Abstract
In the present work, we investigate the photo-electrochemical properties of β′-Mn3(PO4)2 prepared by hydrothermal route at 453 K for the first time. The phosphate was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), FTIR spectroscopy, and UV–Visible diffuse reflectance. The XRD pattern indicates a single phase crystallizing in a monoclinic structure with unit cell constants: a = 8.961(3) Å, b = 9.961(4) Å, and c = 24.138(1) Å, and β = 120.419°, due to the lifting of degeneracy of the Jahn–Teller effect of Mn2+ penta-coordinated. The SEM analysis shows a homogeneous morphology with similar grain sizes in the range 3–13 µm. Optical transitions are determined from diffuse reflectance which indicates direct (2.38 eV) and indirect (2.88 eV) optical transitions; assigned to Mn2+: d-d transition. To our knowledge, the photo-electrochemical characterization of β′-Mn3(PO4)2 is reported for the first time. The exchange current density (29 µA cm−2) is characteristic of good electrochemical stability. The dependence of the interfacial capacitance on the potential (C−2 − E) displays n-type conduction with electrons as majority carriers, a behavior supported by the chrono-amperometry. A flat band potential (Efb) of 0.29 VSCE and an electron mobility (µe) of 1.6 × 10−6 cm2 V−1 s−1 have been determined. The semicircle in the electrochemical impedance spectroscopy (EIS) is due the charge transfer (24.6 kΩ cm2) which falls down to 3.25 kΩ cm2 under visible irradiation, corroborating a semiconducting behavior. The phosphate is stable at neutral pH and is successfully tested for the oxidation of methyl violet (MV). The valence band deriving from O2−: 2p character (2.65 VSCE/7.40 eV) has a strong oxidizing power, able to mineralize the dye radicals. The integrated intensity of the visible light (23 mW cm−2) shows a total MV photodegradation in the presence of β′-Mn3(PO4)2 within 5 h. A first-order model is successfully used with a half-photocatalytic life of 113 min. As expected, the COD removal yield increases, with illumination time, and reaches 4.26% after 5 h while the total organic carbon (TOC) removal rate reached 9%. According to the inhibitor study, the holes (h+) were found to be the main active radicals in the photocatalytic process, followed by the •OH.
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Acknowledgements
The authors are grateful for Dr M. M. Kaci for his technical assistance in the COD analysis.
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This work was financially supported by the Faculty of Chemistry (Algiers).
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Bagtache, R., Djaballah, A.M., Tartaya, S. et al. Physical and photo-electrochemical study of β′-Mn3(PO4)2 and its application to photodegradation of methyl violet under visible irradiation. J Solid State Electrochem 26, 1421–1430 (2022). https://doi.org/10.1007/s10008-022-05164-4
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DOI: https://doi.org/10.1007/s10008-022-05164-4