微晶玻璃烧结过程中晶化和致密化的关系

以钢渣和粉煤灰为主要原料,采用烧结工艺,制得以透辉石为主晶相的微晶玻璃;通过热分析、X射线衍射、收缩率、扫描电镜等分析方法,详细说明了在烧结过程中晶化和致密化的关系;试验结果表明晶化主要发生在烧结的前期,后期以致密化为主,晶化会影响烧结体的致密化。     

高岭土尾矿微晶玻璃的烧结与晶化

本研究对高岭土尾矿为主要原料制备的CaO－Al2O3－SiO2系统玻璃进行了烧结收缩试验,借助X射线衍射分析了影响烧结致密化过程的因素;探讨了玻璃组成对烧结和晶化的影响,采用合适的玻璃组成,用烧结工艺获得了主晶相为β-CaO·SiO2的高岭土尾矿微晶玻璃。     

晶化温度对CaO-Al2O3-SiO2-Fe2O3系粉煤灰微晶玻璃析晶及性能的影响

以粉煤灰、石灰石和无水碳酸钠为原料,通过烧结法制备了以钙长石、钙铁辉石和霞石为晶相的复合晶相微晶玻璃.借助差热分析、X射线衍射及扫描电子显微镜研究了晶化温度(850～1100℃)对微晶玻璃析晶行为、显微形貌和性能的影响.结果表明:随晶化温度的升高钙长石和霞石晶相的含量先增加后降低,钙铁辉石晶相含量逐渐增加,同时微晶玻璃中晶体形态逐渐由球形微晶发育成柱状,最后长成片状;晶化温度的升高有利于微晶玻璃的烧结致密化,1050℃时微晶玻璃的线收缩率和体积密度达到最大,分别为17.04％和2.76 g/cm3,吸水率最小,为0.01％.过高的晶化温度(1100℃)会降低其致密程度.     

烧结粉煤灰建筑微晶玻璃的研究

以烧结粉煤灰为主要原料．利用本地资源钠长石来降低基础玻璃的熔化温度。并测定了微晶玻璃的主要性能，研究了基础玻璃化学成分，热处理制度对烧结、晶化过程及样品外观的影响，确定了合理的玻璃成分范围和工艺制度。     

烧结粉煤灰微晶玻璃装饰板的研究

以粉煤灰为主要原料,采用烧结法制备粉煤灰微晶玻璃装饰板,并借助Ｘ射线衍射法鉴定材料的主晶相。测定了微晶玻璃的主要性能,研究了基础玻璃成分、热处理制度对烧结、晶化过程及样品外观的影响,确定了合理的玻璃成分范围和工艺制度。     

添加氧化铈对堇青石基微晶玻璃的烧结和性能的影响

采用X射线衍射、扫描电镜和差热分析等手段研究了稀土氧化铈对由熔融淬冷法制备的非化学计量组成的堇青石基微晶玻璃的相变、烧结特性和性能的影响。研究结果表明：添加氧化铈能够明显抑制μ-堇青石相的形成和促进μ-堇青石向α-堇青石的转变。氧化铈的加入降低了微晶玻璃的烧结活化能和堇青石微晶玻璃的烧结温度,添加氧化铈质量分数为4％的微晶玻璃的μ-堇青石转变为α-堇青石的最低温度约为900℃,此时烧结样品几乎完全致密化,但氧化铈加入量太多将会阻止微晶玻璃的烧结和晶化。微晶玻璃的抗折强度随氧化铈含量的增加而增加,当氧化铈为4％时样品的抗折强度达到最大值。微晶玻璃的热膨胀系数随着氧化铈含量的增加变化不大。该微晶玻璃可望应用于微电子封装领域,能够与高导电率、低成本的金属如铜、银／钯低温共烧制成电子基板材料。     

白云鄂博尾矿微波还原除铁制备CAS系微晶玻璃工艺研究

利用“微波还原-磁选”除铁后的白云鄂博尾矿制备了CaO-Al2 O3-SiO2 (CAS)系微晶玻璃.借助差热分析、扫描电子显微镜和X射线能谱分析研究了CAS系微晶玻璃经680℃核化后不同晶化温度(870～930℃)对其析晶行为、显微形貌和性能的影响.结果表明:此CAS系微晶玻璃相组成随晶化温度的升高由长石相转变为辉石相,同时微晶玻璃中晶体形态逐渐长大,由方块状小颗粒微晶发育成板条状以及大颗粒的雪花状和方块状的“骨架”微晶;而且适当提高晶化温度有利于微晶玻璃的烧结致密化,进而提高其力学性能,900℃晶化处理的微晶玻璃抗折强度和密度分别为181.2 MPa和3.1 g·cm-3,而且其耐酸碱性能很好.本研究对于开发微晶玻璃新产品、新工艺有重要的指导意义.     

