A composite of Cerium Gadolinium Oxide (GDC) and Nickel Oxide (NiO) was prepared by the co-precipitation method. The synthesized powder is the precursor of Ni-GDC which is a potential anode material for a Solid Oxide Fuel Cell (SOFC). X-ray diffraction results confirm the formation of GDC and NiO, as well as the nanometric dimensions of these formed phases. Mesoporous domains and high surface area are evidenced by the results of Nitrogen physisorption. The crystallinity of the powder and its agglomerated structure are graphically shown in the images obtained by the Scanning Electron Microscopy (SEM) and Transmission Scanning Microscopy (TEM). All these results indicate that co-precipitation is a suitable method for obtaining the GDC-NiO composite.