莫来石基陶瓷复合材料的力学性能

采用热压工艺制得致密的莫来石陶瓷和莫来石基陶瓷复合材料(ZTM、SiC晶须-莫来石、SiC晶须-ZTM)。通过引入SiC晶须或ZrO_2,使莫来石基陶瓷的力学性能有明显改善,SiC晶须和ZrO_2复合强韧则效果更为显著。组成为20vol.％SiC晶须-15vol.％ZrO_2-莫来石陶瓷材料,其室温及800℃的抗弯强度和断裂韧性分别为559MPa及425MPa,7.5MPa·m~(1/2)及7.4MPa·m~(1/2)。实验结果表明,莫来石基复合材料的相变增韧与晶须增韧机制的作用对韧性的贡献有良好的加和性。     

柱状自生长莫来石的制备及显微结构

通过对莫来石材料的分析,设计了在莫来石先质中添加ＡｌＦ３进行密封条件下热处理,生成莫来石晶须晶种,并以其作为生长点,在以后的烧结过程中发育成为柱状颗粒,获得类昌须复合材料的显微结构的实验线路,含ＡｌＦ３莫来石先质试样密闭处理的温度条件是１１５０℃,大于这个温度处理的试样无法获得致密烧结。莫来石柱状生长条件是富铝莫来石晶粒的存在和液相的产生。本工作中经１１５０℃处理后的试样获得良好的烧结密度,材料的     

原位反应合成多孔莫来石质支撑体及其显微结构

采用粉煤灰、烧铝矾七和球黏土为原料,通过原位反应烧结合成球形多孔莫来石质支撑体.考察了烧结温度对多孔莫来石质支撑体相转变、晶粒尺寸、孔径分布和气孔率的影响,并对其莫来石化的机理进行了探讨.研究表明:在1 300℃烧结温度下,二次莫来石在硅铝酸盐液相中通过溶解-沉淀机制开始成核,并于1 400℃烧结发育成针状的晶粒;当烧结温度升至1 500℃时,溶解在液相中的莫来石进行结构调整和生长,并最终在1 550℃发生原位反应并形成刚性交错网络结构的柱状莫来石.在低温(<1 400℃)烧结阶段,二次莫来石的成核和生长引起体积膨胀,导致气孔率随温度的升高而增大;在高温(≥1 500℃)烧结阶段,大量玻璃相的存在使液相烧结占主导,气孔率因体积收缩呈下降趋势.支撑体的平均孔径随烧结温度的升高而增大,其原因是在高温烧结时莫来石生长消耗过多的SiO2使大量微孔联接形成大孔.     

玉米淀粉造孔剂对富铝煤矸石合成轻质莫来石料的影响

为了综合利用煤矸石,以天然富铝煤矸石矿为原料,聚乙烯醇(PVA)为结合剂,玉米淀粉为造孔剂,于1 500℃保温3 h反应烧结合成轻质莫来石料,研究了造孔剂加入量(其质量分数分别为10%、20%、30%、40%、50%)对轻质莫来石烧结性能以及显微结构的影响。结果表明:随着玉米淀粉加入量的增大,合成的轻质莫来石料体积密度明显降低,显气孔率和线收缩率显著增大,玉米淀粉的添加量以40%(w)为宜,此时合成的轻质莫来石料的体积密度和显气孔率分别为1.21 g·cm-3和62%;合成的轻质莫来石料的主晶相为莫来石,次晶相为刚玉,莫来石晶体呈柱状发育,刚玉晶粒被莫来石晶粒包裹,构成了疏松的空间网络结构。     

Al2O3微粉和SiO2微粉对刚玉-莫来石材料性能的影响

在板状刚玉细粉中添加粘土或Al2O3微粉和不同种类的SiO2微粉制成刚玉-莫来石试样,分别于1200℃、1400℃和1600℃保温5 h烧成后,测定试样的体积密度、显气孔率和烧后线收缩率,利用XRD分析了试样在不同温度段的莫来石生成量,研究了添加Al2O3微粉和不同种类的SiO2微粉对材料的烧结性能和莫来石化的影响,并利用SEM观察了试样的显微结构.结果表明(1)加入Al2O3微粉和SiO2微粉均有利于材料的烧结;加入SiO2微粉的纯度和晶形不同,对试样莫来石化的影响也不同,无定形态SiO2微粉(即硅灰)的纯度越高,试样的莫来石生成量也越高.(2)加粘土的试样,其显微结构中柱状莫来石的晶体特征比较明显;而加入SiO2微粉的试样,其莫来石晶体和刚玉晶体相互交错,晶粒较小.     

