LDH hybrids were synthesized from Cl-MgAl-LDHs by anion exchange with short-chain alkyl carboxylateintercalants: CnH2n+1COO- (n = 0-3). Among them, LDH3 (LDH with Mg/Al = 3) hybrids containing acetate (n = 1) and propionate (n = 2) exhibited swelling behavior in water. The action of water on acetate-LDH3 (AcO-LDH3) and propionate-LDH3 (PrO-LDH3) led to semitransparent suspensions via a viscous gel state. From the X-ray diffraction profiles of the gels, only a broad feature was observed by the loss of the sharp reflections. The reflections reappeared for the films obtained by drying the gel, indicating the restacking of the LDH nanosheets into the original stacked structure. Observation using atomic force microscopy revealed delaminated nanosheets with a thickness of 1.1-1.5 nm with the same morphological features as the starting LDHs. XRD measurement and AFM observation supported the formation of unilamellar LDH sheets. Semitransparent self-standing LDH films were obtained by peeling off the films formed on a PE (polyethylene) substrate by drying the colloidal suspension thereon. The thickness of the obtained flexible films ranged from 10 to 25 mu m, and they could be anion exchanged with inorganic and organic anions in the film state.