A ZrSiO4/SiC oxidation protective coating for carbon/carbon composites

In order to improve the oxidation resistance of carbon/carbon (C/C) composites, a ZrSiO₄ coating on SiC pre-coated C/C composites was prepared by a hydrothermal electrophoretic deposition process. Phase compositions and microstructures of the as-prepared ZrSiO₄/SiC coating were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and energy dispersive spectrometer (EDS). The anti-oxidation property and failure mechanism of the multi-layer coating were investigated. Results show that hydrothermal electrophoretic deposition is an effective route to prepare crack-free ZrSiO₄ outer coatings. The multi-layer coating obviously exhibits two-layer structure. The inner layer is composed of SiC phase and the outer layer is composed of ZrSiO₄ phase. The bonding strength between the outer layer coatings and C/C–SiC substrate are 30.38 MPa. The ZrSiO₄/SiC coating displays excellent oxidation resistance and can protect C/C composites from oxidation at 1773 K for 332 h with a mass loss rate of only 0.48 × 10^− 4 g/cm²·h. The mechanical properties of the specimens are 84.36 MPa before oxidation and 68.29 MPa after oxidation. The corresponding high temperature oxidation activation energy of the coated C/C composites at 1573–1773 K is calculated to be 119.8 kJ/mol. The oxidation process is predominantly controlled by the diffusion rate of oxygen through the ZrSiO₄/SiC multi-coating. The failure of the coating is due to the formation of penetrative holes between the SiC bonding layer and the C/C matrix at 1773 K.     

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.     

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.     

A MoSi2-SiC-Si oxidation protective coating for carbon/carbon composites

To protect carbon/carbon (C/C) composites from oxidation, a dense coating has been produced by a two-step pack cementation technique. XRD and SEM analysis shows that the as-obtained coating was composed of MoSi₂, SiC and Si with a thickness of 80-100 μm. The MoSi₂-SiC-Si coating has excellent anti-oxidation property, which can protect C/C composites from oxidation at 1773 K in air for 200 h and the corresponding weight loss is only 1.04%. The weight loss of the coated C/C composites is primarily due to the reaction of C/C substrate and oxygen diffusing through the penetration cracks in the coating.     

A MoSi2/SiC oxidation protective coating for carbon/carbon composites

To protect carbon/carbon (C/C) composites against oxidation, a MoSi₂ outer coating was prepared on pack-cementation SiC coated C/C composites by a hydrothermal electrophoretic deposition. The phase composition, microstructure and oxidation resistance of the prepared MoSi₂/SiC coatings were investigated. Results show that hydrothermal electrophoretic deposition is an effective route to achieve crack-free MoSi₂ outer coatings. The MoSi₂/SiC coating can protect C/C composites from oxidation at 1773 K for 346 h with a weight loss of 2.49 mg cm⁻² and at 1903 K for 88 h with a weight loss of 5.68 mg cm⁻².     

Microstructure and oxidation of multi-layer MoSi2-CrSi2-Si coatings for SiC coated carbon/carbon composites

Multi-layer MoSi₂-CrSi₂-Si anti-oxidation coatings with different compositional ratios were prepared on the surface of SiC coated carbon/carbon (C/C) composites by a two-step pack cementation method. The microstructure and anti-oxidation performance of the coating were studied. The results show that the multi-layered coatings could protect the C/C composites from oxidation in air at 1773 K for 1000 h or 1873 K for 750 h, respectively. The anti-oxidation performance of the multi-layer MoSi₂-CrSi₂-Si coating is mainly attributed to their dense and microcrack-free structure, appropriate thermal expansion coefficient and the well dispersed MoSi₂ and CrSi₂ 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.     

SiC/SiC–YAG–YSZ oxidation protective coatings for carbon/carbon composites

SiC/SiC–YAG–YSZ coatings were prepared by pack cementation, chemical vapor deposition and slurry painting on carbon/carbon (C/C) composites. The microstructures and oxidation behavior of coatings were investigated. The results show that the coatings displayed good oxidation and thermal shock resistance due to a dense glassy layer with silicates formed on the coating of SiC–YAG–YSZ. The weight gain rate of coated C/C composites was 1.77% after oxidation for 150 h at 1773 K. SiC in outer coating can promote the formation of oxygen diffusion barrier and lead to the optimum oxidation resistance for the coatings, compared with YSZ and YAG.     

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.     

ZrSiO4 Oxidation Protective Coating for SiC-Coated Carbon/Carbon Composites Prepared by Supersonic Plasma Spraying

To protect carbon/carbon (C/C) composites against oxidation, ZrSiO₄ oxidation protective coating was prepared on SiC-coated C/C composites by supersonic plasma spraying. X-ray diffraction and scanning electron microscopy were used to analyze the phase and microstructure of the coating. The results show that the as-prepared ZrSiO₄ coating is continuous and well bonded with the SiC inner layer without penetrating crack, which exhibits good oxidation-resistant properties. After oxidation at 1773 K in air for 97 h and nine thermal shock cycles between 1773 K and room temperature, the weight loss of the coated C/C composites was only 0.08%. The excellent oxidation-resistant properties of the coating were attributed to its dense structure and the formation of the stable ZrO₂-SiO₂ glassy mixture on the surface of ZrSiO₄ coating.     

