用于原子探针断层成像的液/固界面的定点和低温标本制备方法。
A method for site-specific and cryogenic specimen fabrication of liquid/solid interfaces for atom probe tomography.
机构信息
Energy and Environment Directorate, Pacific Northwest National Laboratory, P.O. Box 999, Richland, WA 99352, USA.
Earth and Biological Sciences Directorate, Pacific Northwest National Laboratory, P.O. Box 999 Richland, WA 99352, USA.
出版信息
Ultramicroscopy. 2018 Nov;194:89-99. doi: 10.1016/j.ultramic.2018.07.010. Epub 2018 Jul 25.
A site-specific, cryogenic, focused ion beam (FIB) method is presented for the preparation of atom probe tomography (APT) specimens from a frozen liquid/solid interface. As a practical example, the interface between water and a corroded boroaluminosilicate glass has been characterized by APT for the first time. The water/glass interface is preserved throughout specimen preparation by plunge freezing the corroding glass particles with the corrosion solution into slush nitrogen. Site-specific specimen preparation is enabled through a new approach to extract and mount a small volume of material using a cryogenically cooled FIB stage and micromanipulator. The prepared APT specimens are subsequently transferred from the FIB to APT under cryogenic and high-vacuum conditions using a novel FIB/APT transfer shuttle and home-built environmental transfer hub attached to the APT system. Particular focus is given to the technical methods for specimen fabrication under cryogenic conditions. Persistent challenges are discussed in addition to future opportunities for this new specimen preparation method.
提出了一种针对冷冻液/固界面的用于制备原子探针层析术（APT）样品的特定位置、低温、聚焦离子束（FIB）方法。作为一个实际的例子，首次通过 APT 对水和腐蚀的硼铝硅酸盐玻璃之间的界面进行了表征。通过将带有腐蚀溶液的腐蚀玻璃颗粒浸入液态氮中骤冷来保存整个样品制备过程中的玻璃/水界面。通过一种新的方法，使用低温冷却的 FIB 台和微操作器提取和安装小体积的材料，从而实现了特定位置的样品制备。随后，通过一种新型的 FIB/APT 转移吊舱和附在 APT 系统上的自制环境转移中心，在低温和高真空条件下将制备好的 APT 样品从 FIB 转移到 APT。特别关注低温条件下的样品制备技术方法。除了对这种新的样品制备方法的未来机会进行讨论之外，还讨论了持续存在的挑战。
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