超细莫来石粉末的成型与生坯特性

采用水解－沉淀法制备超细莫来石粉末（Ａｌ２Ｏ３／ＳｉＯ２＝７４／２６，质量比），用各种干、湿法成型工艺制得生坯，测定了生坯密度、微观形貌、气孔分布等结构物理状态。结果表明：湿法成型坯体密度比干法高约６％～７％，且坯体结构均匀，气孔分布窄（大多数小于４００Ａ），由此导致在同样烧成条件下湿法成型坯体烧结密度大大高于干法（达１８％～１９％）。通过对成型技术、坯体质量的分析评价，找出了适合于超细粉末成型的     

添加剂对凝胶注模成型工艺过程及坯体性质的影响

在凝胶注模成型工艺过程中，为了制得低粘度、高同相含量的陶瓷悬浮体并成型出性能优良的生坯，常加入一系列合适的添加剂来满足工艺性能（成型和烧结）的要求。本文对加入添加剂前后坯体的抗弯强度和显微结构进行了测试和观察。研究结果表明：分散剂柠檬酸铵可以明显的降低料浆粘度，增加固含量；增塑剂聚乙二醇可以有效的避免氧阻聚所产生的表面起皮和掉粉问题，增加了坯体的塑性；助烧剂氧化镁不仅可以降低氧化铝的烧结温度，在烧结的过程中还可以抑制氧化铝二次再结晶的晶粒长大。     

成型压力对莫来石晶须增强磷酸铬铝基复合材料性能的影响

以磷酸铬铝粘结剂、熔融石英、氢氧化铝、氟化铝为原料,制备以固相烧结莫来石及原位生长莫来石晶须为增强体的磷酸铬铝基复合材料。本文主要研究了烧结工艺过程中不同坯体成型压力对莫来石晶须生长和烧成制品结构、机械性能及介电性能的影响。进行的分析测试有:XRD、SEM、线性收缩、维氏硬度、介电常数等。结果表明:随成型压力增大,制品内部孔隙率降低,线性收缩减小,介电常数、抗弯强度及维氏硬度均随之增大。合理调控原料配方比例与烧结工艺可改善制品材料综合性能以应对不同需求。     

高固相Al2O3凝胶注模流变等性能研究

高分子凝胶注模成型作为一种近净尺寸成型方法,在国内已有研究.成型中,固相含量多见53％左右的研究,重点研究粒径1.5μm,固相含量58％的Al2 O3浆体随pH值变化的剪切稀化流变特性,分散剂不同加入量对浆体悬浮性的影响变化,淀粉加入量对坯体强度的影响,同时研究了消泡剂对高固相含量浆体制备,坯体断面结构以及对烧结体微观气孔分布的影响,分析了不同粒径的Al2 O3颗粒对制备高固相含量浆体粘度的影响等.     

木炭添加量对多孔莫来石陶瓷性能的影响

为了改善以木炭为造孔剂的多孔莫来石陶瓷的性能,以烧结莫来石(0.25~0.3 mm)、SiO2微粉、Al2O3微粉、滑石粉、球黏土、膨润土、甲基纤维素、木炭粉(≤0.044 mm)为原料,研究了不同量的木炭粉(外加质量分数分别为0、2%、4%、6%、8%、10%、12%)对多孔莫来石坯体的成型外观、烘干后的常温耐压强度及1 400℃保温3 h热处理后的显气孔率和常温耐压强度的影响,并对不同木炭添加量的多孔莫来石试样进行了显微结构分析。结果表明:外加质量分数≤8%的木炭,制成的多孔莫来石坯体可较好成型;外加质量分数2%~8%木炭的莫来石坯体与不添加木炭的相比,烘干后试样的常温耐压强度明显提高;多孔莫来石热处理后的显气孔率随着木炭添加量的增加而增加,常温耐压强度随之降低。综合考虑多孔莫来石陶瓷各项性能,木炭外加质量分数不宜超过8%。     

