Using thulium oxide, nitric acid, ammonium metavanadate and citric acid as main raw materials, TmVO4 was successfully prepared by hydrothermal method. TmVO4 samples were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM), thermogravimetry differential scanning calorimetry (TG-DSC), and Fourier transform infrared spectroscopy (FT-IR). Taking methyl orange solution as simulated sewage, the effects of synthesis temperature and illumination time on the photocatalytic activity of TmVO4 were studied. The results show that pure tetragonal zircon TmVO4 samples can be obtained under hydrothermal conditions of 120 °C to 180 °C. The sample prepared at 140°Chas uniform grain size, and the average grain size is about 50 nm. Under ultraviolet light illumination for 30 min, the degradation rate of 10 mg/L methyl orange can reach more than 77% in the presence of TmVO4. The photocatalysis experiment indicated that TmVO4 has good photocatalytic degradation activity for methyl orange.
TmVO4 precursor gel was prepared by sol-gel method using thulium oxide, nitric acid, ammonium metavanadate and citric acid as main raw materials. Then the xerogel was calcined at 600–800 °C in muffle furnace to prepare TmVO4. The prepared samples were characterized by thermogravimetric differential scanning analysis (TG-DSC), X-ray diffraction analysis (XRD), scanning electron microscopy (SEM), diffuse reflectance spectroscopy(DRS) and Fourier transform infrared spectroscopy(FT-IR). The visible-light photocatalytic activity of TmVO4 was studied by using methylene blue solution as simulated wastewater. The result shows that TmVO4 can be obtained by calcination at 700 °C. The average grain size is about 80 nm and the bandgap is 2.16 eV. Under visible-light conditions, the degradation rate of methylene blue can reach more than 90% when methylene blue solution of 10 mg/L was illuminated 60 min in the presence of nanoparticulate TmVO4. The nanoparticulate TmVO4 has excellent photocatalytic degradation activity for methylene blue. Nanoparticulate TmVO4 prepared by sol-gel method has broad application prospects in photocatalytic degradation of organic pollutants.