Fine grained Al2O3/SiC composite ceramic tool material prepared by two-step microwave sintering

Fine-grained Al₂O₃/SiC composite ceramic tool materials were synthesized by two-step microwave sintering. The effects of first-step sintering temperature (T1), content and particle size of SiC on the microstructure and mechanical properties were studied. It was found that the sample with higher content of SiC was achieved with finer grains, and the incorporation of SiC particles could bridge, branch and deflect the cracks, thus improving the fracture toughness. Higher T1 was required for the densification of the samples with higher content of SiC (>5?wt%). The sample containing 3?wt% SiC particles with the mean particle size of 100?nm, which was sintered at 1600?°C (T1) and 1100?°C (T2) for 5?min had the fine microstructure and optimal properties. Its relative density, grain size, Vickers hardness and fracture toughness obtained were 98.37%, 0.78?±?0.31?μm, 18.40?±?0.24?GPa and 4.97?±?0.30?MPa?m^1/2, respectively. Compared to the sample prepared by single-step microwave sintering, although near full densification can be achieved in both two methods, the grain size was reduced by 36% and the fracture toughness was improved by 28% in two-step microwave sintering.     

In situ synthesis of ZrB2–ZrC–SiC ultra-high-temperature nanocomposites by a sol–gel process

ABSTRACT

ZrB₂–ZrC–SiC is one of the ultra-high-temperature ceramic composites with excellent properties. In this research, high-purity ZrB₂–ZrC–SiC nanopowders were synthesised using a carbothermal reduction reaction at a relatively low temperature (1370°C) from cost-effective zirconium(IV) chloride by a sol–gel method. The effect of heat treatment temperature on the synthesis of ZrB₂–ZrC–SiC composite powder was studied. X-ray diffractometry results showed that the phases ZrB₂, β-SiC and ZrC were synthesised at 1370°C. The mean crystallite sizes for each of the phases were calculated using the Scherrer method. The specific surface area for the sample calcined at 1370°C was 81.479?m²?g^?1. SEM observation revealed that the particles had a size lower than 250?nm. Backscattered electron image and map analysis with scanning electron microscopy showed that a suitable phase homogeneity was achieved, as confirmed by energy-dispersive X-ray spectroscopy.     

Fabrication and properties of SiC porous ceramics using a polyurethane preparation process

SiC porous ceramics can be prepared by introducing the polyurethane preparation method into the production process of ceramic biscuits, followed by sintering at 1300?°C for 2?h under N₂ flux after the cross-linking of polycarbosilane at 220?°C for 4?h in air. The microstructures, mechanical properties and infiltrations of the SiC porous ceramics are investigated in detail. The best dispersal effect comes from the SiC slurry with xylene as the solvent and a mixture of Silok®7096 (1?wt%) and Anjeka®6041 (4?wt%) as the dispersant. The compressive strength of SiC porous ceramics with high porosity (69.53%) reaches 16.9?MPa. The heat treatment can increase infiltration, the rate of which (4.296?×?10^?7 mm²) after the heat treatment at 750?°C in air is approximately two times faster than that before the heat treatment. The SiC porous ceramics fabricated in this study will have potential application in active thermal protection systems.     

Low‐Temperature Synthesis of Mesoporous SiC Hollow Spheres by Magnesiothermic Reduction

Mesoporous silicon carbide hollow spheres (SiC‐HS) with a large specific surface area (690.2 m² g^?1) are synthesized at a relatively low temperature of 650°C by magnesiothermic reduction using the template of carbon‐coated mesoporous silica hollow spheres and molten salt as the heat absorbent and solvent. The mesoporous SiC‐HS comprising many small primary crystals (2–4 nm) with a well‐maintained microstructure have good thermal stability and adsorption ability, and are promising as adsorbents to remove organic pollution from water. The synthesis technique can be extended to other nanostructured carbide ceramic materials.     

Elaboration and characterisation of low cost ceramic support membrane

Abstract

A porous tubular ceramic membrane was prepared from low cost Tunisian clay. The characterisation of the raw material and the effect of the sintering temperature on the morphology, pores size distribution and the mechanical properties of the ceramic membrane were studied. A ceramic membrane fired at 1000°C for 1?h presented a mean pore diameter of ～1·04?μm. The porosity was equal to 38?vol.-%. The filtration of a 0·5?g?L^?1 bovine serum albumin solution indicated that the limiting flux of permeate was 245?L?h^?1?m^?2?bar^?1, which corresponded to a retention rate of about 13%.     

