Focused ion beam preparation of samples for X-ray nanotomography

• Published in: Journal of synchrotron radiation 2012-09, Vol.19 (5), p.789-796
• Main Authors: Lombardo, Jeffrey J., Ristau, Roger A., Harris, William M., Chiu, Wilson K. S.
• Format: Article
• Language: English
• Subjects: Beams (radiation); focused ion beam; Ion beams; Ions; Microscopy, Electron, Scanning - methods; Nanocomposites; Nanomaterials; Nanostructure; Particle Size; sample preparation; Scanning electron microscopy; solid-oxide fuel cell; Specimen Handling - methods; Tomography, X-Ray - methods; Tortuosity; X-ray nanotomography; X-Rays
• ISSN: 1600-5775; 0909-0495; 1600-5775
• DOI: 10.1107/S0909049512027252

The preparation of hard material samples with the necessary size and shape is critical to successful material analysis. X‐ray nanotomography requires that samples are sufficiently thin for X‐rays to pass through the sample during rotation for tomography. One method for producing samples that fit the criteria for X‐ray nanotomography is focused ion beam/scanning electron microscopy (FIB/SEM) which uses a focused beam of ions to selectively mill around a region of interest and then utilizes a micromanipulator to remove the milled‐out sample from the bulk material and mount it on a sample holder. In this article the process for preparing X‐ray nanotomography samples in multiple shapes and sizes is discussed. Additionally, solid‐oxide fuel cell anode samples prepared through the FIB/SEM technique underwent volume‐independence studies for multiple properties such as volume fraction, average particle size, tortuosity and contiguity to observe the characteristics of FIB/SEM samples in X‐ray nanotomography.