Electrolyte Solvation and Ionic Association: Part IX. Structures and Raman Spectroscopic Characterization of LiFSI Solvates

Han, Sang-Don; Sommer, Roger D.; Boyle, Paul D.; Zhou, Zhi-Bin; Young, Victor G.; Borodin, Oleg; Henderson, Wesley A.

doi:10.1149/1945-7111/ac9a07

Electrolyte Solvation and Ionic Association: Part IX. Structures and Raman Spectroscopic Characterization of LiFSI Solvates

Journal Article · Mon Nov 28 00:00:00 EST 2022 · Journal of the Electrochemical Society

DOI:https://doi.org/10.1149/1945-7111/ac9a07· OSTI ID:2419630

^[1]; ^[2]; ^[2]; Zhou, Zhi-Bin ^[3]; ^[4]; Borodin, Oleg ^[5]; ^[6]

North Carolina State University, Raleigh, NC (United States); OSTI
North Carolina State University, Raleigh, NC (United States)
Huazhong Univ. of Science and Technology, Wuhan (China)
Univ. of Minnesota, Minneapolis, MN (United States)
Army Research Lab., Adelphi, MD (United States)
North Carolina State University, Raleigh, NC (United States); Army Research Lab., Adelphi, MD (United States)

The bis(fluorosulfonyl)imide anion N(SO₂F)₂⁻ (i.e., FSI⁻) (also referred to as bis(fluorosulfonyl)amide (i.e., FSA-) and imidodi(sulphuryl fluoride)) has attracted tremendous interest in recent years for its utility in both lithium salts and ionic liquids for battery electrolyte applications. To facilitate the understanding of the characteristics of this anion, crystal structures are reported here for the uncoordinated anion in LiFSI-based solvates with cryptand CRYPT-222 and tetraglyme (G4). These crystalline solvates were analyzed by Raman spectroscopy to aid in assigning the Raman bands to the modes of ion coordination found in liquid electrolytes. These structures, as well as a thorough review of other relevant crystallographic data, provide insights into the rather remarkable properties of the FSI- anion with regard to solvate formation and electrolyte properties.

View Accepted Manuscript (DOE)

Research Organization:: North Carolina State University, Raleigh, NC (United States)

Sponsoring Organization:: USDOE Office of Science (SC), Basic Energy Sciences (BES). Materials Sciences & Engineering Division (MSE)

Grant/Contract Number:: SC0002169

OSTI ID:: 2419630

Journal Information:: Journal of the Electrochemical Society, Journal Name: Journal of the Electrochemical Society Journal Issue: 11 Vol. 169; ISSN 0013-4651

