Eu³⁺-doped Gd₂O₂CN₂ was firstly synthesized by a classical solid-state reaction of Li₂CO₃, Eu₂O₃ and GdF₃ under NH₃ gas flow in the presence of graphite at low firing temperature. Powder X-ray diffraction (XRD) analysis indicated that Gd₂O₂CN₂: Eu³⁺crystallizes in a trigonal-type structure with space group P-3m1. Gd₂O₂CN₂: Eu³⁺ shows a sharp red emission band peaking at 626 nm under excitation at 300 nm at room temperature. PL spectra indicates that Eu³⁺ doped Gd₂O₂CN₂ samples emit the typical emission peaks at 614 nm and 626 nm originated from the hypersensitive electric dipole transition (5D0→7F2) of Eu³⁺ ions. The optimized doping concentration of Eu³⁺ ions was found to be 7.5 at. %, and the critical transfer distance was calculated to be 10.907 Å.