Oxidation protection of C/C composites with in situ bamboo-shaped SiC nanowire-toughened Si–Cr coating

An in situ bamboo-shaped SiC nanowire-toughened Si–Cr coating was prepared on the carbon/carbon composites by pack cementation and heat treatment with ferrocene as the catalyst. The microstructures and oxidation behavior of the coating were investigated. Results showed that the coating had a dense microstructure, without the penetrating microcracks, which was primarily attributed to the unusual toughening effect of the bamboo-shaped nanowires resulting from the mechanical interlocking between the nodes and the matrix. The coating exhibited good oxidation protection ability at high temperature. The weight gain of the samples was 0.79% after isothermal oxidation at 1500 °C for 185 h.     

SiC nanowire-toughened MoSi2-SiC coating to protect carbon/carbon composites against oxidation

To protect carbon/carbon (C/C) composites against oxidation, a SiC nanowire-toughened MoSi₂-SiC coating was prepared on them using a two-step technique of chemical vapor deposition and pack cementation. SiC nanowires obtained by chemical vapor deposition were distributed random-orientedly on C/C substrates and MoSi₂-SiC was filled in the holes of SiC nanowire layer to form a dense coating. After introduction of SiC nanowires, the size of the cracks in MoSi₂-SiC coating decreased from 18 ± 2.3 to 6 ± 1.7 μm, and the weight loss of the coated C/C samples decreased from 4.53% to 1.78% after oxidation in air at 1500 °C for 110 h.     

Oxidation-protective and mechanical properties of SiC nanowire-toughened Si–Mo–Cr composite coating for C/C composites

Oxidation-protective SiC nanowire-toughened Si–Mo–Cr composite coating prepared on the carbon/carbon (C/C) composites by chemical vapor deposition and pack cementation was investigated in this study. After incorporating SiC nanowires, the hardness, elastic modulus and fracture toughness of the composite coating were increased by 6.12%, 20.89% and 35.78%, respectively, due to the toughening and strengthening mechanisms including nanowire pullout, nanowire bridging, microcrack deflection and good interaction between nanowire/matrix interface. Thermogravimetric analysis revealed that the maximum weight loss of the coated C/C samples was decreased from 5.87% to 3.93% by incorporating SiC nanowires from room temperature to 1500 °C.     

Bamboo-shaped SiC nanowire-toughened SiC coating for oxidation protection of C/C composites

An oxidation protective bamboo-shaped SiC nanowire-toughened SiC coating was prepared on the carbon/carbon composites by chemical vapor deposition and pack cementation. It is found that incorporating bamboo-shaped SiC nanowires makes the coating hardness and elastic modulus increase by 20.07% and 40.42% and microcrack density decrease by 84.04% due to their unusual toughening mechanism resulting from the nanoscale mechanical interlocking between the nodes and the surrounding matrix, resulting in a good oxidation inhibition for the coated samples. The result showed that the weight loss of the coated samples was only 0.5% after isothermal oxidation at 1500 °C for 72 h.     

Comparison of morphology and microstructure of ablation centre of C/SiC composites by oxy-acetylene torch at 2900 and 3550 °C

High-temperature application above 1600 °C of C/SiC composites requires evaluation of the ablation properties. The C/SiC composites were prepared by low pressure chemical vapor infiltration using CH₃SiCl₃ as precursor. As-prepared C/SiC composites were ablated by oxy-acetylene flame with the temperature of 2900 and 3550 °C. Above 3550 °C, subliming of carbon fiber and silicon carbide matrix was the main ablation behaviour. At 2900 °C, thermal decomposition and oxidation of SiC matrix were the main ablation behaviour. A carbon coating resulted from the pyrolysis of the acetylene prevented the C/SiC from oxidizing dramatically.     

