Fabrication of porous silicon carbide ceramics with high porosity and high strength

Unique porous SiC ceramics with a honeycomb structure were fabricated by a sintering-decarburization process. In this new process, first a SiC ceramic bonded carbon (SiC/CBC) is sintered in vacuum by spark plasma sintering, and then carbon particles in SiC/CBC are volatized by heating in air at 1000 °C without shrinkage. The honeycomb structure has at least two different sizes of pores; ∼20 μm in size resulting from carbon removal; and smaller open pores of 2.1 μm remaining in the sintered SiC shell. The total porosity is around 70% and the bulk density is 0.93 mg/m³. The bending and compressive strengths are 26 MPa, and 105 MPa, respectively.     

Microstructural and mechanical characterization of high strength porcelain insulators for power transmission and distribution applications

Porcelain insulators have prodigious importance in electricity transmission and distribution network because of their high dielectric constant, electrical resistivity, and mechanical strength and these properties are closely connected to the microstructural details of the insulator. Three different porcelain insulators (Sample A, B and C) were reported in the present work. X-ray fluorescence (XRF), X-ray diffraction (XRD), scanning electron microscopy (SEM), three point bending test and density and pore analysis were carried out to investigate the structural and mechanical properties of various insulators. The analysis confirmed that the porcelain insulators are made of industrial alumina, quartz, clay, and feldspar having amorphous as well as crystalline phase in the body. The porosity, density, and bending strength were also calculated and a correlation was developed between mechanical strength of the insulator and various physio-chemical and microstructural properties. Sample A showed the highest value of bending strength i.e. 207.20 MPa and sample C the lowest value of 112.18 MPa while sample B demonstrated the intermediate value of 170.98 MPa. To formulate high strength porcelain insulators, it was concluded that the amount of amorphous phase, dispersed corundum, and mullite content are key factors to control the mechanical strength of porcelain insulators.     

Characterization and oxidation properties of biomorphic porous carbon with SiC gradient coating prepared by PIP method

A biomorphic porous carbon coated with SiC (SiC/BPC) was prepared by controlled carbonizing native pine under Ar atmosphere and then processed with precursor infiltration-pyrolysis (PIP) of organosilane. Microstructure and component of SiC/BPC were analyzed by FT-IR, XRD, SEM and EDS (attached with line scanning program). The non-isothermal oxidation properties and mechanism of SiC/BPC were studied by TGA. The kinetic parameters were calculated through model-free kinetics methods. Experimental results showed that SiC/BPC had a topologically uniform interconnected porous network microstructure; the obtained gradient SiC coating on BPC surface was amorphous and combined well with the carbon surface, which can improve the oxidation resistance of BPC clearly. The non-isothermal oxidation reaction of SiC/BPC exhibited a partial self-accelerating characteristic. The oxidation process was complicated, firstly it was controlled by gas diffusion in coating, then controlled by chemical reaction, and at last it was controlled by gas diffusion and chemical reaction together, the corresponding effective activation energy was calculated also.     

Oxidation behavior of silicon carbide based biomorphic ceramics prepared by chemical vapor infiltration and reaction technique

The oxidation behavior of biomorphic SiC based ceramics with different microstructure and composition was studied at 1450 °C in airflow for 50 h by thermal gravimetric analysis (TGA). SiC with amorphous, coarse grain, crystalline and fine grain crystalline microstructures as well as SiC–Si₃N₄ composite ceramics were processed from paper preforms by chemical vapor infiltration and reaction technique. The ceramics were characterized by X-ray diffraction and scanning electron microscopy coupled with energy dispersive spectroscopy (SEM/EDX) before and after oxidation. The results show that the crystalline SiC with fine grain structure and SiC–Si₃N₄ composite ceramics show very good oxidation resistance at a temperature of 1450 °C.     

