Eu3+ and Sm3+ activated double molybdates, NaLa(1-x)Rx(MoO4)(2) (R = Eu, Sm) and NaEu1-xSmx(MoO4)(2), were prepared by solid-state reaction technique, and the photoluminescent properties were investigated. The results showed that the samples NaLa1-xEux(MoO4)(2) and NaEu1-xSmx(MoO4)(2) exhibit efficient red-emitting under near UV excitation. Because the phosphor NaEu0.92Sm0.08(MoO4)(2) shows higher intensity of Eu3+5D0 --> F-7(2) emission under either 395 (the F-7(0) --> L-5(6) transition of Eu3+) or 404 (the H-6(5/2) --> K-4(11/2) transition of Sm3+) nm excitation, with broadened absorption around 400 nm and appropriate Commission Internationale de l'Eclairage, International Commission on Illumination chromaticity coordinates (x = 0.66, y = 0.34d, it is considered to be a potential red-emitting phosphor for GaN-based light-emitting diode (LED). (C) 2005 The Electrochemical Society.