In the present work, we report a simple experimental strategy for the one-step electrochemical synthesis of nanogranular Cu 2 O films by copper anodization in fluoride-containing ethylene glycol media. Microscopic exploration using field emission scanning electron microscopy (FESEM), atomic force microscopy (AFM) and transmission electron microscopy (TEM), shows the formation of spherical shape grains with sizes ranging from 20 to 40 nm. Raman and X-Ray Photoemission Spectroscopy (XPS) results indicate that only Cu I oxide is obtained. A band gap energy E g = 2.01 eV is estimated from UV-vis reflectance spectroscopy indicating that an indirect transition mechanism between semiconductor bands takes place. These evidences indicate that the present synthesis of nanogranular Cu 2 O films is a promising method for obtaining improved properties of materials for the design of photoelectronic devices.One of the most interesting purposes in the current nanoscience and nanotechnology research is the optimization of synthesis strategies for tuning the properties of materials at nanoscale dimensions for specific applications. Consequently, a wide variety of metallic, semiconductor and polymeric nanostructures with different size and shape-dependent properties have been obtained.Among semiconductor materials, Cu 2 O has been one of the most studied for applications in photovoltaic cells and electrocatalysis as well as for its microbial activity due to the non-toxic nature, availability, low-cost and narrow band gap (E g � 1.9 eV -2.2 eV). [1][2][3][4][5][6] In the last years, several reports on the synthesis and characterization of different Cu 2 O nanostructures using solgel and hydrothermal routes, template assisted growth, electrochemical deposition and anodization, have been published. [3][4][5][6][7][8][9][10][11][12][13][14] Particularly, Allam et al [13] reported the synthesis of various Cu 2 O nanostructured thin films by anodization of Cu foils in aqueous or ethylene glycol media containing hydroxide, chloride and/or fluoride ions. In aqueous alkaline electrolytes, no stable anodic films on the surface were obtained. Electrodeposited Cu 2 O crystallites or dendritic structures were obtained in the presence of chloride ions while in the presence of fluoride ions, uniform nanoporous structures or porous spheroids were achieved. The as-anodized porous nanoarchitectures were composed of a mixture of copper hydroxide and copper oxide phases. On the other hand, for anodization of Cu in ethylene glycol-based electrolytes containing fluoride, leaf-like nanostructures were obtained but no structural film formation was found for the conditions employed. Despite of the variety of nanostructures reported (crystallites, dendritic structures, porous spheroids and leaf-like nanostructures) the synthesis in ethylene glycol media has not been extensively explored. More recently, [14] we have reported that the anodization of copper in alkaline water/ethylene glycol media containing fluoride ions generates nanostructured copper oxide f...