Preparation and Mechanical Properties of SiC Whisker and Nanosized Mullite Particulate Reinforced TZP Composites

The influence of the addition of nanometer mullite particulates and SiC whiskers coated with alumina on the mechanical properties of tetragonal zirconia polycrystals (TZP) was studied. With increasing mullite( p ) content the high-temperature flexural strength increased, and a maximum value of 360 MPa at 1000°C was reached at 15 vol% mullite( p . Furthermore, 10 vol% SiC( w ) reinforced 15 vol% mullite/TZP composites improved the high-temperature strength up to 490 MPa at 1000°C, 2.7 times that of pure TZP matrix. This high-temperature strengthening is attributed to load transfer from TZP matrix to SiC( w ) and mullite particulates. Significant whisker pull-out and interface debonding were also observed on the fractured surfaces when SiC( w ) was coated with Al₂O₃ film.     

Thermal Cyclic Fatigue Behavior of Porous Ceramics for Gas Cleaning

The thermal shock fatigue resistance of cordierite and SiC filters with a mullite filtration layer was evaluated under simulated reverse cleaning conditions. O-ring specimens were thermally shocked by cyclically blowing cold air outward through them while they were exposed to high-temperature flue gas. The calculated values of the tangential tensile stresses induced by the temperature differences between the inner and outer surfaces were found to be largest at the inner surfaces. It was also found that the elastic modulus and the thermal expansion coefficient of the filters affect the magnitude of the thermal stresses more than the thermal diffusivity and thermal transfer area, which were directly related to the microstructure of the filters. Failure of both filters is believed to have initiated at the inner subsurfaces because of the effects of thermal shock. The thermal shock fatigue lifetimes increased as thermal stresses decreased. The fatigue parameters for the SiC and cordierite filters were found to be 41 and 22, respectively. These parameters probably vary over different operating temperature ranges, especially in the case of SiC filters, where changes in their composite microstructures affect their high-temperature strength.     

Mullite Whiskers Grown from Erbia-Doped Aluminum Hydroxide–Silica Gel

Mullite whiskers and anisotropic grains that were derived from erbia-doped aluminum hydroxide–silica gel were studied. Firing 3.0-mol%-erbia-doped isostatically pressed pellets at 1600°C for 1.0–8.0 h resulted in a high surface concentration of mullite whiskers. Their c -axes were aligned preferentially along the pellet surface; the maximum length was 50 μm, and the maximum aspect ratio was 23. The pellet surface was fully covered by mullite whiskers, and small anisotropic grains with a low aspect ratio were observed in the bulk. The voids that were observed in the fracture surfaces were covered fully by mullite whiskers. The large number of voids resulted in an apparent density of 1.60 g/cm³ in the sintered pellets. The molar ratio of alumina to silica in the whiskers was in the range of 1.30–1.45 (an average value of 1.31), regardless of whether the alumina/silica powder compositions were mixed in a 3:2 or 2:1 ratio.     

Preparation and properties of hierarchical structural alumina/mullite composites

Hierarchical structural alumina/mullite composites constructed by alumina platelets inter-locked porous matrices and mullite whiskers secondary structures had been designed and prepared based on the fluorine-catalyzed gas-phase process. In the composites, mullite whiskers grew on the alumina platelets of the matrices to form cactus-like structures, before that, topaz rods as transitional secondary structures formed at lower temperature. The fluorine-etching effects on secondary structures’ nucleation were discussed. The alumina/mullite composites (1300 °C) had low bulk density (1.10 g/cm³), high porosity (71.4%), and proper compression strength (～14.2 MPa), meanwhile, the average filtration efficiencies of PM2.5 and PM10 during the filtration tests were 78% and 76%, respectively. The introduced mullite whiskers with length of ～1 µm had not induced obvious changes on the structural parameters, hence, the alumina/mullite composites (1300 °C) possessed similar particle filtration performances compared with the alumina porous matrices, and both of the two species materials could be applied for hot gas filtration.     

