Carbon-coated Fe-Mg-homogeneously dispersed Li(Mn0.9Fe0.10)(1 -aEuro parts per thousand x) Mg (x) PO4/C (x = 0.00, 0.01, 0.03, 0.05, and 0.07) powders are synthesized via a mechano-chemical liquid-phase activation technique. Fine-sized and Fe2+ and Mg2+ evenly distributed precursors are formed using this efficient approach successfully. The synthesis temperature and the Mg2+ doping ratio are investigated and optimized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy, and electrochemical measurements. Mg doping decreases the lattice parameters of LiMn0.9Fe0.1PO4/C, which will ease the expansion/shrinking effect during the insertion/de-insertion processes. Li(Mn0.9Fe0.1)(0.95)Mg0.05PO4/C synthesised at 700 A degrees C with similar to 3 wt% of carbon additive presents the best comprehensive electrochemical properties, and it displays good rate capability with specific discharge capacity of 153 mAh g(-1) at 0.1C, 140 mAh g(-1) at 1C, and 132 mAh g(-1) at 2C rate. The results suggest that the electrochemical performance of the LiMnPO4-based cathode is improved as (Mn0.9Fe0.1) is partially substituted by Mg.