| Summary: | Ionic liquids (ILs) could serve as a structuring agent, a solvent, or a source of dopant during solvothermal synthesis of semiconductors particles. To understand the role of IL during formation of TiO<sub>2</sub> particles, it is necessary to study the stability of this IL in solvothermal synthesis conditions, as well as studying the surface properties of formed TiO<sub>2</sub> particles. In view of this, the effect of the 2,3,5-triphenyltetrazolium chloride IL ([TPTZ][Cl]) thermal decomposition during the solvothermal reaction and IL content in the reaction system on photoactivity of TiO<sub>2</sub> microparticles has been systematically investigated. The samples obtained by using [TPTZ][Cl] exhibited remarkable photocatalytic properties in phenol degradation reaction under visible light. HPLC analysis of the solvothermal reaction medium and X-ray photoelectron spectroscopy (XPS) analysis of TiO<sub>2</sub> particles revealed that [TPTZ][Cl] was decomposed completely and was incorporated into the TiO<sub>2</sub> lattice. Generally, increasing the reaction time (1, 4, 12, and 24 h) promoted the TiO<sub>2</sub> microspheres formation, as well as raising the visible light-induced photocatalytic activity of the photocatalysts. Longer reaction time was also accompanied by an increase in the efficiency of 2,3,5-triphenyltetrazolium chloride decomposition. The properties of the photocatalysts were investigated by means of UV-VIS diffuse reflectance spectroscopy (DRS), BET surface area measurements, scanning electron microscopy (SEM), X-ray powder diffraction (XRD) analysis, and XPS.
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