This work addresses the combinatorial plating characteristics of dense Pd/Ni/porous stainless steel (PSS) composite membranes in comparison with Pd/PSS membranes. While Pd/PSS membranes were fabricated using 0.1 pin nominal pore size PSS supports, Pd/Ni/PSS membranes were fabricated using 0.5 and 0.1 pm nominal pore size PSS supports. Both Ni and Pd films were deposited using an identified novel electroless plating process that characterizes the optimal utilization of surfactant, sonication and reducing agent contacting pattern in Pd electroless plating baths. It was observed that the combinatorial plating characteristics for Pd/Ni/PSS membranes were significantly different and poorer in comparison with those obtained for the Pd/PSS membranes. In summary, it has been inferred that the introduction of nickel interdiffusion barrier was not fruitful to reduce the critical thickness of dense Pd film without jeopardizing upon the pore densification. (C) 2014 Published by Elsevier B.V.