A controlled nanoscale fabrication of conducting polymer films sets severe requirements for the preparation method and substrate. A new and versatile approach for producing thin polypyrrole films on a variety of surfaces is presented. Purely inorganic thin films are first prepared from poly(metaphosphate) and tetravalent metal ions using a sequential layer‐by‐layer technique. Redox‐active cerium(IV) polyphosphate multilayer and redox‐inactive zirconium(IV) and hafnium(IV) polyphosphate multilayers are prepared. Cerium‐based polyphosphate films grow exponentially with the number of layers but multilayers containing zirconium or hafnium exhibit a linear buildup process. All the studied systems produce relatively smooth films with initial bilayer thickness less than 2 nm. The cerium(IV) containing film is redox‐active, which is shown by its capability to form a polypyrrole layer on its surface by oxidation of pyrrole monomers in the adjacent aqueous solution. This is a general method to produce thin oxidative films of arbitrary size and form on a wide variety of surfaces.

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