A series of M-Zn-Al (M=Mg, Cu) double hydroxide phases with carbonate anion were prepared by coprecipitation of 333 K, from the corresponding nitrate solution and sodium carbonate aqueous solution at pH 10. The characterization and properties of the products were investigated. It seems that reactivity of aluminium ions into the host layer depends on the identity of coexistent divalent cations (magnesium or copper), and the thermal properties of this layer at relatively high temperatures also depend on the nature of divalent cations.