CA2-05 Montmorillonite-based porous clay heterostructures intercalated with ZnO-SiO2: Synthesis and characterization M. Akkari1, P. Aranda2, H. Ben Rhaiem1, A. Ben haj Amara1 and E. Ruiz-Hitzky2 1 UR05/13-01: Physique des Matériaux Lamellaires et Nanomatériaux Hybrides (PMLNMH), Faculté des Sciences de Bizerte, Zarzouna 7021, Tunisia 2 Instituto de Ciencia de Materiales de Madrid, CSIC, Cantoblanco, E-28049 Madrid, Spain, Porous clay heterostructures (PCH) were synthesized following a colloidal route that involves the controlled hydrolysis and polycondensation of tetramethoxysilane in the presence of organoclay as starting material. Heating the resulting materials to eliminate the organic matter. Handling the synthetic parameters was possible to produces ZnO nanoparticles homogeneously dispersed within the delaminated clays. The use of alkoxide mixtures containing the Zinc precursor together with tetramethoxysilane, as a silica precursor, also gives delaminated silicates containing in this case ZnO/SiO2-clay materials. Detailed characterization of the obtained materials included: chemical analyses, transmission electron Microscopy TEM, field emission scanning electron microscopy SEM-EDX, X-ray diffraction XRD, thermogravimetric/differential thermal analysis (TG–DTA), infrared spectroscopy FTIR and specific surface area and porosity determinations, techniques. However, these results confirm very well with FE-SEM, It was observed clearly distribution of the ZnO nanoparticles (NPs) incorpored on the silica-clay, this texture show “spongy-like” in materials. Key words: clays, ZnO nanoparticules (NPs), silica, Porous clay heterostructures Matériaux 2015