The fundamental understanding of the electrode/electrolyte interfacial processes in Lithium/Sodium-ion Batteries (LIBs) and of their dynamics upon cycling is of prime importance for the development of new generation electrode materials. Operando analyses using the utmost sensitive techniques are required to produce an accurate depiction of the underlying processes at the origin of the battery performance decay. Although Raman spectroscopy is already largely used to characterize operating battery materials, it is totally blind to extract the composition of extremely thin layers such as SEI, as the Raman scattering process is in most scenario very inefficient. This can be solved using plasmonic amplifiers (Au@SiO2 core shell nanoparticles) deposited on the electrodes, the so-called SHINERS (Shell-Isolated Nanoparticles-Enhanced Raman Spectroscopy). Introduced by Tian’s group in 2010 [1], the SHINERS technique has yet been scarcely used for the characterization of energy materials. [2] [3] If enhanced Raman Spectroscopy through the use of signal nano-amplifiers (SHINs) shows the required sensitivity, its implementation in operando conditions and particularly on functional materials in contact with organic electrolytes remains challenging. This work through extensive optimization of SHINERS conditions for operando diagnosis of LIB materials, including the design of near-infrared active amplifiers and the control of the photon dose, demonstrates the possibility to track the dynamics of composition of the electrode/electrolyte interface upon cycling of LIB button-cells[4].This study while addressing three major gaps in analytical studies of interfacial processes in LIB electrolyte using enhanced Raman spectroscopy (ex situ and operando), i.e. the usual misconception of in situ cells or/and the inaccurate interpretation of SEI/CEI chemical signatures based on infrared spectra or computed Raman spectra (DFT), provides important insights in the degradation mechanism of organic carbonate electrolytes[5-6] and the origin of the interfacial instability specific to tin.[1] J. F. Li et al., “Shell-isolated nanoparticle-enhanced Raman spectroscopy”, Nature, 464 (2010) 392[2] L. Cabo-Fernandez, D. Bresser, F. Braga, S. Passerini, et L. J. Hardwick, “In-Situ Electrochemical SHINERS Investigation of SEI Composition on Carbon-Coated Zn 0.9 Fe 0.1 O Anode for Lithium-Ion Batteries “, Batteries & Supercaps, 2 (2019) 168[3] C.-Y. Li et al., “Surface Changes of LiNix Mny Co1– x – yO2 in Li-Ion Batteries Using in Situ Surface-Enhanced Raman Spectroscopy “, J. Phys. Chem. C, 124 (2020) 4024[4] Gajan, A. et al .; Lecourt, C.; Bautista, B. E. T.; Fillaud, L.; Demeaux, J.; Lucas, I. T. “Solid Electrolyte Interphase Instability in Operating Lithium-Ion Batteries Unraveled by Enhanced-Raman Spectroscopy”. ACS Energy Letters 2021, 7.[5] L. Wang et al., « Identifying the components of the solid–electrolyte interphase in Li-ion batteries », Nat. Chem., 11 (2019) 789[6] S. A. Freunberger, « Interphase identity crisis », Nat. Chem., 11 (2019) 7...
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