Nanosized YPO4∶Eu3+ was prepared by precipitation method in different pH value solution and at different annealing temperatures, The results of XRD indicate that orient growth of (200) lattice surface exists in nanosized YPO4∶Eu3+ prepared in different pH after treated at 800 ℃, and in samples prepared in alkaline condition after annealed at 800 and 900 ℃, the orient growth of sample synthesized at 1000 ℃ was removed due to crystallized well. By applying the Scherrer formula, the mean particle sizes could be calculated as 20, 34, and 52 nm for samples prepared in alkaline condition after annealed at 800, 900 and 1000 ℃, the TEM image of sample prepared at 800 ℃ is consist with the result of XRD. The excitations and emission spectra of samples were studied. For samples prepared in lower pH value solution and lower treatment temperature, the 5D0-7F2/5D0-7F1 intensity ratios show a significant enhancement in emission spectra, and relative intensity of f-f transitions of Eu3+ ions are much stronger in excitation spectra, which are associated with the different local environment of Eu3+ ions.