Sample Preparation of Energy Materials for X-ray Nanotomography with Micromanipulation

Authors

  • Dr. Yu-chen Karen Chen-Wiegart,

    1. Photon Sciences Directorate, Brookhaven National Laboratory, Upton, New York, 11973 (USA), Fax: (+1) 631 344 3238
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  • Dr. Fernando E. Camino,

    1. Center for Functional Nanomaterials, Brookhaven National Laboratory, Upton, New York 11973 (USA)
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  • Dr. Jun Wang

    Corresponding author
    1. Photon Sciences Directorate, Brookhaven National Laboratory, Upton, New York, 11973 (USA), Fax: (+1) 631 344 3238
    • Photon Sciences Directorate, Brookhaven National Laboratory, Upton, New York, 11973 (USA), Fax: (+1) 631 344 3238===

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Abstract

X-ray nanotomography presents an unprecedented opportunity to study energy storage/conversion materials at nanometer scales in three dimensions, with both elemental and chemical sensitivity. A critical step in obtaining high-quality X-ray nanotomography data is reliable sample preparation to ensure that the entire sample fits within the field of view of the X-ray microscope. Although focused-ion-beam lift-out has previously been used for large sample (few to tens of microns) preparation, a difficult undercut and lift-out procedure results in a time-consuming sample preparation process. Herein, we propose a much simpler and direct sample preparation method to resolve the issues that block the view of the sample base after milling and during the lift-out process. This method is applied on a solid-oxide fuel cell and a lithium-ion battery electrode, before numerous critical 3D morphological parameters are extracted, which are highly relevant to their electrochemical performance. A broad application of this method for microstructure study with X-ray nanotomography is discussed and presented.

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