Oxidation and microstructure of SiCf/SiC composites in moist air up to 1600°C by X-ray tomographic characterization

SiC_f/SiC composites that possess PyC or BN interface layers were fabricated and then oxidized in moist air at 1000, 1200, 1400, and 1600°C. High-resolution CT was used for capturing 3D images and quantifying the SiC phase, mesophase, and voids. The oxidation behavior and microstructural evolution of SiC_f/SiC with PyC or BN interface are discussed in this study. The microstructure of the SiC_f/SiC with a PyC layer was seriously damaged in moist air at high temperature, whereas the BN interface layer enhanced the oxidation resistance of the SiC_f/SiC. These results are also confirmed by using XRD, oxidation mass gain, tensile testing, and SEM measurements. The results of the oxidation behavior and microstructural evolution for SiC_f/SiC oxidized in dry air are also compared with the results of this study. Comparing the SiC_f/SiC with a PyC interface layer, the composite with a BN interface layer oxidized in moist air exhibits a high void growth rate and a low SiO₂ grain growth rate from 1000 to 1600°C. This work will provide guidance for predicting the service life of SiC_f/SiC for multiscale damage rate models of materials at a local scale and will also provide guidance on the life service design of SiC_f/SiC materials.     

Mechanical properties and strengthening mechanism of SiCf/SiC mini-composites modified by SiC nanowires

The effects of the SiC nanowires (SiCNWs) and PyC interface layers on the mechanical and anti-oxidation properties of SiC fiber (SiC_f)/SiC composites were investigated. To achieve this, the PyC layer was coated on the SiC_f using a chemical vapour infiltration (CVI) method. Then, SiCNWs were successfully coated on the surface of SiC_f/PyC using the electrophoretic deposition method. Finally, a thin PyC layer was coated on the surface of SiC_f/PyC/SiCNWs. Three mini-composites, SiC_f/PyC/SiC, SiC_f/PyC/SiCNWs/SiC, and SiC_f/PyC/SiCNWs/PyC/SiC, were fabricated using the typical precursor infiltration and pyrolysis method. The morphologies of the samples were examined using scanning electron microscopy and energy dispersive X-ray spectrometry. Tensile and single-fibre push-out tests were carried out to investigate the mechanical performance and interfacial shear strength of the composites before and after oxidization at 1200 °C. The results revealed that the SiC_f/PyC/SiCNWs/SiC composites showed the best mechanical and anti-oxidation performance among all the composites investigated. The strengthening and toughening is mainly achieved by SiCNWs optimization of the interfacial bonding strength of the composite and its own nano-toughening. On the basis of the results, the effects of SiCNWs on the oxidation process and retardation mechanism of the SiC_f/SiC mini-composites were investigated.     

Microstructure and mechanical performance of SiCf/BN/SiC mini-composites oxidized at elevated temperature from ambient temperature to 1500 °C in air

SiC_f/BN/SiC mini-composites comprising single tow SiC fibre-reinforced SiC with chemical vapour deposited (CVD) BN interface layers were fabricated. The mechanical performance and binding strength of the composites and the fibre/interface for the oxidized SiC_f/BN/SiC mini-composite samples (oxidation at 1000, 1200, 1300, 1400 and 1500 °C in air for two hours) were investigated by tensile tests and fibre push-out tests, respectively. The value of oxidation mass change was also measured. Some unusual phenomena for the SiC_f/BN/SiC mini-composites oxidized at 1000 °C were discovered in this work. The tensile strength reached a maximum value, and the mass gain rate showed as a singular negative value, while the shear strength between the fibre and the matrix was moderate. Scanning electron microscopy, energy dispersive spectrometry, infrared spectroscopy and X-ray diffraction characterization methods were used to reveal the microstructural evolution and investigate the unusual phenomenon during oxidation procedures. This work will provide guidance for predicting the service life of SiC_f/BN/SiC composite materials and may enable these materials to become a backbone for thermal structure systems in aerospace applications.     

Mechanical properties of SiCf/SiC composites with alternating PyC/BN multilayer interfaces

Alternating pyrolytic carbon/boron nitride (PyC/BN)_n multilayer coatings were applied to the KD–II silicon carbide (SiC) fibres by chemical vapour deposition technique to fabricate continuous SiC fibre-reinforced SiC matrix (SiC_f/SiC) composites with improved flexural strength and fracture toughness. Three-dimensional SiC_f/SiC composites with different interfaces were fabricated by polymer infiltration and pyrolysis process. The microstructure of the coating was characterised by scanning electron microscopy, X–photoelectron spectroscopy and transmission electron microscopy. The interfacial shear strength was determined by the single-fibre push-out test. Single-edge notched beam (SENB) test and three-point bending test were used to evaluate the influence of multilayer interfaces on the mechanical properties of SiC_f/SiC composites. The results indicated that the (PyC/BN)_n multilayer interface led to optimum flexural strength and fracture toughness of 566.0?MPa and 21.5?MPa?m^1/2, respectively, thus the fracture toughness of the composites was significantly improved.     

