Cryo-TEM and SANS microstructural study of pluronic polymer solutions

Cryogenic temperature transmission electron microscopy (cryo-TEM) and small-angle neutron scattering (SANS) were combined to give complete microstructural characterization of aqueous solutions of Pluronic F127, an (EO)(99)(PO)(65)(EO)(99) triblock copolymer. The images of vitrified specimens observed by cryo-TEM provided direct information about the building blocks of these systems, i.e., spheroidal micelles. This confirmed the structural model obtained from analysis of SANS data, which, in addition, provide quantitative information about the system. Occasionally spheroidal micelles were pressed closer to each other during specimen preparation, thus giving rise locally to higher concentration. The cubic phase that was thus formed was directly imaged. The existence of this lyotropic liquid crystalline phase was confirmed by SANS of an originally higher concentration solution. When exposed to shear, the polycrystalline phase transforms into a monodomain crystal with cubic symmetry. The system was also used to demonstrate the potential of selective electron beam radiolysis to enhance contrast in radiation-sensitive, inherently low-contrast systems.