Polyimide-silica nanocomposites: spectroscopic, morphological and mechanical investigations

Musto, Pellegrino; Ragosta, G.; Scarinzi, Gennaro; Mascia, L.

doi:10.1016/j.polymer.2003.12.044

Cited by 119 publications

(62 citation statements)

References 18 publications

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“…Several investigations have been reported in which the influence of the inorganic phase on the reactivity of the polyimide precursor has been studied [28,29,38]. In all these reports it has been pointed out that the silica phase exerts a considerable influence on the behaviour of the polyamic acid both in terms of its tendency to form molecular interactions with residual solvent, and with respect to the imidization reaction itself.…”

Section: Reactivity and Curing Behaviourmentioning

confidence: 99%

“…In all these reports it has been pointed out that the silica phase exerts a considerable influence on the behaviour of the polyamic acid both in terms of its tendency to form molecular interactions with residual solvent, and with respect to the imidization reaction itself. In particular, Musto et al [28] performed a time-resolved FTIR analysis on a PI/silica nanocomposite and a pure polyimide (PMDA-ODA) in order to compare the rate and extent of solvent removal from the two systems. It was shown that the presence of the silica precursor within the pre-polymer solution greatly facilitates solvent removal from the film surface.…”

Section: Reactivity and Curing Behaviourmentioning

confidence: 99%

“…These enhancements include primarily modulus, strength and toughness and the magnitude of the effect is related to the compatibility of the organic and inorganic components, as well as to the size and dispersion state of the inorganic phase. In Figures 8 and 9 are shown the results of tensile tests carried out by Musto et al [28] on PI/silica systems obtained using GOTMS as compatibilizing agent. The modulus is found to increase linearly with increasing the concentration of the inorganic phase ( Figure 8).…”

Section: Mechanical and Fracture Propertiesmentioning

confidence: 99%

“…For the compatibilized system the size of the interconnected silica domains ranges from 40 to 415 Ragosta and Musto -eXPRESS Polymer Letters Vol.3, No.7 (2009) [413][414][415][416][417][418][419][420][421][422][423][424][425][426][427][428] Figure 3. SEM micrographs of PI/silica hybrids with 22.3 wt% of silica: a) hybrid without the coupling agent (GOTMS); b) hybrid with the coupling agent (GOTMS) [28]. …”

mentioning

confidence: 99%

“…Mascia and Kioul [5,8,21] and Mascia and coworkers [28,29], showed that the compatibility in PI/silica hybrids can be greatly improved by adding to TEOS solutions a functional alkoxysilane coupling agent such as γ-glycidyloxipropyl trimethoxysilane (GOTMS). The SEM micrographs of Figure 3 for PI hybrids with 22.3 wt% of silica illustrate the compatibilization effect of GOTMS, which brings about a morphological transformation from a dispersed particle microstructure (Figure 3a), in absence of GOTMS to a finely interconnected or co-continuous phase morphology (Figure 3b), with the use of GOTMS [28]. For the compatibilized system the size of the interconnected silica domains ranges from 40 to 415 Ragosta and Musto -eXPRESS Polymer Letters Vol.3, No.7 (2009) [413][414][415][416][417][418][419][420][421][422][423][424][425][426][427][428] Figure 3.…”

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confidence: 99%

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Polyimide/silica hybrids via the sol-gel route: High performance materials for the new technological challenges

Ragosta¹,

Musto²

2009

Express Polym. Lett.

