Recently, demands for 3D structural characterization are rapidly increasing in material science. In response to the demands, we have developed the 3D structural characterization technique using the combined system of focused ion beam scanning electron microscope (FIB-SEM) with a low aberration FIB column, Hitachi NB5000. The FIB-SEM system full automates serial sectioning work for simultaneous or alternating FIB and SEM operation. It is especially important in FIB fabrication to pay attention to fine structural changes that may occur to a sample due to ion-beam damage. Low accelerating voltage condition and cryo-FIB technique helps reduce the electron-beam damage. Currently, with demand for highly active materials such as Lithium (Li) expansion, the requirement to analyze Li using an electron microscope has been increased. But, it reacts with Oxygen and water vapor at atmospheric pressure. Therefore, the handling under the condition of inactive gas is required. In order to analyze materials highly active with atmospheric air, we developed a vacuum system consisting of specimen holders protected from air, a glove box, focused ion beam system, and electron microscope. The effectiveness was tested using negative electrode of lithium ion battery after charged. As a result, it was possible to transport, fabricate and observe the specimen without damage.
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