A series of A2B2 four‐arm, miktoarm stars of polystyrene and polyisoprene have been synthesized. The morphological behavior of these materials has been characterized using TEM, SAXS, and SANS, and was found to agree in general with the predictions of Milner's theory for miktoarm star morphological behavior. One sample was found to exhibit a cylindrical morphology where lamellae were predicted; this behavior is similar to other discrepancies observed in previous studies of miktoarm star morphological behavior. A second sample, predicted to form a bicontinuous morphology, was found to exhibit hexagonally packed cylinders. The tetrafunctional junction point also results in an increase in spacing for the lamellar sample in this series over that of an AB diblock, but not as great as the increase previously observed for A8B8 16‐arm star materials. © 1999 John Wiley & Sons, Inc. J Polym Sci B: Polym Phys 37: 3392–3400, 1999