This work reports on the structural characterization and on the low-temperature upconversion spectroscopy of the nanophosphor prepared by thermal decomposition of a polymeric resin (Pechini’s method [U.S. Patent No. 3,330,697 (July 11 1967)]). The average particle size evaluated from transmission electron microscopy lies in the range of . The high-resolution upconversion luminescence spectrum at in the ultraviolet to near infrared (UV-NIR) spectral regions shows narrow lines, characteristic of transitions occupying both sites with point symmetries and in the oxide cubic system. The excitation spectrum at in the IR region was used to monitor the green upconversion and IR luminescences and it displayed Er and Yb lines. Power dependence measurements at 298 and indicate that the main upconversion mechanism is a two-photon excitation process. The temperature dependence of the upconversion luminescence shows a decrease in the emission intensity with increasing temperature, and such decrease is much more evident for the emission in the violet than in the green and the red regions.