Sm2O3掺杂对纳米莫来石前驱粉体微观结构和烧结性能的影响

为了改善纳米莫来石粉体烧结性能,以硫酸铝和硅酸钠为主要合成原料,添加不同含量Sm2O3,采用共沉淀工艺制备莫来石前驱粉体,经过煅烧得到莫来石纳米粉体,研究了Sm2O3掺杂量对莫来石粉体微观结构和烧结性能的影响.研究表明:当Sm2O3的加入量为4wt%时,合成温度可由传统的1300 ℃左右降低至1000 ℃,晶粒尺寸约为39 nm,比表面积达到95.265 m2/g.说明适当掺杂Sm3+对于合成纳米莫来石具有改善微观结构,促进烧结,促进莫来石晶相形成的作用.     

溶胶-凝胶法制备多晶莫来石连续纤维

以无水氯化铝、铝粉、正硅酸乙酯(TEOS)为原料,通过溶胶-凝胶法合成了双相莫来石溶胶,采用离心纺丝法制备了多晶莫来石连续纤维.结果表明,前驱体溶胶具有良好的纺丝性和稳定性.凝胶纤维1100℃热处理2h,由无定型态转变成γ-Al2O3相,1300℃纤维莫来石化.1400℃烧结后,纤维表面光滑、直径均匀.随着热处理温度的提高,晶粒逐渐长大.     

ZTM材料低温时效处理的研究

通过对ZrO2增韧莫来石陶瓷（TM）低温时效现象的研究,发现材料表面及内部存在的微裂纹是导致材料在200－300℃时效处理后力学性能下降的重要原因。在500－600℃时效处理,材料力学性能提高主要源于可相变t-ZrO2相对含量增加和由逆马氏体相变（counter-martensitic transformation)引起的体积收缩使部分应力得以释放。降低烧结体中 t-ZrO2晶粒尺寸或提高稳定剂Y2O3含量可有效抑制ZTM材料在低温时效处理时的性能退化现象。     

煅烧温度对莫来石质多孔陶瓷材料结构与性能的影响

以粉煤灰漂珠和α-Al2O3粉为原料,AlF3和V2O5作为添加剂,采用挤制成型工艺与无压烧结技术制备了莫来石质多孔陶瓷材料,研究了煅烧温度(分别为1100℃、1200℃、1300℃、1350℃)对试样的物相组成、莫来石质多孔陶瓷的显微结构以及性能的影响,并阐述了粉煤灰漂珠球体表面形成莫来石的机理过程。采用X射线衍射仪(XRD)、场发射扫描电子显微镜(SEM)和力学性能测定等手段表征了制备的莫来石质多孔陶瓷材料。结果表明:煅烧温度的提高有助于针状莫来石晶体的形成,莫来石晶体依托漂珠球壳生长;当煅烧温度从1100℃增加至1350℃,试样中的气孔率先增大后减小,而体积密度和抗压强度则先减小后增大;经1300℃烧制的试样综合性能较佳,气孔率为72.8%,体积密度为0.83 g·cm-3,抗压强度为15.4 MPa。这为固体废弃物粉煤灰漂珠的资源化应用以及多孔隙的莫来石质陶瓷材料的制备提供了新的研究思路。     

氟化铝对红柱石莫来石化的影响

本文主要研究了氟化铝的加入对红柱石矿物转化为莫来石的温度,转化程度以及生成相莫来石的形态的影响.结果表明,加入6wt％氟化铝可以使红柱石矿物在1300℃完全莫来石化;同时氟化铝的加入可以促进莫来石晶体各向异性生长,得到直径为0.5～2.0 μm,长径比为20～40的莫来石晶须,可以用于制备自增韧的莫来石陶瓷或莫来石晶须增强的复合材料.     