Publisher:: IOP PublishingCopyright Statement

Country of Publication:: United States

Language:: English

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Steric Effect Tuned Ion Solvation Enabling Stable Cycling of High-Voltage Lithium Metal Battery Chen, Yuelang; Yu, Zhiao; Rudnicki, Paul Journal of the American Chemical Society, Vol. 143, Issue 44 https://doi.org/10.1021/jacs.1c09006	journal	October 2021
Anion Conformation of Low-Viscosity Room-Temperature Ionic Liquid 1-Ethyl-3-methylimidazolium Bis(fluorosulfonyl) Imide Fujii, Kenta; Seki, Shiro; Fukuda, Shuhei The Journal of Physical Chemistry B, Vol. 111, Issue 44 https://doi.org/10.1021/jp074325e	journal	November 2007
Electrochemical Lithium Intercalation into Graphite in Dimethyl Sulfoxide-Based Electrolytes: Effect of Solvation Structure of Lithium Ion Yamada, Yuki; Takazawa, Yasuyuki; Miyazaki, Kohei The Journal of Physical Chemistry C, Vol. 114, Issue 26 https://doi.org/10.1021/jp1037427	journal	June 2010
Change from Glyme Solutions to Quasi-ionic Liquids for Binary Mixtures Consisting of Lithium Bis(trifluoromethanesulfonyl)amide and Glymes Yoshida, Kazuki; Tsuchiya, Mizuho; Tachikawa, Naoki The Journal of Physical Chemistry C, Vol. 115, Issue 37 https://doi.org/10.1021/jp206881t	journal	August 2011
Glyme–Lithium Salt Equimolar Molten Mixtures: Concentrated Solutions or Solvate Ionic Liquids? Ueno, Kazuhide; Yoshida, Kazuki; Tsuchiya, Mizuho The Journal of Physical Chemistry B, Vol. 116, Issue 36 https://doi.org/10.1021/jp307378j	journal	August 2012
Solvate Structures and Computational/Spectroscopic Characterization of Lithium Difluoro(oxalato)borate (LiDFOB) Electrolytes Han, Sang-Don; Allen, Joshua L.; Jónsson, Erlendur The Journal of Physical Chemistry C, Vol. 117, Issue 11 https://doi.org/10.1021/jp309102c	journal	March 2013
Unusual Li ⁺ Ion Solvation Structure in Bis(fluorosulfonyl)amide Based Ionic Liquid Fujii, Kenta; Hamano, Hiroshi; Doi, Hiroyuki The Journal of Physical Chemistry C, Vol. 117, Issue 38 https://doi.org/10.1021/jp4053264	journal	September 2013
Role of Solution Structure in Solid Electrolyte Interphase Formation on Graphite with LiPF ₆ in Propylene Carbonate Nie, Mengyun; Abraham, Daniel P.; Seo, Daniel M. The Journal of Physical Chemistry C, Vol. 117, Issue 48 https://doi.org/10.1021/jp409765w	journal	November 2013
Sacrificial Anion Reduction Mechanism for Electrochemical Stability Improvement in Highly Concentrated Li-Salt Electrolyte Sodeyama, Keitaro; Yamada, Yuki; Aikawa, Koharu The Journal of Physical Chemistry C, Vol. 118, Issue 26, p. 14091-14097 https://doi.org/10.1021/jp501178n	journal	June 2014
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Solvate Structures and Spectroscopic Characterization of LiTFSI Electrolytes Seo, Daniel M.; Boyle, Paul D.; Sommer, Roger D. The Journal of Physical Chemistry B, Vol. 118, Issue 47 https://doi.org/10.1021/jp505006x	journal	September 2014
Solvent Activity in Electrolyte Solutions Controls Electrochemical Reactions in Li-Ion and Li-Sulfur Batteries Moon, Heejoon; Mandai, Toshihiko; Tatara, Ryoichi The Journal of Physical Chemistry C, Vol. 119, Issue 8 https://doi.org/10.1021/jp5128578	journal	February 2015
Potential Energy Landscape of Bis(fluorosulfonyl)amide Canongia Lopes, José N.; Shimizu, Karina; Pádua, Agílio A. H. The Journal of Physical Chemistry B, Vol. 112, Issue 31 https://doi.org/10.1021/jp803309c	journal	August 2008
Molecular Dynamics Simulation and Pulsed-Field Gradient NMR Studies of Bis(fluorosulfonyl)imide (FSI) and Bis[(trifluoromethyl)sulfonyl]imide (TFSI)-Based Ionic Liquids Borodin, Oleg; Gorecki, W.; Smith, Grant D. The Journal of Physical Chemistry B, Vol. 114, Issue 20 https://doi.org/10.1021/jp911950q	journal	May 2010
Superconcentrated electrolytes for a high-voltage lithium-ion battery Wang, Jianhui; Yamada, Yuki; Sodeyama, Keitaro Nature Communications, Vol. 7, Issue 1 https://doi.org/10.1038/ncomms12032	journal	June 2016
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High rate and stable cycling of lithium metal anode Qian, Jiangfeng; Henderson, Wesley A.; Xu, Wu Nature Communications, Vol. 6, Issue 1 https://doi.org/10.1038/ncomms7362	journal	February 2015
Characterising lithium-ion electrolytes via operando Raman microspectroscopy Fawdon, Jack; Ihli, Johannes; Mantia, Fabio La Nature Communications, Vol. 12, Issue 1 https://doi.org/10.1038/s41467-021-24297-0	journal	June 2021
Raman study of crystalline solvates between glymes CH ₃ (OCH ₂ CH ₂ ) _n OCH ₃ (n = 1, 2 and 3) and LiClO ₄ Grondin, Joseph; Talaga, David; Lassègues, Jean-Claude Phys. Chem. Chem. Phys., Vol. 6, Issue 5 https://doi.org/10.1039/B315475K	journal	January 2004
Raman study of tetraglyme–LiClO ₄ solvate structures Grondin, Joseph; Lassègues, Jean-Claude; Chami, Marianne Phys. Chem. Chem. Phys., Vol. 6, Issue 17 https://doi.org/10.1039/B406578F	journal	January 2004
