Abstract

Niobium oxynitride (NbON) is a promising photoanode material for photoelectrochemical water splitting using visible light up to ∼600 nm in wavelength. However, the NH3 nitridation method widely used for oxynitride synthesis cannot convert Nb2O5 (Nb5+) to crystalline NbON (Nb5+), due to the generation of NbOxNy (Nb2+−3+). To prevent Nb reduction during nitridation, we added O2 as an oxidant to the NH3 nitridation reaction system. Investigation of the relationship between O2 concentration and the crystal phase of the resulting samples revealed that Nb2O5 nitridation produces crystalline NbON (Nb5+) within a specific O2 concentration range. The O2 concentration required to synthesize NbON increases from 0.05% to over 0.40% upon increasing the nitridation temperature from 600 °C to 750 °C. The photoelectrochemical properties of NbON films were also investigated. Under simulated sunlight illumination, a NbON photoanode produced a photocurrent of 0.6 mA cm-2 at 1.2 V vs. RHE in H2O2 aqueous solution.

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