利用高分辨电镜（ＨＲＥＭ）及场发射电镜纳米尺度成分分析技术（ＥＤＳ分析）研究了机械合金化和真空热压技术制备 的纳米 ＮＩＡＩ块体材料的微观结构． ＨＲＥＭ及 ＥＤＳ分析结果表明在球磨过程中形成第二相粒子 Ａｌ２Ｏ３分布于 ＮｉＡｌ晶粒内 部或边界上，分布于晶粒边界上的 Ａｌ２Ｏ３对晶界起钉扎作用，有效地抑制晶粒长大；此外，观察到纳米晶粒间存在无序区，这些 无序区也是抑制晶粒长大的一个因素 The microstructures of nano-NIAI bulk materials prepared by mechanical alloying and vacuum hot pressing techniques were studied by high resolution electron microscope (HREM) and field emission electron microscopy (EDS). The results of HREM and EDS show that the second phase Al2O3 formed during ball milling distributes inside or at the boundary of NiAl grains and the Al2O3 distributed on the grain boundaries acts as a pinning effect on the grain boundaries and effectively inhibits grain growth. In addition, it is observed that there is a disorder zone between the nanocrystal grains, and these disorder zones are also a factor that inhibits grain growth