Herein, we report the preparation of manganese tungstate (MnWO4) nanosheets, nickel tungstate (NiWO4) nanoparticles, manganese nickel tungstate (MnNiWO4) hybrid nanostructures, and manganese nickel tungstate (MnNiWO4) hybrid nanostructures attached to the surface of carbon nanofibers (CNFs) using a simple hydrothermal and wet impregnation method. The prepared photocatalysts were characterized by X-ray diffraction (XRD), Ultraviolet–Visible diffuse reflectance spectroscopy (UV–Vis DRS), Fluorescence spectroscopy (FL), Field emission scanning electron spectroscopy (FESEM), Energy dispersive spectroscopy (EDS), X-ray photoelectron spectroscopy (XPS), and Transmission electron microscopy (TEM) to investigate their crystal structure, optical and electrical properties, microstructure, elemental composition, and structural characteristics. The X-RD and TEM outcomes explain that both the pure and hybrid composite samples have a crystalline nature with nanosheets, nanoparticles, and hybrid nanostructures, which are attached to the carbon nanofibers. Compared to other samples, a significant red shift in the absorption and reduction of the energy band gap (2.81–2.35 eV) was observed for the MnNiWO4/CNF hybrid nanocomposite. Further, an anionic azo dye such as Orange II sodium salt (ONaS) was adopted to check out the photocatalytic activities of the synthesized samples. Under illumination, the MnNiWO4/CNF hybrid nanocomposite exhibited a high degradation efficiency (85%) compared to other photocatalysts. Additionally, this hybrid nanocomposite was used to degrade the anionic dye methyl orange (M.O) and cationic dye methylene blue (M.B) under illumination. The hybrid photocatalyst showed degradation efficiencies of 77% for methyl orange (M.O) and 61% for methylene blue (M.B). Furthermore, kinetic studies have shown that the photocatalytic degradation method follows pseudo-1st-order reaction kinetics. The high photocatalytic performance of the MnNiWO4/CNFs hybrid nanocomposite over other photocatalysts has been ascribed to their size, surface charge, electronic effect, and effective charge-transfer abilities.
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