X-ray nanotomography and focused-ion-beam sectioning for quantitative three-dimensional analysis of nanocomposites

Knowing the relationship between three-dimensional structure and properties is paramount for complete understanding of material behavior. In this work, the internal nanostructure of micrometer-size (10 μm) composite Ni/Al particles was analyzed using two different approaches. The first technique, synchrotron-based X-ray nanotomography, is a nondestructive method that can attain resolutions of tens of nanometers. The second is a destructive technique with sub-nanometer resolution utilizing scanning electron microscopy combined with an ion beam and 'slice and view' analysis, where the sample is repeatedly milled and imaged. The obtained results suggest that both techniques allow for an accurate characterization of the larger-scale structures, while differences exist in the characterization of the smallest features. Using the Monte Carlo method, the effective resolution of the X-ray nanotomography technique was determined to be 48 nm, while focused-ion-beam sectioning with 'slice and view' analysis was 5 nm.The X-ray nanotomography technique was compared with scanning electron microscopy for quantitative three-dimensional analysis of nanocomposite particles.