Semiconductor nanocrystals (NCs) are of great interest for both fundamental research and technological applications. Because of the unique optical and electrical properties the semiconductor NCs are likely to play a key role in the emerging new field of nanotechnology in applications from optoelectronics to chemical sensing devices [1,2]. Until now, there have been reported various methods for the preparation of metal sulfide nanomaterials such as employing biphasic solvothermal interface reaction [3], polymer assisted reaction [4], sonochemical methods [5], microwave irradiation [6], micro emulsions [7], gamma-ray irradiation [8] and so forth. In this study, TGA as a surfactant and TAA as a reducing agent were mixed with lead (II) nitrate to obtain PbS nanoparticles. Products were characterized by IR, AFM, TEM, EDAX, X-RD and PL analysis.