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The YP x V 1-x O 4 (x = 0.3~0.9) assembled spheres with tetragonal phase were prepared hydrothermally under a simple and mild method by the assist of EDTA. The structures and shapes of the prepared samples were significantly affected by the reaction conditions (hydrothermal treatment time, organic additive, pH value and the amount of EDTA in the synthesis solution). The characteristic emission of the spherical YP x V 1-x O 4 : Ln 3+ (Ln = Eu, Sm, Dy or Tm) phosphors were investigated in detail. The results showed that the light color of the YP 0.3 V 0.7 O 4 microspheres can be easily adjusted by doping different lanthanide activators; Y 0.93 Sm 0.07 P 0.3 V 0.7 O 4 and Y 0.95 Eu 0.05 P 0.3 V 0.7 O 4 exhibited strong orange-red and red emission, respectively, and Y 0.93 Sm 0.07 P 0.3 V 0.7 O 4 has a higher quantum efficiency of 76.8 %. For the Y 0.97 Dy 0.03 P x V 1-x O 4 (x = 0.3~0.9) samples, both emission intensities of Dy 3+ and VO 4 3-increase as increasing the P amount, and the quantum efficiency of Y 0.97 Dy 0.03 P 0.9 V 0.1 O 4 can reach 92 %. It can also be found that the light color of the Y 0.97 Dy 0.03 P x V 1-x O 4 samples can be tuned by changing the ratio of P/V, and Y 0.97 Dy 0.03 P 0.5 V 0.5 O 4 can emit the white light under UV excitation.

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