Multilayer oxidation protective coating for C/C composites from room temperature to 1500 °C

To prevent carbon/carbon (C/C) composites from oxidation, a multilayer oxidation resistant coating was prepared. The inner SiC coating was prepared by pack cementation, and the outer SiC-MoSi₂ three-layer coating was obtained by slurry coating using silicon-sol as the caking agent. X-ray diffraction, scanning electron microscopy and energy dispersive X-ray spectroscopy were used to analyze the phase, microstructure and element distribution of the as-prepared coating. The results show that, the as-received multilayer coating has a crack-free structure with the thickness of about 300 μm. It is provided with excellent oxidation resistance from room temperature to 1500 °C in air and can protect C/C composites from oxidation for more than 120 h at 900 °C and more than 110 h at 1500 °C in air. The weight loss of the coated samples during oxidation tests mainly resulted from the oxidation of Mo₅Si₃ and the volatilization of SiO₂ in the coating.     

Influence of preparation temperature on the oxidation resistance and mechanical properties of C/SiC coated C/C composites

A C/SiC oxidation resistance coating was prepared on carbon/carbon (C/C) composites by slurry and pack cementation. The microstructure, oxidation resistance and mechanical properties of C/SiC coating prepared from 1773 to 2573 K were investigated. With the increase of the preparation temperature, the oxidation resistance of C/SiC coating increases, however, the flexure strength decreases gradually. The preparation of C/SiC coating on C/C composites results in the fracture behavior of C/C composites changing from pseudo-plastic to brittle failure model. The decrease of flexure strength is mainly attributed to the decrease of C/C matrix’ flexure strength at high temperature.     

Preparation and oxidation protection of CVD SiC/a-BC/SiC coatings for 3D C/SiC composites

An amorphous boron carbide (a-BC) coating was prepared by LPCVD process from BCl₃-CH₄-H₂-Ar system. XPS result showed that the boron concentration was 15.0 at.%, and carbon was 82.0 at.%. One third of boron was distributed to a bonding with carbon and 37.0 at.% was dissolved in graphite lattice. A multiple-layered structure of CVD SiC/a-BC/SiC was coated on 3D C/SiC composites. Oxidation tests were conducted at 700, 1000, and 1200 °C in 14 vol.% H₂O/8 vol.% O₂/78 vol.% Ar atmosphere up to 100 h. The 3D C/SiC composites with the modified coating system had a good oxidation resistance. This resulted in the high strength retained ratio of the composites even after the oxidation.     

C/SiC复合材料用莫来石/硅酸钇双层涂层的抗氧化性能研究

针对C/SiC复合材料的防氧化要求,在材料表面通过等离子喷涂法制备了莫来石/硅酸钇的双层涂层,对涂层的形貌、组成和结构及其与基底的结合强度进行了表征,开展了1500℃、1h静态空气氧化实验,对抗氧化涂层的结构演变进行了分析,并对C/SiC复合材料氧化实验前后的质量和力学性能变化进行了研究。结果表明,莫来石/硅酸钇双层涂层抗氧化作用较好,涂层C/SiC复合材料的强度保留率达95.3%。     

Oxidation protection of C/SiC coated carbon/carbon composites with Si–Mo coating at high temperature

To protect carbon/carbon (C/C) composites against oxidation, a Si–Mo coating was prepared on C/SiC-coated C/C composites by a simple slurry method. The microstructure of the coating was characterized by X-ray diffraction, scanning electron microscopy and Raman spectra. Results showed that the coating was mainly composed of SiC, MoSi₂ and Si. It could protect C/C composites from oxidation at 1873 K in air for 300 h and withstand 13 thermal cycles between room temperature and 1873 K. The excellent oxidation and thermal shock resistance of the coating was attributed to the formation of dense SiO₂ glass at high temperature. The volatilization of MoO₃ and SiO₂ at 1873 K was the main reason of the weight loss of the coated C/C composites.     

