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In this study, first the ADU gel particle, an intermediate for final UO2 kernel of a HTGR nuclear fuel, was prepared from sol-gelmethod using the broth solution which was made by mixing of the uranyl nitrate, poly vinyl alcohol and tetra-hydrofurfuryl alcohol.The prepared dried-ADU gel particles were converted to the UO2 via UO3 from thermal treatment with the 4% H2 atmosphere. Thesizes of the spherical liquid droplets appeared 1900~2100m, and the harmony between the flow rate of the broth solution and thefrequency and the amplitude of a vibrating system are important factors for the spherical ADU gel particles via the mono size sphericaldroplets. From the XRD and FT-IR analyses, the prepared ADU gel particles were judged to be a UO3·xNH3·yH2O form, and themost important factor during the thermal treatment of the dried-ADU gel particle must be avoided a rapidly heating rate in the of 180~400oC, and the heating rate should be kept below 5oC/min.