制备工艺对多孔碳化硅材料性能的影响

研究了骨料粒径、添加剂种类、质量分数对陶瓷管性能的影响。采用自制装置分别测定了孔径分布、平均孔径、孔隙率和气体通量。用SEM观察其表面形貌。结果表明,使用较细的碳化硅颗粒,气体通量减小,抗弯强度增加;随着造孔剂质量分数的变化,多孔碳化硅陶瓷管的性能也有明显的不同,最佳添加量为10%左右。增加烧结结合剂的加入量,气体通量和抗弯强度均下降。     

Synthesis of hierarchically porous mullite ceramics with improved thermal insulation via foam-gelcasting combined with pore former addition

ABSTRACT

To further improve the thermal insulation performance of porous mullite ceramics used in important industrial sectors, a combined foam-gelcasting and pore-former addition approach was investigated in this work, by which hierarchical porous mullite ceramics with excellent properties, in particular, thermal insulation property, were prepared. Both mesopores (2–50?nm) and macropores (117.8–202.7?μm) were formed in porous mullite ceramics resultant from 2?h firing at 1300°C with various amounts of submicron-sized CaCO₃ pore former. The former mainly arose from the decomposition of CaCO₃, and the latter from the foam-gelcasting process. The porous samples prepared with CaCO₃ addition had low linear shrinkage of 2.35–4.83%, high porosity of 72.98–79.07% and high compressive strength of 5.52–14.82?MPa. Most importantly, they also exhibited a very low thermal-conductivity, e.g. 0.114?W?m^?1?K^?1 at 200°C, which was much lower than in the cases of their counterparts prepared via the conventional foam-gelcasting route.     

A novel and green preparation of porous forsterite ceramics with excellent thermal isolation properties

This work provides a novel and green approach to preparing porous forsterite ceramics by a transient liquid phase diffusion process based on fused magnesia and quartz powders without detrimental additives. The size of quartz particles markedly affected the sintering behaviors, phase composition, microstructure and properties of the porous forsterite ceramics. Fine quartz particles (D₅₀, 3.87?µm) accelerated the rate of the forsterite formation at elevated temperatures and promoted solid-state sintering behavior of the porous ceramics. Conversely, coarse quartz particles (D₅₀, 25.38?µm) reduced the rate of the solid state reaction and a large amount of unreacted SiO₂ and enstatite (MgSiO₃) phases transformed into a transient liquid-phase during the firing process. This effect resulted in a high porosity (approximately 58.89%) and formation of many large pores (mean pore size of 42.36?µm). These features contributed to the excellent thermal isolation properties of the prepared porous forsterite ceramics. The strength of the obtained porous ceramics (about 23.6?MPa) is relatively high compared with those of conventional ceramics.     

Synthesis of Highly Porous Yttria-Stabilized Zirconia by Tape-Casting Methods

Porous ceramics of Y₂O₃-stabilized ZrO₂ (YSZ) were prepared by tape-casting methods using both pyrolyzable pore formers and NiO followed by acid leaching. The porosity of YSZ wafers increased in a regular manner with the mass of graphite or polymethyl methacrylate (PMMA) to between 60% and 75% porosity. SEM indicated that the shape of the pores in the final ceramic was related to the shape of the pore formers, so that the pore size and microstructure of YSZ wafers could be controlled by the choice of pore former. Dilatometry measurements showed that measurable shrinkage started at 1300 K, and a total shrinkage of 26% was observed, independent of the amount or type of pore former used. Temperature-programmed oxidation (TPO) measurements on the green tapes demonstrated that the binders and dispersants were combusted between 550 and 750 K, that PMMA decomposed to methyl methacrylate between 500 and 700 K, and that graphite combusted above 900 K. The porosity of YSZ ceramics prepared by acid leaching of nickel from NiO–YSZ, with 50 wt% NiO, was studied as a function of NiO and YSZ particle size. Significant changes in pore dimension were found when NiO particle size was changed.     