静电纺丝纤维滤材表征及其气液过滤性能

以聚丙烯腈与二甲基甲酰胺为原料配制纺丝溶液,采用静电纺丝技术制备玻璃纤维/聚丙烯腈纤维/玻璃纤维三层复合滤材,研究了纺丝溶液浓度与纺丝电压等参数对纤维形貌及尺寸的影响,分析了复合滤材的过滤性能. 结果表明,控制不同纺丝溶液浓度可得形貌不同的纤维,且溶液浓度越大纤维尺寸越大;纺丝电压对纤维形貌的影响较小,但增加纺丝电压使静电纺纤维层的孔径减小. 相比玻璃纤维滤材,复合滤材过滤效率明显提升,稳态效率最大可提升21%,最易穿透粒径效率最大可提升39%,但复合滤材孔径较小时,过程压降增加了一段跳跃阶段,纳米纤维层表面形成液膜,使复合滤材稳态压降升高.     

Performance of fibrous filters during nanoparticle cake formation

Fibrous filters are highly efficient in removing micrometer particles, but their performance in the nanometer particle range is still little known. The aim of this study was to evaluate pressure drop and collection efficiency during nanoparticles cake formation using commercial fibrous filters. The filter media used were High Efficiency Particulate Air (HEPA) and polyester filters. The aerosols were generated by a commercial inhaler using a 5 g/L solution of NaCl and the particles produced were in the size range from 6 to 800 nm, with a peak at around 40 nm. A superficial velocity (v_s) of 0.06 m/s was employed. During the filtration, the maximum pressure drop established was ?P ₌ ?P_f +980Pa, where ?P_f is the initial pressure drop of the filter. The collection efficiency was determined for a clean filter and for intermediate pressure drops. The filtration curves obtained showed that the HEPA filter provided greater surface filtration, compared to the polyester filter. Comparison of the collection efficiencies for clean filters revealed that the HEPA filter was highly efficient, even in the absence of cake, while the polyester filter showed initial collection efficiencies of between 20 and 40% for particles in the size range from 100 nm to 1000 nm. However, after formation of the filter cake, the collection efficiencies of both filters were almost 100% during the final stage of filtration. This shows that the fibrous filter can be applied in several industrial processes with highly efficient nanoparticle separation, after the formation of a thin layer cake filtration.     

Development and evaluation of multilayer air filter media

Three types of multilayer air filter media were developed and evaluated. Two other existing filters were also used for comparison of filter performance. The pressure drop, the collection efficiency, and the dust-holding capacity of the tested filters were measured, and the internal structure of the filter media was analyzed by using a scanning electron microscope. The multilayer filters tested in this study are composed of pre-surface layer, surface layer, and substrate layer. Among those layers, the surface layer is mainly responsible for particle collection. As a test result, it was found that the thickness of a surface layer has the greatest effect on filtration performance of a multilayer air filter. Additionally, filtration velocity and electrostatic forces should be considered together as important parameters for multilayer air filter design.     

Application of nanofibers to improve the filtration efficiency of the most penetrating aerosol particles in fibrous filters

Conventional, mechanical fibrous filters made of microfibers exhibit a local minimum of fractional collection efficiency in the aerosol particle size-range between 100 and 500 nm, which is called the most penetrating particle size (MPPS). Simple theoretical calculations predict that this efficiency may be significantly increased using nanofibrous media. The main objective of this paper is an experimental verification of these expectations and simultaneously checking whether this anticipated gain in the filtration efficiency is not overpaid with an excessive pressure drop. For this purpose we developed a modified melt-blown technology, which allowed us to produce filters composed of micrometer as well as nanometer sized fibers. One conventional microfibrous filter and five nanofibrous filters were examined. The complete structural characteristics, pressure drop and efficiency of removal of aerosol particles with diameters 10-500 nm were determined for all media. The results of the experiments confirmed that using nanofibrous filters a significant growth of filtration efficiency for the MPPS range can be achieved and the pressure drop rises moderately. Simultaneously, we noticed a shift of the MPPS towards smaller particles. Consequently, the quality factor for bilayer systems composed of a microfibrous support and a nanofibrous facial layer was considerably higher than this one for a conventional microfibrous filter alone. Additionally, it was found that utilization of many-layer nanofibrous filters combined with a single microfibrous backing layer is even more profitable from the quality factor standpoint. Comparing experimental results with theoretical calculations based on the single-fiber theory we concluded that for microfibrous filters a fairly good agreement can be obtained if the resistance-equivalent fiber diameter is used in calculations instead of the mean count diameter determined from the SEM images analysis; in the latter case, filtration efficiency computed theoretically is slightly overestimated. This is even more evident for nanofibrous media, suggesting that in such case a structural filter inhomogeneity has a strong influence on the filter efficiency and its resistance and one should strive for minimization of this effect manufacturing nanofibrous filters as homogeneous as possible. We can finally conclude that fibrous filters containing nanofibers, which are produced using the melt-blown technique, are very promising and economic tools to enhance filtration of the most penetrating aerosol particles.     

