RECENTLY, MUCH INTEREST WAS AROUSED IN SYNTHESIS OF SEMICONDUCTING NANOPARTICLES INTENDED FOR APPLICATION IN MODERN MICROELECTRONIC DEVICES. THE POSSIBILITY OF PRODUCING SEMICONDUCTING NANOPARTICLES WITH CONTROLLABLE SIZE AND SHAPE IS BEING EXTENSIVELY STUDIED.PBS HAS BEEN WIDELY USED IN MANY FIELDS SUCH AS PB+2 ION SELECTIVE SENSOR, IR DETECTORS, SOLAR ABSORBER AND PHOTOGRAPHY [1]. PBS@SIO2 Core-shell NANOPARTICLES WERE SUCCESSFULLY SYNTHESIZED BY THE SIMPLE WET CHEMICAL METHOD. THE SYNTHESIZED PRODUCT HAS BEEN CHARACTERIZED BY POWDER X-RAY DIFFRACTION (XRD), UV–VIS SPECTROPHOTOMETRY, FTIR SPECTROSCOPY, SCANNING ELECTRON MICROSCOPY (SEM), TRANSMISSION ELECTRON MICROSCOPY (TEM), ENERGY DISPERSIVE X-RAY SPECTROSCOPY (EDX). THE CRYSTALLINITY OF THE SIO2 SPHERES, PBS/SIO2 CORE–SHELL NANOSTRUCTURES WERE STUDIED BY XRD.