Synthesis of Ce0.9Gd0.1O1.95 (CGO) powder from a polymeric precursor solution containing a mixture of nitrates, nitric acid, and ethylene glycol was investigated with emphasis on the effect of polymerization of the precursor solution on the crystallization and morphology of the derived solid intermediate and the final oxide powder. It is shown for the first time in this work that the solid intermediate derived from the polymerized solution is present in the form of well-crystallized cerium-gadolinium formate solid solution, Ce1-xGdx(HCOO)(3), exhibiting anisotropic growth. Further polymerization of the precursor solution resulted in the direct formation of loosely agglomerated nanoscaled CGO oxide powder from the polymerized solution at temperatures as low as 130degreesC.