Concentrated electrolytes: decrypting electrolyte properties and reassessing Al corrosion mechanisms McOwen, Dennis W.; Seo, Daniel M.; Borodin, Oleg Energy Environ. Sci., Vol. 7, Issue 1 https://doi.org/10.1039/C3EE42351D	journal	January 2014
LiTFSI in 1-butyl-1-methylpyrrolidinium bis(fluorosulfonyl)amide: a possible electrolyte for ionic liquid based lithium ion batteries Lahiri, Abhishek; Schubert, Thomas J. S.; Iliev, Boyan Physical Chemistry Chemical Physics, Vol. 17, Issue 17 https://doi.org/10.1039/C5CP01337B	journal	January 2015
Colorless organometallic ionic liquids from cationic ruthenium sandwich complexes: thermal properties, liquid properties, and crystal structures of [Ru(η⁵-C₅H₅)(η⁶-C₆H₅R)][X] (X = N(SO₂CF₃)₂, N(SO₂F)₂, PF₆) Komurasaki, Aina; Funasako, Yusuke; Mochida, Tomoyuki Dalton Transactions, Vol. 44, Issue 16 https://doi.org/10.1039/C5DT00723B	journal	January 2015
Thermal stability and decomposition of lithium bis(fluorosulfonyl)imide (LiFSI) salts Kerner, Manfred; Plylahan, Nareerat; Scheers, Johan RSC Advances, Vol. 6, Issue 28 https://doi.org/10.1039/C5RA25048J	journal	January 2016
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Ionic transport in highly concentrated lithium bis(fluorosulfonyl)amide electrolytes with keto ester solvents: structural implications for ion hopping conduction in liquid electrolytes Kondou, Shinji; Thomas, Morgan L.; Mandai, Toshihiko Physical Chemistry Chemical Physics, Vol. 21, Issue 9 https://doi.org/10.1039/C9CP00425D	journal	January 2019
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Electrolyte Solvation and Ionic Association: V. Acetonitrile-Lithium Bis(fluorosulfonyl)imide (LiFSI) Mixtures Han, Sang-Don; Borodin, Oleg; Seo, Daniel M. Journal of The Electrochemical Society, Vol. 161, Issue 14 https://doi.org/10.1149/2.0101414jes	journal	January 2014
A Design Approach to Lithium-Ion Battery Electrolyte Based on Diluted Solvate Ionic Liquids Ueno, Kazuhide; Murai, Junichi; Moon, Heejoon Journal of The Electrochemical Society, Vol. 164, Issue 1 https://doi.org/10.1149/2.0121701jes	journal	October 2016
Electrolyte Solvation and Ionic Association III. Acetonitrile-Lithium Salt Mixtures–Transport Properties Seo, Daniel M.; Borodin, Oleg; Balogh, Daniel Journal of The Electrochemical Society, Vol. 160, Issue 8 https://doi.org/10.1149/2.018308jes	journal	January 2013
Electrolyte Solvation and Ionic Association II. Acetonitrile-Lithium Salt Mixtures: Highly Dissociated Salts Seo, Daniel M.; Borodin, Oleg; Han, Sang-Don Journal of The Electrochemical Society, Vol. 159, Issue 9 https://doi.org/10.1149/2.035209jes	journal	January 2012
Electrolyte Solvation and Ionic Association: VI. Acetonitrile-Lithium Salt Mixtures: Highly Associated Salts Revisited Borodin, Oleg; Han, Sang-Don; Daubert, James S. Journal of The Electrochemical Society, Vol. 162, Issue 4 https://doi.org/10.1149/2.0891503jes	journal	January 2015
Electrolyte Solvation and Ionic Association: IV. Acetonitrile-Lithium Difluoro(oxalato)borate (LiDFOB) Mixtures Han, Sang-Don; Borodin, Oleg; Allen, Joshua L. Journal of The Electrochemical Society, Vol. 160, Issue 11 https://doi.org/10.1149/2.094309jes	journal	January 2013
Solvate Ionic Liquid Electrolyte for Li–S Batteries Dokko, Kaoru; Tachikawa, Naoki; Yamauchi, Kento Journal of The Electrochemical Society, Vol. 160, Issue 8 https://doi.org/10.1149/2.111308jes	journal	January 2013
Electrolyte Solvation and Ionic Association Seo, Daniel M.; Borodin, Oleg; Han, Sang-Don Journal of The Electrochemical Society, Vol. 159, Issue 5 https://doi.org/10.1149/2.jes112264	journal	January 2012
From Ionic Liquids to Solvate Ionic Liquids: Challenges and Opportunities for Next Generation Battery Electrolytes Watanabe, Masayoshi; Dokko, Kaoru; Ueno, Kazuhide Bulletin of the Chemical Society of Japan, Vol. 91, Issue 11 https://doi.org/10.1246/bcsj.20180216	journal	November 2018
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Structures of bis(fluorosulfonyl)imide HN(SO ₂ F) ₂ , bis(trifluoromethylsulfonyl)imide HN(SO ₂ CF ₃ ) ₂ , and their potassium salts at 150 K No authors listed Zeitschrift für Kristallographie - Crystalline Materials, Vol. 213, Issue 4 https://doi.org/10.1524/zkri.1998.213.4.217	journal	April 1998
A Review of Solvate Ionic Liquids: Physical Parameters and Synthetic Applications Eyckens, Daniel J.; Henderson, Luke C. Frontiers in Chemistry, Vol. 7 https://doi.org/10.3389/fchem.2019.00263	journal	April 2019
Electrochemical Evaluation of Lithium-Metal Anode in Highly Concentrated Ethylene Carbonate Based Electrolytes Takeyoshi, Junya; Kobori, Naohiro; Kanamura, Kiyoshi Electrochemistry, Vol. 88, Issue 6 https://doi.org/10.5796/electrochemistry.20-00087	journal	November 2020
Lithium-tin Alloy/Sulfur Battery with a Solvate Ionic Liquid Electrolyte Ikeda, Kohei; Terada, Shoshi; Mandai, Toshihiko Electrochemistry, Vol. 83, Issue 10 https://doi.org/10.5796/electrochemistry.83.914	journal	January 2015

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