利用废弃陶瓷材料制备莫来石轻质材料

为了回收利用废弃陶瓷材料,节约资源,以废弃陶瓷材料为主要原料,加入不同量的黏土(质量分数分别为15%、25%、35%),外加锯末和结合剂,经混料、成型、烘干后,1 200、1 250、1 300、1 350、1 400℃保温3 h热处理,然后检测试样的物理性能,并进行了物相和显微结构分析。结果表明,当废弃陶瓷材料与黏土的质量比为85 15,烧成温度为1 400℃时,试样的综合性能最优;由于热处理过程中发生了莫来石化,试样中的主要物相为莫来石;1 400℃热处理后试样的孔隙直径比1 200℃的大,基质结构也更加致密,由K2O、SiO2、Al2O3组成的液相也较多,因而使材料的强度增大。     

Synthesis of high-performance mullite ceramics based on associated rare-earth kaolin

The objective of this work was to prepare high-purity, high-strength mullite ceramics from low-cost, associated rare-earth kaolin (AREK). A reaction sintering process using calcined AREK and γ-Al₂O₃ powders was used to synthesize high-performance mullite ceramics. Mineralogical, morphological, and chemical characteristics of AREK were given. The effects of associated REEs in kaolin and sintering temperature on the microstructural evolution, phase transformation, and physical properties of mullite were studied. The results showed that the mullite contents were 98.8%, the maximum aspect ratio was 8.22 μm, the relative density was 93.04%, and the micro-Vickers hardness and flexural strength were 10.63 GPa and 184.24 MPa, after sintering at 1500°C for 4 h. For comparison, calcined without rare-earth kaolin was also employed as a raw material to synthesize mullite ceramics, and the mullite content prepared by sintering the two kaolin clays at 1320–1480°C for 4 h was quite similar. However, mullite prepared using AREK forms secondary mullite in the temperature range of 1480–1500°C with a significantly higher mullite content, and therefore, the advantages of preparing mullite based on AREK as the raw material are high purity, low mullitization temperature, and high strength.     

Phase formation,microstructure development,and mechanical properties of kaolin-based mullite ceramics added with Fe2O3

The effects of Fe₂O₃ on phase evolution, density, microstructural development, and mechanical properties of mullite ceramics from kaolin and alumina were systematically studied. X-ray diffraction results suggested that the ceramics consisted of mullite, sillimanite, and corundum, in the sintering range of 1450°C–1580°C. However, as the sintering was raised to 1580°C, mullite is the main phase with a content of 94%, and the corundum phase content is 5.9%. Simultaneously, high-temperature sintering had a positive effect on the densification of the mullite ceramics, where both the bulk density and flexural strength could be optimized by adjusting the content of Fe₂O₃. It was found that 6 wt% Fe₂O₃ was optimal for the formation of rod-shaped mullite after sintering at 1550°C for 3 h. The sample's maximum bulk density was 2.84 g/cm³, with a flexural strength of 112 MPa. Meanwhile, rod-shaped mullite grains with an aspect ratio of ~9 were formed. As a result, a dense network structure was developed, thus leading to mullite ceramics with excellent mechanical properties. The effect of Fe₂O₃ on the properties might be attributed to the fact that Al³⁺ ions in the [AlO₆] octahedron were replaced by Fe³⁺ ions, resulting in lattice distortion.     

Improved mechanical properties and toughening mechanism of mullite ceramics reinforced by introducing Ti3AlC2 particles

Ti₃AlC₂, as a toughening phase, was introduced into mullite ceramics for the first time by the pressureless sintering process aiming at improving the mechanical properties. Significant enhancement in density and mechanical performance of mullite ceramics was achieved through the introduction of Ti₃AlC₂ particles. The density of as-prepared mullite–Ti₃AlC₂ composites was increased by 23% (from 2.86 g/cm³ to 3.51 g/cm³) with Ti₃AlC₂ increasing from 0 wt% to 20 wt%. The formation of the liquid phase and decomposed particles from Ti₃AlC₂ are supposed to be responsible for the densification of mullite–Ti₃AlC₂ composites. The optimal mechanical properties were obtained in the mullite–Ti₃AlC₂ composites with 15 wt% Ti₃AlC₂. The bending strength, fracture toughness as well as Vickers hardness were reached 214.36 MPa, 4.84 MPa·m^1/2, and 9.21 GPa, which are 40%, 74%, and 113% higher than pure mullite ceramics, respectively. The improved mechanical performance was mainly attributed to the synergetic action of crack deflection, crack branching and bridging, and strengthened grain boundary.     

