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Nanoparticle composite microspheres are a versatile material with unique features and wide-ranging applications, including catalysis, biological medicine, and electronic devices. The adsorption behavior of nanoparticles on the surface of microspheres plays a crucial role in determining the further application potentials. The understanding of nanoparticle adsorption behavior on microsphere surfaces is essential for guiding future applications in nanoparticle composite microspheres. In this work, the adsorption behavior of unstable copper nanoparticles (Cu NPs) on polystyrene-based (PS-based) microspheres was investigated. The influence of PS-based microspheres’ surface properties and the oxidation degree of Cu NPs were determined. The adsorption mechanism of Cu NPs on PS-based microspheres was analyzed. Furthermore, the amounts and rates of adsorption were examined. It was found that the Cu …