Sample preparation of energy materials for X-ray nanotomography with micromanipulation

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. It′s all in the prep: Novel sample preparation for X-ray nanotomography by using focused-ion-beam (FIB) and micromanipulation ensures high-quality data. The proposed procedure resolves the issues that cause the view of the sample base to be blocked after FIB milling and during the lift-out process. This method enables the broad application of X-ray nanotomography in microstructure studies.