Mechanical properties of in situ synthesized mullite-based composite ceramics with three-dimensional network structure

Needle-like nanocrystalline mullite powders were prepared through the molten salt process at the temperature of 900°C using coal gangue as raw material. Then, mullite-based composite ceramics were prepared by a conventional solid-state reaction between in situ synthesized mullite and Al₂O₃ powders. Effects of Al₂O₃ content and sintering temperatures on phase compositions, microstructure, and mechanical properties of the mullite-based composite ceramics were also studied. The results show that mullite content productivity increase from 72% to 95%, as the sintering temperature increased from 1480°C to 1580°C, which led to the improvement in the bulk density and flexural strength of the samples. The three-dimensional interlocking structure for mullite-based composite ceramics was obtained by the in situ solid-state reaction process. The maximum bulk density, flexural strength, and fracture toughness for the sample with 15 wt% Al₂O₃ content are 2.48 g/cm³, 139.79 MPa, and 5.62 MPa··m^1/2, respectively, as it was sintered at the temperature of 1560°C for 3 h. The improved mechanical properties of mullite-based composite ceramics maybe ascribed to good densification and increased mullite phase content, as well as to the in situ three-dimensional network structure. Therefore, the results would provide new ideas for high-value utilization of coal gangue.     

以矾土碎矿和煤矸石合成莫来石均质料

采用Ⅰ等高铝矾土碎矿、Ⅱ等高铝矾土碎矿分别与煤矸石配合,并加入活性Al2O3调整m(Al2O3)/m(SiO2),按照矾土基莫来石均质熟料w(Al2O3)=68%～72%的要求,共配成6个混合料,将混合料湿磨至粒度≤0.044mm以均化化学成分,经成型、干燥后分别在1550℃、1600℃、1650℃和1700℃煅烧3h,冷却后测定其显气孔率和体积密度,以确定它们的烧结温度。结果表明:均质料的烧结温度为1700℃;在1700℃烧结制成的矾土基莫来石均质熟料的Al2O3含量为68%～72%,显气孔率<2.5%,体积密度≥2.75g·cm-3,其莫来石晶体发育良好,构成网络结构。同时,还将部分试样分别在800℃、1000℃、1200℃、1300℃、1400℃、1500℃、1600℃、1650℃和1700℃保温3h,测量其烧后线收缩率和显气孔率,并用XRD分析其相组成,据此分析试样在不同温度下所发生的反应。结果表明,试样在1000～1700℃加热过程中的变化可分为3个阶段:1000～1200℃的一次莫来石形成阶段,1200～1500℃的二次莫来石化阶段,以及1500～1700℃的液相烧结阶段。     

高铝煤矸石铝硅分级提取实验研究

分级研究了热活化条件下高铝煤矸石在盐酸和氢氧化钠溶液中的铝硅溶出行为。采用X射线衍射仪（XRD）、扫描电镜（SEM）和比表面积测定仪（BET）对煤矸石试样做了表征分析。通过正交实验分析了反应温度、反应时间、初始酸碱浓度和固液比对热活化处理后高铝煤矸石中Al2O3和酸浸渣SiO2溶出率的影响。结果表明：酸浸溶出Al2O3反应过程中,固液质量比和酸浸时间对溶出率的影响最为显著,酸浸过程的最优工艺条件：初始盐酸质量分数为20%、酸浸温度为90 ℃、酸浸时间为2.5 h、固液质量比为1∶6,在此条件下,Al2O3的浸取率达82.95%;强碱溶解酸浸渣溶出SiO2反应过程最优工艺条件：碱溶温度为95 ℃、碱溶时间为2.0 h、NaOH质量分数为20%、固液质量比为1∶10,在此条件下SiO2溶出率为69.74%,碱溶温度和碱液浓度对溶出率的影响最为显著。     

