期刊
NATURE COMMUNICATIONS
卷 12, 期 1, 页码 -出版社
NATURE PORTFOLIO
DOI: 10.1038/s41467-021-26773-z
关键词
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资金
- DoD through the ARO [W911NF-17-1-0326]
- MURI [W911NF-15-1-0568]
- NSF [CHE-MSN 1905270]
- Soft and Hybrid Nanotechnology Experimental (SHyNE) Resource [NSF ECCS-1542205]
- MRSEC program at the Materials Research Center
- International Institute for Nanotechnology (IIN)
- Keck Foundation
- State of Illinois, through the IIN
- State of Illinois
- Office of The Director, National Institutes of Health of the National Institutes of Health [S10OD026871]
- U.S. Department of Energy, Office of Science [DE-AC02-06CH11357]
- E. I. DuPont de Nemours and Co
- Dow Chemical Company
- Northwestern University
- Ryan Fellowship
- International Institute for Nanotechnology at Northwestern University
Thermoresponsive polymeric materials were studied using liquid-cell transmission electron microscopy combined with variable temperature small angle X-ray scattering to gain insight into their phase transitions and nanoscale assembly dynamics. The multimodal approach provided direct visualization of solvated nanoscale structures and thermally-induced transitions, showing the formation and slow relaxation of core-shell particles with complex microphase separation in the core.
Thermoresponsive polymers are used in numerous technological applications but well established, direct techniques for elucidating their elevated temperature, solution-phase, nanoscale morphologies and dynamics are lacking. Here, the authors examine thermoresponsive polymeric materials by liquid-cell transmission electron microscopy and gain insight into their thermal-responsive behaviour. Herein, phase transitions of a class of thermally-responsive polymers, namely a homopolymer, diblock, and triblock copolymer, were studied to gain mechanistic insight into nanoscale assembly dynamics via variable temperature liquid-cell transmission electron microscopy (VT-LCTEM) correlated with variable temperature small angle X-ray scattering (VT-SAXS). We study thermoresponsive poly(diethylene glycol methyl ether methacrylate) (PDEGMA)-based block copolymers and mitigate sample damage by screening electron flux and solvent conditions during LCTEM and by evaluating polymer survival via post-mortem matrix-assisted laser desorption/ionization imaging mass spectrometry (MALDI-IMS). Our multimodal approach, utilizing VT-LCTEM with MS validation and VT-SAXS, is generalizable across polymeric systems and can be used to directly image solvated nanoscale structures and thermally-induced transitions. Our strategy of correlating VT-SAXS with VT-LCTEM provided direct insight into transient nanoscale intermediates formed during the thermally-triggered morphological transformation of a PDEGMA-based triblock. Notably, we observed the temperature-triggered formation and slow relaxation of core-shell particles with complex microphase separation in the core by both VT-SAXS and VT-LCTEM.
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