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A stable δ- and β-bismuth trioxide was prepared at room temperature by vacuum vapor-phase oxidation. The average crystal size of products was 14.6 nm (by XRD), the d(0.5) value was in the range from 62 nm to 69 nm, and geometric standard deviation(GSD)was from 1.42 to 1.64. The results show that δ-Bi2O3 is formed when quenching rates is rapid and β-Bi2O3 is formed when it is slow. The size of grains increases with rising reaction temperature, flow rate of carrier gas, residual pressure of system and longer growing time of grains.