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Nanostructure and dynamic mechanical properties of silane-functionalized montmorillonite/epoxy nanocomposites
Abstract In this work sodium montmorillonite (Na-MMT) was functionalized with N-(2-aminoethyl)-3-aminopropyl-trimethoxysilane and the corresponding silylated clay was used to modify epoxy matrix cured with triethylenetetramine. The grafting/intercalation of the aminosilane inside the clay galleries were followed by infrared spectroscopy, X-ray diffraction, thermogravimetric analysis and 29Si cross-polarization magic-angle-spinning nuclear magnetic-resonance (CP/MAS NMR) spectroscopy. Epoxy-based nanocomposites were prepared with different amounts of silylated clay or commercial organoclay, Cloisite 30B, whose intercalating agent consists of a methyl, tallow, bis-2-hydroxyethyl quaternary ammonium salt. The degree of intercalation/exfoliation was estimated by X-ray diffraction experiments and confirmed by small angle X-ray scattering. Nanocomposites prepared with silylated clay displayed no peak in both XRD and SAXS curves whereas those prepared with Cloisite 30B exhibited a clear interference peak corresponding to an interlayer spacing d 001 of 4.1nm. The former also presented a better dispersion, with a high proportion of tactoids smaller than 2nm, as estimated by SAXS. From the results of dynamic mechanical analysis it was observed that most of the nanocomposites display higher storage modulus mainly at temperatures above the glass transition temperature. The glass transition temperature is similar or higher than the neat epoxy network for nanocomposites containing 1wt.% of silylated clay or higher.
Graphical abstract Display Omitted Highlights ► Sodium MMT functionalized with N-(2-aminoethyl)-3-aminopropyltrimethoxysilane. ► Preparation of epoxy-based nanocomposites with silylated clay. ► High exfoliation degree was observed from XRD and SAXS measurements.
Nanostructure and dynamic mechanical properties of silane-functionalized montmorillonite/epoxy nanocomposites
Abstract In this work sodium montmorillonite (Na-MMT) was functionalized with N-(2-aminoethyl)-3-aminopropyl-trimethoxysilane and the corresponding silylated clay was used to modify epoxy matrix cured with triethylenetetramine. The grafting/intercalation of the aminosilane inside the clay galleries were followed by infrared spectroscopy, X-ray diffraction, thermogravimetric analysis and 29Si cross-polarization magic-angle-spinning nuclear magnetic-resonance (CP/MAS NMR) spectroscopy. Epoxy-based nanocomposites were prepared with different amounts of silylated clay or commercial organoclay, Cloisite 30B, whose intercalating agent consists of a methyl, tallow, bis-2-hydroxyethyl quaternary ammonium salt. The degree of intercalation/exfoliation was estimated by X-ray diffraction experiments and confirmed by small angle X-ray scattering. Nanocomposites prepared with silylated clay displayed no peak in both XRD and SAXS curves whereas those prepared with Cloisite 30B exhibited a clear interference peak corresponding to an interlayer spacing d 001 of 4.1nm. The former also presented a better dispersion, with a high proportion of tactoids smaller than 2nm, as estimated by SAXS. From the results of dynamic mechanical analysis it was observed that most of the nanocomposites display higher storage modulus mainly at temperatures above the glass transition temperature. The glass transition temperature is similar or higher than the neat epoxy network for nanocomposites containing 1wt.% of silylated clay or higher.
Graphical abstract Display Omitted Highlights ► Sodium MMT functionalized with N-(2-aminoethyl)-3-aminopropyltrimethoxysilane. ► Preparation of epoxy-based nanocomposites with silylated clay. ► High exfoliation degree was observed from XRD and SAXS measurements.
Nanostructure and dynamic mechanical properties of silane-functionalized montmorillonite/epoxy nanocomposites
Silva, Adriana A. (author) / Dahmouche, Karim (author) / Soares, Bluma G. (author)
Applied Clay Science ; 54 ; 151-158
2011-08-10
8 pages
Article (Journal)
Electronic Resource
English
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