In this study, poly(azomethine-ester) s (PAEs) were synthesized via elimination reactions of aromatic dihydroxy compounds containing imine bonding with terephthaloyl chloride. The structures of PAEs containing different aliphatic chains and ether bridges were confirmed by FT-IR, H-1, C-13-NMR and UV-Vis measurements. Electrochemical parameters of the synthesized SBs and PAEs were determined by cyclic voltammetry measurements. Thermal properties of the synthesized monomers and polymers were investigated by TG-DTA, DMA and DSC techniques. Molecular mass distributions of PAEs are determined with gel permeation chromatography measurements. Morphological and topographic properties of the SBs and PAEs containing azomethine linkage in the main chain were investigated by SEM and AFM techniques, respectively. Maximum particle sizes on surfaces of polymers were calculated with AFM analyses. Surface modifications of poly(azomethine-ester) s and maximum particle size on their surface were studied with topographic and 3D AFM images and particular size curves.