Mechanical Milling – Induced Microstructure Changes in Argyrodite LPSCl Solid-State Electrolyte Critically Affect Electrochemical Stability

Wang, Yixian; Hao, Hongchang; Naik, Kaustubh G.; Vishnugopi, Bairav S.; Fincher, Cole D.; Yan, Qianqian; Raj, Vikalp; Celio, Hugo; Yang, Guang; Fang, Hong; Chiang, Yet‐Ming; Perras, Frédéric A.; Jena, Puru; Watt, John; Mukherjee, Partha P.; Mitlin, David

doi:10.1002/aenm.202304530

Title: Mechanical Milling – Induced Microstructure Changes in Argyrodite LPSCl Solid-State Electrolyte Critically Affect Electrochemical Stability

Journal Article · 13 April 2024 · Advanced Energy Materials

DOI: https://doi.org/10.1002/aenm.202304530 · OSTI ID:2341299

^[1]; Hao, Hongchang ^[1]; Naik, Kaustubh G. ^[2]; Vishnugopi, Bairav S. ^[2];

^[3]; Yan, Qianqian ^[3];

^[1];

^[4]; Fang, Hong ^[5];

^[3];

^[6]; Jena, Puru ^[7];

^[8]; Mukherjee, Partha P. ^[2];

^[1]

Univ. of Texas, Austin, TX (United States). Texas Materials Inst. (TMI)
Purdue Univ., West Lafayette, IN (United States)
Massachusetts Inst. of Technology (MIT), Cambridge, MA (United States)
Oak Ridge National Laboratory (ORNL), Oak Ridge, TN (United States)
Rutgers University, Camden, NJ (United States)
Ames Lab., and Iowa State Univ., Ames, IA (United States)
Virginia Commonwealth Univ., Richmond, VA (United States)
Los Alamos National Laboratory (LANL), Los Alamos, NM (United States). Center for Integrated Nanotechnologies (CINT)

Microstructure of argyrodite solid-state electrolyte (SSE) critically affects lithium metal electrodeposition/dissolution. While the stability of unmodified SSE is mediocre, once optimized state-of-the-art electrochemical performance is achieved (symmetric cells, full cells with NMC811) without secondary interlayers or functionalized current collectors. Planetary mechanical milling in wet media (m-xylene) is employed to alter commercial Li₆PS₅Cl (LPSCl) powder. Quantitative stereology demonstrates how milling progressively refines grain and pore size/distribution in the SSE compact, increases its density, and geometrically smoothens the SSE-Li interface. Mechanical indentation demonstrates that these changes lead to reduced site-to-site variation in the compact's hardness. Milled microstructures promote uniform early-stage electrodeposition on foil collectors and stabilize solid electrolyte interphase (SEI) reactivity. Analysis of half-cells with bilayer electrolytes demonstrates the importance of microstructure directly contacting current collector, with interface roughness due to pore and grain size distribution being key. For the first time, short-circuiting Li metal dendrite is directly identified, employing 1.5 mm diameter “mini” symmetrical cell and cryogenic focused ion beam (cryo-FIB) electron microscopy. The branching sheet-like dendrite traverses intergranularly, filling the interparticle voids and forming an SEI around it. Importantly, mesoscale modeling reveals the relationship between Li-SSE interface morphology and the onset of electrochemical instability, based on underlying reaction current distribution.

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Research Organization:: Ames Laboratory (AMES), Ames, IA (United States); Los Alamos National Laboratory (LANL), Los Alamos, NM (United States)

Sponsoring Organization:: USDOE Office of Science (SC), Basic Energy Sciences (BES). Materials Sciences & Engineering Division (MSE); USDOE Office of Science (SC), Basic Energy Sciences (BES). Scientific User Facilities (SUF); USDOE National Nuclear Security Administration (NNSA); USDOE Office of Energy Efficiency and Renewable Energy (EERE), Office of Sustainable Transportation. Vehicle Technologies Office (VTO)

Grant/Contract Number:: AC02-07CH11358; 89233218CNA000001; SC0023438

OSTI ID:: 2341299

Report Number(s):: IS-J--11,316

Journal Information:: Advanced Energy Materials, Journal Name: Advanced Energy Materials Journal Issue: 23 Vol. 14; ISSN 1614-6832

Publisher:: WileyCopyright Statement

Country of Publication:: United States

Language:: English

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25 ENERGY STORAGE
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inorganic solid electrolytes
solid-state battery

Title: Mechanical Milling – Induced Microstructure Changes in Argyrodite LPSCl Solid-State Electrolyte Critically Affect Electrochemical Stability

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