Abstract In this work, the TiFe single phase alloy with CsCl-type structure was synthesized after 20 h of ball milling (mechanical alloying). Alloying process of mixture of Ti and Fe powders to the TiFe phase was discussed. It was found that synthesis of the CsCl-type TiFe phase followed the amorphous phase formation. Hydrogenation properties of obtained TiFe alloy were studied. It was found that the hydrogenation properties of TiFe synthesized by mechanical alloying were different from those of previously reported. The first plateau pressure was found at 0.5 MPa which is slightly higher than the value previously reported. However, the second plateau pressure was found at 25 MPa, which is much higher than the literature value. The maximum amount of hydrogen absorbed in the TiFe alloy was about 1.3 wt.% at 298 K.