The green synthetic route for the synthesis of semiconductor nanoparticles has received special attention recently due to its features, such as low cost and environmental friendliness. The (Z)-2-(pyrrolidin-2-ylidene)thiourea was used as a ligand and allowed to react with zinc acetate to form the ZnS nanoparticles through the homogeneous precipitation method. The polyvinyl pyrrolidone and polyethylene glycol were employed as capping agents, whereas the ammonium solution was used as an activator for the stabilizers. The effects of the concentration of the capping agents on ZnS nanoparticles were investigated. The poly ethylene glycol (PEG)- or (polyvinylpyrollidone) PVP-capped zinc sulfide nanoparticles were then incorporated with polydadmac to form the polymer nanocomposites. The results from various sophisticated instruments, such as spectrophotometer (UV-Vis), photoluminescence (PL), Fourier transform infrared (FTIR), X-ray powder diffraction (XRD), transmission electron microscope (TEM), and scanning electron microscopy (SEM), reveal that the concentrations of capping agents and ammonium solution has great effects on nanomaterials.