The determination of trace free acid content in lithium-ion battery electrolytes by coulometric titration in non-aqueous media

Huang, Cairui; Shen, Congcong; Liu, Jin; Qu, Deyu; Hu, Xiaosong; Lin, Yaojun; Cai, Hongwei

doi:10.1039/c9an01539f

Cited by 5 publications

(4 citation statements)

References 19 publications

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“…The amount of the trace water inside the electrolyte was determined by a Karl Fischer moisture analyzer. A home‐developed coulometric titration method was used to determine the amount of HF 17 . Figure 1 shows the setup for HF titration.…”

Section: Methodsmentioning

confidence: 99%

“…A home-developed coulometric titration method was used to determine the amount of HF. 17 The measurements details were reported elsewhere. 17 A 0.5 M LiCl ethanol solution containing a trace amount of HF was pre-titrated to the end-point of pH 5.50, and then the electrolyte samples were accurately transferred into the pre-titrated solution.…”

Section: Determination Of Trace Water and Hydrofluoric Acid In Electr...mentioning

confidence: 99%

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The impact of a trace amount of water in an electrolyte on the performance of Li‐ion batteries—An empirical kinetic model approach

Liu

Cai

Liu

et al. 2022

Intl J of Energy Research

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Summary A spiral wound‐type lithium‐ion battery (LIB) was assembled with an NCM532 cathode, a graphite anode and an electrolyte containing 1 M LiPF6 in EC/DEC (1:1 by wt). Different amounts of trace water, from 100 to 900 ppm, were intentionally added into the electrolyte. After stabilizing, the water and the hydrofluoric acid contents in the electrolyte were determined with Karl Fischer titration and coulometric titration, respectively. The performance of the LIBs made with the electrolytes of different amounts of trace water was investigated and the effects of the trace water in the electrolyte were revealed. An empirical model was used in this study to calculate the LIBs capacity attenuation constant. By varying the temperature, the activation energy of capacity decay can also be obtained based on the Arrhenius equation. The results indicated that added trace water up to 900 ppm may not significantly harm the cyclic stability of LIBs at least around room temperature. The capacity fade for the cells with the addition of 300 ppm water was slower than those without water addition. The activation energy of capacity decay was also found to be higher as the contents of added trace water are in the range of 100‐400 ppm. This suggests a cost‐reducing process of LIBs manufacture in the moisture control respect. Novelty statement Different amounts of trace water were intentionally added into the electrolyte and variation of water as well as formed HF contents were determined by Karl Fischer titration and coulometric titration, respectively. The kinetic information of water reacted with LiPF6 was then obtained. After introducing those electrolytes into the LIB cells, the performances of those LIBs were investigated and the capacity attenuation constants and capacity decay activation energies upon those LIBs were calculated through a newly suggested empirical kinetic model.

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Section: Methodsmentioning

confidence: 99%

Section: Determination Of Trace Water and Hydrofluoric Acid In Electr...mentioning

confidence: 99%

The impact of a trace amount of water in an electrolyte on the performance of Li‐ion batteries—An empirical kinetic model approach

Liu

Cai

Liu

et al. 2022

Intl J of Energy Research

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“…65,66 In parallel, Coulometric titration was used to determine the slope of the open-circuit voltage vs K + concentration (x) relation at each x value (Figure 4C), which affords the K + diffusion values using Equation S2 (Figure 4D). 67 At the initial stage of K + intercalation, the entire slurry system showed high diffusion coefficients (∼10 −7 cm 2 /s). As K + association progressed, the diffusion rate gradually decreased (∼10 −11 cm 2 /s) owing to fewer vacant sites for potassium association.…”

mentioning

confidence: 95%

“…In this indigo slurry system, the K + diffusion kinetics were investigated using EIS. − By fitting the real impedance (Z′) and the square root of the angular frequency in the low-frequency region, the Warburg coefficient was obtained (Equation S1 and Figure S7). , In parallel, Coulometric titration was used to determine the slope of the open-circuit voltage vs K + concentration ( x ) relation at each x value (Figure C), which affords the K + diffusion values using Equation S2 (Figure D) . At the initial stage of K + intercalation, the entire slurry system showed high diffusion coefficients (∼10 –7 cm 2 /s).…”

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confidence: 99%

Insights into Indigo K⁺Association in a Half-Slurry Flow Battery

et al. 2022

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Potassium-ion batteries (PIBs) are promising energy storage devices owing to the abundance and low cost of potassium. However, the development of PIBs is still in its infancy owing to the poor kinetic diffusivity, limited capacity, and severe side reactions. It is imperative to explore new materials to address the issues of capacity, stability, and cycle life in PIBs. Here, we present a hybrid slurry/flow battery utilizing redox-active organic materials for K+ storage, wherein the indigo slurry serves as the anolyte and K4Fe(CN)6 solution serves as the catholyte. This battery presented a cycle life of 1000 cycles with a capacity of 18.4 Ah/L and capacity retention of ∼83%. Voltammetry measurements and density functional theory calculations indicated that the redox activity of indigo involves a one-step, double-electron process, instead of a two-step, single-electron process. This work provides new insights into the application of organic compounds as association materials for PIBs.

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Determination of base number in lubricants and additives by ASTM D2896: Substitution of chlorinated solvents and alternate electrolyte study

Dutta

Pathiparampil

Murella

et al. 2021

Fuel

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The determination of trace free acid content in lithium-ion battery electrolytes by coulometric titration in non-aqueous media

Abstract: A new quantitative analysis method was proposed, aiming at resolving the difficulty encountered in accurately determining the trace content of a free acid in lithium-ion battery electrolytes in the past 30 years.

Cited by 5 publications

References 19 publications

The impact of a trace amount of water in an electrolyte on the performance of Li‐ion batteries—An empirical kinetic model approach

The impact of a trace amount of water in an electrolyte on the performance of Li‐ion batteries—An empirical kinetic model approach

Insights into Indigo K⁺Association in a Half-Slurry Flow Battery

Determination of base number in lubricants and additives by ASTM D2896: Substitution of chlorinated solvents and alternate electrolyte study

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The determination of trace free acid content in lithium-ion battery electrolytes by coulometric titration in non-aqueous media

Abstract: A new quantitative analysis method was proposed, aiming at resolving the difficulty encountered in accurately determining the trace content of a free acid in lithium-ion battery electrolytes in the past 30 years.

Cited by 5 publications

References 19 publications

The impact of a trace amount of water in an electrolyte on the performance of Li‐ion batteries—An empirical kinetic model approach

The impact of a trace amount of water in an electrolyte on the performance of Li‐ion batteries—An empirical kinetic model approach

Insights into Indigo K+Association in a Half-Slurry Flow Battery

Determination of base number in lubricants and additives by ASTM D2896: Substitution of chlorinated solvents and alternate electrolyte study

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Product

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Insights into Indigo K⁺Association in a Half-Slurry Flow Battery