The procedure for creating a high-surface area electrode from the electrodeposition of Raney nickel powder onto a titanium grid was presented. The procedure to obtain reproducible and scalable electrodes was demonstrated. The electrodeposition of Raney nickel onto the titanium substrate involved electroplating nickel from a large nickel anode in a nickel plating bath containing suspended Raney nickel particles onto a titanium grid cathode. The electrodeposition method realized two materials in the final deposit: pure nickel and Raney nickel particles. Optimization of current density and charge density was performed via a factorial design experimental method to maximize the percentage of Raney nickel powder deposited on the grid. Further statistical analysis was performed to show the reproducibility of producing Raney nickel electrodes through this method. Once these variables were optimized, a scale-up of the deposition process was performed to demonstrate the feasibility of the procedure using larger substrates. Reproducible electrodes were obtained which can find applications in fuel cells as well as electrolytic hydrogen generators. This is an abstract of a paper presented at the 2005 AIChE Annual Meeting and Fall Showcase (Cincinnati, OH 10/30/2005-11/4/2005).