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Sample Preparation of Energy Materials for X‐ray Nanotomography with Micromanipulation
Author(s) -
ChenWiegart Yuchen Karen,
Camino Fernando E.,
Wang Jun
Publication year - 2014
Publication title -
chemphyschem
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 1.016
H-Index - 140
eISSN - 1439-7641
pISSN - 1439-4235
DOI - 10.1002/cphc.201400023
Subject(s) - sample preparation , focused ion beam , materials science , undercut , sample (material) , nanotechnology , nanometre , analytical chemistry (journal) , ion , chemistry , composite material , chromatography , organic chemistry
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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