Hydrogen anti-permeation coatings were formed by chemical reaction using urea and zirconium hydride at a high temperature range. The composition and depth of elements, bond state were analyzed by auger electron spectroscopy(AES) and X-ray photoelectron spectroscopy(XPS) technique. The results indicate that the thickness of coating, which is mainly composed of carbon, nitrogen, oxygen and zirconium, is 3.4μm, of which including nitrogen and carbon the thickness is about 150nm. It shows that the atomic concentration of carbon and nitrogen decreased continuously, while, oxygen and zirconium increased. XPS shows that coating was including ZrO₂, and Zr-OH, Zr-N, C-H, N-H bonds. The mechanism of hydrogen resistance maybe that hydrogen was seized by carbon, nitrogen and oxygen to form C-H, O-H and N-H bonds while it diffuses from zirconium hydrides.