期刊
CRYSTALS
卷 12, 期 11, 页码 -出版社
MDPI
DOI: 10.3390/cryst12111579
关键词
polymer microparticles; metal particles; C-13 solid-state NMR; crystalline structure; relaxation times
资金
- Fundacao para a Ciencia e Tecnologia (FCT) [UID/CTM/50025/2019, PD/BD/114372/2016]
- [CTTI-51/18-IPC]
This study investigates the effect of metal fillers on the structure and molecular dynamics of polyamide 6 microparticles. Results show that the type and concentration of metal fillers have a significant impact on the crystallinity and molecular mobility of the microparticles.
Polymer microparticles are used in additive manufacturing, separation and purification devices, biocatalysis, or for the recognition of biomolecules. This study reports on the effect of metal fillers on the structure and molecular dynamics of polyamide 6 (PA6) microparticles (MPs) containing up to 19 wt.% of Al, Cu, or Mg. These hybrid MPs are synthesized via reactive microencapsulation by anionic ring-opening polymerization in solution, in the presence of the metal filler. C-13 high-resolution solid-state NMR (ssNMR) spectroscopy is employed as the primary characterization method using magic angle spinning (MAS) and cross-polarization (CP)/MAS. Depending on the metal filler, the ssNMR crystallinity index of the MP varies between 39-50%, as determined by deconvolution of the C-13 MAS and CP/MAS spectra. These values correlate very well with the crystallinity derived from thermal or X-ray diffraction data. The molecular dynamics study on PA6 and Cu-containing MP shows similar mobility of carbon nuclei in the kHz, but not in the MHz frequency ranges. The paramagnetic Al and Mg have an observable effect on the relaxation; however, conclusions regarding the PA6 carbon motions cannot be unequivocally made. These results are useful in the preparation of hybrid microparticles with customized structures and magneto-electrical properties.
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