Effects of SiC on the microstructures and mechanical properties of B4C–SiC–rGO composites prepared using spark plasma sintering

In this study, B₄C–SiC–rGO composites with different SiC contents were prepared by spark plasma sintering at 1800 °C for 5 min under a uniaxial pressure of 50 MPa. The effects of SiC on the microstructures and mechanical properties of the B₄C–SiC–rGO composites were investigated. The optimal values for flexural strength (545.25 ± 23 MPa) and fracture toughness (5.72 ± 0.13 MPa·m^1/2) were obtained simultaneously when 15 wt.% SiC was added to 5 wt.%–GO reinforced B₄C composites (BS15G5). It was found that SiC and rGO inhibited the grain growth of B₄C and improved the mechanical properties of the B₄C–SiC–rGO composites. The clear and narrow grain boundaries of rGO–B₄C and rGO–SiC, as well as the semi-coherent B₄C–SiC interface, indicated strong interface compatibility. The twin structures of SiC and B₄C observed in the composites improved their fracture toughness. Crack deflection and crack bridging caused by the SiC grains as well as rGO bridging and rGO pull-out were observed on the crack propagation path.     

Effect of Co addition on microstructural and mechanical properties of WC–B4C–SiC composites

In this study, the effect of Co addition on microstructural and mechanical properties of WC-B₄C–SiC composites sintered by spark plasma sintering (SPS) method was investigated. For this purpose, three batches of WC-B₄C–SiC with different contents of Co (10 vol%, 15 vol%, and 20 Vol %) were sintered at 1400 °C. The results of X-ray diffraction (XRD) analysis of the samples indicated the formation of W₂B₅, W₃CoB₃ as well as the remained C phases and unreacted SiC phase. It was observed that by increasing the Co content, the amount of W₂B₅ phase reduces and W₃CoB₃ and C contents increase. Therefore, W₂B₅ peaks were not detected in the sample containing 20vol% Co. Relative density values above 97% were obtained for all the composites. However, a decrease was observed in relative density by increasing the Co content in the composites. The highest flexural strength (510 ± 42 MPa), fracture toughness (10.34 ± 0.82 MPa m^1/2), and hardness (20.63 ± 0.75 GPa) were also obtained for the sample containing 10vol% Co compared to the other samples. In addition, Transgranular fracture of SiC as well as pulling out of W₃CoB₃ and W₂B₅ particles were observed in the fracture surface micrographs of the samples. The presence of micro-cracks in the SiC grains, fracture of W₃CoB₃ grains, and crack deflection was reported as dominant toughening mechanisms.     

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.     

Microstructures and mechanical properties of B4C–SiC and B4C–SiC–TiB2 ceramic composites fabricated by hot pressing

Boron carbide (B₄C) ceramic composites with excellent mechanical properties were fabricated by hot-pressing using B₄C, silicon carbide (SiC), titanium boride (TiB₂), and magnesium aluminum silicate (MAS) as raw materials. The influences of SiC and TiB₂ content on the microstructural evolution and mechanical properties of the composites were systematically investigated. The mechanism by which MAS promotes the sintering process of composites was also investigated. MAS exists in composites in the form of amorphous phase. It can effectively remove the oxide layer from the surface of ceramic particles during the high temperature sintering process. The typical values of relative density, hardness, bending strength, and fracture toughness of B₄C–SiC–TiB₂ composites are 99.6%, 32.61 GPa, 434 MPa, and 6.20 MPa m^1/2, respectively. Based on the microstructure observations and finite element modeling, the operative toughening mechanism is mainly attributed to the crack deflection along the grain boundary, which results from the residual stress field generated by the thermal expansion mismatch between B₄C and TiB₂ phase.     

Effects of high-temperature annealing on the microstructure and properties of C/SiC–ZrC composites

C/SiC–ZrC composites were prepared by a combining slurry process with precursor infiltration and pyrolysis, and then annealed from 1200 °C to 1800 °C. With rising annealing temperature, their mass loss rate increased, and the flexural strength and modulus decreased from 227.9 MPa to 41.3 MPa and from 35.3 GPa to 22.7 GPa, respectively. High-temperature annealing, which elevated thermal stress and strengthened interface bonding, was harmful to the flexural properties. However, it improved the ablation properties by increasing the crystallization degree of SiC matrix. The mass loss rate and linear recession rate decreased with increasing annealing temperature and those of the samples annealed at 1800 °C were 0.0074 g/s and 0.0011 mm/s respectively. Taking mechanical and ablation properties into consideration simultaneously, the optimum annealing temperature was 1600 °C.     

