Single-crystalline bismuth titanates (Bi12TiO20) with the cubic phase and various morphologies (flower-, belt-, tetrahedral-like) were controllably fabricated by using a mild template-free hydrothermal process. The samples were fully characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), high-resolution TEM, nitrogen porosimetry measurement, UV-vis diffuse reflectance spectroscopy (DRS), and X-ray photoelectron spectroscopy (XPS). The influence of the solvent and the concentration of NO3− in the reaction system on the crystallinity and morphology of the Bi12TiO20 samples was investigated in detail. Bi12TiO20 crystals were used as the sunlight-driven photocatalysts to degrade aqueous dye methyl orange (MO) and p-nitrophenol (PNP), and the influence of Bi12TiO20 morphology on the photocatalytic activity was discussed. Finally, the recyclability of Bi12TiO20 was evaluated through three consecutive runs.
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