Fatigue behavior and damage evolution of SiC/SiC composites under high-temperature anaerobic cyclic loading

In the present study, the fatigue behavior and damage evolution of SiC/SiC minicomposites at elevated temperatures in oxygen-free environment are investigated which are important for their application and are still unclear. The high-temperature fatigue test platform is developed and the fatigue stress-life curve and the stress-strain response are obtained. The test result shows that the life of the material at elevated temperature is shorter than that at room temperature under the same stress level. Moreover, the hysteresis loop width and the residual strain increase with the increasing of the cycles while the hysteresis modulus decreases during the fatigue cycling. The evolution process of matrix cracks is observed using the real-time remote detection system. It is found that matrix cracking is insensitive to the cyclic loading which is similar to room temperature and is due to that the degeneration of the interfacial shear stress reduces the area of high stress in matrix. The fiber/matrix interfacial shear stress under different cycles is determined based on the fatigue modulus of each hysteresis loop. The result shows a fatigue enhancement phenomenon for the interface which is not observed at room temperature.     

The effects of phenolic resin-derived PyC interlayers on microstructure and mechanical properties of Cf/SiC composites

A novel, easy and cost-effective way, infiltration and pyrolysis of phenolic resin solution, was exploited to prepare pyrolytic carbon (PyC) interlayers for carbon fiber/silicon carbide (Cf/SiC) mini-composites. X-ray photoelectron spectroscopy, dynamic contact angle measurement and scanning electron microscope were carried out to characterize chemical structure of carbon fibers (CFs), wetting properties between CFs and phenolic resin solution and microstructure of CFs and their composites, respectively. Remarkably, SEM results showed regulation of uniformity and thicknesses of PyC interlayer could be achieved through controlling the concentration of phenolic resin solution and oxidation condition of CFs. When CFs were treated by 10?min' oxidation with 40?mg/L ozone followed by dip-coating with 4?wt% phenolic solution, uniform PyC interlayer with approximately 120?nm were prepared on CFs. The corresponding Cf/SiC specimens had the largest increase in tensile strength and work of fracture with the improvement of 26.2% and 71.6% from the PyC-free case.     

Mechanical properties of the SiCf/SiC composites reinforced with KD-I and KD-II fibers fabricated assisted by a microwave heating method

SiC_f/SiC composites using KD-I and KD-II SiC fibers braided preforms as the reinforcements were fabricated by applying the polymer impregnation and pyrolysis (PIP) technique with a microwave heating assistance. The microwave heating temperature was 1100 °C, 1200 °C, 1300 °C, and 1400 °C, respectively. Microstructures, flexure properties, and fracture behaviors of the composites were investigated. The KDIISiC_f/SiC composites exhibited higher flexure properties and improved non-brittle fracture characteristics than those of the KD-ISiC_f/SiC composites. The differences in the flexural properties, fracture behaviors and microstructures between the KD-I and KDIISiC_f/SiC composites were discussed based on the tensile properties of the SiC filaments and the interfacial bonding statues in the composites.     

Properties and microstructure evolution of Cf/SiC composites fabricated by polymer impregnation and pyrolysis (PIP) with liquid polycarbosilane

In the present study, a novel liquid polycarbosilane (LPCS) with a ceramic yield as high as 83% was applied to develop 3D needle-punched C_f/SiC composites via polymer impregnation and pyrolysis process (PIP). The cross-link and ceramization processes of LPCS were studied in detail by FT-IR and TG-DSC; a compact ceramic was obtained when LPCS was firstly cured at 120 °C before pyrolysis. It was found that the LPCS-C_f/SiC composites possessed a higher density (2.13 g/cm³) than that of the PCS-C_f/SiC composites even though the PIP cycle for densification was obviously reduced, which means a higher densification efficiency. Logically, the LPCS-C_f/SiC composites exhibited superior mechanical properties. The shorter length and rougher surfaces of pulled-out fibers indicated the LPCS-C_f/SiC composites to possess a stronger bonding between matrix and PyC interphase compared with the PCS-C_f/SiC composites.     

