We have used a double activation method to reduce the size of Pd catalytic particles commonly used as an activation layer for electroless Cu deposition. The method produces Pd particles with sizes reduced by a factor of 4 and density increased by a factor of 10 compared to the single activation method. The first activation and the Pd etching process in the double activation removes the native Ti oxide on TiN surface and largely increase the nucleation sites for Pd. With more nucleation sites, nucleation events Outrun ripening events throughout the deposition time range. However, excessive etching of Pd and the underlying TiN layer could lead to rougher electroless Cu films. Secondary ion mass spectrometry data show that the double activation step does not increase the net amount of Pd deposited on TiN surface; it only changes its particle size and density. Electroless Cu deposited on a doubly Pd activated Surface has a larger grain size and appears to have a lower resistivity. (C) 2008 Published by Elsevier B.V..