Method of Ga removal from a specimen on a microelectromechanical system-based chip for in-situ transmission electron microscopy

Abstract

In-situ transmission electron microscopy (TEM) holders that employ a chip-type specimen stage have been widely utilized in recent years. The specimen on the microelectromechanical system (MEMS)-based chip is commonly prepared by focused ion beam (FIB) milling and ex-situ lift-out (EXLO). However, the FIB-milled thin-foil specimens are inevitably contaminated with Ga⁺ ions. When these specimens are heated for real time observation, the Ga⁺ ions influence the reaction or aggregate in the protection layer. An effective method of removing the Ga residue by Ar⁺ ion milling within FIB system was explored in this study. However, the Ga residue remained in the thin-foil specimen that was extracted by EXLO from the trench after the conduct of Ar⁺ ion milling. To address this drawback, the thin-foil specimen was attached to an FIB lift-out grid, subjected to Ar⁺ ion milling, and subsequently transferred to an MEMS-based chip by EXLO. The removal of the Ga residue was confirmed by energy dispersive spectroscopy.