SiC and ZrN nano-particulate reinforced AlON composites: Preparation,mechanical properties and toughening mechanisms

Due to excellent chemical stability, high rigidity, superior corrosion and wear resistance, aluminum oxynitride (AlON) has been considered as one of most promising candidate ceramic materials in high-performance structural, advanced abrasives and refractory fields. However, it usually exhibited relatively low flexural strength and poor fracture toughness. The study is aimed to develop silicon carbide (SiC) and zirconium nitride (ZrN) nano-particulate reinforced AlON composites with improved mechanical properties and fracture resistance via a hot-press sintering process. It was found that the addition of ZrO₂ nanoparticles would be transformed into ZrN during sintering. Due to the pinning effect of SiC and ZrN nano-particles positioned at grain boundaries of micro-sized AlON particles, the presence of SiC and ZrN nano-particles resulted in the reduction of both porosity and grain size, and a change of fracture mode from intergranular cracking in AlON to intragranular cracking in composites. With presence of 8 wt% SiC and 5.2 wt% ZrN nano-particles, the relative density, microhardness, Young’s modulus, flexural strength and fracture toughness increased. Different toughening mechanisms including crack bridging, crack branching and crack deflection were observed, thus effectively increasing the crack propagation resistance and leading to a considerable improvement in flexural strength and fracture toughness.     

Infiltration of Al2O3/Y2O3 mix into SiC ceramic preforms

Silicon carbide ceramics are very interesting materials to engineering applications because of their properties. These ceramics are produced by liquid phase sintering (LPS), where elevated temperature and time are necessary, and generally form volatile products that promote defects and damage their mechanical properties. In this work was studied the infiltration process to produce SiC ceramics, using shorter time and temperature than LPS, thereby reducing the undesirable chemical reactions. SiC powder was pressed at 300 MPa and pre-sintered at 1550 °C for 30 min. Unidirectional and spontaneous infiltration of this preform by Al₂O₃/Y₂O₃ liquid was done at 1850 °C for 5, 10, 30 and 60 min. The kinetics of infiltration was studied, and the infiltration equilibrium happened when the liquid infiltrated 12 mm into perform. The microstructures show grains of the SiC surrounded by infiltrated additives. The hardness and fracture toughness are similar to conventional SiC ceramics obtained by LPS.     

Effect of the fabrication process on the microstructural evolution of carbon fibers and flexural property on C/SiC composites by the NITE method

Nano-infiltration and transient eutectic phase (NITE) SiC matrix composites are designed for application in aerospace propulsion systems, particularly in fasteners and thrusters. A variety of carbon fibers with different properties have been selected as reinforcements for SiC matrix composites. Carbon fibers are known to be stable at high temperatures; however, the effects of high applied pressure at high temperatures on the fiber microstructure evolution and mechanical properties are not well-known. As a scoping study for fabricating NITE C/SiC composites, the behaviors of various carbon fibers in SiC composites. Pitch-based fibers, namely, GRANOX XN-05 and YS-90A, and a polyacrylonitrile-based fiber, namely, TORAYCA T-300B, were selected for matrix reinforcement. The 3-point bending test results indicated pseudo-ductile behaviors in the cases of YS-90A and T-300B fiber reinforcements. Fracture resistance evaluation based on the single-notch bending test indicated that the YS-90A fiber reinforced composite afforded the highest fracture resistance among the three C/SiC composites. The microstructure evolution on YS-90A and T-300B fibers was limited to near the fiber surface. Therefore, YS-90A and T-300B carbon fibers are potential candidates for reinforcement in NITE C/SiC composites.     

