Micrometer-sized MoO2 hollow spheres were synthesized hydrothermally with ammonium heptamolybdate tetrahydrate as molybdenum source, Cetyltrimethylammonium bromide as structure-directing agent and C2H5OH as reducing agent, respectively. The products were investigated by X-ray diffraction, thermo gravimetry and differential thermal analysis, scanning electron microscopy, transmission electron micraseopy and X-ray photoelectron spectroscopy. A morphology transition of ＂blocks-solid spheres-hollow spheres＂ during the growth procfess was observed and the possible mechanism for the formation of MoO2 samples was proposed to be through a microscale Kirkendall effcct.
