A novel single-layer polycrystalline anatase TiO 2 (SLP TiO 2 ) nanosheet with porous structure was synthesized through a simple solvothermal method by employing rod-like titanyl sulfate as the starting material in the presence of glycerol, followed by calcination. SEM, TEM, X-ray diffraction, FTIR spectroscopy, thermogravimetry coupled to FTIR spectroscopy, solid-state 13 C NMR spectroscopy, and N 2 adsorption/desorption processes were employed to investigate the structure of the products. The structure and morphology were found to be dependent on the experimental conditions,