以湿法制得的斜方晶型三氧化二锑（Sb₂O₃）为原料，采用真空加热法制备了立方晶型的三氧化二锑。采用X射线衍射分析（XRD）和扫描电镜（SEM）对产物进行了表征，研究了体系压强、加热温度、加热时间对三氧化二锑晶型与粒度的影响。结果表明：当加热温度升高时，三氧化二锑由斜方晶型逐渐转变为立方晶型；但当加热温度升高至450 ℃时，已经全部转变为立方晶型的三氧化二锑中，部分立方晶型又开始转变为斜方晶型；随着加热温度的升高，样品团聚程度增加，样品的平均粒度逐渐增大。随着体系压强的下降和加热时间的延长，三氧化二锑由斜方晶型逐渐转变成立方晶型。但体系压强的下降，会增大样品团聚程度以及样品的平均粒度；加热时间延长，样品的平均粒度也逐渐增大。

Cubic Sb₂O₃ was prepared by vacuum heating method using orthorhombic Sb₂O₃ obtained by wet process as raw material.The effects of the system pressure，heating temperature and heating time on Sb₂O₃ crystal form and grain size were investigated by X-ray diffraction（XRD） and scanning electron microscopy（SEM）.The results showed that Sb₂O₃ was gradually changed from orthorhombic crystal to cubic crystal when the heating temperature was increased.When the heating temperature was rised to 450 ℃，some of cubic Sb₂O₃ began to change to orthorhombic Sb₂O₃ again.The agglomeration degree and average particle size of the sample were increased with increasing heating temperature.With the decrease of the system pressure and the extension of the heating time，Sb₂O₃ was gradually transformed from orthorhombic crystal to cubic crystal.However，the decrease of the system pressure would increase the degree of sample agglomeration and the average particle size of the sample.With the prolonged heating time，the average particle size of the sample was gradually increased.