压力对凝胶注模成型95氧化铝陶瓷性能的影响

本文采用低毒的MAM-MBAM凝胶体系代替AM-MBAM有毒体系制备95氧化铝陶瓷,为改善成型后坯体的性能,在凝胶注模成型过程中给予浆料压力.研究发现在压力为0.3 MPa时获得的坯体表面光洁,线收缩率大,体密度高,结构均匀,成品率高,质量好.本文还并研究了压力对95氧化铝陶瓷烧结体线收缩率和体密度以及洛氏硬度的影响.实验结果表明:压力辅助凝胶注模成型所得坯体烧结后性能优于无压直接注模成型坯体,压力为0.3MPa时线收缩率最小,体密度最高可达3.81 g/cm3,洛氏硬度最高.坯体显微结构显示,陶瓷粉料被有机高分子网络很好地粘结在一起,并且压力注模的坯体中陶瓷粉料堆积紧密,结构均匀致密.烧结后,压力注模成型坯体晶粒发育良好,气孔较无压直接注模烧结体少,烧结致密性能优异.     

超细粉注浆成形制备Y—TZP

对用超细ZrO2粉体制制备料浆进行了研究，调制出流动性良好的ZrO2料浆，注浆生坯密度最大可达3．15g/cm^2，研究了料浆调制过程对坯体烧结性能的影响；注浆坯体在1600℃烧结得到接近致密的TZP材料。     

ZrB2-SiC复合材料凝胶注模成型初探

研究了ZrB2-SiC复合材料的凝胶注模成型技术。着重讨论了分散剂、pH值、固相体积含量、有机单体等对ZrB2-SiC复合材料料浆的影响;分析了凝胶注模成型后,排胶前复合材料素坯断面的显微结构以及相对应的烧结体的显微结构。结果表明:当分散剂用量为8.74‰(质量分数),pH为10.8,有机单体含量为3.1%时,可制得固相体积含量为40%,粘度为610mPa.s的ZrB2-SiC复合浆料,此时烧结体的断面主要以穿晶断裂为主;凝胶注模成型的坯体内部的有机聚合物网络因高温而完全分解,使素坯的气孔分布较均匀,利于烧结体致密度的提高。     

球磨过程对α－Al_2O_3注浆成形的影响

对平均粒径为１．４μ的α－Ａｌ_２Ｏ_３以ＰＡＡ为分散剂，以石膏为模具，进行了注浆成形，并在１６００℃下烧结３小时。料浆的球磨过程对生坯的相对密度，烧结体的收缩率及其抗弯强度有很大影响。烧结体的抗弯强度为２３０－３５０ＭＰａ。实验表明：当料浆中ＰＡＡ含量为０．２ｗｔ％（以Ａｌ_２Ｏ_３干基为准），ｐＨ值为８．８时素坯相对密度最大，其值为４９．３％。料浆中颗粒的充分分散有助于提高素坯的相对密度及烧结体的抗弯强度。建议在浇注前对料浆进行充分球磨。     

金属铝粉对刚玉-氮化硅材料性能的影响

借鉴“过渡塑性相工艺”的思想,在刚玉- 氮化硅材料中引入12.5%(质量分数)的铝粉,研究 了铝粉的加入对刚玉-氮化硅材料的成型性能以及 烧成后试样的体积密度、显气孔率、载荷-变形曲线 (断裂韧性)、物相组成和显微结构的影响。结果表 明:在刚玉-氮化硅材料中引入铝粉后,由于铝粉的 塑性有利于成型过程中孔隙的填充,使得干坯致密度 提高;试样在空气气氛中烧成后,由于铝粉原位氧化 生成的活性氧化铝与氮化硅氧化生成的二氧化硅反 应,生成了针柱状的莫来石晶体或晶须,对烧结体具 有补强增韧作用。     

Temperature-Dependent Iron Solubility in Mullite

Sample disks prepared from Al₂O₃ (61 wt%), SiO₂ (28 wt%), and Fe₂O₃(II wt%) powders were sintered at 1270° and 1440°C and then annealed between 1300° and 1670°C. The annealed samples consisted of mullite as the main compound with minor amounts of glass and sometimes magnetite. The iron content of the mullites decreases strongly from ∼ 10.5 wt% Fe₂O₃ at 1300°C to ∼ 2.5 wt% Fe₂O₃ at 1670°C. A complex temperature-controlled exsolution mechanism of iron from mullite is considered.     

