Nanostructured B2 intermetallic compounds NiAl and FeAl have been prep
ared by mechanical alloying (MA) the elemental powder mixtures and sub
sequent heating. The structural evolution during MA was monitored by i
n situ thermal analysis and X-ray diffraction (XRD). The final product
s were characterized by transmission electron microscopy (TEM) and dif
ferential scanning calorimetry (DSC). The results show that the nanocr
ystalline intermetallic compound NiAl, which is difficult to disorder
by milling, was synthesized directly after an exothermic explosive rea
ction; whereas FeAl compound was formed after a thermal process of asm
illed Fe(Al) solid solution obtained through interdiffusion during MA.
The large heat of formation of NiAl compound is the main driving forc
e for the exothermic explosive reaction, and the difference in diffusi
vity between Ni-Al system and Fe-Al system is suggested to be the main
cause of the different behaviors of formation between NiAl and FeAl c
ompounds by MA.