Morphology, thermal and rheological properties of polymer-organoclay composites prepared by melt-blending of polystyrene (PS), poly(methyl methacrylate) (PMMA), and PS/PMMA blends with Cloisite(R) organoclays were examined by transmission electron microscopy, small-angle X-ray scattering, secondary ion mass spectroscopy, differential scanning calorimetry, and rheological techniques. Organoclay particles were finely dispersed and predominantly delaminated in PMMA-clay composites, whereas organoclays formed micrometer-sized aggregates in PS-clay composites. In PS/PMMA blends, the majority of clay particles was concentrated in the PMMA phase and in the interfacial region between PS and PMMA. Although incompatible PS/PMMA blends remained phase-separated after being melt-blended with organoclays, the addition of organoclays resulted in a drastic reduction in the average microdomain sizes (from 1-1.5 mum to ca. 300-500 nm), indicating that organoclays partially compatibilized the immiscible PS/PMMA blends. The effect of surfactant (di-methyl di-octadecyl-ammonia chloride), used in the preparation of organoclays, on the PS/PMMA miscibility was also investigated. The free surfactant was more compatible with PMMA than with PS; the surfactant was concentrated in PMMA and in the interfacial region of the blends. The microdomain size reduction resulting from the addition of organoclays was definitely more significant than that caused by adding the same amount of free surfactant without clay. The effect of organoclays on the rheological properties was insignificant in all tested systems, suggesting weak interactions between the clay particles and the polymer matrix. In the PS system, PMMA, and organoclay the extent of clay exfoliation and the resultant properties are controlled by the compatibility between the polymer matrix and the surfactant rather than by interactions between the polymer and the clay surface.