Solid oxide fuel cells are the electrochemical devices and they convert chemical energy into electrical energy. Decreasing the high operating temperature of SOFC to intermediate temperature range is an important prospect. This book presents the synthesis of SDC-CA electrolyte materials through Sol-gel process and characterization properties like crystal structure by Rietveld refinement, density, morphology, composition analysis, ionic conductivity and activation energy. The contribution of grain and grain boundary conductivity to total ionic conductivity is analyzed from impedance spectroscopy. Impedance data is analyzed by fitting with different models and analogs. Further, specific grain boundary also explained. Experimental results show that the Ca improves the density, ionic conductivity and lowers the activation energy of SDC at intermediate temperatures.