The Ni-P amorphous alloy/ceramic composite membrane of high selectivity and permeability for hydrogen was prepared by a new technique of partial electroless plating. Its permeability and ideal separation factor for H-2/Ar were investigated. The results demonstrated that the permeability of the Ni-P amorphous alloy membrane was almost the same as that of a porous inorganic membrane, but the separation factor for H-2/Ar through the Ni-P membrane was obviously higher than that through a porous inorganic one. The morphology and microstructure of Ni-P amorphous alloy/ceramic composite membrane were characterized by SEM and XRD.