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Abstract. The present review article describes in detail the state-of-the-art of organic-inorganic hybrid materials based on polyimide/silica components. The article is divided in three parts. In the first the basic processing route for the preparation of these systems is described, i.e. the sol-gel technique, along with the strategies developed to control the final morphology. In the second part the curing characteristics, the dynamic-mechanical and the mechanical and fracture properties of hybrids with different morphologies are reviewed. Finally, the more technologically relevant applications devised for these high performance materials are discussed. : nanocomposites, hybrid materials, polyimide, silica, sol-gel eXPRESS Polymer Letters Vol.3, No.7 (2009) [413][414][415][416][417][418][419][420][421][422][423][424][425][426][427][428] Available online at www.expresspolymlett.com DOI: 10.3144/expresspolymlett.2009.51 or as functional materials [14] such as catalyst supports [15] and microelectronic devices [16]. The sol-gel route represents the preferred way for the synthesis of polyimide based hybrids. The classical sol-gel process consists in a two step hydrolysis-condensation reaction, starting with a metal alkoxides M(OR) 4 , typically tetraethoxisilane Si(OCH 2 CH 3 ) 4 or titanium isopropoxide Ti[OCH(CH 3 ) 2 ] 4 , to produce hydroxyl groups followed by the polycondensation of the hydroxyl groups and residual alkoxy groups to form a three-dimensional network [5,[17][18][19][20][21]. Polyimides are particularly suited for this type of process because they can be obtained from polyamic acid precursors, which are soluble in hygroscopic solvents and can, therefore, tolerate the addition of water necessary to bring about the hydrolysis of the metal alkoxide. Moreover, the outstanding thermal stability of polyimides allows the hybrids to be post-cured at very high temperatures (300-350°C) making it possible the development of a very dense inorganic network without inducing appreciable degradation of the organic phase. Polyimide/silica hybrids made by the sol-gel technique are the subject of this review, in which the approaches used for a close control of their final morphology, the effects of the silica phase on the curing process of polyimide precursors, the dynamic-mechanical and the mechanical and fracture properties that these materials can display, and their possible applications will be presented and discussed. Keywords Processing and morphologyA typical procedure for the preparation of PI/silica hybrids via the sol-gel route, involves the following steps: i) The polyamic acid (PAA) (PI precursor) is formed by a polyaddition reaction of a dianhydride [e.g., pyromellitic anhydride (PMDA), 3,3′,4,4′-biphenyltetracarboxylic dianhydride (BPDA), or 2,2-bis(3,4-dicarboxy-phenyl)-hexafluoropropane dianhydride (6FDA)] with a diamine [e.g., 4,4′-oxydianiline (ODA), or p-phenylen diamine (PPA)] in a common solvent [e.g., dimethylacetamide (DMAc), or N-methyl pyrolidone (NMP)]. The reaction and chemical str...

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Section: Reactivity and Curing Behaviourmentioning

confidence: 99%

Section: Reactivity and Curing Behaviourmentioning

confidence: 99%

Section: Mechanical and Fracture Propertiesmentioning

confidence: 99%

mentioning

confidence: 99%

mentioning

confidence: 99%

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Polyimide/silica hybrids via the sol-gel route: High performance materials for the new technological challenges

Ragosta¹,

Musto²

2009

Express Polym. Lett.

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Silica‐ and Silsesquioxane‐Containing Polymer Nanohybrids

Wahab

Kim

2005

Macromolecules Containing Metal and Metal‐Like Elements

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Network density control in epoxy–silica hybrids by selective silane functionalization of precursors

Prezzi

Mascia

2005

Adv Polym Technol

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ABSTRACT:Following previous work on the compatibilization of organic-inorganic hybrids through coupling reactions with the precursor components, the present study evaluates the relative efficiency of different types of coupling agents on the morphology and properties of epoxy-silica hybrids. In particular, this investigation compares the effects of introducing trialkoxysilane functional groups at the chain end (using amine-and mercapto-silanes) with similar types grafted in the middle of the chain of the constituent resin (using an isocyanate silane). The use of coupling agents with a basic character (amine silane type) brings about the formation of denser networks in both constituent phases of the resulting epoxy-silica hybrid, which is manifest through a large increase in the T g and a more extensive suppression of the molecular relaxations within the glass transition regions. Increasing the number of alkoxysilane functional groups at the chain end, with the use of a bis-aminosilane, has a relatively minor effect on the morphology and dynamic mechanical spectra of the resulting epoxy-silica hybrids. It was also found that while the incorporation of small amounts of a high molecular weight epoxy resin causes considerable plasticization of the organic phase, much larger amounts of organic (aliphatic) co-agent within the siloxane

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Polyimide-silica nanocomposites: spectroscopic, morphological and mechanical investigations

Cited by 119 publications

References 18 publications

Polyimide/silica hybrids via the sol-gel route: High performance materials for the new technological challenges

Polyimide/silica hybrids via the sol-gel route: High performance materials for the new technological challenges

Silica‐ and Silsesquioxane‐Containing Polymer Nanohybrids

Network density control in epoxy–silica hybrids by selective silane functionalization of precursors

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