Effect of the pyrolytic carbon (PyC) content on the dielectric and electromagnetic interference shielding properties of layered SiC/PyC porous ceramics

A novel layered SiC/pyrolytic carbon (PyC) porous ceramic was synthesized from a nickel foam substrate via low-pressure chemical vapor infiltration (LPCVI) with SiCl₃CH₃-NH₃-BCl₃-H₂-Ar. The microstructure and phase composition of the PyC deposited via Ni catalysis were investigated. In addition, the effect of the PyC content on the microstructure, conductivity, and electromagnetic shielding effectiveness of a two-layered SiC/PyC porous ceramic were discussed. Both the electrical conductivity (from 0.090 to 0.319?S/cm) and the total shielding effectiveness (from 19.2 to 29.0?dB) of the two-layer SiC/PyC porous ceramic (pore size: 200–400?µm) increased with the PyC content. The high-temperature shielding effectiveness of the sample showed an outstanding stability with temperature and remained nearly unchanged (only 2?dB variation) over the 25–600?°C temperature range.     

Corrosion behaviors of porous reaction-bonded silicon carbide ceramics incorporated with CaO

Reaction-bonded SiC (RBSC) porous ceramics were fabricated at 1450?°C in air by incorporating CaO using ZrO₂ as sintering aids, activated carbon as pore-forming agent, and mullite fibers as reinforcing agent. The effects of CaO content on the properties of the porous RBSC ceramics were studied. Corrosion behaviors of the prepared RBSC porous ceramics in different environments were also investigated. The optimal open porosity, bending strength, average pore size and gas permeability of the ceramics with 0.5% CaO were 40%, 22.5?MPa, 42.9?µm, and 2100?m³/m² h?kPa, respectively. A well-developed neck reaction-bonded by calcium zirconium silicate (Ca₃ZrSi₂O₉) was identified. The porous RBSC ceramics exhibited excellent corrosion resistance in acid and basic solutions. The anti-oxidation temperature of the porous RBSC ceramics could reach 1200?°C in air. The RBSC ceramics maintained the bending strength of 17.5?MPa after 60 cold-hot cycles in air (0–800?°C). The porous RBSC ceramics also exhibited relatively good corrosion resistance in molten salts (NaCl, Na₂SO₄ and CaCl₂). Melten NaOH can aggravate the reaction by breaking the SiO₂ layers on the SiC surface. Overall, these findings offer significant insights into expanding the applications porous RBSC ceramics incorporated with CaO.     

Preparation of ultra-light ceramic foams from waste glass and fly ash

Ultra-light ceramic foams were successfully prepared by a green spheres technique, which used waste glass powder and fly ash as the main material. Besides, borax and SiC were introduced as fluxing agent and foaming agent, respectively. The effects of fly ash content, borax content and sintering temperature on the microstructures and properties of ceramic foams were systematically investigated. The optimum composition is 30?wt-% fly ash, 70?wt-% waste glass, 15?wt-% borax and 0.5?wt-% SiC. Ultra-light ceramic foams sintered at 680–780°C possess bulk density of 0.14–0.41?g?cm^?3, porosity of 82.9–94.1%, compressive strength of 0.91–6.37?MPa and thermal conductivity of 0.070–0.121?W?m^?1?K^?1, respectively. This method is convenient, low-cost and environment friendly, which makes it a promising way for recycling solid wastes.     

Synthesis and characterisation of a submicrometre silicon carbide powder

A beta-silicon carbide powder with a surface area of 30m²g^?l and a mean particle size of < 1μm was produced from the thermal conversion of silicon resin in an atmosphere of hydrogen. The amount of product increased with increasing iron content (0–2.1 wt%) and firing temperature (1200–1500°C). Chemical analysis, X-ray diffraction and i.r. absorption spectrometry were used to follow the conversion reaction.     

Fabrication and properties of ultra highly porous silicon carbide by the gelation–freezing method

Silicon carbide (SiC) with ultra high porosity and unidirectionally oriented micrometer-sized cylindrical pores was prepared using a novel gelation–freezing (GF) method. Gelatin, water and silicon carbide powder were mixed and cooled at 7 °C. The obtained gels were frozen from ?10 to ?70 °C, dried using a vacuum freeze drier, degreased at 600 °C and then sintered at 1800 °C for 2 h. The gels could be easily formed into various shapes, such as cylinders, large pipes and honeycombs using molds. Scanning electron microscopy (SEM) observations of the sintered bodies showed a microstructure composed of ordered micrometer-sized cylindrical cells with unidirectional orientation. The cell size ranging from 34 to 147 μm could be modulated by changing the freezing temperatures. The numbers of cells for the samples frozen at ?10 and ?70 °C were 47 and 900 cells/mm², respectively, as determined from cross-sections of the sintered bodies. The resulting porous SiC with a total porosity of 86%, exhibited air permeability from 2.3 × 10^?11 to 1.0 × 10^?10 m², which was the same as the calculated ideal permeability, and high compressive strength of 16.6 MPa. The porosity, number of cells, air permeability and strength of the present porous SiC were significantly higher than that reported for other porous SiC ceramics.     