Effect of Al addition on the single and cyclic ablation properties of C/C–SiC composites

This article focuses on the damage behavior and mechanism of aluminum addition on reactive melt infiltrated C/C–SiC composites in single and cyclic ablation environments. Plasma ablation tests were performed on C/C–SiC composites containing 20 wt % and 40 wt % aluminum respectively. Coupled with TMA, XRD, SEM and EDS, the results showed that composites with 40 wt % Al had better ablation resistance during the cyclic ablation, while the composites with 20 wt % Al had excellent ablation damage resistance during a single ablation. This difference was due to higher number of microcracks formed inside the composites containing 40 wt % Al than 20 wt % Al, the lower specimen surface temperature during ablation, and the thermal stresses can be released by pore crack expansion during gas reciprocal loading. While in the single continuous loading of gas, the 20 wt % Al composite formed a protective oxide layer with smaller pores and fewer gas and oxygen entry channels, resulting in good resistance to ablation.     

Influence of annealing on the mechanical properties of SiC–Si composites with sub-micron SiC microstructures

The influence of annealing temperature (1000, 1100 and 1200°C) on the mechanical properties of SiC–Si composites has been evaluated. Three SiC powders with particle sizes in the range of 0.24 to 0.7 μm were used to produce the composites. Before application the SiC powders were treated with hydrofluoric acid to remove the extent of SiO₂. With this treatment a successful infiltration of green-bodies especially produced of SiC powder with a mean particle size of 0.24 μm was possible. The bending strength decreased with decreasing SiC starting particle size as well as with increasing annealing temperature. However, the fracture toughness was independent on SiC starting particle size and annealing temperature. XRD diffraction analysis showed that internal stress, expressed by broadening of XRD peaks, is low and had no effects on the mechanical properties of the composites.     

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.     

Preparation and ablation properties of SiC nanowire-reinforced ZrC–SiC coating-matrix integrated C/C composites

A modification of the precursor infiltration pyrolysis (PIP) method was explored to prepare the integrated doped ceramic matrix and coating by the added SiC nanowires layer and shape-stabilization process. The epitaxial layer of SiC nanowires provided surficial attachments for the precursor. And the shape-stabilization process aggregated loose ceramic particles into a coating. Then the SiC nanowire-reinforced ZrC–SiC coating-matrix integrated C/C (S/SZ-CZ/C) composite was simply prepared by the modified PIP method. The bonding strength between the coating and matrix of the S/SZ-CZ/C composite was improved. Through the ablation test, the mass and linear ablation rate of the S/SZ-CZ/C composite were 0.46 mg/s and 0.67 μm/s, which were 60.34 % and 74.91 % lower than those of the SiC nanowire-reinforced C/C–ZrC (S/CZ/C) composite, respectively. The integration of the coating and matrix enabled the formation of a continuous oxide layer of molten SiO₂ and ZrO₂ in the ablation process, which helped to block the oxygen and heat during the ablation test. Thus the ablation resistance of the materials was systematically and effectively improved.     

Effects of SiC content on the densification,microstructure, and mechanical properties of HfB2–SiC composites

To investigate the effects of SiC on microstructure, hardness, and fracture toughness, 0, 10, 20, and 30 vol% SiC were added to HfB₂ and sintered by SPS. Upon adding SiC to 30 vol%, relative density increased about 4%; but HfB₂ grain growth had a minimum at 20 vol% SiC. This may be due to grain boundary silicate glass, responsible for surface oxide wash out, enriched in SiO₂ with higher fraction of SiC. By SiO₂ enrichment, the glass viscosity increased and higher HfO₂ remained unsolved which subsequently lead to higher grain growth. Hardness has increased from about 13 to 15 GPa by SiC introduction with no sensible variation with SiC increase. Residual stress measurements by Rietveld method indicated high levels of tensile residual stresses in the HfB₂ Matrix. Despite the peak residual stress value at 20 vol% SiC, fracture toughness of this sample was the highest (6.43 MPa m^0.5) which implied that fracture toughness is mainly a grain size function. Tracking crack trajectory showed a mainly trans-granular fracture, but grain boundaries imposed a partial deflection on the crack pathway. SiC had a higher percentage in fracture surface images than the cross-section which implied a weak crack deflection.     

