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Graphene encapsulation enabled high-throughput atom probe tomography of liquid specimens
Ultramicroscopy ( IF 2.1 ) Pub Date : 2020-09-01 , DOI: 10.1016/j.ultramic.2020.113036
Shi Qiu 1 , Vivek Garg 2 , Shuo Zhang 1 , Yu Chen 3 , Jian Li 4 , Adam Taylor 5 , Ross K W Marceau 5 , Jing Fu 6
Affiliation  

A new method for imaging liquid specimens with atom probe tomography (APT) is proposed by introducing graphene encapsulation. By tuning the encapsulation speed and the number of encapsulations, controllable volumes of liquid can be encapsulated on a pre-sharpened specimen tip, with the end radius less than 75 nm to allow field ionization and evaporation. Encapsulation of liquid has been confirmed by using various characterization techniques, including electron microscopy and stimulated emission depletion microscopy. The graphene-encapsulated liquid specimen was then directly frozen at the cryogenic stage inside the atom probe instrument, followed by APT imaging in laser-pulsed mode. Using water as a test example, water-related ions have been identified in the acquired mass spectrum, which are spatially correlated to a reconstructed three-dimensional volume of water on top of the base specimen tip, as clearly revealed in the chemical maps. In addition, the proposed method has also been shown to produce multiple liquid specimens simultaneously on a pre-sharpened silicon micro-tip array for high-throughput APT imaging of liquid specimens. It is expected that the proposed lift-out-free method for preparing APT specimens in their hydrated state will open a new avenue for obtaining insights into various materials at atomic resolution.

中文翻译:

石墨烯封装使液体样品的高通量原子探针断层扫描成为可能

通过引入石墨烯封装,提出了一种使用原子探针断层扫描(APT)对液体样品进行成像的新方法。通过调整封装速度和封装数量,可将可控体积的液体封装在预先锐化的样品尖端上,末端半径小于 75 nm,以允许场电离和蒸发。液体的封装已通过使用各种表征技术得到证实,包括电子显微镜和受激发射耗尽显微镜。然后将石墨烯封装的液体样品直接冷冻在原子探针仪器内的低温阶段,然后以激光脉冲模式进行 APT 成像。以水为例,在采集到的质谱图中鉴定出与水相关的离子,正如化学图中清楚地显示的那样,它们在空间上与基础样品尖端顶部重建的三维水体积相关。此外,所提出的方法还被证明可以在预锐化的硅微尖端阵列上同时产生多个液体样品,用于液体样品的高通量 APT 成像。预计所提出的用于制备处于水合状态的 APT 样品的无剥离方法将为以原子分辨率深入了解各种材料开辟一条新途径。
更新日期:2020-09-01
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