Lu3+/Yb3+ and Lu3+/Er3+ Co-doped Sb2Se3 nanomaterials were synthesized by a Co-reduction method in hydrothermal condition. Powder XRD patterns indicate that the LnxLn′xSb2-2xSe3 Ln: Lu3+/Yb3+ and Lu3+/Er3+ crystals (x= 0.00-0.04) are isostructural with Sb2Se3. The cell parameters were increased for compounds upon increasing the dopant content (x). SEM and TEM images show that Co-doping of Lu3+/Yb3+ ions in the lattice of Sb2Se3 results in nanorods while that in Lu3+/Er3+ leads to nanoparticles, respectively. The electrical conductivity of Co-doped Sb2Se3 is higher than the pure Sb2Se3, and increases with temperature. By increasing concentration of Ln3+ ions, the absorption spectrum of Sb2Se3 shows red shifts and someintensity changes. In addition to the characteristic red emission peaks of Sb2Se3, emission spectra of Co-doped materials show other emission bands originating from f-f transitions of the Yb3+ ions.