Anti-oxidation properties of ZrB2 modified silicon-based multilayer coating for carbon/carbon composites at high temperatures

To improve the anti-oxidation ability of silicon-based coating for carbon/carbon (C/C) composites at high temperatures, a ZrB₂ modified silicon-based multilayer oxidation protective coating was prepared by pack cementation. The phase composition, microstructure and oxidation resistance at 1773, 1873 and 1953 K in air were investigated. The prepared coating exhibits dense structure and good oxidation protective ability. Due to the formation of stable ZrSiO₄–SiO₂ compound, the coating can effectively protect C/C composites from oxidation at 1773 K for more than 550 h. The anti-oxidation performance decreases with the increase of oxidation temperature. The mass loss of coated sample is 2.44% after oxidation at 1953 K for 50 h, which is attributed to the decomposition of ZrSiO₄ and the volatilization of SiO₂ protection layer.     

Double SiC coating on carbon/carbon composites against oxidation by a two-step method

To improve the oxidation resistance of C/C composites, a double SiC protective coating was prepared by a two-step technique. Firstly, the inner SiC layer was prepared by a pack cementation technique, and then an outer uniform and compact SiC coating was obtained by low pressure chemical vapor deposition. The microstructures and phase compositions of the coatings were characterized by SEM, EDS and XRD analyses. Oxidation behaviour of the SiC coated C/C composites was also investigated. It was found that the double SiC coating could protect C/C composites against oxidation at 1773 K in air for 178 h with a mass loss of 1.25%. The coated samples also underwent thermal shocks between 1773 K and room temperature 16 times. The mass loss of the coated C/C composites was only 2.74%. Double SiC layer structures were uniform and dense, and can suppress the generation of thermal stresses, facilitating an excellent anti-oxidation coating.     

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.     

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.     

TaSi2 Oxidation Protective Coating for SiC Coated Carbon/Carbon Composites

为提高碳/碳复合材料在高温下的氧化防护性能,利用包埋技术在碳/碳复合材料表面制备了TaSi2/SiC复合涂层。通过XRD、SEM 和 EDS分析了涂层的晶相结构和形貌特征,在1773 K的空气介质中对TaSi2/SiC涂层碳/碳复合材料进行等温氧化实验。结果表明,复合涂层厚度为200 μm,涂层中含有SiC, Si 和TaSi2相,并且涂层中没有明显裂纹出现。EDS结果显示外层TaSi2相可有效地填充内层SiC涂层的空隙,使得内外两层涂层之间没有明显的界面,等温氧化实验曲线说明TaSi2/SiC复合涂层在1773 K的空气介质中可有效保护碳/碳复合材料233 h。     

磁控溅射法制备碳/碳复合材料 SiC/MoSi2-ZrB2 涂层的结构及抗氧化性能研究

通过磁控溅射法在碳/碳复合材料表面成功制得了SiC/MoSi2-ZrB2陶瓷涂层并对结构及其在高温有氧环境中的抗氧化性能进行了研究。结果表明制备的SiC/MoSi2-ZrB2陶瓷涂层呈柱状晶结构且均匀性良好,其在1273K和1773K的有氧环境中氧化60min失重率分别是5.6×10-2 g/cm2 和 6.3×10-2 g/cm2。     

SiC–MoSi2/ZrO2–MoSi2 coating to protect C/C composites against oxidation

To improve the oxidation resistance of carbon/carbon (C/C) composites in air at high temperatures, a SiC–MoSi₂/ZrO₂–MoSi₂ coating was prepared on the surface of C/C composites by pack cementation and slurry method. The microstructures and phase compositions of the coated C/C composites were analyzed by scanning electron microscopy and X-ray diffraction, respectively. The result shows that the SiC–MoSi₂/ZrO₂–MoSi₂ coating is dense and crack-free with a thickness of 250–300 μm. The preparation and the high temperature oxidation property of the coated composites were investigated. The as-received coating has excellent oxidation protection ability and can protect C/C composites from oxidation for 260 h at 1773 K in air. The excellent anti-oxidation performance of the coating is considered to come from the formation of ZrSiO₄, which improves the stability of the coating at high temperatures.     

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.     

Double-layer oxidation protective SiC/Cr-Al-Si coating for carbon-carbon composites

Double-layer oxidation resistant SiC/Cr-Al-Si coating for carbon-carbon composites was prepared by a two-step method of pack cementation and slurry. The phase composition, micro-structure and oxidation resistance of mono-layer SiC coating and double-layer SiC/Cr-Al-Si coating were studied by XRD, SEM, and isothermal oxidation test at 1773 K in air, respectively. Mono-layer SiC coating consists of SiC and Si, which can protect carbon-carbon composites for several hours depending on its thin thickness and porous structure. After adding outer Cr-Al-Si alloy coating, the as-prepared double-layer SiC/Cr-Al-Si coating with a dense surface and about 150 μm thickness showed improved oxidation resistance, which can protect carbon-carbon composites for 197 h with only 0.079 wt.% mass gain. The failure of the double-layer SiC/Cr-Al-Si coating is thought to occur due to the excessive depletion of the outer Cr-Al-Si alloy coating and the appearance of defects in the SiO₂ glass layer.     

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.