Dy3+ activated YPxV1-xO4 phosphors were synthesized via an in situ chemical co-precipitation process with fixed Dy3+ concentration (2mol%) and varying x (x = 0.2, 0.3, 0.4, 0.6, 0.7, 0.8, respectively). In order to obtain the hybrid' precursors, the rare earth coordination polymers with salicylic acid were used as precursors and the polyethylene glycol (PEG) was used as dispersing media. Their microstructure and micromorphology have been analyzed by X-ray powder diffraction (XRD) and scanning electronic microscope (SEM), which indicates that there exist some novel cobblestone-like microcrystalline particles. The characteristic transitions of Dy3+ due to F-4(9/2) -> H-6(15/2) (blue) and F-4(9/2) -> H-6(13/2) (yellow) were detected in the emission spectra and the yellow-to-blue intensity ratio decreased with the increase of x value. (c) 2005 Elsevier B.V. All rights reserved.