Polymerization of hybrid organic-inorganic materials from several silicon compounds followed by TGA/DTA, FTIR and NMR techniques

Hybrid organic-inorganic films have been prepared by hydrolysis and condensation of several silicon compounds: 3-methacryloxypropyltrimethoxysilane (MPTS) or methyltriethoxysilane (MTES) and tetraethyl orthosilicate (TEOS) or tetramethyl orthosilicate (TMOS) precursors using four [TEOS] or [TMOS]/[M...

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Bibliographic Details
Authors: Criado Sanz, María, Sobrados, Isabel, Sanz Lázaro, Jesús
Format: article
Status:Versión aceptada para publicación
Publication Date:2014
Country:España
Institution:Consejo Superior de Investigaciones Científicas (CSIC)
Repository:DIGITAL.CSIC. Repositorio Institucional del CSIC
OAI Identifier:oai:digital.csic.es:10261/98981
Online Access:http://hdl.handle.net/10261/98981
Access Level:Open access
Keyword:NMR
Sol–gel synthesis
Dimensionality
Polymerization
Organic–inorganic hybrids
Description
Summary:Hybrid organic-inorganic films have been prepared by hydrolysis and condensation of several silicon compounds: 3-methacryloxypropyltrimethoxysilane (MPTS) or methyltriethoxysilane (MTES) and tetraethyl orthosilicate (TEOS) or tetramethyl orthosilicate (TMOS) precursors using four [TEOS] or [TMOS]/[MPTS] or [MTES] molar ratios: 0, 0.5, 1 and 2. The progress on the organic and inorganic polymerizations was followed employing thermogravimetric analysis (TGA), differential thermal analysis (DTA), Fourier transform infrared spectroscopy (FTIR), 13C and 29Si nuclear magnetic resonance (NMR). These techniques have provided information about the hybrid network formation inside films. The formation of the hybrids prepared from [TEOS]/[MPTS] and [TMOS]/[MPTS] mixtures was accomplished through the reaction of SiOR groups, via condensation of silanols (inorganic condensation), and opening of the CC double bond in MPTS (organic polymerization). The formation of the hybrids prepared from [TEOS]/[MTES] and [TMOS]/[MTES] mixtures was mainly accomplished through the reaction of SiOR groups. The increment of TEOS or TMOS in MPTS mixtures favored the inorganic (Q3 and Q4 units) condensation. Total degrees of condensation for hybrids synthetized with [TEOS] or [TMOS]/[MTES] were higher than those obtained with [TEOS] or [TMOS]/[MPTS], so MTES favored the formation of hybrids with branched organic structures.

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