CaS:Mn2+, Eu2+ phosphor materials were firstly synthesized in microwave field. The materials synthesized were characterized by XRD, SEM and the fluorescent spectroscopy. The experimental results of XRD and SEM show that the CaS:Mn2+, Eu2+ phosphors possess the crystalline structures with sphere, the mean grain sizes of phosphors are 250 similar to 400nm. The introduction of Mn2+ into CaS:Eu2+, makes the fluorescence of the CaS:Mn2+, Eu2+ phosphor efficiently enhanced since the energy transfer from Mn2+ into Eu2+ ions. This new synthesis method compared to the traditional high temperature solid reaction exhibits interesting features, such as rapid reactions without H-2-H2S protective atmosphere, phosphors with high purity, submicro-scale crystallines, and higher efficient luminescence.