Oxidation resistance of SIC-AlN ceramics coated by oxidation-assisted-pack cementation process

Liquid-phase-pressureless-sintered SiC-AlN-Y₂O₃ composites were coated by means of modified pack cementation process (OXPAC, OXidation-assisted-PAck Cementation) using rare-earth oxides, RE₂O₃ (RE = Sc, Er, Sm, Lu, Ho), as reactive powders. The coatings, composed by the oxidation products of SiC, AlN and rare-earth silicates, were adherent to the substrate, without porosity and with a thickness of 10 μm. The oxidation resistance of the coated SiC-AlN-Y₂O₃ ceramics was also investigated at 1500 °C for a period of 200 h. The coated samples showed specific weight gain lower than the uncoated and pre-oxidised samples. Furthermore, the specific weight gain linearly increased with the rare-earth cationic radius.     

Evaluation of Yttria Coated High Density Graphite with Silicon Carbide Interlayer for Uranium Melting Applications

Yttrium Oxide (Y₂O₃) deposited over High Density Graphite (HDG) by Atmospheric Plasma Spray (APS) process is highly desirable as a chemical barrier coating for reusable Uranium (U) melting crucibles in the pyrochemical reprocessing of spent metallic fuels. In the present study, an oxidation protective Silicon Carbide (SiC) interlayer coating over HDG has been achieved by pack cementation process. The high-temperature oxidation resistance and resistance to thermal fatigue failure of Y₂O₃ coating with and without SiC interlayer were evaluated by performing repeated thermal cycling studies at 1450, 1500 and 1550?°C. The durability performance of Y₂O₃ coating with SiC interlayer in the actual working environment was simulated by performing U melting studies using miniature size HDG coated crucibles. The microstructural, chemical and phase characterization of coatings prior and post thermal cycle failure were carried out by SEM/EDS and XRD techniques. It is observed that the SiC interlayer developed by novel pack cementation technique for the Y₂O₃ top coat extended the thermal cycling and life of the coating with U melting in inert argon gas environment significantly. The occurrence of micro-cracking over Y₂O₃ top coat with SiC interlayer perceived after 33, 30 and 25 thermal cycles at 1450, 1500 and 1550?°C, respectively.     

Effect of silicon/graphite ratio and temperature on oxidation protective properties of SiC/ZrB2–SiC coatings prepared by pack cementation

To investigate the silicon/graphite ratio and temperature on preparation and properties of ZrB₂–SiC coatings, ZrB₂, silicon, and graphite powders were used as pack powders to prepare ZrB₂–SiC coatings on SiC coated graphite samples at different temperatures by pack cementation method. The composition, microstructure, thermal shock, and oxidation resistance of these coatings were characterized and assessed. High silicon/graphite ratio (in this case, 2) did not guarantee higher coating density, instead could be harmful to coating formation and led to the lump of pack powders, especially at temperatures of 2100 and 2200 °C. But residual silicon in the coating is beneficial for high density and oxidation protection ability. The SiC/ZrB₂–SiC (ZS50-2) coating prepared at 2000 °C showed excellent oxidation protective ability, owing to the residual silicon in the coating and dense coating structure. The weight loss of ZS50-2 after 15 thermal shocks between 1500 °C and room temperature, and oxidation for 19 h at 1500 °C are 6.5% and 2.9%, respectively.     

Cf/SiC 复合材料的 ZrB2-SiC/SiC 超高温陶瓷涂层研究

采用两步包埋法在Cf/SiC复合材料表面制备了Zr B_2-SiC/SiC超高温陶瓷涂层。借助SEM、XRD对涂层的微观结构及物相组成进行了分析研究,并进行了高温静态氧化和热震测试。研究表明,1500°C氧化5 h后,涂层表面覆盖有平整的玻璃相氧化层,氧化失重率为6.4%;热震测试10次后涂层的氧化失重率为14%。Zr B_2-SiC/SiC涂层能有效提高Cf/SiC复合材料的高温抗氧化性能。     

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.     

Oxidation behavior of oxidation protective coatings for PIP-C/SiC composites at 1500 °C

Three-dimensional carbon fiber reinforced silicon carbide (C/SiC) composites were fabricated by precursor infiltration and pyrolysis (PIP) with polycarbosilane as the matrix precursor, SiC coating prepared by chemical vapor deposition (CVD) and ZrB₂-SiC/SiC coating prepared by CVD with slurry painting were applied on C/SiC composites, respectively. The oxidation of three samples at 1500 °C was compared and their microstructures and mechanical properties were investigated. The results show that the C/SiC without coating is distorted quickly. The mass loss of SiC coating coated sample is 4.6% after 2 h oxidation and the sample with ZrB₂-SiC/SiC multilayer coating only has 0.4% mass loss even after oxidation. ZrB₂-SiC/SiC multilayer coating can provide longtime protection for C/SiC composites. The mode of the fracture behavior of C/SiC composites was also changed. When with coating, the fracture mode of C/SiC composites became brittle. When after oxidation, the fracture mode of C/SiC composites without and with coating also became brittle.     

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.     

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.     

SiC/SiC复合材料及其应用

日本开发的Nicalon和Tyranno两种品牌的SiC纤维占有世界上绝对性的市场份额。SiC/SiC复合材料典型的界面层是500 nm厚的单层热解碳(PyC)涂层或多层(PyC-SiC)n涂层,在湿度燃烧环境及中高温条件下界面层的稳定性是应用研究的重点。SiC/SiC复合材料,包括CVI-SiC基体和日本开发的Tyranno hex和NITE-SiC基体等,具有耐高温、耐氧化性和耐辐射性的特点,在航空涡轮发动机部件、航天热结构部件及核聚变反应堆炉第一壁材料等方面正开展工程研制应用。     

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.     

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.