High-strength thermal insulating porous mullite fiber-based ceramics

How to improve the strength of fibrous porous ceramics dramatically under the premise of no sacrificing its low density and thermal conductivity has remained a challenge in the high-temperature thermal insulation field. In this paper, a new kind of high-strength mullite fiber-based ceramics composed of interlocked porous mullite fibers was prepared by nanoemulsion electrospinning and dry pressing method. Results show that as to the porous ceramics with the same density (～ 0.8 g/cm³), the three-dimensional skeleton structure composed of porous mullite fibers was much denser than that composed of solid mullite fibers. Therefore, porous mullite fiber-based ceramics exhibited a higher compressive strength (5.53 MPa) than that of solid mullite fiber-based ceramics (3.21 MPa). In addition, porous mullite fiber-based ceramics exhibited a superior high-temperature heat insulation property because the porous structure in fibers could reduce the radiant heat conduction. This work provides new insight into the development of high-temperature thermal insulators.     

Lightweight and thermally insulating aluminum borate nanofibrous porous ceramics

Aluminum borate porous ceramics are excellent candidates for high-temperature insulation applications. Current research on aluminum borate-based porous ceramics mainly focuses on porous ceramics made up of aluminum borate whiskers, whose low aspect ratio leads to a relatively dense porous structure; this results in porous ceramics with low porosity and relatively high thermal conductivity. In this study, we report the manufacturing of aluminum borate nanofibrous porous ceramics by an agar-based gel casting method using electrospun nanofibers with a high aspect ratio as the three-dimensional skeleton structure. We explored the effect of the alumina/boron oxide molar ratio on the microscopic morphology and crystal phase composition of the aluminum borate nanofibers and that of the sintering temperature on the micro and macro properties of porous ceramics based on the nanofibers. The results showed that aluminum borate nanofibers with an alumina/boron oxide molar ratio of 7:2 had the densest microscopic morphology, and the corresponding porous ceramics exhibited a higher porosity (91%) and lower thermal conductivity (0.11 W m^?1 K^?1) after sintering at 1200 °C than aluminum borate porous ceramics with aluminum borate whiskers as the skeleton. The successful synthesis of aluminum borate nanofibrous porous ceramics provides new insights into the development of high-temperature insulators.     

Ultra-low cost porous mullite ceramics with excellent dielectric properties and low thermal conductivity fabricated from kaolin for radome applications

Near-net-shape mullite ceramics with high porosity were prepared from ultra-low cost natural aluminosilicate mineral kaolin as raw material and polystyrene micro-sphere (PS) as pore-forming agent. Microstructure, flexural strength, thermal conductivity and dielectric properties of the ceramics were systematically researched. Results show that the porous mullite ceramics possess fibrous skeleton structure formed by a large quantity of interlocked mullite whiskers, which results in good mechanical properties and low-to-zero sintering shrinkage. Flexural strength of the porous mullite ceramics can be up to 41.01 ± 1.12 MPa, even if the porosity is as high as 62.44%. The dielectric constant and loss tangent of the porous mullite ceramics at room temperature are lower than 2.61 and 5.9 × 10⁻³, respectively. Besides, dielectric constant is very stable with the rising of temperature, and the dielectric loss can be consistently lower than 10⁻² when the temperature is not higher than 800 °C. In addition, thermal conductivity at room temperature is as low as 0.163 W/m/K when the porosity of mullite ceramics is 80.05%. The infiltration of SiO₂ aerogels (SiO₂ AGs) can further decrease the thermal conductivity to 0.075 W/m/K, while has just little effects on the dielectric properties. Excellent mechanical, thermal and dielectric properties show that the porous mullite ceramics have potential applications in radome fields. The porous mullite ceramics prepared from kaolin not only have low cost, but also can achieve near-net-shape.     

