Curing behavior, chain dynamics, and microstructure of high Tg thiol-acrylate networks with systematically varied network heterogeneity

Jones, Brad H.; Alam, Todd M.; Lee, Sangwoo; Celina, Mathew C.; Allers, Joshua P.; Park, Sungmin; Chen, Liwen; Martinez, Estevan J.; Unangst, Jaclynn L.

doi:10.1016/j.polymer.2020.122783

Curing behavior, chain dynamics, and microstructure of high T_g thiol-acrylate networks with systematically varied network heterogeneity

Journal Article · Sun Aug 02 00:00:00 EDT 2020 · Polymer

DOI:https://doi.org/10.1016/j.polymer.2020.122783· OSTI ID:1670733

Jones, Brad H. ^[1]; Alam, Todd M. ^[1]; Lee, Sangwoo ^[2]; Celina, Mathew C. ^[1]; Allers, Joshua P. ^[1]; Park, Sungmin ^[2]; Chen, Liwen ^[2]; Martinez, Estevan J. ^[1]; Unangst, Jaclynn L. ^[1]

Sandia National Lab. (SNL-NM), Albuquerque, NM (United States)
Rensselaer Polytechnic Inst., Troy, NY (United States)

A series of networks is introduced with systematically varied network heterogeneity and high overall values of average glass transition temperature (T_g), based on polymerization of rigid acrylate and aromatic thiol monomers. The curing behavior, chain dynamics, and microstructure of these networks were investigated through a combination of dynamic mechanical analysis and infrared spectroscopy, nuclear magnetic resonance (NMR) spectroscopy, and x-ray scattering, respectively. The maximum T_g achieved during cure can be related to the breadth of the mechanical loss tangent, as others have previously suggested, as well as the temperature dependence of the chain dynamics in the network as monitored by ¹H NMR. In addition, the microstructures of the networks are characterized by periodic, fractal microgels with characteristic length scales of ca. 20–40 nm. Intriguingly, this structural motif persists in the more homogeneous networks exhibiting comparatively narrow glass transitions and chain dynamics, indicating that dynamically homogeneous networks can still exhibit significant compositional heterogeneity at the mesoscale.

View Accepted Manuscript (DOE)

Research Organization:: Sandia National Laboratories (SNL-NM), Albuquerque, NM (United States)

Sponsoring Organization:: USDOE National Nuclear Security Administration (NNSA)

Grant/Contract Number:: AC04-94AL85000

OSTI ID:: 1670733

Alternate ID(s):: OSTI ID: 1809306
OSTI ID: 1690227
OSTI ID: 1690214

Report Number(s):: SAND--2020-7087J; 687277

Journal Information:: Polymer, Journal Name: Polymer Vol. 205; ISSN 0032-3861

Publisher:: ElsevierCopyright Statement

Country of Publication:: United States

Language:: English

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36 MATERIALS SCIENCE
Glass transition
Heterogeneous polymer networks
Microstructure

Curing behavior, chain dynamics, and microstructure of high Tg thiol-acrylate networks with systematically varied network heterogeneity

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Curing behavior, chain dynamics, and microstructure of high T_g thiol-acrylate networks with systematically varied network heterogeneity