Oxidation behavior and ablation properties of MDF-based biomorphic SiC composites

Biomorphic SiC composites were fabricated by infiltration of liquid Si into a preform fabricated from medium-density fiberboard (MDF). The phase compositions, microstructures, oxidation behaviors, and ablation properties of the composites were investigated. The composites were oxidized at elevated temperatures (up to 1450 °C) in air to study their oxidation behavior. Pores and cracks initially formed from the oxidation of residual carbon, followed by melting of residual Si. The ablation resistance of a composite was gauged using an oxy-acetylene torch. The formation of a SiO₂ layer by the oxy-acetylene flame improved the ablation resistance because molten SiO₂ spread over the ablated surface and partially sealed the pores, thus acting as an effective barrier against the inward diffusion of oxygen.     

Static and dynamic oxidation behaviour of silicon carbide at high temperature

SiC has extensive applications in high-temperature oxidation environments. However, few studies have investigated the differences between the static and dynamic oxidation behaviour. In this study, the static and dynamic oxidation of SiC were investigated in air and in plasma wind tunnels, respectively. The results demonstrated that the activation energy of static oxidation was ～68.02 kJ/mol at 1300–1600 ℃, which was approximately ten times that of dynamic oxidation ～7.05 kJ/mol at 1290–1534 ℃. The observed Si-O-C transition layer located at the SiO₂/SiC interface, and its thickness after dynamic oxidation for 300 s was thicker than that after static oxidation for 30 h. In dynamic oxidation, high-speed flowing atomic oxygen reacted directly with SiC, whereas molecular oxygen needed extra energy to break the OO bond and react with SiC in static oxidation. Atomic oxygen also migrated easier in the amorphous SiO₂ coating, contributing to a thicker Si-O-C layer and lower activation energy.     

Porosity features and gas permeability analysis of bi-modal porous alumina and mullite for filtration applications

Bimodal porous structures were prepared by combining conventional sacrificial template and partial sintering methods. These porous structures were analysed by comparing pore characteristics and gas permeation properties of alumina/mullite specimens sintered at different temperatures. The pore characteristics were investigated by SEM, mercury porosimetry, and capillary flow porosimetry. A bimodal pore structure was observed. One type of pore was induced by starch, which acted as a sacrificial template. The other pore type was due to partial sintering. The pores produced by starch were between 2 and 10 µm whereas those produced by partial sintering exhibited pore size of 0.1–0.5 µm. The effects of sintering temperature on porosity, gas permeability, and mullite phase formation were studied. The formation of the mullite phase was confirmed by XRD. Compressive strengths of 37.9 MPa and 12.4 MPa with porosities of 65.3% and 70% were achieved in alumina and mullite specimens sintered at 1600 °C.     

Steam pressure and velocity effects on high temperature silicon carbide oxidation

The effects of steam pressure, velocity, and composition on SiC oxidation kinetics were studied. Pressure effects were tested at 1200°C from 0.1 to 1.4 MPa at a steam velocity of 0.25 cm/s. Velocity effects were tested in two furnaces at 0.45 MPa, 1200°C and 0.1 MPa, 1600°C with velocities ranging from 0.25 to 137 cm/s. Steam composition was altered by changing the reaction vessel material. Oxide morphology and composition were determined using optical and electron microscopy, and X-ray diffraction. Porous oxides were observed whenever structural SiC from the reaction vessel saturated the steam with volatilized silica, H₂, and CO. Oxidation kinetics were calculated by the change in SiC thickness. The steam velocity/recession rate followed a power-law relationship of ~ 0.35 while the steam pressure/recession rate followed a power-law relationship of ~ 1.78.     

