“…(Vaughan and Lussier, 1980;Occelli, 1983;Bergaya et al, 1991) has stimulated research not only for the synthesis of new PILCs, but also for their extensive microscopic characterization. A wide spectrum of analytical techniques, e.g., magic-angle spinning NMR (Plee et al, 1985;Tillak et aL, 1986), EPR (Harsh and Doner, 1984;Braddell et aL, 1987), neutron scattering (Pinnavaia et al, 1984), NMR and HzTPR (Bergaya et al, 1993) and M6ssbauer spectroscopy (Gangas et aL, 1985;Lee Woo et al, 1989;Petridis et al, 1989), has been used for unravelling the structure and the properties of these novel materials. However, in spite of the substantial advance made up to now in the synthesis and characterization of PILCs, the elucidation of additional aspects of the pillared structure (e.g., the diameter of the pillars) is of cardinal importance for understanding the role of their morphology in physicochemical processes occurring in the interlayer space, as well as developing applications,…”