Effect of mullite phase formed in situ on pore structure and properties of high-purity mullite fibrous ceramics

Porous mullite ceramics are potential advanced thermal insulating materials. Pore structure and purity are the main factors that affect properties of these ceramics. In this study, high performance porous mullite ceramics were prepared via aqueous gel-casting using mullite fibers and kaolin as the raw materials and ρ-Al₂O₃ as the gelling agent. Effects of addition of mullite fibers on the pore structure and properties were examined. The results indicated that mullite phase in situ formed by kaolin, and ρ-Al₂O₃ ensured the purity of mullite samples and mullite fibers bonded together to form a nest-like structure, greatly improving the properties of ceramic samples. In particular, the apparent porosity of mullite samples reached 73.6%. In the presence of 75% of mullite fibers, the thermal conductivity was only 0.289 W/m K at room temperature. Moreover, the mullite samples possessed relatively high cold compressive strength in the range of 4.9–9.6 MPa. Therefore, porous mullite ceramics prepared via aqueous gel-casting could be used for wide applications in thermal insulation materials, attributing to the excellent properties such as high cold compressive strength and low thermal conductivity.     

Multilayered mullite ceramics with anisotropic properties

Anisotropic layered porous ceramics are crucial to satisfy the demand for devices with directional functions. However, challenges, such as complicated preparation processes and difficulties in regulating the oriented structure, severely limit their application. Here, multilayered mullite ceramics (MLMCs) with specific porosities and strongly anisotropy properties, were prepared by designing porous thin-layered units and an interlayer layout, in combination with a simple gel-casting. Benefiting from the suitable slurry properties, the samples did not show obvious defects, and a perfect bonding was observed between the layers. The optimized MLMCs exhibited a porosity of 65.12%, the differences in compressive and flexural strengths of 14 ( ± 0.7) and 5 ( ± 0.2) MPa in different pressure directions respectively, and the anisotropy factor of thermal conductivity up to 0.98, as well as exhibited good high temperature thermal insulation properties. Ultimately, the MLMCs formed transverse heat conductor and longitudinal heat insulation heat-transfer patterns, with promising applications in thermal insulation.     

The preparation and properties of high-strength porous mullite ceramics by a novel non-toxic gelcasting process

A novel approach to fabricate porous mullite ceramics with homogeneous pore size and high-strength using green non-toxic and cost-effective poly-γ-glutamic acid (γ-PGA) gelling system was reported for the first time. Effect of γ-PGA addition, additive amount and solid loading on rheological behavior of the slurries, and microstructure and properties of samples were investigated systematically. By optimizing the solid loading of mullite samples, we are able to get the sample with small pores (< 200 µm) dominating (93.3% of the total pores), and compressive strength of the sample reaches up to 26.62 MPa. In addition, the mullite ceramics exhibited high porosity of 75.7% with low thermal conductivity of 0.279 W/(m·K) at room temperature. This study not only provides a green and non-toxic gelling system but also offers porous mullite ceramics with low thermal conductivity and excellent mechanical strength as an energy-saving thermal insulation material.     

Fibrous porous mullite ceramics modified by mullite whiskers for thermal insulation and sound absorption

In order to meet the demand for thermal insulation and sound absorption, fibrous porous mullite ceramics (FPMC) with high porosity and an interconnected pore structure were prepared, followed by a pore structure modification with in situ grown mullite whiskers on the three-dimensional framework of the FPMC. The resultant hierarchical material exhibited superior sound absorption performance in the low-to-medium frequency to most reported sound-absorbing materials, as well as a sufficient compressive strength of 1.26 MPa with low thermal conductivity of 0.117 W·m^?1·K^?1. Moreover, the effects of solid content and mullite whiskers on the microstructure and physical properties of the material were analyzed. The increase of solid content led to increased compressive strength and thermal conductivity and decreased frequency corresponding to the first sound absorption peak. The thermal conductivity and compressive strength of the material increased as the mullite whiskers grew, while the median pore size decreased.     

