Solvent-free synthesis of reactive inorganic precursors for preparation of organic/inorganic hybrid materials

Beneš, Hynek; Galy, Jean; Gérard, Jean‐François; Pleštil, Josef; Valette, Ludovic

doi:10.1007/s10971-011-2534-4

Cited by 8 publications

(13 citation statements)

References 32 publications

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“…According to this value, which is typical of a glassy material, one can conclude the existence of an inorganic‐rich continuous phase. Both, the increase in T α and in modulus resulted from strong interactions created between the organic and inorganic components and the existence of diffuse nanostructures which reduce the motion of polyester chains …”

Section: Resultsmentioning

confidence: 99%

“…These materials can be obtained via different routes: (i) by the addition of preformed nanoparticles or nanoclusters, the most significant examples being layered silicates, silicas, nanotube‐like or needle‐like metal oxides, or polyhedral oligomeric silsesquioxane (POSS), (ii) by in situ generation of an inorganic‐rich phase through a conventional sol–gel process involving hydrolysis and condensation reactions under mild conditions, starting from hydrolysable metal alkoxides, generally alkoxy silanes . These reactions are illustrated in Scheme for tetraethoxysilane (TEOS), often used for the formation of hybrid materials.…”

Section: Introductionmentioning

confidence: 99%

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Synthesis and characterization of hybrid films from hyperbranched polyester using a sol–gel process

Houel

Galy

Charlot

et al. 2013

J of Applied Polymer Sci

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International audienceHybrid organic/inorganic materials were prepared by an in situ sol-gel process using tetraethoxysilane (TEOS) in the presence of hyperbranched polyester. The influences of hyperbranched polyester molar mass as well as the amount of TEOS were examined. The condensation degree was characterized by solid state 29Si NMR. The combination of solubility tests, calcination tests, SAXS and dynamic mechanical analysis allowed us to investigate the hybrid material nanostructure. The results show high compatibility between the inorganic silica phase and the organic polymer phase, due to the spherical shape of the hyperbranched polymer and its numerous hydroxyl groups. As a consequence, a continuous inorganic phase was formed even with a low silica precursor content without any macroscopic phase separation. These hybrid materials have a high Tg and high storage modulus even at an elevated temperature combined with improved thermal stability

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Section: Resultsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Synthesis and characterization of hybrid films from hyperbranched polyester using a sol–gel process

Houel

Galy

Charlot

et al. 2013

J of Applied Polymer Sci

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“…A detailed study of the preparation of the inorganic precursors has been recently described in a previous article 21. Two types of inorganic precursors with (i) amino or (ii) glycido groups were prepared.…”

Section: Methodsmentioning

confidence: 99%

“…Recently, we have developed a solvent‐free sol–gel process, which produced reactive inorganic precursors bearing glycido‐ or amino‐functional groups prepared from monomeric alkoxysilanes 21. This cost‐effective procedure enabled the production of storage‐stable precursors in which the majority of alkoxysilane groups were already condensed into SiOSi bonds.…”

Section: Introductionmentioning

confidence: 99%

Preparation and characterization of organic/inorganic hybrid epoxy networks from reactive inorganic precursors

Beneš

Galy

Gérard

et al. 2011

J of Applied Polymer Sci

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International audienceOrganic/inorganic hybrid networks were prepared by a novel solvent-free two-step synthesis method. In the first step, prehydrolyzedcondensed reactive inorganic precursors (clusters) were prepared by a solgel process from monomeric alkoxysilanes with amino and glycido groups. The second step comprised their addition into epoxy resin and amine hardener, followed by the reaction of all components giving the final hybrid crosslinked materials. Their structure was evaluated by small-angle X-ray scattering, transmission electron microscopy, scanning electron microscopy, and dynamic mechanical and thermal analysis. The morphology of the organic/inorganic hybrid structures formed from glycidoprecursor revealed spherical silica-rich domains forming agglomerates with diameter from 100 to 500 nm. The aminoprecursor led to large highly condensed and branched silicon-rich structures. The organic/inorganic hybrid networks obtained from this precursor consisted of mixed siliconorganic phases covalently interconnected via epoxyamine bonds. Such hybrid networks showed significantly improved thermomechanical properties and better resistance against thermooxidation when compared with the neat epoxyamine network. Thin films as well as bulk materials were successfully prepared by this process

