Hollow spherical NiO particles were prepared using the spray pyrolysis method with different concentrations of precursor. The electrochemical properties of the NiO electrodes, which contained a new type of binder, carboxymethyl cellulose (CMC), were examined for comparison with NiO electrodes with polyvinylidene fluoride (PVDF) binder. The electrochemical performance of NiO electrodes using CMC binder was significantly improved. For the cell made from 0.3 mol L−1 precursor, the irreversible capacity loss between the first discharge and charge is about 43 and 24% for the electrode with PVDF and CMC binder, respectively. The cell with NiO–CMC electrode has a much higher discharge capacity of 547 mAh g−1 compared to that of the cell with NiO–PVDF electrode, which is 157 mAh g−1 beyond 40 cycles.