Cryo-FIB for TEM Investigation of Soft Matter and Beam Sensitive Energy Materials

Journal Article · Tue Oct 04 00:00:00 EDT 2022 · Nanotechnology

DOI:https://doi.org/10.1088/1361-6528/ac92eb· OSTI ID:2426774

Long, Daniel M. ^[1]; Singh, Manish Kumar ^[2]; Small, Kathryn ^[3]; Watt, John Daniel ^[2]

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1. Air Force Research Lab. (AFRL), Wright-Patterson AFB, OH (United States); UES Inc., Beavercreek, OH (United States); Sandia National Lab. (SNL-NM), Albuquerque, NM (United States)
2. Los Alamos National Laboratory (LANL), Los Alamos, NM (United States)
3. Sandia National Lab. (SNL-NM), Albuquerque, NM (United States)

Primarily driven by structural biology, the rapid advances in cryogenic electron microscopy techniques are now being adopted and applied by materials scientists. Samples that inherently have electron transparency can be rapidly frozen (vitrified) in amorphous ice and imaged directly on a cryogenic transmission electron microscopy (cryo-TEM), however this is not the case for many important materials systems, which can consist of layered structures, embedded architectures, or be contained within a device. Cryogenic focused ion beam (cryo-FIB) lift-out procedures have recently been developed to extract intact regions and interfaces of interest, that can then be thinned to electron transparency and transferred to the cryo-TEM for characterization. Several detailed studies have been reported demonstrating the cryo-FIB lift-out procedure, however due to its relative infancy in materials science improvements are still required to ensure the technique becomes more accessible and routinely successful. Here, we review recent results on the preparation of cryo-TEM lamellae using cryo-FIB and show that the technique is broadly applicable to a range of soft matter and beam sensitive energy materials. We then present a tutorial that can guide the materials scientist through the cryo-FIB lift-out process, highlighting recent methodological advances that address the most common failure points of the technique, such as needle attachment, lift-out and transfer, and final thinning.

• Research Organization: Los Alamos National Laboratory (LANL), Los Alamos, NM (United States)
• Sponsoring Organization: USDOE National Nuclear Security Administration (NNSA); USDOE Office of Science (SC). Office of Basic Energy Sciences (BES)
• Grant/Contract Number: 89233218CNA000001; NA0003525
• OSTI ID: 2426774
• Report Number(s): LA-UR--22-26472
• Journal Information: Nanotechnology, Journal Name: Nanotechnology Journal Issue: 50 Vol. 33; ISSN 1361-6528; ISSN 0957-4484
• Publisher: IOP Publishing
• Country of Publication: United States
• Language: English

Related Subjects

36 MATERIALS SCIENCE
cryo-FIB
cryogenic electron microscopy
cryogenic focused ion beam lift-out
low-Z energy materials
soft matter