In this study, polystyrene (PS)/montmorillonite nanocomposites were prepared by melt intercalation, in situ polymerization, and masterbatch methods. In the masterbatch method, as the first step, a high clay content composite of PS–organoclay (masterbatch) was prepared by in situ polymerization, and then the prepared masterbatch was diluted to desired compositions with commercial PS in a twin-screw extruder. The structure and mechanical properties of the nanocomposites were examined. X-ray diffraction (XRD) analysis showed that the d-spacing of the in situ formed nanocomposites increased from 32.9 Å for the organoclay powder to 36.3 and 36.8 Å respectively in nanocomposites containing 0.73 and 1.6 wt% organoclay, indicating intercalation. However, the d-spacing of the other prepared materials remained nearly unchanged when compared with pure organoclay powder. Thus, at these low clay contents, in situ formed nanocomposites showed the best improvement in mechanical properties including tensile, impact strength, and Young's modulus. In situ polymerization method did not prove to be efficient at high clay loadings in terms of intercalation and mechanical properties. At high clay loadings, the effects of the three methods in promoting mechanical properties were not significantly different from each other. POLYM. COMPOS., 27:249–255, 2006. © 2006 Society of Plastics Engineers