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.     

Properties of sintered mullite and cordierite pressed bodies manufactured using Al-rich anodising sludge

Mullite and cordierite based refractory ceramic materials were produced from formulations based on an industrial Al-rich sludge derived from the wastewater treatment of the aluminium anodising process. Some common ceramic raw materials, like ball clay, kaolin, diatomite and talc, were also added. Cylindrical samples processed by uniaxial dry pressing were sintered at different temperatures (between 1300 and 1650 °C, 1 h soak at each temperature) to study the ceramic properties.     

锆刚玉莫来石－碳化硅复合材料的显微结构

用热压的方法制备了Ａｌ２Ｏ３／莫来石（３／１）＋１５％ＡｒＯ２十１０％ＳｉＣ四元复合材料。采用ＡＥＭ和ＡＥＭ－ＥＤＳ等研究了材料的显微结构以及品界两侧金属元素的分布，确定了本材料晶界直接结合的三种形式。     

Preparation of mullite ceramic microfilter membranes using Response surface methodology based on central composite design

In this paper effect of free silica removal from mullite microfilter membranes using different sodium hydroxide (NaOH) concentrations at different temperatures and for different removal times was studied. The prepared membranes were subjected to XRD, SEM, porosity analysis, and mechanical strength measurement. Response surface methodology (RSM) based on central composite design (CCD) was used to design the experiments and analyze three operating parameters including; NaOH solution concentration, NaOH solution temperature and removal time. The optimum porosity of 49.4 was obtained with NaOH solution concentration of 35 wt% at temperature 75 °C and removal time equal to 8 h.Water flux and mechanical strength as important characteristics were measured for all the membranes. For the membrane with the optimum porosity, water flux, mechanical strength, and free silica removal percentage were 61.7 kg/m² h, 21.6 MPa, and 28.2%, respectively. The maximum rejection percentage was 97.2% and emulsion flux for this state was 15.6 kg/m² h at temperature 25 °C and cross flow velocity of 1.5 m/s.     

原位生长莫来石棒晶增强钡长石基复合材料

以煤矸石、碳酸钡和氧化铝为原料,按m(BaO)∶m(Al2O3)∶m(SiO2)=13∶57∶30的配比计算并称量原料,外加3%的白糊精,经球磨、混练、困料后,以10 MPa压力压制成36 mm×20 mm圆柱试样,分别在1500℃3 h、1 550℃3 h、1 550℃6 h、1 550℃9 h和1 600℃3 h条件下进行常压烧结,然后测定烧后试样的体积密度和显气孔率,并进行XRD和SEM分析。结果表明:由BaCO3、α-Al2O3和煤矸石粉料,采用固相反应烧结方法可以制备由单斜钡长石、六方钡长石、莫来石和刚玉4种物相组成的莫来石增强钡长石材料;在本试验条件下,提高煅烧温度和延长保温时间,有利于试样致密化程度的提高,莫来石晶相的发育及其交叉网络结构的形成,以及反应物分布的均匀。     

3D printing of porous low-temperature in-situ mullite ceramic using waste rice husk ash-derived silica

The in-situ mullite (3Al₂O₃·2SiO₂) foams are fabricated by 3D printing (direct ink writing (DIW)) technique and utilize waste rice husk ash (RHA). The Al₂O₃-SiO₂ inks are prepared using an aqueous binder with α-alumina and two different silica sources, i.e., RHA extracted biogenic nano-silica (NS) and commercial silica (CS). The ink rheological features are first designed in terms of solid-to-liquid ratio and dispersant, and found that a higher amount of dispersant is needed for functionalization of NS-containing ink than CS (micro-sized) consisting of ink. Secondly, the DIW log-pile structures are fired at different temperatures (1200?1500 °C), and NS containing samples exhibited remarkable enhanced properties at a lower firing temperature than CS. At 1400 °C, alumina and RHA nano-silica entirely transformed into mullite and retained ～75 % porosity, ～8 MPa cold compressive strength, and thermal conductivity ～0.173 W/m·k that designate a simple and effective way to fabricate of mullite foamy structure.     

