Low-surface-temperature jump behavior of C/SiC composites prepared via precursor impregnation and pyrolysis in high-enthalpy plasma flows

The response of C/SiC composites prepared via precursor impregnation and pyrolysis was investigated in a 1 MW plasma wind tunnel. Under a considerable aero heating of up to 26.2 MJ/kg of specific total enthalpy, the samples were exposed to heat fluxes exceeding 5.7 MW/m² and low pressures of 4.5–6.6 kPa. The samples were able to withstand low heat fluxes and low stagnation pressures, and their carbon-rich nature improved the thermal conductivity, presenting a low steadystate surface temperature. However, a spontaneous jump in the surface temperature at around 1700 °C was observed at high heat fluxes and high stagnation pressures. The jump temperature was lower compared with that reported in previous studies, and was found to increase rapidly to temperatures above 2000 °C. This low-temperature jump phenomenon was associated with the evolution of microstructure during testing, and the underlying mechanism was revealed through the use of thermodynamics analysis.     

Effect of in situ grown SiC nanowires on microstructure and mechanical properties of C/SiC composites

Hexagonal-shaped SiC nanowires were in situ formed in C/SiC composites with ferrocene as catalyst in the densification process of polymer impregnation and pyrolysis. The effect of SiC nanowires on microstructure and properties of the composites were studied. The results show that the in situ formed SiC nanowires were hexagonal, mostly with diamer of about 250 nm, and grew by the vapor–liquid–solid (VLS) mechanism. The C/SiC composite with nanowires shows higher bulk density and flexural strength than the one with no SiC nanowires, and the high temperature flexural strength behavior of C/SiC composites with SiC nanowires was evaluated.     

Processing of Cf/SiC composites by hot pressing using polymer binders followed by polymer impregnation and pyrolysis

Continuous carbon fiber (C_f) reinforced silicon carbide (SiC) matrix composite (C_f/SiC) was processed through hot pressing (HP) using polycarbosilane (PCS) in matrix and polysilazane in interphase regions as polymer binders. HP experiments were conducted at 4 MPa, 1200 °C and 1 h; followed by PCS polymer impregnation and pyrolysis (PIP) at 1200 °C under vacuum. The BN/SiC-Si₃N₄ interphase formed on the C_f cloth during BN dispersed polysilazane polymer coating and pyrolysis. The influence of PCS quantity during HP experiments on C_f/SiC composites was studied. Results suggest that sintering of SiC matrix in C_f/SiC composite improves by increasing PCS content during HP; however, high PCS content increases the liquidity of SiC-PCS mixture to flow out of the composite structure. The C_f/SiC composites with relative density ranging from 79 to 83% and flexural strength from 67 to 138 MPa was achieved.     

Mechanical properties degradation and microstructure evolution of 2D-SiCf / SiC composites in combustion gas environment

Based on the turbine high-temperature combustion gas simulation test platform, the long-term combustion gas environment exposure test of the 2D plain woven SiC_f/BN/SiC composites under two combustion conditions was carried out. Uniaxial tensile test, fracture morphology characterization and non-destructive testing analysis revealed the degradation and microstructure evolution of composites after exposure to combustion gas environment. The results show that the degradation of 2D-SiC_f/SiC composites after exposure to combustion gas environment is manifested as a decrease in static toughness, and the interphase transition is the mesoscopic cause of the decrease in static toughness of the composite.     

Microstructural evolution and mechanical performances of SiC/SiC composites by polymer impregnation/microwave pyrolysis (PIMP) process

SiC/SiC composites were prepared by polymer impregnation/microwave pyrolysis (PIMP) process, and their microstructural evolution and the mechanical performances were characterized. Using non-coated Tyranno SA fiber preforms as reinforcement and impregnation with only allylperhydropolycarbosilane (AHPCS) into the preforms, Tyranno SA/SiC composite (TSA/SiC) with higher density was obtained. While using carbon-coated Tyranno SA fiber preforms, Tyranno SA/C/SiC composite (TSA/C/SiC) with lower density were also fabricated. In this composite, SiC particulate was loaded with polymer precursor (AHPCS) in the first cycle impregnation. Microstructural observation revealed that pore and crack formation was affected by processing conditions. Bending strength was also dependent on the microstructural evolution of the samples. In TSA/SiC composite, relatively strong interfaces contribute to effective load transfer so that higher bending strength could be reached. In the TSA/C/SiC composite, weak interfaces provide a relatively lower strength. Meanwhile, different microstructural evolution and interfacial properties of the composites lead to the variation of the fracture behaviors.     

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.     

