Effect of temperature gradient on the erosion behavior of SiC coating for carbon/carbon composites in a combustion environment

SiC coating with a thickness of 50–70 µm was prepared on the surface of C/C composites by in-situ reaction method. The SiC coated C/C composites were then tested in a wind tunnel where a temperature gradient from 200 to 1600 °C could be obtained to investigate their erosion behavior. The results of wind tunnel test indicated that the service life of C/C composites was prolonged from 0.5 to 44 h after applying the SiC coating. After the wind tunnel test, three typical oxidation morphologies, including glassy SiO₂ layer, porous SiO₂ layer and clusters of honeycomb-like SiO₂ grains, were found on the SiC coated C/C composites. With the decrease of oxidation temperature, the amount of glassy SiO₂ declined and the thermal stress increased, which induced the cracking followed by the degradation of the SiC coating.     

Siliconization elimination for SiC coated C/C composites by a pyrolytic carbon coating and the consequent improvement of the mechanical property and oxidation resistances

Carbon/carbon (C/C) composites have a wide application as the thermal structure materials because of their excellent properties at high temperatures. However, C/C composites are easily oxidized in oxygen-containing environment, which limits their potential applications to a great degree. Silicon carbide (SiC) ceramic coating fabricated via pack cementation (PC) was considered as an effective way to protect C/C composites against oxidation. But the mechanical properties of C/C composites were severely damaged due to chemical reaction between the molten silicon and C/C substrate during the preparation of SiC coating by PC. In order to eliminate the siliconization erosion, a pyrolytic carbon (PyC) coating was pre-prepared on C/C composites by the chemical vapor infiltration (CVI) prior to the fabrication of SiC coating. Due to the retardation effect of PyC coating on siliconization erosion, the flexural strength retention of the SiC coated C/C composites with PyC coating increased from 46.27 % to 107.95 % compared with the specimen without PyC coating. Furthermore, the presence of homogeneous and defect-free PyC coating was beneficial to fabricate a compact SiC coating without silicon phase by sufficiently reacting with molten silicon during PC. Therefore, the SiC coated C/C composites with PyC coating had better oxidation resistances under dynamic (between room temperature and 1773 K) and static conditions in air at different temperatures (1773?1973 K).     

Oxidation and erosion resistance of multi-layer SiC nanowires reinforced SiC coating prepared by CVD on C/C composites in static and aerodynamic oxidation environments

A multi-layer SiC nanowires reinforced SiC (SiCnws-SiC) coating was prepared in-situ on carbon/carbon (C/C) composites by three chemical vapor deposition (CVD) processes. The microstructure and phase composition of the nanowires fabricated on the first-layer SiCnws-SiC coating and the coatings were examined by SEM, TEM, and XRD. The bamboo-like SiC nanowires with a 50?nm diameter and a length of several tens of micrometers are straight, randomly orientated and distributed like a net on the first-layer SiCnws-SiC coating. The growth direction is [111], and the growth mechanism is VS. The multi-layer SiCnws-SiC coating has three layers: the thickness of the first-layer is roughly 400?µm, and the outer two layers are about 200?µm. Each layer has a sandwich structure. The isothermal oxidation and erosion resistance of the multi-layer SiCnws-SiC coating were investigated in an electrical furnace and a high temperature wind tunnel. The results indicated that the weight loss of the multi-layer SiCnws-SiC coated C/C composites was only 1.8% after oxidation in static air at 1773?K for 361?h. Further, the coated sample failed due to fracture of the coating at the clamping position (i.e. 80?mm) after erosion at 1873?K for 130?h in the wind tunnel. The weight loss of the coated C/C composites occurred due to the formation of penetrating cracks in the coating during the oxidation thermal shock. The maximum bending moment and the larger clamping force caused the coating fracture and resulted in intense oxidation of the substrate and the failure of the specimen.     

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.     

