In-situ growth of mullite whiskers and their effect on the microstructure and properties of porous mullite ceramics with an open/closed pore structure

Porous mullite ceramics with an open/closed pore structure were prepared by protein foaming method combined with fly ash hollow spheres. Both the open porosity and total porosity of samples were enhanced by increasing the hollow sphere content. Mullite whiskers with a diameter of 0.2–4 μm were grown in-situ in the porous mullite ceramics with an AlF₃ catalyst, conforming to a vapor-solid growth mechanism. The pore structure of the porous mullite ceramics was significantly affected by the mullite whiskers which increased the open porosity and total porosity. Moreover, the median pore size was reduced from 65.05 μm to 36.92 μm after the introduction of mullite whiskers. The flexural strength and the thermal conductivity of the samples decreased with increasing total porosity. The porosity dependence of the thermal conductivity was well described by the universal model, providing a reference for the prediction of thermal conductivity of porous ceramics with open/closed pores.     

Effect of closed pores on dielectric properties of 0.8Na0.5Bi0.5TiO3-0.2K0.5Bi0.5TiO3 porous ceramics

Porous 0.8Na_0.5Bi_0.5TiO₃-0.2K_0.5Bi_0.5TiO₃ ceramics are fabricated via the pore-forming agent method with polymethyl methacrylate (PMMA) and stearic acid (SA) as pore forming agents, and microstructure observations demonstrate that the porosity, pore shape, and pore sizes can be controlled by the synthesis technology. The dielectric properties of porous ceramics are found not only correlated to the pore-matrix composite model, but also have a significant grain-size effect. Based on the Zener Theory, pining forces exerted by pores on the grain boundary are calculated, to explain the shape effect of pores on grain boundary migration. A phase-field simulation is carried out to investigate pore shape effect on the grain size regulation in porous polycrystalline, and simulation results are in good agreements with experiential results as well as theoretical calculations. Thus, a modified equation is proposed to predict the effective permittivity of the porous piezoelectric ceramics by considering effects of porosity, pore shape and grain size.     

Porous yttria‐Stabilized Zirconia Ceramics Fabricated by Nonaqueous‐Based Gelcasting Process with PMMA Microsphere as Pore‐Forming Agent

Porous yttria‐stabilized zirconia (YSZ) ceramics were fabricated using tert‐butyl alcohol (TBA)‐based gelcasting with monodisperse polymethylmethacrylate (PMMA) microspheres as both pore‐forming agent and lubricant agent. The TBA‐based slurry of 50 vol% solid loading with excellent rheological properties appropriate for casting was successfully prepared by using a commercial polymer dispersant DISPERBYK‐163 as both dispersant and stabilizer. The distribution of the spherical pores made from PMMA microspheres was very homogeneous. Their average diameter decreased from 16.9 to 15.7 μm when the sintering temperature was increased from 1350°C to 1550°C. The compressive strength increased from 14.57 to 142.29 MPa and the thermal conductivity changed from 0.17 to 0.65 W/m·K when the porosity decreased from 71.6% to 45.1%. The results show that this preparation technology can make all the main factors controllable, such as the porosity, the size and shape of pores, the distribution of pores, and the thickness and density of pore walls. This is significant for fabricating porous ceramics with both high compressive strength and low thermal conductivity.     

Effects of pore structure on thermal conductivity and strength of alumina porous ceramics using carbon black as pore-forming agent

In the present work, carbon black (CB) works as a pore-forming agent in the preparation of alumina porous ceramics. The pore structures (i.e. mean pore size, pore size distribution and various pores size proportions) were characterized by means of Micro-image Analysis and Process System (MIAPS) software and mercury intrusion porosimetry. Then their correlation and thermal conductivity as well as strength were determined using grey relation theory. The results showed that the porosity and mean pore size increased against the amount of CB, whereas the thermal conductivity, cold crushing strength and cold modulus of rupture reduced. The <2 μm pores were helpful for enhancing the strength and decreasing the thermal conductivity whereas the >14 μm pores had the opposite effects.     

Preparation of calcium hexaluminate porous ceramics by gel-casting method with polymethyl methacrylate as pore-forming agent

Calcium hexaluminate (CA₆) porous ceramics were prepared by gel-casting method, with α-Al₂O₃ and CaCO₃ as raw materials and polymethyl methacrylate (PMMA) microspheres as pore-forming agent. The effects of the amount of pore-forming agent PMMA microspheres on the phase composition, bulk density, apparent porosity, flexural strength, microstructure, thermal shock stability and thermal conductivity of CA₆ porous ceramics were systematically studied. The pores of CA₆ porous ceramics are mainly formed by the burning loss of PMMA microspheres and the decomposition of organic matter. Adding an appropriate amount of PMMA microspheres as pore-forming agent has a positive effect on the thermal shock stability of CA₆ porous ceramics. When the amount of pore-forming agent is 15 wt%, the volume density of CA₆ porous ceramics is 1.33 g/cm³, the porosity is 63%, the flexural strength is 13.9 MPa, the thermal shock times can reach 9 times, and the thermal conductivity is 0.293 W/(m·K), which can meet the application in refractory, ceramics or high temperature cement industries.     

