Aggregated nanoparticles: Sample preparation and analysis by atom probe tomography
Aggregated nanoparticles: Sample preparation and analysis by atom probe tomography
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DOI：
10.1016/j.ultramic.2020.113082
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发表时间：
2020-11-01
期刊：
影响因子：
2.2
通讯作者：
Bell, David C.
中科院分区：
文献类型：
--
作者：
Barroo, Cedric;Akey, Austin J.;Bell, David C.
原子探针断层扫描（APT）可以测量材料的三维结构和组成，但对于具有挑战性的材料，如纳米颗粒聚集体，需要特定的样品制备程序。事实上，试样内孔隙度的存在影响试样的稳定性和数据的准确性。在这里，纳米颗粒聚集体被转移到一个微操作器尖端，并通过电子束辅助沉积Pt嵌入。需要连续的fib铣削和Pt沉积来制造合适的APT尖端。3D重建显示了15-20 nm纳米颗粒的存在，质谱分析显示催化剂中不存在微量元素，因此可以作为合成特定成分纳米颗粒的质量控制。
Atom probe tomography (APT) allows measurement of the three-dimensional structure and composition of materials, but specific sample preparation procedures are required for challenging materials such as aggregates of nanoparticles. Indeed, the presence of porosity within the specimen affects both the stability of the sample and the accuracy of the data. Here, aggregates of nanoparticles were transferred onto a micromanipulator tip and embedded via electron-beam-assisted deposition of Pt. Successive FIB-millings and Pt-depositions are needed to create suitable APT tips. The 3D reconstruction reveals the presence of 15-20 nm nanoparticles, and massspectral analysis shows the absence of trace elements within the catalyst, thus serving as quality control for the synthesis of nanoparticles with specific compositions.