Abstract: Gradient copolymers, of which the chemical compositions change along chain backbones, can be synthesized only via living polymerization processes. As a novel type of copolymers, synthesis of gradient copolymers and eva luation of their materials properties have received increasing interest recently. Gradient copolymers are potential to be used as damping materials, compatibilizer, etc. Both theoretical and experimental investigations suggested that the composition profiles along chains be an important microstructural parameter for fine-tuning nano-morphologies, and thus physical and functional properties of polymer materials. We used four kinds of methacrylic acid(MAA)/methyl methacrylate(MMA) gradient copolymers, involving uniform MAA/MMA copolymer(Poly(MAA-uni-MMA)), linear MAA/MMA copolymer(Poly(MAA-li-MMA)), triblock MAA/MMA copolymer with a linear gradient mid-block(Poly(MAA-tri-MMA)) and diblock MAA/MMA copolymer (Poly(MAA-di-MMA)), to systematically investigate the influence of composition profiles on their chemical and physical properties in solution, in bulk and in form of film.