New method of synthesis of CO2Al(OH)(7-2x)(CO3)(x).nH(2)O layered double hydroxide (LDH) films by successive ionic layer deposition (SILD) is presented in this paper. The obtained nanolayers were characterized by SEM, EDX, XRD, XPS, FTIR spectroscopy and electrochemical techniques. The results showed that the as-synthesized product is formed by nanosheets with a thickness of 3-5 nm, having hydrotalcite crystal structure. Electrochemical characterization of the sample prepared by 50 cycles of SILD indicated a capacitive behavior with the specific capacitance value of 900 F/g at a current density of 1 A/g and 950 Fig at 0.5 A/g in 1 mol/L KOH aqueous solution. Repeated cycling for 1000 charge-discharge cycles demonstrate that capacitance increases by 6%, so such electrodes may be used as electrodes of hybrid supercapacitors. The presented convenient route of synthesis may be used for the preparation of LDH films with high surface area and a large capacitance. (C) 2014 Elsevier B.V. All rights reserved.