A ceramic oxide ( NaDyTiO4), having layered perovskite structure, has been prepared by a standard high- temperature solid- state reaction technique. X- ray diffraction ( XRD) studies have confirmed material formation under reported condition along with the presence of impurity ( Na2Dy2Ti3O10) as the minor phase. Complex impedance spectroscopy ( CIS) analysis has been carried out to investigate its microstructure and electrical properties as a function of frequency and temperature. CIS analysis has indicated that the electrical behavior of the material sample shows negative temperature coefficient of resistance ( NTCR) typical to a semiconductor. Impedance studies have also indicated the presence of temperature dependent relaxation process in the material with a spread of relaxation time. The d.c. conductivity of the material as evaluated from the impedance spectrum has been observed to be similar to 10(-9) Scm(-1) at room temperature ( T). It has been observed to increase as a function of temperature with a maximum of similar to 10(-5) Scm(-1) at 550 degrees C. The conductivity variation shows a cross over from Mott- type hopping phenomena at lower temperatures to a thermally activated Arrhenius type behavior at high temperature. (c) 2005 Springer Science + Business Media, Inc.