Zn1-x-yNaxCoyO thin films were prepared by pulsed laser deposition (PLD) on Si(111) substrates. The X-ray diffraction(XRD), atomic force microscopy(AFM), fluorescence spectrometer and the Four-probe tester were used respectively to investigate the structure, surface structure, optical and electrical properties of the thin films. The optical and electrical properties of Zn1-x-yNaxCoyO doped with different Na-Co concentrations are investigated. The result indicates that the structure of films are zincite and the doping of Na-Co leads to the red-shift of the UV emission peak of ZnO. When the doping concentration of both Na and Go are 10%, the film has the highest fluoresence intensity located at 397 nm, and the lowest resistivity of 8.34×10-1 Ω ·cm is detected in this film. The reasons of above-mentioned phenomena are discussed in depth.