In this paper, we report on the annealing temperature dependence of the upconversion (UC) phosphor of TiO 2 -ZnO doped with Yb 3+ and Tm 3+ . We prepared samples using metal-organic decomposition (MOD) solutions and Tm 2 O 3 powder, which were analyzed in terms of their photoluminescence (PL) spectra and crystal structures. The PL spectra showed a blue UC phosphor band at a wavelength of 476 nm. The emission intensity was greatest after annealing at 850 °C. By analyzing the crystal structures using an X-ray diffractometer (XRD), it was found that there was a large amount of RE 2 Ti 2 O 7 in the samples annealed at 900 ℃ and above.