In this study, un-doped and Ni-doped MgO nanoparticles have been synthesized, through a simple precipitation method. To investigate the effect of Ni-doping on the structure of MgO, the obtained nanoparticles were characterized using scanning electron microscopy (SEM). Plate/slice-like morphology was clearly observed in the SEM micrographs. FTIR studies also frequency number 841.06 cm-1 appeared in the stretching vibration of metal oxides Mg-O. The irregular nano-sheets that are assembled together by weak interactions provide the plate-like morphology with an increase in unsaturated Ni atoms, oxygen vacancies, and defect sites which render the plate-like MgO more active for catalytic reactions.