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.     

Fabrication and mechanical properties of Al2O3–TiC ceramic composites synergistically reinforced with multi-walled carbon nanotubes and graphene nanoplates

In this study, Al₂O₃–TiC composites synergistically reinforced with multi-walled carbon nanotubes (MWCNTs) and graphene nanoplates (GNPs) were prepared via spark plasma sintering (SPS). The effects of the MWCNT and GNP contents on the phase composition, mechanical properties, fracture mode, and toughening mechanism of the composites were systematically investigated. The experimental results indicated that the composite grains became more refined with the addition of MWCNTs and GNPs. The nanocomposites presented high compactness and excellent mechanical properties. The composite with 0.8 wt% MWCNTs and 0.2 wt% GNPs presented the best properties of all analysed specimens, and its relative density, hardness, and fracture toughness were 97.3%, 18.38 ± 0.6 GPa, and 9.40 ± 1.6 MPa m^1/2, respectively. The crack deflection, bridging, branching, and drawing effects of MWCNTs and GNPs were the main toughening mechanisms of Al₂O₃–TiC composites synergistically reinforced with MWCNTs and GNPs.     

微波加热CO2活化法制备生物质活性炭及其脱硫性能研究

以富含含氮官能团的大豆秸秆为原料前体,结合微波加热的特殊优势,将微波加热技术应用于大豆秸秆热解和活化工艺。以热解固体产物为活化原料,以CO₂为活化剂进行活性炭制备研究,以期制备出高脱硫性能的生物质活性炭。首先通过正交实验设计及极差分析得出最优活化水平,再通过单因素实验法考察微波功率、CO₂流量和活化时间对活性炭产率、孔隙结构以及脱硫性能的影响。对比分析选出最佳活化条件为微波功率900 W,CO₂流量0.10 L/min,活化时间20 min。在此条件下活性炭产率为76.3%（质量）,SO₂饱和吸附容量为112.56 mg/g,比表面积为466.28 m²/g。相比热解炭,活性炭的比表面积更大,孔隙更加丰富,脱硫性能显著提高。     

Influence of processing conditions on the ionic conductivity of holmium zirconate (Ho2Zr2O7)

Nanopowders of holmium zirconate (Ho₂Zr₂O₇) synthesised through carbon neutral sol-gel method were pressed into pellets and individually sintered for 2 h in a single step sintering (SSS) process from 1100 °C to 1500 °C at 100 °C interval and in a two step sintering (TSS) process at (I) −1500 °C for 5 min followed by (II) - 1300 °C for 96 h. Relative density of each of the sintered pellet was determined using the Archimedes’ technique and the theoretical density was calculated from crystal structure data. Grain size was obtained from SEM micrographs using ImageJ. Pellets processed by TSS have been found to be denser (98 %) with less grain growth (1.29 μm) as compared to the pellets processed using SSS process. Ionic conductivity of Ho₂Zr₂O₇ pellets sintered by two different processes was measured using ac impedance spectroscopy technique over the temperature range of 350 °C–750 °C in the frequency range of 100 mHz–100 MHz for both heating and cooling cycles. The temperature dependence of bulk (2.67⨯10⁻³ Scm⁻¹) and grain boundary (2.50⨯10⁻³ Scm⁻¹) conductivities of Ho₂Zr₂O₇ prepared by TSS process are greater than those processed by SSS process suggesting the strong influence of processing conditions and grain size. Results of this study, indicates that the TSS is the preferable route for processing the holmium zirconate as it can be sintered to exceptionally high densities at lower temperature, exhibits less grain growth and enhanced ionic conductivity compared with the samples processed by SSS process. Hence, holmium zirconate can be considered as a promising new oxide ion conducting solid electrolyte for intermediate temperature SOFC applications between 350 °C and 750 °C temperature range.     

