Nano-sized Y2O3 powders were prepared via a sol-gel method starting with Y(NO3)3·6H2O (Yttrium(III) nitrate hexahydrate) and water with ethanol as a cosolvent. Y2O3 is an important rare earth oxide and has been considered for use in nuclear applications, such as ceramic materials, due to its excellent optical and refractory characteristics. It has been used as a chemically stable substrate, a crucible material for melting reactive metals, and a nozzle material for jet casting molten rare earth-iron magnetic alloys. Oxalic acid (C2H2O4) has been adopted as a chelating agent in order to control the rate of hydrolysis and polycondensation, and ammonia was added in order to adjust the base condition. The synthesized Y2O3 powder was characterized using TG/DTA, XRD, FE-SEM, BET and Impedance Analyzer analyses. The powder changed its properties in accordance with the pH conditions of the catalyst. As the pH increases according to the FE-SEM, the grain grew and it showed that the pore size decreased while confirming the effect of the grain size. The nano-material Y2O3 powders demonstrated that the surface area was improved with the addition of oxalic acid with ammonium hydroxide.