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.     

In-situ formation of Ti3SiC2 interphase in SiCf/SiC composites by molten salt synthesis

Titanium silicon carbide (Ti₃SiC₂) film was synthesized by molten salt synthesis route of titanium and silicon powder based on polymer-derived SiC fibre substrate. The pre-deposited pyrolytic carbon (PyC) coating on the fibre was utilized as the template and a reactant for Ti₃SiC₂ film. The morphology, microstructure and composition of the film product were characterized. Two Ti₃SiC₂ layers form the whole film, where the Ti₃SiC₂ grains have different features. The synthesis mechanism has been discussed from the thickness of PyC and the batching ratio of mixed powder respectively. Finally, the obtained Ti₃SiC₂ film was utilized as interphase to prepare the SiC fibre reinforced SiC matrix composites (SiC_f/Ti₃SiC₂/SiC composites). The flexural strength (σ_F) and fracture toughness (K_IC) of the SiC_f/Ti₃SiC₂/SiC composite is 460 ± 20 MPa and 16.8 ± 2.4 MPa?m^1/2 respectively.     

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.     

The effects of preparation temperature on the SiCf/SiC 3D4d woven composite

Continuous silicon carbide fiber reinforced silicon carbide matrix (SiC_f/SiC) composites have promising applications in aero-engine due to their unique advantages, such as low density, high modulus and strength, outstanding high temperature resistance and oxidation resistance. As SiC fibers are main reinforcements in SiC_f/SiC composites, the crystallization rate and initial damage degree of SiC fibers are seriously influenced by preparation temperatures of SiC_f/SiC composites, namely mechanical properties of SiC fibers and SiC_f/SiC composites are influenced by preparation temperatures. In this paper, KD-II SiC fibers were woven into 3D4d preforms and SiC matrix was fabricated by PIP process at 1100 °C, 1200 °C, 1400 °C and 1600 °C. Digital image correlation (DIC) method was adopted to measure the uniaxial tensile properties of these SiC_f/SiC composites. In addition, finite element method (FEM) based on representative volume element (RVE) was adopted to predict the mechanical properties of SiC_f/SiC composites. The good agreements between numerical results and experimental results of uniaxial tensile tests verified the validity of the RVE. In last, the transverse tensile, transverse shear, uniaxial shear properties were predicted by this method. The predicted results illustrated that axial tensile, transverse tensile and axial shear properties were greatly influenced by the preparation temperatures of SiC_f/SiC composites while transverse shear properties were not significantly various. And the mechanical properties of SiC_f/SiC composites peaked at 1200 °C among these four temperatures while their values reached their lowest points at 1600 °C because of thermal damage and brittle failure of SiC_f/SiC composites.     

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.     

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.     

Enhanced microwave absorbance of oxidized SiCf/AlPO4 composites via the formation of a carbon layer on the SiC fibre surface

A single-layer radar-absorbing structure active in the X-band (8.2?GHz to 12.4?GHz) was demonstrated by blending SiC fibres with an AlPO₄ matrix material. The as-prepared SiC_f/AlPO₄ composites were oxidized at 1273?K for several hours to investigate the effects of oxidation on the dielectric and wave-absorbing properties. Scanning and transmission electron microscopy were used to characterize the morphology and microstructure of the composites. The AlPO₄-SiO₂ solid solution during oxidation promoted the formation of a complete carbon layer on the SiC fibre surface. The real and imaginary parts of the SiC_f/AlPO₄ composites increased from 4.2–4.4 to 5.9–7.1 and from 0.08–0.2 to 3.9–5.2, respectively, with increasing oxidation time from 0 to 10?h, respectively. When the thickness of the composites increased from 2.9?mm to 3.3?mm, the wave-absorbing property noticeably improved due to the formation of a carbon layer on the SiC fibre surface after oxidation.     

Mechanical and dielectric properties of SiCf/BN/SiBCN composites via different synthesis technologies

SiC fibers reinforced SiBCN ceramic matrix composites (SiC_f/BN/SiBCN composites) were synthesized by direct chemical vapor infiltration (CVI), polymer infiltration pyrolysis (PIP) or chemical vapor infiltration combined with polymer infiltration pyrolysis (CVI + PIP). It is shown that the insertion of a continuous and dense SiBCN matrix via the CVI process improves the flexural strength and modulus. Interface debonding and fiber pullout happened with 50–100 nm BN interface in CVI and CVI + PIP SiC_f/BN/SiBCN composites. The relative complex permittivity was measured in X-band. Higher ε′′ values in CVI-containing composites can be observed, which can be attributed to the accumulation of C and SiC phases and a multilayer matrix. Strong electromagnetic wave attenuation ability was obtained with high dielectric loss.     