Mullite formation from the pyrolysis of aluminium-loaded polymethylsiloxanes: The influence of aluminium powder characteristics

Polymethylsiloxane (PMS) filled with a range of aluminium powders of different size and morphology have been used to produce precursor mixtures to form mullite bodies. The size and shape of the Al powder is shown to have a strong influence on the temperature and mechanism of mullite formation, on the final microstructure and phase composition of the product. The reaction proceeds by decomposition of the PMS producing amorphous SiO₂. Al oxidation occurs both by reaction with the atmosphere and by reduction of the amorphous SiO₂ to produce α-Al₂O₃. Crystallisation of cristobalite was also observed prior to mullitisation. It is these components of the microstructure that react to produce mullite. The onset of mullite formation occurs at different temperatures, depending on the initial Al powder size and morphology. Large, flake morphology Al powders produced the greatest quantity of mullite and showed the lowest temperatures for mullite formation. XRD analysis identified 3:2 mullite in samples using large Al particles after heating to 1400 °C and at 1700 °C in samples using small Al powders.     

Role of Structural Fe(III) and Iron Oxide Nanophases in Mullite Coloration

Six mullite samples, derived from heat-treated natural kaolinites with various iron content, were investigated and compared to synthetic monophasic mullite. They were analyzed by X-ray diffraction, diffuse reflectance spectroscopy, and electron paramagnetic resonance. To quantify mullite coloration, the CIE colorimetric system was used. In contrast to synthetic mullite, samples showed charge transfer bands involving O²⁻ and Fe³⁺ ions as well as ferric crystal-field transitions due to Fe³⁺ ions in iron oxide nanoparticles. Absorption edges showed red shifts. The resulting yellowness, saturation of which increased with the content of iron oxide nanoparticles, is direct evidence for the coloring effect of Fe³⁺ ions.     

Mullite Formation by Endothermic Reaction of α-Alumina/Silica Microcomposite Particles

The formation of mullite was investigated using microcomposite powders which consist of α-alumina cores and amorphous silica coatings. Differential thermal analysis and X-ray diffraction showed that the mullitization reaction was endothermic. In contrast, mullite forms exothermically in samples prepared by sol-gel processing. The results are shown to be consistent with available thermodynamic data for mullite formation from different alumina and silica phases.     

Role of Iron in Mullite Formation from Kaolins by Mössbauer Spectroscopy and Rietveld Refinement

This paper examines the role of iron in mullite nucleation and growth from kaolins. We chose two typical raw kaolins containing a reduced impurity level and characterized by very different degrees of crystallinity of the kaolinite phase. Both the structural iron in kaolinite and also some iron deposited onto phyllosilicate layers by a chemical route were considered. After firing in the 900–1100°C temperature range, the Fe environment was determined by Mössbauer spectroscopy. From X-ray spectra of samples fired at 1250°C, mullite stoichiometries were obtained by Rietveld refinements. It was shown that iron contributes to the structural reorganization stage of the material, when mullite is nucleated. Fe atoms are essentially in octahedral sites, which favors an increase of the c parameter of the orthorhombic cell. The iron quantity attains a saturation level for an Fe-to-Al ratio between 0.3 and 0.4, depending on the raw kaolinite crystallinity. Besides mullite, the excess iron associates with titanium to form a pseudobrookite phase and hematite.     

