In the present work, systematic study of series of NiOx GDC_(1-x) where x = 0.1–0.6; has been reported for the first time. For the synthesis of homogeneous NiO–GDC nanocomposite powders, the nano-powders of NiO and Ce _0.9 Gd _0.1 O _1.95 (GDC10) synthesized by solution combustion synthesis were mixed in mol % proportion. NiO–GDC nanocomposite can be reduced in situ to form Ni–GDC cermet anode. Hence the Ni–GDC cermet anode combines the catalytic activity and high electronic conduction property of Ni and ionic conductivity of GDC. Nano-crystalline constituents in the NiO–GDC nano composite are believed to give better anodic performance than microcrystalline constituents. Hence the efficient study of the atomistic structure and the accurate characterization of the structural parameters, such as crystallite size and internal strains, are of considerable interest. Therefore the NiO_x–GDC1 _1-x nanocomposite powders were characterized by XRD and FTIR spectroscopy. Further these powders were pelletized, sintered and characterized by FE-SEM and d.c. conductivity.