LIVING CONTROLLED RADICAL polymerization HAS BEEN A POWERFUL TECHNIQUE TOSYNTHESIZE WELL-DEFINED STRUCTURE POLYMER BY CONTROLLING MOLECULAR WEIGHT, MOLECULAR WEIGHT DISTRIBUTION AND TAILORED ARCHITECTURE. THREE ‘‘LIVING’’ RADICALpolymerization TECHNIQUES WHICH ARE RECEIVING MORE AND MORE ATTENTION INACADEMIA ARE NITROXIDE-MEDIATED RADICAL polymerization (NMP) [1], ATOM TRANSFERRADICAL polymerization (ATRP) [2], AND REVERSIBLE ADDITION–FRAGMENTATION CHAINTRANSFER (RAFT) polymerization [3]. RAFT polymerization WAS CONSIDERED AS ONE OFTHE MOST PROMISING CONTROLLED FREE RADICAL polymerization DUE TO ITS COMPATIBILITYWITH A WIDE RANGE OF MONOMERS AND ITS VERSATILITY.IN THE PRESENT WORK, A NOVEL NANOCOMPOSITE WAS PREPARED BASED ON POLY (METHYL METHACRYLATE) /SIO2 USING 4-CYANO-4- [(PHENYLCARBOTHIOYL) SULFANYL] PENTANOIC ACID AS A RAFT AGENT (FIGURE 1).THE STRUCTURE, MORPHOLOGY AND THERMAL PROPERTIES OF THE NANOCOMPOSITES WERE CHARACTERIZED USING FOURIER TRANSFORM INFRARED (FT-IR), HNMR, TRANSMISSION ELECTRON MICROSCOPY (TEM), THERMOGRAVIMETRIC ANALYSIS (TGA), AND DIFFERENTIAL SCANNING CALORIMETRY (DSC), RESPECTIVELY. THE XRD RESULTS ALSO SHOWED THE PROPER INTERCALATION OF POLYMER CHAINS BETWEEN THE SILICATE LAYERS.