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Solid-state nuclear magnetic resonance characterization of PE–PEG/silica hybrid materials prepared by microwave-assisted sol-gel process

Published online by Cambridge University Press:  31 January 2011

Marco Geppi ,
Giulia Mollica ,
Silvia Borsacchi ,
Michele Marini ,
Maurizio Toselli  and
Francesco Pilati
Marco Geppi*
Affiliation:
Dipartimento di Chimica e Chimica Industriale, Università di Pisa, Via Risorgimento 35, 56126 Pisa, Italy
Giulia Mollica
Affiliation:
Dipartimento di Chimica e Chimica Industriale, Università di Pisa, Via Risorgimento 35, 56126 Pisa, Italy
Silvia Borsacchi
Affiliation:
Dipartimento di Chimica e Chimica Industriale, Università di Pisa, Via Risorgimento 35, 56126 Pisa, Italy
Michele Marini
Affiliation:
Dipartimento di Ingegneria dei Materiali e dell’Ambiente, Università di Modena e Reggio Emilia, Via Vignolese 905/A, 41100 Modena, Italy; and Reference Research Centre LABoratorio di Nanocompositi e Ibridi Polimerici multifunzionali (NIPLAB) of consorzio Interuniversitario Nazionale per la Scienza e Tecnologia dei Materiali (INSTM) Consortium, Italy
Maurizio Toselli
Affiliation:
Dipartimento di Chimica Applicata e Scienza dei Materiali, Università di Bologna, Viale Risorgimento 2, 40136 Bologna, Italy; and Reference Research Centre LABoratorio di Nanocompositi e Ibridi Polimerici multifunzionali (NIPLAB) of consorzio Interuniversitario Nazionale per la Scienza e Tecnologia dei Materiali (INSTM) Consortium, Italy
Francesco Pilati
Affiliation:
Dipartimento di Ingegneria dei Materiali e dell’Ambiente, Università di Modena e Reggio Emilia, Via Vignolese 905/A, 41100 Modena, Italy; and Reference Research Centre LABoratorio di Nanocompositi e Ibridi Polimerici multifunzionali (NIPLAB) of consorzio Interuniversitario Nazionale per la Scienza e Tecnologia dei Materiali (INSTM) Consortium, Italy
*
a)Address all correspondence to this author.e-mail: [email protected]
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Abstract

Organic–inorganic hybrid materials were prepared by sol-gel processes starting from tetraethoxysilane (TEOS) and a triethoxysilane-terminated polyethylene–b-poly(ethylene glycol) copolymer (PE–PEG–Si). Curing of the initial reactant solution was carried out under different reaction conditions, and the materials so obtained were investigated by solid-state nuclear magnetic resonance (NMR). In particular, the molecular structure resulting from a conventional oven heating was compared with that obtained by unconventional microwave heating. The results highlighted that the extent of condensation reactions occurring over several hours under conventional heating is very similar to that resulting in 1 min under microwave heating. Additionally, 29Si–magic angle spinning (MAS) spectra showed that even though the overall extent of cross-linking in the inorganic network is only slightly affected by the thermal history of the sample, significantly different distributions of silicon sites can be present. 13C–CP/MAS selective spectra revealed the presence of PE “crystalline” domains within the organic phase, not detectable by differential scanning calorimetry (DSC). Finally, 1H–MAS spectra showed that different hydrogen-bond interactions are present in samples obtained under different curing conditions.

Keywords

Nuclear magnetic resonance (NMR)Microwave heatingSol-gel
Type
Articles
Information
Journal of Materials Research , Volume 22 , Issue 12 , December 2007 , pp. 3516 - 3525
Copyright
Copyright © Materials Research Society 2007

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