In situ FTIR study of the Cu electrode/ethylene carbonate+dimethyl carbonate solution interface

Ikezawa, Yasunari; Nishi, Hironori

doi:10.1016/j.electacta.2007.12.038

Cited by 58 publications

(42 citation statements)

References 27 publications

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“…During delithiation, the initial amount of free and solvating PC species is gradually recovered. Such changes in concentration are much more obviously evidenced here than in the previous in situ FTIR studies, because the present ATR geometry does not introduce mass transport limitations like in the thin‐electrolyte‐layer cells used previously . Since the lithium‐ion concentration increases close to the electrode surface during electrochemical cycling, mass transfer in the electrolyte is not the critical step in silicon lithiation.…”

Section: Resultsmentioning

confidence: 53%

“…From the point of view of ex situ characterization techniques such as X‐ray photoelectron spectroscopy (XPS), FTIR, and Raman spectroscopies, the solid‐electrolyte interphase appears as a solid layer created from insoluble decomposition products of reactions between electrode and electrolyte. These techniques are blind to the part played by the in situ chemical environment on the structure of the SEI, especially the role of the solvent in its vicinity, which is suggested by the first in situ FTIR observations . In situ characterization techniques allow the analysis of the electrode processes to be performed without modifying its natural environment, resulting in an unbiased perception of the SEI layer .…”

Section: Introductionmentioning

confidence: 99%

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Spectroscopic Insight into Li‐Ion Batteries during Operation: An Alternative Infrared Approach

Corte

Caillon

Jordy

et al. 2015

Advanced Energy Materials

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special environment for its characterization appear as steps which in most cases might strongly modify the active material. [ 1 ] Benefi ting from characterization techniques able to analyze the electrodes in situ and in operando therefore appears of uttermost importance for obtaining information of direct relevance regarding the electrode processes. We show in the present work that such pieces of information can be obtained by using in situ Fourier-transform infrared (FTIR) spectroscopy in a suitable geometry, which avoids the traditional limitations associated with this technique and allows for quantitative information to be extracted. [ 2 ] This approach therefore brings significant complementary information to other useful techniques operating in the electrochemical environment, which focus either on electrode materials, such as nuclear magnetic resonance (NMR) [ 3,4 ] or X-ray absorption, diffraction or imaging, [ 5,6 ] or on electrode surfaces, such as scanning probe microscopies. [ 7,8 ] Using infrared spectroscopy at the electrochemical interface has already been attempted in the context of the study of battery electrodes. [9][10][11] The geometry adopted for these studies was however severely limiting the sensitivity, and imposing stringent limitations for the electrochemical conditions (especially in terms of mass-transport limitations), which have direct impact on the obtained results. [ 12 ] Here, we use an alternative approach based on the multiple-internal-refl ection geometry, which allows for benefi ting from an enhanced sensitivity and working in electrochemical conditions similar to those of standard batteries for studying thin-fi lm electrodes. As shown hereafter, such a capability provides useful information of direct relevance for both interfacial and bulk electrode processes.The present study has been devoted to silicon electrodes, studied in a half-cell confi guration against a lithium-metal electrode. Silicon represents an impressive gain in energy density for negative electrodes in Li-ion batteries. One strategy to overcome the poor capacity retention associated with the massive volume expansion of silicon during lithiation is the use of nanosized geometries, for instance, particles, [13][14][15][16] wires, [17][18][19] and tubes. [ 20,21 ] The use of a thin-fi lm geometry also prevents Multiple-internal-refl ection infrared spectroscopy allows for the study of thin-fi lm amorphous silicon electrodes in situ and in operando, in conditions typical of those used in Li-ion batteries. It brings an enhanced sensitivity, and the attenuated-total-refl ection geometry allows for the extraction of quantitative information. When electrodes are cycled in representative electrolytes, the simultaneously recorded infrared spectra give an insight into the solid/electrolyte interphase (SEI) composition. They also unravel the dynamic behavior of this SEI layer by quantitatively assessing its thickness, which increases during silicon lithiation and partially decreases during delithiation. Li-ion solvation ...

