We combine scanning force microscopy experiments with ex-situ swelling in d
ifferent solvent vapors to investigate the microdomain structure of a thin
ABC triblock copolymer film (poly(styrene-b-2-vinylpyridine-b-tert-butyl me
thacrylate)). We demonstrate that short treatment in a selective vapor and
subsequent drying lead to characteristic changes in the surface morphology.
The use of different solvents then allows to unambiguously identify the di
fferent phases present at the surface. This approach is established studyin
g polymer blend and diblock copolymer copolymer thin films of known known m
orphology. It is then applied to the a priori unknown morphology of the BBC
triblock copolymer thin film. The results indicate a laterally microphase-
separated polymer surface in agreement with recent theoretical consideratio
ns, The conclusions are corroborated by XPS measurements monitoring the ave
rage surface composition of the copolymer films.