Substitutional, continuous solid solution of the general formula Y 2-x Yb x O 3 was obtained from the mixture of Y 2 O 3 and Yb 2 O 3 oxides, for the first time by the mechanochemical method in a high-energy ball milling. The monophasic samples of nanocrystalline solid solution for x [ 0.00 and x \ 2.00 were examined by the methods: XRD, DTA, SEM, IR and UV-Vis-DR. As follows from the results, the solid solution crystallizes in cubic system and is isostructural with Y 2 O 3 and Yb 2 O 3. The solution is stable in the air atmosphere up to at least 900°C, and its decomposition temperature decreases with the increase in x, that is, with decreasing number of Yb 3? ions replacing Y 3? ions in the crystal lattice of Y 2 O 3. The energy band gap estimated for the solid solution varies from * 5.30 eV for x = 0.50 to * 4.90 eV for x = 1.50, which means that it is an insulator.