Oxidation resistance and strength retention of ZrB2–SiC ceramics

Oxidation behavior and effect of oxidation on the room-temperature flexural strength were investigated for ZrB₂–10 vol% SiC (ZB10S) and ZrB₂–30 vol% SiC (ZB30S) in air at 1500 °C with times ranging from 0.5 h to 10 h. The oxide scale of both ZB10S and ZB30S was composed of an outer glassy layer and an inner extended SiC-depleted layer. The changes in weight gain, glass layer thickness, and extended SiC-depleted layer thickness with oxidation were measured. Analysis suggested that the extended SiC-depleted layer was most indicative for evaluating the oxidation resistance. Compared to the ZB10S, the improved oxidation resistance in ZB30S was attributed to the viscosity increase of glassy layer and the lower number of ZrO₂ inclusions in the glassy layer. Because of the healing of surface flaws by the glassy layer, the strength increased significantly by ～110% for ZB10S and by ～130% for ZB30S after oxidation for 0.5 h.     

Microstructure and tribological properties of PIP-SiC modified C/C–SiC brake materials

A combination method of precursor infiltration and pyrolysis (PIP), chemical vapor infiltration (CVI) and liquid silicon infiltration (LSI) was proposed to prepare PIP-SiC modified C/C–SiC brake materials. The SiC ceramic matrix pyrolyzed by polymethysilane (PMS) homogeneously dispersed in the fiber bundles region, which improved the plough resistance of local C/C region and the wear resistance of C/C–SiC brake materials. When the braking speed rises to 28 m/s, the fluctuation range of friction coefficient was limited to 0.026. The linear wear rate of the as-prepared composites was could be ~50% less than that of C/C–SiC, when the braking speed was above 15 m/s (for instance, the wear rate of 1.02 μm/(side·cycle) at 28 m/s less than 2.02 μm/(side·cycle) of traditional C/C– SiC). The fading ratio D of CoF under wet conditions was ~11%. The results showed that introducing PIP-SiC could stabilize the braking process and effectively prolong the service life of C/C–SiC brake materials.     

Tribological behavior and wear mechanism of C/C–SiC brake discs based on third-body layer

C/C–SiC composites are promising candidates for heavy-duty tracked vehicle brake discs. A third-body layer (TBL) can be formed on the surface of C/C–SiC self-mated brake discs, which has an important impact on tribological behavior and wear mechanism of brake discs. Herein, the formation conditions and evolution process of TBL and its effect on friction and wear properties were investigated. An appropriate braking pressure and speed (P and V) are beneficial to the cutting of asperities and refinement of wear debris on the contact surface, which are preconditions for the formation of original TBL. The original TBL can be formed under the P·V of 12, 15, and 16, which effectively improve braking stability and reduce the wear rate. During the continuous braking process, the original TBL undergoes growth, stabilization, destruction, and regeneration. Under the frictional heat and compressive stress, wear debris gradually evolves into a uniform and dense TBL. The average coefficient of friction and wear rate reach to the lowest value of .446 and 38.5 × 10⁻³ cm³/MJ, respectively. A continuous high temperature in the later stages of braking leads to severe oxidative wear. The newly formed TBL covers the original surface to form a multilayered structure, indicating the TBL undergoes destruction and regeneration.     

Friction and wear properties of C/C–SiC braking composites

Two series of C/C–SiC composites were fabricated via precursor infiltration pyrolysis (PIP) and chemical vapor infiltration (CVI) using porous C/C composites with different original densities as preforms, respectively. The tribological characteristics of C/C–SiC braking composites were investigated by means of MM-1000 type of friction testing machine. The friction and wear behaviors of the two series of composites were compared and the factors that influence the friction and wear properties of C/C–SiC composites were discussed. Results show that the friction and wear properties relate close-knit to the content of SiC and porosity. As the original preform density increasing, the content of SiC and porosity decrease, and then the friction coefficient increases obviously, the braking time and the wear rate both decrease. Preparation techniques play an important role in the tribological properties of C/C–SiC composites. Compared with PIP process, the samples from CVI have a little higher friction coefficient, shorter braking time and higher wear rate.     

