Eu³⁺ doped sol-gel-precipitation methods prepared ZnO/ZnS red phosphors. XRD, FTIR, TEM, and EDS test methods characterized the structure of the red phosphors at different temperatures. The results showed that the red phosphors contain ZnO and ZnS, samples of the hexagonal phase structure. The luminescent properties and mechanism of the red phosphors were discussed by fluorescence spectrometer. The results showed that combining ZnO and ZnS can form new band structures and increase the composite probability, thus improving the luminescent properties of the red phosphors. Eu³⁺ was located in the non-inversion central lattice in the phosphors, which is dominated by the electric dipole transition ⁵D₀-⁷F₂. The optimal Eu³⁺ doping amount of the phosphor is 0.1 (molar fraction), and the optimal annealing temperature is 800 ℃.