The amorphization process during mechanical alloying (MA) was investigated for the Al-50at%Ti and Al-50at%Ti-10vol%TiB2 powder mixtures. Pure metallic powders of Al and Ti were finely mixed and transformed to the amorphous phase after being milled for about 2880 ks. In the case of Al-50at%Ti-10vol%TiB2 powder, the amorphous alloys with a fine dispersion of TiB2 particles could be obtained for a shorter milling times than that required for the powders without TiB2 ceramics. As a result of heat treatment for the mechanically alloyed amorphous powders, a nanocrystalline intermetallic compound of TiAl (gamma) could be produced. Subsequent grain growth of the gamma phase during heat treatment was investigated by estimating the grain-growth exponent and the activation energy for grain growth. It was found from this estimation that the grain growth was further suppressed as the powders were mechanically alloyed for longer times. Furthermore, the addition of the TiB2 particles that could be dispersed during MA finely and homogeneously in the amorphous matrix was found to be effective for suppression of the gamma grain growth especially at elevated temperatures as well as for a long annealing.