AbstractTo have an improved insight about the compatibilization effect of organoclay on immiscible polymers, two different organoclays and preparation techniques were chosen to prepare polyamide6 (PA6)/polystyrene (PS)/organoclay ternary nanocomposites. The morphology analysis based on the results of X‐ray diffraction, transmission electron microscopy, and scanning electron microscopy demonstrated that the type of organoclay and preparation technique had a significant influence on the dispersion and distribution of organoclay in the polymer. It was concluded that blending PS/organoclay nanocomposite synthesized previously via in situ bulk polymerization, with PA6 can realize the full exfoliation of organoclay in the final ternarynanocomposite, while an intercalated structure was achieved by directly blending the three components. The distribution of organoclay could be controlled by tuning the surface property of clay, and hence the interfacial interaction between clay and the polymer matrix. © 2008 Wiley Periodicals, Inc. J Appl Polym Sci, 2008