In present work, polyvinyl alcohol/copper acetate -nickel acetate composite nanofibers (PVA/Cu(OAc)(2)Ni(OAc)(2) NFs) with various weight percentages of Cu(OAc)(2):Ni(OAc)(2) such as 25:75, 50:50 and 75:25 are fabricated by electrospinning method. After this, the CuO/Ni0 composite NFs are produced after thermal treatment. A calcination temperature at about 600 degrees C is determined by thermal gravimetric analysis. Field -emission scanning electron microscopy (FE-SEM) for morphology characterization indicates that large quantities of the prepared PVA/Cu(OAc)(2)-Ni(OAc)(2) composite fibers have smooth and bead -free surfaces. Fourier transform infrared spectroscopy, FE-SEM and energy dispersive X-ray spectroscopy are used to characterize the CuO/NiO composites. According to FE-SEM results, with increasing of Cu(OAc)(2) content in polymeric solution, the fibers don't remain as continuous structures after calcination and accumulate in the form of nanoparticles. Also, a carbon paste electrode (CPE) bulky modified with CuO/Ni0 composites is used for investigation of the electro-catalytic oxidation of hydrazine hydrate in NaOH solution. The catalytic activities of the synthesized catalysts are studied through cyclic voltammetry, chronoamperometry and electrochemical impedance spectroscopy. The obtained results demonstrate that the most appropriate proportion of Cu(OAc)(2):Ni(OAc)(2) in electrospinning solution to enhance the electro-catalytic ability is 25:75. (C) 2017 Elsevier B.V. All rights reserved.