Effect of porous properties on self-cooling of fired clay plate by evaporation of absorbed water

Porous ceramic plates were prepared from clay and wood charcoal powder at 900 and 1100?°C and their porous properties, water absorption and the cooling effect of porous plates were investigated to produce eco-friendly porous ceramics for cooling by the evaporation of absorbed water. Porous properties were dependent on the firing temperature, and total pore volume, average pore size and porosity, which were 0.38–0.39 cm³/g, 0.15–0.17 μm and 49–50%, respectively at 900?°C and 0.31–0.33 cm³/g, 2.47–2.59 μm and 43–44%, respectively at 1100?°C. By the addition of wood charcoal powder, the cooling rate of porous plate fired at 1100?°C was 1.7 times faster than that of the plate fired at 900?°C and the cooling temperature difference (?T) was around 2.3?°C at 22.5?°C and 52–54% of relative humidity and around 3.2?°C at 29?°C and 77–80% of relative humidity. The porous ceramic plates developed here are potential materials for cooling buildings.     

Controllable preparation of porous ZrB2–SiC ceramics via using KCl space holders

In this work, a novel and facile technique based on using KCl as space holders, along with partial sintering (at 1900 °C for 30 min), was explored to prepare porous ZrB₂–SiC ceramics with controllable pore structure, tunable compressive strength and thermal conductivity. The as-prepared porous ZrB₂–SiC samples possess high porosity of 45–67%, low average pore size of 3–7 μm, high compressive strength of 32–106 MPa, and low room temperature thermal conductivity of 13–34 W m⁻¹ K⁻¹. The porosity, pore structure, compressive strength and thermal conductivity of porous ZrB₂–SiC ceramics can be tuned simply by changing KCl content and its particle size. The effect of porosity and pore structure on the thermal conductivity of as-prepared porous ZrB₂–SiC ceramics was examined and found to be consistent with the classical model for porous materials. The poring mechanism of porous ZrB₂–SiC samples via adding pore-forming agent combined with partial sintering was also preliminary illustrated.     

Design and characterization of porous mullite based semi-vitrified ceramics

Three porous ceramic composites were prepared from readily available raw materials (kaolin, bauxite, feldspar and kyanite). The porous ceramic formulations were sintered at different temperatures ranging from 1200 to 1400°C. The fired specimens were characterized by determining their porosity, bulk density, flexural strength, thermochemical stability, microstructure, water and mercury permeability. Apparent porosity and bulk density in the range 15.57 ± 1.56–42.73 ± 2.28?vol% and 2.23 ± 0.31–2.68 ± 0.41?g?cm^?3 respectively were obtained after firing. The flexural strength was in the range of 32.31 ± 2.1–74.88 ± 2.57?MPa and the thermal expansion coefficient of 5–9 × 10^?6 C^?1. The values of water permeability were 745.4, 641.45 and 525.91?L/m² h?kPa respectively for PK3, PK4 and PK5. It was found that at high temperature (1400?°C), kyanite particles enhanced the porosity and thermal stability by reducing glass formation and improving crystallization. The presence of the interconnected pores with size between 0.03 and 4.50?µm, the high total volume of pores together with the high flexural strength and thermal stability make the synthesized porous ceramics suitable for high-pressure filtering applications.     

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.     

Porous asymmetric microfiltration membranes shaped by combined alumina freeze and tape casting

An assembled asymmetric alumina microfiltration membrane with high performance was prepared by combining freeze and tape casting techniques followed by two sintering steps. Freeze casting was used for manufacturing of the porous support layer with a highly interconnected pore network. Tape casting was applied on the top layer to form a pre-membrane with smaller pore size and controlled thickness, which was set on the sintered support. Morphology influences were investigated for different solid loadings, additives content and the assembled layer membrane structures. No delamination among the layers was observed. The assembled ceramic membrane had an average pore size between 30 and 50 μm together with a top surface layer around 0.35 μm, which is suitable to the microfiltration separation process. Porosity in the range of 26–50 % and water flux of 11–32 m³ m^?2 h^?1 bar^?1 were reached for samples prepared with two sintering steps at 1600 and 1300 °C for 2 h.     