SiC/ZTM Nanocomposite with Needlelike Mullite Grains and Enhanced Mechanical Properties

Zirconia-toughened mullite (SiC/ZTM) nanocomposites were prepared by a chemical precipitation method. The samples showed good sinterability and could be densified to >98.7% of the theoretical density at 1350°–1550°C. Because of the addition of mullite seeds in the starting powder and the pinning effects of ZrO₂ and SiC particles on mullite grain growth, a fine-grained microstructure formed. Mullite grains were generally equiaxed for the sample sintered at 1400°C; whereas, for the sample sintered at 1550°C, most mullite grains took a needlelike morphology, and SiC particles were primarily located within mullite grains. The strength and toughness increased with the increasing sintering temperature, and reached their respective maximum of 780 MPa and 3.7 MPa·m^1/2 for the sample sintered at 1550°C.     

常压烧结莫来石／氧化锆／碳化硅复相陶瓷的研究

本文对莫来石／氧化锆／碳化硅复相陶瓷进行了Ｎ２气氛中常压烧结的研究。实验结果表明：ＳｉＣ粒子添加量≤２０ｖｏｌ％，材料均可致密烧结并可获得均匀的微观结构。ＳｉＣ粒子的加入使材料人力学性能较莫来石／氧化锆陶瓷有明显的提高，并在ＳｉＣ含量为１０ｖｏｌ％时达到峰值，室温强度和断裂韧性分别为６０１ＭＰａ和５．８ＭＰａ＾Ｃ２，接近热压材料。     

Development of Textured Mullite by Templated Grain Growth

Highly textured mullite was obtained by enhancing anisotropic grain growth by TiO₂ doping and by templating grain growth on oriented acicular mullite seed particles in a mullite precursor. Upon heating, the mullite precursor crystallized and densified to an equiaxed microstructure of 1-2 µm mullite grains at which time the mullite seed particles grew rapidly in the length direction ( c -axis) to produce a highly textured microstructure. By changing the seed (template) particle concentration, a range of oriented microstructures and anisotropic grains could be produced.     

Al2O3对ZTM陶瓷结构与性能的影响

本文研究了氧化铝对ZTM陶瓷结构和性能的影响.发现在烧结过程中,氧化铝可固溶于莫来石颗粒形成富铝型柱状莫来石,产生的体积膨胀增强了基质对氧化锆颗粒的约束,使材料中的四方氧化锆相对含量增加,其强韧化效果进一步发挥,明显改善了材料的力学性能.     

Al2O3在莫来石中固溶对ZTM/Al2O3陶瓷结构与性能的影响

研究了加入氧化铝对ZTM陶瓷结构和性能的影响.发现在烧结过程,氧化铝可固溶于莫来石颗粒形成富铝型柱状莫来石,并因其产生的体积膨胀增强了基质对氧化锆颗粒的约束,使材料中的四方氧化锆相对含量增加,其强韧化效果进一步发挥,明显改善了材料的力学性能.     

Sintering and Mechanical Properties of Yttria-Doped Tetragonal ZrO2 Polycrystal/Mullite Composites

Yttria-doped tetragonal ZrO₂ polycrystal (Y-TZP)lmullite composites were sintered at 1450° to 1500°C in air to disperse rodlike mullite grains at the grain boundary of Y-TZP and the mechanical and thermal properties were investigated. The aspect ratios of mullite grain were >2. High fracture strength of 1000 MPa and fracture toughness of 12 MPa·m^1/2 were obtained by dispersing <20 vol% of mullite into Y-TZP. The thermal expansion coefficient of Y-TZP/mullite composites decreased with increasing mullite content. The thermal shock resistance of Y-TZP was greatly improved by dispersion of rodlike mullite grains.     

