Pd-based composite membranes are the attractive membrane materials for hydrogen separation due to their high hydrogen permeability and infinite permselectivity. Thin pure Ni and Pd-Ni alloy membranes with high hydrogen permeation were prepared by the electroless plating method. It is difficult to prepare the dense pure Ni membranes with 1-2 μm thickness for hydrogen separation. However, Pd-Ni alloy membranes with several micrometers thickness showed good permeation performance. Hydrogen permeance of the Pd95Ni5 alloy membrane with fcc phase up to 3.1×10-6 mol/m2 s Pa and the ideal permselectivity over 600 were obtained at 773 K.