Effect of co-deposited SiC nanowires and carbon nanotubes on oxidation resistance for SiC-coated C/C composites

To protect carbon/carbon composites (C/Cs) against oxidation, SiC coating toughened by SiC nanowires (SiCNWs) and carbon nanotubes (CNTs) hybrid nano-reinforcements was prepared on C/Cs by a two-step technique involving electrophoretic co-deposition and reactive melt infiltration. Co-deposited SiCNWs and CNTs with different shapes including straight-line, fusiform, curved and bamboo dispersed uniformly on the surface of C/Cs forming three-dimensional networks, which efficiently refined the SiC grains and meanwhile suppressed the cracking deflection of the coating during the fabrication process. The presence of SiCNWs and CNTs contributed to the formation of continuous glass layer during oxidation, while toughed the coating by introducing toughing methods such as bridging effect, crack deflection and nanowire pull out. Results showed that after oxidation for 45 h at 1773 K, the weight loss percentage of SiC coated specimen was 1.35%, while the weight gain percentage of the SiCNWs/CNTs reinforced SiC coating was 0.03052% due to the formation of continuous glass layer. After being exposed for 100 h, the weight loss percentage of the SiCNWs/CNTs reinforced SiC coating was 1.08%, which is relatively low.     

Oxidation protection of C/C composites with a multilayer coating of SiC and Si + SiC + SiC nanowires

An oxidation protective Si–SiC coating with randomly oriented SiC nanowires was prepared on the SiC-coated carbon/carbon (C/C) composites by a two-step technique. First, a porous network of SiC nanowires was produced using chemical vapor deposition. This material was subjected to pack cementation to infiltrate the porous layer with a mixture of Si and SiC. The nanowires in the coating could efficiently suppress the cracking of the coating by various toughening mechanisms including nanowire pullout, nanowire bridging, microcrack deflection and good interaction between nanowire/matrix interface. The results of thermogravimetric analysis and thermal shock showed that the coating had excellent oxidation protection for C/C composites between room temperature and 1500 °C. These results were confirmed by two additional oxidation experiments conducted at temperature of 900 and 1400 °C, which demonstrated that the coating could efficiently protect C/C composites from oxidation at 900 °C for more than 313 h or at 1400 °C for more than 112 h.     

Oxidation resistance of SiC nanowires reinforced SiC coating prepared by a CVD process on SiC‐coated C/C composites

Oxidation protective SiC nanowires‐reinforced SiC (SiCNWs‐SiC) coating was prepared on pack cementation (PC) SiC‐coated carbon/carbon (C/C) composites by a simple chemical vapor deposition (CVD) process. This double‐layer SiCNWs‐SiC/PC SiC‐coating system on C/C composites not only has the advantages of SiC buffer layer but also has the toughening effects of SiCNWs. The microstructure and phase composition of the nanowires and the coatings were examined by SEM, TEM, and XRD. The single‐crystalline β‐SiC nanowires with twins and stacking faults were deposited uniformly and oriented randomly with diameter of 50‐200 nm and length ranging from several to tens micrometers. The dense SiCNWs‐SiC coating with some closed pores was obtained by SiC nanocrystals stacked tightly with each other on the surface of SiCNWs. After introducing SiCNWs in the coating system, the oxidation resistance is effectively improved. The oxidation test results showed that the weight loss of the SiCNWs‐SiC/PC SiC‐coated samples was 4.91% and 1.61% after oxidation at 1073 K for 8 hours and at 1473 K for 276 hours, respectively. No matter oxidation at which temperature, the SiCNWs‐SiC/PC SiC‐coating system has better anti‐oxidation property than the single‐layer PC SiC coating or the double‐layer CVD SiC/PC SiC coating without SiCNWs.     

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.     

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.     

Ablation behaviour of a TaC coating on SiC coated C/C composites at different temperatures

To improve the ablation resistance of carbon/carbon (C/C) composites, a TaC coating was prepared by supersonic plasma spraying on SiC coated C/C composites. The microstructure and morphology of the coatings were characterised by Scanning Electron Microscopy and X-ray diffraction. The ablation properties were studied at different temperatures under oxyacetylene torch. At 2100 °C, the oxides were blown away and resulted in high ablation rates: 1.2×10^?2 mm/s and 3.9×10^?3 g/s. However, most oxides can remain in ablation centre and serve as a coating at low temperature (1900 and 1800 °C). Therefore, the TaC/SiC coated samples exhibited zero linear ablation rate and lower mass ablation rate.     

