Mechanical properties of sintered ZrB2-SiC ceramics

ZrB₂ ceramics containing 10-30 vol% SiC were pressurelessly sintered to near full density (relative density >97%). The effects of carbon content, SiC volume fraction and SiC starting particle size on the mechanical properties were evaluated. Microstructure analysis indicated that higher levels of carbon additions (10 wt% based on SiC content) resulted in excess carbon at the grain boundaries, which decreased flexure strength. Elastic modulus, hardness, flexure strength and fracture toughness values all increased with increasing SiC content for compositions with 5 wt% carbon. Reducing the size of the starting SiC particles decreased the ZrB₂ grain size and changed the morphology of the final SiC grains from equiaxed to whisker-like, also affecting the flexure strength. The ceramics prepared from middle starting powder with an equiaxed SiC grain morphology had the highest flexure strength (600 MPa) compared with ceramics prepared from finer or coarser SiC powders.     

Synthesis of SiC/SiO2 core–shell powder by rotary chemical vapor deposition and its consolidation by spark plasma sintering

SiC (core) and SiO₂ (shell) powders were synthesized via rotary chemical vapor deposition (RCVD). The SiC particles (3C, <1 μm in diameter) were coated with a layer of SiO₂ (10–15 nm in thickness). Using spark plasma sintering, the SiC/SiO₂ nanopowders were then synthesized into SiC/SiO₂ composite bodies. Although a phase transformation from 3C to 6H was observed at above 2123 K in the sintered monolithic SiC bodies, sintered SiC/SiO₂ bodies did not display such phase transformation. In addition, SiC/SiO₂ bodies did not exhibited grain growth until the sintering temperature reached 2223 K. The density and Vickers hardness of the sintered SiC/SiO₂ bodies increased with increasing sintering temperature. The highest density and hardness of SiC/SiO₂ composite bodies were 98.1% and 24.4 GPa at 2223 K, respectively, which were higher than the corresponding values of 90% and 14 GPa for monolithic SiC bodies.     

Effect of CTAB as a foaming agent on the properties of alumina ceramic membranes

Alumina-ceramic membranes were prepared by gelcasting process using CTAB as a foaming agent. To increase the fineness, the starting alumina powder was milled for 1 h in a ball mill before the casting process. Particle size distribution and surface area measurements of the as-received and milled alumina powder were examined. The casted alumina membranes were sintered at 1500 °C. Sintering parameters in terms of bulk density (BD) and apparent porosity (AP) were determined by the Archimedes method. Pore size distribution of the sintered porous alumina membranes was measured using mercury porosimeter. Microstructure of sintered membranes was investigated by scanning electron microscope (SEM). Cold crushing strength (CCS) of the sintered specimens was also evaluated. The result revealed that the properties of porous ceramics such as porosity, average pore size, pore size distribution and cold crushing strength could be controlled by adjusting the preparation conditions e.g. solid loading, sintering temperature and foaming agent. The open porosity, cold crushing strength and average pore size of the alumina ceramics sintered at 1500 °C were around 58.35%, 18 MPa and178 nm, respectively.     

Microstructural Characterization of Porous Silicon Carbide Membrane Support With and Without Alumina Additive

Porous silicon carbide (SiC) membrane supports sintered at 1500°–1800°C were prepared by cold isostatic pressing (CIP) under different pressures and using different amounts of alumina additive (0%–4%). The relationship between processing factors and pore size and microstructure was examined. Varying the sintering temperature, the CIP pressure and the amount of additive used were found to be effective for controlling pore size and microstructure. The pore size and particle size of the membrane support prepared without alumina were found to increase with increasing sintering temperature. This was attributed to surface diffusion. Densification of the undoped support did not occur, however, because of concurrent pore development. In the SiC membrane support containing 4% alumina, small particles and a pore size of around 100 nm were retained. This was because of the formation of a limited amount of SiO₂–Al₂O₃ liquid phase during sintering.     

