In this paper, Ho 3? /Yb 3? co-doped Sodium Gadolinium Fluoride (NaGdF 4 ) phosphors were synthesized by a facile and efficient hydrothermal method. The samples were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM), energy spectrum (EDS), and photoluminescence (PL). The results of XRD and SEM indicated that the prepared NaGdF 4 samples have the hexagonal structure and good orientation in the case of changing the concentration of Yb 3? . The results of pump power dependence of up-conversion intensity indicated that the energy transfer mechanism from Yb 3? to Ho 3? is a two-photon process. The energy transfer between Ho 3? and Yb 3? under 448 nm excitation was determined by PL spectra and fluorescence lifetimes. All the results proved that the doping of Yb 3? ions can effectively improve the upconversion luminescence of NaGdF 4 phosphors and achieve quantum cutting efficiency of up to 179.8%. Overall, NaGdF 4 :Ho 3? /Yb 3? have potential application in the field of optoelectronic materials.