In situ FIB-SEM characterization and manipulation methods
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Introduction Tools and their functionality often evolve through fusion of simpler instruments. Within the scope of nanotechnology, an evolution has resulted in the focused ion beam-scanning electron microscope (FIB-SEM) instrument. Gallium-based FIB systems, as we know them today, were developed in the 1980s and were quickly adopted by the semiconductor industry as a tool for analysis, repair of masks, and integrated circuit edit.1,2 In the 1990s, FIB and SEM columns were combined to form the two beam platform.3 With further integration of a variety of detectors, a nano-manipulator and a temperature-controlled stage, FIB-SEMs became multifunctional tools that provide a myriad of unique characterization, fabrication, and sample preparation capabilities. Here, we review recent developments and applications of FIB-SEMs for in situ characterization and manipulation of material at the micro- and nanoscale. In these applications, the sample may be mechanically or electrically excited, have material subtracted or added via ion milling or ion beam-induced deposition (IBID) or electron beam-induced deposition (EBID),4 and have its temperature varied from above room temperature to cryogenic levels. Sample manipulation using nano-/microscale probes, which is often necessary to arrange the samples for their analysis or to construct a system, is a common theme across the reviewed FIB-SEM uses.3 Mechanical, electrical, and/or thermal contacts
between the nano-manipulators and the nano-/microscale objects of interest consist of localized welds made using EBID or IBID of carbon, metal,4 electron-curable polymeric glues,5 and, at cryogenic temperatures, ice deposition.6 Mechanical handling can also be achieved without any deposition through use of micro-grippers7 and, in some cases, just physical contact.8 This article describes the current state of the art of this experimental methodology, provides case studies in the areas of mechanical, electrical, and cryogenic characterization, and provides an outlook for new opportunities for in situ characterization and manipulation using FIB-SEMs.
Mechanical testing Over the past decade, there has been tremendous growth in the use of two beam instruments to advance in situ mechanical test methodologies that operate on samples with micro- or nanometer scale dimensions. Characterization of the mechanical properties of a material at this scale is important because the deformation mechanisms are strongly affected by the sample dimensions. For this, FIB-SEMs are used in many aspects of the experiments, including preparation of the micromechanical test samples from bulk material,9–11 transfer of the samples into the mechanical actuation device,12 observing the sample deformation with the SEM,13–15 characterization of local lattice rotation during the test,16,17 preparation of TEM lamellae for
Nicholas Antoniou, Center for Nanoscale Systems, Harvard University; [email protected] Konrad Rykaczewski, School for Engineering of Matter, Transport, and Energy, Arizona State University; kon
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