Foam gel-casting preparation of SiC bonded ZrB2 porous ceramics for high-performance thermal insulation

Lightweight SiC-ZrB₂ porous ceramics is of great potential as thermal insulation material used in aerospace, chemical and energy industries. In this work, a series of SiC bonded ZrB₂ (SiC_b-ZrB₂) porous ceramics with porosity high up to 86.9% were prepared by a simple foam gel-casting method. The SiC_b-ZrB₂ porous ceramic prepared at 1573 K exhibited a low thermal conductivity of 0.280 W/(m?K) and a reasonable compressive strength of 0.52 MPa. It could maintain the original geometric shape and microstructure after a secondary heat treatment at 1473 K in inert atmosphere. When heating the samples with thickness of 30 mm for 12 min with an alcohol spray lamp (～1273 K), the temperatures of the cold sides of SiC_b-ZrB₂ ceramics were all lower than 432 K, demonstrating their exceptional insulation capabilities. The present work provides a simple route to produce robust and thermally-insulating non-oxide porous ceramics for use under high temperature.     

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.     

Microstructural evolution of mullite nanofibrous aerogels with different ice crystal growth inhibitors

Mullite nanofibrous aerogels with low density, low thermal conductivity and high service temperature (as high as 1400 °C) was fabricated by the freeze-casting method, and two different kinds of ice crystal growth inhibitors, glycerol as the cryoprotector and agarose as the gel-former, were adopted respectively to influence the growth of ice crystal, thereby adjusting the sample microstructure (including the pore size and the pore distribution). The addition of glycerol could influence the growth of the ice crystal, leading to the pore structure changing from the cellular pores to the spherical pores and the decrease of the large pore size, consequently resulting in the increase of the sample density and compressive strength. The addition of agarose could inhibit the growth of the ice crystal due to the formation of gel network, resulting in the disappearance of the large pores (cellular pores). The sample with high agarose content exhibited a relatively high compressive strength of 252.41 kPa due to high density and uniform pore structure. The research of this work provides an effective method to regulate the properties of nanofibrous aerogel to meet the demand of different applications.     

Seed assisted in-situ synthesis of porous anorthite/mullite whisker ceramics by foam-freeze casting

Porous anorthite/mullite whisker ceramics with both high strength and low thermal conductivity have been successfully prepared by combining seed-assisted in situ synthesis and foam-freeze casting techniques. The addition of mullite seed was conducive to a reduction in the sintering shrinkage, pore size, and anorthite grain size. This increased the high aspect ratio of mullite whiskers, which enhanced the strength and diminished the thermal conductivity. Mullite whiskers overlapped to form a stable three-dimensional network structure similar to the bird's nest, which was also beneficial to heighten the mechanical properties of the prepared porous ceramics. Through this method, the prepared materials had a high apparent porosity of 87.7–90.2%, a low bulk density of 0.29–0.36 g/cm³, a high compressive strength of 0.65–3.31 MPa, and low thermal conductivity of 0.067–0.112 W/m·K. The results indicated that the method described here can fabricate porous ceramics with excellent properties for further thermal insulating applications.     

Enhancing the thermal insulating properties of lanthanum zirconate porous ceramics via pore structure tailoring

The potentially useful role of lanthanum zirconate (La₂Zr₂O₇, LZO) porous bulk ceramics has been rarely explored thus far, much less the optimisation of its pore structure. In this study, LZO porous ceramics were successfully fabricated using a tert-butyl alcohol (TBA)-based gelcasting method, and the pore structures were tailored by varying the initial solid loading of the slurry. The as-prepared ceramics exhibited an interconnected pore structure with high porosity (67.9 %–84.2 %), low thermal conductivity (0.083–0.207 W/(m·K)), and relatively high compressive strength (1.56–7.89 MPa). The LZO porous ceramics with porosity of 84.2 % showed thermal conductivity as low as 0.083 W/(m·K) at room temperature and 0.141 W/(m·K) at 1200 °C, which is much lower than the counterparts fabricated from particle-stabilized foams owing to its unique pore structure with a smaller size, exhibiting better thermal insulating performance.     