Effects of CVI SiC amount and deposition rates on properties of SiCf/SiC composites fabricated by hybrid chemical vapor infiltration (CVI) and precursor infiltration and pyrolysis (PIP) routes

The SiC_f/SiC composites have been manufactured by a hybrid route combining chemical vapor infiltration (CVI) and precursor infiltration and pyrolysis (PIP) techniques. A relatively low deposition rate of CVI SiC matrix is favored ascribing to that its rapid deposition tends to cause a ‘surface sealing’ effect, which generates plenty of closed pores and severely damages the microstructural homogeneity of final composites. For a given fiber preform, there exists an optimized value of CVI SiC matrix to be introduced, at which the flexural strength of resultant composites reaches a peak value, which is almost twice of that for composites manufactured from the single PIP or CVI route. Further, this optimized CVI SiC amount is unveiled to be determined by a critical thickness t₀, which relates to the average fiber distance in fiber preforms. While the deposited SiC thickness on fibers exceeds t₀, closed pores will be generated, hence damaging the microstructural homogeneity of final composites. By applying an optimized CVI SiC deposition rate and amount, the prepared SiC_f/SiC composites exhibit increased densities, reduced porosity, superior mechanical properties, increased microstructural homogeneity and thus reduced mechanical property deviations, suggesting a hybrid CVI and PIP route is a promising technique to manufacture SiC_f/SiC composites for industrial applications.     

Wear behavior of SiC nanowire-reinforced SiC coating for C/C composites at elevated temperatures

To improve the wear resistance of SiC coating on carbon/carbon (C/C) composites, SiC nanowires (SiCNWs) were introduced into the SiC wear resistant coating. The dense SiC nanowire-reinforced SiC coating (SiCNW-SiC coating) was prepared on C/C composites using a two-step method consisting of chemical vapor deposition and pack cementation. The incorporation of SiCNWs improved the fracture toughness of SiC coating, which is an advantage in wear resistance. Wear behavior of the as-prepared coatings was investigated at elevated temperatures. The results show that the wear resistance of SiCNW-SiC coating was improved significantly by introducing SiC nanowires. It is worth noting that the wear rate of SiCNW-SiC coating was an order of magnitude lower than that of the SiC coating without SiCNWs at 800 °C. The wear mechanisms of SiCNW-SiC coating at 800 °C were abrasive wear and delamination. Pullout and breakage of SiC grains resulted in failure of SiC coating without SiCNWs at 800 °C.     

High-performance 3D SiC/PyC/SiC composites fabricated by an optimized PIP process with a new precursor and a thermal molding method

To improve the efficiency of the polymer impregnation and pyrolysis (PIP) process and the mechanical properties for SiC/SiC composites, 3-dimensional (3D) SiC/SiC were fabricated by a PIP process with a new precursor polymer and the thermal molding method. Liquid polyvinylcarbosilane (LPVCS) with active Si–H and –CHåCH₂ groups was adopted as the SiC matrix precursor. The SiC/SiC composites with superior mechanical properties were efficiently fabricated. The fiber volume of the SiC/SiC was 50.4%. The bulk density and porosity of the SiC/SiC composites were 2.16 g cm⁻³ and 15.4% respectively. The flexural strength and fracture toughness of the SiC/SiC composites were 637.5 MPa and 29.8 MPa m^1/2 respectively. The influences of LPVCS and molding pressure on the performances of the SiC/SiC composites were discussed in-depth.     

Effect of processing technology on structural stability of SiC/SiBCZr ceramic matrix composites

SiC/SiBCZr composites were prepared through polymer impregnation and pyrolysis process using the second generation SiC fibers as raw material. The effects of surface substrate removal, secondary densification, and deposition coating on the structure, mechanical properties, and high temperature stability of SiC/SiBCZr composites were investigated. Results showed that the porosity of SiC/SiC composites could be greatly diminished by the optimized treatment process, and the surface of SiC/SiBCZr composites is uniformly filled into the pores by β-SiC particles, thereby achieving the sealing effect. Meanwhile, the as-prepared SiC/SiBCZr composites had excellent high temperature structural stability. At the later stage of oxidation reaction, borosilicate oxidation products with moderate fluidity, fluid lava form and self repairing function generated from ceramic matrix can effectively inhibit the oxidation reaction and improve the high temperature structural stability of SiC/SiBCZr composites. The above-mentioned high temperature structural stability provided the foundation and technical support for improving the service life and expanding the application of SiC/SiBCZr composites.     

