A cathodic electrosynthesis strategy was conceived and demonstrated for the preparation of Nb_2 O_5 nanorodsanotubes supported on Nb foil. This method involved an interplay of several processes including the chemical attack of fluoride species on the Nb cathode, the electrogeneration of O_2 at a proximal Pt anode, its subsequent diffusion to and electrocatalytic reduction on the Nb cathode, and finally, the chemical reaction between the ionic Nb and oxygen precursor species at the interface to generate the Nb_2 O_5 nanoarchitectures. The oxide nanorodsanotubes were characterized by scanning electron microscopy, X-ray photoelectron spectroscopy, energy dispersive X-ray analyses, and Raman spectroscopy, and their critical dimensions could be tailored via control of the growth variables.
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