Ion Gel Network Formation in an Ionic Liquid Studied by Time-Resolved Small-Angle Neutron Scattering

The Journal of Physical Chemistry. B
Kei HashimotoMitsuhiro Shibayama

Abstract

We report the time-resolved small-angle neutron scattering (SANS) study of tetra-arm poly(ethylene glycol) (TetraPEG) polymer network formation in a typical ionic liquid (IL), 1-ethyl-3-methylimidazolium bis(trifluoromethanesulfonyl)amide ([C2mim][TFSA]). To observe time-dependent SANS profiles, the reaction rate for the AB-type cross-end coupling reaction of TetraPEG macromers was controlled by adding an analogous protic IL, 1-ethylimidazolium TFSA ([C2imH][TFSA]). At polymer concentrations higher than the overlap concentration ( c*), the SANS profile remained unchanged during the gelation reaction, indicating that the network structure was independent of macromer connectivity in a semidiluted solution. On the other hand, at low polymer concentrations, an increase in the SANS profile intensity was clearly observed. The correlation length (ξ), estimated by a fitting analysis based on the Ornstein-Zernike function, increased as the reaction proceeded. This result indicated that the sparsely dispersed macromers formed clusters during the cross-linking process and polymer size growth followed thereafter. We found that the network formation process and homogeneity of the network structure were strongly dependent on the polymer conc...Continue Reading

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