The evolution of research on luminescent phosphors led to research on materials doped with rare earth ions (RE 3+), not only because of their photoluminescent properties, but also for their potential applications in photonics. The search for new photoluminescent materials has led to an investigation of the photoluminescence of RE 3+ present in an aluminum oxide (Al 2 O 3) matrix. This oxide has a transparent window on the short ultraviolet to near infrared, excellent mechanical properties and good chemical stability. Within this context, this work aims to obtain Al 2 O 3 : Er 3+ /Yb 3+. The preparation of Al 2 O 3 : Er 3+ /Yb 3+ involved two synthesis processes. For the co-precipitation process, rings of aluminum cans were used as precursors, and for the sol-gel process, the precursor used was tri-sec-butoxide aluminum. From the XRD results, high heat-treatment temperatures were observed to favor the formation of the α-Al 2 O 3 phase and low temperatures were observed to favor the formation the γ-Al 2 O 3 phase. The analysis of the photoluminescence emission spectra when excited at 980 nm, showed the up-conversion phenomenon with an emission in the visible region. The emission spectra also showed emission between 1400 and 1650 nm, with a maximum at about 1530 nm. The materials exhibit efficient energy absorption in the infrared region, with light emission in the visible region. Furthermore, the spectra show an intense emission in the infrared region assigned to the 4 I 13/2 → 4 I 15/2 transition of Er 3+ , demonstrating excellent potential to be used in optical amplifier device at the third telecommunications window.