Sol-gel derived zirconia membrane on silicon carbide substrate

To enhance the high temperature and chemical corrosion resistances of ceramics membrane, a ZrO₂/SiC ceramic membrane was prepared through sol-gel route followed by the dip-coating technique. The substrate layer was made of pure silicon carbide phase by evaporation-condensation process, and the separation layer was made of zirconia phase by solid-phase sintering process. The substrate layer was sintered at 2200 ℃ in the vacuum, and the pores were distributed in a narrow size range from 4.5–6.0 μm. When the membrane was sintered at 700 ℃, a defect-free separation layer formed on the substrate. With the increase of sintering temperature, the average pore size of the separation layer declined from 63 to 48 nm, and the water permeability declined from 355 to 273 L/(m²·h·bar). Our results indicate the ZrO₂/SiC ceramic membrane has potential applications in the separation of high temperature or chemically corrosive wastewaters.     

Processing and microstructure-permeation properties of silica bonded silicon carbide ceramic membrane

Porous SiC is a valuable membrane material for the microfiltration and ultrafiltration of various wastewaters because of its high hydrophilicity and low fouling tendency, but its preparation has been limited by the high sintering temperature. Here, a silica bonded silicon carbide membrane was prepared by the oxidation of SiC at low temperature. When the SiC substrates were sintered in the temperature range from 1200 to 1400℃, their porosity decreased from 45 % to 37 % while the flexural strength increased from 45 to 59 MPa. For the selective layers made from SiC particles with 0.5 μm in diameter, the average pore sizes that sintered at 1050 and 1150 ℃ were 0.34 and 0.26 μm, respectively, corresponding to the water fluxes of 1080 and 1240 L/(m² h, respectively. Thus, this technique provided a cost-effective path to prepare ceramic membrane at low sintering temperature.     

Effects of SDBS and ZrO2 additives on the microstructure and properties of silicon-bonded SiC porous ceramics

Porous silicon-bonded silicon carbide (SBSC) ceramics were prepared under argon atmosphere, with silicon as pore former and bonding material, simultaneously, sodium dodecyl benzene sulfonate (SDBS) and ZrO₂ as sintering additives, the effects of SDBS and ZrO₂ on the porosity, pore size, mechanical, physical and thermal properties and microstructures were investigated. The results suggested that suitable content of SDBS and ZrO₂ could not only effectively lower the sintering temperature to 1450 °C due to the sticky flow of molten silicon, but also increase the pore structure and improve the bending strength. The reason for this is that SDBS decomposed into Na₂O which reacted with ZrO₂ and impurity SiO₂, which was the native oxide film on the surface of SiC particles, to form a bonding phase between SiC particles to improve the bending strength; meanwhile, the disappearances of impurity SiO₂ would benefit the bond of molten silicon and silicon carbide particles, and silicon melt leaving pores in its original position to increase the pore structure. The optimal apparent porosity, bending strength, average pore size, gas permeance and residual bending strength after thermal shock cycles of SBSC porous ceramic sintered at 1450 °C with 5 wt% SDBS and 6 wt% ZrO₂ were 38.33%, 55.4 MPa, 11.3 μm, 106.4 m³/m²·h·kPa and 28.2 MPa, respectively.     

Tuning microstructures and separation behaviors of pure silicon carbide membranes

This study reports the preparation of silicon carbide ceramic membranes with pure silicon carbide particles without sintering aids. The effects of sintering temperature on the microstructure, mechanical and filtration properties were investigated. The porosity of the substrate layer increased from 37% to 41% when the sintering temperature ranged from 2150 to 2300 °C, whereas the flexural strength increased from 14.5 to 18.2 MPa. The separation layer was coated on the substrate layer using a spray process. When sintered at 1850 °C, a smooth and defect-free layer was formed with an average pore size and layer thickness of 1.2 and 60 μm, respectively. With the increase of average pore size, the filtration flux increased from 2650 to 2800 L/(m² h bar). Such ceramic membranes can be used to separate corrosive wastewater and high-temperature wastewaters owing to the exclusion of sintering aids, unlike the conventional ceramic membranes.     

