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.     

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.     

Influence of SiC nanowires on the properties of SiC coating for C/C composites between room temperature and 1500 °C

To prevent carbon/carbon (C/C) composites from oxidation between room temperature and 1500 °C, a dense SiC nanowire-toughened SiC oxidation resistant coating was prepared by a two-step technique composed of chemical vapor deposition and pack cementation. SiC nanowires could effectively baffle the propagation of the microcracks and avoid the formation of the through-thickness microcracks in the original coating. The results indicated that, after introducing SiC nanowires, the coefficient of thermal expansion of the coating was decreased between 100 and 1500 °C, and the oxidation protective ability for the coated C/C composites was improved largely between room temperature and 1500 °C.     

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/MoSi2–SiC–Si multilayer coating for oxidation protection of carbon/carbon composites

C/SiC/MoSi₂–SiC–Si oxidation protective multilayer coating for carbon/carbon (C/C) composites was prepared by pack cementation and slurry method. The microstructure, element distribution and phase composition of the as-received coating were analyzed by scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS) and X-ray diffraction (XRD). The results show that the multilayer coating was composed of MoSi₂, SiC and Si. It could effectively protect C/C composites against oxidation for 200 h with the mass loss of 3.25% at 1873 K in static air. The mass loss of the coated C/C composites results from the volatilization of SiO₂ and the formation of cracks and bubble holes in the coating.     

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.     

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.     

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.     

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.     

Effect of alloying with Al on oxidation behavior of MoSi2 coatings at 1100 °C

MoSi₂ - 0, 15.3, 22, and 29.3 at.% Al coatings were prepared on the nickel-based super-alloy substrates by electro-thermal explosion ultrahigh speed spraying technology. The analysis showed that the coatings had fine microstructure with grain sizes ranging from 0.5 to 2 μm. The bonding between coating and substrate was typically metallurgical cohesion. The oxidation resistance of the coating was further studied at 1100 °C in air. Al alloyed in MoSi₂ coatings increased the oxidation resistance of the coatings, and the oxidation resistance of MoSi₂-15.3 at.% Al coating was higher than the other two MoSi₂–Al coatings. This suggested the oxidation resistance might have close relations to the obtained grain size.     

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.     

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.     

Thermal fatigue behavior of C/C composites modified by SiC-MoSi2-CrSi2 coating

Carbon/carbon (C/C) composites were modified by SiC-MoSi₂-CrSi₂ multiphase coating by pack cementation, and their thermal fatigue behavior under thermal cycling in Ar and air environments was investigated. The modified C/C composites were characterized by scanning electron microscopy and X-ray diffraction. Results of tests show that, after 20-time thermal cycles between 1773 K and room temperature in Ar environment, the flexural strength of modified C/C samples decreased lightly and the percentage of remaining strength was 94.92%. While, after thermal cycling between 1773 K and room temperature in air for 20 times, the weight loss of modified C/C samples was 5.1%, and the flexural strength of the modified C/C samples reduced obviously and the percentage of remaining strength was only 75.22%. The fracture mode of modified C/C samples changed from a brittle behavior to a pseudo-plastic one as the service environment transformed from Ar to air. The decrease of the flexural strength during thermal cycle in air was primarily attributed to the partial oxidation of modified C/C samples.     

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.     

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.     

The oxidation behavior and mechanical properties of MoSi2–CrSi2–SiC–Si coated carbon/carbon composites in high-temperature oxidizing atmosphere

A MoSi₂–CrSi₂–SiC–Si multi-component coating was prepared on the surface of carbon/carbon (C/C) composites by a two-step pack cementation method. The microstructure, oxidation behavior and mechanical properties of the coating were studied. These results show that the multi-component coating could protect the C/C composites from oxidation in air at 1873 K for 300 h and withstand 30 thermal cycles between 1873 K and room temperature, respectively. The mass loss and mechanical property loss of the coated C/C composites are considered due to the worse fluidity of SiO₂ at intermediate temperatures and the thermal mismatch between the coating and C/C composites.     

Investigation on 3-dimensional carbon foams/LiFePO4 composites as function of the annealing time under inert atmosphere

The morphological and electrochemical investigation of 3-dimensional (3D) carbon foams coated with olivine structured lithium iron phosphate as function of the annealing time under nitrogen atmosphere is reported. The LiFePO₄ as cathode material for lithium ion batteries was prepared by a Pechini-assisted sol-gel process. The coating has been successfully performed on commercially available 3D-carbon foams by soaking in aqueous solution containing lithium, iron salts and phosphates at 70 °C for 2-4 h. After drying-out, the composites were annealed at 600 °C for different times ranging from 0.4 to 10 h under nitrogen. The formation of the olivine-like structured LiFePO₄ was confirmed by X-ray diffraction analysis performed on the powder prepared under similar conditions. The surface investigation of the prepared composites showed the formation of a homogeneous coating by LiFePO₄ on the foams. The cyclic voltammetry curves of the composites show an enhancement of electrode reaction reversibility by increasing the annealing time. The electrochemical measurements on the composites showed good performances delivering a discharge specific capacity of 85 mAh g⁻¹ at a discharging rate of C/25 at room temperature after annealing for 0.4 h and 105 mAh g⁻¹ after annealing for 5 h.     

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.     

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.     

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.