Fabrication of cylindrical SiCf/Si/SiC-based composite by electrophoretic deposition and liquid silicon infiltration

Cylindrical SiC-based composites composed of inner Si/SiC reticulated foam and outer Si-infiltrated SiC fiber-reinforced SiC (SiC_f/Si/SiC) skin were fabricated by the electrophoretic deposition of matrix particles into SiC fabrics followed by Si-infiltration for high temperature heat exchanger applications. An electrophoretic deposition combined with ultrasonication was used to fabricate a tubular SiC_f/SiC skin layer, which infiltrated SiC and carbon particles effectively into the voids of SiC fabrics by minimizing the surface sealing effect. After liquid silicon infiltration at 1550 °C, the composite revealed a density of 2.75 g/cm³ along with a well-joined interface between the inside Si/SiC foam and outer SiC_f/Si/SiC skin layer. The results also showed that the skin layer, which was composed of 81.4 wt% β-SiC, 17.2 wt% Si and 1.4 wt% SiO₂, exhibited a gastight dense microstructure and the flexural strength of 192.3 MPa.     

The effect of alumina-based sintering aid on the microstructure,selected mechanical properties,and coefficient of friction of Cf/SiC composite prepared via spark plasma sintering (SPS) method

C_f-SiC air brake discs are being developed due to their high-temperature oxidation resistance compared to conventional C_f/C discs. The C_f-SiC air brake discs should have a coefficient of friction (COF) close to 0.4, a low wear rate, a density higher than 95% of the theoretical density, and flexural strength of more than 200 MPa. To reach the properties of C_f-SiC composite to the required characteristics of the air brake disc, different amounts of alumina-based sintering aid were used. For this purpose, first silicon carbide nanoparticles, sintering aids Al₂O₃–MgO, MgAl₂O₄, Al₂O₃–Y₂O₃, Al₂O₃–SiO₂–MgO, and carbon fiber (20 wt%) with a 5-mm length were prepared. Next, the final composite bulk was created via the SPS method at 1900 °C under a pressure of 50 MPa. The density of the sample sintered with the Al₂O₃–SiO₂–MgO sintering aid was higher than that of other sintering aids. The density value was obtained at 98% and 100% at 8 wt% and 4 wt% respectively. It was also found that the use of 4 wt% of Al₂O₃–SiO₂–MgO offered better mechanical properties compared to 8 wt%, due to the absence of Al₈Si₄O₂₀ phase at 4 wt%. The examination of mechanical properties showed that the hardness (3564 Vickers) and flexural strength (479 MPa) of the sample with the Al₂O₃–SiO₂–MgO sintering aid were higher than those of other sintering aids. The samples with the Al₂O₃–SiO₂–MgO sintering aid with 4 wt% revealed a COF of 0.41, showing the closest feature to the desired indices of aircraft brake discs.     

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.     

Addition of carbon fibers into B4C infiltrated with molten silicon

Boron carbide added with 0–20?wt% carbon fibers was subject to Si infiltration. Samples mainly consist of B₁₃C₂, β-SiC and unreacted Si. Some amount of SiB₆ and α-SiC was also detected, while formation of B₁₂(B,C,Si)₃ phase was suppressed due to short infiltration time. The carbon fibers react with Si and result in formation of a composite core-shell fiber with SiC-shell and C-core. Theoretical estimations suggest that these composite fibers have a strong influence on the enhancement of the bending strength. Although apparently in good agreement with experimental data showing an increase of bending strength up to 510?±?27?MPa in the sample with 10?wt% carbon fiber, the implications of phase changes with the carbon fiber amount has to be carefully considered. At higher amounts of carbon fibers, bending strength decreases.     

Fabrication and properties of Cf/Ta4HfC5-SiC composite via precursor infiltration and pyrolysis

In this study, a C_f/Ta₄HfC₅-SiC ultra-high-temperature ceramic matrix composite exhibiting a homogeneous phase distribution was successfully fabricated via precursor infiltration and pyrolysis processing. Initially, the pyrolysis and solid solution mechanisms exhibited by the Ta₄HfC₅ precursor were investigated and characterized through TG-MS and XRD analysis. The as-fabricated C_f/Ta₄HfC₅-SiC composite exhibited a density and open porosity of 2.84 g/cm³ and 10.62 vol%, respectively. It also exhibited outstanding mechanical properties, with a flexural strength of 339 ± 20 MPa and fracture toughness of 11.56 ± 0.77 MPa·m^1/2. The C_f/Ta₄HfC₅-SiC composite demonstrated strong ablation resistance under a heat flux of 5 MW/m² at ~2400℃, with corresponding linear and mass recession rates of 5.33 μm/s and 6.18 mg/s, respectively. The combination of strong mechanical properties and ablation resistance provides a solid basis for the use of the C_f/Ta₄HfC₅-SiC composite in a new generation of ultra-high-temperature materials.     

