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In situ SAXS studies of a prototypical RAFT aqueous dispersion polymerization formulation: monitoring the evolution in copolymer morphology during polymerization-induced self-assembly

DOI: 10.1039/D0SC03411H DOI Help

Authors: Adam Czajka (University of Sheffield) , Steven P. Armes (University of Sheffield)
Co-authored by industrial partner: No

Type: Journal Paper
Journal: Chemical Science , VOL 6

State: Published (Approved)
Published: September 2020
Diamond Proposal Number(s): 21776

Open Access Open Access

Abstract: Small-angle X-ray scattering (SAXS) is used to characterize the in situ formation of diblock copolymer spheres, worms and vesicles during reversible addition–fragmentation chain transfer (RAFT) aqueous dispersion polymerization of 2-hydroxypropyl methacrylate at 70 °C using a poly(glycerol monomethacrylate) steric stabilizer. 1H NMR spectroscopy indicates more than 99% HPMA conversion within 80 min, while transmission electron microscopy and dynamic light scattering studies are consistent with the final morphology being pure vesicles. Analysis of time-resolved SAXS patterns for this prototypical polymerization-induced self-assembly (PISA) formulation enables the evolution in copolymer morphology, particle diameter, mean aggregation number, solvent volume fraction, surface density of copolymer chains and their mean inter-chain separation distance at the nanoparticle surface to be monitored. Furthermore, the change in vesicle diameter and membrane thickness during the final stages of polymerization supports an ‘inward growth’ mechanism.

Subject Areas: Chemistry

Instruments: I22-Small angle scattering & Diffraction


Discipline Tags:

Organic Chemistry Material Sciences Polymer Science Chemistry

Technical Tags:

Scattering Small Angle X-ray Scattering (SAXS)