The block microstructure of a series of diblock copolymer ionomers was investigated using synchrotron small-angle x-ray scattering (SAXS). The base materials used were poly[styrene-b-(ethylene/propylene)] (SEP) diblock copolymers with a constant total molecular weight of ca. 50 kg/mol, but three different compositions : 20.3 wt%, 35.6 wt% and 50.4 wt% polystyrene (PS). The polystyrene microphase structures for these unmodified diblock copolymers were cylindrical, lamellar and lamellar, respectively. Ionomers were synthesized from the block copolymers by lightly sulfonating the PS blocks, followed by neutralization to the sodium and zinc salts. The introduction of ionic species into the PS blocks perturbed the block morphology. The inhibition of the formation of an ordered block microphase was found to increase with increasing strength of ionic interactions for the different cations