Preparation of hollow SiC spheres by combustion synthesis

Hollow spherical β-SiC was successfully prepared in argon by combustion synthesis using Si powder and polytetrafluoroethylene (PTFE) powder. The phase composition and morphology of spherical products can be controlled by adjusting the Si/C₂F₄ molar ratio (M_Si/(C2F4)). When M_Si/(C2F4) = 3, the phase content of β-SiC is the highest (up to 85.54%), and hollow spherical products obtained; When M_Si/(C2F4) ≥ 5, the Si/SiC microspheres are solid. The synthesis mechanism of hollow β-SiC microspheres is as follows: Si particles react with PTFE releasing heat. Then unreacted Si absorbs heat to form liquid phase microspheres, which is equivalent to the core template to form β-SiC microspheres by reaction with cracked C. Meanwhile, the silicon diffuses from the core to the shell to form the cavity. This method can synthesize the hollow spherical β-SiC in a simple way without prearranged spherical template and long synthesis cycle.     

Additive manufacturing of Csf/SiC composites with high fiber content by direct ink writing and liquid silicon infiltration

Direct ink writing (DIW) provides a new route to produce SiC-based composites with complex structure. In this study, we additive manufactured short carbon fiber reinforced SiC ceramic matrix composites (Csf/SiC composites) with different short carbon fiber content through direct ink writing combined with liquid silicon infiltration (LSI). The effects of short carbon fiber content on the microstructure and mechanical properties of the DIW green parts and the final Csf/SiC composites were investigated. The results showed that the Csf content played an important role in maintaining the structure of the green parts. As the Csf content increases, the dimension deviation ratio of the sample decreased at all stages. With the Csf content of 40 vol%, the final Csf/SiC composite had low free Si content and high β-SiC content. The maximum density, tensile strength and bending strength of the Csf/SiC composites were 2.88 ± 0.06 g/cm³, 53.68 MPa and 253.63 MPa respectively. It is believed that this study can give some understanding for the additive manufacturing of fiber reinforced ceramic matrix composites.     

Tribo-mechanical characterization of spark plasma sintered chopped carbon fibre reinforced silicon carbide composites

Short carbon fibre (C_f) reinforced silicon carbide (SiC) composites with 7.5 wt% alumina (Al₂O₃) as sintering additive were fabricated using spark plasma sintering (SPS). Three different C_f concentrations i.e. 10, 20 and 30 wt% were used to fabricate the composites. With increasing C_f content from 0 to 20 wt%, micro-hardness of the composites decreased ~28% and fracture toughness (K_IC) increased significantly. The short C_f in the matrix facilitated enhanced fracture energy dissipation by the processes of crack deflection and bridging at C_f/SiC interface, fibre debonding and pullout. Thus, 20 wt% C_f/SiC composite showed >40% higher K_IC over monolithic SiC (K_IC≈4.51 MPa m^0.5). Tribological tests in dry condition against Al₂O₃ ball showed slight improvement in wear resistance but significantly reduced friction coefficient (COF, μ) with increasing C_f content in the composites. The composite containing 30 wt% C_f showed the lowest COF.     

Effects of preform pore structure on infiltration kinetics and microstructure evolution of RMI-derived Cf/ZrC-ZrB2-SiC composite

Reactive melt infiltration (RMI) is often used to fabricate highly dense ceramic matrix composite by infiltration of alloy melt into porous preform. Here, C_f/B₄C-C preforms with various pore structures were prepared, and the effects of pore structure on the ZrSi₂ melt infiltration and the as-received C_f/ZrC-ZrB₂-SiC composites were investigated. Compared with the preform prepared by slurry impregnation (SI), the preform prepared by sol impregnation shows more uniform pore size distribution, which leads to more homogeneous melt infiltration, as well as more uniform formation of ZrC-ZrB₂-SiC and better mechanical properties in the composites. The calculation results of infiltration kinetics indicate that the pore radius decreases quickly during the melt infiltration. As the time needed for pore closure in sol-preform is longer than that in SI-preform, it makes the infiltration kinetics more favorable in the former preform. This study can provide guidance for the pore structure regulation in the fabrication of RMI-composites.     

