C/SiC composites are raising great interest as a thermal shielding for aerospace applications, provided that they are protected from oxidation by suitable coatings Conversely, ultra high temperature ceramics, and in particular ZrB 2 , is among the best oxidation resistant materials as known A new type of oxidation protective coating (ZrB 2 /SiC coating) was produced on C/SiC composites The composites were produced by precursor infiltration and pyrolysis (PIP), which is a simple and low cost method; the coating was ZrB 2 mixed with SiC, which was fabricated by painting slurry on the surface of the composite followed by chemical vapor deposition (CVD) SiC on the top Mechanical tests were conducted before and after oxidation test Anti-ablation property was tested under oxy-acetylene torch Oxidation test shows that the uncoated samples are oxidized quickly and the weight loss reaches 292% and the reservation of original flexural strength is only 674%, while the weight loss of ZrB 2 /SiC coated samples is only 519%, and the reservation of original flexural strength is 374% ZrB 2 /SiC coating can provide longtime protection for C/SiC composites at 1973 K Compared with the uncoated composites, the linear and mass ablation rates of the coated composites decreased by 621% and 461%, respectively, after ablation for 30 s The formation of zirconia and silicon dioxide from the oxidation of ZrB 2 /SiC improved the ablation resistance of the composites, because of the evaporation at elevated temperature, which absorbed heat from the flame and reduced the erosive attack to carbon fibers and SiC matrix

ZrB2/SiC as a protective coating for C/SiC composites: Effect of high temperature oxidation on mechanical properties and anti-ablation property

Multi-layered UHTC composites for use in an extreme oxidation environment were fabricated by co-sintering. The multi-layered composite system consists of three layers and was designed with (i) an outer surface with the capacity to withstand heat fluxes in excess of 25 MW m−2, (ii) an intermediate layer with the ability to curtail diffusion of O2 and (iii) a bottom layer with better performance at high temperatures. One design has MeB2 (where Me = Zr or Hf) as the outer or top layer, MeCxOy as the intermediate layer and MeB2/SiC as the bottom layer. Since little is known about MeCxOy ceramics, a detailed study has been carried out to synthesise and characterise them focussed on controlling MeCxOy stoichiometry. During co-sintering, the outer MeB2 layer thickness played a crucial role in providing a crack-free component. Indicative calculations of the residual stresses confirm that a compressive stress due to bending of the disks can stop crack growth through the MeB2 layer when its thickness is increased to 3 mm, and that the tensile stress in the bottom layer is also reduced. The cross-section microstructure of the optimised multi-layered UHTC composite shows a crack-free seamless interface.

Development of multi-layered thermal protection system (TPS) for aerospace applications

Ablation is an erosive phenomenon with removal of material by a combination of thermo-mechanical, thermo-chemical, and thermo-physical factors with high temperature, pressure, and velocity of combustion flame. Materials with outstanding thermo-mechanical and thermo-chemical properties are required for future high-temperature components. C/SiC is a kind of great potential high-temperature structural material in aeronautics and astronautics with low specific weight, high specific strength, good thermal stability, oxidation resistance and excellent resistance to ablation. In this paper, the ablation phenomenon and mechanisms were summarized adequately. The ablated surface of C/SiC composites could be divided into three regions from center to external. In general, the higher the density, the lower the ablation rate; the lower the ablation temperature and less time, the lower the ablation rate, and the preparation methods also had a great influence on the ablation property. Thermo-physical and thermo-mechanical attacks were the main ablation behavior in the center region; oxidation was the main ablation behavior in the transition region and the border oxidation region.

Ablation behavior and mechanism analysis of C/SiC composites

In order to satisfy the requirements for the thermal protection system to serve at ultrahigh temperatures, carbon fiber reinforced silicon carbide-hafnium carbide (C/SiC-HfC) composites were fabricated by reactive melt infiltration method. The ablation behaviors of C/SiC-HfC composites were examined in plasma wind tunnel. The results indicated that ablation was controlled by the oxidation of HfC-SiC under dissociated oxygen conditions at low heat flux and stagnation pressure. However, a sudden temperature jump caused by the change in the catalytic surface from silica to hafnia was observed at high heat flux and stagnation pressure during ablation. The increase in surface temperature was further accelerated by the burning of carbon fiber and recombination of carbon and nitrogen on it.