Preparation and mechanical properties of Ti3SiC2/SiC functionally graded materials

Ti₃SiC₂/SiC functionally graded materials (FGMs) were prepared via hot-pressing sintering followed by positioning impregnation. Positioning impregnation is a novel technique for local impregnation targeted at graded layers that exhibit poor sintering behaviour. The positioning impregnation process significantly densified layers with SiC volume fractions of more than 70% while only slightly affecting the densities of the other layers and preserving sufficiently weak interfaces between layers. FGMs that were hot pressed at 1600 and 1700 °C and then subjected to impregnation showed not only high flexural strengths but also zigzag load-displacement behaviour. The flexural strengths of these FGMs were 436 and 485 MPa, respectively; in comparison, the values for the FGMs without impregnation that were hot pressed at 1600, 1700 and 1800 °C were 235, 268 and 328 MPa, respectively. Moreover, the fracture toughnesses of these FGMs were 8.23 and 7.15 MPa m^1/2, respectively; in comparison, the values for the FGMs without impregnation that were hot pressed at 1600, 1700 and 1800 °C were 6.77, 7.05 and 4.65 MPa m^1/2, respectively.     

Microstructural evolution of SiC powder in molten silicon

SiC_powder/Si_matrix composites represent a new class of microstructurally toughened materials. The interactions between molten silicon and submicronic SiC powder have been considered since it could originate some limitations on the final properties of the material. Experiments putting in interaction a SiC powder and molten Si were performed while heating up to final values ranging between 1450 and 1600?°C for duration up to 8?h. The volume ratio of SiC and silicon was equal to one and SiC particles were freely dispersed within the liquid. X-ray diffraction analyses demonstrated that the apparent crystallites size increase of SiC powder followed a ripening law corresponding to a limitation either by volume diffusion or by dissolution into the liquid. Depending on the relevant mechanism, the activation energy of the crystallites’ growth has been found equal to 357?±?50?kJ?mol^?1 or 441?±?57?kJ?mol^?1. An agglomeration-coarsening process of SiC particles was also identified which promoted a quick formation of larger particles.     

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.     

Microstructure and mechanical properties of SiC platelet reinforced BaOAl2O32SiO2 (BAS) composites

BaOAl₂O₃2SiO₂ (BAS) glass–ceramic powders were prepared by sol–gel technique. SiC platelet reinforced BAS glass–ceramic matrix composites with high density and uniform microstructure were fabricated by hot-pressing. The effect of additional crystalline seeds on hexagonal to monoclinic phase transformation of Barium aluminosilicate was studied. The effects of SiC platelet content on the microstructure and mechanical properties of the composites were also investigated. The results showed that the flexural strength and fracture toughness of the BAS glass–ceramic matrix composites can be effectively improved by the addition of silicon carbide platelets. The main toughening mechanism was crack deflection, platelets' pull-out and bridging. The increased value of flexural strength is contributed to the load transition from the matrix to SiC platelets.     

Appropriate thickness of pyrolytic carbon coating on SiC fiber reinforcement to secure reasonable quasi-ductility on NITE SiC/SiC composites

Pyrolytic carbon (PyC) coating of silicon carbide (SiC) fibers is an important technology that creates quasi-ductility to SiC/SiC composites. Nano-infiltration and transient eutectic-phase (NITE) process is appealing for the fabrication of SiC/SiC composites for use in high temperature system structures. However, the appropriate conditions for the PyC coating of the composites have not been sufficiently tested. In this research, SiC fibers, with several thick PyC coatings prepared using a chemical vapor infiltration continuous furnace, were used in the fabrication of NITE SiC/SiC composites. Three point bending tests of the composites revealed that the thickness of the PyC coating affected the quasi-ductility of the composites. The composites reinforced by 300?nm thick coated SiC fibers showed a brittle fracture behavior; the composites reinforced 500 and 1200?nm thick PyC coated SiC fibers exhibited a better quasi-ductility. Transmission electron microscope research revealed that the surface of the as-coated PyC coating on a SiC fiber was almost smooth, but the interface between the PyC coating and SiC matrix in a NITE SiC/SiC composite was very rough. The thickness of the PyC coating was considered to be reduced maximum 400?nm during the composite fabrication procedure. The interface was possibly damaged during the composite fabrication procedure, and therefore, the thickness of the PyC coating on the SiC fibers should be thicker than 500?nm to ensure quasi-ductility of the NITE SiC/SiC composites.     

