Preprint Article Version 1 Preserved in Portico This version is not peer-reviewed

A Facile Two-Step Thermal Process for Producing Dense Phase Pure Cubic Ta-Doped Lithium Lanthanum Zirconium Oxide Electrolyte for Upscaling

Diwakar Karuppiah
,
Dmitrii Komissarenko
,
Nur Sena Yuzbasi
ORCID logo ,
Yang Liu
,
Pradeep Vallachira Warriam Sasikumar
,
Amir Hadian
,
Thomas Graule
,
Frank Clemens
ORCID logo ,
Gurdial Blugan
* ORCID logo
Version 1 : Received: 16 October 2023 / Approved: 17 October 2023 / Online: 18 October 2023 (03:02:05 CEST)

A peer-reviewed article of this Preprint also exists.

Karuppiah, D.; Komissarenko, D.; Yüzbasi, N.S.; Liu, Y.; Warriam Sasikumar, P.V.; Hadian, A.; Graule, T.; Clemens, F.; Blugan, G. A Facile Two-Step Thermal Process for Producing a Dense, Phase-Pure, Cubic Ta-Doped Lithium Lanthanum Zirconium Oxide Electrolyte for Upscaling. Batteries 2023, 9, 554. Karuppiah, D.; Komissarenko, D.; Yüzbasi, N.S.; Liu, Y.; Warriam Sasikumar, P.V.; Hadian, A.; Graule, T.; Clemens, F.; Blugan, G. A Facile Two-Step Thermal Process for Producing a Dense, Phase-Pure, Cubic Ta-Doped Lithium Lanthanum Zirconium Oxide Electrolyte for Upscaling. Batteries 2023, 9, 554.

Abstract

An inorganic solid electrolyte is the most favorable candidate for replacing flammable liquid electrolytes in lithium batteries. Lithium Lanthanum Zirconium Oxide (LLZO) is considered as a promising solid electrolyte due to its safe operating potential window (0-5V) combined with its good electrochemical stability. In this work, 250 g batches of pre-sintered Tadoped (Li7La3Zr1.6Ta0.4O12, TaLLZO) were synthesized for bulk production of dense LLZO electrolyte. A simple two-step thermal treatment process was developed. The first thermal step at 950 °C initiates nucleation of LLZO carefully controlling process parameters such as heating atmosphere, temperature and dopant concentration. In the second thermal step at 1150 °C, sintered discs were obtained as solid electrolytes, with relative densities of 96%. X-ray diffraction analysis confirmed the phase purity of the sintered TaLLZO disc, and refined data was used to calculate the lattice parameter (12.944 Å). Furthermore, the presence of the Ta dopant in the disc was confirmed through X-ray photoelectron spectroscopy (XPS) analysis. The ionic and electronic conductivity values of TaLLZO disc were 104 S cm-1 and 10-10 S cm-1, respectively. These values confirm that the prepared (Ta-LLZO) discs exhibit ionic conductivity while being electronically insulating, being suitable for use as solid electrolytes with the requisite electrical properties.

Keywords

solid electrolyte; lithium batteries; LLZO, solid state batteries, lithium metal

Subject

Chemistry and Materials Science, Electrochemistry

Copyright: This is an open access article distributed under the Creative Commons Attribution License which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited.

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