Effect of sonication time on the synthesis of the CdS nanoparticles within the matrix obtained through the covalent functionalization of multiwall carbon nanotube (MWCNT) with maleic anhydride (MA) - 1-octene copolymer was investigated. Cadmium chloride and thiourea were used as the raw materials. MWCNTs used for the matrix were synthesized by Catalytic Chemical Vapor Deposition using Fe-Co/Al2O3 as the catalyst. The obtained nanostructures were characterized by FTIR, XRD, Raman spectroscopy, TEM, SEM, TG and UV-Vis spectroscopy. Electrophysical properties of the polymer nanocomposites obtained using different periods of time for sonication were comparably investigated. The average CdS particle diameter was between 3.9-7.9nm as confirmed independently by TEM and XRD. UV-Vis spectroscopy revealed that the obtained nanostructures are appropriate base materials for making optical devices.