In situ mullite foam fabrication using microwave energy

In situ mullite ceramic foams were fabricated using polymeric sponge replication method from ceramic slurry containing alpha alumina and kaolin mixtures. Ceramic preforms were processed using microwave energy and conventional heating. The sintered foam samples were characterized by SEM and XRD observations, density measurements and compression tests in order to observe the effect of two different sintering techniques on the structure and properties. It was found that the microwave processing was completed in a shorter burning out and sintering cycle and produced structures having higher mullite transformation ratio and fine grains.     

Macrostructural changes of polymer replicated open cell cordierite based foams upon sintering

Abstract

The goal of this work was to clarify the macrostructural changes that take place upon sintering of open cell cordierite based foams. A methodology, based on optical image analysis, was developed to assess the structure of open-cell foams, which allowed evaluating the macrostructure of both cordierite based foams obtained by the replication process and their polymeric templates. The parameters used to describe the structures were the size of the cell and the window, the window shape factor, the strut thickness and the volume fraction of the material. The experimental evidence gathered opened the way to understand the physical/chemical transformations involved in the polymer burnout and the ceramic sintering processes, as well as their influence on the ceramic final structure. The observed trends provide guidance for tailoring 'replicated' cordierite based foams, in view of the required application.     

Behaviour of open-cell cordierite foams under compression

Cordierite foams were produced using the polymer foam replication method. The effects of both the structure of the polymeric foam template and the slurry's solid loads on the compressive strength and the sintered structure of the ceramic foam were evaluated in order to achieve the optimal manufacturing conditions. The compressive strengths of cordierite foams were measured at room temperature. Polyurethane (PU) foams were used as templates. Aqueous ceramic suspensions were prepared with solids weight fraction ranging from 50 to 65%. The effects of both the PU density and the solids volume fraction on porosity and strength of the developed cordierite foams were evaluated. The cordierite foams produced are of semiclosed-cell type. Some impregnation difficulties were experienced with increasing of the PU density. The compressive strength of the cordierite foams increased (from 0.1 to 2 MPa) with increasing solids volume fraction. These data are in agreement with the predictions of the model developed by Gibson and Ashby. However, the exponent of the model was half of the measured one (≈3) over the range of relative densities investigated (80–90%). Such discrepancy might be related to several factors such as the morphological differences in the structural unit of the developed foams with respect to a cubic open-cell foam or to the mixture of both open and closed cells or to the presence of non-periodic cells. In addition, it was found that the compressive strengths depended on the cell size for foams of similar relative densities and generally decreased with increasing of the cell size, which deviates from the theoretical predictions. When the starting polymeric substrate contained a higher fraction of closed cell windows, however, the ceramic material present on the cellular structure was not only distributed on the struts but also filled the cell walls. This contributed to an increase of the relative density of the cordierite foams and consequently to higher compressive strengths.     

不同铝源对SiC/堇青石复相多孔陶瓷的制备及性能影响

以碳化硅、氮化铝、层析氧化铝、氢氧化铝、氟化铝、滑石为主要原料,石墨为造孔剂通过原位反应烧结技术制备碳化硅/堇青石复相多孔陶瓷.研究了含铝化合物种类、烧结温度、石墨含量对SiC/堇青石复相多孔陶瓷相组成、微观结构、气孔率和抗折强度的影响,同时对S0组在1200℃烧结温度下制得的SiC/堇青石复合多孔陶瓷的孔径分布进行了测试分析.结果表明:以AlN为铝源在1200℃下烧结,石墨含量在15％时,堇青石结合SiC多孔陶瓷的抗弯强度和气孔率两项综合性能达到最优,气孔率为31.99％,相应的弯曲强度86.20 MPa.S0组的平均孔径大小在3.0191 μm.     

Experimental and numerical analysis of the complex permittivity of open-cell ceramic foams

Open-cell ceramic foams are promising materials in the field of microwave heating. They can be manufactured from susceptor materials and can, therefore, be used as selective heating elements. In this study, the complex permittivities of ceramic foam materials, including silicon-infiltrated silicon carbide (SiSiC), pressureless sintered silicon carbide (SSiC), silicate-bonded silicon carbide (SBSiC), and cordierite were determined. The dielectric properties of the foams were determined by the cavity perturbation technique using a TE₁₀₄ WR340 waveguide resonator at 2.45 GHz. Samples were preheated in a tubular furnace, enabling temperature-dependent permittivity measurements up to 200 °C. The effective dielectric constant and effective loss factor were found to depend on the porosity and material composition of the foam. The SiSiC material had a higher effective dielectric constant than the SSiC and SBSiC ceramics. The effective dielectric constant of the foams showed a trend of gradual increase with increasing temperature. Some selected dielectric mixing relations were then applied to describe the effective permittivity of the foams and compare them with predictions from finite element simulations performed using the CST Studio Suite. The foam morphologies and simple block inclusions were used in the simulations.     