换热器用针状莫来石增强堇青石陶瓷材料

以耐火粘土、高铝矾土及滑石为原料研制了堇青石基陶瓷材料，并对其组织和性能尤其是抗热震性进行了研究。结果表明，堇青石基体上分布着外状莫来石的材料具有更高的抗热震性。对换热器用陶瓷材料抗热震性参数进行了讨论，指出抗热震损伤多数R''更适合于作为优选陶瓷换热器用材料的指标。     

关于莫来石陶瓷焊补颗粒熔融时间模拟计算的探讨

通过对莫来石陶瓷焊补传热过程剖析,建立了单个喷补颗粒传热过程模型,借助于稳定态传热公式,计算出不同喷补颗粒加热熔融时间,这为莫来石陶瓷焊补颗粒配比及其操作规程的制订提供了重要的理论依据。     

Fabrication and properties of three-directional orthogonal aluminosilicate fiber fabric-reinforced mullite composite

In this study, a three-directional orthogonal aluminosilicate fiber fabric-reinforced mullite composite with excellent properties was prepared by the precursor impregnation and pyrolysis (PIP) method. The influence of the number of PIP cycles on the microstructure and mechanical properties of the composite was studied. The density and mechanical properties of the composite enhanced with increasing number of PIP cycles. After the 6th PIP cycle, the density of the composite increased by only 0.8%, and the flexural strength and fracture toughness of the composite reached 130.1 MPa and 4.91 MPa m^1/2, respectively. Moreover, the thermal shock resistance of the composite was investigated by the high-low temperature (from 1300 °C to room temperature) thermal treatment and water quenching method. The strength retention rate of the composite after 10 high-low temperature thermal cycles was 90.1%; the retention rate dropped to 79.5% after 15 thermal cycles. The composite with the critical thermal shock temperature difference 843.9 °C displayed excellent thermal shock resistance.     

Mullite fiber cloth-reinforced mullite composite fabricated via an optimized layer-by-layer assembly method

This article reports the fabrication of fiber cloth-reinforced mullite composite via an optimized layer-by-layer (LbL) assembly method involving the infiltration and pyrolysis of fiber cloth with mullite precursor (PIP) followed by brushing matrix onto the treated fiber cloth and hot pressing. The influence of fiber content on the microstructure and mechanical properties of composite are investigated and the crack propagation is discussed to explain the toughening mechanisms. The composite with 30?vol% fiber content exhibited a high density 2.89?g/cm³, flexural strength 135.5?MPa and fracture toughness 4.13?MPa?m^1/2. After PIP pretreatment, the gaps existed in the fiber bundle are filled with mullite matrix which transform from mullite precursor, improving the density from 2.89?g/cm³ to 2.94?g/cm³, flexural strength from 135.5?MPa to 163.2?MPa and fracture toughness from 4.13?MPa?m^1/2 to 4.55?MPa?m^1/2. The optimized LbL assembly method realizes the creation of fiber cloth-reinforced mullite composites with high density and excellent mechanical properties.     

莫来石结合刚玉-碳化硅质浇注料的组成与性能

研究了莫来石结合刚玉-碳化硅质浇注料的组成和性能的关系。借助SEM分析了浇注料的显微结构。掺入适当比例的氧化铝微粉和氧化硅微粉,有利于系统中二次莫来石的反应生成,可以改善浇注料的性能。     