Superior hydrophobicity of nano-SiO2 porous thermal insulating material treated by oil-in-water microemulsion

Nano-SiO₂ porous thermal insulating material (TIM) has drawn tremendous research interests due to its advantages of low density, high porosity and low thermal conductivity. However, its long-term stability in humid environment can be severely deteriorated by the high hydrophilicity resulting from tetrahedral coordination of oxygen and capillary effect of porous structure. It is still a great challenge to cost-effectively fabricate bulk TIM with superior hydrophobicity and consequent remarkable self-cleaning capability. Herein, via an oil-in-water microemulsion treatment, we have proposed a new strategy to construct 3D superior hydrophobic nano-SiO₂ porous TIM. The polymethylhydrosiloxane-modified TIM exhibits a large water contact angle of 166°, and corresponding excellent self-cleaning characteristic while maintaining low thermal conductivity of 0.031 W/m·K. Moreover, our high hydrophobicity of TIM exhibits excellent durability under high temperature up to 400 °C, high humidity of 100%, and chemical erosions. Detailed knowledge of the physical chemistry basis of the superior hydrophobic nano-SiO₂ porous TIM can provide great opportunity to fabricate advanced self-cleaning and heat insulating devices especially targeted for harsh environments.     

Multi-functional mullite fiber-based porous ceramics with a multilevel pore structure assembled by alumina platelets and mullite whiskers

Mullite fiber-based porous ceramics have been widely used in the field of heat insulation. To further broaden their applications in other fields, such as filtration and sound absorption, mullite whiskers and alumina platelets were introduced as the secondary structural materials in mullite fiber-based porous ceramics by a sol-gel combining heat-treating method, and new fiber-based porous ceramics with a unique multilevel pore structure were developed. By adjusting the molar ratios of aluminium tri-sec-butoxide to aluminium fluoride and calcination temperature, these fiber-based porous ceramics not only presented the characteristics of lightweight (maximum density of 0.38 g/cm³) and good heat insulation (minimum thermal conductivity of 0.11 W/mK) comparable to traditional fiber-based porous ceramics, but also showed a superior specific surface area (up to 11.5 g/m²) and excellent sound absorption performance (average sound absorption coefficient as high as 0.728). Owing to these outstanding characteristics, the corresponding porous ceramics are expected to be promising multifunctional materials in diverse fields, especially thermal insulation and sound absorption.     

Mechanical evaluations of mullite fibrous ceramics processed by filtration and in situ pyrolysis of organic precursor

Highly porous mullite fiber-based ceramics with a three-dimensional cross structure were successfully designed and fabricated by filtration method. To address the thermal migration of silica sol, polysiloxane was introduced in the bonding system as high temperature binder to form more stable nods in the skeleton as opposed to silica sol which would migrate to the surface of fibers during the sintering process. Due to the lapped structure of mullite fibers, all products showed high porosity(74.1%～80.9%), low density(0.554g/cm³～0.608g/cm³) and relatively low thermal conductivity(<0.14 W/(m*K)). The reaction process of in situ porolysis and fracture mechanisms were illustrated, respectively. Besides, results showed that both sintering temperature and binder content had significant influence on the microstructure and mechanical properties of the products.     

Preparation of novel reticulated prickly porous ceramics with mullite whiskers

Porous materials are widely used in heat exchangers, sewage treatment, electromagnetic shielding, thermal insulation, gas adsorption, photocatalytic due to their high specific surface area. The specific surface area of materials plays a pivotal role in them. It can be enhanced by increasing the porosity of the material, but the cost of this improvement is reducing the strength of the material. In order to improve performance, it is necessary to increase its surface area without reducing the strength of the material. In this work, mullite porous ceramics with mullite whisker on the inside and outside surfaces structures, which known as prickly porous ceramics(PPCs). They were fabricated using polyurethane foam coated with slurries as the pore-forming agents, sintered after secondary impregnation with silica sol and ammonium fluoroaluminate. The the sintering temperature as well as slurry composition of secondary impregnation were tuned to tailor the strength and surface structures of the PPCs. In addition, the potential of PPCs as high-temperature catalyst supports was demonstrated. Overall, the PPCs demonstrated large surface areas and high mechanical strength. This study paved the way for the fabrication of high-performance porous ceramics.     

