The effect of relatively small additions (1-5 wt%) of nickel, nickel boride (NiB), and iron to promote the liquid-phase sintering of titanium diboride (TiB 2 ) has been studied. Carbon also was added to some samples, to reduce the amount of oxygen impurities in the TiB 2 ceramics. Green bodies that were formed by uniaxial pressing were sintered in a graphite furnace at 1300°-1700°C, both under vacuum and in a 500 mbar argon atmosphere, and high densities (>94% of theoretical density) were obtained at temperatures ≥1500°C. The weight loss of the samples during sintering was shown to be dependent on the densification rate and the final density and was not governed only by the thermodynamics of the system. Significant exaggerated grain growth was observed in samples with nickel, NiB, and iron during sintering at 1700°C. The exaggerated grain growth was observed to be closely related to the oxygen content of the samples and to temperature. The addition of carbon strongly reduced the density and the oxygen content and, thereby, inhibited grain growth. We have proposed that the exaggerated grain growth is enhanced by surface diffusion in a titanium-oxide-rich layer on the TiB 2 grains.
The evaporation of silicon carbide (SiC) ceramics during sintering has been studied by thermogravimetry in a graphite furnace filled with argon. The SiC powder compacts contained 7.5 wt% eutectic composition of Y2O3–Al2O3 to promote liquid‐phase sintering. A weight loss of 1–11 wt% was observed during sintering, depending on the sintering temperature and sintering time. The weight loss severely influenced the final density and the microstructure of the SiC ceramics. Particularly, the oxide sintering aids, which were homogeneously distributed in the green ceramics, were observed to segregate and form particular patterns that were dependent on the temperature, sintering time, and the total weight loss. Possible heterogeneous reactions evolving volatile species have been discussed in relation to the experimental observations.
The densification of aluminum nitride using Ca12Al14O33 as a sintering aid has been studied with emphasis on the effect of using coarse or fine powder, the amount of sintering aid, the sintering temperature, and embedding. Both crystalline and amorphous grain boundary phases were observed. Significant weight losses were observed for coarse‐grained samples, and if suitable embedding was not used. Porous and coarse‐grained ceramics with high contiguity and minor amounts of secondary phases were obtained by enhanced evaporation while dense ceramics were obtained limiting the evaporation. High weight losses in the graphite environment resulted in formation of a dense AlN surface layer.
Microporous two‐phase AlN–SiC composites were prepared using Al4C3 and either Si (N2 atmosphere) or Si3N4 (Ar atmosphere) as precursors. The reaction mechanisms of the two synthesis routes and the effect of processing conditions on reaction rate and the material microstructures were demonstrated. The exothermic reaction between Si and Al4C3 under N2 atmosphere was shown to be a simple processing route for the preparation of porous two‐phase AlN–SiC materials. The homogeneous two‐phase AlN–SiC composites had a grain size in the range of 1–5 μm, and the porosity varied in the range of 36%–45%. The bending strength was 50–60 MPa, in accordance with the high porosity.
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