Adsorption in Periodically Ordered Mesoporous Organosilica Materials Studied by in Situ Small-Angle X-ray Scattering and Small-Angle Neutron Scattering

Modified periodically ordered mesoporous organosilica materials were prepared starting from a recently introduced type of sol−gel precursor, containing both organic moieties and hydrolyzable Si-OR groups. In order to thoroughly characterize the mesoporosity and its accessibility, different probe gases were used in conventional gas adsorption experiments. Furthermore, in situ small-angle X-ray scattering (SAXS) and small-angle neutron scattering (SANS) were applied to study the mesoporosity and the sorption processes, taking advantage of scattering contrast matching conditions. Thereby, the materials were characterized not only by different probe molecules but also at different temperatures (nitrogen at 77 K, dibromomethane at 290 K and perfluoropentane at 276 K). The comparison between the standard and in situ SAXS/SANS adsorption experiments revealed valuable information about the porosity and microstructure of the materials. It is demonstrated that the organic moieties are homogeneously distributed; that is, they do not phase-separate from silica on the nanometer scale.