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Selenium-containing polystyrene (DSe-PS) microspheres were synthesized by soap-free emulsion polymerization using 1,2-bis(2,3,5,6-tetrafluoro-4-vinylphenyl)diselane (FVPDSe) and divinylbenzene (DV as crosslinking agents. The particle size of the obtained DSe-PS was characterized by a scanning electron microscope and dynamic light scattering. The results showed that the diameter of the obtained DSe-PS microspheres could be adjusted by changing the ratio of the monomer and crosslinker/water. The diselenide moiety in the obtained DSe-PS mic