Structural Characterization of Ordered Mesoporous Silica Prepared by a Sol–Gel Process Using Urea-Based Cationic Gemini Surfactants

Mesoporous silica nanoparticles have been synthesized through sol–gel synthesis in basic conditions. Gemini surfactants having urea in the headgroups were used as pore-forming agents. The effect of the spacer length of the surfactant on the particle morphology was studied on the sub-micrometer and nanometer scales using nitrogen porosimetry, small-angle X-ray scattering (SAXS), ultra-small-angle neutron scattering, and scanning and transmission electron microscopy (SEM, TEM). Depending on the spacer, spherical and/or cylindrical nanoparticles formed in different proportions, as revealed by statistical analysis of SEM micrographs. All prepared materials showed the hexagonal pore structure characteristic of the MCM-41 molecular sieves, with the exception of the sample prepared using the gemini surfactant with the shortest spacer length. The influence of the spacer length on the lattice parameter of the pore network, as well as the average size of the ordered domains, has been assessed by SAXS and TEM. Detailed analysis of the TEM images revealed a spread of the lattice parameter in a range of 10–20%. The broadening of the diffraction peaks was shown to be due to the combination of the effects of the finite domain size and the variance of the lattice parameter across the crystalline domains. The structural differences between the silica gels synthesized with the different surfactants were related to the variation of the micelle morphologies, reported in previous light scattering and small-angle scattering experiments. No connection could be revealed between the micelle shape and size and the pore sizes, showing that surfactants with a broad range of spacer lengths can equally well be used for the preparation of MCM-41 materials.