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. 2016 Oct 17:6:35291.
doi: 10.1038/srep35291.

Exploring 3D microstructural evolution in Li-Sulfur battery electrodes using in-situ X-ray tomography

Assiya Yermukhambetova  1   2 , Chun Tan  1 , Sohrab R Daemi  1 , Zhumabay Bakenov  2   3 , Jawwad A Darr  4 , Daniel J L Brett  1 , Paul R Shearing  1
Affiliations

Exploring 3D microstructural evolution in Li-Sulfur battery electrodes using in-situ X-ray tomography

Assiya Yermukhambetova et al. Sci Rep. .

Abstract

Lithium sulfur (Li-S) batteries offer higher theoretical specific capacity, lower cost and enhanced safety compared to current Li-ion battery technology. However, the multiple reactions and phase changes in the sulfur conversion cathode result in highly complex phenomena that significantly impact cycling life. For the first time to the authors' knowledge, a multi-scale 3D in-situ tomography approach is used to characterize morphological parameters and track microstructural evolution of the sulfur cathode across multiple charge cycles. Here we show the uneven distribution of the sulfur phase fraction within the electrode thickness as a function of charge cycles, suggesting significant mass transport limitations within thick-film sulfur cathodes. Furthermore, we report a shift towards larger particle sizes and a decrease in volume specific surface area with cycling, suggesting sulfur agglomeration. Finally, we demonstrate the nano-scopic length-scale required for the features of the carbon binder domain to become discernible, confirming the need for future work on in-situ nano-tomography. We anticipate that X-ray tomography will be a powerful tool for optimization of electrode structures for Li-S batteries.

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Figures

Figure 1
Figure 1
(a) Charge/discharge profile of the S-composite cathode tomography cell after 1, 2 and 10 cycles, (b) variation of discharge capacity for the electrochemical test cell and in-situ tomography cell with cycling at 0.15 mA cm−2.
Figure 2
Figure 2
From top left (a,b,c) 2D virtual slices from tomography images of Li-S cell before and after cycling for 2 and 10 cycles at 0.15 mA cm−2. (d) Combined image of same virtual slice across different cycles. Scale bar represents 50 μm.
Figure 3
Figure 3
Volume rendering of the sulfur phase for (a) the uncycled cathode and (b) the cathode after 10 cycles. Scale bar represents 50 μm.
Figure 4
Figure 4. Particle size distribution of sulfur particles before and after cycling for 2 and 10 cycles.
Percentage of particles is shown on log scale to enhance visualization of trends in larger particles with comparatively small percentages.
Figure 5
Figure 5. Volume specific surface area (VSSA) distribution of sulfur particles before and after cycling for 2 and 10 cycles.
Smaller VSSA values correspond to larger particle sizes as the surface area to volume ratio decreases with increasing volume.
Figure 6
Figure 6. Sulfur phase fraction as a function of thickness of the electrode where 0 μm represents the current collector position.
Figure 7
Figure 7
left (a) X-ray Zernike phase contrast nano-CT on S-composite used, carbon binder domain indicated by the white arrow; right (b) volume rendering of segmented sulfur particles. Scale bars represent 10 μm.
See this image and copyright information in PMC

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