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.
Highlights
In-situ transmission electron microscopy (TEM), an analytical technique that allows the real-time observation of the microstructural evolution induced by external stimuli such as heating, electrical biasing, and mechanical deformation, is an important current research topic
The two specimens were thermally treated under identical conditions, focused ion beam (FIB) milling of the latter thin-foil specimen resulted in the accumulation of the Ga residue that affected the silicide reaction
Ar+ ion milling in the FIB system was utilized in this study for the necessary removal of the Ga residue
Summary
In-situ transmission electron microscopy (TEM), an analytical technique that allows the real-time observation of the microstructural evolution induced by external stimuli such as heating, electrical biasing, and mechanical deformation, is an important current research topic. There has been a recent increase in the use of microelectromechanical system (MEMS)-based chips for in-situ TEM experiments; the preparation of the specimens for these experiments has become challenging. The aforementioned limitations can be overcome by preparing the MEMS-based chip specimens by ex-situ lift-out (EXLO) of the FIB-milled lamellae. EXLO was the first lift-out technique to be implemented for FIBmilled specimens and has been applied to various material systems (Heringer et al 1996; Giannuzzi et al 1997). It is a simple, fast technique that takes less than 5 min to manipulate a specimen for analysis
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