Effect of MgO addition and sintering parameters on mullite formation through reaction sintering kaolin and alumina

Abstract

In the present work, the influence of MgO addition and sintering parameters on the formation and densification of mullite was investigated. The morphology of powders and the microstructure of the sintered samples were characterised by means of a scanning electron microscope. X-ray diffraction was used to characterise phases formed in sintered samples. The density of sintered samples was measured using a densimeter and quantified according to the Archimedes principle. MgO was added at 1, 2, 3, 4, 5 and 6 wt-% to kaolin and alumina and the powders were ball milled for 5 h then uniaxially compacted at 75 MPa and finally sintered at 1500, 1550, 1600 and 1650°C for 2, 4, 6 and 8 h. It was found that addition of MgO not only affected mullite formation but also promoted grain growth. For samples containing 0, 1 and 2 wt-%MgO only mullite was formed. While, in addition to mullite, Al₂O₃ was present in sample containing 3 wt-%MgO. At higher MgO content (4, 5 and 6 wt-%), three phases, i.e. mullite, Al₂O₃ and spinel, were formed. Addition of 1 wt-%MgO increased the density of all samples for all sintering times and higher densities corresponded to higher sintering temperatures. At higher MgO content, higher temperatures led to lower densities and lower temperatures led to higher densities for almost all sintering times.     

Fine milling of fused mullite and mullite-corundum

Conclusions Milling time during the fine grinding of fused mullite and mullite-corundum powders in a vibromill instead of a ballmill can be reduced by a factor of five. The addition of sulfite lye or ethyl silicate in amounts of 0.1% reduces by a factor of 12–18 the vibromilling time, but iron pickup is increased. Grinding in a jet mill causes the specific surface to be much less than milling in a vibromill; the capacity for sintering such powders is impaired.Translated from Ogneupory, No. 6, pp. 17–18, June, 1981.     

Corrosion behavior of volcanic ash on sintered mullite for environmental barrier coatings

The high-temperature corrosion behavior of volcanic ash(VA) in attacking sintered mullite was investigated, and the corrosion resistibility of mullite environmental barrier coatings (EBCs) to VA was predicted. Sintered mullite specimens were prepared by using the spark plasma sintering method. These specimens were subjected to a hot corrosive environment—molten Icelandic VA at 1400 °C—for three different duration times (2, 12, and 48 h). The microstructure and phase of the specimens were analyzed by using a scanning electron microscope equipped with an accessory system for energy dispersive spectroscopy and X-ray diffraction. In addition, in-situ high-temperature X-ray diffraction was carried out to identify the dynamics of phase evaluation in the volcanic ash and mullite mixture powders. Results show that a reaction layer was generated and continuously dissolved into the melted volcanic ash. The primary incursive component is iron; however, a minimal amount of sodium plays a more important role in disintegrating sintered mullite.     

Porous Mullite Preforms via Fused Deposition

Nonrandom porous mullite ceramic preforms were fabricated by the indirect fused deposition process. MgO was added to commercial mullite powders as a sintering aid. The influence of porosity and the amount of MgO on the densification and mechanical properties was studied. The shrinkage and compressive strength of the porous samples were found to increase with increasing MgO content. At constant MgO concentration, shrinkage was found to decrease linearly as the volume fraction of porosity increased. The compressive strength of porous samples decreased with an increase in the volume fraction of porosity at constant MgO content.     

Toughened carbon nanotube–iron–mullite composites prepared by spark plasma sintering

Carbon nanotube–iron–mullite nanocomposite powders were prepared by a direct method involving a reduction in H₂–CH₄ and without any mechanical mixing step. The carbon nanotubes are mostly double- and few-walled (3–6 walls). Some carbon nanofibers are also observed. The materials were consolidated by spark plasma sintering. Their electrical conductivity is 2.4 S/cm whereas pure mullite is insulating. There is no increase in fracture strength, but the SENB toughness is twice than the one for unreinforced mullite (3.3 vs. 1.6 MPa m^1/2). The mechanisms of carbon nanotube bundle pullout and large-scale crack-bridging have been evidenced.