碳酰胺与氢化锆高温下原位反应层的AES/XPS分析

AES and XPS Analysis on Hydrogen Permeation Barrier Formed by Reaction between Urea and Zirconium Hydride at High Temperature

采用碳酰胺高温分解产生含C、O、N源与氢化锆原位反应制备阻氢渗透层,借助俄歇电子能谱(AES)和X射线光电子能谱(XPS)等手段对阻氢渗透层元素成分及深度、键态进行分析。AES结果表明:氢化锆表面原位反应层由C、N、O、Zr元素组成,随溅射时间增加,O、Zr元素含量增加,C、N元素含量降低。原位反应层厚度约3.4μm,其中含N、C层深度约150 nm。氢化锆表面阻氢渗透层XPS分析表明,表面层存在ZrO_2,同时有Zr-OH、Zr-N、C-H、N-H键。氢在扩散过程中被C、O、N捕获表明含C、O、N的氢化锆表面原位反应层对氢的渗透有一定的阻碍作用。

Hydrogen permeation barriers were prepared by the chemical reaction between urea and zirconium hydride at high temperature. The composition and depth of elements, bond state were analyzed by auger electron spectroscopy（AES） and X-ray photoelectron spectroscopy（XPS）. AES results indicate that the barrier is mainly composed of carbon, nitrogen, oxygen and zirconium, whose thickness is about 3.4 μm, including 150 nm of nitrogen and carbon. The atomic concentration of carbon and nitrogen decreases continuously, while the content of oxygen and zirconium increases with longer sputtering time. XPS shows that the barrier contains ZrO2 as well as Zr-OH, Zr-N, C-H and N-H bonds. The mechanism of hydrogen resistance may be that hydrogen is captured by carbon, nitrogen and oxygen to form C-H, N-H and O-H bonds, respectively, when it diffuses from zirconium hydrides. Therefore, the prepared coatings can prevent hydrogen permeation effectively.