We had made CaAl4O7:Tb3+, Ce3+ samples by sintering the sample at 1,300 degrees C in reduction environment N2 + 5% H2. Emission lines corresponding to the 3D4 to 7Fj(J = 6,5,4,3) optical transitions of the Tb2+ ions were observed at 485,545,590 and 620 nm respectively. The particle size of the sample was controlled to less that 1 micron. The lattice of the sample was rather regular in atomic scale and showed very good quality. CaAl4O7:Tb3+, Ce3+ materials can reduce structure uncertainty of the host and remain typical optical properties of the Tb3+ emitting center.