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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
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