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采用Ｘ射线衍射、扫描电镜、显微硬度测试等多种分析测试手段研究了纯元素混合粉末Ｆｅ５０Ａｌ５０、Ｆｅ５０Ｎｂ５０及Ｆｅ７５Ｓｉ２５的机械合金化过程．结果表明：球磨３０ｈ后，Ｆｅ５０Ｎｂ５０转变为非晶结构，Ｆｅ７５Ｓｉ２５粉末形成具有ｂｃｃ结构的α－Ｆｅ（Ｓｉ）固溶体，Ｆｅ５０Ａｌ５０的球磨产物为α－Ｆｅ（Ａｌ）＋Ｆｅ３Ａｌ＋Ａｌ１３Ｆｅ４三组混合结构．延－延组合的Ｆｅ５０Ａｌ５０及Ｆｅ５０Ｎｂｂ２５０形成具有层片复合结构的粉末．其显微硬度在球磨初期迅速增高，延长球磨时间，增高速度减慢最后趋于稳定．而延－脆组合的Ｆｅ７５Ｓｉ２５粉末在球磨初期则形成具有弥散复合结构的粉末，其粒度变化在球磨初期与Ｆｅ５０Ａｌ５０及Ｆｅ５０Ｎｂ５０不同，无明显增大趋势．对Ｆｅ－Ｍ机械合金化的产物进行了热力学分析．
The mechanical alloying process of Fe50Al50, Fe50Nb50 and Fe75Si25 pure powders was studied by X-ray diffraction, scanning electron microscopy and microhardness test. The results show that the Fe50Nb50 is transformed into amorphous structure after ball milling for 30h, the α-Fe (Si) solid solution with bcc structure is formed by Fe75Si25 powder, and the mixed structure of α-Fe (Al) + Fe3Al + Al13Fe4 is the milling product of Fe50Al50. Delay-delay combination of Fe50Al50 and Fe50Nbb250 to form a laminated composite powder structure. The microhardness rapidly increased in the early ball milling, extending ball milling time, increase the speed slowed down finally stabilized. The ductile - brittle combination of Fe75Si25 powder in the early stage of ball milling with a dispersed composite structure of the powder, the particle size changes in the early ball milling and Fe50Al50 and Fe50Nb50 different, no significant increase in the trend. The thermodynamic analysis of the Fe-M mechanical alloying product was carried out.