Nanosized ytterbium doped yttria powders were prepared by citrate-gel combustion techniques. As-synthesized precursor and calcined powders were characterized for their crystalline structure, particle size and morphologies. Nanocrystalline Yb 3+ :Y 2 O 3 powders with pure cubic yttria crystal structure were obtained by calcination of as-prepared precursors at 1100°C for 3h. Powders obtained were well dispersed with an average particle size of 60nm. By using the obtained powders, nearly full dense Yb 3+ :Y 2 O 3 ceramics were produced by vacuum sintering at 1800°C for 12h. The emission spectrum of the sintered ceramics under the excitation wavelength of 905nm illustrates that there are three fluorescence peaks locating at 976nm, 1030nm and 1075nm respectively, all corresponding to the 2 F 5/2 → 2 F 7/2 transitions of ytterbium ion.