Evaporation-condensation derived silicon carbide membrane from silicon carbide particles with different sizes

Silicon carbide ceramic is a promising membrane material because of the high corrosive and high temperature resistance, and the excellent hydrophility. Here, a silicon carbide ceramic membrane with both substrate layer and separate layer composed of pure silicon carbide phase was successfully prepared. The effect of particle size on the microstructure and properties was investigated. The substrates were prepared from three silicon carbide particles at 2200 ℃. With the content increase of fine particle, the average pore size increased from 5.6 μm to 14.1 μm; meanwhile, the flexural strength of the substrate increased from 14.1 MPa to 24.6 MPa. The separation layers were made from particles of 3.0 μm and 0.5 μm. When sintered at 1900 ℃, the separation layer formed pore network with homogeneous structure. Such silicon ceramic membrane can be used in harsh conditions, including high temperature wastewater and strongly corrosive wastewater.     

A novel combination of precursor pyrolysis assisted sintering and rapid sintering for construction of multi-composition coatings to improve ablation resistance of SiOC ceramic modified carbon fiber needled felt preform composites

A double-layer coating composed of MoSi₂–SiO₂–SiC/ZrB₂–MoSi₂–SiC was designed and successfully constructed by a novel combination of precursor pyrolysis assisted sintering and rapid sintering to improve the ablation resistance of SiOC ceramic modified carbon fiber needled felt preform composites (CSs). The ZrB₂–MoSi₂–SiC inner layer coating was in relatively uniform distribution in the zone of 0–3 mm from the surface of CSs through the slurry/precursor infiltration in vacuum and SiOC precursor pyrolysis assisted sintering, which played a predominant role in improving oxidation and ablation resistance and maintaining the morphology of CSs. The MoSi₂–SiO₂–SiC outer layer coating was prepared by the spray and rapid sintering to further protect CSs from high-temperature oxidation. The ablation resistance of CSs coated with double-layer coating was evaluated by an oxygen-acetylene ablation test under the temperature of 1600–1800 °C with different ablation time of 1000 and 1500 s. The results revealed that the mass recession rates increased with the rise of ablation temperature and extension of ablation time, ranging from 0.47 g/(m²·s) to 0.98 g/(m²·s) at 1600–1800 °C for 1000 s and from 0.72 g/(m²·s) to 0.86 g/(m²·s) for 1000–1500 s at 1700 °C, while the linear recession rates showed negative values at 1700 °C due to the formation of oxides, such as SiO₂ and ZrO₂. The ablation mechanism of the double-layer coating was analyzed and found that a SiO₂–ZrO₂–Mo_4.8Si₃C_0.6 oxidation protection barrier would be formed during the ablation process to prevent the oxygen diffusion into the interior CSs, and this study provided a novel and effective way to fabricate high-temperature oxidation protective and ablation resistant coating.     

Characterization of B4C-SiC ceramic composites prepared by ultra-high pressure sintering

Additive-free boron carbide (B₄C) – silicon carbide (SiC) ceramic composites with different B₄C and β-SiC powders ratio were densified using the high-pressure “anvil-type with hollows” apparatus at 1500 °C under a pressure of 4 GPa for 60 s in air. The effect of starting powders ratio on the composites sintering behavior, relative density, microstructural development, and thermomechanical properties was studied. The sintered samples hardness was found to be in the range from 24 to 31 GPa. The thermal conductivity measurements, conducted in the temperature range from room temperature to 1000 °C, showed that the thermal diffusivity of sintered samples was between 6 and 9.5 mm²/s whereas the thermal conductivity was in the range from 16 to 28 W/(m K). The results of this study show that the high-pressure sintering can be a very effective low-temperature densification method for the obtainment of additive-free B₄C - β-SiC ceramic composites.     

Highly electrically and thermally conductive silicon carbide-graphene composites with yttria and scandia additives

