Advanced preparation of plan-view specimens on a MEMS chip for in situ TEM heating experiments

Abstract

In situ transmission electron microscopy (TEM) is a powerful tool for advanced material characterization. It allows real-time observation of structural evolution at the atomic level while applying different stimuli such as heat. However, the validity of analysis strongly depends on the quality of the specimen, which has to be prepared by thinning the bulk material to electron transparency while maintaining the pristine properties. To address this challenge, a novel method of TEM samples preparation in plan-view geometry was elaborated based on the combination of the wedge polishing technique and an enhanced focused ion beam (FIB) workflow. It involves primary mechanical thinning of a broad sample area from the backside followed by FIB-assisted installation on the MEMS-based sample carrier. The complete step-by-step guide is provided, and the method’s concept is discussed in detail making it easy to follow and adapt for diverse equipment. The presented approach opens the world of in situ TEM heating experiments for a vast variety of fragile materials. The principle and significant advantage of the proposed method are demonstrated by new insights into the stability and thermal-induced strain relaxation of Ge Stranski–Krastanov islands on Si during in situ TEM heating. Graphical abstract: [Figure not available: see fulltext.]