Effect of SiC nanowires on the mechanical properties and thermal conductivity of 3D-SiCf/SiC composites prepared via precursor infiltration pyrolysis

In this study, SiC nanowires (SiC_NWS) were grown in situ on the surface of PyC interface through chemical vapor infiltration (CVI) to improve the mechanical characteristics and thermal conductivity of three-dimensional SiC_f/SiC composites fabricated via precursor infiltration pyrolysis (PIP). The effect of SiC_NWS on the properties of the obtained composites was investigated by comparing them with conventional SiC_f/PyC/SiC composites. After the deposition of SiC_NWS, the flexural strength of the SiC_f/SiC composites was found to increase by 46 %, and the thermal conductivity showed an obvious increase at 25?1000 °C. The energy release of the composites in the damage evolution process was analysed by acoustic emission. The results indicated that the damage evolution process was delayed owing to the decrease in porosity, the crack deflection and bridging of the SiC_NWS. Furthermore, the excellent thermal conductivity was attributed to the thermally conductive pathways formed by the SiC_NWS in the dense structure.     

Synthesis of coatings on SiC fibers and their effects on microstructure and mechanical properties of SiCf/SiBCN composites

In this study, the amorphous C, ZrB₂, and BN single-layer coatings as well as C/BN, C/ZrB₂, ZrB₂/BN, and C/ZrB₂/BN composite coatings were prepared on SiC fibers (SiC_f) by an in situ synthesis and solution impregnation–pyrolysis method. Subsequently, SiC_f/SiBCN composites were fabricated by hot-pressing sintering at 1900℃/60 MPa/30 min to explore the influence of different coatings on the microstructure and mechanical performance of resulting composites. After the preparation of single-layer-coated SiC_f, the SiC_f(BN) or SiC_f(ZrB₂) tended to be overlapped with each other, whereas the dispersion of amorphous C–coated SiC_f was satisfying. Besides, some uneven areas and attached particles have appeared on fiber surfaces of the SiC_f(BN) or SiC_f(ZrB₂), whereas smooth and dense surfaces of amorphous C–coated SiC_f were observed. Because the uniformity of ZrB₂ coatings can be partially damaged by the subsequent coating process of BN, the composite coatings of ZrB₂/BN and C/ZrB₂/BN were thereby not suitable for strengthening SiBCN matrix. The SiC_f/SiBCN composites with C/ZrB₂ coatings have desirable comprehensive mechanical properties. Nevertheless, the conventional toughening mechanisms such as fiber pull-out and bridging, and crack deflection are not available for these composites because the serious crystallization of SiC_f leading to great strength loss, resulting in catastrophic brittle fracture.     

Microstructure and mechanical properties of quasi-isotropic chopped fiber-reinforced PyC–SiC matrix composite prepared by novel nondamaging method

In this work, quasi-isotropic chopped carbon fiber-reinforced pyrolytic carbon and silicon carbide matrix (C_f/C–SiC) composites and chopped silicon carbide fiber-reinforced silicon carbide matrix (SiC_f/SiC) composites were prepared via novel nondamaging method, namely airlaid process combined with chemical vapor infiltration. Both composites exhibit random fiber distribution and homogeneous pore size. Young's modulus of highly textured pyrolytic carbon (PyC) matrix is 23.01 ± 1.43 GPa, and that of SiC matrix composed of columnar crystals is 305.8 ± 9.49 GPa in C_f/C–SiC composites. Tensile strength and interlaminar shear strength of C_f/C–SiC composites are 52.56 ± 4.81 and 98.16 ± 24.62 MPa, respectively, which are both higher than those of SiC_f/SiC composites because of appropriate interfacial shear strength and introduction of low-modulus and highly textured PyC matrix. Excellent mechanical properties of C_f/C–SiC composites, particularly regarding interlaminar shear strength, are due to their quasi-isotropic structure, interfacial debonding, interfacial sliding, and crack deflection. In addition to the occurrence of crack deflection at the fiber/matrix interface, crack deflection in C_f/C–SiC composites takes also place at the interface between PyC–SiC composite matrix and the interlamination of multilayered PyC matrix. Outstanding mechanical properties of as-prepared C_f/C–SiC composites render them potential candidates for application as thermal structure materials under complex stress conditions.     