Effect of SiC content,additives and process parameters on densification and structure–property relations of pressureless sintered ZrB2–SiC composites

The effect of SiC content, additives, and process parameters on densification and structure–property relations of pressureless sintered ZrB₂–(10–40 vol%) SiC particulate composites have been studied. The ZrB₂–SiC composite powders mixed by ball-milling with 1.2 wt% C (added as phenolic resin) and 3 wt% B₄C have been uniaxially cold-compacted and sintered in argon environment at 1950–2050 °C for 2 h, or at 2000 °C for durations between 1/2 and 3 h. The amount of densification is found to increase with sintering duration, and by prior holding at 1250 and 1600 °C for reduction of oxide impurities (ZrO₂, B₂O₃ and SiO₂) on powder particle surfaces by the aforementioned additives. Presence of SiC with average size smaller than that of ZrB₂ appears to aid in densification by enhancing green density, increasing WC content by erosion of milling media, and inhibiting matrix grain growth. Both SiC and WC appear to aid in reduction of oxide impurities. Furthermore, the impurities enriched in W, Fe and Co obtained from milling media are found to be segregated at ZrB₂ grain boundaries, and appear to assist in densification by forming liquid phase, which completely wets the ZrB₂ grains. Hardness increases with SiC content or with sintering duration till 1 h, but decreases for periods ≥2 h due to grain growth. The experimentally measured elastic moduli approaches corresponding theoretically predicted values with increasing SiC content due to reduction in porosity.     

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.     

Processing and microstructure characterization of porous corundum–spinel ceramics prepared by in situ decomposition pore-forming technique

Porous corundum–spinel ceramics were prepared from Al(OH)₃ and basic magnesium carbonate by an in situ decomposition pore-forming technique. Apparent porosity was detected by Archimedes’ Principle with water as medium. Pore size distribution and the volume percentage of micropores were measured by mercury intrusion porosimetry, and the microstructure was analyzed by SEM. The apparent porosity of the sintered sample decreased with increasing the Al(OH)₃ content in the raw mixture. With increasing temperature from 1200 °C to 1300 °C the porosity of the sample increased rapidly, from 1300 °C to 1500 °C the apparent porosity increased slightly, while it decreased rapidly when the temperature increased from 1500 °C to 1600 °C. The pores in the samples consist of two groups. One group is composed of micropores whose diameter is mostly in the range from 150 nm to 300 nm while the other is composed of bigger pores whose diameter is in the range from 0.5 μm to 1 μm. It was found that the composition of the starting powders and the sintering temperature are responsible for the apparent porosity and the pore size distribution of the samples. However the spinel formation and sintering play a more important role on porosity and pore size distribution.     

Fabrication and characterization of sintered TiC-SiC composites

Some TiC-SiC composites with different SiC volume contents (0, 10, 25 and 50%) are prepared by spark plasma sintering (SPS). The relationship between density, grain growth and temperature is studied in order to fabricate dense and nano-sized TiC-SiC composites. A sintering by SPS at 1800 °C during 5 min allowed to form TiC-SiC composites with relative density above 95% and an homogeneous distribution of TiC (grain size from 270 to 900 μm) and nano-sized SiC. With the increasing of SiC volume contents, Vickers hardness and fracture toughness are improved; thermal conductivity at room temperature is increased whereas at high temperature it is reduced. In future studies, those materials will be irradiated to characterize monolithic TiC and TiC-SiC composites behaviour under irradiation.     