Wetting and Joining of Mullite Ceramics by Active-Metal Braze Alloys

Mullite and ZrO₂-toughened mullite (ZTM) were joined with Ag─Cu eutectic braze alloys that contain Ti or Zr as active elements. Although neither the alloy compositions nor the processing conditions were optimized, four-point bend strengths of joined bars were as high as 108 MPa. Joining reactions were studied by conducting separate sessile drop experiments with molten Ti─Ag─Cu and Zr─Ag─Cu alloys on mullite for times and temperatures that were similar those used for joining. Detailed compositional and microstructural analyses of those metal–ceramic interfaces revealed a complex reaction zone in which the oxide of the active element was a principal reaction product. Compared with the Ti-containing alloys, those with Zr were more refractory, they were less reactive with the mullite, and the Zr did not segregate as completely to the interface during heating.     

Anisotropic Grain Growth in Diphasic-Gel-Derived Titania-Doped Mullite

Densification and anisotropic grain growth in diphasic-gel-derived, titania-doped mullite were studied. Titania enhanced initial and intermediate stage densification in diphasic mullite gels by reducing the glass viscosity. Rodlike anisotropic mullite grains started to grow in titania-doped diphasic mullite gels once a dense, equiaxed microstructure was achieved. The onset temperature for anisotropic grain growth decreased with increasing titania concentration because the sintering temperature for final-stage densification decreased. The lowest onset temperature for anisotropic grain growth was ∼1500°C in 5 wt% titania-doped mullite. The aspect ratio and area fraction of anisotropic mullite grains increased with higher titania concentration and were strongly dependent on the initial titania particle size. Kinetic studies demonstrated that anisotropic grain growth in titania-doped diphasic mullite gels followed the empirical equation Gⁿ - G ₀ ⁿ = Kt , with growth exponents of 3 and 6 for the length [001] and thickness [110] directions, respectively. The activation energies for grain growth were 690 kJ/mol for the length and 790 kJ/mol for the thickness directions.     

Sintering and Microstructure of Mullite Aerogels

Mullite (3Al₂O₃·2SiO₂) was prepared by a sol-gel process and dried by supercritical extraction with CO₂. The aerogel (<0.05 of the theoretical density of mullite) experienced a shrinkage of up to 0.6 and reached a density of only ∼0.5 of theoretical after 1 h at 1350°C Mechanically compacted aerogels, however, sintered to nearly theoretical density below 1200°C. This density is somewhat higher than those of gels prepared by conventional drying (i.e., exposure to the atmosphere) and is considerably higher than mullite prepared from mixed powders at higher temperatures. Although the X-ray diffraction pattern of the sintered gels was almost identical to that of mullite, transmission electron microscopy and energy-dispersive microanalysis showed two types of grain structure. Elongated grains with an Al/Si atomic ratio corresponding to that of stoichiometric mullite were surrounded by equiaxed grains with a lower Al/Si ratio.     

Development of mullite fibers and novel zirconia-toughened mullite fibers for high temperature applications

Polycrystalline mullite fibers and novel zirconia-toughened mullite (ZTM) fibers with average diameters between 9.7 and 10.3 μm containing 3, 7 and 15 wt.-% tetragonal ZrO₂ (ZTM3, ZTM7, ZTM15) in the final ceramic were prepared via dry spinning followed by continuous calcination and sintering in air. A shift in the formation of transient alumina phases and tetragonal ZrO₂ to higher temperatures with increasing amounts of ZrO₂ was observed. Concomitantly, the mullite formation temperature was lowered to 1229 °C for ZTM15 fibers. X-ray diffraction revealed formation of the desired tetragonal crystal structure of ZrO₂ directly from the amorphous precursor. Room temperature Weibull strengths of 1320, 1390 and 1740 MPa and Weibull moduli of 9.5, 7.1 and 9.0 were determined for mullite, ZTM3 and ZTM15 fibers, respectively. Average Young’s moduli ranged from 190 to 220 GPa. SEM images revealed crack-free fiber surfaces and compact microstructures independent of the amount of ZrO₂.