Zinc oxide (ZnO) doped with transition metals like Fe, Co, Ni, Mn led to ferromagnetism in this material and development of such materials demonstrated their use in spintronic devices. In this work, Ni-doped ZnO films were deposited using a simple and economic process, chemical spray pyrolysis. The grown layers were analyzed using X-ray photoelectron spectroscopy (XPS) and Raman spectroscopy techniques and the results discussed. Ni-doped ZnO thin films were deposited on glass at a substrate temperature of 350 0C using a spray pyrolysis technique. The concentration of Ni in the layers was varied in the range, 0 – 15%. 0.1 M concentrated solutions of zinc acetate and nickel sulphate were used as the precursors. Compressed purified air was used as a carrier gas at a flow rate of 8 l/min and the solution was sprayed at a flow rate of 6 ml/min. The nozzle to substrate distance was fixed at 20 cm. The grown layers were uniform, pin hole free and well adherent to the substrate surface. The X-ray photoelectron spectroscopy (XPS) analysis revealed the presence of Zn, Ni, O and C in the films. Fig.1 shows the XPS spectrum of Zn1-xNixO film with x=10 %. The composition of the films was found to me approximately uniform across the thickness of the layers. The intensity of Zn 2p3/2 and Zn 2p1/2 peaks decreased with the increase of Ni-doping concentration in the films and the intensities of Ni 2p1/2 and Ni 2p3/2 peaks increased. The observed energy difference between Ni 2p3/2 (870.09 eV) and Ni 2p1/2 (853.3 eV) peaks is found to be 17.6 eV. The fact that this value do not match with the value for pure Ni and Ni-related oxides indicated that Ni atoms were successfully incorporated into ZnO lattice and are in +2 state. The Raman spectra showed a strong peak at 1085.8 cm-1 (Fig. 2) that correspond to the wurtzite crystal structure of ZnO in addition to other peaks related to other defect states. The intensity of the ZnO peak increases with the increase of Ni-doping concentration and also the peak moved slightly towards lower wavenumber side. No other peaks corresponding to the secondary phases of Nirelated oxides were found in the Raman spectra. This indicates the effective incorporation of Ni in ZnO lattice.figureFig.1. XPS spectrum Zn0.9Ni0.1O film. Fig.2. Raman spectra of Zn1-xNixO films.