The core–shell TiO2 nano-layer spheres were synthesized by hydrothermal method without surfactant, using tetraisopropyl titanate, diethylenetriamine and water as the capping agents. The structure of the products was characterized with X-ray diffraction (XRD), transmission
electron microscope (TEM) and scanning electron microscopy (SEM). The possible formation mechanism and electrocatalytic degradation characters of the products were also discussed.