A simple combustion process has been proposed to systematically synthesize Ca3((P, V)O4)2: Eu3+. All the Ca3((P, V)O4)2: Eu3+ products were characterized by x-ray diffraction (XRD), scanning electron microscopy (SEM) and fluorescence spect rophotometer. The results indicate that Ca3((P, V)O4)2: Eu3+ phosphor particles is special morphology with quadrate of length 2.5 μm and breadth 1 μm. From the photoluminescence spectra for Ca3((P, V)O4)2: Eu3+, the remarkable emission transition 5D0 – 7F0 are assigned to Eu3+ ions substituted for Ca2+, and the most intense emission transition 5D0 – 7F2 indicates at noncenter symmetrical environment for Eu3+ ions. It was observed that the spectral features possess sharp and bright emission for a red emitting nanophosphors potential applications.