Influence of phenyl-trisilanol polyhedral silsesquioxane on properties of epoxy network glasses

Bruce X. Fu, Madhu Namani, Andre Lee

    Research output: Contribution to journalArticle

    • 116 Citations

    Abstract

    The influence of phenyl-trisilanol polyhedral silsesquioxane (POSS-triol) on the thermo-mechanical properties and curing of epoxy-amine networks were investigated using dynamic mechanical analysis (DMA) and Fourier transform infrared spectroscopy (FT-IR). Two of the most common epoxy monomers, diglycidyl ether of Bisphenol A (DGEBA), tetraglycidyl diamino diphenyl methane (TGDDM) were used. These epoxies were cured with linear aliphatic diamine: 2-Methyl-1,5-pentadiamine (Dytek® A) or diamine terminated polypropylene oxide (Jeffamine® D230). Using an identical curing schedule, when minor amounts of POSS-triol were added to the epoxy-amine networks, we found a significant improvement on value of Tg. Due to the small quantity of POSS-triol used, this enhancement in Tg is attributed to the catalytic activity of phenyl-trisilanol POSS in promoting a more completely cured epoxy network. This argument is consistent with observed increases in the rubbery plateau modulus due to increases in the crosslink density. But unlike other catalysts such as phenol, we did not observe acceleration of reaction in the pre-gelation stage by this acidic POSS-silanol. Because of its nanoscopic size, this acidic POSS-silanol promotes additional epoxy-amine crosslinking in the post-vitrification stage, which is dominated by diffusion-control mechanisms. We believe this can be utilized in fabrication of fiber-reinforced composites using the resin transfer molding process, where maintaining the low viscosity for a period of time is required to eliminate porosity and to produce higher Tg materials at a lower post-cure temperature.

    Original languageEnglish (US)
    Pages (from-to)7739-7747
    Number of pages9
    JournalPolymer
    Volume44
    Issue number25
    DOIs
    StatePublished - Nov 14 2003

    Profile

    Amines
    Curing
    Aldrin
    Polypropylene oxides
    Vitrification
    Resin transfer molding
    Dynamic mechanical analysis
    Gelation
    Crosslinking
    Phenols
    Fourier transform infrared spectroscopy
    Ethers
    Catalyst activity
    Methane
    Porosity
    Monomers
    Viscosity
    Fabrication
    Glass
    Mechanical properties

    Keywords

    • Epoxy
    • POSS-silanol
    • Silsesquioxane

    ASJC Scopus subject areas

    • Organic Chemistry
    • Polymers and Plastics

    Cite this

    Influence of phenyl-trisilanol polyhedral silsesquioxane on properties of epoxy network glasses. / Fu, Bruce X.; Namani, Madhu; Lee, Andre.

    In: Polymer, Vol. 44, No. 25, 14.11.2003, p. 7739-7747.

    Research output: Contribution to journalArticle

    Fu, Bruce X.; Namani, Madhu; Lee, Andre / Influence of phenyl-trisilanol polyhedral silsesquioxane on properties of epoxy network glasses.

    In: Polymer, Vol. 44, No. 25, 14.11.2003, p. 7739-7747.

