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The present study reports on a versatile method of the preparation of polystyrene−ZnO composite particles with core−shell or raspberry-like morphology. SEM analysis revealed that ZnO has been deposited on the surface of functionalized polystyrene beads as either a continuous thin layer or small clusters, depending on the reaction parameters. We propose that the interaction between ZnO nanoparticles and β-diketone groups, present on the surface of polystyrene beads, is the driving force for the preparation of these composite particles. IR spectroscopy was used to prove the interaction between ZnO nanoparticles and β-diketone groups. X-ray diffraction of the PS/ZnO particles revealed diffraction peaks corresponding to wurtzite ZnO crystalline phase. TGA results demonstrated that the ZnO contents of composite particles can be varied by changing the concentration of Zn(Ac)2·2H2O salt prior to reaction. The composite particles produced are envisioned to have applications as the building blocks for fabrication of sensors, transducers, actuators, UV detectors, and optoelectronic devices.