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“…An alternative route to incorporate silica into the polymer matrix is the sol-gel process involving a series of hydrolysis and condensation reactions under mild conditions starting from hydrolyzable multifunctional alkoxysilanes as inorganic precursors for forming inorganic domains, being tetraethoxysilane (TEOS) the most typical one. 8,9,10,11,12 Using this route it is possible to grow an inorganic phase into an organic matrix allowing a fine dispersion of the inorganic phase even at molecular level. Another advantage of the in situ generation of the inorganic phase is that the addition of a small amount of nanoparticles drastically increases the viscosity, which is always an important issue in coatings applications whereas the formulation applied before the sol-gel process still has a low viscosity.…”

Section: Introductionmentioning

confidence: 99%

Hybrid epoxy networks from ethoxysilyl-modified hyperbranched poly(ethyleneimine) and inorganic reactive precursors

Acebo

Fernández‐Francos

Santos³

et al. 2015

European Polymer Journal

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New epoxy-silica hybrid coatings were prepared by a dual process consisting of a sol-gel process using tetraethoxysilane (TEOS) or 3-glycidyloxypropyl trimethoxysilane (GPTMS) in the presence of hyperbranched poly(ethyleneimine) with ethoxysilyl groups at the chain ends (PEI-Si) followed by a homopolymerization of diglycidylether of bisphenol A (DGEBA) using 1-methylimidazole (1-MI) as anionic initiator. The influence of the amount of TEOS and GPTMS in the characteristics of the coating was examined. Thin transparent films were obtained and their morphology was observed by transmission electron microscopy (TEM). The hydrolytic condensation was confirmed by 29Si-NMR studies. Cage-like nanometric structures were formed in case of adding GPTMS and bigger silica particles on adding TEOS to the formulation. Thermal stability was evaluated by thermogravimetry and the scratch resistance properties were also investigated, showing an improvement in resistance to break and to detachment in all the coatings containing GPTMS. Polymer Journal as you recommended us.As you mentioned in your decision letter the main remark is that the novelty has not been stressed sufficiently. However, the general comments of the reviewers were not bad.We recognized that the redaction did not include the novelty until we reach the discussion part and therefore we have included in the new version your opinion and we have stressed the novelty achieved in our work from the beginning. We have also included some changes suggested by the reviewers. Thus, we hope you can go further with the acceptance of our paper in European Polymer Journal.Looking forward to hearing from you, I remain. Cover LetterComments to the reviewers.Reviewer #1: Graphical abstract:It is not clear what the authors want to transmit in the graphical abstract. The paper is not directly addressing the application procedure of the coatings. The graphical abstract should be adapted to show more clearly the real work addressed in this paper. We have changed completely the graphical abstracts and we hope that the new version clearly represent the work contained in the article HighlightsThe highlights do not reflect the main findings / advances in this paper. They should be rewritten to show the key findings / novelty. We have also changed and stressed the key findings AbstractThe abstract needs to be revised. Does the TEOS / GPTMS affect the properties of the hyperbranched polymer? So yes, in which direction? The abstract should be more indicative of what the reader will find in the paper. The abstract has been rewritten. The addition of TEOS does not affect the properties of the hyperbranched polymer, but the properties of the final hybrid thermoset. The addition of TEOS leads to the formation of bigger particles, quite different from the cage-like particles formed from PEI-Si and/or GPTMS. The addition of GPTMS produces an improvement in resistance to break and to detachment in all the coatings. The incorporation of GPTMS to TEOS containing formulations allowed to prepar...

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Solvent-free synthesis of reactive inorganic precursors for preparation of organic/inorganic hybrid materials

Cited by 8 publications

References 32 publications

Synthesis and characterization of hybrid films from hyperbranched polyester using a sol–gel process

Synthesis and characterization of hybrid films from hyperbranched polyester using a sol–gel process

Preparation and characterization of organic/inorganic hybrid epoxy networks from reactive inorganic precursors

Hybrid epoxy networks from ethoxysilyl-modified hyperbranched poly(ethyleneimine) and inorganic reactive precursors

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