Novel green-emitting Yb 3+ and Tb 3+ co-doped LaNbO 4 particles were prepared through a facile sol-gel and combustion method. X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), thermogravimetric and differential thermal analysis (TG-DTA), up-conversion luminescence (UCL) with different powers and varied concentrations, and luminescent lifetimes were employed to test the prepared samples. The XRD data exhibit that a sample with high crystallinity can be acquired at 1000 °C. FE-SEM images show homogeneous and spherical grains after Yb 3+ and Tb 3+ are co-doped in the LaNbO 4 samples. TG-DTA reveals that the LaNbO 4 synthetic process is accompanied by a temperature increase. In our work, we utilize a 980 nm laser to excite Yb 3+ ions to achieve the 2 F 7/2 → 2 F 5/2 transition, and the LaNbO 4 :Yb 3+ , Tb 3+ sample exhibits intense green emission. Luminescent spectra at different powers demonstrated the two-photon absorption process; meanwhile, the corresponding energy transfer mechanism from Yb 3+ to Tb 3+ and the emission of Tb 3+ under 980 nm laser excitation was described via an energy level diagram. Moreover, concentration-dependent up-conversion luminescent properties were systematically explored, and it was confirmed that LaNbO 4 :0.15Yb 3+ ,0.02Tb 3+ exhibits the strongest luminescent properties. In particular, as the content of Yb 3+ ions increases, the 5 D 4 → 7 F 6 transition quickly becomes stronger, resulting in the emitted color shifting from green to blue. Therefore, the emitted color can be tuned by adjusting the content of Yb 3+ ions. The excellent up-conversion emission properties of the obtained samples allow for their potential application in the fields of 3D display technologies and 3 solid-state lasers.