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Title: Investigating Chain Dynamics in Highly Crosslinked Polymers using Solid–State 1H NMR Spectroscopy

Abstract

Solid state 1H NMR line–shape analysis and (double quantum) DQ 1H NMR experiments have been used to investigate the segmental and polymer chain dynamics as a function of temperature for a series of thermosetting epoxy resins produced using different diamine curing agents. In these thermosets, chemical crosslinks introduce topological constraints leading to residual stresses during curing. Materials containing a unique ferrocene–based diamine (FcDA) curing agent were evaluated to address the role of the ferrocene fluxional process on the atomic–level polymer dynamics. Here, at temperatures above the glass transition temperature (Tg), the DQ 1H NMR experiments provided a measure of the relative effective crosslink and entanglement densities for these materials and revealed significant polymer chain dynamic heterogeneity in the FcDA–cured thermosets.

Authors:
ORCiD logo [1]; ORCiD logo [1]
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  1. Sandia National Lab. (SNL-NM), Albuquerque, NM (United States)
Publication Date:
Research Org.:
Sandia National Lab. (SNL-NM), Albuquerque, NM (United States)
Sponsoring Org.:
USDOE National Nuclear Security Administration (NNSA)
OSTI Identifier:
1559498
Report Number(s):
SAND-2019-8648J
Journal ID: ISSN 0887-6266; 677894
Grant/Contract Number:  
AC04-94AL85000
Resource Type:
Accepted Manuscript
Journal Name:
Journal of Polymer Science. Part B, Polymer Physics
Additional Journal Information:
Journal Volume: 57; Journal Issue: 17; Journal ID: ISSN 0887-6266
Publisher:
Wiley
Country of Publication:
United States
Language:
English
Subject:
37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY; DGEBA; DQ; epoxies; NMR; thermosets

Citation Formats

Alam, Todd M., and Jones, Brad H. Investigating Chain Dynamics in Highly Crosslinked Polymers using Solid–State 1H NMR Spectroscopy. United States: N. p., 2019. Web. doi:10.1002/polb.24869.
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Alam, Todd M., & Jones, Brad H. Investigating Chain Dynamics in Highly Crosslinked Polymers using Solid–State 1H NMR Spectroscopy. United States. https://doi.org/10.1002/polb.24869
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Alam, Todd M., and Jones, Brad H. Fri . "Investigating Chain Dynamics in Highly Crosslinked Polymers using Solid–State 1H NMR Spectroscopy". United States. https://doi.org/10.1002/polb.24869. https://www.osti.gov/servlets/purl/1559498.
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@article{osti_1559498,
title = {Investigating Chain Dynamics in Highly Crosslinked Polymers using Solid–State 1H NMR Spectroscopy},
author = {Alam, Todd M. and Jones, Brad H.},
abstractNote = {Solid state 1H NMR line–shape analysis and (double quantum) DQ 1H NMR experiments have been used to investigate the segmental and polymer chain dynamics as a function of temperature for a series of thermosetting epoxy resins produced using different diamine curing agents. In these thermosets, chemical crosslinks introduce topological constraints leading to residual stresses during curing. Materials containing a unique ferrocene–based diamine (FcDA) curing agent were evaluated to address the role of the ferrocene fluxional process on the atomic–level polymer dynamics. Here, at temperatures above the glass transition temperature (Tg), the DQ 1H NMR experiments provided a measure of the relative effective crosslink and entanglement densities for these materials and revealed significant polymer chain dynamic heterogeneity in the FcDA–cured thermosets.},
doi = {10.1002/polb.24869},
journal = {Journal of Polymer Science. Part B, Polymer Physics},
number = 17,
volume = 57,
place = {United States},
year = {2019},
month = {8}
}
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https://doi.org/10.1002/polb.24869
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Cited by: 7 works
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Figures / Tables:

FIGURE 1 FIGURE 1: Chemical structure of the epoxy resin and curing agents being investigated.
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    Figures / Tables found in this record:

    FIGURE 1 (p. 4)figure
    FIGURE 2 (p. 7)figure
    Figure 3 (p. 11)figure
    Table 1 (p. 12)table
    FIGURE 4 (p. 13)figure
    FIGURE 5 (p. 16)figure
    FIGURE 6 (p. 18)figure
    FIGURE 7 (p. 20)figure
    FIGURE 8 (p. 22)figure
    FIGURE 9 (p. 23)figure
    Table 2 (p. 24)table
    Table 3 (p. 24)table
    FIGURE 10 (p. 25)figure
    Table 4 (p. 25)table
    FIGURE 11 (p. 28)figure
    FIGURE S1 (p. 39)figure
    FIGURE S2 (p. 40)figure
    FIGURE S3 (p. 41)figure
    FIGURE S4 (p. 42)figure
    FIGURE S5 (p. 43)figure
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