Abstract: Ni(CH₃COO)₂+PVP-Zn(CH₃COO)₂+PVP-Ti(OC₄H₉)₄+CH₃COOH+PVP composite cables had been fabricated through modified electrospinning equipment. NiO-ZnTiO₃-TiO₂ coaxial trilayered nanocables were obtained by the calcination of the relevant composite cables at 600℃. The samples were characterized by use of thermogravimetric-differential thermal analysis (TG-DTA), X-ray diffractometry (XRD), Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). Formation mechanism of NiO-ZnTiO₃-TiO₂ coaxial trilayered nanocables was preliminarily proposed. The results show that the samples are NiO-ZnTiO₃-TiO₂ coaxial trilayered nanocables. The core layer is NiO, and its diameter is about (42.024±4.405) nm. The middle layer is ZnTiO₃, and its thickness is about (55.385±7.681) nm. The outer layer is TiO₂, the thickness is about (70.747±7.373) nm.