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A nanocomposite (NC) of titanium (IV) oxide (TiO2) and molybdenum (VI) oxide (MoO3) was synthesized using a hydrothermal route. Detailed analyses using transmission electron microscopy, X-ray diffraction, X-ray fluorescence (XRF), Brunauer–Emmett–Teller (BET) isotherms, X-ray photoelectron spectroscopy, Raman, and diffuse reflectance infrared Fourier transform spectroscopy were carried out and confirmed the successful formation of pure TiO2-MoO3 (Ti-Mo) NC. The Ti-Mo NC possesses sizes in the range of 150–500 nm. XPS, Raman, and DRIFT shift measurements confirmed the formation of mixed oxide linkage in the form of Ti-O-Mo. Sorption of nitrogen isotherms revealed a significant increase in the number and pore widths of mesopores in the NC. Water sorption isotherms revealed enhanced affinity of the nanocomposites for water relative to the pure metal oxides. The BET surface area for Ti-Mo NC from the nitrogen adsorption isotherm was 129.3 m2/g which is much higher than the pure metal oxides (i.e., 37.56 m2/g for TiO2 and 2.21 m2/g for MoO3). The Ti-Mo NC provided suitable adsorption sites that captured the studied carbamates from the solution and promoted their photodegradation process. The photocatalytic degradation of MB in the presence of the catalyst was enhanced by 2.9 and 5.5 folds upon irradiation with white LED and 302 nm UV light sources, respectively.

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