A flexible method for the preparation of thin film samples for in situ TEM characterization combining shadow-FIB milling and electron-beam-assisted etching

• Published in: Ultramicroscopy 2016-12, Vol.171, p.82-88
• Main Authors: Liebig, J.P., Göken, M., Richter, G., Mačković, M., Przybilla, T., Spiecker, E., Pierron, O.N., Merle, B.
• Format: Article
• Language: English
• Subjects: Electron microscopes; Electron-beam-assisted etching; Etching; FIB; Ion beams; Mechanical testing; Micromechanical testing; Microstructure; Preserves; Thin films; Transmission electron microscopy; XeF2
• ISSN: 0304-3991; 1879-2723
• DOI: 10.1016/j.ultramic.2016.09.004

A new method for the preparation of freestanding thin film samples for mechanical testing in transmission electron microscopes is presented. It is based on a combination of focused ion beam (FIB) milling and electron-beam-assisted etching with xenon difluoride (XeF2) precursor gas. The use of the FIB allows for the target preparation of microstructural defects and enables well-defined sample geometries which can be easily adapted in order to meet the requirements of various testing setups. In contrast to existing FIB-based preparation approaches, the area of interest is never exposed to ion beam irradiation which preserves a pristine microstructure. The method can be applied to a wide range of thin film material systems compatible with XeF2 etching. Its feasibility is demonstrated for gold and alloyed copper thin films and its practical application is discussed. •A new method for the preparation of sub-micron tensile specimens from thin films is presented.•The method is based on the combination of focused ion beam milling and electron-beam-assisted xenon difluoride etching.•It enables the target preparation of individual microstructural defects.•The sample section is protected from ion beam damage by the use of a shadow milling geometry.