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In this work, GdAlO3:Pr3+ was successfully prepared by the Pechini method at lower temperatures when compared to others methods such as solid-state synthesis and sol-gel process. In accordance to the XRD data, the fully crystalline single-phase GdAlO3 could be obtained at 900 °C. Luminescence measurements indicate Gd → Pr3+ energy transfer. In the emission spectra, the 3P0 →3 H4 (blue emission) and 1D2 →3 H4 (red emission) transitions of Pr3+ ions can be observed and the ratio between their intensities depends on the Pr3+ content due to the cross-relaxation phenomenon.