CaO—Al2O3—SiO2系统玻璃的微晶化

介绍了制造CaO-Al_2O_3-SiO_2系统玻璃的方法.研究了这种微晶玻璃的晶化制度、晶核剂类型;讨论了玻璃的微晶化机理.     

透辉石系统微晶玻璃釉用熔块的晶化行为

利用DTA、XRD、SEM、高温显微镜等测试手段研究了CaO -MgO -Al2 O3-SiO2 系统微晶玻璃釉用熔块的晶化行为 ,计算了其晶体生长活化能 ,分析了热处理过程中烧结与晶化的关系 ,同时对该熔块制作高耐磨墙地砖釉的可能性进行了验证     

烧结粉煤灰建筑微晶玻璃的研究

以粉煤灰为主要原料, 用钠长石降低基础玻璃的熔化温度, 测定了微晶玻璃的主要性能, 研究了基础玻璃化学成分和热处理制度对烧结、晶化过程及样品外观的影响, 确定了合理的玻璃成分范围和工艺制度。     

Investigation on low-temperature reactive viscous flow sintering behavior of lanthanum-borate glass-ceramic with BaTi4O9 ceramic filler

In this paper, the sintering behavior of the lanthanum-borate (B₂O₃-La₂O₃-MgO-TiO₂,BLMT) glass-ceramic with BaTi₄O₉ filler composite was investigated in terms of the wetting behavior, interfacial reaction, sinter-shrinkage process, sintering activation energy, as well as phase and microstructure evolution with change in filler contents and sintering temperature. Our research suggested that the glass is unable to wet the filler material within a temperature up to 1000 °C, indicating that the densification process of composites is dominated by viscous flow of glass matrix. The increase in filler content that performs as a rigid particle in composite causes the rise in the sinter-shrinkage-onset and -end temperature, thereby proving that the viscous-flow densification of the composites with x≤ 30 wt% filler content is accomplished before the crystallization of BLMT glass, whereas the composites with x≥ 40 wt% cannot. After densification, a chemical reaction that almost synchronizes with the glass crystallization occurred between glass and ceramic, which not only imposes significant influence on the crystallization behavior, but eradicates the closed pore formed by the viscous flow and the induced crystallization porosity. The densification process of the BaTi₄O₉ filler-BLMT glass composite was referred to as two-stage reactive assisted viscous flow sintering process which consists of viscous flow of glass, of the crystallization process of glass, and/or of the chemical reaction between glass and filler.     

Densification and Phase Development of Spodumene–Cordierite Glass Powder Mixtures

The sintering and crystallization of spodumene-cordierite glass-ceramics that are made from mixtures of Li₂O-Al₂O₃-SiO₂ (LAS) and MgO-Al₂O₃-SiO₂(MAS) glass powders were investigated. Pure LAS and MAS powders have good sinterability. However, the densification of LAS was drastically reduced when small amounts of MAS were added. When larger amounts of MAS were added, the amount of densification further increased. The decrease in the Li₂O content in the LAS glass promoted the densification of the mixed glass samples. The above-mentioned results can be explained by examining the crystallization temperature, which is influenced by the interactions between the LAS and MAS glass particles. The lower the temperature of crystallization, the less sintering occurred. For the sintered samples, the phase that crystallized from the MAS glass was alpha-cordierite, and that which crystallized from the LAS glass was ß-spodumene or high-quartz solid solution, depending on the Li₂O content in the LAS glass.     