Fabrication and characterization of B4C–ZrB2–SiC ceramics with simultaneously improved high temperature strength and oxidation resistance up to 1600 °C

B₄C–30 vol% ZrB₂ and B₄C–30 vol% ZrB₂–10 vol% SiC ceramics were prepared using hot pressing, and their room temperature flexural strength, high temperature flexural strength and oxidation behavior were investigated and compared each other. Both room temperature and high temperature flexural strength were improved by adding SiC particles. The oxidation mechanism was also studied, showing the oxidation product of SiC sealed the porosity and cracks, which was helpful to high temperature strength and oxidation resistance improvement.     

The high temperature reaction of ammonia with carbon and SiC–C ceramics

This contribution aimed at developing a treatment under ammonia in order to eliminate free carbon from the surface of SiC-based fine ceramics like fibers or coatings. The reaction of NH₃ with graphitic and non-graphitic carbon was first investigated through kinetic measurements, in situ gas phase analysis and physicochemical investigations of the solid. The carbon etching rate is controlled by heterogeneous reactions involving active sites arising from bulk structural defects and the formation of HCN. A selection of SiC-based fibers and coatings with various carbon contents and (micro)structures was treated in ammonia in favorable conditions. The analyses of the tested SiC–C specimens revealed a reduction of the free carbon content and, simultaneously, a nitridation of the initial Si–C–(O) continuum over a reaction layer. The growth rate, composition and the volume change of this layer vary with the initial microstructure. The ammonia treatment is able to restore the adhesion of carbon-contaminated surfaces.     

Effect of fiber architecture and density on the ablation behavior of carbon/carbon composites modified by Zr–Ti–C

Three carbon/carbon (C/C) composites modified by Zr–Ti–C, with different fiber architecture in preforms and the same density, were prepared using chemical vapor infiltration and reactive melt infiltration methods. Two other samples with the same architecture in preforms and different density were also fabricated by the same methods. Their ablation behaviors were examined by oxy-acetylene flame. The results showed that the samples with chopped web needled perform had better ablation resistance than that of the samples with needle-integrated and fine-weave pierced perform. In the models of ablation behaviors, the sealing time of pores and gaps on the ablated surfaces has been defined to indirectly estimate the ablation property. The analysis of models also indicated that high density of the composites and appropriate small diameter of bundles of carbon fibers led to the short sealing time and good ablation resistance of the C/C–carbide composites.     

Ablation resistance and mechanism of SiC–LaB6 and SiC–LaB6–ZrB2 ceramics under plasma flame

In this study, silicon carbide-lanthanum hexaboride (SiC–LaB₆) and silicon carbide–lanthanum hexaboride–zirconium boride (SiC–LaB₆–ZrB₂) ceramics were fabricated by spark plasma sintering at 1900 °C, and their ablation resistance was tested under plasma flames over 2300 °C. The results indicate that the SiC–LaB₆–ZrB₂ ceramic exhibits better ablation resistance than the SiC–LaB₆ ceramic. After ablation under the plasma flame for 60 s, the mass and linear ablation rates of the SiC–LaB₆ ceramic were 15.83 μg/s and 1.08 μm/s, respectively, while those of SiC–LaB₆–ZrB₂ were -8.42 μg/s and -0.27 μm/s. With the addition of ZrB₂, SiC–LaB₆–ZrB₂ ceramic attained a high density and fewer inner oxygen diffusion channels. Moreover, the ZrO₂–La₂O₃–SiO₂ oxide scale with good self-healing ability and excellent stability was formed in the ablation centre, which can retard the further oxidation during ablation.     

