Abstract: Cobalt nitrate and polyvinylpyrrole(PVP) were used as the raw materials to make the spinning solution in this paper. The precursor fibers and the calcined fibers were characterized and analyzed by scanning electron microscope, synchronous thermal analyzer, X-ray diffractometry, and transmission electron microscopy. The feasibility and optimal experimental conditions for the preparation of cobalt oxide nanofibers by electrospinning technology were investigated. The results show that, in the condition of the PVP(K30) mass fraction of 43%, cobalt nitrate mass of 2 g, and the optimum equipment parameters, an uniform and smooth cobalt nitrate/PVP precursor fiber with a diameter of about 600 nm can be prepared. After calcination at 600 ℃, the cobalt oxide nanofibers with the diameter of about 30 nm can be obtained.