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Selective Molecular Annealing: In Situ Small Angle X-ray Scattering Study of Microwave-Assisted Annealing of Block Copolymers

DOI: 10.1039/C7CP03578K DOI Help

Authors: Daniel T. W. Toolan (University of Sheffield) , Kevin Adlington (University of Nottingham) , Anna Isakova (Aston University) , Alexis Kalamiotis (University of Nottingham) , Parvaneh Mokarian-tabari (University College Cork) , Georgios Dimitrakis (University of Nottingham) , Christopher Dodds (University of Nottingham) , Thomas Arnold (Diamond Light Source) , Nick J. Terrill (Diamond Light Source) , Wim Bras (ESRF - The European Synchrotron) , Daniel Hermida Merino (ESRF - The European Synchrotron) , Paul D. Topham (Aston University) , Derek J. Irvine (University of Nottingham) , Jonathan R. Howse (University of Sheffield)
Co-authored by industrial partner: No

Type: Journal Paper
Journal: Phys. Chem. Chem. Phys.

State: Published (Approved)
Published: July 2017
Diamond Proposal Number(s): 10439 , 13002

Abstract: 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 ≥ 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.

Journal Keywords: microwaves; polymers; nanoscale self-assembly; in situ small angle x-ray scattering; diblock copolymer

Subject Areas: Chemistry, Physics


Instruments: I07-Surface & interface diffraction , I22-Small angle scattering & Diffraction

Other Facilities: European Synchrotron Radiation Facility