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Characterization of surface and porous properties of synthetic hybrid lamellar silica
Authors:Gilles Toussaint,Miguel Angel Rodriguez,Rudi Cloots,Juan Rubio,Fausto Rubio,Bé    dicte Vertruyen,Catherine Henrist
Affiliation:
  • a GREENMAT, Department of Chemistry, B6a, University of Liege, Sart Tilman, B-4000 Liège, Belgium
  • b Instituto de Cerámica y Vidrio, CSIC, C/ Kelsen, 5, 28049 Madrid, Spain
  • Abstract:
    Synthetic lamellar silica and hybrid lamellar silicas have been prepared by liquid crystal templating, template extraction and silanization. The samples have been characterized by thermogravimetric analysis (TGA), carbon analysis, spectroscopy, X-ray diffraction (XRD) and nitrogen adsorption. The XRD analyses have shown that the lamellar periodic stacking is preserved for all samples. The quantity and type of organic molecules at the silica surface have been evaluated by carbon analysis, TGA and spectroscopy. The covalent grafting of the solvent used for extraction of the initial surfactant has been highlighted by these analyses. The nitrogen adsorption analyses have revealed three categories of pores and two types of samples. The initial lamellar silica exhibits a very low specific surface area and plate-like type of pores. The second type of samples is made up of the hybrid samples and the initial substrate from whom the surfactant has been extracted. These samples show a significantly higher specific surface area with interlamellar spaces corresponding to narrow-slit like mesopores around 4 nm. The nitrogen adsorption data analysis has highlighted the presence of micropores within the silica sheets. The difference of the specific surface is due to pore blocking by the surfactant impeding the access to nitrogen into interlamellar spaces and by the silanes covering the pores once the surface modified. The presence of micro and mesopores combined to a high BET specific surface of 612 m²/g makes these lamellar silicas interesting materials for catalysis applications.
    Keywords:TEOS, tetraethoxysilane   XRD, X-ray diffraction   GPTMS, 2-glycidoxypropyltrimethoxysilane   PEOTMS, 2-[methoxy(polyethyleneoxy)propyl)]trimethoxysilane   NMR, nuclear magnetic resonance   TGA, thermogravimetric analysis   DSC, differential scanning calorimetry
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