Oxidation behaviour of C/C–SiC brake discs tested on full-scale bench rig

C/C–SiC composites are considered to be strong candidates for the new generation of high-speed train brake discs. To achieve a better application, it is necessary to improve understanding of the oxidation behaviour of C/C–SiC brake discs after a full-scale bench test rig. In this study, full-scale braking bench tests for C/C–SiC self-mated brake pairs were conducted under a braking speed of 350–420 km/h and a braking pressure of 17–28 kN. Moreover, the oxidation behaviour and mechanisms of the C/C–SiC brake discs during the practical braking process were investigated. The results indicate that the oxidation behaviour is highly dependent on the friction surface region of the C/C–SiC brake disc owing to the distribution of microcracks, the formation of friction films, the difference in temperature, and the contact content with O₂. Specifically, the oxidation depths of the friction layer on the inner circumferential surface, middle friction surface, and outer circumferential surface were 278.3, 252.1, and 359.9 μm, respectively. Furthermore, the oxidation reaction preferentially occurs in the active area of the C fibre and pyrolytic carbon (PyC) during the braking process.     

Flexural strength and fracture behavior of ZrB2–SiC ultra-high temperature ceramic composites at 1800 °C

ZrB₂–15 vol.%SiC and ZrB₂–30 vol.%SiC composites with smaller starting particle sizes in which the particle sizes of ZrB₂ and SiC are 2 μm and 0.5 μm, respectively, demonstrated marked plasticity and significant reduction in the flexural strength at 1800 °C. The flexural strengths of these two composites are 112 ± 12 MPa and 48 ± 10 MPa, respectively, and their corresponding strength retentions are 13% and 7%, respectively. Large ZrB₂ grains were commonly observed in the samples containing 15 vol.%SiC, which are always the sites for the crack initiation. Cavities were found in the samples containing 30 vol.%SiC and the grain boundaries are the main sites for the crack and cavity nucleation. To improve ultra-high temperature strength, larger starting particle sizes (ZrB₂ and SiC are 5 μm and 2 μm, respectively) were used for the preparation of ZrB₂–15 vol.%SiC. This sample fractured in an elastic manner up to 1800 °C and showed a very high strength with a value of 217 ± 16 MPa.     

Effect of SiC nanowires on the thermal shock resistance of joint between carbon/carbon composites and Li2O–Al2O3–SiO2 glass ceramics

In order to improve the bonding property of joint between SiC modified carbon/carbon (C/C) composites and Li₂O–Al₂O₃–SiO₂ (LAS) glass ceramics, SiC nanowires were attempted as the reinforcement materials in the interface region of SiC transition layer and Li₂O–MgO–Al₂O₃–SiO₂ (LMAS) gradient joining interlayer. The C/C–LAS joint with SiC nanowire-reinforced interface layer was prepared by a three-step technique of pack cementation, in situ reaction and hot-pressing. The microstructure and thermal shock resistance of the as-prepared joints were examined. The average shear strength of the joined samples with SiC nanowires increased from 24.9 MPa to 31.6 MPa after 40 thermal cycles between 1000 °C and room temperature, while that of the joined samples without SiC nanowires dropped from 21.4 MPa to 8.3 MPa. The increase of thermal shock resistance of the C/C–LAS joints was mainly attributed to the toughening mechanism of SiC nanowires by pullout, bridging and crack deflection.     

Anisotropic tribological behavior of LSI based 2.5D needle-punched carbon fiber reinforced Cf/C–SiC composites

C_f/C–SiC composites were fabricated via liquid silicon infiltration with 2.5D needle-punched carbon fiber reinforced C_f/C composites. The effect of surface topography and carbon content of the C_f/C–SiC composites on the tribological properties was researched by the ball-on-disk reciprocating tribometer. The results indicate that different fiber layers and cross-section of the composites have various surface topography and show significant differences in the friction and wear properties. By the wear morphology and model analyses, the reason for the tribological anisotropy of the composites is that the distribution of carbon and SiC phases in the composites are inhomogeneous caused by the difference of the carbon fiber orientation and the relative content in each layer. Moreover, the wear rate of the short-cut fiber web layer was the lowest and there is an obvious linear decrease in coefficient of friction with increase of carbon content. The present work explains why the tribological properties of the composites are inconsistent and provides a way to adjust the friction properties of composite materials by optimizing the friction surface.     