Fabrication and characterisation of cellular alumina articles produced via radiation curable dispersions

A general and versatile method for the production of cellular materials from radiation curable solvent-free colloidal ceramic dispersions containing pore formers has been developed. By this technique cellular ceramic articles with a precisely controlled porosity, cell size and shape are obtained for compositions containing solid pore formers. Monolithic bulk samples are obtained by thermal curing, whereas thin films and multi-layered articles are advantageously produced by UV curing. In this work the influence of three different spherical pore former types, PE, PS and PMMA, on the processing and final properties of the porous materials using alumina as model material is studied. The effect of pore former type and concentration on rheology, curing behaviour, debinding and sintering steps as well as thermal conductivity and mechanical strength of the sintered cellular materials is presented. It is also shown that the choice of pore former type modifies the sintering behaviour and resulting properties.     

Gas permeability and mechanical properties of porous alumina ceramics with unidirectionally aligned pores

Porous alumina ceramics having unidirectionally aligned cylindrical pores were prepared by extrusion method and compared with porous ceramics having randomly distributed pores prepared by conventional method, and their gas permeability and mechanical properties were investigated. SEM micrographs of the porous alumina ceramics prepared by the extrusion method using nylon fibers as the pore former showed excellent orientation of cylindrical pores. The bending strength and Weibull modulus of the extruded porous alumina ceramics with 39% porosity were 156 MPa and 17, respectively. These mechanical properties of extruded samples were higher than those of the conventional porous alumina ceramics. The strength decreased from 156 to 106 MPa with increasing pore size from 8.5 to 38 μm. The gas permeability of the extrusion samples is higher than that of the conventional samples and increased with increasing of porosity and pore size.     

Development and mechanical characterization of novel ceramic foams fabricated by gel-casting

Porous ceramic materials are of considerable interest for a variety of chemical and industrial applications in extremely harsh conditions, particularly at very high temperatures for long time periods. A combined gel-casting-fugitive phase process employing agar as a natural gelling agent and polyethylene spheres as pore formers was exploited to produce porous ceramic bodies. Alumina and alumina–zirconia powders were used to prepare samples having a porosity of about 65–70–75 vol%. The composite powder was produced by a surface modification route, i.e. by coating a well-dispersed alpha-alumina powder with a zirconium chloride aqueous solution. On thermal treatment, ultra-fine tetragonal zirconia grains were formed on the surface of the alumina particles. SEM observations and image analysis were used to characterize the microstructure of porous samples and uniaxial compressive tests were carried out to measure their mechanical behavior.     

Surface properties of porous carbons obtained from polystyrene-based polymers within inorganic templates: role of polymer chemistry and inorganic template pore structure

Three inorganic adsorbents were applied as templates to produce porous carbons from polystyrene-based organic polymers. As matrices, amorphous silica gel, mesoporous alumina and microporous zeolite 13X were used. Organic precursors were polystyrene sulfonic acid (co-maleic acid) sodium salt and polystyrene co-maleic acid isobutyl/methyl mixed ester. The impregnated templates were carbonized at 800 °C. After removal of inorganic matrices porous carbons were obtained. Materials were characterized by adsorption of nitrogen, thermal analysis, potentiometric titration and SEM. Owing to the template carbonization, highly mesoporous carbons were obtained (S_BET up to 1500 m²/g, V_t up to 3 cm³/g) with majority of pores with sizes between 20–200 Å. Although the carbons were not replicas of their matrices, the carbonization within the confined space with utilization of self-released pore formers resulted in unique carbonaceous materials with very acidic surface. That acidity is linked to either exothermic effect of sodium reactivity with moist air or susceptibility for air oxidation of small graphene layers formed in the confined pore space.     