Permeability of the porous Al2O3 ceramic with bimodal pore size distribution

Porous Al₂O₃ ceramics with bimodal pore size distribution were fabricated by partial sintering with monodispersed PMMA micro balls as pore agent. The porosity of the fabricated porous Al₂O₃ is increased with content of the pore agent increase, the bulk density and bending strength are decreased, accordingly. Relations between pressure drop and flow velocity of the air through the porous Al₂O₃ fit the Forchheimer's equation well for compressible fluid. Due to pores introduced by the pore agent, the Darcy permeability and inertial permeability of the porous Al₂O₃ are increased obviously. For given flow velocity, with increase of the PMMA content, the Forchheimer's number of the fluid through the porous Al₂O₃ is decreased, which results in decrease of the inertial resistance ratio to the total pressure drop. The porous Al₂O₃ ceramics with pores introduced by the monodispersed PMMA micro balls show higher permeability while the filtration selectivity is not deteriorated.     

抛光渣体系发泡陶瓷的发泡性能研究

以工业上成熟的抛光渣体系配方制备发泡陶瓷,探讨了烧结温度对其发泡性能的影响。同时,与外加发泡剂的抛光渣体系发泡陶瓷试样的显微结构、线收缩和体积膨胀率进行了对比分析,探讨了孔结构对发泡陶瓷试样强度和热稳定性的影响。研究发现,抛光渣具备一定的发泡能力,自身可发泡形成尺寸为10~200 μm(1 160~1 220 ℃)的球形气孔结构,孔壁的结构较致密。其对烧结温度十分敏感,在1 180~1 200 ℃范围内,发泡陶瓷试样的体积膨胀了2倍。外加SiC发泡剂能显著提高抛光渣体系发泡陶瓷试样的发泡能力,使其气孔尺寸增加10倍左右,但气孔形状不规则,孔壁结构中存在微小气孔。研究结果表明,外加发泡剂后,抛光渣自身发泡形成的壁孔结构使发泡陶瓷气孔率增加,强度损失较少,导热系数降低,且壁孔结构中的气孔分布不均匀,使发泡陶瓷的热稳定性降低。     

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.     

Mechanical and dielectric properties of porous magnesium aluminate (MgAl2O4) spinel ceramics fabricated by direct foaming-gelcasting

Porous ceramic materials have been broadly applied in various fields due to their multifunctional properties. Optimization of their microstructural characteristics, such as pore morphology, total porosity, and pore size distribution, which determine various properties of the final products, is crucial to improve their performances and thus extend their applications. In this study, single-phase porous MgAl₂O₄ materials were fabricated by direct foaming–gelcasting. With an increase in the foam volume from 260 to 350 mL, the total porosity and pore size of the porous ceramic increased, and its microstructure varied from mostly closed cells to open cells containing interconnected large pores (40–155 μm) and small circular windows (10–40 μm) in the ceramic skeleton. The total porosity could be tailored from 84.91% to 76.08% by modulating the sintering temperature and foam volume and the corresponding compressive strengths were in the range of 2.8–15.0 MPa. The compressive strength exhibited a power-law relationship with the relative density with indices of approximately 3.409 and 3.439, respectively. Porous MgAl₂O₄ ceramics exhibited low dielectric constants in the range of 1.618–1.910 at room temperature, which are well matched with theoretical calculations on account of a modified Bruggeman model. The porous MgAl₂O₄ ceramics with good mechanical and dielectric properties controlled easily by various sintering temperatures and foam volumes are promising for practical applications.     

Porous alumina ceramics with enhanced mechanical and thermal insulation properties based on sol-treated rice husk

To improve the properties of porous alumina ceramics, which were typically prepared by adding pore-forming agents, rice husk (RH) as pore-forming agent was pretreated with zirconia sol. The effects of sol-treatment on the thermal conductivity and compressive strength of the resultant ceramics were characterized. Furthermore, the pore size distribution, pore shape, microstructure, and phase evolution also were studied. The results showed that the RH pretreatment optimizes the microstructure of the ceramic pores. Moreover, complete morph-genetic RH is clearly observed in the pores, which is established as a key factor in improving the properties of the resultant ceramic. The thermal insulation properties are determined to significantly improve, although the thermal conductivity increases slightly with the increment of zirconia sol concentration from 5 to 10?wt%. Meanwhile, after sintering at 1550?°C, the compressive strength is significantly greater for the specimen prepared with 10?wt% zirconia sol-treated RH (65.56?MPa) than that with untreated RH (43.37?MPa). Hence, it was demonstrated that the use of zirconia sol-pretreated RH as a pore-forming agent could enhance the mechanical and thermal insulation properties of porous alumina ceramics.     

