A kind of hybrid multilayer film based on mercaptobenzoic acid-capped Au nanoparticles (MBA-Au-NPs)and photoreactive nitrodiazoresin (NDR) has been fabricated via electrostatic self-assembly. Upon exposureto UV light, the initial ionic bonds between the layers of the film convert into covalent bonds and the filmstability toward polar solvents, salt, or surfactant solutions increases significantly. The micropatternedNDR/MBA-Au-NP film with the covalently linked architecture was formed by selecting exposure of thefilm through a photomask and later developed in sodium dodecyl sulfate (SDS) aqueous solution. Themetallic Au-NP micropatterns, furthermore, are produced by sintering the micropatterned NDR/MBA-Au-NP film at 550
C, at which the organic components are removed completely. The well-definedmicropatterns were characterized with atomic force microscopy (AFM), field emission scanning electronmicroscopy (FE-SEM), microscope with a charge-coupled device (CCD) camera, and X-ray photoelectronspectroscopy (XPS).