Sintering behaviors and properties of porous ceramics derived from artificially cultured diatom frustules

Bimodal porous ceramics with high strength have been fabricated by conventional powder metallurgy utilizing artificially cultured diatom frustules (DFs). The effect of sintering temperature on thermal behaviors, phase transition, and pore structures features of DFs-based porous ceramics is investigated between 800 and 1200°C. The phase evolution of DFs powders is investigated with thermal analysis (DIL and DSC-TG). Phase transition behaviors analyzed with XRD, Raman, and FT-IR spectra confirm the transformation of quartz into cristobalite phases occurs under 1050°C. Sintering under 950°C could bind DFs powders tightly into high strength porous ceramics while maintain the multilayer pore structures simultaneously, having porosity of 56.4%, compressive strength of 15.0 MPa and surface area of 50.9 m²/g, respectively. Slit-shaped microstructures and mesopores (2-50 nm) are observed in DFs-based porous ceramics sintered under 1050°C. Collapse and blockage of pore structures as well as partial fusion of DFs particles happened at the temperature of 1100°C, indicating the presence of diminished multilayers and particle agglomeration.     

Preparation and characterization of porous alumina ceramics through starch consolidation casting technique

This work aims at studying the influence of thermal treatment on the microstructure, resistivity and technological properties of porous alumina ceramics prepared via starch consolidation casting (SCC) technique. Colloidal suspensions were prepared with three different contents of alumina solid loading (55, 60 and 65 mass%) and corn starch (3, 8 and 13 mass%). The sintered samples at 1400, 1500, 1600 and 1700 °C, show open porosity between 46 and 64%, depending on the starch content in the precursor suspensions and sintering temperature. The pore structures were analyzed by SEM. The effect of corn starch content on the apparent porosity, pore size distribution, linear shrinkage and electrical resistivity as well as cold crushing strength of the sintered porous alumina ceramics was also measured. These porous alumina ceramics are promising porous ceramic materials for using in a wide range of thermal, electrical and bioceramics applications as well as filters/membranes and gas burners, due to their excellent combination properties.     

Effects of pore shape and porosity on the properties of porous PZT 95/5 ceramics

Porous lead zirconate titanate (PZT 95/5) ferroelectric ceramics were prepared by sintering compacts consisting of PZT and pore formers. The piezoelectric, dielectric and ferroelectric properties of porous PZT ceramics were investigated as a function of pore shape and porosity. Piezoelectric coefficient (d₃₃), dielectric constant (ɛ₃₃) and remnant polarization (P_r) decreased with an increase in porosity, and the porous PZT ceramics with spherical pores exhibited better properties than that with irregular pores. Furthermore, the electrical conductivities of PZT ceramics were investigated to explain the phenomena that porous PZT ceramics exhibited lower dielectric loss (tan δ) than dense PZT ceramics in the temperature range from 250 to 500 °C.     

Processing and piezoelectric properties of porous PZT ceramics

5–45% porous lead zirconate titanate (PZT) ceramics were fabricated by adding pore formers such as polymethyl methacrylate (PMMA) and dextrin and sintering at 1200 °C for 2 h. The optimum heating procedure was decided according to the thermogravimetric analysis of pore formers. The effects of different pore formers and their content on the microstructure and piezoelectric properties were investigated. With an increase in the content of pore formers, the porosity of sintered ceramics increased, which led to reduced dielectric constant (ɛ₃₃) and longitudinal piezoelectric coefficient (d₃₃) as well as enhanced hydrostatic piezoelectric voltage coefficient (g_h) and hydrostatic figures of merit (d_h g_h). The hydrostatic figures of merit (d_h g_h) of 41% porous PZT were 10 times more than that of 95% dense PZT.     

