Calcium aluminate phosphor co-doped Eu(2+), Dy(3+), Nd(3+) is prepared by the combustion method. We study systemically the influences of the quantity of mixed Dy(3+) ion, the quantity of flux H(3)BO(3), the differences in dispersing methods between magnetic stirring and ultrasonic dispersing and the combustion temperature on the long-persistence phosphor. The analytical results indicate that Dy(3+) ion improves the properties of the phosphors CaAl(2)O(4):Eu(2+), Nd(3+). The appropriate quantity of flux H(3)BO(3 )to( )reduce the forming temperature of the sample was determined. The monoclinic single phase of CaAl(2)O(4) formed at 500 degrees C and remained steady. The calcium aluminate co-doped Eu(2+), Dy(3+), Nd(3+) was synthesized by dispersal of the raw material using the ultrasonic method, and it had better optical properties.