Dense silicon carbide/graphene nanoplatelets (GNPs) and silicon carbide/graphene oxide (GO) composites with 1 vol.% equimolar Y₂O₃–Sc₂O₃ sintering additives were sintered at 2000 °C in nitrogen atmosphere by rapid hot-pressing technique. The sintered composites were further annealed in gas pressure sintering (GPS) furnace at 1800 °C for 6 h in overpressure of nitrogen (3 MPa). The effects of types and amount of graphene, orientation of graphene sheets, as well as the influence of annealing on microstructure and functional properties of prepared composites were investigated. SiC-graphene composite materials exhibit anisotropic electrical as well as thermal conductivity due to the alignment of graphene platelets as a consequence of applied high uniaxial pressure (50 MPa) during sintering. The electrical conductivity of annealed sample with 10 wt.% of GNPs oriented parallel to the measuring direction increased significantly up to 118 S·cm⁻¹. Similarly, the thermal conductivity of composites was very sensitive to the orientation of GNPs. In direction perpendicular to the GNPs the thermal conductivity decreased with increasing amount of graphene from 180 W·m⁻¹ K⁻¹ to 70 W·m⁻¹ K⁻¹, mainly due to the scattering of phonons on the graphene – SiC interface. In parallel direction to GNPs the thermal conductivity varied from 130 W·m⁻¹ K⁻¹ up to 238 W·m⁻¹ K⁻¹ for composites with 1 wt.% of GO and 5 wt.% of GNPs after annealing. In this case both the microstructure and composition of SiC matrix and the good thermal conductivity of GNPs improved the thermal conductivity of composites.     

Microstructures and mechanical properties of high-entropy (Ti0.2Zr0.2Hf0.2Nb0.2Ta0.2)C ceramics with the addition of SiC secondary phase

The relationships between microstructures and mechanical properties especially strength and toughness of high-entropy carbide based ceramics are reported in this article. Dense (Ti_0.2Zr_0.2Hf_0.2Nb_0.2Ta_0.2)C (HEC) and its composite containing 20 vol.% SiC (HEC-20SiC) were prepared by spark plasma sintering. The addition of SiC phase enhanced the densification process, resulting in the promotion of the formation of the single-phase high-entropy carbide during sintering. The high-entropy carbide phase demonstrated a fast grain coarsening but SiC particles remarkably inhibited this phenomena. Dense HEC and HEC-20SiC ceramics sintered at 1900 °C exhibits four-point bending strength of 332 ± 24 MPa and 554 ± 73 MPa, and fracture toughness of 4.51 ± 0.61 MPa·m^1/2 and 5.24 ± 0.41 MPa·m^1/2, respectively. The main toughening mechanism is considered to be crack deflection by the SiC particles.     

Corrosion resistant ZrO2/SiC ultrafiltration membranes for wastewater treatment and operation in harsh environments

This work focused on the fabrication of a ZrO₂/SiC ultrafiltration membrane by dip coating a high porous SiC support with a ZrO₂ slurry prepared by ceramic processing. The membranes were sintered in different temperatures (1000−1300 °C). With the optimal temperature, it was obtained a mechanically strong, homogenous, and defect free separation layer with 45 μm of thickness and average pore size of 60 nm. A pure water permeability of 360 L.m⁻² h⁻¹ bar^-1 and high retentions of humic acid, indigo dye, and hemoglobin were observed. In a pilot test with an olive oil/water emulsion, 99.91 % of oil was removed without fouling. Long-term corrosion tests at basic and acid baths did not cause change in pore size and morphology. In conclusion, the ZrO₂/SiC membrane has potential to operate in harsh conditions (e.g. heavily contaminated industrial effluents or urban wastewaters) and when severe membrane cleaning and disinfection are required, such as food and pharmaceutical industries.     

Strong and tough laminated ceramics prepared from ceramic foams

Here, we present a novel strategy to prepare laminated ceramics by combining the ceramic foams and hot-pressing sintering. Al₂O₃ and ZrO₂ ceramic foams prepared by the particle-stabilized foaming method was cut into thin slices and then directly laminated and hot-pressing sintered. Al₂O₃/ZrO₂ laminated ceramics with various structures were prepared. Compared with the slices prepared by conventional process, ceramic foams can easily regulate the thickness of laminate to resemble the nacre-like structure. In addition, the grain in the ceramic foams have lower activity and shrinkage rate, thereby weakening the residual tensile internal stress caused by grain coarsening and differences in coefficient of thermal expansion. The effects of layer number and thickness ratio on residual stress and the structure-activity relationship between mechanical properties and microstructure were investigated. The fracture toughness, flexural strength, and work of fracture of the optimal Al₂O₃/ZrO₂ laminated ceramics are 8.2 ± 1.3 MPa·m^1/2, 356 ± 59 MPa, and 216 J·m^?2, respectively.     

