In this work, we present a novel approach for synthesis of europium (III)-doped SrR 2 O 4 :Eu 3+ (R=Y, Lu) superfine phosphor with a precursor prepared in water-in-oil microemulsion. The precursor of oxalates formed in a reaction between Sr(NO 3 ) 2 -Y(NO 3 ) 3 (Lu(NO 3 ) 3 )-Eu(NO 3 ) 3 and H 2 C 2 O 4 in reverse microemulsions composed of OP-10, iso-pentanol, cyclohexane and water. X-ray diffraction results confirmed the formation of SrY 2 O 4 :Eu 3+ and SrLu 2 O 4 :Eu 3+ at 1000 °C and 900 °C respectively. FE-SEM images showed the superfine powder of SrR 2 O 4 :Eu 3+ has a rugby-like shape and a diameter of 70–100 nm. Upon excitation with 257–272 nm UV light, all the SrR 2 O 4 :Eu 3+ (R=Y, Lu) powders show bright red emission due to the 4f–4f transitions of Eu 3+ ions, and the highest photoluminescence intensity at 618 nm for SrY 2 O 4 :Eu 3+ and 615 nm for SrLu 2 O 4 :Eu 3+ was found at a content of about 9 mol% Eu 3+ and 6 mol% Eu 3+ respectively. Splitting of the 5 D 0 → 7 F 0 and 5 D 0 → 7 F 1 emission transitions revealed that the Eu 3+ ions occupied two nonequivalent sites in the crystalline lattice by substituting Y 3+ or Lu 3+ ions.