Mesoporous iron phosphates were synthesized using sodium dodecyl sulfate (SDS) and cetyltrimethylammonium bromide (CTAB) as surfactants. The material synthesized in the presence of SDS was not applied as a positive electrode active material of a lithium battery. The results show that the obtained FePO has a mesoporous structure with a specific surface area of 70 m g and a dominant pore diameter of 3 nm. Those mesoporous were characterized by different microstructural and electrochemical analyzes. Among the materials studied under different conditions, those calcined at 450°C preserve mesoporous structures and exhibit the best electrochemical performance when used as active materials of the positive electrodes of lithium batteries. Effectively, a relatively high specific capacity of 135 and 122 mAh g was registered at C/20 collected experimentally by the samples synthesized in the presence of SDS and CTAB, respectively.