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Tetragonal phase NaLn(MoO4)2 (Ln = Yb, Tm, Er, Y, Dy, Gd, Eu, Sm, and Ce) submicrocrystals were successfully synthesized by a hydrothermal method. It was found that higher reaction temperature and larger ionic radius of RE ions are beneficial for the formation of NaLn(MoO4)2 submicrocrystals. NaY(MoO4)2 was demonstrated to be a good host material for different lanthanide ions. In the up-conversion luminescence spectra of NaY(MoO4)2:Yb3+/Er3+ under 980 nm excitation, the green emissions (2H11/2/4S3/2 → 4I15/2) were observed and the red emission (4F9/2 → 4I15/2) completely vanished, which could be attributed to the efficient cross-relaxation of 4I11/2 + 2G7/2 → 4F7/2 + 2H11/2/4S3/2 between Er3+ ions. In the up-conversion luminescence spectra of NaY(MoO4)2:Yb3+/Tm3+, the blue emissions (1G4 → 3H6 and 1D2 → 3F4) were observed and the near-infrared emission (3H4 → 3H6) completely vanished, which could be attributed to the inefficient nonradiative relaxation of 3F2,3 → 3H4. In addition, the down-conversion luminescence properties of NaY(MoO4)2:Eu3+ were studied in detail.
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