Oxidation behavior of three dimensional C/SiC composites in air and combustion gas environments

A three dimensional C/SiC composite was prepared and flexural strengths during combustion atmosphere and weight changes in air were investigated. When oxidized in air, the C/SiC composite gained weight above the cracking temperature, and lost weight below the cracking temperature. The weight loss reached its maxumum value at about 700°C. When oxidized during combustion atmosphere, the composite always lost weight due to the large temperature gradient along the specimen. The strengths were lowest at the area close to the nozzle wall where the flame temperature was about 700°C. There were four oxidation zones along the specimens. There was an unoxidized zone (I) at the surporting end. Close to this was the cracking-oxidation zone (II). At the high-temperature end was the coating-oxidation zone (IV). Between the coating-oxidation and cracking-oxidation zones was the transition zone (III). Uniform, non-uniform and superficial oxidation regimes were observed which were considered to be responsible for the weight changes in air and strength changes during combustion atmosphere.     

Oxidation behavior of SiC/glaze-precursor coating on carbon/carbon composites

In order to improve the oxidation behavior of carbon/carbon composites in a wide range of temperature, a new SiC/glaze-precursor coating was developed.The SiC layer was produced by slurry and sintering, while the glaze precursor layer was prepared by slurry and drying. The microstructures and phase compositions of the coating were analyzed by SEM and XRD, respectively. The oxidation resistance of the coated composites was investigated using both isothermal and temperature-programmed thermogravimetric analysis in the temperature range from room temperature to 1600 °C. The results showed that the oxidation behavior of the coating was mainly controlled by the diffusion of oxygen during the test.The coating showed excellent oxidation resistance and self-healing ability in a wide range of temperature.     

Mullite-Al2O3-SiC oxidation protective coating for carbon/carbon composites

In order to exploit the unique high temperature mechanical properties of carbon/carbon (C/C) composites, a new type of oxidation protective coating has been produced by a two-step pack cementation technique in an argon atmosphere. XRD analysis showed that the internal coating obtained from the first step was a gradient SiC layer that acts as a buffer layer, and the multi-layer coating formed in the second step was an Al₂O₃-mullite layer. It was found that the as-received coating characterized by excellent thermal shock resistance on the surface of C/C composites during exposure to an oxidizing atmosphere at 1873 K, could effectively protect the C/C composites from oxidation for 45 h. The failure of the coating is due to the formation of bubble holes on the coating surface.     

Oxidation protective multilayer coatings for carbon-carbon composites

An oxidation protective double layered coating was deposited on a carbon-carbon composite (C/C) using a simple and low cost method. A surface modification of the C/C was obtained by direct reaction of liquid silicon with the C/C, promoting the formation of a 5-10 μm β-SiC layer on the composite surface. The inner layer, in contact with the C/C, is a composite made with a barium borosilicate glass matrix (SABB) and boron carbide particles; the outer layer is another composite layer formed by a SABB glass matrix and yttrium oxide particles. The layers are deposited by a slurry technique. Oxidation tests were carried out in a furnace in air, in order to verify the coating stability and its effectiveness. No mass loss of the C/C composite was observed after 100 h at 1200°C, while after 150 h at 1300°C the C/C mass loss did not exceed 1%.     

Oxidation behavior and protection of carbon/carbon composites prepared using rapid directional diffused CVI techniques

The oxidation kinetics of carbon/carbon (C/C) composites prepared using a rapid directional diffused (RDD) CVI process were studied. The results showed that the Arrhenius curve for the RDD CVI C/C composites consists of two straight lines, the intercept of which is at about 700 °C at the linear oxidation stage. The oxidation rates are controlled by the surface reaction at 600-700 °C, and the corresponding activation energy is 121 kJ/mol. Between 700 and 800 °C, the oxidation rates are dominated by chemical reaction and diffusion, and the relevant activation energy is 80 kJ/mol. SEM investigation showed that the oxidation starts with original pores on the C/C composite surface with the carbon fiber and matrix oxidized simultaneously. An inexpensive and easily pasted coating containing epoxy organic silicon resin, borates, refractory particulates, etc. was developed. After isothermal temperature, thermal cycle and immersion water oxidation tests, the coating was demonstrated to exhibit good oxidation-resistance properties. The oxidation-resistant mechanism of the coating is discussed.     