高温除尘碳化硅膜的制备及其抗腐蚀特性

采用喷涂法在碳化硅（SiC）支撑体上覆膜,根据碳化硅材料的氧化特性,设计了有氧烧结和氩气烧结随温度转换的组合烧结制度,并通过优化保温时间降低碳化硅陶瓷膜烧结成本。研究结果表明,新的烧结制度能有效地控制有氧烧结阶段产生的二氧化硅（SiO₂）量,并促进其与烧结助剂氧化锆（ZrO₂）等在气氛烧结阶段的反应,反应生成的锆英石相和添加莫来石相共同形成SiC颗粒连接颈部。制备的碳化硅陶瓷膜平均孔径为3.03 μm,气体通量为175 m³?m^-2?h^-1?kPa^-1。且在100℃的0.25 mol?L^-1的H₂SO₄溶液和0.25 mol?L^-1的NaOH溶液中腐蚀6 h后,膜层表面形貌无明显变化,具有较强的抗腐蚀性能。     

AlN-Re2O3液相烧结碳化硅

采用非氧化物AlN和Re2O3作为复合烧结助剂(Re2O3-La2O3与Y2O3)进行碳化硅液相烧结得到了致密的烧结体.烧结助剂占原料粉体总质量的20%,其中:AIN与(La0.5Y0.5)2O3的摩尔比为2:1,在30MPa压力下,1850℃保温0.5h热压烧结的碳化硅陶瓷,抗弯强度>800MPa,断裂韧性>8MPa·m1/2,明显高于同组分1 950℃无压烧结0.5h的碳化硅陶瓷的抗弯强度(433.7MPa)和断裂韧性(4.8MPam·m1/2.热压烧结的陶瓷晶粒呈单向生长,断裂模式为沿晶断裂.同组分无压烧结碳化硅陶瓷的显微结构可以观察到核壳结构.     

Combined role of SiC particles and SiC whiskers on the characteristics of spark plasma sintered ZrB2 ceramics

In this research work, the effects of silicon carbide (SiC) as the most important reinforcement phase on the densification percentage and mechanical characteristics of zirconium diboride (ZrB₂)-matrix composites were studied. In this way, a monolithic ZrB₂ ceramic (as the baseline) and three ZrB₂ matrix specimens each of which contains 25 vol% SiC as reinforcement in various morphologies (SiC particulates, SiC whiskers, and a mixture of SiC particulates/SiC whiskers), have been processed through spark plasma sintering (SPS) technology. The sintering parameters were 1900 °C as sintering temperature, 7 min as the dwell time, and 40 MPa as external pressure in vacuum conditions. After spark plasma sintering, a relative density of ~96% was obtained (using the Archimedes principles and mixture rule for evaluation of relative density) for the unreinforced ZrB₂ specimen, but the porosity of composites containing SiC approached zero. Also, the assessment of sintered materials mechanical properties has shown that the existence of silicon carbide in ZrB₂ matrix ceramics results in fracture toughness and microhardness improvement, compared to those measured for the monolithic one. The simultaneous addition of silicon carbide particulates (SiC_p) and whiskers (SiC_w) showed a synergistic effect on the enhancement of mechanical performance of ZrB₂-based composites.     

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.     

Ablation behavior of C/SiC with YSZ and ZrB2 coatings under high-energy laser irradiation

Carbon fiber-reinforced silicon carbide (C/SiC) composites are important candidates for laser protection materials. In this study, ablation mechanism of C/SiC coated with ZrO₂/Mo and ZrB₂–SiC/ZrO₂/Mo under laser irradiation was studied. ZrB₂–SiC multiphase ceramic and ZrO₂ ceramic were successfully coated on C/SiC composite by atmospheric plasma spraying technology with Mo as transition layer. Phase evolution and morphology of composite were investigated by X-ray diffraction, scanning electron microscopy, and transmission electron microscopy. Moreover, ablation behavior of the composite was investigated by laser confocal microscopy. Results showed that ablation mechanism of C/SiC composite was controlled by phase transformation, thermal reaction, and thermal diffusion, with solid–liquid transition of ZrB₂ and ZrO₂ being dominant factor. Endothermic reaction and good thermal diffusivity of coatings were also important factors affecting ablation performance. Reflectivity effect of ZrO₂ coating was limited under high-energy laser irradiation. Compared with ZrO₂/Mo single-phase-monolayer coating, designed ZrB₂–SiC/ZrO₂/Mo coating showed better ablation performance, and breakdown time of C/SiC increased from 10 to 40 s. The depletion of liquid phase in molten pool was identified as an important factor responsible for rapid failure of C/SiC. The coating failed when the entire liquid phase was consumed within molten pool, followed by rapid damage of C/SiC substrate. Results of this study can provide theoretical guidance and research ideas for design and application of laser protective materials.     

