Monophasic and hybrid nanostructures of KNbO 3 and α-Fe 2 O 3 have been prepared using a hydrothermal process for photoelectrocatalytic and photocatalytic applications. Powder X-ray diffraction studies showed the formation of KNbO 3 , α-Fe 2 O 3 , and KNbO 3 /α-Fe 2 O 3 with average grain sizes of 18.3, 11.5, and 26.1 nm and Brunauer–Emmett–Teller (BET) specific surface areas of 4, 100, and 20 m 2 /gm, respectively. Under simulated solar irradiation, the as-prepared heterostructure shows enhanced photoelectrocatalytic oxygen evolution reaction (OER) activity compared to pristine KNbO 3 and α-Fe 2 O 3 . Significant photocatalytic activity of as-synthesized KNbO 3 /α-Fe 2 O 3 heterostructure photocatalyst was obtained for removal of methylene blue organic dye under visible light, and the percentage activity was found to be 11, 49, and 89% for KNbO 3 , α-Fe 2 O 3 , and KNbO 3 /α-Fe 2 O 3 photocatalysts, respectively. The dielectric constant was found to be 250.2, 65.2, and 251.5 for KNbO 3 , α-Fe 2 O 3 , and KNbO 3 /α-Fe 2 O 3 heterostructure, respectively, at 50 °C and 500 kHz frequency.

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