Oxidation protection of carbon/carbon composites with SiC/indialite coating for intermediate temperatures

In order to improve the oxidation resistance of carbon/carbon composites at intermediate temperatures, a novel double-layer SiC/indialite coating was prepared by a simple and low-cost method. The internal SiC transition layer was prepared by pack cementation and the external indialite glass–ceramic coating was produced by in situ crystallization of ternary MgO–Al₂O₃–SiO₂ glass. The microstructures and morphologies of coating were determined by scanning electron microscopy (SEM), X-ray diffraction (XRD) and energy dispersive spectroscopy (EDS). Oxidation resistance of the as-coated C/C composites was evaluated in ambient air at temperature from 800 °C to 1200 °C. Nearly neglectable mass loss was measured after 100 h isothermal oxidation test, indicating that SiC/indialite coating possesses excellent oxidation protection ability. The as-coated samples have a good thermal shock resistance and no obvious damage was found in the coating even after suffered more than 11 thermal cycles between test temperature and room temperature. The oxidation protection mechanism of this coating was also discussed.     

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

A double layer nanostructure SiC coating was prepared by chemical vapor reaction and chemical vapor deposition to protect carbon/carbon composites from oxidation. The obtained dense coating reveals a typical crystalline structure and combines well with the substrate. The outer layer of the coating consists of SiC nanocrystals and nanowires, whereas the inner layer is mainly composed of SiC microcrystals, nanocrystals and nanowires. The oxidation and cyclic thermal shock test performed at 1400 °C in air demonstrates that the prepared dense nanostructure coating has excellent anti-oxidation behavior and thermal shock resistance at high temperature. After 400 h oxidation and 34 cycles of thermal shock from 1400 °C to room temperature, the weight loss of the coated sample is only 1.67%. In the oxidation process, the amorphous silica formed at the beginning of the oxidation crystallizes to cristobalite as oxidation time increased. The formation of cristobalite resulted in micro-cracks formed along grain boundaries in the cyclic thermal shock test. As only cracks are formed on the coating surface, it can be concluded that the formation of the penetration cracks may be the reason for the weight loss of the SiC coated composite.     

Tensile creep behavior of three-dimensional four-step braided SiC/SiC composite at elevated temperature

This article presents experimental results for tensile creep deformation and rupture behavior of three-dimensional four-step braided SiC/SiC composites at 1100 °C and 1300 °C in air. The creep behavior at 1300 °C exhibited a long transient creep regime and the creep rate decreased continuously with time. The creep behavior at 1100 °C exhibited an apparent steady-rate regime and the creep deformation was smaller than that at 1300 °C. However, the creep rupture time at both temperatures showed little difference. The mechanisms controlling creep deformation and rupture behavior were analyzed.     

Ablation resistance of HfB2-SiC coating prepared by in-situ reaction method for SiC coated C/C composites

To improve the ablation resistance of SiC coating, HfB₂-SiC coating was prepared on SiC-coated carbon/carbon (C/C) composites by in-situ reaction method. Owing to the penetration of coating powders, there is no clear boundary between SiC coating and HfB₂-SiC coating. After oxyacetylene ablation for 60 s at heat flux of 2400 kW/m², the mass ablation rate and linear ablation rate of the coated C/C composites were only 0.147 mg/s and 0.267 µm/s, reduced by 21.8% and 60.0%, respectively, compared with SiC coated C/C composites. The good ablation resistance was attributed to the formation of multiple Hf-Si-O glassy layer including SiO₂, HfO₂ and HfSiO₄.     

Oxidation resistance of SiC/SiC composites containing SiBC matrix fabricated by liquid silicon infiltration

The mechanical behavior and oxidation resistance of SiC/SiC-SiBC composites were studied in this work. According to the debonding criterion of He and Hutchinson, the debonding could occur at the BN interphase, which insures that the fibers can well play the strengthening and toughening performance. The oxidation resistance of SiC/SiC-SiBC composites consisting of SiC fibers with thermal expansion coefficients (CTE) of 5.1 × 10^?6 K^?1 and 4.0 × 10^?6 K^?1 was compared. The composites consisting of SiC fibers with higher CTE show slight weight changes at 800, 1000, and 1200 °C, and the corresponding strength retention ratios are 109.6%, 103.2% and 102.9%, exhibiting excellent oxidation resistance. The CTE of composites consisting of SiC fibers with higher CTE matches well with the CTE of SiC coating, so rarely no cracks can be formed in the coating, which inhibits the inward diffusion of oxidizing medium and leads to high strength retention ratios after oxidation tests.     