Fabrication of transparent neodymium-doped yttrium aluminum garnet ceramics by high solid loading suspensions

Dense neodymium-doped yttrium aluminum garnet (Nd:YAG) transparent ceramic was obtained by slip casting and solid-state reaction. The colloidal behavior of the aqueous suspensions of neodymia, yttria, and alumina mixed powders using Dispex A as dispersant was investigated. The variation in zeta potential due to pH alteration was studied. The isoelectric point (IEP) was at pH 4.5 and 4 for the specimens with and without Dispex A, respectively. The optimal dispersion conditions were achieved for the suspensions at pH 9.6 with 0.4 wt% Dispex A. The green body prepared by slip casting was vacuum sintered from 1200 °C to 1750 °C. The grain size of the sintered body increased, and the pore size decreased with increasing sintering temperature. Pore-free Nd:YAG transparent ceramic with a grain size of 5–10 μm was obtained by sintering at 1750 °C for 10 h. The in-line transmittance of the annealed specimen reached 80.8% at 1064 nm.     

Effect of sintering temperature on compressive strength of porous yttria-stabilized zirconia ceramics

Porous yttria-stabilized zirconia (YSZ) ceramics were fabricated by tert-butyl alcohol (TBA)-based gel-casting method for potential applications in heat-insulation materials. The effect of sintering temperature on compressive strength of porous YSZ ceramics was investigated on the basis of measurements linear shrinkage, porosity and pore size. As the sintering temperature increased from 1350 to 1550 °C, a decrease of porosity from 77 to 65%, a decrease of average pore size from and an increase of linear shrinkage from 15.4 to 31.8% were observed. The compressive strength increased remarkably from 3 to 27 MPa with increasing sintering temperature from 1350 to 1550 °C, which was related to the corresponding change of linear shrinkage, porosity, pore size and microstructure. A remarkable decrease of compressive strength with increasing porosity was observed. The compressive strength decreased also with increasing pore size.     

Effect of solid loading and carbon additive on microstructure and mechanical properties of 3D-printed SiC ceramic

3D-printed SiC ceramics were prepared by direct ink writing and solid-phase sintering. The effects of sintering temperature, solid loading, and carbon additive on microstructures and mechanical properties of 3D-printed SiC parts were investigated. It was found that the sintering temperature affected the evolution of the microstructure and mechanical properties of the sintered SiC parts. A high solid loading promoted the densification and mechanical properties of the sintered SiC parts. However, the solid loading exceeded 40 vol.%, which decreased the density and mechanical properties of the samples. The carbon additives could improve the densification of the SiC parts and enhance their mechanical properties. When the sucrose content increased from 0 to 8 wt.%, the open porosity of the SiC part decreased from 26.12% to 3.15%, whereas the flexural strength increased 2.19 times. Using the optimized components and process parameters, the high-performance 3D-printed SiC parts were achieved.     

Particle size reduction of anthracite coals during devolatilization in a thermobalance reactor

The effects of devolatilization temperature (750-900 °C), coal size (2-12 mm) and coal properties (carbon content, Hardgrove index (HGI), pore volume) of anthracite coals on the primary fragmentation and particle size reduction during devolatilization have been determined in a thermobalance reactor. The fragmentation index increases with increasing devolatilization temperature and particle size. The fragmentation index is also influenced by coal properties, such as carbon content, HGI, pore volume, etc. Thus, the reduction ratio of particle size before and after devolatilization increases with increasing devolatilization temperature and particle size.     

利用黄金尾矿制备发泡陶瓷的研究

中国黄金尾矿资源量大,作为二次资源在建筑材料领域的综合利用有着重要的经济价值和环境意义。以黄金尾矿为主要原料,SiC为发泡剂,通过高温制备发泡陶瓷,用激光共聚焦显微镜、XRD等手段,研究了烧结温度、黄金尾矿掺入量、原料粒度对材料的容重、真气孔率和孔径等性能的影响。研究表明:随着烧结温度的升高,发泡陶瓷材料的真气孔率和孔径增大,容重减小;材料的真气孔率和容重随着黄金尾矿掺入量的增大分别降低和提高,随着原料粒度的减小分别提高和降低,气孔孔径随着黄金尾矿掺量的增大和原料粒度的减小均呈下降趋势。优化后,在烧成温度1 050 ℃,黄金尾矿掺入量50%(质量分数),黄金尾矿平均粒度D(50)=5.6 μm,SiC平均粒度D(50)=3.0 μm的条件下可制备出性能良好的发泡陶瓷。     

