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Cubic and monoclinic Gd2O3:Eu 3+phosphors in the range of nano-scale and submicron-scale were prepared by a modified solution combustion method. Coexistence of cubic and monoclinic phases was found in the highest luminescent sample synthesized at 600℃. In relation to commercial sample, the relative luminescence intensity was 49.8%. The shape of emission spectrum of the sample thus changed and the charge-transfer-state band of excitation spectrum slightly shift toward higher energies. With increasing the annealing temperature, phase transformation and correlative optical properties of Gd2OP3:Eu3+ phosphors were studied. It was found that the samples were dominated by cubic structure and monodinic structure at temperatures below and above 900℃.