We describe a novel chemical vapor deposition (CVD) procedure for depositing a Pd activation layer for subsequent electroless Cu deposition. The two-step process uses a continuous precursor transfer step followed by a batch H-2 reduction step to achieve efficient utilization of the Pd (hfac)(2) precursor. The resulting activation layer contains both isolated Pd (0) clusters (ca. 10 nm average diam) and also dispersed Pd (II) species that appear to be stabilized by residual (hfac) fragments. The activation layer produces growth rates for Cu electroless deposition that are similar to values reported for Pd activation layers prepared using wet chemical methods. The Cu growth rate is independent of the Pd (0) cluster density, which suggests that Cu nucleation occurs at both Pd (0) clusters and the dispersed Pd (II) species. The Cu films shows poor adhesion upon drying, which we attribute to weak film attachment at the Pd (II) sites. (c) 2007 The Electrochemical Society.