选煤厂矸石外排清洁生产技术研究与应用

矸石是采煤和选煤过程中排放的固体废物,济三煤矿产生的矸石由汽车向矿外排放,给矿井的安全生产、清洁生产带来较大危害,另外由于汽柴油价格上涨,工程汽车维修费用高,汽车排矸提高了矿井的生产成本。为此提出了安装大型齿辊式破碎机,取消大块矸石手选,修建矸石外排输送带,将各排矸点的矸石统一集中向矿外排放的解决方案。新方案实施后,不但可以取消手选,降低职工劳动强度及安全事故率,更可以降低运营成本,实现矿井的清洁生产。     

煅烧高铝煤矸石-矿渣-水玻璃系地聚合物材料的研究

根据地聚合物合成原理，采用煅烧高铝煤矸石-磨细矿渣-水玻璃系合成地聚合物类材料。深入研究了高铝煤矸石-矿渣-水玻璃系统材料的制备、性能的测试评价、水化硬化机理和最优制备工艺参数选择。材料中矿渣对早期强度起主要作用，煅烧高铝煤矸石对后期强度贡献较大。在矿渣和高铝煤矸石质量比处于合理状态时，材料各龄期强度均较优。高铝煤矸石类地聚合物材料的抗压强度随水玻璃模数的减小而增大，随水玻璃掺量的增大而增大，随液胶比的减小而增大。水玻璃模数为1．049，矿渣与煅烧高铝煤矸石的配比为4：6，激发剂掺量为22％，液胶比为0．35时，复合材料28d抗压强度达到了41．7MPa。     

Fabrication and application of porous materials made from coal gangue: A review

Coal gangue (CG), which is mainly generated during coal excavation, mining, and coal washing, is an industrial solid waste that is recognized as an environmental pollutant. The ever-increasing amount of CG produced is a serious threat to the ecological environment and property safety, especially in China, which is the largest coal producer and consumer in the world. Considerable studies have investigated means for utilizing CG worldwide. This review summarizes and discusses various porous inorganic materials made from CG, including cement-based porous materials, porous bricks, porous ceramics (cordierite and mullite) and glasses, porous geopolymers, zeolites, aerogels, and porous carbon materials. Different preparation processes and performances of each type of porous inorganic materials were reviewed. Porous CG-based materials can be used as promising adsorbents for the removal of various pollutants and have good potential for use in construction industry as well as catalyst material applications. Besides, porous materials obtained from CG have also been tested as slow-release fertilizers after the absorption of phosphate, as electrode materials, and as oil-in-water separation agents. The systematic summary of porous materials based on CG aims at promoting high-value-added applications for this waste. Future research directions for the use of CG as a raw material are also presented.     

Synthesis and application evaluation in lithium battery furnace of mullite insulating refractory bricks from tailings

In order to realize efficient and comprehensive utilization of kyanite tailings (KT) mullite insulating firebrick (M-IFB) with high strength and low thermal conductivity with spherical-low connectivity porous were success fully prepared by using KT and alumina as the main raw material. Control of the porosity and properties of mullite insulating firebrick can be easily and accurately achieved by adjusting the heat treatment temperature and the amount of forming agent. The compressive strengths, bulk density, thermal conductivities, liner change, and porosities ranged from 25.86–53.26 MPa, .58–1.61 g/cm³, .236–.599 W/(m·K), −1.01 to −.426 % and 66.89 to 78.63 %, respectively. The creep rate of M-IFB was compared with that of current insulating bricks after them used in the baking kiln of lithium ion battery cathode materials in the laboratory to simulate the environment. The results show that the M-IFB corrosion resistance was obviously superior to the current insulation bricks. The high porosity high strength mullite insulating firebrick prepared by this method is expected to be used in thermal insulation system of kiln to realize the comprehensive utilization of solid waste.     