Effects of porous C/C density on the densification behavior and ablation property of C/C–ZrC–SiC composites

C/C–ZrC–SiC composites were prepared by precursor infiltration and pyrolysis process using a mixture solution of organic zirconium-containing polymer and polycarbosilane as precursors. Porous carbon/carbon (C/C) composites with density of 0.92, 1.21 and 1.40 g/cm³ were used as preforms, and the effects of porous C/C density on the densification behavior and ablation resistance of C/C–ZrC–SiC composites were investigated. The results show that the C/C preforms with a lower density have a faster weight gain, and the obtained C/C–ZrC–SiC composites own higher bulk density and open porosity. The composites fabricated from the C/C preforms with a density of 1.21 g/cm³ exhibit better ablation resistance with a surface temperature of over 2400 °C during ablation. After ablation for 120 s, the linear and mass ablation rates of the composites are as low as 1.02 × 10⁻³ mm/s and −4.01 × 10⁻⁴ g/s, respectively, and the formation of a dense and continuous coating of molten ZrO₂ solid solution is the reason for their great ablation resistance.     

Mechanical,structural and oxidation resistance enhancement of carbon foam by in situ grown SiC nanowires

A method for processing carbon foams containing both silicon carbide (SiC) nanowires and bulk SiC and silicon nitride (Si3N4) phases has been developed by reaction of powder mixtures containing precursors for carbon, sacrificial template, silicon (Si), short carbon fibers (SCF) and activated carbon (AC). In situ growth of Si nanowires during pyrolysis of the foam at 1000 °C under N2 changed the foam׳s microstructure by covering the porous skeleton inside and out. In situ-grown SiC nanowires were found smoothly curved with diameters ranging around two main modes at 30 and 500 nm while their lengths were up to several tens of micrometers. SCF were found effectively mixed and well-bonded to pore walls. Following density, porosity and pore size distribution analyses, the heat-treated (HT) foam was densified using a chemical vapor infiltration (CVI) process. Thereafter, density increased from 0.62 to 1.30 g/cm³ while flexural strength increased from 29.3 to 49.1 MPa. The latter increase was attributed to the densification process as well as to low surface defects, presence of SCF and coating, by SiC nanowires, of the entire SiC matrix porous structure. The foam׳s oxidation resistance improved significantly from 58 to 84 wt% residual mass of the heat treated and densified sample. The growth mechanism of Si nanowires was supported by the vapor–liquid–solid mechanism developed under pyrolysis conditions of novolac and reducing environment of coal cover.     

Microstructure and ablation behavior of SiC coated C/C–SiC–ZrC composites prepared by a hybrid infiltration process

In this study, C/C–SiC–ZrC composites coated with SiC were prepared by precursor infiltration pyrolysis combined with reactive melt infiltration. The pyrolysis behavior of the hybrid precursor was investigated using thermal gravimetric analysis-differential scanning calorimetry, X-ray diffraction, and scanning electron microscopy techniques. The microstructure and ablation behavior of the composites were also investigated. The results indicate that the composites exhibit an interesting structure, wherein a ceramic coating composed of SiC and a small quantity of ZrC covers the exterior of the composites, and the SiC–ZrC hybrid ceramics are partially embedded in the matrix pores and distributed around the carbon fibers as well. The composites exhibit good ablation resistance with a surface temperature of over 2300 °C during ablation. After ablation for 120 s, the mass and linear ablation rates of the composites are 0.0026 g/s and 0.0037 mm/s, respectively. The great ablation resistance of the composites is attributed to the formation of a continuous phase of molten SiO₂ containing SiC and ZrO₂, which seals the pores of the composites during ablation.     

Thermomechanical characterisation of coal tar pitch- based carbon containing SiC nanoparticles

Coal tar pitch (CTP) modified with silicon carbide nanoparticles (nSiC) was used as a carbon binder precursor for the manufacture of carbon materials. Carbon samples were prepared in the form of a composition consisting of synthetic coke, graphite and nSiC- modified CTP prior to heat treatment at temperatures from 800 °C to 2800 °C. The effect of ceramic nanofiller in CTP on oxidation resistance of carbon samples obtained at various temperatures was studied. Physical and mechanical properties of carbon samples obtained at 2000 °C and 2800 °C were analysed. nSiC presence in CTP was found to change the elevated temperature properties of carbon samples. The oxidation tests conducted at 600 °C in air showed a significant improvement of the resistance of carbon samples modified with small amount of nSiC and annealed at 2000 °C. Properties investigated included characteristics important for application of carbon materials for carbon electrode manufacturing, i.e., electrical and thermal conductivities as well as mechanical properties. Due to microstructural changes of carbon samples in the presence of nSiC filler physical and mechanical properties improved after annealing the samples at high temperature in comparison to unmodified carbon samples.     

