A typical hybrid nanostructure was prepared consisting of lead sulfide (PbS) nano-crystals, embedded in titanium oxide (TiO2) using sol-gel method. The synthesis procedure was monitored by Fourier transform infrared spectroscopy Spectroscopic investigations indicated that PbS nano-crystals are embedded in the TiO2 matrix with no strong Ti-O-Pb-S bonding. The size PbS hybrid nanostructures decreased with diminishing lead and sulfur mole concentrations. The smallest size of NCs has been obtained in 10% of mole concentration (30-45 nm particle size for the hybrid nanostructure) The morphology and microstructure of the nano hybrid was investigated by scanning electron microscope and X-ray diffraction (c) 2010 Elsevier B.V All rights reserved.