A diblock copolymer consisting of a polystyrene segment with M(n) = 18700 and a poly (methylphenylsilylene) segment with M(n) = 9000 was found to microphase separate when a film was cast from THF. The microphase segregation was studied using both transmission electron microscopy and scanning force microscopy. The bulk morphology consisted of cylinders of poly(methylphenylsilylene) in a polystyrene matrix. The deposition of block copolymer micelles assembled in 1,4-dioxane solution was observed by scanning force microscopy when a dilute solution in this selective solvent was cast on mica and quickly evaporated. Besides the micelles, a thin polymer film was formed by adsorption of molecularly dissolved chains.