Effects of starting powder on microstructure and thermal conductivity of pressureless-sintered fully ceramic microencapsulated fuels

The effects of the starting SiC powder (α or β) with the addition of 5.67 wt% AlN–Y₂O₃–CeO₂–MgO additives on the residual porosity and thermal conductivity of fully ceramic microencapsulated (FCM) fuels were investigated. FCM fuels containing ～41 vol% and ～37 vol% tristructural isotropic (TRISO) particles could be sintered at 1870 °C using α-SiC and β-SiC powders, respectively, via a pressureless sintering route. The residual porosities of the SiC matrices in the FCM fuels prepared using the α-SiC and β-SiC powders were 1.1% and 2.3%, respectively. The thermal conductivities of FCM pellets with ～41 vol% and ～37 vol% TRISO particles (prepared using the α-SiC and β-SiC powders, respectively) were 59 and 41 Wm^?1K^?1, respectively. The lower porosity and higher thermal conductivity of FCM fuels prepared using the α-SiC powder were attributed to the higher sinterability of the α-SiC powder than that of the β-SiC powder.     

Fabrication of carbon fiber reinforced ceramic matrix composites with improved oxidation resistance using boron as active filler

Boron was introduced into C_f/SiC composites as active filler to shorten the processing time of PIP process and improve the oxidation resistance of composites. When heat-treated at 1800 °C in N₂ for 1 h, the density of composites with boron (C_f/SiC-BN) increased from 1.71 to 1.78 g/cm³, while that of composites without boron (C_f/SiC) decreased from 1.92 to 1.77 g/cm³. So when boron was used, two cycles of polymer impregnation and pyrolysis (PIP) could be reduced. Meanwhile, the oxidation resistance of composites was greatly improved with the incorporation of boron-bearing species. Most carbon fiber reinforcements in C_f/SiC composite were burnt off when they were oxidized at 800 °C for 10 h. By contrast, only a small amount of carbon fibers in C_f/SiC-BN composite were burnt off. Weight losses for C_f/SiC composite and C_f/SiC-BN composite were about 36 and 16 wt%, respectively.     

Preparation of SiCf/Si–O–C composites by impregnation pyrolysis of polysiloxane and its electromagnetic wave absorption properties

High-temperature structural electromagnetic wave (EMW) absorption materials are increasing in demand because they can simultaneously possess the functions of mechanical load-bearing, heatproof, and EMW absorption. Herein, SiC_f/Si–O–C composites were prepared by precursor impregnation pyrolysis using continuous SiC fibers needled felt as reinforcement and polysiloxane as a precursor, respectively. The phase composition, microstructure, complex permittivity, and EMW absorption properties of SiC_f/Si–O–C composites after annealing at various temperatures were investigated. The annealing at 1400–1500°C affects positively the EMW absorption performance of the composites, because the β-SiC microcrystals and SiC nanowires were generated by the activation of carbothermal reduction reaction in the composites, and the aspect ratio of SiC nanowires increased with the rise of temperature. The composites exhibit optimal EMW absorption performance, with the effective absorption bandwidth covering the entire X-band and the minimum reflection loss (RL_min) of −32.8 dB at 4.0 mm when the annealing temperature is raised to 1500°C. This is because that the impedance matching is improved as the rising of ε′ and decreasing of ε″ due to the conversion of free carbon in the composite into SiC nanowires.     

Direct ink writing of chopped carbon fibers reinforced polymer-derived SiC composites with low shrinkage and high strength

The chopped carbon fiber reinforced SiC (C_f/SiC) composite has been regarded as one of the excellent high-temperature structural materials for applications in aerospace and military fields. This paper presented a novel printing strategy using direct ink writing (DIW) of chopped fibers reinforced polymer-derived ceramics (PDCs) with polymer infiltration and pyrolysis (PIP) process for the fabrication of C_f/SiC composites with high strength and low shrinkage. Five types of PDCs printing inks with different C_f contents were prepared, their rheological properties and alignment of carbon fiber in the printing filament were studied. The 3D scaffold structures and bending test samples of C_f/SiC composites were fabricated with different C_f contents. The results found that the C_f/SiC composite with 30 wt% C_f content has high bending strength (～ 7.09 MPa) and negligible linear shrinkage (～ 0.48%). After the PIP process, the defects on the C_f/SiC composite structures were sufficiently filled, and the bending strength of C_f/SiC composite can reach up to about 100 MPa, which was about 30 times greater than that of the pure SiC matrix without C_f. This work demonstrated that the printed C_f/SiC composites by using this method is beneficial to the development of the precision and complex high-temperature structural members.     

