A surfactant assisted co-precipitation method was employed for the preparation of nano crystalline NiO-MgO with high specific surface area. The effects of several process parameters such as refluxing time; refluxing temperature and calcination temperature were investigated on the structural properties of the powders. The prepared samples Were characterized by X-ray diffraction (XRD), N-2 adsorption (BET); temperature programmed reduction (TPR), thermal gravimetric analysis (TGA) and scanning electron microscopy (SEM) techniques. The obtained results showed that increase of refluxing time and temperature increased the specific surface area and decreased the crystallite size. The results revealed that the addition of surfactant has a significant effect on the synthesis of MgO nanocrystals and led to obtain a powder with high surface area. The powder prepared with a surfactant to metal molar ratio of 0.03 was employed as catalyst in methane reforming with carbon dioxide. (C) 2014 The Society of Powder Technology Japan. Published by Elsevier B.V. and The Society of Powder Technology Japan. All rights reserved.