Spray drying is a physical process of granulating fine powders that is used widely in the chemical, pharmaceutical, ceramic, and food industries. It is generally used to produce flowable fine powders for mechanized processing. Occasionally it is used to fabricate sintered bodies like cemented carbides, and has been used to produce sintered fuel and actinide microspheres . As a physical process, it can be adapted to many powder types and mixtures and thus, has appeal for dispersion nuclear fuels, and waste forms of various compositions. It also permits easy recycling of unused powders, and generates minimal chemical waste streams that can arise in chemical sol/gel processing. On the other hand, the containment of the radioactive powders, present safety challenges that need to be addressed . Detailed formal procedures and methods for characterizing and processing UO2/ThO2 mixtures have been established and approved by the Purdue Radiological Control Committee for (1) ball-milling, (2) viscosity and rheology measurements on slurries, (3) sintering, (4) co-precipitation, (5) particle size analysis using laser scattering, (6) surface area analysis using the BET technique, (7) X-ray diffraction, (8) stoichiometry measurement, (9) zeta potential measurements and (10) ceramographic preparation. The spray drying procedures represented a particular challenge since they deal with the handling of loose powders. Studies were carried out to formulate suitable stable, dense and homogeneous aqueous slurries of urania and thoria powders for the production of urania-thoria microspheres by the spray drying method. The studies included (a) particle size distribution after ball-milling, (b) viscosity, (c) zeta potential, (d) slurry flowability, stability and cleanability, (e) microsphere green strength, and f) effects of organic dispersants on the above properties. After formulating the slurry, U,ThO2 microspheres were produced using a commercial, laboratory-scale spray dryer modified for handling these radioactive materials. The microspheres thus obtained were dried at 473 K for 4 hours, presintered at 1173 K for 2 hours and sintered at 1923 K for 10 hours.