The microemulsion AEO-9/butanol/cyclohexane/nitrate aqueous solution (or ammonium salt aqueous solution) was studied, which was used as micro-reactor in preparing long afterglow phosphor materials SrAl2O4: Eu2+ ,Dy3+. The phase behavior of microemulsion was investigated. The radius of inner water droplet Rw and the change of standard free energy ΔG*o→i were obtained by means of dilution method and theoretical calculation. The result shows that with the increase of W/S, the area of microemulsion region decreases, Rw and ΔG*o→i increase and the microemulsion stability decreases. The structure change and formation area of microemulsion AEO-9/butanol/cyclohexane/nitrate aqueous solution ( or ammonium salt aqueous solution) were offered for the adoption of a synthesis method with newly high efficiency and utility. The particular size and its distribution theory gist, fluorescence life-span, and quenching concentration parameter data were expected. A new approach was explored for finding a new preparation method of rare earths afterglow materials and increasing luminescence intensity without crashing.