In the present work, manganese cobaltite (MnCo2O4) spinel (MCO) was synthetized by Pechini and hydrothermal method, characterized and photocatalytically evaluated toward H2 production through water splitting under visible-light irradiation. Characterization consisted in Thermogravimetry analysis (TGA), X-ray diffraction (XRD), X-ray photoelectron spectroscopy, scattering transmission electronic microscopy, BET surface area, UV-Vis spectroscopy, cyclic voltammetry, Hall effect, and photoluminescence. The MCO were evaluated as photocatalyst using an artificial visible light lamp and monitored by gas chromatography. XRD analysis found a pure spinel phase MCO. The surface area was ∼5 m2·g−1 for the MCO synthetized by Pechini and increased to 155 m2·g−1 with the hydrothermal method with acetates as precursors. The Pechini MCO showed higher carrier mobility but the fastest recombination. Photocatalytic evaluation of the MCOs showed that the highest photocatalytic activity generated was 12 μmol H2/gcat at 8 h with the MCO obtained by hydrothermal method with the acetates.
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