The electrochemical capacitive behavior of NiFe2O4 ceramic powders prepared by combustion synthesis, polyol-mediated and sol-gel methods was studied. The phase formation and morphological characterizations of synthesized materials were carried out through thermal analysis (TG-DTA), powder X-ray diffraction (XRD) and scanning electron microscopy (SEM). Electrochemical performance of these electrode materials as capacitors was investigated in aqueous NaCl electrolyte using cyclic voltammetry (CV) and the corresponding specific capacitance (SC) values were determined. The observed electrochemical double layer capacitive (EDLC) behavior in NiFe2O4 depends on the morphology which can be controlled by the synthesis method adopted. NiFe2O4 synthesized by sol-gel method exhibited a specific capacitance of 97.5 F/g which is higher than the capacitance values of NiFe2O4 obtained through other synthesis methods. (C) 2011 The Electrochemical Society. [DOI: 10.1149/1.3601863] All rights reserved.