Facile synthesis of SiOx spheres or dumbbell-shaped β-SiC whiskers on expanded graphite by silicon vapor deposition

A facile method was developed to synthesize SiO_x spheres or dumbbell-shaped β-SiC whiskers on expanded graphite (SiO_x/EG or β-SiC/EG) by silicon vapor deposition without catalyst. With the carbon black atmosphere, the above hybrids were synthesized above 1100 °C in a graphite crucible where silicon powder was placed under the expanded graphite (EG). The growth of SiO_x spheres is controlled by vapor-solid mechanism at 1100 °C and 1200 °C. Namely, the active carbon atoms absorbed SiO (g) and Si (g) to form SiC nuclei. Then, the SiO₂, residual SiO (g) and Si (g) deposited on SiC nuclei to form SiO_x spheres. At 1300 °C and 1400 °C, the same SiO_x spheres formed on EG as well as many dumbbell-shaped β-SiC whiskers. The growth of dumbbell-shaped β-SiC whiskers is controlled by vapor-vapor and vapor-solid mechanism successively. In a word, firstly, the β-SiC whiskers with defects formed via the reaction between Si (g) and CO (g). After that, the SiO₂, residual SiO (g) and residual Si (g) preferentially deposited on defects, then deposited on other parts of β-SiC whiskers to form dumbbell-shaped SiC whiskers.     

Material removal mechanisms,processing characteristics and surface analysis of Cf-ZrB2-SiC in micro-EDM

C_f-ZrB₂-SiC is a new composite material with excellent properties for making the next-generation aerospace component. This material is extremely difficult to removal by mechanical machining, and there is a lack of research on feasible secondary processing methods of this composite at present. Micro-EDM is not limited by material hardness, so it is very suitable for machining this material. In this paper, the Material removal mechanisms and processing characteristics of C_f-ZrB₂-SiC by micro-EDM is analyzed. The removal mechanism of composite materials is explored though the discharge crater morphology, and the single-discharge experiments of each phase materials with different medium and different energies are also carried out as a reference. Electrical discharge milling experiments of C_f-ZrB₂-SiC are performed to explore the medium on processing index, and found that the best surface quality and maximum processing efficiency can be realized in kerosene. An experiment with four factors (pulse width, voltage, peak current, capacitance) and three indexes (surface roughness, MRR, TWR) is designed to analyze the C_f-ZrB₂-SiC process characteristics of micro-EDM and the response surface diagram and second-order regression equation are obtained. Milling the C_f-ZrB₂-SiC by electrical discharge according to the optimal combination of surface roughness parameters deduced above, the as-machined surface is analyzed including the surface morphology by SEM, element content by EDS and the surface phase by XRD. The feasibility and advantages of micro-EDM on machining C_f-ZrB₂-SiC are prove.     

Fabrication method,dielectric properties,and electromagnetic absorption performance of high alumina fly ash-based ceramic composites

Mullite-Al₂O₃-SiC composites were in-situ synthesized through carbothermal reduction reaction of fly ash (FA) with a high alumina content and activated carbon (AC). The effects of sintering temperature, holding time, and amount of AC on the β-SiC yield, microstructure, dielectric properties, and electromagnetic (EM) absorption performance of the composites in the 2–18 GHz frequency range were studied. The results show that increasing the AC improves the porosities of the composites, with the highest porosity of 56.17% observed. The β-SiC yield varies considerably as the sintering parameters were altered, with a maximum yield of 23% achieved under conditions of 12 wt% AC, 1400 °C sintering temperature, and 3 h holding time. With a thickness of 3.5 mm, this composite has excellent EM absorption performance, exhibiting a minimum reflection loss (RL_min) of -51.55 dB at 7.60 GHz. Significantly, the maximum effective absorption bandwidth (EAB) reaches 3.39 GHz when the thickness is 3.0 mm. These results demonstrate that the composite prepared under ideal conditions can absorb 99.99% of the waves passing through it. Because of the interfacial polarization, conductive loss, and impedance matching of the heterostructure, the synthesized mullite-Al₂O₃-SiC composites with densities ranging from 1.43 g/cm³ to 1.62 g/cm³ demonstrate outstanding EM attenuation capabilities. Therefore, this study presents a remarkable way of utilizing fly ash to fabricate inexpensive, functional ceramic materials for EM absorption applications.     

