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Novel sol–gel derived PLA-siloxane-PEO nanocomposite with enhanced thermal properties and hydrolytic stability

  • Original Paper: Nano-structured materials (particles, fibers, colloids, composites, etc.)
  • Published:
Journal of Sol-Gel Science and Technology Aims and scope Submit manuscript

Abstract

This work presents the synthesis, structural investigation, and some properties of a new PLA-Siloxane-PEO hybrid featuring covalent bonds between polymers and siloxane nodes. The synthesis simultaneously connecting PLA and PEO chains directly to the inorganic phase is first achieved through the use of sol–gel process. The structural features, thermal properties and chemical stability of this biocompatible system have been studied by Fourier-transform infrared spectroscopy (FTIR), Raman spectroscopy, 29Si Nuclear Magnetic Resonance (NMR), scanning electron microscopy (MEV), X-ray diffraction (XRD), small-angle X-ray scattering (SAXS), thermogravimetric analysis (TGA), and differential scanning calorimetry (DSC). SEM and SAXS measurements showed that the siloxane nodes act as crosslinks between the polymer chains promoting high miscibility between PLA and PEO. FTIR, Raman XRD, DSC, and TGA showed that the presence of the siloxane nodes diminishes the crystallinity of both polymers and increases their thermal resistance. In addition to the absence of brittleness due to the low crystalline character of PLA, this new material exhibits a fantastic resistance to PLA degradation in aqueous medium, attributed both to the presence of the siloxane particles acting as a barrier towards water diffusion and to the hydrophilic PEO segments which may attract water molecules, preventing PLA hydrolysis. All of these characteristics offer an amazing perspective for the use of this hybrid material in biological, medical, and pharmaceutical applications.

Structural model of the new PLA-Siloxane-PEO composite in which PEO chains, PLA chains, and siloxane particles are interpenetrated at nanoscopic scale. Such structure induces simultaneously high thermal stability, high resistance to degradation, and absence of brittleness.

Highlights

  • Siloxane nodes bonded to polymer chains promotes PLA–PEO miscibility.

  • Presence of siloxane nodes promote PLA–PEO miscibility enhances PLA thermal stability and inhibits PLA crystallization and degradation.

  • Low PLA crystallinity induces absence of brittleness.

  • Presence of siloxane nodes and PEO inhibits PLA degradation.

  • Biocompatible material exhibiting high chemical stability in aqueous medium.

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Data availability

All data generated during the study are available from the corresponding author by request.

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Acknowledgements

This study was financed in part by the Coordenação de Aperfeiçoamento de Pessoal de Nível Superior—Brasil (CAPES) Finance Code 001. Instituto de Química of UNESP (Araraquara, Brazil) for Si29 NMR results. Centro de Tecnologia Mineral-CETEM of UFRJ (Rio de Janeiro, Brazil) for the opportunity of SEM and Raman measurements. Helmholtz-Zentrum Berlin für Materialien und Energie (Germany), for the SEM Images at high magnification. Laboratório Nacional de Luz Síncrotron (LNLS, Campinas, Brazil) for providing beamtime in the line SAXS1 (Proposal ID:20190043) and XRD beamlines. This work benefited from the use of the SasView application, originally developed under NSF award DMR-0520547. SasView contains code developed with funding from the European Union’s Horizon 2020 research and innovation program under the SINE2020 project, grant agreement No 654000.

Author contributions

ROS: Conceptualization, methodology, validation, formal analysis, investigation, data curation, writing—original draft, and visualization; JMR: validation, investigation; ACS: conceptualization, methodology, resources, writing review and editing, funding acquisition; KD: conceptualization, methodology, resources, writing review and editing, supervision, project administration, funding acquisition.

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  1. Instituto de Macromoléculas Professora Eloisa Mano (IMA), Universidade Federal do Rio de Janeiro (UFRJ), Centro de Tecnologia, Bloco J, Cidade Universitária, Avenida Horácio Macedo, 2030, Rio de Janeiro-RJ, 21941-598, Brazil

    Ranielle de Oliveira Silva, Alexandre Carneiro Silvino, Jessica Massa Ribeiro & Karim Dahmouche

  2. Campus de Duque de Caxias, Universidade Federal do Rio de Janeiro (UFRJ), Duque de Caxias-RJ, 25265-970, Brazil

    Karim Dahmouche

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  1. Ranielle de Oliveira Silva
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Silva, R.d.O., Silvino, A.C., Ribeiro, J.M. et al. Novel sol–gel derived PLA-siloxane-PEO nanocomposite with enhanced thermal properties and hydrolytic stability. J Sol-Gel Sci Technol 99, 512–526 (2021). https://doi.org/10.1007/s10971-021-05611-0

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