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Polyester-inorganic nanocomposite ma...
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Lambert, Alexander Adam, III.
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Polyester-inorganic nanocomposite materials via sol-gel reactions: Synthesis and characterization of fundamental properties.
紀錄類型:
書目-電子資源 : Monograph/item
正題名/作者:
Polyester-inorganic nanocomposite materials via sol-gel reactions: Synthesis and characterization of fundamental properties./
作者:
Lambert, Alexander Adam, III.
面頁冊數:
131 p.
附註:
Source: Dissertation Abstracts International, Volume: 64-03, Section: B, page: 1271.
Contained By:
Dissertation Abstracts International64-03B.
標題:
Chemistry, Polymer. -
電子資源:
http://pqdd.sinica.edu.tw/twdaoapp/servlet/advanced?query=3084202
Polyester-inorganic nanocomposite materials via sol-gel reactions: Synthesis and characterization of fundamental properties.
Lambert, Alexander Adam, III.
Polyester-inorganic nanocomposite materials via sol-gel reactions: Synthesis and characterization of fundamental properties.
- 131 p.
Source: Dissertation Abstracts International, Volume: 64-03, Section: B, page: 1271.
Thesis (Ph.D.)--The University of Southern Mississippi, 2003.
A scheme was developed for producing poly(ethylene terephthalate (PET) <italic> ionomer</italic>)/silicate hybrid materials via polymer-<italic>in situ</italic> sol-gel reactions for tetraethylorthosilicate (TEOS) using different solvents. Scanning electron microscopy/EDAX studies revealed that silicate structures can be grown deep within PET ionomer films that were melt pressed from silicate-incorporated resin pellets. <super>29</super>Si solid-state NMR spectroscopy revealed considerable, successful Si-O-Si bond formation, but also a significant fraction of uncondensed SiOH groups. <super>23</super>Na solid-state NMR spectra suggested the presence of ionic aggregates within the unfilled PET ionomer and that these aggregates do not suffer major structural re-arrangements by silicate incorporation. For an ionomer treated with TEOS using MeCl<sub>2</sub> solvent, Na<super> +</super> ions are less self-associated than in the unfilled control, suggesting silicate intrusion between PET-SO<sub>3</sub><super>−</super> Na<super> +</super> ion pair associations. The ionomer treated with TEOS + tetrachloroethane had more poorly formed ionic aggregates, which illustrates the influence of solvent type on ionic aggregation. First-scan DSC thermograms for the ionomers demonstrate an increase in crystallinity after the incorporation of silicates, but solvent induced crystallization also appears to be operative. Second-scan DSC thermograms also suggest that the addition of silicate particles is not the only factor implicated in re-crystallization, and that solvent type is important even in second scan behavior. Silicate incorporation does not profoundly affect the second scan T<sub>g</sub> vs. solvent type, <italic>i.e</italic>., chain mobility in the amorphous regions is not severely restricted by silicate incorporation. Re-crystallization and melting in these hybrids appears to be due to an interplay between a solvent induced crystallization that strongly depends on solvent type, and interactions between PET chains and <italic> in situ</italic>-grown, sol-gel-derived silicate particles.Subjects--Topical Terms:
1018428
Chemistry, Polymer.
Polyester-inorganic nanocomposite materials via sol-gel reactions: Synthesis and characterization of fundamental properties.
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A scheme was developed for producing poly(ethylene terephthalate (PET) <italic> ionomer</italic>)/silicate hybrid materials via polymer-<italic>in situ</italic> sol-gel reactions for tetraethylorthosilicate (TEOS) using different solvents. Scanning electron microscopy/EDAX studies revealed that silicate structures can be grown deep within PET ionomer films that were melt pressed from silicate-incorporated resin pellets. <super>29</super>Si solid-state NMR spectroscopy revealed considerable, successful Si-O-Si bond formation, but also a significant fraction of uncondensed SiOH groups. <super>23</super>Na solid-state NMR spectra suggested the presence of ionic aggregates within the unfilled PET ionomer and that these aggregates do not suffer major structural re-arrangements by silicate incorporation. For an ionomer treated with TEOS using MeCl<sub>2</sub> solvent, Na<super> +</super> ions are less self-associated than in the unfilled control, suggesting silicate intrusion between PET-SO<sub>3</sub><super>−</super> Na<super> +</super> ion pair associations. The ionomer treated with TEOS + tetrachloroethane had more poorly formed ionic aggregates, which illustrates the influence of solvent type on ionic aggregation. First-scan DSC thermograms for the ionomers demonstrate an increase in crystallinity after the incorporation of silicates, but solvent induced crystallization also appears to be operative. Second-scan DSC thermograms also suggest that the addition of silicate particles is not the only factor implicated in re-crystallization, and that solvent type is important even in second scan behavior. Silicate incorporation does not profoundly affect the second scan T<sub>g</sub> vs. solvent type, <italic>i.e</italic>., chain mobility in the amorphous regions is not severely restricted by silicate incorporation. Re-crystallization and melting in these hybrids appears to be due to an interplay between a solvent induced crystallization that strongly depends on solvent type, and interactions between PET chains and <italic> in situ</italic>-grown, sol-gel-derived silicate particles.
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Isothermal studies confirmed that the crystallization rate and melting behavior of PET 5% Na<super>+</super> ionomers depend on processing conditions.
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PET ionomer/ORMOSIL composites were formed via <italic>in situ</italic> sol-gel reactions using the ionic regions of PET as preferential reaction sites. TGA analysis revealed successful uptake for all three different solvents and TEOS:MTES composition ratios. TGA derivative curves suggest that for the THF and MeCl<sub>2</sub> carrier solvent systems the MTES-generated network interacts more with the PET ionomer matrix. In the case of TCE, the TEOS-generated network interaction appears to be more operative. First scan DSC traces reveal that the <italic>in situ</italic> sol-gel processing of ORMOSIL phases induces PET ionomer crystallinity, although systems with higher silicate uptake have reduced induced crystallinity. Second scan DSC traces show that T<sub>g</sub> is not effected by the incorporation of silicates into the PET ionomer. Also, for the ORMOSIL phases generated using THF and MeCl<sub>2</sub> as the swelling solvent, only the pure silicate networks (synthesized using only TEOS) allow recrystallization and melting during the quick scan timeframe. It is thought that the presence of semi-organic MTES silicate networks do not allow fast nucleation onto the inorganic nuclei. (Abstract shortened by UMI.)
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