Low-temperature sintering of silicon carbide membrane supports from disks to single- and 19-channel tubes

As the configuration of asymmetric ceramic membranes is determined by the membrane supports, a low temperature sintering process was developed to prepare ceramic membrane supports from disks to single- and 19-channel tubes. The residual of NaA zeolite was introduced into the silicon carbide (SiC) matrix, and porous SiC membrane supports were successfully prepared at 1100 °C. Compared with the disk-like support, the open porosity, average pore size and pure water permeance of the single-channel supports obviously increased, and their bending strength decreased accordingly. These differences were mainly attributed to the incorporation of organic plasticizer and the change in molding process. Notably, the pure water permeance of disks, single- and 19-channel tubes was 70 ± 3, 74 ± 4 and 22 ± 1 m³·m^?2·h^?1·bar^?1, respectively, which was much higher than the previously reported values. Therefore, this work provides important guides to develop of new generation ceramic membranes for practical application.     

Hypercrosslinked porous polyporphyrin by metal-free protocol: characterization,uptake performance,and heterogeneous catalysis

Through metal-free protocol, hypercrosslinked porous polyporphyrin with permanent porosity was obatined via the Friedel–Crafts alkylation of tetracarbazolylporphyrin using formaldehyde dimethyl acetal as an external cross-linker. Its chemical structure and porosity was well characterized and confirmed. The BET specific surface area value of HCP-TCPP is 1050 m² g^?1 and related dominant pore size is centered at 0.63 nm. The adsorption amount of methanol by HCP-TCPP is high up to 800 mg g^?1 (about 25.0 mmol g^?1) at its saturated vapor pressure, which is higher than that of toluene (600 mg g^?1, 6.5 mmol g^?1). Further study indicates that polymer HCP-TCPP, possessing the high BET specific surface area and total pore volume, exhibits good hydrogen uptake of 3.44 wt % (77 K) and high carbon dioxide uptake of 41.1 wt % (298 K) at 18.0 bar. Besides, the obtained porous polymer can also be used as an effective heterogeneous catalyst for the Knoevenagel condensation between various aldehydes and malononitrile.     

Grain-growth-induced high electrical conductivity in SiC–BN composites

SiC–BN composites were fabricated by conventional hot-pressing from β-SiC and h-BN nanopowders with 2?vol% yttria as a sintering additive. Electrical and thermal properties of the composites were investigated as a function of initial BN content. Owing to the nanosize of the starting powders, the grain-growth-assisted N-doping of the SiC lattice was significantly enhanced during liquid-phase sintering, yielding the highest-reported electrical conductivity of ~124 (Ω?cm)^?1 for a SiC–4-vol% BN composite. The typical values of electrical resistivity and thermal conductivity of the SiC–4-vol% BN composite at room temperature were 8.1?×?10^?3 Ω?cm and 92.4?W?m^?1 K^?1, respectively.     

Porous Si3N4 ceramics prepared by aqueous gelcasting using low–toxicity DMAA system: Regulatable microstructure and properties by monomer content

In this study, the low–toxicity monomer N, N–dimethylacrylamide (DMAA), serving as both gelling agent and pore–forming agent, was adopted to fabricate porous Si₃N₄ ceramics with a regulatable microstructure and property by aqueous gelcasting. Results indicate that monomer content played an important role in regulating and optimizing the properties of sintered bodies. With increasing monomer content (5.94–30.69?wt%), both slurry viscosity (maximum 0.14?Pa?s at 95.40 s^?1) and green body strength (11.35–49.23?MPa) exhibited monotonic increasing trends, demonstrating superior mechanical properties to those obtained using the neurovirulent acrylamide (AM) gelling system. The increased monomer content not only improved porosity, but also promoted α→β–Si₃N₄ transformation as well as β–Si₃N₄ grain growth through enhancing the connectivity of interlocking pores and accelerating the vapor phase transport during liquid–phase sintering. These variations in phase composition and microstructure derived from the varied monomer content further resulted in monotonic changes in porosity (40.32–51.50%), mean pore size (0.27–0.38?μm), flexural strength (202.77–132.15?MPa), fracture toughness (2.93–2.32?MPa?m^1/2), dielectric constant (3.48–2.78) and loss (3.52–3.09?×?10^?3) at 10?GHz for sintered bodies, displaying an excellent comprehensive properties. This study suggests a promising prospect for DMAA in preparation of high–performance porous Si₃N₄ ceramics by aqueous gelcasting.