Abstract
We present FIB/SEM tomography combined with an optimized embedding procedure and osmium tetroxide staining to trace and visualize the initial self-conditioning step as well as degradation processes of [5,15-bis(ethynyl)-10,20-diphenylporphinato]copper(II) (CuDEPP) composite electrodes for the first time. Staining with osmium tetroxide allowed visualizing chemical changes of the active CuDEPP material. Four composite electrode samples prior and after cycling with different cycle numbers in LiPF6 electrolyte (i.e., pristine, one, 200 and 2000 charging cycles) were investigated and for all samples 3D reconstructions with a voxel size of 7.15 × 7.15 × 20 nm3 were performed. The samples were further analyzed by wavelength-dispersive X-ray (WDX) spectroscopy revealing the insertion of the electrolyte into the active material of the electrode. The formation of an interphase adjacent to the inner pore space of the active CuDEPP material could be unambiguously identified. In addition, Raman spectroscopy results confirmed the self-conditioning and degradation processes of the metalloporphyrin complex.
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