Aligned carbon nanotube sheet high efficiency particulate air filters

Aerosol filters, made with conventional micro-fiber fabrics, are designed to efficiently capture small particles from the air. Filters constructed of nano-fiber fabric structures provide even greater filtration efficiency than conventional micro-fiber fabrics due to their higher surface area and smaller pore size. Carbon nanotubes (CNTs) are very small diameter fibers that have the potential to be integrated into filters to further increase particle capture efficiency. In this study, CNT sheets, drawn from millimeter tall CNT arrays, were integrated between traditional micro-fiber fabrics to produce aerosol filters. The filtration performance of the novel filters showed that when the number of CNTs layers increased, the filtration efficiency increased dramatically, while the pressure drop also increased. In order to meet high efficiency particulate air (HEPA) filter requirements with a reasonable pressure drop, CNTs were laid in a cross-plied structure within the filter. The results demonstrated that the three layer cross-ply structure provided 99.98% filtration efficiency at 0.3 μm particle size at a 10 cm/s face velocity, making it a viable method for producing low basis weight HEPA filters utilizing CNTs as the main filtration component.     

Microscopic Mechanisms of Oxidation in SiC-Whisker-Reinforced Mullite/ZrO2 Matrix Composites

The oxidation of SiC whiskers, contained in alkoxide-derived mullite-based matrices and exposed in air at 1000–1350°C for up to 1000 h, has been studied by analytical TEM, high-resolution SEM, and XRD. Silicon carbide whiskers were effectively protected from oxidation when embedded in a pure mullite matrix, but oxidized considerably when embedded in mullite/ZrO₂ matrices. The oxidation mechanisms varied with matrix composition and exposure temperature. At 1350°C the amorphous layer first crystallized as cristobalite, then gradually incorporated alumina. At later times, the mullite portion of the mullite/ZrO₂ matrix dissolved extensively into the layer. Also, the zirconia particles reacted with silica to form zircon. At 1200°C less extensive interdiffusion and chemical reaction occurred, and the silica layer devitrified into cristobalite and quartz. At 1000°C no interdiffusion or chemical reaction was seen, and the silica layer tended to devitrify into quartz. The thickness of the oxide layer around a SiC whisker in a particular matrix depended on the morphology and composition of grains abutting it or adjacent to it.     

Colloidal Processing and Mechanical Properties of Whisker-Reinforced Mullite Matrix Composites

Aqueous colloidal suspensions in the two systems of CVD-processed ultrafine mullite powder (<0.1 μm), -Si₃N₄ whisker and -mullite whisker, were prepared near the isoelectric point of mullite (pH 7.0) to prevent cracking during drying of wet green compacts consolidated by filtration. The freeze-dried porous green compacts were hot-pressed with a carbon die at 1500°C for 1 h at a pressure of 39 MPa in N₂ atmosphere. The relative densities of the mullite matrix composites with whiskers of 0 to 10 vol% were in the range of 95.2% to 99.8%. Increasing the fraction of Si₃N₄ whisker increased the density, flexural strength, and fracture toughness of the hot-pressed composites. On the other hand, addition of the mullite whisker increased the fracture toughness but decreased the density and strength of the composites.     