Oxidation behavior of C–SiC composites with a Si–W coating from room temperature to 1500°C

Oxidation tests of carbon fiber reinforced silicon carbide composites with a Si–W coating were conducted in dry air from room temperature to 1500°C for 5 h. A continuous series of empirical functions relating weight change to temperature after 5 h oxidation was found to fit the test results quite well over the whole temperature range. This approach was used to interpret the different oxidation mechanisms. There were two cracking temperatures of the matrix and the coating for the C–SiC composite. Oxidation behavior of the C–SiC composite was nearly the same as that of the coated C–C composite above the coating cracking temperature, but weight loss of the C–SiC composite was half an order lower than that of the coated C–C composite below the cracking temperature. As an inhibitor, the SiC matrix increased the oxidation resistance of C–SiC composites by decreasing active sites available for oxidation. As an interfacial layer, pyrolytic carbon decreased the activation energy below 700°C. From 800°C to 1030°C, uniform oxidation took place for the C–SiC composite, but non-uniform oxidation took place for the coated C–C composite in the same temperature range. The Knudsen diffusion coefficient could be used to explain the relationship between weight loss and temperature below the coating cracking temperature and the matrix cracking temperature.     

Gradient HfB2-SiC multilayer oxidation resistant coating for C/C composites

The gradient HfB₂ modified SiC coating was prepared on the surface of SiC-coated C/C composites by in-situ synthesis. Anti-oxidation behaviors of the coated C/C samples at 1773, 1873 and 1973?K were investigated. The results show that the gradient HfB₂ modified SiC coatings possess excellent oxidation resistance, which can protect C/C substrates from oxidation for 800, 305 and 100?h at 1773, 1873 and 1973?K, respectively. In addition, with the oxidation temperature increasing, the evaporation of the Hf-Si-O glass layer and the active oxidation of SiC were accelerated, which is the reason for the worst oxidation resistance of the sample at 1973?K among the three temperatures.     

Tribological application of carbon nanotubes in a metal-based composite coating and composites

Ni-P-carbon nanotube (CNT) composite coating and carbon nanotube/copper matrix composites were prepared by electroless plating and powder metallurgy techniques, respectively. The effects of CNTs on the tribological properties of these composites were evaluated. The results demonstrated that the Ni-P-CNT electroless composite coating exhibited higher wear resistance and lower friction coefficient than Ni-P-SiC and Ni-P-graphite composite coatings. After annealing at 673 K for 2 h, the wear resistance of the Ni-P-CNT composite coating was improved. Carbon nanotube/copper matrix composites revealed a lower wear rate and friction coefficient compared with pure copper, and their wear rates and friction coefficients showed a decreasing trend with increasing volume fraction of CNTs within the range from 0 to 12 vol.% due to the effects of the reinforcement and reduced friction of CNTs. The favorable effects of CNTs on the tribological properties are attributed to improved mechanical properties and unique topological structure of the hollow nanotubes.     

SiC coating toughened by SiC nanowires to protect C/C composites against oxidation

A dense SiC coating toughened by SiC nanowires was prepared on carbon/carbon (C/C) composites using a two-step technique of chemical vapor deposition (CVD) to protect them against oxidation. The morphologies and crystalline structures of the coatings were characterized by scanning electron microscopy, transmission electron microscopy and X-ray diffraction. SiC nanowires played a role in decreasing the size of the cracks and improving the thermal shock resistance of the coating. The result of thermal shock between 1773 K and room temperature for 21 times indicates that, compared with the SiC coating without SiC nanowires, the average size of the cracks in the SiC coating toughened with SiC nanowires reduced from 5 ± 0.5 to 3 ± 0.5 μm. The weight loss of the SiC coated C/C composites decreased from 9.32 to 4.45% by the introduction of SiC nanowires.     

Multilayer coating with self-sealing properties for carbon-carbon composites

This work proposes a simple and low cost method to deposit an effective multilayer protective coating on carbon-carbon composites (C/C). The first layer is made of molybdenum disilicide particles in a barium boron aluminosilicate glass (SABB); the second (external) layer is made of yttrium oxide modified SABB. A study of the reactions between the yttrium oxide and the SABB glass is presented. The coated C/C were submitted to thermal cycling or thermal aging tests up to 1300 °C in air. Weight losses were less than 0.5% in 50 h of thermal cycling and less then 1% in 150 h of thermal aging.     

Design of a C/SiC functionally graded coating for the oxidation protection of C/C composites

To reduce the residual thermal stress between the carbon fiber-reinforced carbon (C/C) composites and the SiC coating layer, functionally graded materials (FGM) consisting of a C/SiC compositionally graded layer (C/SiC interlayer) were adopted. After designing the compositional distribution of the C/SiC interlayer which can relieve the thermal stress effectively, the deposition conditions of the entire compositional range of the C/SiC composites were determined using a thermodynamic calculation. According to the design and calculation the C/SiC interlayer and the SiC outer layer were deposited on the C/C composites by a low pressure chemical vapor deposition (LPCVD) method at deposition temperatures of 1100 and 1300 °C. The stress calculation and the experimental results suggested that the SiC-rich compositional profile in the FGM layer is the most effective for relieving the thermal stress and increasing the oxidation resistance.     

