The invention discloses a rare earth doped sodium lutetium fluoride up-conversion luminescence nano-material. The molecular formula of the nano-material is represented by NaLuF4:Ce,Yb,Eu, wherein a molar ratio of Lu:Ce:Eu:Yb is (83-X):X:15:2, and X is any number in a range of 0 to 10; and the particle size of the nano-material is 6-12 nm, the nano-material is in a monodisperse state in n-hexane or cyclohexane, and nano-particles have an irregular spherical or orthohexagonal morphology. The invention also discloses a preparation method of the nano-material. A series of NaLuF4:Ce, Eu,Yb up-conversion luminescence nano-material doped with different proportions of Ce<3+> is synthesized by using the method. Experiments prove that the up-conversion luminous efficiency of the nano-material is affected by the doping proportion of the doped element Ce, so a new way is provided for the development of the novel up-conversion nano-material, and the nano-material has a wide application prospect.