Li 2 Mn 1-x Fe x (PO 3 ) 4 (x=0, 0.2, 0.4, 0.6, 0.7) solid solution phase has been successfully prepared via solid-state reaction. The Rietveld refinement results indicate that the Li 2 Mn 1-x Fe x (PO 3 ) 4 (x=0, 0.2, 0.4, 0.6, 0.7) solid solutions with orthorhombic structure can be obtained and the lattice parameters (including a, b, c, and V) decrease with the increasing of Fe concentration. Partial substitution of manganese with iron enhances the electrochemical performance; there, the discharge-specific capacity of the samples obviously increases from 21 mAh/g for x=0 to 59 mAh/g for x=0.7, which is 85 % capacity of that one lithium removal. The cyclic voltammetric (CV) curves present the Mn 2+ /Mn 3+ redox couple situated at 4.6 and 1.8 V and Fe 2+ /Fe 3+ redox couple located at 4.3 and 2.3 V, which can be observed in cathodic and anodic sweeps. Such a low discharge potential value for M 2+ / M 3+ redox couple may be attributed to the zigzag [(PO 3 ) 1− ] n chains in this structure.