Fluorocarbon finishing agents were prepared by γ-ray initiated emulsion polymerization of fluorine-containing acrylates at different doses. Copolymerization of the fluorocarbon monomer and butyl acrylate was also studied. Morphology and size distribution of the emulsion particles were investigated by transmission electron microscopy and dynamic light scattering, respectively. Influence of fluorine-containing monomer on water and oil repellency property of final products was discussed. It was found that conversion of the dodecafluoroheptyl methacrylate was 98% at 5kGy and hexafluorobutyl acrylate was fully polymerized at 10kGy. Water repellency of the emulsion product derived from dodecafluoroheptyl methacrylate was Grade six and the oil repellency was Grade three.