Nanostructured Co x Ni 1−x -Al layered triple hydroxides (Co x Ni 1−x -Al LTHs) have been successfully synthesized by a facile hydrothermal method using glycine as chelating agent. The samples were characterized by Xray diffraction, thermogravimetry, Fourier transform infrared spectroscopy and scanning electron microscopy. The morphologies of Co x Ni 1−x -Al LTHs varied with the Co content and its effect on the electrochemical behavior was studied by cyclic voltammetry and galvanostatic chargedischarge techniques. Electrochemical data demonstrated that the Co x Ni 1−x -Al LTHs with Co/Ni molar ratio of 3:2 owned the best performance and delivered a maximum specific capacitance of 1,375 Fg −1 at a current density of 0.5 A g −1 and a good high-rate capability. The capacitance retained 93.3% of the initial value after 1,000 continuous charge-discharge cycles at a current density of 2 A g −1 .