In this research, the mechanism of mechanical alloying (MA) synthesis of TiFe intermetallic compound (IMC) from individual components Ti and Fe has been studied. The partition coefficient of the apparent diffusion and the reaction rate constant during MA solid-state synthesis of the TiFe intermetallic compound in a planetary ball mill have been estimated. The results indicate that the apparent diffusion coefficient is close to 10–11 cm2/s that is approximately one order higher than the conventional high temperature diffusion coefficient. The reaction rate constant is close to 1.75·10−6. The relation between the structure and the hydrogen storage properties of MA synthesized IMC TiFe have been briefly discussed