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Red emitting Y2O3:Eu3+ (5 and 10 at.%) submicronic particles were synthesized through ultrasonic spray pyrolysis method from the pure nitrate solutions at 900 °C. The employed synthesis conditions (gradual increase of temperature within triple zone reactor and extended residence time) assured formation of spherical, dense, non-agglomerated particles that are nanostructured (crystallite size ∼20 nm). The as-prepared powders were additionally thermally treated at temperatures up to 1200 °C. A bcc Ia-3 cubic phase presence and exceptional powder morphological features were maintained with heating and are followed with particle structural changes (crystallite growth up to 130 nm). Emission spectra were studied after excitation with 393 nm wavelength and together with the decay lifetimes for Eu3+ ion 5D0 and 5D1 levels revealed the effect of powder nanocrystalline nature on its luminescent properties. The emission spectra showed typical Eu3+5D0 → 7Fi (i = 0, 1, 2, 3, 4) transitions with dominant red emission at 611 nm, while the lifetime measurements revealed the quenching effect with the rise of dopant concentration and its more consistent distribution into host lattice due to the thermal treatment.