We report the formation of MgCoSiO4 materials by a high-temperature solid-state reaction, a molten salt method and a mixed solvothermal approach. The preparation process had a profound effect on the morphology and particle size of the materials. Mesoporous MgCoSiO4 was obtained for the first time by the non-surfactant mixed solvothermal approach. The electrochemical intercalation of bivalent Mg2+ cations into MgCoSiO4 as an electroactive species for rechargeable magnesium batteries was further investigated. Preliminary electrochemical data indicated that mesoporous MgCoSiO4 had a higher peak current, a larger discharge capacity and a higher flat plateau compared with the corresponding bulk materials.