Coatings for preventing hydrogen escaping were formed on disk-type ZrH1.8 by in-situ oxidation method. Urea was placed and in vacuum chamber and decomposed into complicated chemical compound including carbon, nitrogen, oxygen source. The phase structure and morphology of coatings were analyzed by X-ray diffraction (XRD) and scanning electron microscope (SEM). The composition and depth of elements, bond states were tested by auger electron spectroscopy (AES) and X-ray photoelectron spectroscopy (XPS) technique. The results indicate that weight of coatings increased with temperatures rised. XRD shows the phase structure of coatings consists mainly of ZrN and ZrO2, including monoclinic ZrO2 (m-ZrO2) and tetragonal ZrO2 (t-ZrO2). SEM depicts coatings were accumulated and combined densely with substrate. AES indicates that the coating is mainly composed of carbon, nitrogen, oxygen and zirconium, which show that the atomic concentration of carbon and nitrogen decreased continuously, while, oxygen and zirconium increased with sputter time incresing. XPS shows that coating was including Zr-O、Zr-C、Zr-N-O、Zr-N、O-H bonds. It is possible the C, N, O atoms synergistic effect, making the coating has good resistance hydrogen permeation.