Porous mullite blocks with compositions containing kaolin and alumina waste

In the production of alumina by the Bayer process, the calcination step generates a waste containing ~90% aluminum oxide (Al₂O₃). Due to the high content of this oxide, this waste can be used as a source of alumina in porcelain formulations, especially those used in the synthesis of mullite. The purpose of this study was to produce porous mullite blocks using compositions containing kaolin and alumina waste. The compositions were formulated based on a mullite stoichiometry of 3:2. Heat treatments were carried out in a conventional furnace at temperatures of 1450 to 1500 °C, applying a heating rate of 5 °C/min and a 1-h hold time at the firing temperature threshold. The powders were characterized by means of X-ray fluorescence (XRF); X-ray diffraction (XRD); thermal analysis (TGA-DTA); scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The physic mechanical properties of the test specimens: water absorption, apparent porosity, linear shrinkage and flexural strength were also evaluated. The XRD results revealed the formation of mullite as the major phase. The morphological analysis by SEM revealed typical mullite needles originating from clay minerals. The size of the mullite needles was calculated based on the TEM analysis, which indicated diameters smaller than 400 nm, confirming the nanometric dimensions of the needles. The flexural strength test of the specimens indicated that this parameter ​​tends to increase as the temperature is raised.     

Thermal conductivity in mullite/ZrO2 composite coatings

Mullite-based multilayered structures have been suggested as promising environmental barrier coatings for Si₃N₄ and SiC ceramics. Mullite has been used as bottom layer because its thermal expansion coefficient closely matches those of the Si-based substrates, whereas Y–ZrO₂ has been tried as top layer due to its stability in combustion environments. In addition, mullite/ZrO₂ compositions may work as middle layers to reduce the thermal expansion coefficient mismatch between the ZrO₂ and mullite layers. Present work studies the thermal behaviour of a flame sprayed mullite/ZrO₂ (75/25, v/v) composite coating. The changes in crystallinity, microstructure and thermal conductivity of free-standing coatings heat treated at two different temperatures (1000 and 1300 °C) are comparatively discussed. The as-sprayed and 1000 °C treated coatings showed an almost constant thermal conductivity (K) of 1.5 W m⁻¹ K⁻¹. The K of the 1300 °C treated specimen increased up to twice due to the extensive mullite crystallization without any cracking.     

Effect of dispersants on the rheology of aqueous silicon carbide suspensions

The effect of cationic and anionic dispersants on aqueous suspensions of as-received and surface-modified silicon carbide particles has been studied via observation of the rheological behaviour. Only the cationic dispersants were effective for the as-received SiC, with polyethyleneimine being superior to Hyamine 2389 probably as a result of a greater electrosteric interaction. SiC particles modified using Al(NO₃)₃ behaved like alumina and so could be dispersed using the anionic dispersants ammonium polyacrylate and polymethacrylate. Such dispersions displayed no heteroaggregation when alumina was added, although the order of mixing could significantly affect the rheological behaviour of the suspension. Nevertheless, the suspensions appeared robust to slight fluctuations in pH.     

Effects of in situ synthesized mullite whiskers on compressive strength of mullite fiber brick

The method of in situ synthesis of mullite whiskers by gas-phase deposition and reaction was applied to improve the compressive strength of the mullite fiber brick. During the preparation process, silica sol, Al(NO₃)₃ solution and NH₄F solution were introduced into the fibrous brick in the form of ions or sol through vacuum impregnation and freeze drying, and the silica sol, Al(NO₃)₃ and NH₄F served as the silica sources, aluminum source and catalyst, respectively. Effects of process parameters (concentration of impregnation solutions, holding time, sintering temperature) on compressive strength and elastic modulus of the fibrous brick during the in situ toughening process were analyzed. SEM and XRD analysis results demonstrated that the mullite whiskers were synthesized on the surface of mullite fibers based on the reaction of AlOF and SiF₄. What is more, the whiskers on adjacent fibers intersected with each other and formed many unfixed lap-jointing points, resulting in the increase of compressive strength and elastic modulus. Although the density and thermal conductivity of the sample after the generation of mullite whiskers fabricated with the optimum process were 0.406 g/cm³ and 0.1262 W/(m K), respectively, which were slightly higher than that of the raw fibrous brick (0.375 g/cm³ density and 0.1069 W/(m K) thermal conductivity, respectively), the corresponding compressive strength and elastic modulus of the sample reinforced with the whiskers increased to 1.45 MPa and 42.03 MPa, respectively, which were much higher than that of the raw fibrous brick (0.39 MPa compressive strength and 6.5 MPa elastic modulus).     

