An nanoparticles are synthesized in situ upon the electron beam exposure of a poly(vinyl alcohol) (PVA) thin film containing Au(III). The e-beam-irradiated areas are insoluble in water (negative-tone resist), and AU-PVA nanocomposite patterns with a variable profile along the structure can be thus generated (3D lithography) in a single step. A local characterization of the generated patterns is performed by high-resolution transmission electron microscopy and UV-vis localized Surface plasmon resonance microspectroscopy. This characterization confirms the presence of crystalline nanoparticles and aggregates.