Abstract: Nanocrystalline intermetallic compound NiAl was Synthesized by evaporating NiAl master alloy in inert-gas followed by in situ compaction, and its structure was studied by means of X-ray diffractometry and transmission electron microscope. Experimental results reveal that the assynthesized nanocrystalline sample has a mean grain size of less than 10 nm and it is dominantly composed of the cubic structure phase NiAl. However, nanocrystalline Ni3Al as a trace phase mixed in NiAl phase, was also detected by transmission electron microscope observation.