Nanocrystalline yttria doped ceria powder has been prepared by auto-combustion of a transparent gel formed by heating an aqueous acidic solution containing methylol urea, urea, cerium(III) nitrate and yttrium(III) nitrate. The TGA and DSC studies showed the combustion reaction of the gel initiated at 225 degrees C and completed within a short period of time. XRD spectrum of the combustion product reveals the formation of phase pure cubic yttria doped ceria during the combustion process. Loose agglomerate of yttria doped ceria particle obtained by the combustion reaction could be easily deagglomerated by planetary ball milling and the powder obtained contains particles in the size range of 0.05-3.3 mu m with D-50 value of 0.13 mu m. The powder particles are aggregate of nanocrystallites with a wide size range of 14-105 nm. Pellets prepared by pressing the yttria doped ceria powder sintered to 95.2% TD at 1400 degrees C. (c) 2006 Elsevier Ltd. All rights reserved.