Two methodologies to build new nanostructured hybrid layered nanocomposites are presented. The first one involves the preparation of hybrid metal/polymer nanolayers (NLs) by combining two monolayer preparation techniques: Horizontal Precipitation Langmuir Blodgett method (HP-ML), for copolymer monolayers and sputter deposition technique, for Au NLs deposition. The second methodology is aimed to prepare regular arrays of nanopores, with diameter ranging between 40-100 nm, in ultra-thin films of electroactive polymers, to obtain embedded regular arrays of nanopores filled by a further electroactive organic component. The produced hybrid MLs have been characterized by means of X-ray Photoelectron Spectroscopy (XPS), Atomic Force Microscopy (AFM) and Grazing Incidence X-ray Diffraction (GI-XRD). In the first case, current-voltage (I-V) measurements demonstrate that the multilayers exhibit a bipolar conduction behaviour (electrons and holes carriers), with a peculiar transition in the nature of the majority carriers (from holes to electrons) above a threshold number of bilayers. In the second case, it is found that the degree of pore filling, as well as the polymer crystallinity can be easily modulated, prompting the tuning of the photoresponse of the nanocomposites
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