Figure 1 shows the XRD patterns of nickel sulphide thin films grown at pH 2.5 for 3 hours under different solution concentrations. The observed peaks at 2θ = 30.2°, 50.3° and 59.5° positions correspond to the (111), (220) and (311) planes. The comparison of the observed diffraction peaks with the standard (JCPDS Reference code: 00-052-1027) confirmed that the material is the cubic of nickel sulphide [11]. Comparison between the films deposited at 0.075 M and 0.1 M reveals that the intensity of the peaks increased, indicating better crystalline phase in the films prepared at lower concentration. This could be clearly seen in the peak attributable to (111) plane, which is more intense. On the other hand, the peaks marked “◊” in the Figure 1 at 2θ =35.4° and 45.2° are belong to indium tin oxide [12] (JCPDS Reference code: 01-089-4597). These peaks are come from ITO glass used as substrate during deposition process