Abstract: The MnCo₂O_4.5 hollow microspheres were synthesized in one step via a combination of template and hydrothermal methods, with glucose as sacrificial template and metal chlorides as precursors.The influence of the reaction conditions, including the glucose concentration, molar ratio of glucose to metal chloride, reaction temperature/time, addition of acetic acid catalyst, on the size and surface microstructures of MnCo₂O_4.5 hollow microspheres was investigated with scanning electron microscope, X-ray diffraction and energy dispersive spectroscopy.The preliminary results show the reaction conditions have a major impact.To be specific, under the conditions, including a temperature of 180℃, a heating time of 12 h and a proper glucose concentration, good hollow microspheres, comprising the spherical shell~20 nm in thickness and formed of MnCo₂O_4.5 nanoparticles~30 nm in size, were synthesized after high temperature calcination in air for removal of carbonaceous cores.