Flexural modulus of SiC/SiC composites sintered by microwave and conventional heating

To deeply study the variation mechanisms of mechanical properties, flexural modulus of SiC fibers reinforced SiC matrix (SiC/SiC) composites prepared by conventional and microwave heating at 800?°C–1100?°C was discussed in detail. The elastic modulus of fibers and matrix, interface bonding strength and porosity of SiC/SiC composites were considered together to analyze the changing tendencies and differences in their flexural modulus. The elastic modulus of fiber and matrix was determined by nanoindentation technique and interface characteristics applying fiber push-out test. The porosity and microstructure examinations were characterized by mercury intrusion method, X-ray Diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscope (TEM). Moreover, two conflicts between the changing trends of elastic modulus and chemical compositions of composite components were focused and explained. Results indicate that three factors played different roles in the flexural modulus of SiC/SiC composites and residual tensile stress in composite components led to the conflicts between their elastic modulus and chemical compositions.     

Mechanical behaviour of the constituents inside carbon-fibre/carbon-silicon carbide composites characterised by nano-indentation

The Young's modulus, hardness, fracture toughness and ductility of the key constituents were characterised using nano-indentation for three types of carbon-fibre/carbon silicon carbide composite manufactured through different routes and/or using different carbonaceous raw materials. Under indentation, all of the carbon constituents demonstrated much less ductile deformation than the silicon carbide and silicon did in these composites. Between two types of PAN-based carbon fibre, as well as of pyrolytic carbon, a difference of around a factor of two was evident in the Young's modulus and hardness. For the silicon carbide, a difference of around 100 GPa and 5 GPa was recorded for the mean Young's modulus and hardness respectively; for silicon, only a small variation was evident. The estimated mean fracture toughness of the silicon carbide ranged between 0.7 and 1.2 MPa.m^1/2, whilst the silicon was approximately 0.6 MPa.m^1/2. Results for the constituents were discussed in terms of their elastic/plastic behaviour.     

Crack propagation analysis of SiCf/SiC composites by gas permeability measurement

Permeability of helium gas through the NITE-SiC_f/SiC composites after applying tensile stress was measured experimentally in a vacuum apparatus. Tensile stress equal to 1.1-1.2 times the proportional limit stress (PLS) was applied parallel to the direction of the reinforced fiber. Results of the permeability experiments revealed that the permeability rapidly increased when threshold stress was applied on the specimens. The permeability of helium gas was governed by the narrowest diameter of the permeation pathway. In the case of NITE composites, the diameter of the pathway was calculated to be below 0.65 μm. The NITE composites exhibited superior performance even when the applied stress was greater than 1.2 times the PLS. Fiber bundles considerably magnified the permeability of helium gas because of the relatively large pore size of the intra-fiber bundles. Transverse cracks propagated with increasing stress and they connected fiber bundles when the applied stress was 1.10-1.15 times the PLS.     

Effect of SiC ceramics on thermoelectric properties of SiC/SnSe composites for solid-state thermoelectric applications

Tin selenide (SnSe) based thermoelectric materials with varying amounts of embedded silicon carbide (SiC) particles were fabricated, and their thermoelectric properties were investigated. The SiC particles were evenly distributed in the SnSe matrix, thereby leading to the formation of the SiC/SnSe composite samples. The introduction of SiC into the SnSe matrix improved the power factors, owing mainly to an increase in the Seebeck coefficient, and a decrease in the thermal conductivity arising from the formation of phonon-scattering centers. Consequently, a ZT of 0.125 (at 300 K) was obtained for the SiC/SnSe composite with a SiC content of 1 wt%; this value was larger than that of the pristine SnSe. The results of this study indicate that the introduction of SiC particles into the SnSe matrix constitutes an efficient strategy for achieving thermoelectric enhancement for solid-state applications.     

