The inclusion of the organic guest aniline into Cu(II)-exchanged hectorite thin films has been investigated. The subsequent polymerization of aniline on the clay surface and in the intergallery regions are studied using scanning force microscopy (SFM), electron paramagnetic resonance (EPR) spectroscopy, powder x-ray diffraction (XRD), and impedance spectroscopy;EPR and XRD data show that in addition to strong polymerization of aniline on the clay surface, polymerization also occurs in the intergallery regions of the clay. Using standard lift-off techniques or razor cleaving, the exposed intergallery polyaniline is successfully imaged for the first time using noncontract SFM in phase-contrast mode. The nearly two-dimensional polymer sheets formed in these regions exhibit none of the nanometer-scale grain of bundle structure commonly associated with polyaniline synthesized using techniques such as electrochemical or vacuum deposition. The electrical response of the resulting clay-conducting polymer composites is also investigated for thin films fabricated on 15 mu m interdigitated arrays. Preliminary results indicate that these composite materials may be highly suitable as chemical sensors for a variety of important gases and vapors such as ethanol and hexane.