Abstract

Aberration-corrected scanning transmission electron microscopy (STEM) is widely used for atomic-level imaging of materials but severely requires damage-free and thin samples (lamellae). So far, the preparation of the high-quality lamella from a bulk largely depends on manual processes by a skilled operator. This limits the throughput and repeatability of aberration-corrected STEM experiments. Here, inspired by the recent successes of “robot scientists”, we demonstrate robotic fabrication of high-quality lamellae by focused-ion-beam (FIB) with automation software. First, we show that the robotic FIB can prepare lamellae with a high success rate, where the FIB system automatically controls rough-milling, lift-out, and final-thinning processes. Then, we systematically optimized the FIB parameters of the final-thinning process for single crystal Si. The optimized Si lamellae were evaluated by aberration-corrected STEM, showing atomic-level images with 55 pm resolution and quantitative repeatability of the spatial resolution and lamella thickness. We also demonstrate robotic fabrication of high-quality lamellae of SrTiO3 and sapphire, suggesting that the robotic FIB system may be applicable for a wide range of materials. The throughput of the robotic fabrication was typically an hour per lamella. Our robotic FIB will pave the way for the operator-free, high-throughput, and repeatable fabrication of the high-quality lamellae for aberration-corrected STEM.

Highlights

  • Aberration-corrected scanning transmission electron microscopy (STEM) is widely used for atomiclevel imaging of materials but severely requires damage-free and thin samples

  • These results suggest that the robotic FIB system may be applicable for a wide range of materials

  • The automation software is a new version of AutoTEM 4, which was used in a pioneering work of a semi-automated FIB s­ ystem[30]

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Summary

Introduction

Aberration-corrected scanning transmission electron microscopy (STEM) is widely used for atomiclevel imaging of materials but severely requires damage-free and thin samples (lamellae). The preparation of the high-quality lamella from a bulk largely depends on manual processes by a skilled operator This limits the throughput and repeatability of aberration-corrected STEM experiments. Current methods to prepare such high-quality lamellae from bulk materials largely depend on manual processes and the knowledge of a skilled user These limit the throughput of the full workflow of aberration-corrected STEM experiments and suppress the repeatability of the sample quality and the resulting STEM images. One may suggest the automation of the FIB operation as an ideal solution to achieve the high throughput and repeatability of preparing high-quality lamellae The concept of such science automation (or robot scientists) has been widely demonstrated in b­ iology23,24, ­chemistry[25,26], and materials ­science[27,28,29], where a robotically-controlled system conducts a set of templated experiments without the attendance of a human operator. We aim to establish an operator-free, high-throughput, and repeatable method to fabricate high-quality STEM lamellae by a robotic FIB system

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