Oxidation protection of SiC-coated C/C composites by SiC nanowire-toughened CrSi2–SiC–Si coating

Oxidation protective SiC nanowire-toughened CrSi₂–SiC–Si coating was prepared on SiC-coated carbon/carbon composites by chemical vapor deposition and pack cementation. SiC nanowires in the coating suppressed the cracking of the coating via various toughening mechanisms including nanowire pullout, microcrack bridging by nanowire and microcrack deflection, resulting in a good oxidation inhibition for the coated samples. The results showed that the maximal weight loss of the coated samples was only 2.55% in thermogravimetric analysis from room temperature to 1500 °C, and the weight loss of the coated samples was only 1.24% after isothermal oxidation at 1500 °C for 316 h.     

SiC nanowire-toughened SiC-MoSi2-CrSi2 oxidation protective coating for carbon/carbon composites

To prevent carbon/carbon (C/C) composites from oxidation, a dense SiC nanowire-toughened SiC-MoSi₂-CrSi₂ multiphase coating was prepared by the two-step technique composed of chemical vapor deposition (CVD) and pack cementation. The coatings were characterized by scanning electron microscopy (SEM), energy dispersive spectroscopy (EDS) and X-ray diffraction (XRD). SiC nanowires could decrease the dimension of cracks and improve the oxidation and thermal shock resistance of SiC-MoSi₂-CrSi₂ multiphase coating. Oxidation test shows that, after introducing SiC nanowires, the weight loss of the coated sample can be reduced from 1.06% to 0.64% after oxidation at 1773 K for 155 h and decreased from 6.92% to 3.42% after thermal cycling between 1773 K and room temperature for 30 times.     

Oxidation protection and behavior of C/C composites with an in situ SiC nanowire–SiC–Si/SiC–Si coating

An in situ SiC nanowire–SiC–Si/SiC–Si protective coating was prepared on C/C composites by pack cementation and heat treatment. SiC nanowires suppressed the cracking of the coating by nanowire pullout and bridging and microcrack deflection, avoiding the oxidation of C/C composites. Results showed that the oxidation of the samples was a continuous weight gain process. The oxidation behavior was fitted to the parabolic–linear model and the final weight gain was 1.8% during thermogravimetric analysis from 50 to 1600 °C. The oxidation behavior was fitted to the parabolic model and the final weight gain was 0.51% during isothermal oxidation at 800 °C.     

C/SiC/Si-Mo-B/glass multilayer oxidation protective coating for carbon/carbon composites

To prevent carbon/carbon (C/C) composites from oxidation, a self-sealing multilayer oxidation resistant coating including a C/SiC gradient inner layer, a Si-Mo-B middle layer and a glass exterior layer was prepared by pack cementation and slurry method. Scanning electron microscopy and X-ray diffraction were used to analyze the microstructure and phase composition of the as-prepared coating. The isothermal and thermal shock oxidation resistance of the coating was also investigated. The results showed that the multilayer coating exhibited excellent oxidation resistance from room temperature to 1873 K. It could effectively protect C/C composites for 100 h at 1173 K and 150 h at 1873 K, and endure 40 thermal cycles between 1873 K and room temperature. The excellent oxidation and thermal shock resistance could be attributed to the gradient structure and the self-sealing property of the multilayer coating.     

Microstructure and anti-oxidation property of Si-W-Cr coating for SiC coated carbon-carbon composites

To protect carbon/carbon (C/C) composites from oxidation at high temperature, a Si-W-Cr coating was prepared on the surface of SiC coated C/C composites by a simple pack cementation technique. The microstructure and phase composition of the as-received multi-coating were examined by SEM, XRD and EDS. The coating obtained by first step pack cementation was porous α-SiC structure. New phases of WSi₂ and CrSi₂ together with α-SiC deposited on the porous SiC inner layer. Oxidation test shows that the weight loss of single SiC coated C/C is up to 8.21% after 9 h in air at 1773 K, while the weight loss of Si-W-Cr/SiC coated C/C composites is only 2.26% after 51 h. After thermal cycling between 1773 K and room temperature for 40 times, the weight loss is only 3.36%. The weight loss of coated C/C composites was primarily due to the reaction of C/C matrix and oxygen diffusing through the penetrable cracks in the coating.     

