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A master's thesis from Aalborg University
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Synthesis and Characterization of a Hybrid SiO2 /PCL Material via Sol-Gel Synthesis

Author

Term

4. Term

Publication year

2022

Submitted on

Pages

44

Abstract

Dette speciale undersøger sol-gel-syntese af et hybridmateriale baseret på silica og polycaprolacton (SiO2/PCL) samt dets grundlæggende egenskaber. For at muliggøre netværksdannelse i den organiske fase blev PCL’s endestoppe funktionaliseret med akrylatgrupper, hvorefter den modificerede polymer blev kombineret med en dannende silicanetværk med henblik på samtidig krydsbinding og polymerisering af den uorganiske fase. Vellykket modifikation af PCL blev bekræftet ved 1H-NMR-spektroskopi, og der blev fremstillet transparente, homogene monolitiske prøver med op til 20 % polymerindhold. Materialernes struktur og sammensætning blev karakteriseret ved FTIR- og XRD-spektroskopi samt termogravimetrisk analyse (TGA). Krydsbinding kunne opnås i PCL-opløsninger, men ikke i det hybride materiale, som derfor forblev for sprødt til mekaniske målinger. Forekomsten af revner, sandsynligvis relateret til gelens svind under tørring, understreger behovet for yderligere organisk krydsbinding for at give tilstrækkelig sammenhæng i det hybride netværk.

This thesis investigates the sol-gel synthesis of a silica/polycaprolactone (SiO2/PCL) hybrid material and its basic properties. To enable network formation in the organic phase, PCL end groups were functionalized with acrylate moieties, and the modified polymer was combined with a forming silica network to target simultaneous cross-linking and inorganic polymerization. Successful PCL modification was confirmed by 1H NMR spectroscopy, and transparent, homogeneous monolithic samples with up to 20% polymer content were obtained. The materials’ structure and composition were characterized by FTIR and XRD spectroscopy and thermogravimetric analysis (TGA). Cross-linking was achieved in PCL solutions but not within the hybrid materials, which remained too brittle for mechanical testing. The occurrence of cracks, likely related to gel shrinkage during drying, highlights the need for additional organic cross-linking to impart sufficient integrity to the hybrid network.

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