Effect of thickness of SiC films on compression and thermal properties of SiC/CF composites

Commonly, carbon foam derived from commercially available melamine foam showed brittle characteristics. In this paper, the carbon foam was prepared via the direct carbonization of the melamine foam, and chemical vapor deposition was employed to deposit ultra-thin SiC films on the CF skeleton. The evolution, microstructure, mechanical strength, and thermal properties of the as-prepared SiC/CF composites were investigated. Test results showed that a novel SiC skeleton with a three-dimensional interconnected network was prepared successfully. The thickness of the SiC filmes had a significant influence on the compression and thermal properties of the composites. The SiC/CF-II possessed a higher compression performance than that of SiC/CF-I, while the thermal insulation was relatively much poorer. This present work had some reference meaning to the correlation studies of the thermal insulation material for the potential applications while bearing live loads.     

Microstructure and properties of (SiC, TiB2)/B4C composites by reaction hot pressing

(SiC, TiB₂)/B₄C composites were fabricated by reactive hot-pressing B₄C, Si₃N₄, -SiC and TiC powders, with (Al₂O₃ + Y₂O₃) as sintering additives. According to the thermodynamics principles, the possible reaction equations and the reaction products for the system were determined. By means of XRD, SEM of surface thermally etched and TEM the phase composition was determined. It was shown that the phase composition of sintered body was B₄C, -SiC, BN and TiB₂, and the matrix was B₄C and -SiC. The typical values of hardness, bending strength, fracture toughness and the relative density of the composites can reach HRA 88.6, 554 MPa, 5.6 MPa m^1/2 and 95.6%, respectively. Furthermore, the microstructures of the composites were analyzed by TEM, SEM and energy spectrum methods. The results show the presence of laminated structure and a clubbed frame dispersion phase and bunchy dispersion phase among the matrix. Some intragranular structures were also found in the B₄C grains. Microstructural analysis indicates that the new formed phase, uniform and fine grains, and the layered and clubbed structure play an important role in improving the properties of the composites. Fractography and crack propagation suggest that crack deflection and crack bridging are the possible toughening mechanisms.     

Processing and mechanical performance of 3D Cf/SiCN composites prepared by polymer impregnation and pyrolysis

The processing of 3D carbon fiber reinforced SiCN ceramic matrix composites prepared by polymer impregnation and pyrolysis (PIP) route was improved, and factors that determined the mechanical performance of the resulting composites were discussed. 3D C_f/SiCN composites with a relative density of ∼81% and uniform microstructure were obtained after 6 PIP cycles. The optimum bending strength, Young's modulus and fracture toughness of the composites were 75.2 MPa, 66.3 GPa and 1.65 MPa m^1/2, respectively. The residual strength retention rate of the as-pyrolyzed composites was 93.3% after thermal shock test at ΔT = 780 °C. It further degraded to 14.6% when the thermal shock temperature difference reached to 1180 °C. The bending strength of the composites was 35.6 MPa after annealing at 1000 °C in static air. The deterioration of the bending strength should be attributed to the strength degradation of carbon fibers and decomposition of interfacial structure.     

Microstructure and mechanical properties of hot-pressed SiC/(W,Ti)C ceramic composites

SiC/(W, Ti)C ceramic composites with different content of (W, Ti)C solid-solution were produced by hot pressing. The effect of (W, Ti)C content on the microstructure and mechanical properties of SiC/(W, Ti)C ceramic composites has been studied. Densification rates of the SiC/(W, Ti)C ceramic composites were found to be affected by addition of (W, Ti)C. Increasing (W, Ti)C content led to increase the densification rates of the composites. The sintering temperature was lowered from 2100 °C for monolithic SiC to 1900 °C for the SiC/(W, Ti)C composites. Results show that additions of (W, Ti)C to SiC matrix resulted in improved mechanical properties compared to pure SiC ceramic. The fracture toughness and flexural strength continuously increased with increasing (W, Ti)C content up to 60 vol.%, while the hardness decreased with increasing (W, Ti)C content.