Block copolymers poly(methy1 methacrylate)-block-polystyrene-block-poly(methyl methacrylate) and polystyrene-block-poly(tert-butyl methacrylate) were prepared by anionic polymerization and were studied in dilute solution as well as in the bulk state. The viscometric study revealed that the block copolymers exhibit a conformational "transition" occurring in a narrow temperature range. Films were obtained with the same copolymers by casting at different temperatures, chosen below and above the "transition". From the investigation of these f i i s by differential scanning calorimetry, using the entropy relaxation method, and by dynamic mechanical measurements, it was shown that the block copolymers exhibit a rather segregated structure if they are obtained below the "transition" temperature, and that they adopt a quasi-Gaussian conformation (implying a better miscibility of the two kinds of blocks) if the solvent is evaporated above the "transition" temperature.