Lithium Ion (Li-ion) batteries store energy and power billions of devices globally, so manufacturers face pressure to ensure high energy density while maintaining safety. Among a battery’s components, a thin separator material prevents physical contact between electrodes while directing ion transport within a cell. Both processes impact cell rate performance, cycle life, and safety [1]. Therefore, an in-depth understanding of separator structure is essential to improving batteries [2-4]. 2D and 3D electron microscopy (EM) effectively characterize separator structure; however, due to intrinsic beam sensitivity to most separators, care is needed to accurately characterize separator structure in its native state. Our work tested 2D scanning EM (SEM) and 3D DualBeamTM (Focused Ion Beam-Scanning Electron Microscope, FIB-SEM) imaging conditions to understand their effect on recovered separator structure.We investigated battery separator structure using a Thermo Scientific ApreoTM SEM and Thermo Scientific DualBeam systems equipped with CryoMAT. The SEM assisted with understanding surface-level electron beam damage in 2D and the DualBeam uncovered 3D structure using FIB milling. In the 2D case, we found the accelerating voltage could warp the separator. Low kV imaging is thus recommended to minimize structure damage.Additionally, in 2D SEM cross-section studies, sample preparation could affect separator structure. We tested an Al2O3-coated composite separator by FIB milling at three different temperatures (Figure 1). We found that cryogenic temperatures (-80° C; i.e., cryo-FIB) achieved the highest quality cross-section (Figure 1). FIB milling at either room temperature (25° C) or ultracold temperature (-180° C) both introduced defects on the microstructure.Finally, given the previous result, we collected 3D separator structure via cryo-FIB. With the 3D image stack, we used Thermo Scientific Avizo™ Software to recover structural parameters: open pore volume fraction, closed pore count and volume fraction, pore connectivity, tortuosity, and permeability. Such information should be useful for understanding battery separator performance. It is expected the strategies discussed in this talk will facilitate separator technology development.
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