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We demonstrate the fabrication by anodization of niobium oxide microcones, several microns long, from aqueous solutions of 1 wt% hydrogen fluoride (HF) with varied sodium fluoride (NaF) concentration (0–1 M). Raman spectroscopy and x-ray diffractometer analysis revealed the as-grown microcones to be crystalline Nb_2O_(5−x) with preferred (1 0 0) and (0 1 0) orientations. The overall Nb_2O_(5−x) formation rate increased with the increasing NaF concentration, and structures as tall as 20 μm were achieved in just 20 min of anodization at 1 M NaF. Rapid formation of niobia microcones was even observed in the absence of HF at this NaF concentration. Photocatalytic activity for water oxidation was highest for microcones grown under the highest NaF concentration.

Rapid and controlled electrochemical synthesis of crystalline niobium oxide microcones