Crack tolerant silicon carbide ceramics prepared by liquid-phase assisted oscillatory pressure sintering

Silicon carbide ceramics were prepared by liquid-phase assisted oscillatory pressure sintering (OPS) with graphene and in-situ synthesized SiC whisker as the reinforcements. The effects of sintering temperature on the densification, morphology and mechanical performances of the SiC_p-SiC_w-graphene ceramics were investigated. In the temperature range from 1700 to 1800 °C, the densification rate of SiC_p-SiC_w-graphene ceramics was accelerated, ascribing to the reduction in viscosity of the glassy phase. At 1800 °C, the flexural strength and fracture toughness of the OPS ceramics corresponded to 697 MPa and 5.8 MPa m^1/2, respectively, which were higher than that of the hot-pressed ceramics under the same temperature conditions. Multiphase toughening mechanisms, such as whisker bridging and pullout, graphene bridging and delamination, were considered as the primary mechanisms. This work demonstrates an effective strategy to prepare silicon carbide ceramics at low sintering temperature.     

The effect of transition metal carbides MeC (Me = Ti,Zr, Nb,Ta, and W) on mechanical properties of B4C ceramics fabricated via pressureless sintering

In this study, boron carbide-metallic boride (B₄C-MeB_x, Me = Ti, Zr, Nb, Ta, or W) multiphase ceramics were fabricated via in situ pressureless sintering at 2250 °C for 1 h. The effects of transition metal carbides, namely, TiC, ZrC, NbC, TaC, and WC, on the phase composition, microstructure, and mechanical properties of the ceramics were investigated. The results showed that MeC could facilitate the sintering densification of B₄C by distributing second-phase particles uniformly throughout the B₄C. Additionally, the main phases observed were B₄C and (Me, W)B_x (Me = Ti, Zr, Nb, or Ta) due to the doping of a small amount of WC during the ball milling process. As a result, the mechanical properties of B₄C-MeB_x showed significant improvements when compared with those of single-phase B₄C ceramics. B₄C–NbB₂ ceramics were found to exhibit the best mechanical properties, with an elastic modulus of 393.0 GPa, a hardness of 28.7 GPa, a flexural strength of 368.0 MPa, and a fracture toughness of 6.94 MPa m^1/2.     

Grain size effect on microwave dielectric properties of Na2WO4 ceramics prepared by cold sintering process

In this work, cold sintering was adopted to prepare Na₂WO₄ ceramics with different grain sizes ranging from 0.632 μm to 17.825 μm. Their microstructures, complex impedance, and microwave dielectric properties were studied in-depth. It was found that samples with relative densities higher than 92% can be successfully synthesized by cold sintering process at a low temperature of 240 °C. However, their electrical properties have strong dependence on the grain size. Specifically, the resistance of grain boundaries decreases dramatically with the increase of grain sizes, while the quality factor has a positive correlation with the grain sizes of Na₂WO₄ ceramics. Excellent microwave dielectric properties, including permittivity = 5.80, Q × f = 22,000 GHz, and TCF = −70 ppm/°C, are obtained for Na₂WO₄ ceramics with a grain size of 4.477 μm prepared by cold sintering process.     

Effect of oscillatory pressure on the sintering behavior of ZrO2 ceramic

Zirconia ceramics were prepared by oscillatory pressure sintering (OPS) and hot pressing (HP). The result revealed that OPS could enhance densification compared to HP when sintering temperature was higher than a critical value. The onset temperature for rapid grain growth was found to be same for both techniques. However, rate of grain growth in OPS was lower than that in HP. Furthermore, the result also showed that samples prepared by OPS exhibited higher hardness than those prepared by HP when sintering temperature was higher than the critical value. The improved hardness was solely due to the higher density of the samples prepared by OPS.     

微波作用磷矿分解反应动力学研究

通过微波和加热作用下的磷矿分解反应动力学实验对照,探讨了微波场对磷矿分解过程的影响.     

微波辐射对木薯淀粉结构的影响

考察了不同含水量的木薯淀粉经不同形式（敞口和封口形式）微波辐射的温度变化曲线及其多层次结构.结果表明：无论以那种形式辐射,木薯淀粉样品含水量越低,样品温度升高幅度越大,且都会出现等温转换,含水量越高等温转换时间越长,敞口辐射较封口辐射的等温转换更显著; FTIR结果显示,微波辐射不破坏木薯淀粉分子的化学键,没有新的化合物产生,红外结晶指数略有降低;偏光显微镜和光学显微镜的结果显示,木薯淀粉的结晶结构有所变化,而其形态结构没有变化.这些结果表明,经微波加工的木薯淀粉食品对人或其他生物是安全的.