Effect of bentonite addition on fabrication of reticulated porous SiC ceramics for liquid metal infiltration

SiC with different particles and a clay mineral bentonite (montmorillonite) were mixed in water to prepare ceramic slurry. The slurry was then infiltrated high porous polyurethane sponge. Excess slurry was squeezed out to adjust ceramic rate in the infiltrated body. The pore walls were coated with ceramic mix after the infiltrated body was dried. The polyurethane containing SiC particles and bentonite was fired in a box furnace to burn out the polyurethane from the body at 500 °C for 30 min. The remaining porous ceramic bodies were sintered at elevated temperatures to give strength. SiC particles with bentonite surface coating took polyurethane pore forms after firing the sponge. Bentonite was both used as binder for ceramic slurry at room temperatures and the sintering additives at elevated temperatures. Therefore, increasing bentonite addition gives higher strength to the resulting ceramic performs.     

Improvement of wetability,sinterability, mechanical and electrical properties of Al2O3-Ni nanocomposites prepared by mechanical alloying

The wetability improvement and particle size reduction of alumina/Ni composites through mechanical alloying were addressed. Their effect on the sinterability (at high temperature), mechanical and electrical properties were studied. Al₂O₃ matrix nanocomposites reinforced with different volume fractions of Ni up to 10 vol% were prepared by mechanical alloying. The milled powders were cold pressed and sintered at different firing temperatures up to 1600 °C. The morphology of powders and the microstructure of sintered bodies were investigated by transmission electron microscopy (TEM) and scanning electron microscopy (SEM) coupled with energy dispersive spectroscopy (EDS), respectively. Furthermore, relative density, apparent porosity, mechanical properties and electrical resistivity of the sintered composites were investigated. The results revealed that Al₂O₃ matrix was successfully coated with Ni thin film through mechanical alloying; the thickness of coat was increased with increasing the Ni content. Moreover, the increasing of both Ni content and sintering temperature up 1600 °C, led to a remarkable increase in the relative density and facture toughness of the sintered specimen. On the other hand, microhardness and elastic modulus were decreased with increasing of Ni content, while they increased significantly with the increase of sintering temperature. The electrical resistivity was decreased with increasing Ni content and sintering temperature.     

Studies on ionic conductivity of stabilized zirconia ceramics (8YSZ) densified through conventional and non-conventional sintering methodologies

Densification studies of 8 mol% yttria stabilized zirconia ceramics were carried out by employing the sintering techniques of conventional ramp and hold (CRH), spark plasma sintering (SPS), microwave sintering (MWS) and two-stage sintering (TSS). Sintering parameters were optimized for the above techniques to achieve a sintered density of >99% TD. Microstructure evaluation and grain size analysis indicated substantial variation in grain sizes, ranging from 4.67 μm to 1.16 μm, based on the sintering methodologies employed. Further, sample was also sintered by SPS technique at 1425 °C and grains were intentionally grown to 8.8 μm in order to elucidate the effect of grain size on the ionic conductivity. Impedance spectroscopy was used to determine the grain and grain boundary conductivities of the above specimens in the temperature range of RT to 800 °C. Highest conductivity of 0.134 S/cm was exhibited by SPS sample having an average grain size of 1.16 μm and a decrease in conductivity to 0.104 S/cm was observed for SPS sample with a grain size of 8.8 μm. Ionic conductivity of all other samples sintered vide the techniques of TSS, CRH and MWS samples was found to be ∼0.09 S/cm. Highest conductivity irrespective of the grain size of SPS sintered samples, can be attributed to the low densification temperature of 1325 °C as compared to other sintering techniques which necessitated high temperatures of ∼1500 °C. The exposure to high temperatures while sintering with TSS, CRH and MWS resulted into yttria segregation leading to the depletion of yttria content in fully stabilized zirconia stoichiometry as evidenced by Energy Dispersive Spectroscopy (EDS) studies.     

