Hydrothermal synthesis of bismuth niobates and their application in azo-dyes photo-discoloration

Highlights: • A new method of synthesis for obtaining pure phase bismuth niobates is proposed. • α-BiNbO₄ and β-BiNbO₄ were obtained by the calcination of an amorphous precursor. • Nanosized bismuth niobates have shown high band gap energies (3.2–3.4 eV). • Bismuth niobates are very efficient in the photo-discoloration of methyl orange. - Abstract: Bismuth niobates were obtained by hydrothermal synthesis using bismuth (III) nitrate pentahydrate [Bi(NO₃)₃·5H₂O] and a Lindqvist potassium hexaniobate [K_8-xH_xNb₆O₁₉.nH₂O] as soluble precursors. Pure crystalline Bi₅Nb₃O₁₅, β-BiNbO₄ and α- BiNbO₄ were obtained as pure phases through co-precipitation at pH = 8, followed by hydrothermal treatment and calcination at 600, 700 or 800 °C, respectively, which are milder temperatures than those used in solid state, citrate sol-gel and ball milling methods. Band gap energies of α-BiNbO₄ and β-BiNbO₄ were estimated by UV–vis diffuse reflectance spectroscopy (DRS) as 3.2–3.4 eV, which are higher than experimental values reported in the literature. The materials were evaluated in the methyl orange azo-dye photo-discoloration under UV irradiation and complete bleach was attained. The triclinic phase presented a better efficiency as a photocatalyst than the orthorhombic phase. Unexpectedly, the mixture of both phases resulted in the highest photocatalytic efficiency, similar to that found for Degussa P25 commercial catalyst.