Stress-induced anisotropy during sintering of hierarchical porosity ceramics

There is significant interest in the design and processing of porous ceramics due to their use in a variety of applications including energy storage, catalysis, adsorption, separation, and life science applications. For many of these applications, it is desirable to have a hierarchical porous structure in which there is a distinct difference between sizes of pores. Our previous study has shown that microstructure and properties of porous materials become anisotropic after sinter-forging. In particular, the small interparticle pores (intrinsic pores) orient parallel to the applied compressive stress, in contrast to large pores from pore formers (extrinsic), which orient perpendicular to the applied stress. However, the pore size, for transition from extrinsic to intrinsic behavior, (transient pore size) has not been quantified. In this study, we report on the effect of applied stresses during sinter-forging on the morphology (shape and size) of pores of different size. Based on these results, we propose a two-step approach to predict transient pore size for hierarchically porous ceramics. We use this approach to quantify the effect of applied stresses on the transient pore size. Finally, we postulate that the stress dependence of the transient pore size may be related to sintering stress—a fundamental quantity in continuum models of sintering. In addition, it can be used to calculate the effective surface energy of complex sintering systems.     

Processing and properties of low cost macroporous alumina ceramics with tailored porosity and pore size fabricated using rice husk and sucrose

The present study demonstrates a cost effective way to fabricate porous ceramics with tailored microstructures using rice husk (RH) of various range of particle sizes as a pore former and sucrose as a binder as well as a pore former. Sample microstructures reveal randomly oriented elongated coarse pores and fine pores (avg. size 4 μm) created due to burnout of RH and sucrose, respectively. Porous alumina ceramics with 20–66 vol% porosity and 50–516 μm avg. pore size (length), having isolated and/or interconnected pores, were fabricated using this process. Mechanical properties of the porous samples were determined as a function of porosity and pore microstructure. The obtained porous ceramics exhibited flexural strength of 207.6–22.3 MPa, compressive strength of 180–9.18 MPa, elastic modulus of 250–18 GPa and hardness of 149–18 HRD. Suggested application area includes thermal, filtration, gas purging etc.     

Porous YSZ ceramics with unidirectionally aligned pore channel structure: Lowering thermal conductivity by silica aerogels impregnation

The previous report of this work has demonstrated the fabrication and properties of porous yttria-stabilized zirconia (YSZ) ceramics with unidirectionally aligned pore channels. As a follow-up study, the present work aims at lowering the thermal conductivity of the porous YSZ ceramics by silica aerogels impregnation. The porous YSZ ceramics were immersed in an about-to-gel silica sol. Both the unidirectionally aligned pore channels and the inter-grain pores by grain stacking in the channel-pore wall of the porous YSZ ceramics were impregnated with the silica sol. After aging and supercritical drying, silica aerogels formed in the macroporous network of the porous YSZ ceramics with unidirectionally aligned pore channels. The influences of silica aerogel impregnation on the microstructure and properties of porous YSZ ceramics with unidirectional aligned pore channels were investigated. The porosity decreased after impregnation with silica aerogels. Both microstructure observation and pore size distribution indicated that both channel-pore size and inter-grain pore-size decreased significantly after impregnation with silica aerogels. Impregnating porous YSZ ceramics with silica aerogels remarkably lowered the room-temperature thermal conductivity and enhanced the compressive strength. The as-fabricated materials are thus suitable for applications in bulk thermal isolators.     

Sintering Behavior of Gehlenite. Part I: Self-Forming, Macro-/Mesoporous Gehlenite—Pore-Forming Mechanism, Microstructure, Mechanical, and Physical Properties

