Crystalline/amorphous binary mixtures of polystyrene with different tacticities, syndiotactic/atactic isomers (sPS/aPS), have been systematically studied to reveal the composition dependence of the blend morphologies, i.e., sPS lamellar structure and aPS diluent segregation, developed after isothermal crystallization. To reveal the molecular weight effect of the aPS diluents, four different $\overline M _{\rm w}$ of aPS were used to prepare blends with various compositions. After being melt crystallized isothermally at 250 °C, all blends were investigated by means of POM, WAXS, and SAXS as well as SEM and TEM to reveal the spherulitic and lamellar morphologies developed.magnified image