Ablation behavior of C/SiC-HfC composites in the plasma wind tunnel

A double layer nanostructure SiC coating for anti-oxidation protection of carbon/carbon composites prepared by chemical vapor reaction and chemical vapor deposition

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

In order to improve the anti-oxidation performance of carbon fiber reinforced silicon carbide (C/SiC) composites, SiC coating was prepared by chemical vapor deposition (CVD). The effects of high-temperature annealing and the anti-oxidation properties of coated composites were investigated. The results showed that CVD-SiC coating, which was β-SiC phase, was fabricated successfully on the PIP-C/SiC with thickness of about 30 μm. It was clear that visible cracks existed and the ratio of weight loss increased with the annealing temperature increasing, while the flexural strength of coated composites greatly decreased with the elevation of the annealing temperature. Coated composites showed the best anti-oxidation ability at 1773 K (1.73 wt.%). During thermal cycle tests, the weight loss of coated sample was 0.68 wt.% and the percentage of remaining strength was 98.1%. The decrease of flexural strength during the tests was primarily due to the oxidation of the coated samples by oxygen or vapor.

Microstructures and mechanical properties of CVD-SiC coated PIP-C/SiC composites under high temperature

Fused silica ceramics are widely applied for radome materials, crucibles, and vanes, but the mechanical properties were deteriorated due to the cristobalite crystallization. The fused silica ceramics added with by β-Si3N4 whiskers were prepared by a slip-casting method to retard the cristobalite crystallization. The influences of the sintering environments and the β-Si3N4 whiskers on the microstructure and phase structure were investigated. The silanol (Si-(OH)n) and oxygen vacancies (VO) in the fused silica in formed in different conditions were studied by Fourier Transform Infra-Red (FT-IR) and X-ray photoelectron spectroscopy (XPS), and the results indicated that the ball-milled produced a large amount of the silanol groups onto the surface of the fused silica particles. The fused silica heated in the vacuum created the maximum oxygen vacancies (24.2%) on the surfaces. Silanol groups reacted with the β-Si3N4 whiskers, and the O atoms in the silanol groups were fixed into the bulk materials. And the crystallization kinetics and the activation energy of Si3N4w/SiO2 ceramics at the temperature ranging from 1200 to 1400°C were calculated based on the JMA(Johnson-Mehl-Avrami) model. The activation energy of the fused silica ceramics with the addition of the β-Si3N4 is 506.2 kJ/mol, increased by 23.6% than that of the pure fused silica ceramic. 

Influence of β‐Si
 3
 N
 4
 whiskers on sintering and crystallization of fused silica ceramics

Fused silica ceramic has become one of the most widely used radome materials in the world since the 1970s. But its poor mechanical properties restricted its application to some extent. To improve the mechanical properties of the fused silica ceramic and keep its characteristic for radome materials, silicon nitride (Si3N4) whisker-reinforced fused silica ceramics were prepared by a slip-casting method in the work. The influence of Si3N4 whisker contents on the properties of the slurry was studied, indicating that the preferable pH values of the slurry were 4–6 and whisker contents were 10 wt.%. The flexural strength of as-prepared Si3N4w/SiO2 ceramic was about 74.35 MPa, exhibiting an increase of 7.75% over that of the pure silica sample. Its dielectric constant in the range from 8 to 12 GHz and tanδ under 10 GHz were, respectively, 3.37 and .0011. It is of great interest to find that Si3N4w/SiO2 has excellent oxidization resistance and its mass maintains even at 1270°C. 

Fabrication and characterization of Si
 3
 N
 4
 whisker‐reinforced SiO
 2
 ceramic for radome materials

ZrC-Zr2Si coating was prepared on carbon fiber reinforced silicon carbide matrix composites (C/SiC) by pack cementation method to prevent these composites from oxidation. SEM, EDS and XRD were applied to analyze the surface and cross-section morphologies, element distribution and phase composition of the coating, respectively. The results show that the coating made by the technique exhibits excellent oxidation resistance. The optimizing infiltration composition and process was: 60wt.%Zr-Si, 30wt.%PCS-DVB, 10wt.%Al2O3, holding 8 hours at 1400°C in Ar protecting atmosphere, ZrC-Zr2Si coating is obtained, homogeneous and density. The weight loss percentage of the coated C/SiC is only 1.52％after oxidation in air at 1500°Cfor 30min.

ZrC-Zr2Si Coating on Carbon Fiber Reinforced Silicon Carbide Matrix Composites Prepared by Pack Cementation Method

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Papers

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

Microstructures and mechanical properties of CVD-SiC coated PIP-C/SiC composites under high temperature

Influence of β‐Si 3 N 4 whiskers on sintering and crystallization of fused silica ceramics

Fabrication and characterization of Si 3 N 4 whisker‐reinforced SiO 2 ceramic for radome materials

ZrC-Zr2Si Coating on Carbon Fiber Reinforced Silicon Carbide Matrix Composites Prepared by Pack Cementation Method