The developed Sol-Gel Hydrolysis Process was applied to produce uranium oxide microspheres suitable for use as nuclear fuel. Different preparation conditions of washing, feed solution aging and microsphere soaking were tried to produce dense UO3- and UO2-micospheres. The effect of reduction time and temperature on the density and porosity of the microspheres was carried out to optimize the preparation parameters. The total surface area, total pore volume and pore radius of UO3- and UO2-microspheres were measured through N2gas adsorption and application of the BET-equation at 77 K. The effect of the preparation conditions on crystallite size of the samples was made through ray diffraction analysis. Examination of the prepared uranium oxides by differential thermal analysis and thermal gravimetric analysis was carried out.