Koç Ömer, Jenkins Benjamin M, Haley Jack, Hofer Christina, Meier Martin S, Jones Megan E, Harrison Robert W, Preuss Michael, Moody Michael P, Grovenor Christopher R M, Frankel Philipp
Department of Materials, The University of Manchester, Oxford Road, M13 9PL, UK.
Department of Materials, University of Oxford, Parks Road, Oxford, OX1 3PH, UK; University of Rouen Normandie, INSA Rouen Normandie, CNRS, Groupe de Physique des Matériaux UMR 6634, F-76000 Rouen, France.
Ultramicroscopy. 2025 Jul 13;277:114210. doi: 10.1016/j.ultramic.2025.114210.
Specimen preparation is a key step in the characterisation of materials systems. For high-resolution characterisation techniques such as transmission electron microscopy (TEM) and atom probe tomography (APT), it is necessary to have a sample preparation method that creates the nano-scale samples required for analysis but does not significantly modify the initial microstructure. The preparation of hexagonal close-packed materials by focussed ion beam milling (FIB) and electropolishing has previously been shown to be complicated by hydride formation. The formation of hydrides can be reduced by the application of cryogenic temperatures during the final stages of Ga ion FIB milling, which are often conducted at low accelerating voltages in order to minimise irradiation-induced damage. Xe ion plasma FIBs are now commonly used in the preparation of samples due to their higher milling rates. However, the severity of the hydride formation in hexagonal close-packed materials during Xe ion milling is unclear. In this paper, we compare Xe and Ga FIB milling to prepare Zr samples at ambient and cryogenic temperatures. By studying TEM and APT samples, we are able to compare the levels of hydride formation after FIB preparation caused by the different preparation techniques. APT is used to estimate the levels of hydrogen in the samples. These results represent an important contribution to researchers who use FIB preparation to create TEM and APT specimens from hexagonal close-packed metals such as zirconium.
样品制备是材料系统表征的关键步骤。对于诸如透射电子显微镜（TEM）和原子探针断层扫描（APT）等高分辨率表征技术，需要一种样品制备方法，该方法能制备出分析所需的纳米级样品，同时又不会显著改变初始微观结构。先前已表明，通过聚焦离子束铣削（FIB）和电解抛光制备六方密排材料会因氢化物形成而变得复杂。在Ga离子FIB铣削的最后阶段施加低温可以减少氢化物的形成，这些阶段通常在低加速电压下进行，以尽量减少辐照引起的损伤。由于Xe离子等离子体FIB的铣削速率更高，现在常用于样品制备。然而，六方密排材料在Xe离子铣削过程中氢化物形成的严重程度尚不清楚。在本文中，我们比较了Xe和Ga FIB铣削在常温及低温下制备Zr样品的情况。通过研究TEM和APT样品，我们能够比较不同制备技术导致的FIB制备后氢化物形成水平。APT用于估计样品中的氢含量。这些结果对使用FIB制备从诸如锆等六方密排金属中制备TEM和APT样品的研究人员具有重要意义。
