Al-containing nickel layered double hydroxide was prepared by liquid phase deposition (LPD) using aluminum metal or compounds as the fluorine scavenger in the equilibrium reaction of nickel-fluorine complex ion. The obtained phases depend on the Al content when it is solely used as F- scavenger; alpha-nickel hydroxide is the predominant phase and a small amount of beta-phase is detected. In contrast pure Ni-Al LDH/C composites, isostructural and isomorphic to alpha-Ni(OH)(2) are obtained at any range of Al content from 0 to ca. 30 mol % of [Al]/[Al + Ni]. High stability of LDH in 6 M aqueous KOH solution was performed because of low impurity of cation species.