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Section: Resultsmentioning

confidence: 53%

Section: Introductionmentioning

confidence: 99%

Spectroscopic Insight into Li‐Ion Batteries during Operation: An Alternative Infrared Approach

Corte

Caillon

Jordy

et al. 2015

Advanced Energy Materials

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“…The FTIR spectra of samples 2 to 6 were similar,b ut showed some differences compared with that of Celb,i ncluding the appearance of intense bands at 1650 and 1410 cm À1 ,i na greement with the presence of carbonate groups. [30][31][32][33][34] The presence of the carbonate functional group is confirmedb yt he weak 825-720 and 685-650cm À1 bending bands of carbonates out of plane and in plane,r espectively. [35] The decrease in the strength of the bandsa t3 400, 1290, and 1060 cm À1 ,c orresponding to OÀHa nd CÀOH bonds, respectively,c onfirmed the decrease of OÀHf unctions.…”

Section: Resultsmentioning

confidence: 99%

A New Way to Produce Cellobiose Carbonates Using Green Chemistry

et al. 2016

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The preparation of cellulose derivatives using green (i.e., environmentally friendly) reagents would improve sustainability and reduce concerns arising from the use of non-green reagents. The objective of this work was to prepare cellobiose carbonate using a green reagent, dimethyl carbonate. The carbonation reaction was carried out in the presence of ethanolic potassium hydroxide solution and dimethyl carbonate for 6 h at a range of temperatures (25-70 °C). A cellobiose derivative was successfully prepared with a recovered yield of more than 70 % and characterized by FTIR and NMR spectroscopy techniques. The presence of a grafted disaccharide with a degree of substitution higher than 2 was determined by (13) C NMR analysis. The spectra of the prepared cellobiose carbonate exhibited peaks that were associated with cellulose molecules (C1 -C6 ) and corresponded to carbonate functions at around 159.4 ppm.

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“…The main peaks corresponding to EC molecular at 1480, 1391, 1161, and 1070 cm −1 were assigned to the scissoring and wagging vibrations of CH 2 , and the stretching vibration of CO. The 1774 cm −1 peak was attributed to CO stretching, and the 1800 cm −1 peak to the overtone of the ring breathing mode in EC 38. The peaks corresponding to DMC at 1751, 1454, and 1282 cm −1 were assigned to the CO stretching vibration, CH 3 scissoring vibrations, and CO stretching vibration, respectively.…”

Section: Resultsmentioning

confidence: 99%

Electrospun poly(lithium 2‐acrylamido‐2‐methylpropanesulfonic acid) fiber‐based polymer electrolytes for lithium‐ion batteries

Cui

Tang

2012

J of Applied Polymer Sci

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Novel single-ion conducting polymer electrolytes based on electrospun poly(lithium 2-acrylamido-2methylpropanesulfonic acid) (PAMPSLi) membranes were prepared for lithium-ion batteries. The preparation started with the synthesis of polymeric lithium salt PAMPSLi by free-radical polymerization of 2-acrylamido-2-methylpropanesulfonic acid, followed by ion-exchange of H þ with Li þ . Then, the electrospun PAMPSLi membranes were prepared by electrospinning technology, and the resultant PAMPSLi fiber-based polymer electrolytes were fabricated by immersing the electrospun membranes into a plasticizer composed of ethylene carbonate and dimethyl carbonate. PAMPSLi exhibited high thermal stability and its decomposition did not occur until 304 C. The specific sur-face area of the electrospun PAMPSLi membranes was raised from 9.9 m 2 /g to 19.5 m 2 /g by varying the solvent composition of polymer solutions. The ionic conductivity of the resultant PAMPSLi fiber-based polymer electrolytes at 20 C increased from 0.815 Â 10 À5 S/cm to 2.12 Â 10 À5 S/cm with the increase of the specific surface area. The polymer electrolytes exhibited good dimensional stability and electrochemical stability up to 4.4 V vs. Li þ /Li. These results show that the PAMPSLi fiber-based polymer electrolytes are promising materials for lithium-ion batteries.

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In situ FTIR study of the Cu electrode/ethylene carbonate+dimethyl carbonate solution interface

Cited by 58 publications

References 27 publications

Spectroscopic Insight into Li‐Ion Batteries during Operation: An Alternative Infrared Approach

Spectroscopic Insight into Li‐Ion Batteries during Operation: An Alternative Infrared Approach

A New Way to Produce Cellobiose Carbonates Using Green Chemistry

Electrospun poly(lithium 2‐acrylamido‐2‐methylpropanesulfonic acid) fiber‐based polymer electrolytes for lithium‐ion batteries

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