction perpendicular to the axial direction of SiC fibers, SiC fibers cannot bear the load and the low interfacial bonding strengths between SiC fiber/BN interphase (F/I) and BN interphase/SiC matrix (I/M) both decrease the matrix cracking stress, so the corresponding values are 36.6 ± 6.9 MPa and 0.9 ± 0.5 MPa?m^1/2, respectively. The thermal expansion behaviors of UD SiC_f/SiC composites are similar to those of SiC fibers in the direction parallel to the axial direction of SiC fibers, and are similiar to those of SiC matrix in the direction perpendicular to the axial direction of SiC fibers. The total electromagnetic shielding effectiveness (EM SE_T) of UD SiC_f/SiC composites attains 32 dB and 29 dB when the axial direction of SiC fibers is perpendicular and parallel to the electric field direction, respectively. The difference of conductivity in different directions is the main reason causing the different SE_T. And the dominant electromagnetic interference (EMI) shielding mechanism is absorption for both studied directions.     

Effects of cyclic tensile loading on the rupture behavior of orthogonal 3-D woven SiC fiber/SiC matrix composites at elevated temperatures in air

This study examined the rupture mechanisms of an orthogonal 3D woven SiC fiber/BN interface/SiC matrix composite under combination of constant and cyclic tensile loading at elevated temperature in air. Monotonic tensile testing, constant tensile load testing, and tension–tension fatigue testing were conducted at 1100 °C. A rectangular waveform was used for fatigue testing to assess effects of unloading on the damage and failure behavior. Microscopic observation and single-fiber push-out tests were conducted to reveal the rupture mechanisms. Results show that both oxidative matrix crack propagation attributable to oxidation of the fiber–matrix interface and the decrease in the interfacial shear stress (IFSS) at the fiber–matrix interface significantly affect the lifetime of the SiC/SiC composites. A rupture strength degradation model was proposed using the combination of the oxidative matrix crack growth model and the IFSS degradation model. The prediction roughly agreed with the experimentally obtained results.     

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).     

Matrix cracking of 2D SiC/SiC composite characterized by in situ SEM and nano-CT

Two-dimensional plain-woven silicon carbide (SiC) fiber-reinforced SiC matrix (2D SiC/SiC) composite was prepared by polymer infiltration-pyrolysis (PIP). Matrix cracking mechanisms of the composite were investigated by in situ SEM and nano-CT to grasp tensile damage evolution. Results showed that PIP-SiC matrix possessed low-fracture energy with non-homogeneous distribution, leading to simultaneous initiation of matrix cracking outside transverse fiber bundles and in unreinforced regions. Cracks then got deflected along weak fiber/matrix interface, which accelerated crack proliferation within the composite. With an increase in the stress, cracks subsequently deflected along plain-woven layers and converged to form longitudinal macrocracks. The composite was finally delaminated via sliding.     

Effect of intermediate heat treatment on mechanical properties of SiCf/SiC composites with BN interphase prepared by ICVI

SiC_f/SiC composites with BN interface were prepared through isothermal-isobaric chemical vapour infiltration process. Room temperature mechanical properties such as tensile, flexural, inter-laminar shear strength and fracture toughness (K_IC) were studied for the composites. The tensile strength of the SiC_f/SiC composites with stabilised BN interface was almost 3.5 times higher than that of SiC_f/SiC composites with un-stabilised BN interphase. The fracture toughness is similarly enhanced to 23 MPa m^1/2 by stabilisation treatment. Fibre push-through test results showed that the interfacial bond strength between fibre and matrix for the composite with un-stabilised BN interface was too strong (>48 MPa) and it has been modified to a weaker bond (10 MPa) due to intermediate heat treatment. In the case of composite in which BN interface was subjected to thermal treatment soon after the interface coating, the interfacial bond strength between fibre and matrix was relatively stronger (29 MPa) and facilitated limited fibre pull-out.     

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.     

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.     

Tensile and Stress-Rupture Behavior of SiC/SiC Minicomposite Containing Chemically Vapor Deposited Zirconia Interphase

The tensile and stress-rupture behavior of SiC/SiC minicomposite containing a chemically vapor deposited (CVD) ZrO₂ interphase was evaluated. Fractographic analyses showed that in situ fiber strength and minicomposite failure loads were strongly dependent on the phase contents and microstructure of the ZrO₂ interphase. When the ZrO₂ interphase structure possessed a weakly bonded interface within the dense ZrO₂ interphase coating layer, the interphase sufficiently protected the fiber surface from processing degradation and promoted matrix crack deflection around the fibers. With this weakly bonded interphase, the stress-rupture properties of SiC/SiC minicomposite at 950° and 1200°C appeared to be controlled by fiber rupture properties, and compared favorably to those previously measured for state-of-the-art BN fiber coatings.     

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.     

High-temperature flexural strength of I-CVI processed Cf/SiC composites with variable interphases

The effect of single-layer pyrocarbon (PyC) and multilayered (PyC/SiC)_n=4 interphases on the flexural strength of un-coated and SiC seal-coated stitched 2D carbon fiber reinforced silicon carbide (C_f/SiC) composites was investigated. The composites were prepared by I-CVI process. Flexural strength of the composites was measured at 1200 °C in air atmosphere. It was observed that irrespective of the type of interphase, the seal coated samples showed a higher value of flexural strength as compared to the uncoated samples. The flexural strength of 470 ± 12 MPa was observed for the seal coated C_f/SiC composite samples with multilayered interphase. The seal coated samples with single layer PyC interphase showed flexural strength of 370 ± 20 MPa. The fractured surfaces of tested samples were analyzed in detail to study the fracture phenomena. Based on microstructure-property relations, a mechanism has been proposed for the increase of flexural properties of C_f/SiC composites having multilayered interphase.     

Interpreting acoustic energy emission in SiC/SiC minicomposites through modeling of fracture surface areas

The relationship between acoustic emission (AE) and damage source areas in SiC/SiC minicomposites was modeled using insights from tensile testing in-scanning electron microscope (SEM). Damage up to matrix crack saturation was bounded by: (1) AE generated by matrix cracking (lower bound) and (2) AE generated by matrix cracking, and fiber debonding and sliding in crack wakes (upper bound). While fiber debonding and sliding exhibit lower strain energy release rates than matrix cracking and fiber breakage, they contribute significant damage area and likely produce AE. Fiber breaks beyond matrix crack saturation were modeled by two conditions: (i) only fiber breaks generated AE; and (ii) fiber breaks occurred simultaneously with fiber sliding to generate AE. While fiber breaks are considered the dominant late-stage mechanism, our modeling indicates that other mechanisms are active, a finding that is supported by experimental in-SEM observations of matrix cracking in conjunction with fiber failure at rupture.     

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.     

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.     

Mechanical and microwave dielectric properties of SiCf/SiC composites with BN interphase prepared by dip-coating process

The BN interphase of SiC fiber-reinforced SiC matrix (SiCf/SiC) composites was fabricated by dip-coating process with boric acid and urea as precursor. The results show that the tensile strength of SiC fiber decreases about 30% after BN coating treatment, but the BN coating has little influence on the electrical resistivity of SiC fiber. Compared with the as-received SiCf/SiC composites, the SiCf/SiC composites with BN interphase exhibit a toughened fracture behavior, and the flexural strength is about 2 times that of the as-received SiCf/SiC composites. From the microstructural analysis, it can be confirmed that the BN interphase plays a key part in weakening interfacial bonding, which can improve the mechanical properties of SiCf/SiC composites remarkably. Owing to the close dielectric properties between SiC and BN, the complex permittivity of SiCf/SiC composites with and without the BN interphase is similar.