用行星球磨对TiB2原粉进行处理,并用X射线光电子能谱仪,X射线衍射仪,能量色散X射线荧光光谱仪等对TiB2在球磨过程中的氧化行为进行分析。结果表明:在室温下TiB2粉末存在表面氧化,而球磨加速TiB2粉末氧化,随着球磨时间的延长,TiB2粉末的氧化程度加大;酸洗及离心作用造成硼的流失,使B和Ti的摩尔比失调,最终形成TiO2和少量硼酸包覆TiB2结构;通过改变不同球磨工艺,发现湿磨加Ar保护工艺使TiB2被氧化程度明显降低。 TiB2 powder was treated by planetary ball milling. The oxidation behavior of TiB2 in ball milling was analyzed by X-ray photoelectron spectroscopy, X-ray diffraction and energy dispersive X-ray fluorescence spectrometer. The results show that there is surface oxidation of TiB2 powder at room temperature, while ball milling accelerates the oxidation of TiB2 powder. With the extension of ball milling time, the oxidation degree of TiB2 powder increases; the loss of boron is caused by pickling and centrifugation, Than the imbalance, the final formation of TiO2 and a small amount of boric acid coating TiB2 structure; by changing the ball milling process and found that wet grinding and Ar protection process TiB2 oxidation was significantly reduced.