The surface enrichment in thin bilayer films of poly(vinyl chloride) (
PVC) and deuterated poly(methyl methacrylate) (PMMAd) was studied by n
eutron reflectometry. X-ray photoelectron spectroscopy (XPS) and stati
c secondary ion mass spectrometry (SSIMS). In a layer system, where th
e PVC film is placed on top of a thin PMMA film. the PMMA chains migra
te to the surface, although annealing of the films is performed below
the glass transition temperature of PMMA. In addition, the surface seg
regation in blends of these materials was studied by XPS and SSIMS. In
all cases PMMA is enriched at the surface. Results from the different
techniques, probing different sample depths, are consistent, if an ex
ponential concentration profile of PMMAd at the surface is assumed. Co
ncentration profiles at the surface are discussed with respect to theo
retical models and diffusion coefficients are estimated.