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Biomass charcoal-doped titanium dioxide (C/TiO2) composites were proposed by microwave-hydrothermal and calcination method using tetrabutyl titanate as the titanium source and lignin as the carbon source. TiO2 crystals with different morphologies could be successfully adsorbed onto the surface of biomass charcoal. These products were investigated by X-ray powder diffraction (XRD), scanning electron microscopy (SEM), thermogravimetric analysis (TG), derivative thermogravimetric (DTG), UV–vis diffuser flection spectroscopy (UV–vis), Fourier transform infrared spectroscopy (FT-IR), and Brunauer–Emmett–Teller (BET). The photocatalytic activities of the as-obtained composites were checked under visible light irradiation. The results showed that both the microwave-hydrothermal temperature and time played an important role in the microstructure and photocatalytic activity of the samples. The rapid microwave-hydrothermal with the thermal post-treatment provides a promising route for the fabrication of biomass charcoal-doped nanocomposites materials. Keywords: Microwave-hydrothermal, Titanium dioxide, Biomass charcoal, Nanocomposites, Photocatalytic