The effects of thermal treatment conditions on ADU (ammonium diuranate) prepared by SOL-GEL method, so-called GSP (Gel supported precipitation) process, were investigated for kernel preparation. In this study, ADU compound particles were calcined to particles in air and Ar atmospheres, and these particles were reduced and sintered in 4%-/Ar. During the thermal calcining treatment in air, ADU compound was slightly decomposed, and then converted to phases at . At , the phase appeared together with . After sintering of theses particles, the uranium oxide phases were reduced to a stoichiometric . As a result of the calcining treatment in Ar, more reduced-form of uranium oxide was observed than that treated in air atmosphere by XRD analysis. The final phases of these particles were estimated as a mixture of and .