通过机械合金化法制备了Ａｌ９４Ｖ４Ｆｅ２ 合金粉末， 该粉末由纳米尺寸的ｆｃｃＡｌ 相及非晶颗粒组成， 两者的尺寸分别为７ｎｍ 和１０ ｎｍ 。应用ＤＴＡ 方法检测合金粉末的热稳定性。合金粉末从非平衡相向平衡相转变经历了两个阶段。制备具有非晶颗粒和纳米ｆｃｃＡｌ 相共存结构的合金粉末的最佳工艺条件为４０∶１ 的球料比加７２ ｈ 球磨 Al94V4Fe2 alloy powder was prepared by mechanical alloying method. The powder consists of nanocrystalline fccAl phase and amorphous particles, and their sizes are 7nm and 10nm respectively. Application of DTA method to detect the thermal stability of alloy powder. Alloy powder transition from non-equilibrium to equilibrium phase has gone through two stages. The optimum process conditions for the preparation of the alloy powder with the coexistence structure of amorphous particles and nanocrystalline fccAl phase are the ball material ratio of 40:1 and the ball milling time of 72 h