Robust Local Thickness Estimation of Sub‐Micrometer Specimen by 4D‐STEM

Skoupý, Radim; Boltje, Daan B; Šlouf, Miroslav; Mrázová, Kateřina; Láznička, Tomáš; Taisne, Clémence M; Krzyžánek, Vladislav; Hoogenboom, Jacob P.; Jakobi, Arjen J.

doi:10.1002/smtd.202300258

Cited by 4 publications

References 36 publications

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Robust Preparation of Sub‐20‐nm‐Thin Lamellae for Aberration‐Corrected Electron Microscopy

Tsurusawa,

Uzuhashi,

Kozuka

et al. 2024

Small Methods

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Aberration‐corrected scanning transmission electron microscopy (STEM) has been advancing resolution, sensitivity, and microanalysis due to the intense demands of atomic‐level microstructural investigations. Recent STEM technologies require preparing a thin lamella whose thickness is ideally below 20 nm. Although focused‐ion‐beam/scanning‐electron‐microscopy (FIB/SEM) is an established method to prepare a high‐quality lamella, nanometer‐level controllability of lamella thickness remains a fundamental problem. Here, the robust preparation of a sub‐20‐nm‐thin lamella is demonstrated by FIB/SEM with real‐time feedback from thickness quantification. The lamella thickness is quantified by back‐scattered‐electron SEM imaging in a thickness range between 0 and 100 nm without any reference to numerical simulation. Using real‐time feedback from the thickness quantification, the FIB/SEM terminates thinning a lamella at a targeted thickness. The real‐time feedback system eventually provides 1‐nm‐level controllability of the lamella thickness. As a proof‐of‐concept, a near‐10‐nm‐thin lamella is prepared from a SrTiO3 crystal by our methodology. Moreover, the lamella thickness is controllable at a target heterointerface. Thus, a sub‐20‐nm‐thin lamella is prepared from a LaAlO3/SrTiO3 heterointerface. The methodology offers a robust and operator‐independent platform to prepare a sub‐20‐nm‐thin lamella from various materials. This platform will broadly impact aberration‐corrected STEM studies in materials science and the semiconductor industry.

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