A novel kind of pore self-forming macro-/mesoporous gehlenite (2CaO·Al₂O₃·SiO₂) ceramic (abbreviated C₂AS) having a highest porosity of 80% corresponding to a volume expansion of 134% during sintering has been developed. The pore self-forming ability, microstructure, mechanical, and thermal physical properties of the porous ceramic are related to the sintering temperature. The gehlenite ceramic shows a very good pore self-forming ability over a very wide range of temperature from 900° to 1450°C. No vesicant is required and no hydrothermal treatment is needed, as is generally the case for other kinds of porous ceramics or glasses. The pore self-forming ability of the C₂AS porous ceramic can be attributed to the escape of the adsorbed water vapor during the sintering process, due to automatic hydration of the fine, amorphous, flakey-shaped starting C₂AS powder particles synthesized by the organic steric entrapment (PVA) method, as well as to their fine, porous microstructure. The pores of the ceramics can be either open or closed, and the average pore size ranges from 0.6 to 1.1 μm, corresponding to a porosity of 75%–80%, respectively. The porous ceramic can preserve nanometer-sized (26–50 nm) crystallites up to 1000°C. Sintered or thermally treated under different conditions, the porous ceramics exhibit relatively high flexural strengths ranging from 9.1 to 15.4 MPa, with a standard deviation of 0.3 and 4.2 MPa, respectively. Thermal properties of the porous ceramic up to 1000°C, including thermal expansion coefficient, thermal diffusivity, specific heat, and thermal conductivity, were investigated, and the stability of the porous ceramic in boiling water was also studied.     

多孔陶瓷的制备、性能及应用：（I）多孔陶瓷的制造工艺

多孔陶瓷的制备方法很多，其成孔机理主要有机械挤出、颗粒堆积、成孔剂、发泡、多孔模板、凝结结构成孔。本文根据成孔机理的不同综述了多孔陶瓷的制备工艺最新研究进展。     

Synthesis and thermal shock evaluation of porous SiC ceramic foams for solar thermal applications

Reticulated porous ceramics with structural features spanning across multiple length scales are emerging as the primary media in a variety of demanding mass and heat transfer applications, most notably solar-assisted synthetic fuel processing. In this study, we focus on engineering of the open pore silicon carbide (SiC)-based foams in such catalytic applications. We evaluate the mechanical integrity and thermal stability of these porous structures. X-ray tomography analyses of the 3D structures reveal the presence of dual pore size distribution different by up to an order of magnitude in length scale. We further study the effect of thermal shock—induced via water quenching—on the SiC structures and we conclude that the mechanical properties of the ceramic foams are significantly reduced after thermal stress. Comparison of SEM micrographs—before and after thermal shock—reveals that needle-like features appear inside the foam matrix. These elongated defects may be responsible for structural and mechanical weakening.     

多孔陶瓷的制备、性能及应用:(Ⅰ)多孔陶瓷的制造工艺

多孔陶瓷的制备方法很多 ,其成孔机理主要有机械挤出、颗粒堆积、成孔剂、发泡、多孔模板、凝结结构成孔。本文根据成孔机理的不同综述了多孔陶瓷的制备工艺最新研究进展。     

Novel fabrication route for porous silicon carbide ceramics through the combination of in situ polymerization and reaction bonding techniques

For the first time, an in situ polymerization technique was applied to produce mullite‐bonded porous SiC ceramics via a reaction bonding technique. In this study, SiC microsized particles and alumina nanopowders were successfully coated by polyethylene (PE), which was synthesized from the particle surface in a slurry phase reactor with a Ziegler–Natta catalyst system. The thermal studies of the resulting samples were performed with differential scanning calorimetry and thermogravimetric analysis. The morphology analysis obtained by transmission electron microscopy and scanning electron microscopy (SEM) confirmed that PE was successfully grafted onto the particle surface. Furthermore, the obtained porous ceramics were characterized in terms of their morphologies, phase composition, open porosity, pore size distribution, and mechanical strength. SEM observations and mercury porosimtery analysis revealed that the quality of the dispersion of nanosized alumina powder into the microsized SiC particles was strongly enhanced when the particles were coated by polymers with in situ polymerization. This resulted in a higher strength and porosity of the formed ceramic porous materials with respect to the traditional process. In addition, the X‐ray diffraction results reveal that the amount of mullite as the binder increased significantly for the samples fabricated by this novel method. The effects of the sintering temperature, forming pressure, and polymer content on the physical and mechanical properties of the final porous ceramic were also evaluated in this study. © 2014 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2014 , 131, 40425.