In this work, we prepared thin films of nickel sulfide by spray pyrolysis on substrates of the glass at temperature of 300°C. The solution used is a mixture of nickel acetate and thiourea as a source of nickel and sulfur respectively, acetic acid was used as a complexing agent, and then heated the resulting layers in an ordinary furnace at 300°C at different times of 1h, 2h and 3h to study the annealing time effect on the physical and chemical properties. The characterization methods used indicate remarkable changes in the structural, electrical, morphological and optical properties of NiS films under annealing time. The results obtained have shown that the prepared NiS films contain good crystallization, dense morphology, good stochiometric ratio and high conductivity, and these specifications make them a potential candidate as electrode material for application in super-capacitors.