Effect of LiAlSiO4 particle size on the properties of LAS/SiC porous ceramics with near zero thermal expansion

Near zero thermal expansion porous ceramics were fabricated by using SiC and LiAlSiO₄ as positive and negative thermal expansion materials, respectively, bonded by glassy material. The microstructure, mechanical properties, and thermal expansion behavior of LAS/SiC porous ceramics with different particle sizes of LiAlSiO₄ were investigated. The results indicated that the coefficient of thermal expansion of the LAS/SiC porous ceramics decreased from 0.5206×10⁻⁶ to −1.1053×10⁻⁶ K⁻¹ with increasing the LiAlSiO₄ particle size from ~45 µm to ~125 μm. It was attributed to the reduction in the reaction between LiAlSiO₄ and SiO₂ as the particle size of LiAlSiO₄ increased. Young’s modulus increased from 36 MPa to 54 MPa as the sintering temperature increased from 850 °C to 950 °C because of the good bonding between the SiC grains and the glass materials.     

Improvement of microstructural properties of 3Y-TZP materials by conventional and non-conventional sintering techniques

3 mol% Y₂O₃-stabilized zirconia nanopowders were fabricated using various sintering techniques; conventional sintering (CS) and non-conventional sintering such as microwave (MW) and pulsed electric current-assisted-sintering (PECS) at 1300 °C and 1400 °C. A considerable difference in the densification behaviour between conventional and non-conventional sintered specimens was observed. The MW materials attain a bulk density 99.4% theoretical density (t.d.) at 1300 °C, while the CS materials attain only 92.5% t.d. and PECS 98.7% t.d. Detailed microstructural evaluation indicated that a low temperature densification leading to finer grain sizes (135 nm) could be achieved by PECS followed by MW with an average sintered grain size of 188 nm and CS 225 nm. It is believed that the high heating rate and effective particle packing are responsible for the improvements in these properties.     

Electrically conductive SiC ceramics processed by pressureless sintering

Polycrystalline SiC ceramics with 10 vol% Y₂O₃-AlN additives were sintered without any applied pressure at temperatures of 1900-2050°C in nitrogen. The electrical resistivity of the resulting SiC ceramics decreased from 6.5 × 10¹ to 1.9 × 10⁻² Ω·cm as the sintering temperature increased from 1900 to 2050°C. The average grain size increased from 0.68 to 2.34 μm with increase in sintering temperature. A decrease in the electrical resistivity with increasing sintering temperature was attributed to the grain-growth-induced N-doping in the SiC grains, which is supported by the enhanced carrier density. The electrical conductivity of the SiC ceramic sintered at 2050°C was ~53 Ω⁻¹·cm⁻¹ at room temperature. This ceramic achieved the highest electrical conductivity among pressureless liquid-phase sintered SiC ceramics.     

Oxidation protection of SiC in porcelain tile ceramics by adding Si powder

Polishing porcelain tile residues (PPR) have accumulated to millions of tons and increases every year. It has become important to recycle the PPR due to the economic gains and environmental sustainability of doing so. However, its direct recycling in the production of porcelain tile has been limited by the fact that SiC particles oxidise during sintering which prevents the processing of dense ceramics. In this study, Si powder was introduced into the porcelain ceramics matrix containing SiC. The effect of Si powder additive on inhibiting the oxidation of SiC was evaluated using the relative density and the microstructure of the sintered samples. Results showed that the porcelain body containing SiC could be fully densitified when the suitable content of Si powder addition is introduced. These results indicate that it is a promising method to effectively protect the oxidation of SiC particles in the porcelain ceramics matrix during sintering.