The practical application of Ti-Al system intermetallic compounds is expected as an advanced light heat resistant material. TiAl group out of them, as for the specific strength, has an equivalent maximum working temperature as that of the nickel base alloy, which is utilized as a turbine material for the current aircraft, and moreover it is also said that it is superior in the creep and rupture properties to the latter. In this study, by mechanical alloying (MA) of each mixed powder of Ti-Al and Ti-B, by suing heptane as a grinding aid, each MA powder of the amorphous TiAl containing carbon and extremely fine compound TiB2 were prepared, and subsequently the true density sintering by the hot isostatic pressing (HIP) was performed, and by doing these, the preparation of TiAl/TiB2 system composite material with a high composite ratio of TiO2 was tried. Consequently, by the MA treatment of the mixed powder of Ti and B for more than 50 hours, the compound powder of TiB2 mixed with TiB could be prepared, and its hardness has shown the maximum value Hmv=l200 with a composition of TiAl/25 mol % TiB2. 14 refs., 10 figs., 2 tabs.