Tb3+ doped ZnMoO4 materials were synthesized by combustion method. XRD results show that the samples completely formed single ZnMoO4 phase at 700 ℃ which belongs to Trigonal, while the incorporation of Tb3+ does not affect the basic structure of ZnMoO4. The TG-DTA results show that the samples fully formed ZnMoO4 phase due to the energy absorption at about 680 ℃. IR results show that there were no other organic peaks after burning at 700 ℃, indicating that citric acid has been completely decomposed and Tb3+ ions have been fully integrated into the lattice of ZnMoO4. SEM results show that the dispersion of particles gradually increases along with the improvement of the temperature.The best excitation wavelength was 488 nm when the monitoring wavelength was 544 nm, which corresponds to the 5D4→7F5 transition of Tb3+. Finally, a valuable green fluorescent powder of ZnMoO4∶Tb3+ has been obtained.