Polymerization reactions in methyltriethoxysilane studied through 29Si NMR with polarization transfer

Brunet, F.

doi:10.1016/s0022-3093(98)00403-7

Cited by 72 publications

(103 citation statements)

References 46 publications

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“…The ICSG resist was mixed in aqueous solution under acidic conditions. We used a 1:14 MTEOS/H 2 O molar ratio, and adjusted the pH at 3.1 with acetic acid, for total hydrolysis of the alkoxy-silane groups and moderate condensation [15,17]. The resist was aged for 24 h at ambient temperature before use.…”

Section: Methodsmentioning

confidence: 99%

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Nanoimprint Lithography on Silica Sol–Gels: A Simple Route to Sequential Patterning

et al. 2009

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Section: Methodsmentioning

confidence: 99%

“…The silanol groups condense into Si-O-Si siloxane bonds, and the decrease in the silanol peak intensity signals the progress of the condensation. [15] In order to reproduce the thermal cycles used during the imprinting process, an in situ heat stage was used. The FTIR experiments were performed without the poly(dimethylsiloxane) (PDMS) stamp.…”

mentioning

confidence: 99%

Nanoimprint Lithography on Silica Sol–Gels: A Simple Route to Sequential Patterning

et al. 2009

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“…The other two species found in these gels are the Q 2 species, which appears at −91.7 ppm (0%) and −91.7 ppm (30%), and the Q 4 species, which appears at −110.9 ppm (0%) and −109.9 ppm (30%). In 29 Si NMR studies, the classical notations are T for silicon with three oxygen-bridging atoms and Q for silicon with four oxygen-bridging atoms (Brunet 1998;Van Nieuwenhuyse et al 2008). …”

Section: Nmrmentioning

confidence: 99%

Characterisation of hybrid xerogels synthesised in acid media using methyltriethoxysilane (MTEOS) and tetraethoxysilane (TEOS) as precursors

et al. 2011

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The mild synthetic conditions provided by the sol-gel process and the versatility of the colloidal state allow for the mixing of inorganic and organic components at the nanometre scale in virtually any ratio for the preparation of hybrid materials. Our interest in hybrid xerogels focuses on combining their porosity with other properties to prepare optic-fibre sensors. The specific aim of this paper is to synthesise hybrid xerogels in acid media using methyltriethoxysilane (MTEOS) and tetraethoxysilane (TEOS) as silica precursors and to investigate the effect of the MTEOS molar ratio on the structure and porous texture of xerogels. Gelation time exponentially increased as the MTEOS molar ratio increased. Increasing the MTEOS molar ratio yielded xerogels with lower density and lower particle size. The incorporation of MTEOS resulted in new FTIR bands at 1276 and 791 cm −1 , which was attributed to vibrational modes of methyl group. The band around 1092 cm −1 associated with siloxane bonds shifted to lower wavenumbers and split into two bands. The 29 Si spectra only showed the Q n (n = 2, 3, 4) signal in xerogels with 0% MTEOS and the T n (n = 2, 3) signal in xerogels with 100% MTEOS; hybrid xerogels showed both Q and T signals. From XRD peaks at 2θ around 9°, we inferred that xerogels (>70% MTEOS) consisted of nanocrystalline CH 3 -SiO 3/2 species. Increasing the MTEOS molar ratio produced xerogels with lower pore volumes and lower average pore size. The integration of methyl groups on the surface decreased the surface polarity and, in turn, the characteristic energy.

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“…[31][32][33][34][35] However, hydrolysis of diethoxy silane with an excess amount of water causes the formation of different silanediols, such as D 4 , D 5 , D 6 , and the cyclic oligomers from the subsequent condensation reaction of silanols. 36,37 The hydrolysis of dimethyldiethoxy silane (DMDES) with amidized 3-(2-aminoethyl)aminopropylmethyldimethoxy silane (KLM-602) or ␥-amino-propyltriethoxy silane (␥-APS) as an internal standard and controlled by the moisture flux. Their hydrolysis and polysiloxane conversion have been investigated by NMR measurements and reported in this article.…”

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confidence: 99%

NMR spectroscopic studies of dimethyldiethoxy silane hydrolysis and polysiloxane conversion

Tsai

Lee

Chen

2002

J of Applied Polymer Sci

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ABSTRACT:The hydrolysis rate of alkoxy silane (dimethyldiethoxy silane, DMDES, etc.) is a linear relationship vs. the reaction time under the moisture flux control. The hydrolysis process results in formation of the linear polysiloxane products by a subsequent condensation reaction. An amidized alkoxy silane (3-(2-aminoethyl)aminopropylmethyldimethoxy silane, KLM-602 or ␥-aminopropyl-triethoxy silane, ␥-APS) serves as an internal standard of DMDES hydrolysis kinetics measurements. The hydrolysis kinetics of DMDES with the amidized alkoxy silane and the subsequent linear polysiloxanes conversion have been evaluated and characterized by 29 Si-and 13 C-NMR NMR spectroscopic measurements.

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Polymerization reactions in methyltriethoxysilane studied through 29Si NMR with polarization transfer

Cited by 72 publications

References 46 publications

Nanoimprint Lithography on Silica Sol–Gels: A Simple Route to Sequential Patterning

Nanoimprint Lithography on Silica Sol–Gels: A Simple Route to Sequential Patterning

Characterisation of hybrid xerogels synthesised in acid media using methyltriethoxysilane (MTEOS) and tetraethoxysilane (TEOS) as precursors

NMR spectroscopic studies of dimethyldiethoxy silane hydrolysis and polysiloxane conversion

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