The thermal decomposition behaviour of UO 3 gel microspheres has been studied. Thermal analysis involved DTA, TG, DTG and X-ray examination.The effects of washing the UO 3 gel microspheres with hot water and with ammonia solution were investigated, as were the effects of soaking the microspheres in ammonia solution before or after washing on the crystallite size.The results indicate that the thermal decomposition of UO3 gel microspheres includes five steps: the first two for dehydration, the third for ammonia removal, the fourth for ammonia oxidation and the last step for UO 3 recrystallization. This paper describes a study of the thermal analysis and X-ray diffraction of UO3 gel microspheres prepared by hydrolysis [1]. Hydrolysis is one of several sol-gel processes [2-4] which have been developed for the fabrication of UO3 microspheres can be used as fuel kernels in coated particle fuel for high-temperature gas cooled reactors. For the application of UO3 microspheres in light water and fast breeder reactor fuel elements, two different fuel forms are being considered. Sphere-pack fuel rods are formed by the vibrocompactions of microspheres and pelletizing of the microspheres.Hydrolysis is a very simple process based on the rapid solidification of droplets from a fairly concentrated uranyl nitrate solution (about !.4 M) containing urea and hexamethylenetetramine at temperatures of about 90 ~ in silicone oil. The resulting microspheres are deep-orange and fully transparent. After washing in CC14 to remove silicone oil, the kernels are either washed with hot water for 10 rain at 95 ~ or with 3% ammonia solution for 2 hours at 25 ~ Hot water-washed microspheres are opaque and yellow, while ammonia-washed microspheres are transparent and orange.