Fissile molybdenum dioxide (MoO 2 ) was synthesized using a rheological phase reaction as a novel method suitable for a large scale up. The oxalate precursor was initially prepared at 80°C and was treated at different temperatures. The physical characterization was carried out by thermogravimetry and differential thermal analysis (TG/DTA), X-ray diffractometer (XRD) and scanning electron microscope (SEM). The results of TG/DTA and XRD indicate that the oxalate precursor begins to yield MoO 2 at 250°C and a single phase MoO 2 with monocline symmetry is formed at 350°C. The electrochemical characteristics of fissile MoO 2 as an anode material for lithium batteries have also been studied and the morphological properties were found to play an important role in the cycling stability. The activated MoO 2 displays 484mAhg −1 capacity in the initial charge process with a capacity retention of 83.1% after 40 cycles in the range of 0.01–2.00V versus metallic lithium at a current density of 100mAg −1 . The SEM results reveal that there is a correlation between the cycling performance of the MoO 2 powders and their morphological properties.