IN THE LAST FEW DECADES, NANOSTRUCTURED SEMICONDUCTING MATERIALS HAVE ATTRACTED SIGNIFICANT ATTENTION IN SCIENCE AND TECHNOLOGY BECAUSE OF THEIR OUTSTANDING OPTICAL AND ELECTRICAL PROPERTIES AND EXTENSIVELY POTENTIAL APPLICATIONS IN DIFFERENT AREAS, INCLUDING MICROELECTRONICS, ELECTROOPTICS, PHOTOCATALYSIS, PHOTOELECTROCHEMISTRY, ENERGY CONVERSION AND BIOLOGICAL IMAGING [1, 2].AMONG THE SEMICONDUCTING MATERIAL, PbS IS A WELL-KNOWN P–P SEMICONDUCTOR WITH CUBIC CRYSTAL STRUCTURE AND NARROW BANDGAP (0.41 EV AT 300 K). LEAD SULFIDE HAVING A LARGE EXCITON BOHR RADIUS (18 NM) SHOWS STRONG QUANTUM-SIZE EFFECTS IN NANOCRYSTALLINE FORM AND HAS BEEN WIDELY USED IN OPTOELECTRONIC DEVICES [3, 4].IN THIS WORK, WE HAVE SUCCESSFULLYREPORTED A SIMPLE, CLEAN, CHEAP AND TEMPLATE-FREE SYNTHESIS ROUTE OF WELL-DEFINED PbS NANOSTRUCTURES VIA NEW PRECIPITATION METHOD USING PB (CH3COO) 2.3H2O AS A PRECURSOR AND THIOUREA AS A SULFUR SOURCE UNDER ALKALINE MEDIA. THIS EXPERIMENTS WERE PERFORMED IN TWO DIFFERENT TEMPERATURES (ROOM TEMPERATURE AND 70OC) AND IN THE PRESENCE OF SURFACTANT ORSURFACTANT-FREE CONDITIONS. THE STRUCTURE AND MORPHOLOGY OF AS-PREPARED PbS NANOSTRUCTURES WERECHARACTERIZED BY X-RAY DIFFRACTION (XRD), FIELD EMISSION SCANNING ELECTRON MICROSCOPY (FESEM) AND PHOTOLUMINESCENCE SPECTROSCOPY.