原位反应烧成莫来石-堇青石复合材料及其特性(英文)

通过原位反应烧成方法制备了不同莫来石、堇青石含量比的复合材料。首先,根据堇青石和莫来石的理论化学组成,分别将高岭土、工业氧化铝和滑石混合,配制出堇青石生料粉(C粉)和莫来石生料粉(M粉)。然后,再将C粉和M粉按不同的设计比例混合,烧结制备出一系列莫来石-堇青石复合材料。添加V2O5添加剂,考察其对烧结复合材料的影响。并通过X射线衍射,微观结构观察,热力学性质检验,比较了不同莫来石、堇青石含量比的复合材料的特性。制备的莫来石-堇青石复合材料所用的烧结温度可降低至1380℃,且复合材料中堇青石和莫来石晶体发育良好,复合材料抗热震性好。     

In situ synthesis of three-dimensional nanofiber-knitted ceramic foams via reactive sintering silicon foams

Three-dimensional ceramic nanofiber-assembled materials with large specific surface area and excellent thermal insulation properties are attracting increasing interests for their unique structure and promising applications. In this paper, we propose a facile methodology to fabricate three-dimensional silicon nitride nanofiber-knitted ceramic foams via in situ reactive synthesis from silicon foams. Silicon particle-stabilized foams are fabricated for the first time using long-chain surfactant cetyltrimethyl ammonium bromide as a hydrophobic modifier. First, the fabrication and stability of silicon foams are investigated. Based on the stable silicon foams, silicon nitride-based nanofiber-knitted ceramic foams are synthesized via in situ reactive sintering in nitrogen atmosphere. The novel ceramic foam materials consist of three-dimensional nanofiber-assembled strut wall and nanofiber-spheres in the pores. The diameter of obtained silicon nitride nanofibers ranges from 15 to 100 nm. The unique nanofiber-knitted foams may have potential applications in specific fields, including catalysis, adsorption, separation, and thermal insulation.     

Silicon carbide particle reinforced mullite composite foams

Silicon carbide particle reinforced mullite composite foams were produced by the polymer replica method using alumina and kaolin to form in situ mullite matrix. Up to 20 wt.% silicon carbide particles (SiCp) were added to aqueous ceramic slurry to explore its effect on the rheological behaviour of ceramic slurries and also properties of as sintered products. By means of solid loading optimisation and sintering enhancement by silicon carbide, mullite based ceramic composite foams of higher strength were obtained. The strength of the as sintered foams was found to depend greatly on the phase composition, relative density of the structures and the amount of SiCp addition. By studying the effect of the additive concentration, on the mechanical properties of the ceramic matrix, it is found that the optimal silicon carbide addition is 20 wt.%.     

低成本大孔陶瓷膜支撑体的制备与表征(英文)

以高岭土和白云石为主要原料,通过反应烧结法制备低成本大孔陶瓷膜支撑体,对制备的支撑体进行了结构和性能表征.结果表明:在高岭土中引入质量分数为20%的白云石,可显著抑制高岭土的高温烧结;加入白云石后制备的支撑体在1 150~1 300℃保温1h后,主晶相为莫来石、堇青石和钙长石,平均孔径和抗弯强度随烧成温度升高而增大,而水通量和孔隙率降低;加入20%白云石并在1 250℃保温1 h制各的大孔支撑体的孔隙率和平均孔径分别为44.6%和4.7μm,抗弯强度和纯净水通量分别达到47.6MPa和10.76m3/(m2·h·bar).     

