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Abstract: Hollow core–shell MoO2 microspheres were successfully synthesized via a simple one-pot template-free approach for the first time. The crystalline structure of the products was characterized by Powder X-ray diffraction (XRD), the morphology and particle size of the products were analyzed by Transmission Electron Microscope (TEM). The microsphere formation mechanism was discussed, and an Ostwald ripening accompanied by self-assembly process was proposed for the formation of the core–shell and hollow structures. When used as an anode material for lithium ion battery, this unique MoO2 structure could store large amount of Li+, and cycled well. The electrochemical performance of core–shell MoO2 microspheres was much better than that of bulk MoO2. [Copyright &y& Elsevier]