A series of well-defined poly(methylmethacrylate) (PMMA)-b-poly(alkylacrylate)-b-PMMA triblock copolymers (MAM) has been synthesized by transalcoholysis of PMMA-b-poly(tert-butylacrylate)-b-PMMA precursors by alkyl alcohols. The molecular weight (MW) of the outer PMMA blocks is in the 10,000-50,000 range, compared to 50,000-200,000 for the inner poly(alkylacrylate) block. Phase separation, as studied in direct space by atomic force microscopy, is observed for all the investigated triblock copolymers, except for the PMMA-b-poly(ethylacrylate)-b-PMMA and the PMMA-b-poly(n-propylacrylate)-b-PMMA triblocks of 10,000-50,000-10,000 MW. The ultimate tensile strength measured for the MAM triblocks is strongly dependent on the MW between chain entanglements for the central block. The tensile behavior is however affected by the partial miscibility of the outer and inner blocks when the PMMA MW is low. When this situation prevails, it makes the melt processing possible at temperatures lower than 200 degreesC. (C) 2001 Elsevier Science Ltd. All rights reserved.