Microemulsion synthesis of ms/tz-BiVO₄ composites: The effect of pH on crystal structure and photocatalytic performance

In this work, BiVO₄ composites, containing the tetragonal zircon phase (tz-BiVO₄), and monoclinic scheelite phase (ms-BiVO₄), were synthesized using the microemulsion method. The effect of pH on phase composition and photocatalytic activity were investigated. Based on X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM), a ms/tz-BiVO₄ composite forms at pH = 1.0 and pure ms-BiVO₄ is obtained in the pH range 4.0–10.0. The three primary steps in preparing BiVO₄ were monitored by optical microscopy and the role played by the microemulsion on the phase composition of BiVO₄ is explained. Photoluminescence spectroscopy (PL), UV–visible diffuse reflectance spectroscopy (UV-DRS), Brunauer-Emmett-Teller (BET), linear sweep voltammetry (LSV) and electrochemical impedance spectroscopy (EIS) were employed to characterize the physical and chemical properties of BiVO₄ composites. The composite formed at pH = 1 exhibited the lowest hole-electron (h⁺-e^-) recombination rate, resulting in the highest photocatalytic activity towards microcystin-LR (MC-LR), with near 100% removal of MC-LR in 5 h. ESR and trapping experiments indicated that MC-LR degradation was mediated primarily by hydroxyl radicals (•OH), superoxide radicals (O₂^•−) and photogenerated holes (h⁺).