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.     

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.     

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.     

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.     

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.     

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.     

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. ©     

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.     

Efficient fabrication of carbon/silicon carbide composite for electromagnetic interference shielding applications

Ceramic matrix composites are typically prepared by a costly, time-consuming process under severe conditions. Herein, a cost-effective C/SiC composite was fabricated from a silicon gel-derived source by Joule heating. The β-SiC phase was generated via carbothermal reduction, and the carbon fabric showed a well-developed graphitic structure, promoting its thermal and anti-oxidation stabilities. Owing to the excellent dielectric loss in carbon fabric, SiC and SiO₂ as well as the micropore structure of the ceramic matrix, the absolute electromagnetic interference shielding (EMI) effectiveness (SSE/t) reached 948.18 dB?cm²?g^-1 in the X-band, exhibiting an excellent EMI SE. After oxidation at 1000 °C for 10 h in the air, the SSE/t of the composite was only reduced to 846.02 dB?cm²?g^-1. The C/SiC composite promises the efficient fabrication of high-temperature resistant materials for electromagnetic shielding applications.     

Microstructural and mechanical evaluation of a Cu-based active braze alloy to join silicon nitride ceramics

Self-joining of St. Gobain Si₃N₄ (NT-154) using a ductile Cu-Al-Si-Ti active braze (Cu-ABA) was demonstrated. A reaction zone (∼2.5-3.5 μm thick) developed at the interface after 30 min brazing at 1317 K. The interface was enriched in Ti and Si. The room temperature compressive shear strengths of Si₃N₄/Si₃N₄ and Inconel/Inconel joints (the latter created to access baseline data for use with the proposed Si₃N₄/Inconel joints) were 140 ± 49 MPa and 207 ± 12 MPa, respectively. High-temperature shear tests were performed at 1023 K and 1073 K, and the strength of the Si₃N₄/Si₃N₄ and Inconel/Inconel joints were determined. The joints were metallurgically well-bonded for temperatures above 2/3 of the braze solidus. Scanning and transmission electron microscopy studies revealed a fine grain microstructure in the reaction layer, and large grains in the inner part of the joint with interfaces being crack-free. The observed formation of Ti₅Si₃ and AlN at the joint interface during brazing is discussed.     

高强度刚玉碳化硅浇注料的研制

以棕刚玉和碳化硅为主要原料、铝酸钙水泥为结合剂,制备出了一种高强度的刚玉碳化硅浇注料。通过优化颗粒级配,调整水泥和复合微粉的加入量,测定试样在各种因素影响下的常温和高温强度。结果表明,研制出的刚玉碳化硅浇注料既具有较高的常温强度,又具有很高的高温强度。     

Ultra-high-temperature mechanical behaviors of two-dimensional carbon fiber reinforced silicon carbide composites: Experiment and modeling

Carbon fiber reinforced silicon carbide (C/SiC) composites are enabling materials for components working in ultra-high-temperature extreme environments. However, their mechanical properties reported in the literature are mainly limited to room and moderate temperatures. In this work, an ultra-high-temperature testing method for the mechanical properties of materials in inert atmosphere is presented based on the induction heating technology. The flexural properties of a 2D plain-weave C/SiC are studied up to 2600 °C in inert atmosphere for the first time. The deformation characteristics and failure mechanisms at elevated temperatures are gained. Theoretical models for the high-temperature Young’s modulus and tensile strength of 2D ceramic matrix composites are then developed based on the mechanical mechanisms revealed in the experiments. The factors contributing to the mechanical behaviors of C/SiC at elevated temperatures are thus characterized quantitatively. The results provide significant understanding of the mechanical behaviors of C/SiC under ultra-high-temperature extreme environment conditions.     

Microstructural and mechanical properties of porous Si3N4 carbon coated ceramic brazed with a cobalt-silicon filler

The Co_22.5Si_77.5 (at.%) braze was used to bond porous Si₃N₄ ceramics. The effects of brazing temperature on microstructure and the bonding strength of the joint were studied. The results reveal that no visible reaction layer was observed. The corresponding joint strength was low. In order to improve the joint strength a carbon coated modification of the porous Si₃N₄ substrate was suggested. The impact of this modification on the joint properties was examined. It was established that a SiC reaction layer with a thickness from ∼15 μm to ∼65 μm was formed at the interface and SiC nanowires were observed when the temperature increased from 1280 °C to 1340 °C. The maximum shear strength of the carbon coated and uncoated joints were 115 MPa and 44 MPa, respectively. The significant improvement of the joint strength was attributed to the SiC reaction layer and a strengthening by the presence of SiC nanowires. .     