Processing of reaction-bonded B4C–SiC composites in a single-mode microwave cavity

In this study, the reaction sintering of boron carbide, which consists in doing reactive infiltration of molten silicon throughout a porous sample made of B₄C and carbon graphite was investigated. Thus, it has been shown that a single-mode microwave cavity can be successfully used to produce reaction-bonded B₄C–SiC composite. A specific package, consisting of a SiC based susceptor and a boron nitride based insulating container, was used to heat up the B₄C–Si system using a single-mode microwaves cavity under an Ar–H₂ atmosphere. Pore-free B₄C–SiC composite successfully produced consists of a mixture of B₄C and polygonal shaped β-SiC within a residual silicon matrix. The indentation technique permits to determine mechanical properties of the samples which are compared to those obtained conventionally. It appears that the average hardness (H≈22 GPa) value is quite constant all along the sample thickness which highlights good homogeneity of the samples obtained. Some aspects of the microstructure are also discussed and compared to those of samples conventionally obtained.     

High-performance B4C–TiB2–SiC composites with tuneable properties fabricated by reactive hot pressing

In this work, we systematically studied the effects of powder characteristics (B₄C, TiC and Si powders) on the existential form of toughening phases (SiC and TiB₂) as well as the overall microstructure and properties of B₄C–TiB₂–SiC composites fabricated by reactive hot pressing. The particle size of the TiC powder plays a largely determining role in the development of novel toughening phases, the TiB₂–SiC composite structure, that are formed in the B₄C matrix, while the Si particle size affects the agglomerate level of the SiC phase. The TiB₂–SiC composite structure and SiC agglomerates enhance the fracture toughness, but decrease the flexural strength. Both the microstructure and mechanical properties of B₄C–TiB₂–SiC composites can be effectively tuned by regulating the combinations of the particle sizes of the starting powders. The B₄C–TiB₂–SiC composites demonstrate flexural strength, fracture toughness and Vickers hardness in the respective range of 567–632 MPa, 5.11–6.38 MPa m^1/2, and 34.8–35.6 GPa.     

Mechanical properties and deformation mechanisms of B4C–TiB2 eutectic composites

Samples of B₄C–TiB₂ eutectic are laser processed to produce composites with varying microstructural scales. The eutectic materials exhibit both load dependent and load independent hardness regimes with a transition occurring between 4 and 5 N indentation load. The load-independent hardness of eutectics with a microstructural scale smaller than 1 μm is about 31 GPa, and the indentation fracture toughness (5–10 N indenter load) of the eutectics is 2.47–4.76 MPa m^1/2. Indentation-induced cracks are deflected by TiB₂ lamellae, and indentation-induced spallation is reduced in the B₄C–TiB₂ eutectic compared to monolithic B₄C. Indentation-induced amorphization in monolithic B₄C and the B₄C phase of the eutectic is detected using Raman spectroscopy. Sub-surface damage is observed using TEM, including microcracking and amorphization damage in B₄C and B₄C–TiB₂ eutectics. Dislocations are observed in the TiB₂ phase of eutectics with an interlamellar spacing of 1.9 μm.     

Effect of heat treatment on the mechanical properties of PIP–SiC/SiC composites fabricated with a consolidation process

Continuous SiC fiber reinforced SiC matrix composites (SiC/SiC) have been considered as candidates for heat resistant and nuclear materials. Three-dimensional (3D) SiC/SiC composites were fabricated by the polymer impregnation and pyrolysis (PIP) method with a consolidation process, mechanical properties of the composites were found to be significantly improved by the consolidation process. The SiC/SiC composites were then heat treated at 1400 °C, 1600 °C and 1800 °C in an inert atmosphere for 1 h, respectively. The effect of heat treatment temperature on the mechanical properties of the composites was investigated, the mechanical properties of the SiC/SiC composites were improved after heat treatment at 1400 °C, and conversely decreased with increased heat treatment temperature. Furthermore, the effect of heat treatment duration on the properties of the SiC/SiC composites was studied, the composites exhibited excellent thermal stability after heat treatment at 1400 °C within 3 h.     

Effects of density and heat treatment of C/C preforms on microstructure and mechanical properties of C/C–SiC composites

Twill multidirectional carbon-fiber-reinforced carbon and silicon carbide composites (i.e., C/C–SiC) were prepared via chemical vapor infiltration combined with reactive melt infiltration process. The effect of heat treatment (HT) on the microstructure and mechanical properties of C/C–SiC composites obtained by C/C preforms with different densities was thoroughly investigated. The results show that as the bulk density of C/C preforms increases, the thickness of the pyrolytic carbon (PyC) layer increases and open pore size distribution narrows, making the bulk density and residual silicon content of C/C–SiC composites decrease. Moreover, the flexural strength and tensile strength of the C/C–SiC composites were improved, which can be attributed to the increased thickness of the PyC layer. The compressive strength reduces due to the decrease of the ceramic phase content. HT improves the graphitization degree of PyC, which reduces the silicon–carbon reaction rate and thereby the content of the SiC phase. HT induces microcracks and porosity but not obviously affects the mechanical properties of C/C–SiC composites. However, the negative impact of HT can be compensated by the increased density of the C/C preforms.     

