The preparation of nanoscaled palladium ͑Pd͒ particles for catalyzation of electroless copper ͑Cu͒ plating has been investigated in this research. Nanosized Pd catalysts were electrochemically deposited on Si/SiO 2 /Ta x N substrates using displacement activation and sensitization activation, and their formation and microstructures were characterized. By displacement activation, large Pd particles with nonuniform size distribution from 20 to 200 nm are observed, resulting in subsequent rough and discontinuous Cu films electrolessly deposited on these Pd catalysts. In comparison, tremendous, small, and uniform Pd nanoparticles of about 10 nm are obtained by sensitization activation as fine nucleation sites for following electroless deposition of smooth and conformal Cu films. Nucleation, growth, coalescence, and then connection and film growth steps are observed in the formation process of Cu films. No preferred orientation of both electrolessly deposited Cu films is found. Well-controlled, electrochemically deposited nanoscaled Pd catalysts and uniform Cu films can be used as 65 nm Cu interconnect metallization.When the sizes of material structures are scaled down to nanometers, surfaces will occupy tremendous portions of whole materials and play very important roles. Surface effect, small-size effect, and even quantum effects are thus caused and severely affect the physical and chemical properties of these nanosized materials. Especially the insufficient coordination sites and high surface energy resulting in the high activity of these large amounts of surface atoms renders the application of nanosized materials to catalysts very possible. 1 For example, nickel, iron, and cobalt ferromagnetic nanoparticles have attracted a lot of interest as catalysts for the preparation of carbon nanotubes. 1 Copper with low electrical resistivity, good mechanical properties, and high electromigration resistance is used for interconnect metallization in dual-damascene structures of ultralarge-scale integrated ͑ULSI͒ circuits. 2-4 Electrochemical Cu plating, one of the Cu deposition techniques, becomes much attractive in semiconductor manufacturing industry because of its low processing temperature, high step coverage, high selectivity, and low cost. 4-7 However, sputtered Cu seed layers are still necessary for Cu electroplating, while their deposition technique is not adequate due to the insufficient gap-filling capability when the linewidths of integrated circuits ͑ICs͒ for next generation decrease to 65 nm. 8 Since that, the growth of Cu films with high selectivity and good step coverage by electroless deposition has been intensively studied. [9][10][11][12][13][14][15] One of the most important factors to influence the quality and morphologies of the electrolessly deposited Cu films is the activation step to seed the inert substrates prior to the nucleation and growth of Cu films. A large amount of uniformly distributed, nanoscaled catalysts dominates the success of activation process and subsequent electroless plating. Two ...