Filtration Efficiency and Pressure Drop of Miniature Diesel Particulate Filters

A method was developed to evaluate miniature diesel particulate filters (DPFs). To validate the performance of the instrumentation and test apparatus, measurements were made using silicon carbide (SiC) and cordierite miniature filters with representative microstructures. Filtration efficiency (FE), the most penetrating particle size (MPPS), and pressure drop were measured for catalyzed and uncatalyzed advanced ceramic material (ACM) acicular mullite and representative commercial filters to determine the impact of substrate morphology, the formation of a soot cake, and the presence of a catalyst coating on filtration properties. FE measurements demonstrated that filter geometry and microstructure significantly influence initial filtration performance. ACM filters had high initial FE and the MPPS near ～200 nm. Reduction of the ACM pore size in the absence of a reduction in porosity increased initial FE even more, but its influence on MPPS was not resolvable. The presence of a catalyst and washcoat on the ACM increased the pressure drop but increased initial FE and reduced MPPS to <100 nm. The addition of a washcoat allowed the rapid buildup of a soot cake, which resulted in a more rapid rate of increase in FE compared to uncatalyzed ACM. The similarity in the ACM and cordierite soot cakes after a long loading time is consistent with theory that suggests the formation of the soot cake depends primarily on the Péclet (Pe) number, which is influenced only by macroscopic filter geometry and prevailing test conditions.

Copyright 2013 American Association for Aerosol Research     

聚结层排布对高压天然气净化用滤芯过滤性能影响的实验研究

本工作利用聚结滤芯过滤性能实验装置,通过改变滤芯内部的滤材排布,研究了聚结层为单一滤材以及由不同滤材排布组合的滤芯过滤性能,分析了聚结层排布方式对过滤效率、压降、饱和度及液体分布的影响。结果表明,由单一滤材组成的滤芯过滤效率随滤材孔径减小而增大,但孔径最小时由于压降较高,导致滤芯综合过滤性能反而最差。疏油在前、亲油在后的聚结层排布方式可提高滤芯过滤效率、减少液滴二次夹带,且以两层相同滤材交错排列的滤芯过滤效率比单层滤材交错排列明显更高,压降也相对较低,使得综合过滤性能显著提升。继续增加进气侧的疏油滤材层数可延缓压降增长、提高运行寿命,滤芯稳态品质因子达到最大值(0.30 kPa-1)。聚结层排布方式对滤芯过滤性能的影响主要通过改变液体分布形式而实现,且末层滤材的通道结构变化是导致不同聚结层排布方式的滤芯过滤性能出现差异的主要原因。     

SiC_w/莫来石和SiC_w/Y-TZP/莫来石复合材料的力学性能与显微结构

以莫来石为基体,SiC晶须(SiC_w)和Y-TZP(Y_2O_3稳定的四方ZrO_2多晶)为两种补强剂,采用热压烧结工艺,制备SIC_w/莫来石和SIC_w/Y-TZP/英来石复合材料。研究了复合材料的力学性能与显微结构,并对强化增韧机制进行了分析。结果表明,SiC晶须补强莫来石,可以改善其强度和断裂韧性。若SiC晶须和Y-TZP共同补强英来石,则可以进一步提高其强度和断裂韧性。晶须引起裂纹偏转,晶须拔出以及由ZrO_2相变引起的微裂纹增韧是该复合材料的主要增韧机制。SiC晶须和Y-TZP两种补强剂的共同作用,对莫来石强度和断裂韧性的提高具有叠加或协同效应。     

Preparation and characterization of diesel particle filter (DPF) with hierarchical microstructure for catalytic combustion of soot

Mullite whiskers were prepared on the wall of cordierite honeycomb ceramics using the gas-phase growth method. Subsequently, Co/Ce_0.75Zr_0.25O₂ catalyst was loaded on the mullite whiskers to form hierarchical microstructure by the sol-gel technology for catalytic combustion of soot. Scanning electron microscopy, energy dispersive X-ray spectroscopy, Fourier transform-infrared spectroscopy, X-ray diffraction and Transmission electron microscopy were used to characterize the structural morphology and phase compositions. The filtration capability can be improved by mullite whiskers growth on the wall of cordierite honeycomb ceramics, and the microstructural feature is similar to the pseudostratified ciliated epithelium on the tracheal cavity surface (one section of human respiratory system). The Co/Ce_0.75Zr_0.25O₂ catalyst decreased the ignition temperature of soot particles oxidation, and the cycle stability experiment confirmed that Co/CZ@M/C sample has good structural stability and stable catalytic performance. The high-efficiency filtration and the low-temperature catalytic oxidation of soot particles are combined with the hierarchical microstructure of Co/CZ@M/C, which has potential application in the diesel particulate filter (DPF) field.     

