Electrospinning is a versatile method for preparation of submicron-size fibers under ambient temperature. We demonstrate a new approach based on this method for preparing an electrode which consists of the fibers coated with nickel oxide (NiO) and acetylene black (AB) on their surfaces. The NiO/polymer fibrous electrodes show the electrochemical responses based on the electrochemical reaction of Ni(OH)(2) which is produced from NiO in alkaline aqueous solution. The capacitance of the test half cell with the as prepared NiO/polymer fibrous electrode in 1 mol l(-1) KOH aqueous solution is 5.8 Fg(-1) (per gram of NiO). Heat treatment (at 150 degrees C for 1 h in the air) of the NiO/polyrner fibrous electrode increases the capacitance of the NiO/polyrner fibrous electrode. The capacitance ofthe cell with the heat treated (HT) NiO/polymer fibrous electrode is 163 Fg(-1) (per gram of NiO). SEM observation of the heat treated electrode suggests that partial melt ofthe fibers on the Current collector forms the conducting passes and networks between the NiO particles and the collector and increases the specific capacity of the fibrous electrode. (C) 2009 Elsevier B.V. All rights reserved.