以钼粉、羰基铁粉、无定形硼粉和硼铁粉为原料,采用真空烧结法制备了Mo2FeB2粉体.利用X射线衍射仪(XRD)、扫描电子显微镜(SEM)分析产物的物相演变规律和微观形貌,取得以下结果:在1400℃下反应2h可以得到相组成单一的Mo2FeB2粉体；用硼铁粉代替羰基铁粉为铁源可以大幅降低反应产物的颗粒和晶粒尺寸,并减少其晶格畸变,制备的Mo2FeB2粉体颗粒尺寸为5μm左右,晶粒尺寸在64nm左右.
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