Electrical properties of biomorphic SiC ceramics and SiC/Si composites fabricated from medium density fiberboard

A study has been made of the dependences of the electrical resistivity and the Hall coefficient on the temperature in the range 1.8-1300 K and on magnetic fields of up to 28 kOe for the biomorphic SiC/Si (MDF-SiC/Si) composite and biomorphic porous SiC (MDF-SiC) based upon artificial cellulosic precursor (MDF - medium density fiberboards). It has been shown that electric transport in MDF-SiC is effected by carriers of n-type with a high concentration of ∼10²⁰ cm⁻³ and a low mobility of ∼0.4 cm² V⁻¹ s⁻¹. The specific features in the conductivity of MDF-SiC are explained by quantum effects arising in disordered systems and requiring quantum corrections to conductivity. The TEM studies confirmed the presence of disordering structural features (nanocrystalline regions) in MDF-SiC. The conductivity of MDF-SiC/Si composite originates primarily from Si component in the temperature range 1.8-500 K and since ∼500 to 600 K the contribution of MDF-SiC matrix becomes dominant.     

Relationship between bending strength of bulk porous silicon carbide ceramics and grain boundary strength measured using microcantilever beam specimens

The relationship between the bending strength of bulk porous SiC ceramics and the grain boundary strength measured using microcantilever beam specimens of SiC bicrystals was investigated. The average value of the grain boundary strength was 39.2 GPa, and its higher value was roughly equal to that derived using an ab-initio calculation. The strengths of the specimens having only one neck were estimated by analyzing the effect of the specimen size on the strength of bulk porous SiC ceramics and by also analyzing the grain boundary strength and the stress concentration at the neck surface. The estimated strengths were generally consistent of the order of several hundred MPa, meaning that the strength of porous SiC ceramics should be dependent on the stress concentration at the neck and the grain boundary strength. Furthermore, they were in a better agreement using smaller neck curvature, smaller neck diameter, and lower grain boundary strength.     

Preparation and characterization of porous Si3N4-bonded SiC ceramics and morphology change mechanism of Si3N4 whiskers

Porous Si₃N₄-bonded SiC ceramics with high porosity were prepared by the reaction-sintering method. In this process, Si₃N₄ was synthesized by the nitridation of silicon powder. The X-ray diffraction (XRD) indicated that the main phases of the porous Si₃N₄-bonded SiC ceramics were SiC, α-Si₃N₄, and β-Si₃N₄, respectively. The contents of β-Si₃N₄ were increased following the sintering temperature. The morphology of Si₃N₄ whiskers was investigated by scanning electron microscope (SEM), which was shown that the needle-like (low sintering-temperature) and rod-like (higher sintering-temperature) whiskers were formed, respectively. From low to high synthesized temperature, the highest porosity of the porous Si₃N₄ bonded SiC ceramic was up to 46.7%, and the bending strength was ~11.6?MPa. The α-Si₃N₄ whiskers were derived from the reaction between N₂ and Si powders, the growth mechanism was proved by Vapor–Solid (VS). Meanwhile, the growth mechanism of β-Si₃N₄ was in accordance with Vapor–Solid–Liquid (VSL) growth mechanism. With the increase of sintering temperature, Si powders were melted to liquid silicon and the α-Si₃N₄ was dissolved into the liquid then the β-Si₃N₄ was precipitated successfully.     

Fabrication of wood-like porous silicon carbide ceramics without templates

The porous silicon carbide ceramics with wood-like structure have been fabricated via high temperature recrystallization process by mimicking the formation mechanism of the cellular structure of woods. Silicon carbide decomposes to produce the gas mixture of Si, Si₂C and SiC₂ at high temperature, and silicon gas plays a role of a transport medium for carbon and silicon carbide. The directional flow of gas mixture in the porous green body induces the surface ablation, rearrangement and recrystallization of silicon carbide grains, which leads to the formation of the aligned columnar fibrous silicon carbide crystals and tubular pores in the axial direction. The orientation degree of silicon carbide crystals and pores in the axial direction strongly depends on the temperature and furnace pressure such as it increases with increasing temperature while it decreases with increasing furnace pressure.     

