Browsing by Author "Matovic, Branko"

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    Low temperature sintering additives for silicon nitride
    (2003) Matovic, Branko; Aldinger, Fritz (Prof. Dr.)
    Pressureless sintering of Si3N4 with two new additives based on the Li2O-Y2O3 system (LiYO2) and on the Li2O-Al2O3-SiO2 system (LiAlSiO4) were investigated in this study. Experiments were conducted in the areas of powder processing, sintering optimization, phase transformation characterization and microstructural development. Sintered materials were characterized by fracture toughness and thermal diffusivity measurements. The experimental results are summarized in the following: Using three different mechanical mixing processes (attrition milling, ball milling and vibratory milling) for the introduction of additives (LiYO2) into Si3N4 powders, the best results are obtained for attrition milling. This method yields a good dispersion of the additive powder in fine unagglomerated Si3N4 without contamination. It also yields good sintering characteristics. For the LiYO2 system, the densification depends largely on the content of sintering additive. A larger amount of additive means a higher volume of liquid phase, which is favorable for efficient particle rearrangement resulting in higher values of density rate. In case of the LiAlSiO4 additive, it is found that the densification is less dependent on the additive content. The overall sintering kinetics at the low temperatures is less retarded when using the LiYO2 additive in comparison to the LiAlSiO4 additive, resulting in higher densities obtained at lower temperatures and shorter annealing times. With prolonged heating time, the differences in the degree of densification become smaller. The kinetics of phase transformation in the both systems are found to be of first order. In the LiYO2 system, the transformation rate constant increases with increasing additive content. While the opposite behavior is noticed in case of the LiAlSiO4 additive, i.e. the rate constant decreases with higher additive content. The phase transformation is always completed at a later stage than the densification. The lag between the two phenomena in the sintering process is more pronounced with the Li2O-Al2O3-SiO2 additive system. The alpha to beta Si3N4 transformation is accompanied by grain growth. Upon prolongation of the annealing time the grain size and the morphology of the growing beta-Si3N4 particles are significantly changed from equiaxed to elongated. The grain growth becomes anisotropic, leading to rod-like betaƒ{Si3N4 crystals. The growth rate is higher in the LiYO2 system than in the LiAlSiO4 system. At 1600„aC, the microstructure of Si3N4 ceramics sintered with both the additives is characterized by a homogeneous distribution of elongated beta Si3N4 grains and glassy phase located in thin layers at grain boundaries and at triple points. The maximum values obtained for fracture toughness are 6.8 and 6.2 for the materials sintered with LiYO2 and LiAlSiO4 additives, respectively, at 1600„aC for 8 h. The higher value of fracture toughness in the LiYO2 system is attributed to its microstructure with a higher aspect ratio of the elongated beta-Si3N4 grains. Thermal conductivity of the material sintered with the LiYO2 additive is higher in comparison to that sintered with LiAlSiO4 additive. In the LiAlSiO4 system, partial dissolution of Al3+ in the beta-Si3N4 grains results in increasing phonon scattering and hence decreases the thermal conductivity.