Using sequential living anionic polymerization we synthesized well-defined linear ABC triblock terpolymers from polystyrene (PS), poly(2-vinylpyridine) (P2VP), and poly(tert-butyl methacrylate) (PtBMA). The length of the PtBMA block was systematically increased at constant block length ratios of the PS and P2VP blocks. The microdomain structures were characterized by transmission electron microscopy (TEM) and small angle X-ray scattering (SAXS). With increasing PtBMA block size we observe a systematic change in the bulk structure of the block copolymers. (C) 2003 Elsevier Ltd. All rights reserved.