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This work reports a simple, direct, and easy route to prepare thin films between graphene-like materials and two hexacyanometallates, based on metal cation modification in graphene oxide (GO) thin films obtained by the liquid/liquid interfacial route. The reaction between GO and Cu 2 + or Fe 3 + ions in aqueous solution yields GO/Cu 2 + or GO/Fe 3 + , and the nature of the interactions between the GO and the metal cations were demonstrated by FT-IR. GO/Cu 2 + and GO/Fe 3 + can be chemically reduced to reduced graphene oxide/metal nanoparticles (rGO/ Cu or rGO/Fe) thin films. Both GO/metal cation or rGO/metal nanoparticles thin films were used as working electrodes for electrodeposition of their respective hexacyanometallates (Prussian blue, PB, and its copper analogue, Cu-PBA) based on a heterogeneous reaction between ferricyanide ions in the electrolyte solution and the metallic species in the electrode. The PB and Cu-PBA formation in all electrodes was confirmed by Raman spectroscopy, X-ray diffraction, cyclic voltammetry, and scanning electron microscopy, characterized as welldefined nanometric cubes homogeneously dispersed over the rGO sheets.

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