ZnO is a direct wide band-gap Ⅱ-Ⅵ semiconductor material. For decades, ZnO has gained more and more attention as a wide band semiconductor. This paper introduced a modified homogeneous precipitation method to prepare sheet Ni-doped ZnO crystal. The preparation process was studied and the mechanism of this method was discussed. The properties of the sheet Ni-doped ZnO crystal and the effects of growth parameters on the quality of sheet Ni-doped ZnO crystal were studied using XTJ30-micro image manipulation system, thermal analysis system, X-ray diffraction. etc.