4.2 Article

Three-dimensional imaging of chemical phase transformations at the nanoscale with full-field transmission X-ray microscopy

Journal

JOURNAL OF SYNCHROTRON RADIATION
Volume 18, Issue -, Pages 773-781

Publisher

INT UNION CRYSTALLOGRAPHY
DOI: 10.1107/S0909049511019364

Keywords

X-ray microscopy; synchrotron X-ray imaging; Li-ion battery; XANES

Funding

  1. Assistant Secretary for Energy Efficiency and Renewable Energy (Office of Vehicle Technologies of the US Department of Energy) [DE-AC02-05CH11231]
  2. US Department of Energy (Office of Science, Office of Basic Energy Sciences) [DE-SC0001294]
  3. National Institutes of Health (NIH)/National Institute of Biomedical Imaging and Bioengineering (NIBIB) [5R01EB004321]
  4. Department of Energy, Office of Basic Energy Sciences

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The ability to probe morphology and phase distribution in complex systems at multiple length scales unravels the interplay of nano-and micrometer-scale factors at the origin of macroscopic behavior. While different electron-and X-ray-based imaging techniques can be combined with spectroscopy at high resolutions, owing to experimental time limitations the resulting fields of view are too small to be representative of a composite sample. Here a new X-ray imaging set-up is proposed, combining full-field transmission X-ray microscopy (TXM) with X-ray absorption near-edge structure (XANES) spectroscopy to follow two-dimensional and three-dimensional morphological and chemical changes in large volumes at high resolution (tens of nanometers). TXM XANES imaging offers chemical speciation at the nanoscale in thick samples (> 20 mu m) with minimal preparation requirements. Further, its high throughput allows the analysis of large areas (up to millimeters) in minutes to a few hours. Proof of concept is provided using battery electrodes, although its versatility will lead to impact in a number of diverse research fields.

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