Effect of the incorporation of SiC nanowire with double protective layers on SiC coating for C/C composites

To maintain the thermal stability of SiC nanowires during SiC coating fabrication process, carbon and SiC double protective layers were covered on the surface of nanowires. And SiC nanowires with double protective layers toughened SiC coating were prepared by pack cementation. The results showed that after introducing the SiC nanowires with double protective layers, the fracture toughness of the SiC coating was increased by 88.4 %. The coating protected C/C for 175 h with a mass loss of 3.67 %, and after 51 thermal shock cycles, the mass losses of the oxidized coating were 3.96 %. The double protective layers are beneficial to improve the thermal stability of nanowires, leading to good fracture toughness and thermal shock resistance of SiC coating. SiC nanowires consume the energy of crack propagation by fracture, pullout and bridging, leading to an increase in fracture toughness.     

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.     

SiC coating with high crack resistance property for carbon/carbon composites

A novel SiC coating with a relatively high crack resistance property (crack extension force (G_C): 12.0 J·m^?2) and outstanding thermal shock resistance was achieved merely by pack cementation. Compared with the conventional SiC coating with Al₂O₃ addition (AOSC2), SiC coating with Al–B–C additions (ABSC2) possesses refined and denser microstructure owing to different effects in promoting SiC densification under different additions. Therefore, the improvement in microstructures results in superior mechanical capabilities, antioxidation performance (900 °C), and thermal shock resistance (between 1500 °C and room temperature).     

Effect of co-deposited SiC nanowires and carbon nanotubes on oxidation resistance for SiC-coated C/C composites

To protect carbon/carbon composites (C/Cs) against oxidation, SiC coating toughened by SiC nanowires (SiCNWs) and carbon nanotubes (CNTs) hybrid nano-reinforcements was prepared on C/Cs by a two-step technique involving electrophoretic co-deposition and reactive melt infiltration. Co-deposited SiCNWs and CNTs with different shapes including straight-line, fusiform, curved and bamboo dispersed uniformly on the surface of C/Cs forming three-dimensional networks, which efficiently refined the SiC grains and meanwhile suppressed the cracking deflection of the coating during the fabrication process. The presence of SiCNWs and CNTs contributed to the formation of continuous glass layer during oxidation, while toughed the coating by introducing toughing methods such as bridging effect, crack deflection and nanowire pull out. Results showed that after oxidation for 45 h at 1773 K, the weight loss percentage of SiC coated specimen was 1.35%, while the weight gain percentage of the SiCNWs/CNTs reinforced SiC coating was 0.03052% due to the formation of continuous glass layer. After being exposed for 100 h, the weight loss percentage of the SiCNWs/CNTs reinforced SiC coating was 1.08%, which is relatively low.     

Improved thermal conductivity and mechanical properties of SiC/SiC composites using pitch-based carbon fibers

Pitch-based carbon fibers were assembled in horizontal and thickness directions of SiC/SiC composites to form three-dimensional heat conduction networks. The effects of heat conduction networks on microstructures, mechanics, and thermal conductivities were investigated. The results revealed the benefit of introducing heat conduction networks in the densification of composites. The maximum bending strength and interlaminar shear strength of the modified composites reached 568.67 MPa and 68.48 MPa, respectively. These values were equivalent to 18.6% and 69.4% increase compared to those of composites without channels. However, channels in thickness direction destroyed the continuity of fibers and matrix, creating numerous defects. As the volume fraction of heat conduction channels rose, the pinning strengthening effect of channels and influence of defects competed with each other to result in first enhanced mechanical properties followed by a decline. The in-plane thermal conductivity was found anisotropic with a maximum value reaching 86.20 W/(m·K) after introducing pitch-based carbon unidirectional tapes. The thermal conductivity in thickness direction increased with volume fraction of pitch-based carbon fibers and reached 19.13 W/(m·K) at 3.87 vol% pitch-based carbon fibers in the thickness direction. This value was 90.75% higher than that of composites without channels.     

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.     

