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

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. One-nanometer-level thickness controllability in preparing sub-20-nm-thin lamellae for aberration-corrected STEM investigations is demonstrated. FIB/SEM quantifies the lamella thickness between 0 and 100 nm by back-scattered-electron SEM imaging. The thickness quantification provides real-time feedback on the autonomous termination of an FIB thinning process. Our methodology offers robust and operator-independent preparation of thin lamellae from various materials, including heterostructural materials. image