Hydrogen‐Bond Directed Self‐Organized Lamellar Nanostructured Benzene Bridged‐Polysilsesquioxane Free‐Standing Monolithic Structures via sol‐gel Method

Nucleation and growth of co‐continuous nanophase morphology of benzene‐bridged organosilica nanostructured free‐standing films and monoliths via sol‐gel self‐condensation is successfully described and characterized. Hydrogen‐bonded periodic lamellar benzene bridged‐organosilica free‐standing monoliths with long‐range order are synthesized via one‐step acidic sol‐gel self‐organization of 1,4‐bis (triethoxysilyl)benzene (BTSB). High resolution X‐ray diffraction (HRXRD), field emission scanning electron microscopy (FESEM), solid‐state NMR spectroscopy, and nitrogen isotherms have been used to confirm the overall structural characterization of final hybrid monoliths. HRXRD patterns of hybrid monoliths show several clear peaks in the range of 2θ = 1.5–40° due to the formation of ordered lamellar nanostructure. HRXRD clearly suggests that the final monoliths have the lamellar nanostructure in which hydrophobic benzene groups are packed in a head‐to‐tail manner within organosilicate layers. NMR analysis of the final monoliths substantiates that the organosilica lamellar structures are formed via hydrogen bonding. SEM images for the resultant monoliths show very co‐continuous and fragmented morphology. This hydrogen‐bonded large periodicity is supported by structural model.