Dynamics of Polymerization and Gelation in Epoxy Nanocomposites via X-ray Photon Correlation Spectroscopy

Trigg, Edward B.; Wiegart, Lutz; Fluerasu, Andrei; Koerner, Hilmar

doi:10.1021/acs.macromol.1c00727

Dynamics of Polymerization and Gelation in Epoxy Nanocomposites via X-ray Photon Correlation Spectroscopy

Journal Article · Thu Jun 17 00:00:00 EDT 2021 · Macromolecules

DOI:https://doi.org/10.1021/acs.macromol.1c00727· OSTI ID:1807930

^[1]; ^[2]; Fluerasu, Andrei ^[2]; ^[3]

Air Force Research Lab. (AFRL), Wright-Patterson AFB, OH (United States); UES, Inc., Dayton, OH (United States)
Brookhaven National Lab. (BNL), Upton, NY (United States)
Air Force Research Lab. (AFRL), Wright-Patterson AFB, OH (United States)

The details of the curing process of epoxy resins are notoriously difficult to ascertain, hampering polymer matrix composite manufacturing. Here, the curing of a series of six epoxy resins containing dilute spherical nanoparticles was investigated via X-ray photon correlation spectroscopy (XPCS). The resin formulation was varied to achieve a range of crosslink densities and topologies. Prior to gelation, the viscosities obtained from XPCS agreed with bulk rheology. A clear dynamic transition was detected in all samples, where the q-scaling changes from approximately q2^.2 to q¹, indicating a transition from sub-diffusive to ballistic-like nanoparticle motion. For the samples with a high crosslink density, this change was abrupt and coincided with gelation, and there was no evidence of crosslink heterogeneity. Chain entanglement played a role in the transition for samples with lower crosslink density. Finally, this work reveals the potential of XPCS to deliver new quantitative insights into the curing process of thermosetting resins.

View Accepted Manuscript (DOE)

Research Organization:: Brookhaven National Laboratory (BNL), Upton, NY (United States)

Sponsoring Organization:: USDOE Office of Science (SC), Basic Energy Sciences (BES)

Grant/Contract Number:: SC0012704

OSTI ID:: 1807930

Report Number(s):: BNL--221714-2021-JAAM

Journal Information:: Macromolecules, Journal Name: Macromolecules Journal Issue: 13 Vol. 54; ISSN 0024-9297

Publisher:: American Chemical SocietyCopyright Statement

Country of Publication:: United States

Language:: English

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Related Subjects

36 MATERIALS SCIENCE
amines
epoxy
fluid dynamics
gelation
nanocomposite
organic polymers
thermoset
viscosity
x-ray photon correlation spectroscopy

Dynamics of Polymerization and Gelation in Epoxy Nanocomposites via X-ray Photon Correlation Spectroscopy

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