Pore-forming agent induced microstructure evolution of freeze casted hydroxyapatite

There were interconnected small lamellar pores, big spherical pores and ceramic walls in the hydroxyapatite (HAP) ceramics fabricated by a freeze casting/pore-former method. As keeping the content of polymethyl methacrylate (PMMA) constant and decreasing the size of PMMA, the size of spherical pores and length of ceramic wall both decreased, and the compressive strength increased. As keeping the size of PMMA and decreasing the content of PMMA, the open porosity decreased and compressive strength increased. The shapes of pores caused by ice crystals were reticular, lamellar and treelike, in turn. The HAP ceramics with the spherical pores of 150-250 μm, open porosity of 62.13% and compressive strength of 7.01 MPa are prospective to have biomedical application.     

High porous ceramics with isometric pores by a novel saponification/gelation/freeze-casting combined route

A new route based on the combination of saponification/gelation/freeze-casting processes, in which the water was used as the solvent, was proposed to produce highly porous ceramics with isometric pores. The saponification reaction using gelatin promoted an inter-connected and equiaxial pore structure with the absence of lamellar pores, even using water as a solvent. The final porosity was up to ∼95 %, and the average pore size ranged from ≈200 up to 500 μm. The amount of saponifying agent had a significant influence on the pore size, while the contents of solids had a more substantial effect on the open porosity. The results indicate that the in situ production of surfactant combined with freeze casting technique allows obtaining ceramics with high porosity and isometric pores even using water as a solvent.     

Novel design of elongated mullite reinforced highly porous alumina ceramics using carbonized rice husk as pore-forming agent

A facile strategy for the fabrication of elongated mullite reinforced porous alumina ceramics (PACs) using carbonized rice husk (CRH) as pore-forming agent and silica source is reported for the first time. A large amount of elongated mullite is synthesized in pores due to the reaction of amorphous silica in CRH skeleton and alumina ceramic powder. Elongated mullite acts as the bridges between pore walls, enhancing the compressive strength of PACs. Furthermore, secondary pores from the intersection of elongated mullite is favor of decreasing of the thermal conductivity. High performance PAC with porosity of 74.3% has been fabricated by employing 25 wt% CRH, which possesses relatively low thermal conductivity of 0.189 W/(m•K) and ultra-high compressive strength of 45 MPa. Its comprehensive performance is much better than that of existing ceramic materials. Our findings present a facile, eco-friendly and effective approach to fabricate high performance PACs as the high-temperature thermal insulation materials.     

Dendritic porous alumina with high porosity by directional freeze casting using a binary solution for bacterial removal

High-porosity dendritic porous alumina was fabricated by using tertiary butanol (TBA) hydrate crystals combined with directional freeze casting. The porosity of this porous alumina approximated 80 %, and its high porosity resulted in high water flux. Dendritic pores improved the physical interception capability of porous ceramics due to the intrinsic moving paths and intercepts from the pore structure. Changes in the TBA content (from 70 vol.% to 85 vol.%) caused a change in pore size from 36.58 μm to 11.54 μm and pore structure (change order: snowflake, dendritic, rod-like, and needle-like), which are important factors affecting water flux and interception capability. The interception and removal of Escherichia coli by 7 mm-height porous ceramics with dendritic structure and an average pore size of 27.90 μm reached 100 % at pH 7.2. This study provides a simple and low-cost method for the effective removal of bacteria.     

成孔剂的量对多孔氧化铝支撑体孔结构的影响

以氧化铝为骨料,淀粉及其它有机粘结剂为成孔剂制备出管状多孔氧化铝支撑体。系统地考察了成孔剂对多孔氧化铝支撑体孔结构的影响。研究表明:当支撑体中成孔剂的质量分数 <10%时,支撑体的孔隙率稳定在35%左右。当成孔剂的质量分数在 10% ~25%之间时,支撑体的孔隙率随成孔剂量的增大而显著增加。当成孔剂的质量分数>25%时,在保证支撑体完整性的前提下,支撑体的孔隙率随成孔剂量的增大变化不大,稳定在 45%左右。成孔剂质量分数的增加会使支撑体的平均孔径增大,孔径分布变宽,平均孔径与最可几孔径的差值增大。     

Effect of starch on pore structure and thermal conductivity of diatomite-based porous ceramics

