Erbium and ytterbium doped barium titanate nanopowders were prepared using the hydrothermal method. A barium titanate structure doped with rare earth ions manifested new characteristics and improved the field of application of optical devices such as trichromatic tubes, LCD displays, lamps, and infrared lasers. In this work, BaTiO3:Er3+ and BaTiO3:Yb3+ were prepared using barium chloride [BaCl2], titanium butoxide [C16H36O4Ti], erbium chloride [ErCl3] and ytterbium chloride [YbCl3] as precursors. Anhydrous methanol was employed as a solvent. Metallic potassium was used to promote solubility in the system and increase the pH to 13. This method yielded the formation of a predominantly cubic structure in both Er3+ and Yb3+ doped BaTiO3 powders. Characteristic bondings of BaTiO3 were observed with FT-IR spectroscopy. The predominantly cubic structure was confirmed by X-ray diffraction and micro-Raman analyses. The particle size (∼30 nm) was estimated using the Scherrer equation and X-ray diffraction data. The results were presented and discussed.