Metastable hexagonal molybdenum trioxide has been synthesized by chemical precipitation and hydrothermal treatment at low temperature. X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM) were used to characterize the product, which has a unique hexagonal prism-like morphology. Excellent electrochemical performances were exhibited: the first reversible discharge specific capacity can reach 402 mAh g(-1) versus Li metal at 0.1 mA cm(-2) (voltage range 1.2-4.0 V). (C) 2005 Elsevier Ltd. All rights reserved.