Polymeric thin films which had a high-ordered structure were fabricated from adipic acid (ADA), 4,4'-diaminodiphenylmethane dihydrochloride (DAM), and N-hydroxysuccinimide (NHS) and 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (EDC) as condensing agents by a self-assembly method. UV-Vis and quartz crystal microbalance (QCM) measurements were used to monitor the layer-by-layer deposition process. FTIR reflection absorption spectroscopy (FTIR-RAS) was also carried out in order to confirm the polymerization of monomers. The surface morphology of the films was investigated with an atomic force microscope (AFM). These results indicated that ADA and DAM were alternately deposited and polymerized with condensing agents on nanoscale.