Abstract: By using gas-solid reaction method, the hydrogen permeation barrier with 5 ～ 20 μm thickness was prepared on the surface of zirconium and zirconium hydride. The examinations of the morphology and structure of the barrier were accomplished by optical microscope and SEM. The compositions of the barrier were determined by EDS. The phases in the barrier were also analyzed by XRD. The results indicate that the barrier is well distributed and compact, moreover it combines firmly with the matrix. There are Zr, O, C, P and H etc. elements in the barrier. Otherwise the oxygen diffuses in matrix apparently. The main phases of the barrier are the ZrO_2 and ZrP. There exists the ZrC phase or other phases.