Influence of mechanical activation on combustion synthesis of fine silicon carbide (SiC) powder

The influence of mechanical activation of powder mixtures of Si and C, via high energy attrition milling (up to 12 h), on combustion synthesis of SiC was experimentally investigated. β-SiC fine powder was successfully fabricated in 1.0 MPa N₂ atmosphere without other additional treatments, such as preheating, electric action, or chemical activation. Relatively weak peaks of α-SiC, α-Si₃N₄ and Si₂ON₂ were also found in the final products. The experimental results and their theoretical treatment showed that mechanical activation via high energy ball-milling provides to the initial Si/C powder mixture extra energy, which is needed to increase the reactivity of powder mixture and to make possible the ignition and the sustaining of combustion reaction to form SiC.     

Pressureless sintered silicon carbide tailored with aluminium nitride sintering agent

This study reports the influence of aluminium nitride on the pressureless sintering of cubic phase silicon carbide nanoparticles (β-SiC). Pressureless sintering was achieved at 2000 °C for 5 min with the additions of boron carbide together with carbon of 1 wt% and 6 wt%, respectively, and a content of aluminium nitride between 0 and 10 wt%. Sintered samples present relative densities higher than 92%. The sintered microstructure was found to be greatly modified by the introduction of aluminium nitride, which reflects the influence of nitrogen on the β-SiC to α-SiC transformation. The toughness of sintered sample was not modified by AlN incorporation and is relatively low (around 2.5 MPa m^1/2). Materials exhibited transgranular fracture mode, indicating a strong bonding between SiC grains.     

Silicon carbide-based foams derived from foamed SiC-filled phenolic resin by reactive infiltration of silicon

Macro-cellular porous silicon carbide-based foams were fabricated by reactive infiltration of melt silicon into porous carbonaceous preforms pyrolyzed from foamed SiC-filled phenolic resins (PF). The SiC-filled PF foams were prepared at 80 °C with different heating rate. The effect of heating rate on the foaming behavior of the liquid SiC-filled PF mixture and the microstructure of the foams were investigated. The foamed SiC-filled PF was then pyrolyzed at 1000 °C and infiltrated by melt Si at 1600 °C, leading to the formation of open macro-cellular structure. At a heating rate of 6 °C min⁻¹, Si-infiltrated foams with a porosity of ~72% and a mean pore size of ~0.5 mm were obtained. The Si-infiltrated foams with dense struts mainly inherited the pore structure of pyrolyzed preforms. The main phases of SiC-based foams were α-SiC, β-SiC and the remnant Si, which contributed to high compressive strength of the SiC-based foams.     

Preparation and properties of C/SiC/ZrO2 porous composites by hot isostatic pressing the pyrolyzed preforms

Three phase mixture of C/SiC/ZrO₂ porous composites were prepared from commercially available phenolic resin, Si and ZrO₂ powders. In the first step, mixed powders were pyrolyzed at 850 °C in vacuum to obtain a carbonized microporous material and then hot isostatically pressed at 1200, 1300 and 1350 °C for 10 min in an argon pressure of 50 MPa to prepare C/SiC/ZrO₂ porous composites, in second step. The hot isostatic pressing led to the increase in density from 3.28 to 3.48 g/cm³ and reduction in porosity (from 32 to 20%) of the composites. X-ray diffraction analyses revealed the existence of β-SiC and carbon might be amorphous in the composites. According to the results of scanning electron microscopy, the crystal growth of β-SiC with facets was observed at 1350 °C. In addition, the energy dispersive spectroscopy showed that carbon/silicon atomic ratio was 1:1 in the crystals. X-ray photoelectron spectroscopy of the composites suggested that evolved gaseous molecules, due to the decomposition of phenolic resin, reacted with molecules containing Si to form β-SiC. The formation and growth of β-SiC in addition to the densification of matrix by hot isostatic pressing led to the increase in hardness (max.: 13.99 GPa) at higher temperatures.