Controlling the electrical resistivity of porous silicon carbide ceramics and their applications: A review

Porous silicon carbide (SiC)-based ceramics are widely used in numerous applications of technical importance owing to their exceptional structural (e.g., excellent chemical, mechanical, and thermal stability) and functional (e.g., controlled electrical resistivity) properties. Porous SiC with controlled electrical resistivity is required for various advanced applications, for example, power electronic devices, semiconductor processing parts, fusion reactors, thermoelectric energy conversion, electromagnetic shielding, and environmental applications such as heatable filters. The electrical properties of sintered porous SiC are significantly affected by its chemical composition, processing conditions, and microstructure. This article reviews the influence of certain critical factors, such as the polytype, doping conditions, porosity (%), additive composition (oxide additives, element additives, metal nitride/carbide additives, etc.), and processing conditions on the electrical resistivity of porous SiC. Novel applications of porous SiC with controlled electrical resistivity are also discussed in this review.     

Chemical bonding of silicon carbide

The effect of several variables such as the type of binder and additive, the temperature, time, furnace atmosphere, particle size and forming pressure, on the strength of chemically bonded SiC specimens was studied. It was shown that the highest compressive strength (43·67 MPa at 500°C) can be obtained by using optimum amounts of orthophosphoric acid and aluminium hydroxide as binder and additive respectively. Various stages in the structural development were followed by DTA, XRD and SEM/EDX analysis. It was shown that by using aluminium hydroxide and kaolin additives, phosphate bonding could be preserved at the specimen surfaces up to 1450°C. ©     

Development and characterization of silicon dioxide clad silicon carbide optics for terrestrial and space applications

Silicon carbide (SiC), a non-oxide ceramic with superior thermo-mechanical stability, chemical and radiation resistive properties, finds extensive utilization in optical instruments for terrestrial and space applications. However, its inherent porous texture (α-HCP) becomes a deterrent for high-performance optical telescopes, although several techniques of surface alterations over sintered or reaction-bonded SiC are available. In the present work, the physical vapour deposition (PVD) technique is adopted to deposit a thick (～5 μm) Silicon dioxide (SiO₂) clad layer on a sintered and optically polished SiC (SSiC) substrate. SiO₂ clad layer coated SSiC (SDO-SSiC) substrate reduces the surface porosity of SSiC which is found to be suitable for optical mirror application. Finally, an Al based reflective and oxides protective coatings are deposited on SiO₂ clad layer to achieve reflective behaviour. The surface figure of 75 nm PV (peak-to-valley) and less than 2 nm surface micro-roughness values are achieved which meets the stringent optical telescope specifications for terrestrial and space applications. The structural and nano-mechanical properties of presently developed SiO₂ clad layer-based SiC telescopic mirror have been characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-Ray Analysis (EDX), atomic force microscopy (AFM), and nanoindentation techniques. The optical properties are investigated by optical profilometry and wavelength based spectrometric (both in visible and infrared ranges) techniques. Finally, space worthiness studies viz., thermo-vacuum, thermal storage, thermal shock and relative humidity tests have been carried out successfully. The process of cleaning, grinding and polishing at each substrate preparation stage and coatings are also reported comprehensively.     

Pressureless sintering of multilayer graphene reinforced silicon carbide ceramics for mechanical seals

ABSTRACT

The silicon carbide (SiC) ceramics containing multilayer graphene derived from graphite exfoliation were successfully prepared by pressureless sintering, and the effect of graphene content on the sintering behaviours, microstructure, mechanical, tribological, electrical and thermal properties was investigated in detail. The bulk density, bending strength and hardness of the composite ceramics gradually decrease with the increase of graphene content, but the friction, conductance and thermal conductance properties are improved obviously. When the graphene content reaches 5?wt-%, the dry friction coefficient of 0.22, electrical conductivity of 2724.14 S?1?m?1 and thermal conductivity of 8.5?W?(m?1?K?1) can be obtained, indicating good comprehensive mechanical, tribological, electrical and thermal properties. This multilayer graphene reinforced silicon carbide ceramic is a promising seal material instead of SiC seal materials containing graphite to be applied in next-generation mechanical seals.     

