32
H. Kaur et al.
Fig. 18 In-situ ATR-FTIR spectra of lithiated silicon electrodes acquired after applying 5 mV
potential (spectra collected after applying potential for 1 h) with variation in incidence angle from
40 ◦ –65 ◦ . Adapted with permission from [16]. Copyright, 2017, American Chemical Society
provides the flexibility of retrieving SEI information under different conditions of
potential and cyclability of the electrolyte to understand its surface mechanism. In this
complete study, the retrieved results with in-situ ATR-FTIR showed DEDOHC as the
major SEI product on native silicon oxide film during the initial cycling process that
contributes towards the capacity losses. While for long-term cycling, LIEDC came
out as a potential reduction product on the lithiated silicon electrode that participated
in the passivation process over the cracked surfaces (after consuming electrons).
Thus, these studies [16] successfully achieved the SEI product information during
cyclic lithiation/de-lithiation as verified by cyclic voltammograms (CV) and showed
the enormous ability of ATR-FTIR spectroscopy as a technique to elucidate the
detailed molecular-level information in tracing out the surface mechanism within
various electrochemical devices.
Kollath et al. [98] focused on improving the silicon electrode electrochemical
performance by probing the physicochemical properties of a binder polymer in
contact with the silicon electrode by using ex-situ ATR-FTIR spectroscopy. This
study was further verified and conducted with the analysis of XAS, AFM, and TGA to
evaluate the performance of LIBs. The authors used poly(1-pyrenemethyl methacrylate) (PPy) as a binder due to a dual conductive-additive functionality of this polymer
to preserve the mechanical integrity of composite electrodes. The powdered PPys
immersed in the electrolyte solution (1.2 M LiPF6, EC: DC: fluorinated carbonate
(FEC) in the ratio 2.1:4.9:3 v/v) for 24 h, filtered, washed with DMC and dried for 24 h
in the glove box. The obtained FTIR spectra (Fig. 19, panel a) of PPy exposed to the
electrolyte, suggested no chemical degradation of PPy in the electrolyte and include
1775 and 1810 cm
−1 attributed to solvent trapped in the PPy structure. The molecular
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