Sintering in Nitrogen Atmosphere of Iron-Rich Glass-Ceramics

The sintering and the crystallization of two iron-rich glass compositions (45–75-μm powder fractions) were studied in air and nitrogen atmospheres. The phase formation was evaluated by differential thermal analysis, while the densification, by dilatometry; the crystalline phases were identified by X-ray diffraction and the structure observed by scanning electron microscopy. It was highlighted that, due to the absence of Fe²⁺ oxidation and lower viscosity of the parent and residual glasses, the sintering in nitrogen atmospheres occurs at 100°–200°C lower temperature. In the same time the higher amount of crystal phase, formed during sinter–crystallization in inert atmosphere, improves the mechanical properties. A value of 120 MPa for the bending strength was obtained after 1-h sintering at 960°C in N₂.     

Effect of the Heating Rate on the Relative Rates of Sintering and Crystallization in Glass

The sintering of glass can sometimes be impeded by crystallization. In the optimum process the glass should sinter to full density before the onset of crystallization. In an earlier paper we showed how sinter-forging experiments can be used to investigate the coupling between densification and crystallization. Here we demonstrate that increasing the heating rate can delay crystallization so that a certain glass can sinter to full density.     

Role of Particle Substructure in the Sintering of Monosized Titania

Monosized titania particles (∼0.35-μ diameter) prepared by controlled hydrolysis of titanium tetraethoxide in ethanol were found to be porous agglomerates of ∼6-nm primary particles. The sintering behavior of compacts constituted of monodispersed agglomerates was evaluated, and changes in macroscopic dimensions were correlated with changes in particle microstructure and chemistry. The total volume shrinkage during sintering was ≥87%. Five contributions to the total shrinkage and the temperature ranges for the associated processes were identified: removal of chemisorbed water (from ambient to 250°C), crystallization to anatase (between 250° to 425°C), intra-agglomerate densification (425° to 800°C), conversion of anatase to rutile (600° to 800°C), and inter-agglomerate densification (>800°C). Approximately one-half the compact shrinkage was the result of agglomerate substructure changes. Studies of the agglomerate structural evolution indicated the intra-agglomerate densification and crystallite growth rates are the secondary factors, after compact packing, that influenced microstructure development.     

Properties of sintered glass-ceramics in the diopside–albite system

A series of sintered glass-ceramics belonging to the system diopside–albite, forming by surface crystallization 30, 50 and 65% diopside, was investigated. In order to study the effect of bulk crystallization on the sintering a 0.7% of Cr₂O₃ as nucleation agent was added in one of the compositions.

The crystallization was evaluated by DTA and density measurements and the degree of densification by the linear shrinkage and total porosity. These results were confirmed by SEM and XRD, respectively. The mechanical properties of the final glass-ceramics were measured and discussed as a function of the percentage of crystal phase formed and kind of crystallization (i.e., surface or bulk).     

Effect of uniaxial load on the sintering behaviour of 45S5 Bioglass powder compacts

The effect of a uniaxial compressive load on the sintering behaviour of 45S5 Bioglass^® powder compacts was investigated by means of sinter-forging. In comparison to free sintering, densification kinetics was enhanced and the degree of crystallization was reduced. Significantly lower sintering temperatures, i.e. 610 °C instead of 1050 °C, can be employed to obtain dense Bioglass^® parts when sintering is performed under uniaxial load. The effect of mechanical loading on microstructure (pore density, shape and orientation) is discussed. The results of the investigation are relevant in connection with the development of sintered Bioglass^® substrates for bone replacement devices, where both porosity and crystallinity of the part require careful control and low densification temperatures are sought.     

Sintering and Microstructure Modification of Mullite/Zirconia Composites Derived from Silica-Coated Alumina Powders

This paper addresses the densification and microstructure development during firing of mullite/zirconia composites made from silica-coated-alumina (SCA) microcomposite powders. Densification occurs in two stages: in the presence of a silica–alumina mixture and after conversion to mullite. The first stage of densification occurs through transient viscous phase sintering (TVS). This is best promoted by rapid heating, which delays the crystallization of silica to higher temperatures. A further sintering stage is observed following mullitization. The introduction of seeds promotes solid-state sintering, most probably due to refinement of the mullite matrix. For seed concentrations up to about 1% the sintering kinetics depend on seed concentration. This suggests that nucleation still remains the rate-controlling mullitization step. Above this concentration the reaction becomes growth controlled. Introduction of seeds also promotes direct mullitization without transient zircon formation that was observed in a previous study of the same process without seeding. Seeding also promotes the development of elongated grains by way of a solid-state recrystallization process.