Layered double hydroxide (LDH) is one of the nano ordered layered compounds. Layered double hydroxide well known for its ability to intercalate anionic compounds has been prepared conventionally only with divalent and trivalent cations. In this study, Zn-Al-Ti LDH consisting of di-, tri- and tetra-valent cations was prepared and reacted with organic monocarboxylic, dicarboxylic and aromatic acids at high or room temperature. In the case of carbonate anion as the guest, XRD patterns of the prepared LDH (Zn-Al-Ti-CO3) showed two interlayer spacing 0.67 and 0.75 nm. These values mean that the carbonate anions have two Orientations between the layers. After intercalation reactions with organic acids, the interlayer spacing of Zn-Al-Ti LDH increased and organic-inorganic nano-hybrid materials formed. The Zn-Al-Ti LDH and intercalated compounds characterized by chemical analysis (C, H, N), Electron spectroscopy for chemical analysis (ESCA), X-ray diffraction, infrared spectra (IR), thermal analyses (TG, DTG and DTA) and scanning electron microscope (SEM). (c) 2007 Elsevier B.V. All rights reserved.