Imaging a solvent‐swollen polymer gel network by open liquid transmission electron microscopy

Author:

Srivastava Satyam1ORCID,Ribbe Alexander E.1,Russell Thomas P.123ORCID,Hoagland David A.1ORCID

Affiliation:

1. Department of Polymer Science and Engineering University of Massachusetts Amherst Amherst Massachusetts USA

2. Materials Sciences Division Lawrence Berkeley National Laboratory Berkeley California USA

3. Advanced Institute for Materials Research (WPI‐AIMR) Tohoku University Sendai Japan

Abstract

AbstractVisualizing the network of a solvent‐swollen polymer gel remains problematic. To address this challenge, open transmission electron microscopy (TEM) was applied to thin gel films permeated by a nonvolatile ionic liquid. The targeted physical gels were prepared by cooling concentrated solutions of poly(ethylene glycol) in 1‐ethyl‐3‐methyl imidazolium ethyl sulfate [EMIM][EtSO4]. During the cooling, gelation occurred by a frustrated crystallization of the dissolved polymer, leading to a percolated, solvent‐permeated semicrystalline network in which nanoscale polymer crystals acted as crosslinks. Crystalline features ranging from ~5 to ~200 nm were observed, with the visible network strands dominantly consisting of long curvilinear crystallites of ~15–20 nm diameter. Nascent spherulites irregularly decorated the network, creating a complex structural hierarchy that complicated analyses. Lacking diffraction contrast, TEM did not visualize the many disordered, fully solvated PEG chains present in the voids between crystals. Recognizing that a network's three dimensionality is ambiguous when assessed through two‐dimensional microscopy projections, a small gel region was studied by TEM tomography, revealing a nearly isotropic three‐dimensional arrangement of the curvilinear crystallites, which displayed remarkably uniform cylindrical cross sections.

Funder

National Science Foundation

Publisher

Wiley

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