HfC nanowires to improve the toughness and oxidation resistance of Si-Mo-Cr/SiC coating for C/C composites

To improve the oxidation resistance of carbon/carbon (C/C) composites, a dense HfC nanowire-toughened Si-Mo-Cr/SiC multilayer coating was prepared by chemical vapor deposition (CVD) and pack cementation. The microstructure, thermal shock and isothermal oxidation resistance of the coating were investigated. HfC nanowires could improve the toughness of the coating and suppress the coating cracking. After incorporating HfC nanowires in the coating, both of the thermal shock and isothermal oxidation resistance of the coating were obviously improved. The multilayer coating with HfC nanowires could effectively protect C/C composites at 1773 K for 270 h, whose weight loss is only 0.19%. The good oxidation resistance is mainly attributed to the formation of a compound glass layer containing SiO₂ and Cr₂O₃.     

Oxidation behavior of fine-grained SiC-B4C/C composites up to 1400 °C

Fine-grained B₄C-SiC/C composites were fabricated using a ball-milling dispersion process. The oxidation behaviors of both fine-grained B₄C-SiC/C composites and coarse-grained B₄C-SiC/C composites at temperatures of up to 1400 °C were analyzed by the differential thermal analysis technique, and the surface morphology of the composites after isothermal oxidation at 800, 1200 and 1400 °C was examined by scanning electron microscopy (SEM). The results indicated that fine-grained B₄C-SiC/C composites had excellent oxidation resistance with self-healing properties at 1400 °C. A general model and mechanism for self-protection against oxidation of carbon materials were proposed.     

Dynamic oxidation resistance and residual mechanical strength of ZrB2-CrSi2-SiC-Si/SiC coated C/C composites

To improve oxidation resistance of carbon/carbon (C/C) composites, a multiphase double-layer ZrB₂-CrSi₂-SiC-Si/SiC coating was prepared on the surface of C/C composites by pack cementation. Thermogravimetry analysis showed that the as-prepared coating could provide effective oxidative protection for C/C composites from room temperature to 1490 °C. After thermal cycling between 1500 °C and room temperature, the fracture behaviors of the as-prepared specimens changed and their residual flexural strengths decreased as thermal cycles increased. The specimen after 20 thermal cycles presented pseudo-plastic fracture characteristics and relatively high residual flexural strength (83.1%), while the specimen after 30 thermal cycles failed catastrophically without fiber pullout due to the severe oxidation damage of C/C substrate especially the brittleness of the reinforcement fibers.     

A MoSi2-SiOC-Si3N4/SiC anti-oxidation coating for C/C composites prepared at relatively low temperature

In this study, SiC coating for C/C composites was prepared by pack cementation method at 1773 K, and MoSi₂-SiOC-Si₃N₄ as an outer coating was successfully fabricated on the SiC coated samples by slurry method at 1273 K. The microstructure and phase composition of the coatings were analyzed. Results showed that a porous β-SiC inner coating and a crack-free MoSi₂-SiOC-Si₃N₄ coating are formed. Effect of Si₃N₄ content on the oxidation resistance of the coated C/C composites at 1773 K in air was also investigated. The weight loss curves revealed that introducing the appropriate proportion of Si₃N₄ could improve the oxidation resistance of coating. The MoSi₂-SiOC/SiC coated C/C sample had an accelerated weight loss after oxidation in air for 20 h. However, the coating containing 45% Si₃N₄ could protect C/C composition from oxidation for 100 h with a minute weight loss of 0.63%.     

Oxidation resistance and mechanical properties of LaB6-MoSi2-SiC ceramic coating toughened by SiC nanowires

To improve the high-temperature tolerance of carbon/carbon composites, a compact SiC-nanowires toughened LaB₆-MoSi₂-SiC/SiC (SiCnws-LMS/SiC) coating was designed and fabricated by combination of multiple methods including pack cementation, chemical vapor deposition and supersonic atmospheric plasma spraying. Isothermal oxidation results indicated that the mass loss of LMS/SiC coating decreased from 4.34?±?0.28% to 1.12?±?0.23% after oxidation for 200?h at 1773?K benefit from the addition of SiCnws. Absence of obvious cracks and voids in the coating after oxidation test indicated that the interfaces between various phases and SiCnws could obstruct the crack propagation by releasing the thermal stress in the coating. Meanwhile, after the introduction of SiCnws, the bonding strength and flexural strength of the coating were respectively increased by 54.54% and 59.77% compared to the LMS/SiC coating without SiCnws. The improved mechanical properties could be attributed to the pullout and bridging effects of SiCnws, which created multi-scaled reinforcements, thereby enhancing the load bearing capacity to increase the fracture toughness of the coating.