Nickel may be produced in acidic chloride-sulfate based electrolytes. Nickel is initially deposited on stainless steel or titanium cathodes to produce starting sheets while chlorine gas is evolved on DSA anodes. Stress in the nickel deposit may cause bending of the cathode sheet. In addition, irregular growth such as dendrite formation may occur. In extreme cases, short-circuiting of electrodes will happen. Fundamental electrochemical studies of the initial stages of the electrodeposition process may give valuable information for obtaining smooth nickel deposits. Electrochemical experiments of nickel deposition were carried out on titanium substrates using cyclic voltammetry and potential step, and examined with SEM imaging. The measurements were performed at different deposition potentials and times to get an overall picture of the nucleation and growth of nickel on titanium substrates. Further deposition studies have been performed using in situ AFM to study the whole process from single nickel nuclei to a cohesive layer, and determine the nucleation mode and characteristics. The effects of electrolyte composition and pH will be presented. The pre-treatment of the substrate is important for the nucleation and properties of the nickel deposit. The figure illustrates the different nucleation overpotential for a smooth and rough titanium substrate. Figure 1