Ex Situ and Operando XRD and XAS Analysis of MoS2: A Lithiation Study of Bulk and Nanosheet Materials

Quilty, Calvin D.; Housel, Lisa M.; Bock, David C.; Dunkin, Mikaela R.; Wang, Lei; Lutz, Diana M.; Abraham, Alyson; Bruck, Andrea M.; Takeuchi, Esther S.; Takeuchi, Kenneth J.; Marschilok, Amy C.

doi:10.1021/acsaem.9b01538

Title: Ex Situ and Operando XRD and XAS Analysis of MoS₂: A Lithiation Study of Bulk and Nanosheet Materials

Journal Article · Thu Sep 26 00:00:00 EDT 2019 · ACS Applied Energy Materials

DOI:https://doi.org/10.1021/acsaem.9b01538· OSTI ID:1604319

Quilty, Calvin D. ^[1]; Housel, Lisa M. ^[1]; Bock, David C. ^[2]; Dunkin, Mikaela R. ^[1];

^[2];

^[1]; Abraham, Alyson ^[1]; Bruck, Andrea M. ^[1];

^[3];

^[1];

^[3]

Stony Brook Univ., NY (United States)
Brookhaven National Lab. (BNL), Upton, NY (United States)
Stony Brook Univ., NY (United States); Brookhaven National Lab. (BNL), Upton, NY (United States)

Molybdenum(IV) sulfide (MoS₂) has generated significant interest as an electroactive material for Li-ion batteries because of its high theoretical capacity, good rate capability, and minimal volume changes during cycling. An important challenge toward implementing this material is understanding the many polymorphs of MoS₂ that can be (de)stabilized by electrochemical lithiation and nanosizing. To this end, bulk MoS₂ and nanosheet-type MoS₂ were characterized both as solids (X-ray diffraction (XRD), X-ray absorption spectroscopy (XAS), X-ray photoelectron spectroscopy (XPS), and inductively coupled plasma-optical emission spectroscopy (ICP-OES)) and during electrochemical cycling within operando X-ray analysis compatible lithium cells (operando XRD and ex situ XAS). We report in situ XRD shows that the bulk 2H-MoS₂ phase is converted to 1T-Li_xMoS₂ upon discharge and that this change is only partially reversible upon charge. Furthermore, operando XRD identifies the nanosheet MoS₂ as the metastable 1T' phase and shows that this phase is conserved upon discharge. Ex situ XAS provides additional structural insights into the local structure of MoS₂, confirming that the 1T' phase is the correct assignment of the nanosheet MoS₂ and revealing an irreversible local distortion that occurs during cycling. This local distortion is likely a factor in the increased capacity fade observed in the nanosheet cells. This work provides important insights into the structure of MoS₂ and how that structure is affected by nanosizing and cycling, which can inform other studies of nanosheet layered materials.

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Research Organization:: Energy Frontier Research Centers (EFRC) (United States). Center for Mesoscale Transport Properties (m2mt); Brookhaven National Lab. (BNL), Upton, NY (United States)

Sponsoring Organization:: USDOE Office of Energy Efficiency and Renewable Energy (EERE), Vehicle Technologies Office (EE-3V); USDOE Office of Science (SC), Basic Energy Sciences (BES)

Grant/Contract Number:: SC0012704

OSTI ID:: 1604319

Report Number(s):: BNL-213708-2020-JAAM

Journal Information:: ACS Applied Energy Materials, Vol. 2, Issue 10; ISSN 2574-0962

Publisher:: American Chemical Society (ACS)Copyright Statement

Country of Publication:: United States

Language:: English

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Cited by: 25 works

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25 ENERGY STORAGE
molybdenum(IV) sulfide
layered materials
lithium battery
in situ X-ray diffraction
X-ray absorption spectroscopy
X-ray analysis compatible pouch cells

Title: Ex Situ and Operando XRD and XAS Analysis of MoS2: A Lithiation Study of Bulk and Nanosheet Materials

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Title: Ex Situ and Operando XRD and XAS Analysis of MoS₂: A Lithiation Study of Bulk and Nanosheet Materials