Joining of mullite ceramics with yttrium aluminosilicate glass interlayers

Pellets of yttrium aluminosilicate glass (Y₂O₃:Al₂O₃:SiO₂ = 30:20:50 mol%) powder were used as the filler interlayers (0.4 mm thick) to join two mullite substrates. The glass interlayer partially melted at joining temperature to bond the substrates and then crystallized during cooling to have better bonding strength. The results showed that joining could be performed at 1390–1420 °C for 1–5 h with applied pressure of 0.02 MPa. After joining, the thickness of glass layers varied between 250 μm and 80 μm, depending upon the temperatures. The glass interlayer crystallized into cristobalite, mullite and Y₂Si₂O₇. When joining mullite/3 mol%yttria–zirconia substrates using the same glass pellet, a layer of zircon/mullite was formed at the interface, indicating that reaction occurred between glass and substrates. The formation of zircon usually accompanied with cracks in the substrates. These cracks deteriorated the strength. The achievable three-point bending strengths were 139 MPa for joined mullite and 76 MPa for joined mullite/3 mol%yttria–zirconia.     

Development of cordierite/mullite composites using industrial wastes

Ceramics containing cordierite and mullite as their principal phases are promising for many applications, due to properties such as a low coefficient of thermal expansion, high durability, low dielectric constant, resistance to thermal shock, and refractoriness. The objective of this study was to produce ceramic composites suitable for use as refractory materials. The raw materials were subjected to chemical characterization and the formulations to physical, chemical, and mineralogical characterization. The specimens were formed by pressing, dried at 110°C, and sintered from 1150°C to 1300°C for 2 hours. The following properties were then determined: linear shrinkage, water absorption, apparent porosity, and flexural modulus of rupture. The phases formed, crystal morphology, and coefficient of thermal expansion were evaluated. The cordierite and mullite phases were observed in all formulations at 1250°C and 1300°C. The results obtained from the formulations with a higher content of fine kaolin residue suggest that these formulations have the potential to be used for the manufacture of refractory materials such as furnace rollers and supports.     

Low-temperature reaction-sintering of mullite ceramics with an Y2O3 addition

Mullite ceramics were fabricated at relatively low temperatures from powder mixtures of -Al₂O₃ and quartz, with an Y₂O₃ addition. The mullitization process was analyzed by X-ray diffraction. The densification behavior was investigated as a function of the Y₂O₃ content, sintering temperature and holding time as well as mullite seeds. It has been shown that mullitization occurs via a nucleation and growth mechanism within an yttrious aluminosilicate glass, but lattice and grain-boundary diffusion becomes important during the densification process. Moreover, the incorporation of mullite seeds was observed to enhance both mullitization and densification. At 1400°C for 5 h or 1450°C for 2 h, 15 mol% Y₂O₃-doped and 5 mol% mullite-seeded specimens can be sintered to almost full density.     

Silicon carbide whiskers reinforced SiOC ceramics through digital light processing 3D printing technology

Polymer derived silicon oxycarbide ceramic materials and silicon carbide whiskers reinforced ceramic composite are prepared through digital light processing (DLP) 3D printing technology in the present work. A new type of UV-curable preceramic polymer is firstly synthesized and then two types of photopolymer resins with and without SiC whiskers as reinforcement are prepared. Due to the high curing rate and good fluidity of the resins, they are applied in DLP 3D printing and various 3D objects with complicated structures and high printing resolution have been printed. The derived ceramic materials show amorphous microstructure and there is no apparent porosity and cracking throughout the whole sample surface of the ceramic materials and the SiC whiskers are uniformly embedded in the ceramic matrix and remain intact and unaffected during the pyrolysis process. The SiC whiskers reduced the shrinkage and mass loss. More importantly, it significantly improves the mechanical performance of the derived ceramic materials in which the compressive strength increases from 77.5 ± 10.2 MPa to 98.4 ± 12.3 MPa. Benefiting from the easiness of the fabrication, high printing resolution and excellent mechanical performance, the derived ceramic materials have great potential applications in various areas.