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Poly(methyl methacrylate) (PMMA)/sodium montmorillonite (Na-MMT) nanocomposites were prepared with a novel method utilizing a macroazoinitiator (MAI). To induce the intergallery polymerization of methyl metha-crylate (MMA), the MAI containing a poly(ethylene glycol) (PEG) segment was intercalated between the lamel lae of Na-MMT and swelled with water to enhance the diffusion of MMA into the gallery. The structure of the nano composite was examined using X-ray diffraction and transmission electron microscopy, and the thermal properties were examined using differential scanning calorimetry and thermogravimetry. The PMMA/Na-MMT nanocomposite prepared by intergallery polymerization showed a distinct enhancement of its thermal properties; an approximately 30oC increase in its glass transition temperature and an 80~100oC increase in its thermal decomposition temperature for a 10% weight loss.