Synthesis and potential applications of silicon carbide nanomaterials / nanocomposites

The rapid development of nanotechnologies has accelerated the research in silicon carbide (SiC) nanomaterial synthesis and application. SiC nanomaterials have unique chemical and physical properties, such as distinctive electronic and optical properties, good chemical resistance, high thermal stability, and low dimensionality. These properties lead to a wide range of applications. The progress in SiC nanomaterials in recent years is significant, but a review of the progress is lacking. This article is designed to fill the gap. The review first summarizes various methods for preparing different SiC nanomaterials/nanocomposites, including the carbothermal method, chemical vapor deposition method, and other synthesis techniques using unconventional energy sources such as microwave, plasma, solar energy, and neutron irradiation. Discussion is then made on the significant applications of the SiC nanomaterials/nanocomposites, especially in sensors, catalyst supports, energy storage materials, structural reinforcement, and semiconductor materials. Finally, the conclusion of this review is made with the possible future development trends.     

Microstructure evolutions of SiC whiskers at high temperature and its effects on silicon carbide ceramics

SiC whisker with a single-crystal structure is promising in enhancing the strength and toughness of advanced structural ceramics, owing to its excellent properties. However, studies on its microstructure evolution at high temperature (>2000 °C) are scarce. Herein, SiC whiskers were calcined at 2100 °C, and XRD, SEM, and TEM were employed to analyze microstructure evolutions. Compared with raw whiskers, XRD results indicated serious annihilation of stacking faults after calcination. The annihilation led to the fracture of whiskers and the formation of β-SiC grains, and then partial grains underwent the phase transformation to form hexagonal prism and triangular prism α-SiC grains with diameters of about 10 μm, according to SEM and TEM results. Furthermore, SiC ceramics containing different whisker contents were innovatively fabricated by pressureless solid-state sintering. The flexural strength and fracture toughness of SiC ceramic containing 10 vol% whiskers were 540 MPa and 5.1 MPa m^0.5, resulting in 38% and 11% higher values than those without whiskers, respectively.     

Electrical,thermal, and mechanical properties of porous SiC-nitride composites

The effects of nitride (AlN, BN, TiN) addition on the electrical, thermal, and mechanical properties of porous SiC-nitride composites were investigated within a porosity range of 40–74 %. The electrical conductivity was predominantly controlled by chemistry rather than porosity, whereas the thermal conductivity was more susceptible to changes in porosity. These results suggest that the electrical conductivity of porous SiC ceramics can be tuned independently from the thermal conductivity by nitride addition. At constant thermal conductivity (∼5 Wm⁻¹ K^-1), the electrical conductivity of the baseline specimen (6.3 × 10^-3 Ω^-1 cm^-1) could be: (1) increased by an order of magnitude (8.3 × 10^-2 Ω^-1 cm^-1) by adding AlN and (2) decreased by an order of magnitude (7.0 × 10^-4 Ω^-1 cm^-1) by adding BN. Typical electrical conductivity and thermal conductivity values of the porous SiC-10 vol% TiN composite were 5.3 × 10^-1 Ω^-1 cm^-1 and ∼14.0 Wm⁻¹ K^-1, respectively, at 51 % porosity.     

Processing and properties of glass-bonded silicon carbide membrane supports

Porous SiC membrane supports were fabricated from SiC and glass frit at a temperature as low as 850 °C in air by a simple pressing and heat-treatment process. The effects of the initial SiC particle size and frit content on the porosity, flexural strength, and air permeation of the membrane supports were investigated. During heat-treatment, the glass frit transformed to a viscous glass phase, which acted as a bonding material between SiC particles and as a protecting layer for severe oxidation of SiC particles. The porosity of the porous SiC membrane supports could be controlled within a range of 37–46% with the present set of processing conditions. The typical flexural strength, permeability, and specific air flow rate of the porous membrane supports fabricated using 23 μm SiC particles with 15 wt% glass frit were 75 MPa, 4.2 × 10⁻¹³ m², and 32.4 L/min/cm², respectively.