Ultrafine particles of Ir-Ta binary oxides have been prepared by a sol-gel process consisting of hydrolysis and condensation of metal alkoxides in the liquid phase. The binary oxides calcined at 500-degrees-C consisted of IrO2 rutile-type phase and Ta2O5 amorphous phase, while iridium oxide contained not only IrO2 rutile-type phase but also iridium metallic phase.