Joining of C/SiC composites by spark plasma sintering technique

CVD–SiC coated C/SiC composites (C/SiC) were joined by spark plasma sintering (SPS) by direct bonding with and without the aid of joining materials. A calcia-alumina based glass–ceramic (CA), a SiC + 5 wt% B₄C mixture and pure Ti foils were used as joining materials in the non-direct bonding processes. Morphological and compositional analyses were performed on each joined sample. The shear strength of joined C/SiC was measured by a single lap test and found comparable to that of C/SiC.     

Oxidation behaviour of SiC ceramic coating for C/C composites prepared by pressure-less reactive sintering in wet oxygen: Experiment and first-principle simulation

SiC ceramic coating, for prevention of C/C composites against oxidation, was prepared by pressure-less reactive sintering to investigate the oxidation behaviour in an oxidising environment containing water vapour at 1773 K. The experimental results demonstrated that the oxidation behaviour of porous SiC ceramics could be divided into two stages, following the parabolic model, which was attributed to the variation in the contact area involved in the oxidation reactions. During the entire oxidation process, water vapour could accelerate the oxidation of the SiC ceramics, according to the weight change. By first-principle calculations, the accelerated oxidation rate of the SiC ceramics was attributed to weakened Si–O and Al–O bonds in the formed glassy scale, which were caused by hydroxide radicals from the water. Atomic thermal motions at high temperature could lead to the breakage of the network structure, promoting the diffusion and solution of oxidising gases. When the as-prepared SiC ceramics were applied as anti-oxidative coatings for the C/C composites, the SiC ceramic coating and C/C matrix could be sealed and protected faster per unit time, because water vapour was beneficial to the formation of a glassy layer. The weight loss of the C/C matrix could be attributed to unsealed microcracks inside the SiC coating in the initial stage.     

Significance of modification of slurry infiltration process for the precursor impregnation and pyrolysis process of SiCf/SiC composites

Several intermediate steps were applied before the precursor infiltration and pyrolysis process to improve the infiltration of SiC slurry for promoting the infiltration of SiC slurry into fiber voids. These steps include sonication, popping, electrophoretic deposition, vacuum infiltration and cold isostatic pressing (CIP). The intermediate processes, especially popping and CIP, had a beneficial effect on green density enhancement and improving the homogeneous infiltration of the slurry into fiber fabrics. The density of the SiC_fiber/SiC_filler green body was 2.20 g/cm³, which corresponded to 68 % of relative density. The SiC_f/SiC composite has a high density of 2.65 g/cm³ after seven PIP cycles.     

Oxidation degradation and mechanical reduction on C/SiC composites with artificial notch defects

Continuous carbon fiber reinforced silicon carbide matrix composites (C/SiCs) have been widely used in aeronautic and astronautic fields because of their more attractive high temperature properties with less structural weight. However, reinforcing carbon fibers are susceptible to oxidation especially when the notch defects (ND) expose them to air. Mechanical tests, microstructural characterization combined with computed tomography (CT) were performed to explore the effect of the ND on the oxidation behavior and residual properties of the C/SiCs. Results showed that, before oxidation, the remaining bending strengths of the C/SiCs with even 5 ND numbers maintained still above 93%, indicating that increase of the ND numbers had little effect on mechanical properties. However, after oxidation at 700 °C, weight loss ratio of the C/SiCs with the ND numbers of 0, 1, 3 and 5 increased from 1.01% to 3.73%. It suggested that the more the ND numbers, the greater the proportion of carbon fiber exposed to air, and the less the oxidation resistance. Meanwhile, the residual bending strength remaining ratio of the C/SiCs largely reduced from 83.7% to 60.7% with the increase of ND numbers. It pointed out that the ND induced oxidation degradation of the reinforcing fiber caused higher sensitivity to the mechanical strength of the C/SiCs, and with the increase in the ND numbers, the strengths decreased more obviously.     

Cyclic ablation behavior and microstructure evolution of multi-layer coating on C/C composites under oxyacetylene torch

The cyclic ablation resistance of coated carbon/carbon (C/C) composites play crucial roles in their further engineering applications and development due to the cyclic ablation environment accompanied by rapid heating and cooling and high-speed heat flow scouring, which can reflect the performance stability of the coating. In this research, a (SiC/HfC)₄/SiC (SHS) multi-layer coating was prepared on C/C composites. Compared with single layer (SiC and HfC coating) coated sample, the mass and linear ablation rate of SHS coated sample after three ablation cycles (60 s × 3) were only 0.64 mg/s and 0.53 μm/s, respectively. This is mainly because the introduction of many interfaces inhibits the propagation of cracks, the irregular cracks region only exists in the outer layer. Besides, the oxide layer with dense structure was formed near the C/C substrate, which could prevent oxygen from penetrating into the coating and continue to play a protective role.     