Transient liquid phase diffusion process for porous mullite ceramics with excellent mechanical properties

Porous mullite ceramics were fabricated by the transient liquid phase diffusion process, using quartz and fly-ash floating bead (FABA) particles and corundum fines as starting materials. The effects of sintering temperatures on the evolution of phase composition and microstructure, linear shrinkage, porosity and compressive strength of ceramics were investigated. It is found that a large amount of quartz and FABA particles can be transformed into SiO₂-rich liquid phase during the sintering process, and the liquid phase is transient in the Al₂O₃-SiO₂ system, which can accelerate the mullitization rate and promote the growth of mullite grains. A large number of closed pores in the mullite ceramics are formed due to the transient liquid phase diffusion at elevated temperatures. The porous mullite ceramics with high closed porosity (about 30%) and excellent compressive strength (maximum 105?MPa) have been obtained after fried at 1700?°C.     

用煤矸石代黏土配料时矿化剂的选择与最佳掺量的研究

采用正交试验法研究了以煤矸石代替黏土烧制水泥熟料时矿化剂的选择及最佳掺量问题。借助SEM、物理检验等测试手段,对熟料的矿物组成、显微结构和物理性能进行了分析。结果表明,煅烧该类水泥熟料时,较为理想的矿化剂是单掺P2O5,其最佳掺量约为生料的0.3%。     

Out-of-plane mechanical characterization of acicular mullite and aluminum titanate diesel particulate filters

This study characterizes the flexural and compressive behavior of two porous ceramic honeycombs commonly used in diesel particulate filtration, acicular mullite and aluminum titanate. Compression along the axis normal to the honeycomb cross-section, referred to as out-of-plane compression, is compared to in-plane flexure. The relationship between these loading modes is assessed using the failure strength and elastic modulus of the honeycomb structure and the constituent wall material. Weibull analyzes showed that flexure and out-of-plane compression exhibit similar behavior in cases where failure is governed by a single flaw, such as in acicular mullite. However, in heavily microcracked systems like aluminum titanate, compressive failure occurs by damage accumulation rather than growth of a single flaw, so compressive failure strengths are higher than flexural ones. Buckling was also shown to occur in both systems, but the geometries required are unlikely to be encountered in practical application. In the context of filter life assessment, failure in flexure occurs at much lower stresses for systems that rely on microcracking to accommodate thermal strains, so flexure is better suited as an estimate of filter strength.     

Effects of micro-sized mullite on cristobalite crystallization and properties of silica-based ceramic cores

Silica-based ceramic cores are extensively used in investment casting process, during which they must exhibit sufficient flexural strength and deformation resistance. In this study, micro-sized mullite was used as an additive to silica-based ceramic cores to optimize their high temperature properties. To investigate the effects of micro-sized mullite on cristobalite crystallization, mechanical and thermal properties of silica-based ceramic cores, ceramic cores with different amounts of micro-sized mullite were fabricated. The XRD results showed that additional micro-sized mullite diminished the crystallization of cristobalite at high temperatures, primarily caused by the mullite related compressive stresses on the surface regions of fused silica particles. Three-point bending tests and SEM results showed that micro-sized mullite had a more significant effect on the flexural strength of ceramic cores compared with conventional additives. Particularly, the fracture mechanism of silica-based ceramic cores had been changed from intergranular fracture into a mixed fracture consisting of both intergranular and transgranular fracture. The mechanical and thermal properties of ceramic cores were all reduced slightly as the mullite content exceed 4.6 wt%. Hence, to optimize the properties of silica-based ceramic cores, the micro-sized mullite content should not exceed 4.6 wt%.     

