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X-Ray Nanotomography and Focused Ion Beam Sectioning
for Quantitative Three-dimensional Analysis of Nanocomposites


C. Shuck1, M. Frazee2, A. Gilman2, M. Beason3, I. Gunduz3, K. Matous2, R. Winarski4 and A. Mukasyan1

1Department of Chemical and Biomolecular Engineering
2Department of Aerospace and Mechanical Engineering
University of Notre Dame, Notre Dame, IN, 46556, USA.

3Department of Mechanical Engineering, Purdue University, West Lafayette, IN 47907, USA.

4Argonne National Laboratory, Center for Nanoscale Materials, Argonne, IL 60439, USA.


Abstract

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

Conclusions

   
    X-ray nanotomography is a new technique that offers significant benefits for characterization of a wide range of materials, including biological samples and inorganics. It fulfills a role for nondestructive 3D characterization of samples with high accuracy in a short period of time. The technique currently offers 11.8 nm pixel size of the optics, and ~48 nm effective pixel size after reconstruction, however there is room for increased resolution with equipment improvements. Overall, the ability of research groups to access synchrotron facilities is incredibly valuable; accurate, reliable characterization of nanomaterials is key to fundamental understanding and progress as a whole. However, because of the limitations of this technique, care must be taken to ensure that convergence of the data is reached, measured through rigorous statistical analysis.
  

Acknowledgments


    This work was supported by the Department of Energy, National Nuclear Security Administration, under Award Number DE-NA0002377 as part of the Predictive Science Academic Alliance Program II. Funding from the Defense Threat Reduction Agency (DTRA), Grant Number HDTRA1-10-1-0119. Counter-WMD basic research program, Dr. Suhithi M. Peiris, program director is also gratefully acknowledged. Funding from the National Defense Science and Engineering Graduate Fellowship is acknowledged. Use of the Center for Nanoscale Materials and the Advanced Photon Source, both Office of Science user facilities, was supported by the U.S. Department of Energy, Office of Science, Office of Basic Energy Sciences, under Contract No. DE-AC02-06CH11357.

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2016 Notre Dame and Dr. Karel Matous