TiNb 2 O 7 and TiTa 2 O 7 phases are synthesized by solid-state reaction method and are investigated for electrochemical Li insertion/extraction. The electrochemical insertion of Li in these phases is characterized by both solid solution and two-phase regimes. The structure is stable toward Li insertion/extraction. The first cycle discharge capacity values are 307mAhg −1 and 215mAhg −1 in the voltage range of 3.0–1.0V for TiNb 2 O 7 and TiTa 2 O 7 phases, respectively. The discharge capacities of TiNb 2 O 7 and TiTa 2 O 7 are 212mAhg −1 and 100mAhg −1 , respectively, after 20 cycles.