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Natrium super ionic conductor (NASICON) materials providing attractive properties such as high ionic conductivity and good structural stability are considered as very promising materials for use as electrodes for lithium- and sodium-ion batteries. Herein, a new high-performance electrode material, Li0.5Ni0.5Ti1.5Fe0.5(PO4)3/C, was synthesized via the sol-gel method and was electrochemically tested as an anode for lithium ion batteries, providing enhanced electrochemical performance as a result of nickel substitution into the lithium site in the LiTi2(PO4)3 family of materials. The synthesized material showed good ionic conductivity, excellent structural stability, stable long-term cycling performance, and improved high rate cycling performance compared to LiTi2(PO4)3. The Li0.5Ni0.5Ti1.5Fe0.5(PO4)3/C electrode delivered reversible capacities of about 93 and 68% of its theoretical one at current rates of 0.1 C (6.42 mA·g-1) after 100 cycles and 5 C (320.93 mA·g-1) after 1000 cycles, respectively. Theoretically, three Li+ ions can be inserted into the vacancies of the Li0.5Ni0.5Ti1.5Fe0.5(PO4)3/C structure. However, when the electrode is discharged to 0.5 V, more than three Li+ ions are inserted into the NASICON structure, leading to its structural transformation, and thus to an irreversible electrochemical behavior after the first discharge process.