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Morphological investigation of ternary and semicrystalline organic-inorganic hybrid nanocomposite

da Silva, Laura C. E. ; do Carmo Gonçalves, Maria and Plivelic, Tomás LU (2022) In Journal of Materials Science 57. p.6196-6211
Abstract
Organic–inorganic (O–I) hybrid nanocomposites have already been widely investigated in the optoelectronic industry and are emerging in the biomedical field. In both cases, a thorough knowledge of the O–I hybrid morphology is key for reaching tailored properties of the devices; however, up to now little is known on this matter. Herein, we used advanced X-ray scattering and microscopy techniques to investigate in detail the morphology and nanostructure of a biocompatible, ternary, and semicrystalline O–I hybrid nanocomposite made up of poly(ε-caprolactone) (PCL) and poly(ethylene glycol) (PEG), cross-linked by in situ-generated silsesquioxane structures (SS). Results showed that phase separation occurred at all length scales. At the... (More)
Organic–inorganic (O–I) hybrid nanocomposites have already been widely investigated in the optoelectronic industry and are emerging in the biomedical field. In both cases, a thorough knowledge of the O–I hybrid morphology is key for reaching tailored properties of the devices; however, up to now little is known on this matter. Herein, we used advanced X-ray scattering and microscopy techniques to investigate in detail the morphology and nanostructure of a biocompatible, ternary, and semicrystalline O–I hybrid nanocomposite made up of poly(ε-caprolactone) (PCL) and poly(ethylene glycol) (PEG), cross-linked by in situ-generated silsesquioxane structures (SS). Results showed that phase separation occurred at all length scales. At the microscale, irreversible PCL/PEG phase separation generated a globular morphology, where PEG-rich spherical domains were uniformly distributed within a PCL-rich matrix. At the nanoscale, partial organic/inorganic phase segregation resulted in the formation of polysilsesquioxane nanoparticles in both matrix and domains. Finally, an unusual crystalline behaviour was observed for the ternary O–I hybrid nanocomposite, PCL-PEG/SS, where PCL crystallization was anticipated and PEG crystallization was delayed in comparison with the binary PCL/SS and PEG/SS O–I hybrids as well as to a blend of the uncross-linked PCL and PEG precursors. These results provide new insights on how the competing processes of phase separation, crystallization, and inorganic cross-linking affect the overall morphology and nanostructure of O–I hybrid nanocomposites and, therefore, might be useful for establishing relevant structure–property relationships. (Less)
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author
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organization
publishing date
type
Contribution to journal
publication status
published
subject
in
Journal of Materials Science
volume
57
pages
16 pages
publisher
Springer
external identifiers
  • scopus:85126146274
ISSN
0022-2461
DOI
10.1007/s10853-022-07003-3
project
Structural Characterization of Multicomponent Biodegradable Polymeric Systems by Synchrotron X-ray Scattering and Transmission Electron Microscopy
language
English
LU publication?
yes
id
30c6c768-d2cd-4ca6-a4c7-9cf67fb806c8
date added to LUP
2022-07-20 11:36:48
date last changed
2022-08-22 04:04:02
@article{30c6c768-d2cd-4ca6-a4c7-9cf67fb806c8,
  abstract     = {{Organic–inorganic (O–I) hybrid nanocomposites have already been widely investigated in the optoelectronic industry and are emerging in the biomedical field. In both cases, a thorough knowledge of the O–I hybrid morphology is key for reaching tailored properties of the devices; however, up to now little is known on this matter. Herein, we used advanced X-ray scattering and microscopy techniques to investigate in detail the morphology and nanostructure of a biocompatible, ternary, and semicrystalline O–I hybrid nanocomposite made up of poly(ε-caprolactone) (PCL) and poly(ethylene glycol) (PEG), cross-linked by in situ-generated silsesquioxane structures (SS). Results showed that phase separation occurred at all length scales. At the microscale, irreversible PCL/PEG phase separation generated a globular morphology, where PEG-rich spherical domains were uniformly distributed within a PCL-rich matrix. At the nanoscale, partial organic/inorganic phase segregation resulted in the formation of polysilsesquioxane nanoparticles in both matrix and domains. Finally, an unusual crystalline behaviour was observed for the ternary O–I hybrid nanocomposite, PCL-PEG/SS, where PCL crystallization was anticipated and PEG crystallization was delayed in comparison with the binary PCL/SS and PEG/SS O–I hybrids as well as to a blend of the uncross-linked PCL and PEG precursors. These results provide new insights on how the competing processes of phase separation, crystallization, and inorganic cross-linking affect the overall morphology and nanostructure of O–I hybrid nanocomposites and, therefore, might be useful for establishing relevant structure–property relationships.}},
  author       = {{da Silva, Laura C. E. and do Carmo Gonçalves, Maria and Plivelic, Tomás}},
  issn         = {{0022-2461}},
  language     = {{eng}},
  month        = {{03}},
  pages        = {{6196--6211}},
  publisher    = {{Springer}},
  series       = {{Journal of Materials Science}},
  title        = {{Morphological investigation of ternary and semicrystalline organic-inorganic hybrid nanocomposite}},
  url          = {{http://dx.doi.org/10.1007/s10853-022-07003-3}},
  doi          = {{10.1007/s10853-022-07003-3}},
  volume       = {{57}},
  year         = {{2022}},
}