Carbonate Solvent Systems Used in Lithium-Ion Batteries

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Carbonate Solvent Systems Used in Lithium-Ion Batteries ( carbonate-solvent-systems-used-lithium-ion-batteries )

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energies Article Determining the Composition of Carbonate Solvent Systems Used in Lithium-Ion Batteries without Salt Removal Mohammad Parhizi 1, Louis Edwards Caceres-Martinez 1 , Brent A. Modereger 2, Hilkka I. Kenttämaa 2, Gozdem Kilaz 1,* and Jason K. Ostanek 1,* 􏰁􏰂􏰃 􏰅􏰆􏰇 􏰈􏰉􏰊􏰋􏰌􏰂􏰍 Citation: Parhizi, M.; Caceres-Martinez, L.E.; Modereger, B.A.; Kenttämaa, H.I.; Kilaz, G.; Ostanek, J.K. Determining the Composition of Carbonate Solvent Systems Used in Lithium-Ion Batteries without Salt Removal. Energies 2022, 15, 2805. https://doi.org/10.3390/en15082805 Academic Editors: Alon Kuperman and Alessandro Lampasi Received: 7 March 2022 Accepted: 4 April 2022 Published: 12 April 2022 1 2 * Correspondence: gkilaz@purdue.edu (G.K.); jostanek@purdue.edu (J.K.O.) Abstract: In this work, two methods were investigated for determining the composition of carbon- ate solvent systems used in lithium-ion (Li-ion) battery electrolytes. One method was based on comprehensive two-dimensional gas chromatography with electron ionization time-of-flight mass spectrometry (GC×GC/EI TOF MS), which often enables unknown compound identification by their electron ionization (EI) mass spectra. The other method was based on comprehensive two- dimensional gas chromatography with flame ionization detection (GC×GC/FID). Both methods were used to determine the concentrations of six different commonly used carbonates in Li-ion battery electrolytes (i.e., ethylene carbonate (EC), propylene carbonate (PC), dimethyl carbonate (DMC), diethyl carbonate (DEC), ethyl methyl carbonate (EMC), and vinylene carbonate (VC) in model compound mixtures (MCMs), single-blind samples (SBS), and a commercially obtained electrolyte solution (COES). Both methods were found to be precise (uncertainty < 5%), accurate (error < 5%), and sensitive (limit of detection <0.12 ppm for FID and <2.7 ppm for MS). Furthermore, unlike the previously reported methods, these methods do not require removing lithium hexafluorophosphate salt (LiPF6) from the sample prior to analysis. Removal of the lithium salt was avoided by diluting the electrolyte solutions prior to analysis (1000-fold dilution) and using minimal sample volumes (0.1 μL) for analysis. Keywords: lithium-ion batteries; electrolyte; two-dimensional gas chromatography (GC×GC); mass spectrometry (MS); flame ionization detector (FID); analytical techniques 1. Introduction Lithium-ion (Li-ion) batteries are the predominant energy storage and conversion device in various applications, such as portable consumer electronics, electric vehicles (EVs), grid storage, space applications, and military applications [1–3]. Li-ion batteries offer several advantages over other rechargeable batteries, such as high energy density and power density, low self-discharge rate, and long life [4]. However, decomposition reactions occur within Li-ion batteries under certain operating conditions, which negatively impact the performance of the battery and impose safety hazards by generating toxic and flammable compounds. For instance, under abuse conditions, decomposition reactions generate a significant amount of heat and gaseous products, leading the cell into thermal runaway. Thermal runaway is frequently accompanied by the release of flammable and toxic gases during the venting process and afterward. The rates and pathways of these decomposition reactions, the composition and amount of the gaseous products, and heat generation rates are affected by the solvent(s) used within the electrolyte solution, which can vary significantly [5]. The most common electrolytes used in Li-ion batteries comprise a conducting salt such as lithium hexafluorophosphate (LiPF6) dissolved in a mixture of organic carbonate solvents. School of Engineering Technology, Purdue University, 401 N. Grant St., West Lafayette, IN 47907, USA; mparhizi@purdue.edu (M.P.); lcaceres@purdue.edu (L.E.C.-M.) Department of Chemistry, Purdue University, 560 Oval Dr., West Lafayette, IN 47907, USA; bmodereg@purdue.edu (B.A.M.); hilkka@purdue.edu (H.I.K.) Publisher’s Note: MDPI stays neutral with regard to jurisdictional claims in published maps and institutional affil- iations. Copyright: © 2022 by the authors. Licensee MDPI, Basel, Switzerland. This article is an open access article distributed under the terms and conditions of the Creative Commons Attribution (CC BY) license (https:// creativecommons.org/licenses/by/ 4.0/). Energies 2022, 15, 2805. https://doi.org/10.3390/en15082805 https://www.mdpi.com/journal/energies

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