Hybrid Organic-Inorganic Sol-Gel Materials Based on Epoxy-Amine Systems

Innocenzi, Plinio; Kidchob, Tongjit; Yoko, Toshinobu

doi:10.1007/s10971-005-2290-4

Cited by 117 publications

(75 citation statements)

References 45 publications

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“…Epoxy/ silica hybrids may be prepared by simply dispersing preformed silica particles or (better) by promoting the "in-situ" formation of a silicate phase through sol-gel chemistry. The "in-situ" method allows obtaining a wide range of morphologies ranging from the particles dispersion to the formation of co-continuous organic-inorganic networks [11][12][13]. Furthermore, the sol-gel process allows tailoring the interface between organic and inorganic phases through the adequate selection of both the silane precursors of the inorganic phase and the sol-gel reaction conditions [14,15].…”

Section: Introductionmentioning

confidence: 99%

Effects of post cure treatment in the glass transformation range on the structure and fire behavior of in situ generated silica/epoxy hybrids

Bifulco

Tescione

Capasso

et al. 2018

J Sol-Gel Sci Technol

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Effects of post cure treatment in the glass transformation range on the structure and fire behavior of in situ generated silica/epoxy hybrids Abstract A new "in situ" sol-gel synthesis procedure was exploited to produce silica/epoxy nanocomposites with 6 wt.% maximum silica content. 3-Aminopropyltriethoxysilane (APTS) was used as a coupling agent. The experimental results (fouriertransform infrared spectroscopy, FTIR, small-angle X-ray scattering, SAXS, transmission electron microscopy, TEM, nuclear magnetic resonance, NMR, and dynamic mechanical analysis, DMA) support that the structure consists of nanosized silica particles (maximum 1.25 nm in size) embedded in a hybrid co-continuous network. A post cure non-isothermal heating from 15 to 100°C (beyond the Tg of the neat epoxy) caused Tg and storage modulus to increase. The fire behavior, that, owing to severe regulations (i.e., in aerospace engineering), often prevents composites applications, was also studied. The formed silica domains prevented melt dripping phenomena during vertical flame spread tests. Cone calorimetry tests showed a remarkable decrease of the heat release rate (HRR) for all the hybrid systems with respect to the neat cured resin, even at very low silica loadings (i.e., 2 wt.%). This decrease was much more pronounced for the hybrid structures that were not subjected to the post cure thermal treatment. The use of multiple structural investigation techniques allowed to choose among multiple hypothesis and conclude that nanoparticles clustering is the main reason of the effects of the post curing treatments. Graphical Abstract SAXS of the samples before (EPO) and after (EPO_t) post cure thermal treatment in the glass transformation range. Effect of the post cure on the glass transformation temperature (Tg) and heat release rate (HRR) Photos of samples EPO and EPO 2% Si after vertical flame spread tests Highlights• A hybrid co-continuous network embedding nanoparticles (maximum 1.25 nm in size) was obtained;• A post-cure was performed above the glass transformation temperature, T g , of neat epoxy;• The post cure makes T g , storage modulus and Heat Release Rate (HRR) to increase;• No dripping in flame test and up to 40% HRR reduction for only 2 wt.% silica content is observed;• The post cure effects depend on nanoparticles clustering in the glass transformation range.

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Section: Introductionmentioning

confidence: 99%

Effects of post cure treatment in the glass transformation range on the structure and fire behavior of in situ generated silica/epoxy hybrids

Bifulco

Tescione

Capasso

et al. 2018

J Sol-Gel Sci Technol

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“…This process is very much controlled by the catalyst whose concentration and nature largely affect the polycondensation reactions. 32), 33) An important role in the synthesis is also played by water and the solvent; on the other hand water and ethanol are also by-products of the GPTMS solgel reactions. A large variety of catalysts have been used for the opening of the epoxy groups, acid 16) and basic 19), 34) catalysts, photocatalysts.…”

Section: A Short Overview Of the Chemistry Of Gptmsmentioning

confidence: 99%

Crystallization in hybrid organic-inorganic materials through self-organization from 3-glycidoxypropyltrimethoxysilane

Innocenzi

Figus

Kidchob

et al. 2011

J. Ceram. Soc. Japan

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Hybrid organicinorganic materials can organize into layered crystalline structures through self-organization when bridged silsesquioxanes are used in the solgel synthesis. Crystallization is, however, also observed in hybrid materials when 3-glycidoxypropyltrimethoxysilane is left to react in highly basic conditions; this synthesis route shows a peculiar property which is the possibility of preparing also crystalline hybrid films by controlling the solgel process. The crystalline films exhibit optical anisotropy and are optically transparent. In this article we briefly review the main achievements of our research group in the field.

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“…Methoxy groups of GPTMS are hydrolyzed to produce silanol, which then condenses to form the silica network [18]. The opening of the epoxy ring may occur at room temperature and an organic network may be formed using amine containing compounds [17][18][19]. Each active hydrogen in the amino group can open and bind to one epoxy group.…”

Section: Introductionmentioning

confidence: 99%

Coating of L-Arginine Modified Silica on Magnetite through Two Different Sol-Gel Routes

2017

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Hybrid Organic-Inorganic Sol-Gel Materials Based on Epoxy-Amine Systems

Cited by 117 publications

References 45 publications

Effects of post cure treatment in the glass transformation range on the structure and fire behavior of in situ generated silica/epoxy hybrids

Effects of post cure treatment in the glass transformation range on the structure and fire behavior of in situ generated silica/epoxy hybrids

Crystallization in hybrid organic-inorganic materials through self-organization from 3-glycidoxypropyltrimethoxysilane

Coating of L-Arginine Modified Silica on Magnetite through Two Different Sol-Gel Routes

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