In the present research two different kinds of nickel oxide/gadolinium-doped ceria (NiO-GDC) (I and II) nanocomposites were prepared by means of the sol-gel method. The Ni(II) complex (NiLH2), [Ni(pydc) (2) center dot 2 (pyda center dot H) center dot 2H(2)O], [pydc (2,6-Pyridinedicarboxylic acid), pyda (2,6-diaminopyridine)], and Ni(NO3) (2) center dot 6H(2)O have been used as precursors. Characterization of the products was carried out by Fourier transform infrared spectroscopy, scanning electron microscopy, energy-dispersive X-ray spectroscopy, transmission electron microscopy, X-ray powder diffraction, zeta potential, thermogravimetric analysis, and nitrogen adsorption-desorption Brunauer, Emmett, and Teller measurements. The X-ray powder diffraction results showed that the crystal lattice of compound (I) was obtained as a cubic fluorite structure and was found to have an average crystalline size of 48-63 nm. The comparison of the zeta potential of compounds (I) and (II) has shown that compound (I) can carry a more positive charge and is almost stable. The scanning electron microscope and Brunauer, Emmett, and Teller analysis of compound (I) revealed large homogeneous agglomerated pores and surface area. The results show that if compound (I) is used in solid oxide fuel cells, it could be a suitable material for the anode of solid oxide fuel cells.