Probing the Formation of Cathode-Electrolyte Interphase on Lithium Iron Phosphate Cathodes via Operando Mechanical Measurements

Bal, Batuhan; Ozdogru, Bertan; Nguyen, Dan Thien; Li, Zheng; Murugesan, Vijayakumar; Çapraz, Ömer Özgür

doi:10.1021/acsami.3c05749

Probing the Formation of Cathode-Electrolyte Interphase on Lithium Iron Phosphate Cathodes via Operando Mechanical Measurements

Journal Article · Sat Sep 02 00:00:00 EDT 2023 · ACS Applied Materials and Interfaces

DOI:https://doi.org/10.1021/acsami.3c05749· OSTI ID:2203228

Bal, Batuhan ^[1]; Ozdogru, Bertan ^[2]; Nguyen, Dan Thien ^[3]; Li, Zheng ^[4]; ^[3]; ^[5]

The School of Chemical Engineering, Oklahoma State University, Stillwater, Oklahoma 74078, United States
The School of Chemical Engineering, Oklahoma State University, Stillwater, Oklahoma 74078, United States; Center for Energy Conversion & Storage Systems, National Renewable Energy Laboratory, Golden, Colorado 80401, United States
Physical and Computational Sciences Directorate, Pacific Northwest National Laboratory, Richland, Washington 99352, United States; Joint Center for Energy Storage Research (JCESR), Lemont, Illinois 60439, United States
Joint Center for Energy Storage Research (JCESR), Lemont, Illinois 60439, United States; Davidson School of Chemical Engineering, Purdue University, West Lafayette, Indiana 47907, United States
The School of Chemical Engineering, Oklahoma State University, Stillwater, Oklahoma 74078, United States; Chemical, Biochemical and Environmental Engineering, The University of Maryland − Baltimore County, Baltimore, Maryland 21250, United States

Interfacial instabilities in electrodes control the performance and lifetime of Li-ion batteries. While the formation of solid-electrolyte interface (SEI) on anodes has received much attention, there is still lack of understanding about the formation of cathode-electrolyte interface (CEI) on the cathodes. To fill this gap, we report on dynamic deformations on lithium iron phosphate, LiFePO₄ cathodes during charge / discharge by utilizing in-operando digital image correlation, impedance spectroscopy and Cryo X-ray photoelectron spectroscopy. LiFePO4 cathodes were cycled in either LiPF₆, LiClO₄ or LiTFSI- containing organic liquid electrolytes. Beyond the first cycle, Li-ion intercalation results in a nearly linear correlation between electrochemical strains and the state of (dis)-charge, regardless of the electrolyte chemistry. However, during the first charge in LiPF₆ - containing electrolyte, there is a distinct irreversible positive strain evolution at the onset of anodic current rise as well as current decay at around 4.0V. Impedance studies show the increase in surface resistance in the same potential window, suggesting the formation of CEI layers on the cathode. The chemistry of the CEI layer was characterized by X-ray photoelectron spectroscopy. LiF is detected in CEI layer starting as early as 3.4 V and Li_$$x$$PO_$$y$$F_$$z$$ appeared at voltages higher than 4.0 V during the first charge. In conclusion, our approach offers new insights into the formation mechanism of CEI layers on the cathode electrodes, which is crucial for the development of robust cathode and electrolyte chemistries for higher performance batteries.

View Accepted Manuscript (DOE)

Research Organization:: National Renewable Energy Laboratory (NREL), Golden, CO (United States)

Sponsoring Organization:: USDOE Office of Science (SC), Basic Energy Sciences (BES)

Grant/Contract Number:: AC36-08GO28308; SC0021251

OSTI ID:: 2203228

Alternate ID(s):: OSTI ID: 2008444
OSTI ID: 2222894
OSTI ID: 2281648

Report Number(s):: NREL/JA--5700-87815; MainId:88590; UUID:d39d5203-149e-40fc-80b3-3966ffa99a32; MainAdminId:70903

Journal Information:: ACS Applied Materials and Interfaces, Journal Name: ACS Applied Materials and Interfaces Journal Issue: 36 Vol. 15; ISSN 1944-8244

Publisher:: American Chemical Society (ACS)Copyright Statement

Country of Publication:: United States

Language:: English

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