Highly porous fibrous mullite ceramic membrane with interconnected pores for high performance dust removal

Porous fibrous mullite ceramic membranes with different content of fibers were successfully fabricated by molding method for dust removal. The properties of the samples, such as microstructure, porosity, bulk density and mechanical behavior were analyzed. Owing to the highly porous three-dimensional structure of ceramic membranes, all the samples exhibited low density (lower than 0.64?g/cm³), high porosity (higher than 73%), low linear shrinkage (lower than 1.0%) and low thermal conductivity (lower than 0.165?W/mK). Significantly, the as-prepared porous ceramic membrane possessed of enhanced dust removal efficiency with almost 100% for 3–10?µm, 97% for 1.0?µm, 87% for 0.5?µm and 82% for 0.3?µm dust particles in diameter from dust-laden air passed through the test module. Moreover, the pressure drop was lower than 80?Pa when the airflow linear velocity reached 1.25?m?min^?1. The results indicated that the ceramic membranes prepared in this work were promising high efficiency dedusting materials for the application in gas filtration field.     

Mechanical and thermal behavior of cellular mullite materials

In this paper, the mechanical behavior and thermal properties of cellular mullite bodies obtained by thermal direct-consolidation of foamed aqueous suspensions of mullite-bovine serum albumin (BSA) and mullite-BSA-methylcellulose (MC) were studied. The mechanical behavior of cellular mullite materials sintered at 1600 °C was evaluated by diametral compression at room temperature, 1000 °C and 1300 °C. The variation in the thermal diffusivity and thermal conductivity at temperatures up to 900 °C was determined using the laser-flash method. The results of the mechanical and thermal evaluation were analyzed based on the porosity features of the sintered materials, which was determined in turn by the starting system used for shaping the bodies.     

Effects of firing temperature on the microstructures and properties of porous mullite ceramics prepared by foam-gelcasting

Porous mullite ceramics were prepared at 1300–1600°C for 2?h via a foam-gelcasting route using industrial-grade mullite powders as the main raw material, Isobam 104 as the dispersing and gelling agent, triethanolamine lauryl sulphate as the foaming agent and sodium carboxymethyl cellulose as the foam stabilising agent. The effects of firing temperature on the sintering behaviour of green samples as well as microstructures and properties of final porous mullite products were investigated. With increasing the temperature from 1300 to 1600°C, linear shrinkage and bulk density values of fired samples increased, whereas their porosity decreased. Mechanical strength and thermal conductivity values of fired samples decreased with increasing their porosities. Even at a porosity level as high as 79.4%, compressive and flexural strengths of fired samples (with average pore size of 314?μm) remained as high as 9.0 and 3.7?MPa, respectively, and their thermal conductivity (at 200°C) remained as low as 0.21?W?(m^?1?K^?1).     

Preparation and characterization of porous mullite ceramics via foam-gelcasting

Porous mullite ceramics were prepared via foam-gelcasting using industrial grade mullite powder as the main raw materials, Isobam-104 as the dispersing and gelling agent, sodium carboxymethyl cellulose as the foam stabilizing agent, and triethanolamine lauryl sulfate as the foaming agent. The effects of processing parameters such as type and amount of additive, solid loading level and gelling temperature on rheological properties and gelling behaviors of the slurries were investigated. The green samples after drying at 100 °C for 24 h were fired at 1600 °C for 2 h, and the microstructures and properties of the resultant porous ceramic samples were characterized. Based on the results, the effects of foaming agent on the porosity level, pore structure and size and mechanical properties of the as-prepared porous mullite ceramics were examined. Porosity levels and pore sizes of the as-prepared samples increased with increasing the foaming agent content up to 1.0%, above which both porosity levels and pore sizes did not change. The compressive strength and flexural strength of the as-prepared sample with porosity of 76% and average pore size of 313 μm remained as high as 15.3±0.3 MPa and 3.7±0.2 MPa, respectively, and permeability increased exponentially with increasing the porosity.