Fabrication and characterization of biomorphic cellular C/SiC–ZrC composite ceramics from wood

Biomorphic cellular C/SiC–ZrC composite ceramics were fabricated from pine and oak wood precursors. Carbonaceous preforms were first prepared by wood pyrolysis and subsequently infiltrated with polyzirconobutanediol (PZC) and polycarbosilane (PCS) to form the composite ceramics. TGA/DTG and dilatometric analysis were used to study the pyrolysis of the wood precursor. XRD and SEM analyses were applied to characterize the microscopic properties of the resulting biomorphic cellular C/SiC–ZrC composite ceramics. Compared with oak, pine was preferable for preparation of cellular C/SiC–ZrC composite ceramics because of its unique microstructure. The SiC–ZrC phase distribution differed within the composite ceramics. In addition, the compression strengths of wood, charcoal, and cellular C/SiC–ZrC composite ceramics were measured in the axis direction. Results showed the improved compression strength of biomorphic cellular C/SiC–ZrC composite ceramics when the impregnation cycles were repeated.     

Enhanced bonding strength and thermal cycling performance of MoSi2–CrSi2–SiC–Si coating for carbon/carbon composites by surface modification via blasting treatment

Before the preparation of MoSi₂–CrSi₂–SiC–Si coating, blasting treatment of carbon/carbon (C/C) composites, as a surface modification method, was conducted under oxyacetylene torch. MoSi₂–CrSi₂–SiC–Si coating was prepared on the treated C/C composites by pack cementation, where an interlock interface was formed between the coating and the C/C substrate. After blasting treatment, the thermal expansion coefficient mismatch between the coating and C/C substrate was alleviated efficiently, and the bonding strength of the coating was increased by 45.6% and reached 26.2 MPa. To simulate the real working condition, thermal cycling test was conducted under oxyacetylene torch from 1600 °C to room temperature to construct an environment of combustion gas erosion. Due to the improvement of bonding strength and the alleviation of thermal expansion coefficient mismatch between the coating and the C/C substrate, thermal cycling performance of MoSi₂–CrSi₂–SiC–Si coating was enhanced. After 25 thermal cycles, the mass loss of the coated C/C composites without blasting treatment was up to 2.4%, and the C/C substrate was partially exposed. In contrast, the mass loss of the coated C/C composites with blasting treatment was only 1.1%.     

Ablation mechanism of C/C–SiC and C/C–SiC–ZrC composites in hypersonic oxygen-enriched environment

In this study, C/C–SiC and C/C–SiC–ZrC composites were prepared via chemical vapor infiltration and polymer infiltration pyrolysis, and the ablation mechanism under hypersonic oxygen-rich environmental conditions was investigated. The C/C–SiC composites demonstrate an excellent ablation resistance in a hypersonic oxygen-rich environment with a relatively low temperature and speed of approximately 1800 K and 1100 m/s, respectively. It is only in the ablation center area with higher temperatures that a certain degree of thermochemical ablation was observed. The mass and linear ablation rates of C/C–SiC composites (0.027 g/s and 0.117 mm/s, respectively) showed a significant increase in a hypersonic oxygen-rich environment with a temperature and velocity of approximately 2050 K and 2000 m/s, respectively. The high-temperature ablation resistance of ZrC-modified C/C–SiC–ZrC composites improved significantly. However, the ZrC ceramic component had a considerable impact on the ablation resistance of the material. The structural integrity of C/C–20SiC–30ZrC composites was relatively high in hypersonic oxygen-rich environments with a jet temperature and velocity of 2050 K and 2000 m/s, respectively, and mass and linear ablation rates were 0.012 g/s and 0.015 mm/s, respectively. When the ZrC content increased by 40%, the ablation resistance of the composite reduced significantly, whereas the mass and linear ablation rates increased to 0.043 g/s and 0.130 mm/s, respectively.     

