In the present work clay/polystyrene hybrids were prepared by emulsion polymerization, and subsequent coagulation technique. Two different coagulants, magnesium sulfate and aluminum sulfate, were used in order to compare the coagulation efficiency, and the final structure and dispersion-state were analyzed by X-ray diffraction method. Aluminum sulfate-water solution is more effective in coagulation of polystyrene emulsion than magnesium sulfate-water solution. Small peaks near 2 theta = 6 degrees appear in XRD diffraction patterns of all the hybrids. It is confirmed that these small XRD peaks are ascribed with the ordering of silicate layers between which hydrated metal complex polycations are located with layers of water molecules.