LnxSb2-xS3 (Ln: Yb3+, Er3) based nanomaterials were synthesized by a co-reduction method. Powder XRD patterns indicate that the LnxSb2-xS3 crystals (Ln = Yb3+, Er3+, x = 0.00-0.09) are isostructural with Sb2S3. The cell parameter a and c increase for Ln = Er3+ and Yb3+ upon increasing the dopant content (x), while b decreases. SEM images show that doping of the lanthanide ions in the lattice of Sb2S3 result in nanoflowers and nanoparticles. Emission spectra of Yb3+ doped materials, in addition to the characteristic red emission peaks of Sb2S3 emission, show other bands originating very probably from the 2F5/22F7/2 in case of Yb3+ doped crystals.The electrical conductance of Ln-doped Sb2S3 is higher than pure Sb2S3 and increase with temperature.