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Operando EQCM-D with Simultaneous in Situ EIS: New Insights into Interphase Formation in Li Ion Batteries
Paul Scherrer Inst, Electrochem Lab, CH-5232 Villigen, Switzerland.
Uppsala University, Disciplinary Domain of Science and Technology, Chemistry, Department of Chemistry - Ångström, Structural Chemistry.ORCID iD: 0000-0002-0366-7228
Paul Scherrer Inst, Electrochem Lab, CH-5232 Villigen, Switzerland.
Uppsala University, Disciplinary Domain of Science and Technology, Chemistry, Department of Chemistry - Ångström, Structural Chemistry. Paul Scherrer Inst, Electrochem Lab, CH-5232 Villigen, Switzerland.ORCID iD: 0000-0001-5653-0383
2019 (English)In: Analytical Chemistry, ISSN 0003-2700, E-ISSN 1520-6882, Vol. 91, no 3, p. 2296-2303Article in journal (Refereed) Published
Abstract [en]

An operando electrochemical quartz crystal microbalance with dissipation monitoring (EQCM-D) with simultaneous in situ electrochemical impedance spectroscopy (EIS) has been developed and applied to study the solid electrolyte interphase (SEI) formation on copper current collectors in Li-ion batteries. The findings are backed by EIS simulations and complementary analytical techniques, such as online electrochemical mass spectrometry (OEMS) and X-ray photoelectron spectroscopy (XPS). The evolution of mass and the mechanical properties of the SEI are directly correlated to the electrode impedance. Electrolyte reduction at the anode carbon active material initiates dissolution, diffusion, and deposition of reaction side products throughout the cell and increases electrolyte viscosity and the ohmic cell resistance as a result. On Cu the reduction of CuOx and HF occurs at >1.5 V and forms an initial LiF-rich interphase while electrolyte solvent reduction at <0.8 V vs Li+/Li adds a second, less rigid layer on top. Both the shear storage modulus and viscosity of the SEI generally increase upon cycling but-along with the SEI Li+ diffusion coefficient-also respond reversibly to electrode potential, likely as a result of Li+/EC interfacial concentration changes. Combined EIS-EQCM-D provides unique prospects for further studies of the highly dynamic structure-function relationships of electrode interphases in Li ion batteries.

Place, publisher, year, edition, pages
AMER CHEMICAL SOC , 2019. Vol. 91, no 3, p. 2296-2303
National Category
Physical Chemistry Materials Chemistry
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URN: urn:nbn:se:uu:diva-378386DOI: 10.1021/acs.analchem.8b04924ISI: 000458220300090PubMedID: 30569698OAI: oai:DiVA.org:uu-378386DiVA, id: diva2:1293753
Available from: 2019-03-05 Created: 2019-03-05 Last updated: 2019-03-05Bibliographically approved

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