The multilayer films from diazoresin (DR) and poly(sodium acrylate, PANa) or alkali hydrolytic maleic anhydride/styrene copolymer (PMSNa) were fabricated on mica. During the fabrication process the absorbance increases about 0\^033 for every fabrication cycle, indicating that the thickness of the film increases regularly. Under irradiation of UV light or heating, following the -N\-2\++ decomposition, the inoic bond of the film converts to covalent bond. The morphologies of the film after DMF etching for the different films (irradiatied or unirradiated etc) were observed by Atomic Force Microscopy (AFM) and the result shows that the ability of the film against etching from polar solvent increases obviously. The conversion of bond nature from ionic to covalent was verified preliminarily by FTIR spectral analysis.