Mineralogical and dielectric properties of mullite and cordierite ceramics produced using wastes

In this work technical ceramics containing industrial inorganic wastes was carried out. Ceramic formulations prepared with clay, magnesium oxide and residues of kaolin and alumina as raw materials, were formed in a disk-shaped specimens using the uniaxial pressing process and sintering at temperatures from 950°C to 1400°C. The mineralogical, physical and dielectric characteristics of the fired samples were investigated. The dielectric properties, the relative dielectric constant (ε_r) and the loss tangent (tan δ) were evaluated at frequencies of 0.1, 1, 10, and 100?kHz at room temperature. Mullite and cordierite were present as major phases at the highest temperatures. Relative dielectric constant values closest to that of mullite (ε_r = ~ 5 to ~ 6) and cordierite (ε_r =?~ 4 to ~ 6) at 1?kHz. On the other hand, the lowest dielectric losses (tan δ ~ 0.06 to ~ 0.04) were observed for the formulations containing the mullite major phase, and tan δ ~ 0.009 to ~ 0.003 for formulations that showed cordierite as main phase. It was verified that an increase in temperature promoted a reduction of porosity, a property that had a direct influence on the dielectric properties of the formulations. The materials obtained from the residues presented low dielectric constants and loss tangents, which make them suitable for use in electrical and electronic systems.     

Influences of mullite fibers on mechanical and thermal properties of silica-based ceramic cores

Mullite fibers composite silica-based ceramic cores were successfully prepared by injection molding. The effects of mullite fibers on the mechanical and thermal properties of ceramic cores were investigated. The results indicated that the linear shrinkage was significantly decreased and the porosity was gradually increased with the increase of mullite fibers. In addition, the flexural strength for the room temperature and the simulated casting temperature of 1500°C was increased to a maximum value when the content of mullite fibers was about 1 wt.%, and then decreased with the increase of mullite fibers. The mullite fibers of 1 wt.% presented excellent mechanical properties with a linear shrinkage of .65%, a porosity of 6.96%, and a flexural strength of 17 MPa at room temperature and 34.83 MPa at the simulated casting temperature of 1500°C. Besides, the change in microstructure and properties in various contents of mullite fibers were analyzed.     

Microscopic regulation of plant morphological pores on mechanical properties of porous mullite materials

Generally, a multilayer structure is present inside a walnut shell, and the residual structure of the walnut shell is retained after impregnation and firing. When the walnut shell is used as a pore-forming agent, this structure helps in improving the mechanical and thermal insulation properties of the lightweight porous materials. In this study, porous mullite materials (PMMs) with plant morphological structure pores were prepared using a-Al₂O₃ and silica powder as the raw materials with addition of sol-impregnated walnut shell powder (WSP). The influence of sol type and firing temperature on the pore structure of the PMMs was analyzed, which affected the compressive strength and thermal conductivity. The plant morphological porous structure was observed in the samples after sol impregnation. After firing at different temperatures, the porous structure gradually contracted and supported the pores, improving the mechanical properties, while the complex porous structure increased the heat conduction path, thereby improving the insulation performance. Using WSP impregnated with silica-sol and zirconia-sol as pore-forming agents, PMMs with higher compressive strength and relatively low thermal conductivity (TC) were prepared.     

煤矸石和赤泥协同提取氧化铝过程矿相转变研究

开展了煤矸石和赤泥协同提取氧化铝研究，考察了添加赤泥对煤矸石活化提取氧化铝及对助剂碳酸钠消耗量的影响，并利用TG-DSC和XRD研究了赤泥添加对煤矸石活化过程的影响。结果表明，“煤矸石-赤泥-Na₂CO₃”混合样中氧化铝的溶出率随Na/Al摩尔比和煅烧温度的增加而增加，在Al/Si摩尔比为1的条件下，当Na/Al摩尔比为1.2、煅烧温度为850℃时，混合样的氧化铝溶出率可达到91.7%，与碳酸钠直接活化煤矸石相比，碳酸钠消耗量可降低77.9%。TG-DSC和XRD的结果表明，煤矸石、赤泥以及碳酸钠在低于700℃时相互作用比较弱，在高于800℃时三者发生相互作用，赤泥的加入由于调整了样品中的Al/Si摩尔比，使反应的最终物相选择性地向Na∶Al∶Si摩尔比为1∶1∶1的霞石和沸石相转化。     

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.