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

To protect carbon/carbon (C/C) composites against oxidation, a mullite coating was prepared on SiC precoated C/C composites by a hydrothermal electrophoretic deposition process. The phase composition, microstructure and oxidation resistance of the prepared mullite/SiC coatings were investigated. Results show that hydrothermal electrophoretic deposition is an effective route to achieve crack-free mullite coatings. The mullite/SiC coating displays excellent oxidation resistance and can protect C/C composites from oxidation at 1773 K for 322 h with a weight loss rate of only 4.89 × 10^?4 g/cm² h. The failure of the multi-layer coatings is considered to be caused by the volatilization of silicate glass layer, the formation of microholes and microcracks on the coating surface and the formation of penetrative holes between the SiC bonding layer and the C/C matrix at 1773 K. The corresponding high temperature oxidation activation energy of the coated C/C composites at 1573–1773 K is calculated to be 111.11 kJ/mol.     

Improved dielectric and electromagnetic interference shielding properties of ferrocene-modified polycarbosilane derived SiC/C composite ceramics

In order to enhance the dielectric and electromagnetic interference shielding (EMI) properties, the SiC/C composite ceramics were fabricated by pyrolysis of ferrocene-modified polycarbosilane. The microstructure evolutions, dielectric properties, EMI and microwave absorption properties of SiC/C composite ceramics were investigated. The increases of both ferrocene contents and annealing temperatures led to the increases of crystallizations of SiC and carbons. Crystallized carbons including carbon nanowires, turbostratic carbons, onion-like carbons and graphene-like carbons were obtained in the materials. The carbon nanowires were longest when the 5 wt.% ferrocene-modified polycarbosilane was annealed at 1250 °C. These carbons played a more important role than SiC in the increases of dielectric and EMI properties. The average real and imaginary permittivities of materials increased from 4.4 and 0.7 to 38.9 and 39.6, respectively. The materials exhibited high total shielding effectiveness, high absorption shielding effectiveness and low reflection shielding effectiveness, which were 36.6, 30.1 and 6.5 dB, respectively.     

Effect of temperature gradient on the erosion behavior of SiC coating for carbon/carbon composites in a combustion environment

SiC coating with a thickness of 50–70 µm was prepared on the surface of C/C composites by in-situ reaction method. The SiC coated C/C composites were then tested in a wind tunnel where a temperature gradient from 200 to 1600 °C could be obtained to investigate their erosion behavior. The results of wind tunnel test indicated that the service life of C/C composites was prolonged from 0.5 to 44 h after applying the SiC coating. After the wind tunnel test, three typical oxidation morphologies, including glassy SiO₂ layer, porous SiO₂ layer and clusters of honeycomb-like SiO₂ grains, were found on the SiC coated C/C composites. With the decrease of oxidation temperature, the amount of glassy SiO₂ declined and the thermal stress increased, which induced the cracking followed by the degradation of the SiC coating.     

Ablation resistance of HfC coating reinforced by HfC nanowires in cyclic ablation environment

To improve the ablation resistance of carbon/carbon composites in cyclic ablation environment, SiC/HfC ceramic coating reinforced by HfC nanowires was prepared. The microstructure, bonding strength, coefficient of thermal expansion and cyclic ablation resistance of the as-prepared coating were investigated. After incorporating HfC nanowires, the bonding strength between inner SiC coating and outer HfC coating was increased. HfC nanowires could relieve the coefficient of thermal expansion mismatch between inner and outer coating and improve the toughness of the outer coating. By introducing HfC nanowires, the coated sample’s cyclic ablation resistance was improved. After cyclic ablation under oxyacetylene flame for 60 s × 3, the mass and linear ablation rates of the coated sample with HfC nanowires were only 0.444 mg/s and −0.767 μm/s, respectively.     

Effect of SiC coating and heat treatment on the thermal radiation properties of C/SiC composites

The effects of SiC coating and heat treatment on the emissivity were investigated for 2D C/SiC composites prepared by CVI in the 6–16 μm range. SiC coating had an obvious effect on the spectral emissivity of the composites but caused just 5% difference in the total emissivity. A radiation transport model was applied to explain those changes caused by SiC coating. Heat treatment affected the thermal radiation properties of the composites through the microstructure evolution. Base on the complementary analytical techniques, the changes in the emissivity were attributed to a good graphitization degree of carbon phases, large β-SiC grain sizes and high α-SiC content resulting in high emissivity.