In this study, the new sulfone group-containing poly(azomethine-urethane)s (PAZUs) were synthesized to investigate the effects various diisocyanates on the thermal, fluorescence, electrochemical and morphological properties. The structures of PAZUs have been confirmed by FT-IR, NMR, and SEC analyses. The electrochemical behaviors of the PAZUs were examined by cyclic voltammetry. Optical properties were investigated by UV-Vis and fluorescence measurements. The PAZUs were further characterized by TGA, DSC, SEM, and AFM techniques. TGA analyses results showed considerable increase in the thermal stability of polyurethanes due to the introduction of azomethine bond in the main chain. Consequently, because of the fine thermal properties the obtained materials can be used to produce thermally stable materials.