Search

Mesoporous silica particles of MCM-41 type were synthesized by sol-gel method from tetraethyl orthosilicate (TEOS) in 2-methoxyethanol and deionized water mixture in base conditions at room temperature. Ammonia or sodium hydroxides were used as catalysts and cetyl-trimethylammonium bromide (CTAB) and n-dodecyl-trimethylammonium bromide (DTAB) as structure directing agents. The porosities and the ordered structure have been analyzed using transmission and scanning electron microscopy, small angle neutron and X-ray diffraction, nitrogen adsorption, thermal analysis and FTIR spectroscopy. The samples consist of spherical particles of sub-micrometer size, with radially arranged pores. The comparison of the effect of the different surfactants and catalysts shows that by varying the surfactant type and their proportion, the pore sizes can be controlled. As compared to the commonly used ammonia catalyst, the use of NaOH as catalyst results in a much smaller porosity of the as-prepared materials. These materials are not resisting to the heat treatment at 700 C used for the template removal, and the ordered porous structure is completely lost.

The present work contributes to elucidating the differences between silica gels obtained by low doses ultrasonic activation, and those obtained by the conventional method, termed as classical sol gel. Silica matrices were produced by sol-gel synthesis process, assisted and non-assisted by an ultrasonic field, and subsequently characterized by various methods. Nitrogen adsorption and small-angle neutron scattering (SANS) measurements provided texture and microstructure of the dried gels. The adsorption results show that the sample sonicated for 2 hours presents the most ordered microstructure, characterized by pore shape close to spherical and the narrowest size distribution - about 90 % of the pores for this sample fall into the mesopore range (2-50 nm). SANS data reveal the formation of primary structural units of sizes around 1.5-2 nm which are small linear or branched polymeric species of roughly spherical shape and with rough surface. They are generated in the very early stage of sol gel process, as a result of hydrolysis and condensation reactions. The aggregated primary units form the secondary porous structure which can be described as a rough surface with fractal dimension above 2. The best porosity characteristics were obtained for the sample activated for 2 hours, indicating the optimal doses of sonication in the present conditions. Our results demonstrate the possibility of tailoring the pore size distribution using a low power ultrasonic bath. .