AFM, LVHRSEM, and cross-sectional TEM of the near-surface morphology of diblock copolymers
Application of block copolymers as adhesives and biomedical devices requires an understanding of the surface composition and morphology of these materials. Microscopy techniques offer excellent depth and lateral resolution and therefore can provide direct microstructural and compositional surface data. Previous workers frequently used only a single microscopy technique to investigate the influence of an external surface constraint on the morphology. The implementation of several different microscopy techniques, each with its own strengths, affords a very complete characterization of the surface composition and morphology of self-assembling diblock copolymers.The investigation of solvent-cast and annealed thick (1 mm) films of two poly(styrene-b-butadiene) (SB) diblock copolymers, which usually self-assemble to form alternating poly(styrene) (PS) and poly (butadiene) (PB) lamellar microdomains, by three complementary microscopy techniques: cross-sectional transmission electron microscopy (CSTEM), low-voltage high-resolution scanning electron microscopy (LVHRSEM), and atomic force microscopy (AFM) is discussed. For CSTEM and LVHRSEM imaging, contrast between the PS and PB phases was enhanced by preferential staining of the PB phase with the vapors of a 4% aqueous osmium-tetroxide (OsO4) solution for 24 hours.