Influence of Carbon Content on Ceramic Injection Molding of Reaction‐Bonded Silicon Carbide

Reaction‐bonded silicon carbide (RBSC) was prepared by ceramic injection molding (CIM) technique with feedstocks containing silicon carbide (SiC), a wax‐based organic system and different amounts of carbon black. As a critical effect of the reaction sintering process, carbon was introduced from the carbon black and the decomposition product of the organic polymers, respectively. This study described the influence of carbon content on the mixing and injection process firstly and then emphasized the debinding process since it played a large role in the process of the pyrolysis of organic. Results indicated that the preferable thermal debinding was performed in N₂ and the optimal performance was obtained for RBSC with 7 wt.% of carbon black, with the density of 2.98 g/cm³, apparent porosity of 0.24%, bending strength of 301.59 MPa and fracture toughness of 4.18 MPa·m^1/2.     

Organic-inorganic composites for novel optical transformation induced by high-energy laser ablation

High-energy continuous-wave (CW) laser has been considered as a significant technology in recent decades. Such laser can destroy conventional materials in an extremely short time, necessitating their protection. In this study, zirconium carbide (ZrC) and silicon carbide (SiC) particle-modified short silicon carbide fiber-reinforced phenolic resin matrix composites (SiC/BPF-ZS) with significant anti-laser performance were designed and prepared. Our results showed that the ceramic particles and SiC fibers rapidly oxidized, leading to the formation of a ceramic coating composed of ZrO₂ and SiO₂. Owing to the formation of the ceramic coating, the reflectivity of the composites improved significantly from 15.8% to 73.2% after ablation at 500 W/cm² for 30 s. Additionally, the SiC fibers played an important role in the formation of a high-reflectivity coating during laser ablation. Contrast experiments indicated that SiC fibers lead to better performance than the carbon fibers. The high reflectivity and low mass ablation rate are demonstrated to be the key factors improving the anti-laser ablation performance of the SiC/BPF-ZS composites.     

Oxidation and cracking/spallation resistance of ZrB2–SiC–TaSi2–Si coating on siliconized graphite at 1500 °C in air

A ZrB₂–SiC–TaSi₂–Si coating on siliconized graphite substrate was prepared by a combination process of slurry brushing and vapor silicon infiltration. The high-temperature oxidation behavior and cracking/spallation resistance of the as-prepared coating were investigated in detail. It was revealed that the oxidation kinetics at 1500 °C in static air followed a parabolic law with a relatively low oxidation rate constant down to 0.27 mg/(cm²·h^0.5). The crack area ratio of the as-prepared coating was determined as 3.8 × 10⁻³ after severe thermal cycling from 1500 °C to room temperature for 20 times. Apart from the formation of ZrO₂ as skeleton phase with SiO₂ as infilling species, the good oxidation and cracking/spallation resistance of the coating also could be attributed to its unique duplex-layered structure, i.e., a dense ZrB₂–SiC–TaSi₂ major layer filled with Si and an outermost Si cladding top layer. Meanwhile, the strong adhesion strength of the SiC transition layer with the graphite substrate and the outer ZrB₂–SiC–TaSi₂–Si layer was a vital factor as well.     

Fabrication and microstructure of Al2O3–ZrO2(3Y)–SiC nanocomposites

Al₂O₃–ZrO₂(3Y)–SiC composite powder was prepared by the heterogeneous precipitation method. Calcinating temperature of the powder was important to obtain dense sintered body. The nanocomposites were got by hot-pressing, and addition of ZrO₂ did not raise the sintering temperature. Some Al₂O₃ grain shape was elongated, and Al₂O₃ grain size was about μm. Nano SiC particles were observed uniformly distributing throughout the composites, and most of them were located within the matrix grains. Because SiC particles located within ZrO₂ grains influenced the phase transformation of ZrO₂, the sintering of nanocomposites, which controlled grain size and transformable ZrO₂ amount, become important to get high performance. The strength of 80 wt% Al₂O₃–15 wt% ZrO₂–5 wt% SiC nanocomposites was 555 MPa, and toughness was 3·8 MPa m^1/2, which were higher than those of monolithic Al₂O₃ ceramics. ©