Sintering behaviour of ultrafine NbC and TaC powders

Compositional and microstructural changes upon firing ultrafine (300 to 400 Å) stoichiometric NbC and TaC powder lots have been studied up to a temperature of 1600° C. Substantial amounts of oxygen impurities, mostly oxide particles or layers are eliminated by reductions with hydrogen, free carbon or the carbides themselves. TGA showed these reactions to take place at 700 to 1400° C with maxima around 1000 to 1100° C. Low temperature sintering is inhibited by this impurity and its removal is thus essential. Other impurities (Ni, Cr, Fe) were also found in the starting powders in total concentration 0.5 to 1%. They give rise to a liquid phase located at grain edges at temperatures as low as 1100° C which then controls microstructure development. It dissolves to some extent in the carbide matrix at high temperature, and has a tendency to rise to the free surface of the samples. Compositional and structural heterogeneities are thus produced between bulk and surface at high temperatures. Owing to these impurity effects, it was not possible to clearly evaluate the influence of powder granulometry.