TiB$_2$powders were prepared by mechanical alloying, and the effect of Zr and Ta substitution for Ti was investigated. It was possible to produce titanium diboride phase by mechanical alloying titanium and boron elemental powders for 280 hours. The amorphization reaction, a common process which occurs during mechanical alloying, has not been found. When zirconium of which atomic radius was larger than that of titanium was substituted for Ti, the alloying time was greatly reduced. On the contrary, substitution of tantalum for titanium prolonged the alloying time because of the less negative heat of formation of tantalum diboride than that of titanium diboride.