Dispersion and Grinding of Oxide Powders into an Aqueous Slurry

The present paper deals with a comprehensive analysis of the dispersion behavior of oxide powders to determine accurate conditions for mixing and grinding dense slurries without the use of steric dispersing agents. The experimental support of the work was the synthesis of (Zr,Sn)TiO4 microwave dielectric ceramics by the solid-state reaction of raw materials mixed and ground by attrition milling. Zeta potential measurements were performed on the raw materials versus pH to determine the optimum pH of the slurry, allowing a good dispersion of all the species: the absolute value of the zeta potential of every powder >20 mV, with all potentials having the same sign. During the grinding process, as the surface of the materials increases due to the breakup of the grains, surface reaction occurs with the dispersion liquid, and pH must be continuously adjusted to be maintained at an adequate level. We have correlated these characterizations of the optimal processing conditions with the rheological behavior of the slurries, thus providing an analysis of the flocculated or deflocculated state. When applied to synthesizing (Zr,Sn)TiO4 microwave dielectric ceramics, these conclusions made it possible to produce reproducible resonators with a k= 37 dielectric constant and characterized by a quality factor, Q×F > 60 000 GHz measured at 3 GHz, the highest value reported for this composition.