Layered double hydroxide (LDH) has positive charge between the layers and is known as anion exchangeable clay being able to intercalate various organic and inorganica nions. In this study, organic-inorganic layered nanohybrids were prepared by intercalation of organic carboxylate anions into Zn/Al LDH in an aqueous solution. Four intercalation compounds were prepared by the reactions of succinate, terephthalate, 4-pyridinecarboxylate, and p-hydroxybenzoate anions with Zn/Al LDH in aqueous solution. Interlayer spacing of these four intercalation compounds decreased by the thermal treatment at 363 K, and recovered by the treatment in water, reversibly.