Medium sized spherical particles (with diameters below 100 μm) of ceramic materials (Al203 and Al203 +8%TiO2) were produced in the following steps: (1) preparation of concentrated hydroxide sols of cations by extraction of anions using Primene JMT, (2) formation of sol emulsion in 2-ethylhexanol-1 containing various amounts of surfactants (EH), (3) gelation of emulsion drops by extraction of water with partially dehydrated EH, (4) non-destructive thermal treatment. Principal properties of the sol depend on the temperature of the extraction process. For preparation of lowanionic sols a two step extraction process, separated by digestion of the aqueous phase at boiling point, was necessary. It was found that the parameters of emulsion formation as well as the properties of the sols significantly influence the particle size distribution. It was concluded that lowering of the sol- EH interracial tension by the surfactant does not influence the process. On the contrary the “anti-clustering” effect of surfactants is essential for preparation of perfect spherical powders. The thermal decomposition of gels to oxides is determinant for densities, specific surface area and carbon content. Medium sized spherical powders are free flowing. The compactibility and sinterability of those powders are poor. However drastic reduction of particle size by milling (connected with their transformation to irregular shape) significantly improves the sinterability.