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Mesoporous silica matrices derived from sol-gel process assisted by low power ultrasonic activation

Savii Cecilia (Institute of Chemistry Timisoara of Romanian Academy, Romania.2)
Almásy László (Laboratory for Neutron Scattering, PSI and ETH Zürich, Villigen, Switzerland + Adolphe Merkle Institute, University of Fribourg, Fribourg, Switzerland)
Ionescu Claudia (Department of Physics, University of Warwick, Coventry, United Kingdom.9)
Székely Kinga Noémi (Research Institute for Solid State Physics and Optics, Budapest, Hungary.1)
Enache Corina (Institute of Chemistry Timisoara of Romanian Academy, Romania.2)
Popovici Mihaela (IMEC, Heverlee, Belgium)
Sora Ioan (Faculty de Electrotechnics, University 'Politehnica' Timisoara, Romania.2)
Nicoara Dan (Faculty de Electrotechnics, University 'Politehnica' Timisoara, Romania.2)
Savii Gustav George (Faculty de Electrotechnics, University 'Politehnica' Timisoara, Romania.2)
Resiga Susan Dana (Faculty of Physics, West University of Timisoara, Timisoara, Romania.2)
Subrt Jan (Department of Solid State Chemistry, Institute of Inorganic Chemistry, Academy of Sciences of the Czech Republic, Řež, Czech Republic)
Štengl Václav (Department of Solid State Chemistry, Institute of Inorganic Chemistry, Academy of Sciences of the Czech Republic, Řež, Czech Republic)

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. .

Keywords: mesoporous silica matrix, sol-gel, sonication, SANS, fractal structure, specific surface area