Oxidation resistance and thermal cycling properties of the SiCnws–SiC coating on the C/SiC composites

SiC coatings reinforced with SiC nanowires were prepared on carbon/silicon carbide (C/SiC) composites through chemical vapor reaction route and chemical vapor deposition (CVD). The SiC nanowires were introduced to mainly improve the interface bonding properties of the coating and C/SiC composites. The microstructure, phase composition, thermal cycling, and bonding strength of the SiCnws–SiC coating were investigated. After nine thermal cycles, the weight loss of the SiCnws–SiC-coated C/SiC composites was only 4.6 wt.%. Tensile test results show that the tensile strength of the SiCnws–SiC-coated C/SiC composites was more than 4.5–4.6 MPa. The introduction of SiC nanowires effectively improved interface bonding strength, thus enhancing the thermal cycling and mechanical properties of the coating.     

Fabrication and mechanical properties of laminated HfC–SiC/BN ceramics

Laminated HfC–SiC/BN ceramics were successfully fabricated by tape casting and hot pressing. Fully dense HfC–SiC ultra-high temperature ceramics with homogeneous structure were obtained. The introduction of the weak BN layer resulted in a slight decrease of the flexural strength but significantly improved the fracture toughness compared with monolithic HfC–SiC ceramics. The fracture toughness of laminated HfC–SiC/BN ceramics in the parallel direction peaked at 8.06 ± 0.46 MPa m^1/2, which increased by 115% than that of monolithic HfC–SiC ceramics. The composites showed non-catastrophic fracture behaviors in both parallel and perpendicular directions. It indicates that laminated structure design is a promising approach to obtain full density HfC–SiC ceramics with high fracture toughness.     

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.     

Microstructure and ablation mechanism of C/C–SiC composites

C/C–SiC composites were prepared by molten infiltration of silicon powders, using porous C/C composites as frameworks. The porosities of the C/C–SiC composites were about 0.89–2.8 vol%, which is denser than traditional C/C composites. The ablation properties were tested using an oxyacetylene torch. Three annular regions were present on the ablation surface. With increasing pyrocarbon fraction, a white ceramic oxide layer formed from the boundary to the center of the surface. The ablation experimental results also showed that the linear and mass ablation rates of the composites decreased with increasing carbon fraction. Linear SiO₂ whiskers of diameter 800 nm and length approximately 3 μm were formed near the boundaries of the ablation surfaces of the C/C–SiC composites produced with low-porosity C/C frameworks. The ablation mechanism of the C/C–SiC composites is discussed, based on a heterogeneous ablation reaction model and a supersaturation assumption.     

Ablation resistance of HfC–SiC coating prepared by supersonic atmospheric plasma spraying for SiC-coated C/C composites

In order to improve the ablation properties of carbon/carbon composites, HfC–SiC coating was deposited on the surface of SiC-coated C/C composites by supersonic atmospheric plasma spraying. The morphology and microstructure of HfC–SiC coating were characterized by SEM and XRD. The ablation resistance test was carried out by oxyacetylene torch. The results show that the structure of coating is dense and the as-prepared HfC–SiC coating can protect the C/C composites against ablation. After ablation for 30 s, the linear ablation rate and mass ablation rate of the coating are −0.44 μm/s and 0.18 mg/s, respectively. In the ablation center region, a Hf–Si–O compound oxide layer is generated on the surface of HfC–SiC coating, which is conducive to protecting the C/C composites from ablation. With the ablation time increasing to 60 s, the linear ablation rate and mass ablation rate are changed to −0.38 μm/s and 0.26 mg/s, respectively. Meanwhile, the thickness of the outer Hf–Si–O compound layer also increases.