Thin supported palladium membranes were prepared using electroless plating technique. The intrinsic plating kinetics were determined for hydrazine-based palladium plating baths. Mathematical models were developed to predict film thickness and plating rate as a function of plating parameters (i.e., reactant concentrations, temperature and time). Analyses of film surface microstructure indicate that grain structure is dependent on both plating chemistry and plating rate. The evolution of film morphology during electroless plating was also investigated. Hydrogen permeation study demonstrated that film structure has a significant influence on the permeation performance of the palladium membrane.