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Materials 2018, 11(2), 275; doi:10.3390/ma11020275

Thermal Behavior and Structural Study of SiO2/Poly(ε-caprolactone) Hybrids Synthesized via Sol-Gel Method

1
Department of Basic and Applied Science for Engineering (S.B.A.I.), Sapienza University of Rome, via del Castro Laurenziano 7, Roma, I-00161, Italy
2
Department of Sustainability, ENEA-Casaccia Research Center, Via Anguillarese 301, Rome, 00123, Italy
3
Ecoricerche S.r.l., Via Principi Normanni, Capua 81043, Italy
4
Department of Industrial and Information Engineering, University of Campania Luigi Vanvitelli, via Roma 29, Aversa, 81031, Italy
*
Authors to whom correspondence should be addressed.
Received: 15 January 2018 / Revised: 6 February 2018 / Accepted: 6 February 2018 / Published: 10 February 2018
(This article belongs to the Special Issue Sol-Gel Chemistry Applied to Materials Science)
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Abstract

SiO2-based organic-inorganic hybrids (OIHs) are versatile materials whose properties may change significantly because of their thermal treatment. In fact, after their preparation at low temperature by the sol-gel method, they still have reactive silanol groups due to incomplete condensation reactions that can be removed by accelerating these processes upon heating them in controlled experimental conditions. In this study, the thermal behavior of pure SiO2 and four SiO2-based OIHs containing increasing amount (6, 12, 24 and 50 wt %) of poly(ε-caprolactone) (PCL) has been studied by simultaneous thermogravimetry (TG) and differential scanning calorimetry (DSC). The FTIR analysis of the gas mixture evolved at defined temperatures from the samples submitted to the TG experiments identified the mechanisms of thermally activated processes occurring upon heating. In particular, all samples already release ethanol at low temperature. Moreover, thermal degradation of PCL takes place in the richest-PCL sample, leading to 5-hexenoic acid, H2O, CO2, CO and ε-caprolactone. After the samples’ treatment at 450, 600 and 1000 °C, the X-ray diffraction (XRD) spectra revealed that they were still amorphous, while the presence of cristobalite is found in the richest-PCL material. View Full-Text
Keywords: sol-gel method; SiO2–based hybrids; poly(ε-caprolactone); TG-DSC; TG-FTIR; X-ray diffraction analysis sol-gel method; SiO2–based hybrids; poly(ε-caprolactone); TG-DSC; TG-FTIR; X-ray diffraction analysis
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This is an open access article distributed under the Creative Commons Attribution License which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited. (CC BY 4.0).

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MDPI and ACS Style

Vecchio Ciprioti, S.; Tuffi, R.; Dell’Era, A.; Dal Poggetto, F.; Bollino, F. Thermal Behavior and Structural Study of SiO2/Poly(ε-caprolactone) Hybrids Synthesized via Sol-Gel Method. Materials 2018, 11, 275.

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