Ring compression properties of SiCf/SiC composites prepared by chemical vapor infiltration

SiC fiber reinforced SiC matrix (SiC_f/SiC) composites prepared by chemical vapor infiltration are one of promising materials for nuclear fuel cladding tube due to pronounced low radioactivity and excellent corrosion resistance. As a structure component, mechanical properties of the composites tubes are extremely important. In this study, three kinds of SiC_f preform with 2D fiber wound structure, 2D plain weave structure and 2.5D shallow bend-joint structure were deposited with PyC interlayer of about 150–200?nm, and then densified with SiC matrix by chemical vapor infiltration at 1050?°C or 1100?°C. The influence of preform structure and deposition temperature of SiC matrix on microstructure and ring compression properties of SiC_f/SiC composites tubes were evaluated, and the results showed that these factors have a significant influence on ring compression strength. The compressive strength of SiC_f/SiC composites with 2D plain weave structure and 2.5D shallow bend-joint structure are 377.75?MPa and 482.96?MPa respectively, which are significantly higher than that of the composites with 2D fiber wound structure (92.84?MPa). SiC_f/SiC composites deposited at 1100?°C looks like a more porous structure with SiC whiskers appeared when compared with the composites deposited at 1050?°C. Correspondingly, the ring compression strength of the composites deposited at 1100?°C (566.44?MPa) is higher than that of the composites deposited at 1050?°C (482.96?MPa), with a better fracture behavior. Finally, the fracture mechanism of SiC_f/SiC composites with O-ring shape was discussed in detail.     

Influence of pyrolysis and melt infiltration temperatures on the mechanical properties of SiCf/SiC composites

In order to improve the degree of matrix densification of SiC_f/SiC composites based on liquid silicon infiltration (LSI) process, the microstructure and mechanical properties of composites according to various pyrolysis temperatures and melt infiltration temperatures were investigated.Comparing the microstructures of SiC_f/C carbon preform by a one-step pyrolysis process at 600 °C and two-step pyrolysis process at 600 and 1600 °C, the width of the crack and microcrack formation between the fibers and matrix in the fiber bundle increased during the two-step pyrolysis process. For each pyrolysis process, the density, porosity, and flexural strength of the SiC_f/SiC composites manufactured by the LSI process at 1450–1550 °C were measured to evaluate the degree of matrix densification and mechanical properties. As a result, the SiC_f/SiC composite that was fabricated by the two-step pyrolysis process and LSI process showed an 18% increase in density, 16%p decrease in porosity, and 150% increase in flexural strength on average compared to the composite fabricated by the one-step pyrolysis process.In addition, among the SiC_f/SiC specimens fabricated by the LSI process after the same two-step pyrolysis process, the specimen that underwent the LSI process at 1500 °C showed 30% higher flexural strength on average than those at 1450 or 1550 °C. Furthermore, under the same pyrolysis temperature, the mechanical strength of SiC_f/SiC specimens in which the LSI process was performed at 1500 °C was higher than that of the 1550 °C although both porosity and density were almost similar. This is because the mechanical properties of the Tyranno-S grade SiC fibers degraded rapidly with increasing LSI process temperature.     

Oxidation and thermal shock resistant properties of Al-modified environmental barrier coating on SiCf/SiC composites

SiC_f/SiC ceramic matrix composites (CMCs) are being widely used in the hot-sections of gas-turbines, especially for aerospace applications. These CMCs are subjected to surface recession if exposed to heat-corrosion. In this research, an alternative environmental barrier coating (EBC) is introduced to protect the SiC_f/SiC CMC from high temperature degradation that is, Al film was deposited on the surface of SiC_f/SiC CMC followed by heat-treatment in a vacuum. After that, a dense Al₂O₃ overlay was in-situ synthesized on the surface of CMC, and in this process the microstructure evolution of SiC_f/SiC CMC was analyzed. The oxidation and thermal shock resistance were characterized, showing that the Al-modified SiC_f/SiC CMC has a better oxidation resistance, because the dense Al₂O₃ overlay can hinder oxygen diffusion from environment. What is more, the water-quenching testes show that the Al-modified SiC_f/SiC CMC has a good spallation resistance.     

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.     

Synchrotron X-ray tomographic characterization of CVI engineered 2D-woven and 3D-braided SiCf/SiC composites

The properties of ceramic matrix composites strongly depend upon their complex internal structures. To better understand and improve the properties of the silicon carbide fiber-reinforced silicon carbide matrix composites (SiC_f/SiC), we explored the microstructural properties of composites reinforced with either two-dimensional (2D) woven or three-dimensional (3D) braided preforms using synchrotron X-ray computed microtomography. Transects and volumetric images of the composites were reconstructed from objection images and the microstructures were investigated in three spatial directions. The network of void space in a composites was visualized in 3D and quantitative analysis of the porosity was performed to characterize the fiber-tissue structures. 2D-woven SiC_f/SiC composite exhibited important fluctuations of porosity in different directions and the stacking of plies had a significant effect on the porosity distribution. In contrast, 3D-braided SiC_f/SiC composites showed much less variation of porosity. We found the degree of densification of the composite also influenced the porosity distribution.