The interlayer structure of organoclay is one of the key factors, together with the shear rate during processing and the matrix polarity, which act on the possibility of polymer nanocomposite formation and, as a consequence, on the morphology and properties of the polymerclay hybrids. Three organoclays with different interlayer structures (population and packing density) were used in this work to prepare composites with PET and to study the morphology of the resulting hybrids (using x-ray diffraction (XRD) and transmission electron microscopy (TEM)). The organoclay with the most populous interlayer structure (CN) did not show any traces of nanocomposite formation; the organoclay with the less populous interlayer structure (VG) showed some evidences of layer exfoliation, such as lower intensity of x-ray diffraction peak. Finally, the organoclay with the less populous and packed interlayer structure (IT) showed no diffraction peak and layers very separated from their original cristallites, features characteristic of exfoliated polymer nanocomposites.