Considering the low-cost and environmental protection, the porous ceramics with high porosity using natural diatomite powder were successfully prepared by utilizing hot injection moulding and sacrificial fugitives. The impacts of different content of starch as a pore-forming agent on the phase composition, mechanical properties, thermal conductivity, and micro-structure of porous ceramics were investigated. The results demonstrate that starch content can significantly affect the mechanical properties and thermal conductivity of diatomite-based porous ceramics. When the starch content increased from 0 wt % to 50 wt %, the porosity increased from 61.2% to 80%, while the thermal conductivity decreases from 0.239 W/(m K) to 0.098 W/(m K). The low thermal conductivity of porous ceramics may be related to the macroporous–mesoporous composite structure. With the starch content increased, a greater chance of starch granule contact, higher internal pore sizes and a wider pore size distribution in the prepared samples, which resulting in lower mechanical strength, such as the three-point bending strength from 2.83 MPa to 0.46 MPa.     

Controllable preparation of porous ZrB2–SiC ceramics via using KCl space holders

In this work, a novel and facile technique based on using KCl as space holders, along with partial sintering (at 1900 °C for 30 min), was explored to prepare porous ZrB₂–SiC ceramics with controllable pore structure, tunable compressive strength and thermal conductivity. The as-prepared porous ZrB₂–SiC samples possess high porosity of 45–67%, low average pore size of 3–7 μm, high compressive strength of 32–106 MPa, and low room temperature thermal conductivity of 13–34 W m⁻¹ K⁻¹. The porosity, pore structure, compressive strength and thermal conductivity of porous ZrB₂–SiC ceramics can be tuned simply by changing KCl content and its particle size. The effect of porosity and pore structure on the thermal conductivity of as-prepared porous ZrB₂–SiC ceramics was examined and found to be consistent with the classical model for porous materials. The poring mechanism of porous ZrB₂–SiC samples via adding pore-forming agent combined with partial sintering was also preliminary illustrated.     

Optimal design on the mechanical and thermal properties of porous alumina ceramics based on fractal dimension analysis

In order to investigate the relationship between pore structure and thermal conductivity as well as mechanical strength, porous alumina ceramics (PAC) with various pore structures were fabricated, using starch as the pore‐forming agent. Fractal theory was employed to characterize the pore size distribution more accurately than ever used parameters. The results show that the increase in starch content in PAC leads to an enhanced porosity, a higher mean pore size, and reduced fracture dimension, thermal conductivity and strength. The fractal analysis indicated that the fractal dimension decreases gradually and reaches its minimum value with increasing the starch content up to 25 wt%, but the further incorporation results in an opposite trend. It is suggested from micro‐pore fractographic analysis that the optimization of both thermal insulation performance and mechanical strength are positively correlated with the increase in the mean pore size and proportion of 2‐14 μm pores but negatively corrected with the porosity. These results provide a new perspective and a deeper understanding for fabrication of PAC with both excellent thermal insulation and mechanical performance.     

矾土基合成莫来石质多孔陶瓷的研制

采用发泡法与添加造孔剂相结合,以高铝矾土和高岭土为骨料,长石作熔剂,并添加适量的煤、MgSO4和CaSO4作发泡剂,煤为造孔剂,PVA为粘结剂,干压成型后于1500℃左右烧成制备了莫来石质多孔陶瓷。制得的多孔陶瓷莫来石生成量高达90%以上,其气孔分布均匀,孔径分布范围为100～300μm;气孔率高达52.3%（闭孔气孔率为38.7%,开孔气孔率为13.6%）;体积密度为0.9731g/cm3;抗压强度为25.1317MPa;导热系数为0.143W/（m.K）的多孔陶瓷。     

Low Cost Porous Alumina with Tailored Microstructure and Thermal Conductivity Prepared using Rice Husk and Sucrose

This study demonstrates a cost‐effective way to fabricate porous ceramics with tailored porosity and pore microstructure using 5–40 wt% rice husk (RH) in <75 μm, 75–180 μm, 180–355 μm, 355–420 μm, and 420–600 μm size, as pore former. Sucrose, used as binder, also acted as a pore former. Porous alumina compacts with 20%–66% volume fraction porosity and 50–516 μm pore size (length) were successfully fabricated. Microstructure of samples reveal randomly oriented elongated coarse pores and fine pores (avg. size 4 μm), created during burnout of RH and sucrose, respectively. Samples with isolated and/or interconnected pores were fabricated using this process. Thermal conductivity of the samples prepared was measured using Transient Plane Source (TPS) technique. Thermal conductivity ranges from 1.2 to 24 W/mK. Experimental results agree closely with predictions made based on Effective Medium Theory (EMT) for a two‐phase system.