Nitroxide-mediated radical polymerization (NMP) combined with the semibatch process was used to synthesize poly(N, N-dimethylacrylamide-grad-butylacrylate), called poly(DMA-grad-BuA), in the presence of SG1 as a control agent and the alkoxyamine (MAMA) as an initiator. The pseudo-instantaneous composition was used to characterize the gradient copolymers. The variation of the addition rate of DMA influences the incorporation of DMA in the macromolecular chains. The preliminary surface characterization by the measure of the static water contact angle of the gradient copolymers films indicated that the monomer unit sequence in the polymer chain strongly influences the surface properties. The rheological properties of gradient copolymers in bulk were also studied and discussed in relation to their local structure.