    Research output: Contribution to journalArticle

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    abstract = "The influence of phenyl-trisilanol polyhedral silsesquioxane (POSS-triol) on the thermo-mechanical properties and curing of epoxy-amine networks were investigated using dynamic mechanical analysis (DMA) and Fourier transform infrared spectroscopy (FT-IR). Two of the most common epoxy monomers, diglycidyl ether of Bisphenol A (DGEBA), tetraglycidyl diamino diphenyl methane (TGDDM) were used. These epoxies were cured with linear aliphatic diamine: 2-Methyl-1,5-pentadiamine (Dytek® A) or diamine terminated polypropylene oxide (Jeffamine® D230). Using an identical curing schedule, when minor amounts of POSS-triol were added to the epoxy-amine networks, we found a significant improvement on value of Tg. Due to the small quantity of POSS-triol used, this enhancement in Tg is attributed to the catalytic activity of phenyl-trisilanol POSS in promoting a more completely cured epoxy network. This argument is consistent with observed increases in the rubbery plateau modulus due to increases in the crosslink density. But unlike other catalysts such as phenol, we did not observe acceleration of reaction in the pre-gelation stage by this acidic POSS-silanol. Because of its nanoscopic size, this acidic POSS-silanol promotes additional epoxy-amine crosslinking in the post-vitrification stage, which is dominated by diffusion-control mechanisms. We believe this can be utilized in fabrication of fiber-reinforced composites using the resin transfer molding process, where maintaining the low viscosity for a period of time is required to eliminate porosity and to produce higher Tg materials at a lower post-cure temperature.",
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    N2 - The influence of phenyl-trisilanol polyhedral silsesquioxane (POSS-triol) on the thermo-mechanical properties and curing of epoxy-amine networks were investigated using dynamic mechanical analysis (DMA) and Fourier transform infrared spectroscopy (FT-IR). Two of the most common epoxy monomers, diglycidyl ether of Bisphenol A (DGEBA), tetraglycidyl diamino diphenyl methane (TGDDM) were used. These epoxies were cured with linear aliphatic diamine: 2-Methyl-1,5-pentadiamine (Dytek® A) or diamine terminated polypropylene oxide (Jeffamine® D230). Using an identical curing schedule, when minor amounts of POSS-triol were added to the epoxy-amine networks, we found a significant improvement on value of Tg. Due to the small quantity of POSS-triol used, this enhancement in Tg is attributed to the catalytic activity of phenyl-trisilanol POSS in promoting a more completely cured epoxy network. This argument is consistent with observed increases in the rubbery plateau modulus due to increases in the crosslink density. But unlike other catalysts such as phenol, we did not observe acceleration of reaction in the pre-gelation stage by this acidic POSS-silanol. Because of its nanoscopic size, this acidic POSS-silanol promotes additional epoxy-amine crosslinking in the post-vitrification stage, which is dominated by diffusion-control mechanisms. We believe this can be utilized in fabrication of fiber-reinforced composites using the resin transfer molding process, where maintaining the low viscosity for a period of time is required to eliminate porosity and to produce higher Tg materials at a lower post-cure temperature.

    AB - The influence of phenyl-trisilanol polyhedral silsesquioxane (POSS-triol) on the thermo-mechanical properties and curing of epoxy-amine networks were investigated using dynamic mechanical analysis (DMA) and Fourier transform infrared spectroscopy (FT-IR). Two of the most common epoxy monomers, diglycidyl ether of Bisphenol A (DGEBA), tetraglycidyl diamino diphenyl methane (TGDDM) were used. These epoxies were cured with linear aliphatic diamine: 2-Methyl-1,5-pentadiamine (Dytek® A) or diamine terminated polypropylene oxide (Jeffamine® D230). Using an identical curing schedule, when minor amounts of POSS-triol were added to the epoxy-amine networks, we found a significant improvement on value of Tg. Due to the small quantity of POSS-triol used, this enhancement in Tg is attributed to the catalytic activity of phenyl-trisilanol POSS in promoting a more completely cured epoxy network. This argument is consistent with observed increases in the rubbery plateau modulus due to increases in the crosslink density. But unlike other catalysts such as phenol, we did not observe acceleration of reaction in the pre-gelation stage by this acidic POSS-silanol. Because of its nanoscopic size, this acidic POSS-silanol promotes additional epoxy-amine crosslinking in the post-vitrification stage, which is dominated by diffusion-control mechanisms. We believe this can be utilized in fabrication of fiber-reinforced composites using the resin transfer molding process, where maintaining the low viscosity for a period of time is required to eliminate porosity and to produce higher Tg materials at a lower post-cure temperature.

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