Preparation of refractory cordierite using amorphous rice husk silica for thermal insulation purposes

This study aims to investigate the effect of sintering temperatures on the phase formation and physical characteristics of refractory cordierite prepared from rice husk silica, Al₂O₃, and MgO powders. The samples were subjected to sintering temperatures of 1050–1350 °C, and development of structures was characterized using Fourier Transform Infrared (FTIR) spectroscopy, X-ray diffraction (XRD) coupled with Rietveld analysis, scanning electron microscopy (SEM) and dilatometry. The results obtained indicated the significant role of sintering temperatures on phase transformation of spinel and cristobalite into cordierite, in which at sintering temperatures of 1230–1350 °C the cordierite emerges as a dominant phase, while spinel and cristobalite are practically undetected. Formation of cordierite was followed by decrease in density, porosity, and thermal expansion coefficient, while for hardness and bending strength the opposite was true. Thermal expansion coefficient of the sintered sample at 1350 °C is 3.3×10⁻⁶/°C and the XRD analysis demonstrated that the main crystalline phase is cordierite. Based on these characteristics, the samples are considered as insulator, suggesting their potential use in refractory devices.     

Facile preparation of thermal insulation materials by microwave sintering of ferronickel slag and fly ash cenosphere

A novel approach for preparing thermal insulation materials by microwave sintering of ferronickel slag (FNS) in the presence of fly ash cenosphere (FAC) was proposed and evaluated. The study showed that during microwave radiation, the contact interface between FNS and FAC would preferentially form magnesium iron chromate spinel and magnesium iron aluminate spinel particles as hot spots by absorbing microwave vigorously, promoting decomposition and transformation of the raw materials into the thermal insulation phases, mainly cordierite and enstatite. After sintering at 900 °C by microwave for only 20 min with the addition of 25 wt% FAC, a thermal insulation material with thermal conductivity of 0.41 W/(m·K), bulk density of 1.46 g/cm³, compressive strength of 30.72 MPa, water absorption of 21.07%, and linear shrinkage of 7.06% was obtained. Compared with the conventional sintering method, the temperature was reduced by 300 °C, with the sintering time shortened by 6 times. This study represents a good example for clean and efficient value-added utilization of FNS, FAC and other relavent solid wastes.     

Surface Precipitation Route for the Development of Cordierite-Zirconia Composites

Based on the interfacial electrochemical properties of aqueous cordierite dispersion, a novel interfacial scheme for fabricating cordierite-ZrO₂ composite with a dense and homogeneous microstructure was proposed and tested. In the present processing route, cordierite particles were first uniformly coated with a thin layer (∼40 nm) of aluminum hydroxide by an in situ surface-induced coating. Then, a controlled surface precipitation of ultrafine zirconium hydroxide precursor onto the coated cordierite particles was performed to obtain a composite with a uniform spatial distribution of the dispersed ZrO₂ particles throughout the matrix. The coated layer acted to suppress the formation of zircon phase during sintering. The enhanced fracture toughness observed in the presence of ZrO₂ was partly attributed to the t → m transformation toughening of the dispersed tetragonal ZrO₂ particles.     

铝钒土含量对低膨胀高远红外瓷质卫生陶瓷性能的影响

采用煤矸石废料、劣质原料黑滑石和铝钒土为主要原料,通过原位生长法制备了堇青石质低膨胀高远红外瓷质卫生陶瓷。利用XRD、SEM和性能测试研究铝钒土含量对堇青石卫生陶瓷性能的影响。实验结果表明:铝钒土含量对吸水率、抗折强度和膨胀系数具有较明显的影响,而对远红外辐射率并未带来不利的影响,所有样品的远红外率均保持在0.93以上。当铝钒土含量为27%,煤矸石33wt.%,黑滑石37%时,陶瓷性能达到最优:吸水率为0.04%,热膨胀系数为2.74×10-6/℃,抗折强度为87.4 MPa。这主要是由于样品的主晶相堇青石含量最高,并且烧结致密化程度高,其中气孔分布更加均匀所致。相关研究结果对环境保护和工业废物的资源化利用有着积极意义。     

Fabrication and Characterization of Near‐Net‐Shape In Situ Reaction‐Bonded Porous Cordierite/SiC Ceramics

Porous cordierite/SiC ceramics were fabricated by in situ reaction bonding using α‐SiC, α‐Al₂O_3, and MgO powders as the starting materials. During sintering, part SiC is oxidized to SiO₂ and then the latter reacts with Al₂O₃ and MgO to form cordierite. As a result, porous cordierite/SiC ceramics were obtained, and the ceramics are strengthened by the residual SiC. Due to the large volume expansion introduced by the oxidation of SiC, the ceramics exhibit small sintering‐induced dimension variations. In addition, a fine‐grained microstructure and good thermal and mechanical properties were obtained for the porous cordierite/SiC ceramics.     

