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Visualization of Li Profile in an All-Solid-State Li-Ion Battery By In Situ Electron Holography and Spatially-Resolved Eels
Figure 1(a) shows a schematic of our battery model sample. The Li2O-Al2O3-TiO2-P2O5-based glass-ceramics sheet (LATP) was used as the solid electrolyte, and the LiCoO2 positive electrode was deposited on one side. The negative electrode was prepared in situ by Li insertion reaction to the negative side LATP [2].
After 50 CV cycles, the negative side region was lifted out by a focused ion beam method and the TEM sample was prepared. The TEM image (Fig. 1(b)) shows a slightly different contrast around the interface. Fig. 1(c) shows the Li spectrum image detected by SR-EELS, the horizontal and vertical axes correspond to the electron energy loss and the sample position of the Fig. 1(b) in the vertical direction, respectively. The Li profile (Fig. 1(d)) was similar to the potential profile (Fig. 1(e)). Therefore, the EH detects the nanometer scale potential change due to the Li insertion reaction. The electronic structure changes of the other important elements (Ti and O) due to the Li insertion will be discussed in this presentation.
This work was supported by the RISING project of the New Energy and Industrial Technology Development Organization (NEDO) in Japan.
[1] K. Yamamoto et al., Angew. Chem. Int. Ed. 49 (2010) 4414 - 4417.
[2] Y. Iriyama et al., Electrochem. Commun. 8 (2006) 1287-1291.