Selective molecular annealing: in situ small angle X-ray scattering study of microwave-assisted annealing of block copolymers

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Toolan, Daniel T. W.
Adlington, Kevin
Isakova, Anna
Kalamiotis, Alexis
Mokarian-Tabari, Parvaneh
Dimitrakis, Georgios
Dodds, Christopher
Arnold, Thomas
Terrill, Nick J.
Bras, Wim
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Royal Society of Chemistry
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Microwave annealing has emerged as an alternative to traditional thermal annealing approaches for optimising block copolymer self-assembly. A novel sample environment enabling small angle X-ray scattering to be performed in situ during microwave annealing is demonstrated, which has enabled, for the first time, the direct study of the effects of microwave annealing upon the self-assembly behavior of a model, commercial triblock copolymer system [polystyrene-block-poly(ethylene-co-butylene)-block-polystyrene]. Results show that the block copolymer is a poor microwave absorber, resulting in no change in the block copolymer morphology upon application of microwave energy. The block copolymer species may only indirectly interact with the microwave energy when a small molecule microwave-interactive species [diethylene glycol dibenzoate (DEGDB)] is incorporated directly into the polymer matrix. Then significant morphological development is observed at DEGDB loadings [greater-than-or-equal]6 wt%. Through spatial localisation of the microwave-interactive species, we demonstrate targeted annealing of specific regions of a multi-component system, opening routes for the development of "smart" manufacturing methodologies.
Microwave annealing , Block copolymer self-assembly , Block copolymer species
Toolan, Daniel T. W.; Adlington, Kevin; Isakova, Anna; Kalamiotis, Alexis; Mokarian-Tabari, Parvaneh; Dimitrakis, Georgios; Dodds, Christopher; Arnold, Thomas; Terrill, Nick J.; Bras, Wim; Hermida Merino, Daniel; Topham, Paul D.; Irvine, Derek J.; Howse, Jonathan R. (2017) 'Selective molecular annealing: in situ small angle X-ray scattering study of microwave-assisted annealing of block copolymers'. Physical Chemistry Chemical Physics, 19 (31):20412-20419. doi:10.1039/C7CP03578K
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© Royal Society of Chemistry 2017. This document is the Accepted Manuscript version of a Published Work that appeared in final form in Physical Chemistry Chemical Physics, after peer review and technical editing by the publisher. To access the final edited and published work see