Abstract: The effects of glucose on the morphology of the microspheres of zinc oxide were first studied, and then 5% NiO/ZnO microspheric adsorbents were prepared by impregnation method and hydrothermal synthesis. The morphology and structure of NiO/ZnO microspheres were analyzed by N₂ adsorption, scanning electron microscopy (SEM), X-ray diffraction (XRD) methods, and the effects of the preparation method of NiO/ZnO microspheric adsorbents on the physicochemical properties were examined. Furthermore, Ni/ZnO microsphere adsorbent was prepared by reduction with H₂, over which the performance of adsorption desulfurization was tested in a fixed bed reactor by using thiophene as the sulfur compounds in model gasoline.The results show that the specific surface area and pore volume of the NiO-ZnO microspheric adsorbents prepared by hydrothermal method are as high as 40.45 m²/g and 0.096 cm³/g, respectively, in contrast to the ones prepared by the impregnation method, and the composite Ni-ZnO microspheric adsorbents exhibit a favorable desulfurization activity. Under the conditions including a temperature of 350℃, a pressure of 1.0 MPa, a volume space velocity of 6 h^-1, and a hydrogen to simulated oil volume ratio of 60, the sulphur contents in simulated oil decrease from 1.5×10^-4 to less than 10^-5. Also, the adsorbents boast a good regeneration capacity and a potential application value in industry.