Floating zone crystal growth, structure, and properties of a cubic Li5.5La3Nb1.5Zr0.5O12 garnet-type lithium-ion conductor

Ramette, Caleb; Pressley, Lucas; Avdeev, Maxim; Lee, Minseong; Kushwaha, Satya; Krogstad, Matthew; Sarker, Suchismita; Cardon, Paul; Ruff, Jacob; Khan, Mojammel; Kataoka, Kunimitsu; McQueen, Tyrel; Ji, Huiwen

doi:10.1039/d3ta04606k

Title: Floating zone crystal growth, structure, and properties of a cubic Li_5.5La₃Nb_1.5Zr_0.5O₁₂ garnet-type lithium-ion conductor

Journal Article · Mon Sep 25 00:00:00 EDT 2023 · Journal of Materials Chemistry. A

DOI:https://doi.org/10.1039/d3ta04606k· OSTI ID:2203417

^[1]; Pressley, Lucas ^[2];

^[3];

^[4]; Kushwaha, Satya ^[5]; Krogstad, Matthew ^[6]; Sarker, Suchismita ^[7]; Cardon, Paul ^[1]; Ruff, Jacob ^[7]; Khan, Mojammel ^[5];

^[8];

^[5]; Ji, Huiwen ^[1]

Univ. of Utah, Salt Lake City, UT (United States)
Johns Hopkins Univ., Baltimore, MD (United States)
Australian Nuclear Science and Technology Organisation (ANSTO), Lucas Heights, NSW (Australia); Univ. of Sydney, NSW (Australia)
Los Alamos National Laboratory (LANL), Los Alamos, NM (United States). National High Magnetic Field Lab. (MagLab)
Platform for the Accelerated Realization, Analysis and Discovery of Interface Materials (PARADIM)
Argonne National Laboratory (ANL), Argonne, IL (United States). Advanced Photon Source (APS)
Cornell Univ., Ithaca, NY (United States). Cornell High Energy Synchrotron Source (CHESS)
National Inst. of Advanced Industrial Science and Technology (AIST), Tsukuba (Japan)

As a promising candidate for solid-state electrolytes in Li-ion batteries, the garnet-type Li-ion conductor series Li_5+xLa₃Nb_2-xZr_xO₁₂ (LLNZO) (0 ≤ x ≤ 2) exhibits high ionic conductivity at room temperature. However, no previous single-crystal growth or characterization has been reported for LLNZO compositions 0 ≤ x ≤ 1. To obtain a complete understanding of the trend in the structure–property relationship in this class of materials, we used the floating zone (FZ) method to grow a single crystal of Li_5.5La₃Nb_1.5Zr_0.5O₁₂ that was 4 mm in diameter and 10 mm in length. Using Laue neutron single-crystal diffraction, two distinct Li sites were observed: tetrahedral 24d and octahedral 96h sites. The maximum entropy method (MEM) based on neutron single-crystal diffraction data was used to map Li nuclear density and estimate that the bottleneck of Li transport exists between neighboring tetrahedral and octahedral sites, and that Li is delocalized between split octahedral sites. Room-temperature Li-ion conductivity in Li_5.5La₃Nb_1.5Zr_0.5O₁₂ measured with electrochemical impedance spectroscopy (EIS) was 1.37 × 10^-4 S cm^-1. The Li migration activation energy was estimated to be 0.50 eV from EIS and 0.47 eV from dielectric relaxation measurements. The Li-ion jump attempt rate was estimated to be 1.47 × 10¹² Hz while the time scale of successful migration is 10^-7 to 10^-6 s.

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Research Organization:: Los Alamos National Laboratory (LANL), Los Alamos, NM (United States)

Sponsoring Organization:: USDOE; National Science Foundation (NSF)

Grant/Contract Number:: 89233218CNA000001; DMR-2039380; 2145832; DMR-2128556

OSTI ID:: 2203417

Report Number(s):: LA-UR-23-30252

Journal Information:: Journal of Materials Chemistry. A, Vol. 11, Issue 40; ISSN 2050-7488

Publisher:: Royal Society of ChemistryCopyright Statement

Country of Publication:: United States

Language:: English

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Title: Floating zone crystal growth, structure, and properties of a cubic Li5.5La3Nb1.5Zr0.5O12 garnet-type lithium-ion conductor

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Title: Floating zone crystal growth, structure, and properties of a cubic Li_5.5La₃Nb_1.5Zr_0.5O₁₂ garnet-type lithium-ion conductor