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透射电子显微镜(TEM)是电子显微学的重要工具之一,其中制备高质量的样品是获得研究成果的关键之一。FIB结合了精细加工技术和微分析技术,具有在亚微米线度上的微细加工和高分辨率成像的能力,成为强有力的TEM制样工具。Zr的热中子吸收截面小,在高温高压水中具有良好的耐腐蚀性能和力学性能,因而锆合金被用作压水堆核电站中核燃料元件的包壳材料。锆合金氧化膜的晶体结构控制其耐腐蚀性能。针对用于透射电镜观察的锆合金氧化膜截面样品制备较为困难的问题,介绍了氧化膜截面TEM样品的手工制备方法与过程,对比了应用双束型FIB制备截面TEM样品的优点。
Transmission electron microscopy (TEM) is one of the most important tools of electron microscopy. One of the key points to get the research results is to prepare high quality samples. FIB combines microfabrication and microanalysis techniques with the ability to perform microfabrication and high-resolution imaging on submicron dimensions, making it a powerful TEM sample preparation tool. The thermal neutron absorption cross section of Zr is small and has good corrosion resistance and mechanical properties in high temperature and high pressure water. Thus, Zr alloy is used as a cladding material for nuclear fuel elements in PWR nuclear power plants. The crystal structure of zirconium alloy oxide film controls its corrosion resistance. Aiming at the difficult preparation of cross-section sample of zirconium alloy oxide film for transmission electron microscope observation, the preparation method and process of oxide film cross-section TEM sample are introduced. The advantages of using double-beam FIB to prepare cross-section TEM sample are compared.