C/SiC/MoSi2–Si multilayer coatings for carbon/carbon composites for protection against oxidation

To improve the oxidation resistance of carbon/carbon (C/C) composites, a C/SiC/MoSi₂–Si multilayer oxidation protective coating was prepared by slurry and pack cementation. The microstructure of the as-prepared coating was characterized by scanning electron microscopy, X-ray diffraction and energy dispersive spectroscopy. The isothermal oxidation and erosion resistance of the coating was investigated in electrical furnace and high temperature wind tunnel. The results showed that the multilayer coating could effectively protect C/C composites from oxidation in air for 300 h at 1773 K and 103 h at 1873 K, and the coated samples was fractured after erosion for 27 h at 1873 K h in wind tunnel. The weight loss of the coated specimens was considered to be caused by the formation of penetration cracks in the coating. The fracture of the coated C/C composites might result from the excessive local stress in the coating.     

Microstructure and oxidation resistance of Si–Mo–B coating for C/SiC coated carbon/carbon composites

A self-sealing Si–Mo–B oxidation resistance coating was prepared on C/SiC coated carbon/carbon (C/C) composites by slurry and high temperature treatment method. The oxidation resistance of the coating increases at 1173 K and first increases then decreases at 1873 K with the increase of B content from 0 to 20 wt.%. The C/SiC/gradient Si–Mo–B multilayer coating can protect C/C composite from oxidation for 100 h at 1173 K and 125 h at 1873 K. The good oxidation resistance of the coating in broad temperature range could be attributed to its good self-sealing property.     

Oxidation and ablation resistance of ZrB2–SiC–Si/B-modified SiC coating for carbon/carbon composites

ZrB₂–SiC–Si/B-modified SiC coating was prepared on the surface of carbon/carbon (C/C) composites by two-step pack cementation. The coating could efficiently provide protection for C/C composites from oxidation and ablation. The improvement of oxidation resistance was attributed to the self-sealing property of the multilayer coating. A dense glassy oxide layer could afford the high temperature up to 2573 K and efficiently protect C/C composites from ablation.     

Si-W-Mo coating for SiC coated carbon/carbon composites against oxidation

In order to prevent carbon/carbon (C/C) composites from oxidation at 1773 K, a Si-W-Mo coating was prepared on the surface of SiC coated C/C composites by a simple pack cementation technique. The microstructures and phase composition of the as-received multi-coating were examined by SEM, XRD and EDS. It was seen that the compact multi-coating was composed of α-SiC, Si and (W_xMo_1 − x)Si_2. Oxidation behaviour of the SiC/Si-W-Mo coated C/C composites was also studied. After 315 h oxidation in air at 1773 K and thermal cycling between 1773 K and room temperature for 17times, no weight loss of the as-coated C/C composites was measured. The excellent anti-oxidation ability of the multi-coating is attributed to its dense structure and the formation of the stable glassy SiO₂ film on the coating surface during oxidation.     

Effect of SiC/ZrC ratio on the mechanical and ablation properties of C/C–SiC–ZrC composites

The effect of SiC/ZrC weight ratio on the mechanical and ablation properties of carbon/carbon composites modified by SiC nanowires reinforced SiC–ZrC ceramics (C/C–SiC–ZrC) was studied. Results showed that C/C–SiC–ZrC composites with a SiC/ZrC ratio of 1:1.5 exhibited good mechanical and ablation properties. The flexural strength and modulus were 201 ± 20 MPa and 18 ± 1 GPa, respectively. After ablation for 120 s, the linear and the mass ablation rate were 0.012 mm/s and 0.0019 g/s. The good performance is attributed to a higher density, the reinforcing effect of SiC nanowires and the proper SiC/ZrC ratio.