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The phase behavior of gels of E40B10 in 0.2 mol dm-3 aqueous K2SO4 was studied as a function of temperature and concentration. E40B10 is a diblock copolymer of poly(oxyethylene) (E) and poly(oxybutylene) (B), where the subscripts denote the number of repeats. The phase of the material was characterized by both simultaneous rheology and small-angle X-ray scattering, (SAXS). Depending on polymer volume fraction in the range 23−38% a body-centered cubic (bcc) structure or a face-centered cubic (fcc) structure was observed at low temperature, and at high temperature a hexagonally packed rod structure was formed. The phase transitions were shown to be characterized by discontinuous changes in the values of the dynamic shear moduli. A bcc−fcc transition was observed at high concentration, the corresponding transition temperature increasing with increasing polymer concentration. The effects of reciprocating shear were shown to increase the degree of order, manifested as a sharpening of the diffraction peaks in the SAXS pattern. The dynamic moduli decreased rapidly on the application of oscillatory shear and recovered equally rapidly when the deformation ceased. The decrease in moduli was shown, via the SAXS patterns acquired simultaneously, to be correlated to structural changes within the gel.

The simultaneous time-resolved study of structure development and reaction kinetics during polymer processing is an experimental method that has great potential in developing a deeper understanding of the parameters that govern the formation of structure and therefore polymer properties. A combination of synchrotron radiation small-angle x-ray scattering and Fourier-transform infrared spectroscopy experiments have been performed on a series of model segmented block copolyurethanes. These studies confirm that the driving force for structure development in polyurethanes is the thermodynamics of phase separation rather than hydrogen bonding.

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