Nanoparticle LiTi2(PO4)3 was prepared by solvothermal and calcination methods. LiTi2(PO4)3-xh(x = 5, 7, 9, 13) was successfully synthesized under different calcination times in nitrogen atmosphere, and LiTi2(PO4)3–7h showed excellent rate and electrochemical performance. It delivered discharge capacities of 141.2, 119.9, 109.8, 98.2, 87.3, and 76.7 mAh·g−1 at rates of 0.5, 1, 2, 5, 10, and 20C, respectively. In particular, its initial discharge capacity can reach 123.3 mAh·g−1 at the high rate of 10C. Hence, these superior properties demonstrate that LiTi2(PO4)3–7h has great application advantages as a cathode for lithium-ion batteries.