The film formation study of latex blends based on fluorinated and fluorine-free acrylates demonstrates the ability of atomic force microscopy (AFM) to distinguish between the two latex components. The film formation and accumulation of the fluorine containing component at the surface upon annealing can be monitored. New developments in sample preparation allow to study the bulk morphology and nanostructure of cryomicrotomed samples by AFM. This technology was applied to investigate poly(propene)/poly(1-olefin) blends as well as filler modified 1,4-BR/SBR blends. In the first case, miscibility and compatibility windows were found for poly(propene)/poly(ethene-co-1-butene) blends depending on the 1-butene content. In the second case it is demonstrated that systematic AFM measurements can provide information about the local distribution of the filler particles as well as about the morphology of the immiscible rubber components.