The effects of the drying conditions on the thermal behaviour of UO3 gel microspheres were studied by TG, DTA and X-ray examination. The effects of drying with air, steam or alcohol on the crystal structure and crystallite size were also studied. The results indicate that the thermal decomposition of UO3 gel microspheres involves five steps: the first two for dehydration, the third for ammonia release, the fourth for ammonia oxidation, and the last one for UO3 recrystallization. It was also found that the crystal growth varied from 110 Å after air drying to 512 Å and 496 Å after steam and alcohol treatment respectively.