Tribological performance of SiC coating for carbon/carbon composites at elevated temperatures

SiC coating was deposited on carbon/carbon (C/C) composites by chemical vapor deposition (CVD). The effects of elevated temperatures on tribological performance of SiC coating were investigated. The related microstructure and wear mechanism were analyzed. The results show that the as-deposited SiC coating consists of uniformity of β-SiC phase. The mild abrasive and slight adhesive wear were the main wear mechanisms at room temperature, and the SiC coating presented the maximum friction coefficient and the minimum wear rate. Slight oxidation of debris was occurred when the temperature rose to 300?°C. As the temperature was above 600?°C, dense oxide film formed on the worn surface. The silica tribo-film replaced the mechanical fracture and dominated the frication process. However, the aggravation of oxidation at elevated temperatures was responsible for the decrease of friction coefficient and the deterioration of wear rate. The SiC coating presented the minimum friction coefficient and the maximum wear rate when the temperature was 800?°C.     

SiC nanowire-toughened MoSi2-WSi2-SiC-Si multiphase coating for improved oxidation resistance of C/C composites

To improve the oxidation resistance of carbon/carbon (C/C) composites at high temperature, a SiC nanowire-toughened MoSi₂-WSi₂-SiC-Si multiphase coating was prepared by chemical vapor deposition (CVD) and pack cementation. The microstructure, mechanical properties and oxidation resistance of the coating were investigated. After the introduction of SiC nanowires, the elastic modulus, hardness, and fracture toughness of the MoSi₂-WSi₂-SiC-Si coating were increased by 25.48%, 4.09% and 45.03%, respectively. The weight loss of the coated sample with SiC nanowires was deceased from 4.83–2.08% after thermal shock between 1773 K and room temperature for 30 cycles and the weight loss is only 3.24% after isothermal oxidation at 1773 K in air for 82 h. The good oxidation resistance of the coating is mainly attributed to that SiC nanowires can effectively inhibit the propagation of cracks in the coating by the toughening mechanisms including bridging and pull-out.     

Effect of SiC coating and heat treatment on the thermal radiation properties of C/SiC composites

The effects of SiC coating and heat treatment on the emissivity were investigated for 2D C/SiC composites prepared by CVI in the 6–16 μm range. SiC coating had an obvious effect on the spectral emissivity of the composites but caused just 5% difference in the total emissivity. A radiation transport model was applied to explain those changes caused by SiC coating. Heat treatment affected the thermal radiation properties of the composites through the microstructure evolution. Base on the complementary analytical techniques, the changes in the emissivity were attributed to a good graphitization degree of carbon phases, large β-SiC grain sizes and high α-SiC content resulting in high emissivity.     

Effect of SiC interphase on the mechanical,high-temperature dielectric and high-temperature microwave absorption properties of the SiCf/SiC/Mu composites

In this study, SiC interphase was prepared via a precursor infiltration-pyrolysis process, and effects of dipping concentrations on the mechanical, high-temperature dielectric and microwave absorption properties of the SiC_f/SiC/Mu composites had been investigated. Results indicated that different dipping concentrations influenced ultimate interfacial morphology. The SiC interphase prepared with 5 wt% PCS/xylene solution was smooth and homogeneous, and no bridging between the fiber monofilament could be observed. At the same time, SiC interphase prepared with 5 wt% PCS/xylene solution had significantly improved mechanical properties of the composite. In particular, the flexural strength of the composite prepared with 5 wt% PCS/xylene solution reached 281 MPa. Both ε′ and ε′′ of the SiC_f/SiC/Mu composites were enhanced after preparing SiC interphase at room temperature. The SiC_f/SiC/Mu composite prepared with 5 wt% PCS/xylene solution showed the maximum dielectric loss value of 0.38 at 10 GHz. Under the dual action of polarization mechanism and conductance loss, both ε′ and ε′′ of the SiC_f/SiC/Mu composites enhanced as the temperature increased. At 700 °C, the corresponding bandwidth (RL ≤ ?5 dB) of SiC_f/SiC/Mu composites prepared with 5 wt% PCS/xylene solution can reach 3.3 GHz at 2.6 mm. The SiC_f/SiC/Mu composite with SiC interphase prepared with 5 wt% PCS/xylene solution is expected to be an excellent structural-functional material.     