Glass foam of macroporosity using glass waste and sodium hydroxide as the foaming agent

Glass foams using float glass waste and sodium hydroxide were produced. The influence of the sodium hydroxide amount in the foam formulation was studied. Titanium dioxide was used as a strengthening agent. The variations of temperature, heating rate and sintering time were investigated during the synthesis process. Open porosity was estimated using mercury porosimetry. The morphology of the glass foams was evaluated using scanning electron microscopy, phase formation was studied using X-ray diffraction, and chemical composition was estimated using X-ray fluorescence. As a result, glass foams with macroporosity were obtained. Since the glass foams used glass waste as reactant, the results suggest the development of an alternative route for glass recycling.     

泡沫碳化硅陶瓷材料的研究进展

泡沫碳化硅陶瓷材料除了孔隙率高、比表面积大,还具有相对密度小、优良的热学、力学、电学、声学性能等特性,已经广泛应用于化工、机械、生物、环保等领域。本文总结了泡沫碳化硅陶瓷材料的主要制备技术,包括粉末烧结法、固相反应烧结法、含硅树脂热解法以及气相沉积法等。阐述了泡沫碳化硅陶瓷材料的几种优良特性,包括结构特征、流体阻力、抗氧化性、吸波性等。最后举例介绍了该陶瓷在催化、过滤、生物学等领域的应用现状,重点介绍了其作为塔内件在化工领域中的应用,指出为满足对泡沫碳化硅陶瓷更高性能的需求,不仅要对现有技术进行集成创新,更要挖掘和开发泡沫碳化硅的潜在优势。     

Reuse of mineral wool waste and recycled glass in ceramic foams

Novel ceramic foams have been prepared by high temperature sintering of waste mineral wool and waste glass using SiC as a foaming agent. The aim of the research was to understand the effects of composition and sintering conditions on the properties and microstructure and produce commercially exploitable ceramic foams. Optimum ceramic foams were formed from 40 wt% mineral wool waste and 2 wt% SiC, sintered at 1170 °C using a heating rate of 20 °C/min with a 20 min hold at peak temperature. The ceramic foams produced had a bulk density of 0.71 g/cm³ and a uniform pore size distribution. The research shows that ceramic foams can be formed from waste mineral wool and these can be used for thermal insulation with associated economic and environmental benefits.     

Fabrication of Stainless-Steel-Fiber-Reinforced Cordierite-Matrix Composites of Tubular Shape Using Electrophoretic Deposition

Stainless-steel (316L) fiber mats shaped into tubular geometry were used to reinforce cordierite. The cordierite-matrix composites were manufactured using electrophoretic deposition and pressureless sintering. The sintered composites, which had an internal and external deposit thickness of ∼1 mm, were free of surface cracks when a deposition time of 2.5 min was used. Metal-fiber-reinforced cordierite composites such as those developed here may constitute a promising alternative for manufacturing damage-tolerant tubular components for applications at temperatures up to ∼900°C.     

Preparation of Synthetic Cordierite by Solid-State Reaction via Bismuth Oxide Flux

A comparative study of the solid-state reaction synthesis of cordierite with and without the use of a flux was performed, varying the sintering temperatures between 900° and 1400°C. Bi₂O₃ proved to be a useful additive for lowering the temperature needed for the reaction to take place. The deviation from the ordered β-cordierite phase was analyzed using the distortion index Δ as a factor of merit. The values obtained for Δ in all compositions showed that cordierite tended to a much-ordered structure with increased sintering temperatures.     

Synthesis of bone-like structured foams

Here we present a processing route to produce multi-structured ceramic foams based on the combination of particle-stabilized foams with polymeric sponges to produce positive and negative templating structures. Polyester sponges are infiltrated with freshly produced calcium aluminate–alumina foams and upon sintering either positive templating structures are produced when wetting the sponges, or negative templating foams with a percolating pore network are obtained when completely filling the sponges. Additionally, by combining different layers of these particle-stabilized foam infiltrated sponges, various different structures can be produced, including sandwich structures, pore size gradients, and ceramic bone-like structures applying to different types of bone. The particle-stabilized foams used were in situ self-hardening calcium aluminate cement enriched alumina foams to obtain crack-free samples with pore interconnections and tailorable pore sizes.