Effect of SiC nanoparticles on in-situ synthesis of SiC whiskers in corundum–mullite–SiC composites obtained by carbothermal reduction

Corundum–mullite–SiC composites were synthesised using a carbothermal reduction method. The effects of SiC nanoparticles and sintering temperatures on the phase transformation of the composites and the synthesis of SiC whiskers were studied by X-ray diffraction, scanning electron microscopy, and transmission electron microscopy. Results indicated that corundum, mullite, and SiC whiskers were produced as final products at 1600–1650 °C. SiC whiskers were formed through the vapor–solid mechanism. The added SiC nanoparticles worked as nucleating agents to facilitate the carbothermal reduction of aluminosilicates and formation of SiC whiskers. The sample with the added SiC nanoparticles exhibited a high yield of β-SiC of 17.1%. Furthermore, the SiC nanoparticles decreased the formation temperature of SiC whiskers from the original 1600 °C to 1500 °C, and the porosity of the composites was increased from 56.7% to 64.7% by increasing the partial pressure of SiO gas. This study provides an insight into the more efficient synthesis of composites with SiC whiskers through the carbothermal reduction of aluminosilicates.     

Fibrous ceramic membrane constructed by mullite whiskers for the treatment of oil-in-water emulsions

Ceramic membranes with high porosity and excellent separation efficiency are necessary for the efficient treatment of large-scale wastewaters. However, the conventional ceramic membranes are usually prepared by particles-packing, which inhibits the advances of separation efficiency because of the low porosity and connectivity. Here, a fibrous ceramic membrane with mullite whiskers-interlocked structure was prepared by gas-solid reaction. The effects of aluminum fluoride (AlF₃) on the formation and growth of mullite whiskers, and then the permeability and selectivity of the ceramic membranes were investigated. With the increase of AlF₃ contents, the mullite phase evolved from needle-like, rod-like to flake-like structure, thus the catalyst accelerated the growth of mullite whiskers in the diameter direction. For the ceramic membrane sintered at 1400°C, the porosity increased from 58% to 76% while the average pore sizes increased from 0.65 to 3.93 μm because of the whisker-constructed structures. For the ceramic membrane sintered at 1450°C, the emulsion flux increased stably from 295 L/(m²·h) to 992 L/(m²·h) with the increase of trans-membrane pressure, and the oil rejection exceeded 98%. Thus, this study provides a feasible strategy for the preparation of ceramic membranes with high porosity and excellent separation performances.     

CVD Mullite Coatings in High-Temperature, High-Pressure Air–H2O

Crystalline mullite was deposited by chemical vapor deposition (CVD) onto SiC/SiC composites overlaid with CVD SiC. Specimens were exposed to isothermal oxidation tests in high-pressure air + H₂O at 1200°C. Unprotected CVD SiC formed silica scales with a dense amorphous inner layer and a thick, porous, outer layer of cristobalite. Thin coatings (∼2 μm) of dense CVD mullite effectively suppressed the rapid oxidation of CVD SiC. No microstructural evidence of mullite volatility was observed under these temperature, pressure, and low-flow-rate conditions. Results of this preliminary study indicate that dense, crystalline, high-purity CVD mullite is stable and protective in low-velocity, high-pressure, moisture-containing environments.     

莫来石晶须的生长机理研究

本研究采用湿化学法制备莫来石晶须，主要讨论了晶须生长机理。研究结果表明，高温下产生的AIF3和SIF4气相在莫来石晶核表面通过气—固化学反应形成高长径比莫来石晶须。     

金属丝网过滤器性能影响因素研究

对金属丝网过滤器性能的影响因素进行了综合分析,为过滤器的良好运行提供建议。在分析过滤机理的基础上,从过滤效率、压降、残余压降三个方面,分析了过滤器性能的影响因素,包括丝网结构、循环次数、过滤速度、流体浓度及温度、颗粒粒径、滤饼的可压缩性、最大允许压降、反吹压力等。结果表明,各因素之间互相影响,实际过滤过程中须综合考虑,以达到过滤器的预期性能。