Ti3SiC2 interphase coating in SiCf/SiC composites: Effect of the coating fabrication atmosphere and temperature

The SiC fibers were coated with Ti₃SiC₂ interphase by dip-coating. The Ti₃SiC₂ coated fibers were heat-treated from 900 °C to 1100 °C in vacuum and argon atmospheres to comparatively analyze the effect of temperature and atmosphere on the microstructural evolution and mechanical strength of the fibers. The results show that the surface morphology of Ti₃SiC₂ coating is rough in vacuum and Ti₃SiC₂ is decomposed at 1100 °C. However, in argon atmosphere, the surface morphology is smooth and Ti₃SiC₂ is oxidized at 1000 °C and 1100 °C. At 1100 °C, Ti₃SiC₂ oxidized to form a thin layer of amorphous SiO₂ embedded with TiO₂ grains. Meanwhile, defects and pores appeared in the interphase scale. As a result, the fiber strength treated in the argon was lower than that treated in vacuum. The porous Ti₃SiC₂ interphase fabricated under vacuum was then employed to prepare the SiC_f/SiC mini composite by chemical vapor infiltration (CVI) combined with precursor infiltration pyrolysis (PIP), and can effectively improve the toughness of SiC_f/SiC mini composite. The propagating cracks can be deflected within the porous interphase layer, which promotes fiber pull-outs under the tensile strength.     

Effect of oxidation and residual stress on mechanical properties of SiC seal coated C/SiC composite

The effect of oxidation and thermal residual stress on mechanical properties of SiC seal coated C/SiC composite at ambient temperature and high temperature were studied. The oxidation of SiC seal coated C/SiC composite at 1300 and 1500 °C resulted in carbon fibres burn area near through thickness micro cracks in the SiC seal coating. With the increase in exposure time, the formation of SiO₂ layer in SiC matrix near carbon fibres burns area was found. Residual mechanical properties of SiC seal coated C/SiC composite after exposure in air show significant degradation. First time, a continuous measurement of Young's modulus with temperature of C/SiC composite was carried out using an impulse excitation technique. The effect of relaxation of thermal residual stress on mechanical properties was observed with the help of continuous measurement of Young's modulus as a function of temperature in an inert atmosphere.     

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.     

Microstructures and oxidation behaviors of Al-modified and Al2O3-modified SiC coatings on carbon/carbon composites via pack cementation

Al₂O₃-modified SiC (AOSC) and Al-modified SiC (ASC) coatings were prepared on carbon/carbon (C/C) composites by one-time pack cementation (PC). Their microstructures and anti-oxidation performances were studied. Compared with ASC coating, AOSC coating shows more conspicuous defects (micro-cracks and holes) and lower densification. ASC coating can offer better oxidation resistance and thermal shock resistance to C/C composites than AOSC coating. Al additive can more efficiently improve the sinterability of SiC, which causes the above results. Besides, Al₂O₃ oxidation product is more stable than SiO₂ (l) of oxidized SiC at 1500 °C based on the thermodynamic analysis.     

Effects of SiC/HfC ratios on the ablation and mechanical properties of 3D Cf/HfC-SiC composites

Effects of SiC/HfC ratios on the ablation and mechanical properties of 3D C_f/HfC–SiC composites by precursor impregnation and pyrolysis (PIP) process were investigated systematically. Both strength (flexural and compressive strength) and modulus increase as the SiC/HfC ratio are improved. The compact and stiff HfC-SiC matrix in addition to the carbon fiber and PyC interphase with less reaction damage accounts for the improved mechanical properties of C_f/HfC-SiC with higher SiC/HfC ratios. Meanwhile, both weight loss and erosion depth of C_f/HfC-SiC are improved with the increased SiC/HfC ratios. Therefore, in order to balance the ablation and mechanical properties, an appropriate SiC/HfC ratio should be considered.