High ionic conductivity of doped ceria at comparatively lower operating temperatures (not, vert, similar650 °C) makes it suitable solid oxide fuel cell (SOFC) electrolyte. In the present investigation, successful attempt has been made to synthesize Ce0.9Gd0.1O1.95 (GDC10) solid solution by cost effective and simple chemical method of combustion where in the combustion of precursors results in the formation of nanoparticles relatively at lower processing temperature. The thermogravimetric study was carried out to understand the ignition temperature and optimize the fuel-to-oxidant ratio. The successful synthesis of single phase nanocrystalline GDC10 was confirmed by XRD, TEM and particle size analysis. Further SEM and surface measurements were carried out to confirm higher sample densities.