Influence of SPS temperature on the properties of TiC–SiCw composites

Titanium carbide (TiC) composites containing 10 vol% silicon carbide whisker (SiC_w) were spark plasma sintered at different temperatures of 1800, 1900, and 2000 °C under a pressure of 40 MPa and a holding time of 7 min. At the sintering temperature of 1900 °C, the relative density, Vickers hardness, and flexural strength of the sintered samples hit their maximum values of 98.7%, 24.4 GPa, and 511 MPa, respectively. The microstructural characteristics of the sintered samples were assessed by optical and field emission scanning electron microscopy (FESEM) and XRD. The results revealed that at 1900 °C, the dispersion of SiC_w in the TiC matrix was homogenous, no chemical reaction took place between the reinforcement and the matrix, and produced a fine-grained microstructure. It was found that the thermal conductivity of SPSed samples did not have the same trend with relative density and mechanical properties. A maximum value of 32.3 W/mK was measured for the thermal conductivity of the composite sintered at 2000 °C.     

Processing–microstructure–properties relationships of MoSi2–SiC composites

Silicon carbide green bodies with and without carbon-fibre reinforcement have been infiltrated with MoSi₂–Si–X in order to produce high-temperature resistant materials. X is Cr, Ti, Al or B respectively. By adding silicon and one of these components to MoSi₂ the melting point is lowered dramatically. The composites therefore could be gained by melt infiltration at max. 1600 °C. During infiltration the additives react within the infiltrated body with carbon or silicon to form high-temperature resistant carbides or silicides. Thermodynamic calculations have been performed to analyse the reactions during infiltration. The infiltration parameters have been studied with respect to the resulting microstructure and properties. By fitting the amount of additives to the quantity of carbon in the SiC-body (or vice versa) no decrease in strength could be observed up to 1500 °C. The fracture toughness can be increased by the use of high-modulus carbon fibres. The most promising X-element for a high-temperature resistant material is titanium.     

Effect of impregnated phenolic resin on the properties of Si–SiC ceramic matrix composites fabricated by SLS-RMI

Selective laser sintering (SLS) combined with reaction melt infiltration was used to fabricate Si–SiC ceramic matrix composites, and the effects of different concentrations of phenolic resin (PF) on the properties of the SLS green body and carbonized and final Si–SiC samples were investigated. The results showed that the impregnation with PF can increase the bulk density, reduce the porosity of the samples at all stages, and improve the mechanical properties of the reactive bonded samples. The degree of densification and mechanical properties of the sample gradually enhanced with an increase in PF concentration. The main phases of the Si–SiC composites were free Si, α-SiC, β-SiC, plus an extremely small amount of Al–Si alloy, and the SiC and the Si phase contents increased and decreased, respectively, as the concentration of PF increased when measured using Rietveld refinement and image analysis software. The macroscopic properties of the samples improved greatly after precursor infiltration pyrolysis (PIP) treatment with 66.7%vol PF-ethanol solution twice. According to the crystal nucleation-growth theory, it was inferred that the infiltrated PF could provide a certain amount of pyrolytic carbon in the carbonized specimen. During the reaction bonded process, the carbon formed by carbonization pyrolysis first dissolves into the molten Si and reaches saturation. With the further dissolution of carbon, [C] and [Si] in the liquid phase contact each other to form β-SiC nuclei, the nuclei that precipitate at the pore wall position and gradually form a continuous interfacial layer of β-SiC. The β-SiC layer prevents the liquid Si from direct contact with C inside the prefabricated body, therefore, further reactants diffuse through the layer. Finally, the fine crystalline β-SiC grains were fabricated inside the specimen.     

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 properties of B4C–CrB2 binary eutectic composites prepared by arc-melting

B₄C–CrB₂ composites were prepared by arc-melting using B₄C and CrB₂ powders as raw materials. The eutectic composition of B₄C–CrB₂ system was 30B₄C–70CrB₂ (mol%) with a labyrinth-like irregularly layered eutectic microstructure, composed of B₄C phase about 1–2 μm in thickness dispersing in CrB₂ matrix, much smaller than raw powders. The interface of the eutectic composite was well bonded, and there were edge dislocations at the interface to alleviate the interface mismatch. The eutectic temperature of B₄C–CrB₂ composites was approximately 2200 K. At the eutectic composition, the B₄C–CrB₂ composites showed the maximum Vickers hardness (24.6 GPa) and fracture toughness (4.3 MPa m^1/2) at room temperature.