Ablation behavior of C/C-ZrC and C/SiC-ZrC composites fabricated by a joint process of slurry impregnation and chemical vapor infiltration

C/C-ZrC and C/SiC-ZrC composites were fabricated by a joint process of slurry impregnation and chemical vapor infiltration, in which ZrC matrix was obtained by slurry impregnation process, while C or SiC matrix was introduced by chemical vapor infiltration process. The as fabricated C/C-ZrC and C/SiC-ZrC composites have densities of 1.67 g cm^?3 and 1.91 g cm^?3 respectively. Tensile strength is 89.4±8.4 MPa and 182.2±14.0 MPa respectively for the as prepared C/C-ZrC and C/SiC-ZrC. Ablation behavior of the C/C-ZrC and C/SiC-ZrC composites under air plasma was studied and compared in detail. Due to different oxidation resistance and heat transfer capacity of the matrix, these two ZrC based composites showed various ablation behavior. The linear erosion rate is 48 µm s^?1 and 39 µm s^?1 respectively for C/C-ZrC and C/SiC-ZrC composites.     

Significant improvement of resistance to dry/water oxygen corrosion at medium and high temperatures of SiC/SiC composites upon matrix modification by Ca-Y-Al-Si-O microcrystalline glass

Matrix modification is of great significance for the densification of CVI-SiC/SiC, as well as the improvement of self-healing and oxidation resistance. A eutectic component of Y₂O₃-Al₂O₃-SiO₂ system modified with CaO (CYAS) was used in this study to modify SiC/SiC at 1400 °C. The oxidation behaviour of the composites was investigated under dry/water oxygen atmosphere at 900 °C and 1300 ℃. Compared to the relatively dense SiC/SiC, the modified SiC/SiC showed a slight increase in flexural strength and fracture toughness at room temperature, as well as a significant increase in oxidation resistance and densification. Our work provides a low-cost, simple-to-operate, short-cycle densification method for CVI-SiC/SiC composites that increases their oxidation resistance without compromising their mechanical properties at room temperature.     

Effect of off-axis angle on mesoscale deformation and failure behavior of plain-woven C/SiC composites with digital image correlation

In this study, the deformation response and failure behavior of a plain-woven C/SiC composite were investigated under on-axis and off-axis tensile loading. Digital image correlation (DIC) was utilized to characterize the full-field deformation and mesoscale strain distribution. The test results indicate a strong influence of the woven architecture on the mechanical properties and strain distribution, and the materials exhibit failure modes dependent on the loading directions or off-axis angles: the fracture positions of different layers are the same under off-axial load, while for on-axil loading, the fracture positions of different layers do not affect each other. SEM results provide direct evidence that the width of the off-axis specimen has a great influence on the mechanical properties. The reduction of the modulus and strength of off-axis specimen, is not only due to the off-axis loading, but also due to the reduction of effective bearing area or effective bearing fiber.     

Oxidation behavior of SiC/glaze-precursor coating on carbon/carbon composites

In order to improve the oxidation behavior of carbon/carbon composites in a wide range of temperature, a new SiC/glaze-precursor coating was developed.The SiC layer was produced by slurry and sintering, while the glaze precursor layer was prepared by slurry and drying. The microstructures and phase compositions of the coating were analyzed by SEM and XRD, respectively. The oxidation resistance of the coated composites was investigated using both isothermal and temperature-programmed thermogravimetric analysis in the temperature range from room temperature to 1600 °C. The results showed that the oxidation behavior of the coating was mainly controlled by the diffusion of oxygen during the test.The coating showed excellent oxidation resistance and self-healing ability in a wide range of temperature.     

Mechanical and dielectric properties of SiCf/SiC composites fabricated by PIP combined with CIP process

2D KD-1 SiC fiber fabrics were employed to fabricate SiC_f/SiC composites by an improved polymer infiltration and pyrolysis (PIP) process, combined with cold isostatic pressing (CIP). The effect of CIP process on the microstructure, mechanical and dielectric properties of SiC_f/SiC composites was investigated. The infiltration efficiency was remarkably improved with the introduction of CIP process. Compared to vacuum infiltration, the CIP process can effectively increase the infiltrated precursor content and decrease the porosity resulting in a dense matrix. Thus SiC_f/SiC composites with high density of 2.11 g cm⁻³ and low porosity of 11.3% were obtained at 100 MPa CIP pressure, together with an increase of the flexural strength of the composites from 89 MPa to 213 MPa. Real part (ε′) and the imaginary part (ε″) of complex permittivity of SiC_f/SiC composites increase and vary from 11.7-i9.7 to 15.0-i12.8 when the CIP pressure reaches 100 MPa.