Microstructure,mechanical behavior and flow resistance of freeze-cast porous 3YSZ substrates for membrane applications

Freeze-cast porous 3YSZ with different porosities were characterized as mechanical load carrying supports for oxygen transport membrane applications. Porosity influence on mechanical properties, i.e. elastic modulus and fracture stresses was assessed with biaxial ring-on-ring bending tests. The flow resistance was characterized in terms of the pressure drop using different gases to reveal the effect of the porous support on the accessing of the inlet gas flow to the functional dense membrane layer. Both properties were discussed in terms of the influence of porosity and pore structure, and compared with the properties of porous 3YSZ produced via pressing and sintering.     

高频红外碳硫仪测定碳化硅中的SiC

对试样进行灼烧预处理,除去挥发分和游离C。用纯SiC和纯SiO2合成标准样品校正仪器,用锡粒、纯铁、钨粒作为助熔剂,高频燃烧红外吸收法测定碳化硅中的SiC。该法简便,准确可靠,实际样品分析结果满意。     

Low-temperature fabrication and characterization of porous SiC ceramics using silicone resin as binder

Commercially available silicone resin and silicon carbide (SiC) powders were adopted as the starting materials for the fabrication of porous SiC ceramics. During the heat treatment process, silicone resin experienced an organic–inorganic transformation and acted as the bonding material between SiC particles at a low temperature of 1000 °C. The mean particle size of starting SiC powders and silicone resin content can control the pore size, open porosity and fracture strength. The flexural strength of porous SiC ceramics increases with increasing silicone resin content and decreasing mean particle size of SiC powders. Larger pores can be obtained with coarser starting SiC powders and higher silicone resin content. The fracture surface of porous SiC ceramics was observed.     

Porous silicon carbide structures with anisotropic open porosity for high- temperature cycling applications

We have prepared porous silicon carbide by a novel two-step template method. Graphite/SiC composites of required size and shape are first fabricated by hot pressing at 2125 °C, followed by the removal of the graphite template by controlled heat treatment. The anisotropy in the composite structure is restored after the removal of the template and porous SiC with anisotropic properties is obtained. The composite can be easily machined by electrical discharge machining because of the presence of graphite, and porous SiC can be obtained by heat treatment, solving the inherent difficulty in the machining of SiC. The mechanical properties, thermal conductivity, and thermal shock resistance of porous SiC have been studied in both directions. The material shows good thermal shock resistance in the perpendicular to pressing direction even at 1400 °C. Hence porous SiC suitably machined preserving the proper direction can be a potential candidate for thermal cycling applications.     

Effect of carbon nanoparticle reinforcement on mechanical and thermal properties of silicon carbide ceramics

This research presents an analysis of the influence of graphene reinforcement on the thermal and mechanical properties of silicon carbide ceramics, at 2.5% (wt%) graphene content. The SiC composites, containing various carbon nanofillers (graphene oxide and graphene nanoparticles), were sintered by the classical two stage spark plasma sintering method. Two current modes were used, the continuous mode and the pulsed current mode. The results from photothermal radiometry and investigations of the mechanical properties showed that graphene additives significantly improve the thermal properties and toughness of material, sintered from a SiC powder. An 45% growth in the toughness was observed, which increased from 1.21 to 1.75?MPa/m^1/2. The thermal diffusivity value also increased from 0.60 to 0.71?cm²/s and giving an improvement in thermal properties of 18%. The friction coefficient reached 7% giving an increase in value from 0.62 to 0.66. Microscopic investigations supported the photothermal radiometry (PTR) results. Whilst, thermal imaging revealed homogeneity of the local thermal properties of the products fabricated from the starting SiC powder.     

The fabrication and mechanical properties of SiC/SiC composites prepared by SLS combined with PIP

Traditionally, SiC components with complex shapes are very difficult or even impossible to fabricate. This paper aims to develop a new manufacturing process, combining selective laser sintering (SLS), cold isostatic pressing (CIP) and polymer infiltration pyrolysis (PIP), to manufacture complex silicon carbide parts and improve the mechanical properties of silicon carbide ceramic parts. The density and porosity of SiC/SiC composites were measured. Furthermore, the mechanical properties of the specimens with cold isostatic pressing and the specimens without cold isostatic pressing were compared. The bending strength of the specimens with cold isostatic pressing was 201?MPa, and the elastic modulus was 1.27?GPa. And, the bending strength of the specimens without cold isostatic pressing was 142?MPa, and the elastic modulus was 0.88?GPa. Increasing the density of SiC/SiC can enhance the mechanical properties of SiC/SiC composites.