Influence of Powder Milling and Annealing Parameters on the Formation of Cubic Li<sub>7</sub>La<sub>3</sub>Zr<sub>2</sub>O<sub>12</sub> Compound

Li-ion batteries are widely used as energy storage devices due to their excellent electrochemical performance. The cubic Li<sub>7</sub>La<sub>3</sub>Zr<sub>2</sub>O<sub>12</sub> (c-LLZO) compound is regarded as a promising candidate as a solid-state el...

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Main Authors: Dariusz Oleszak, Mirosława Pawlyta, Tomasz Pikula
Format: Article
Language:English
Published: MDPI AG 2021-12-01
Series:Materials
Subjects:
Online Access:https://www.mdpi.com/1996-1944/14/24/7633
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author Dariusz Oleszak
Mirosława Pawlyta
Tomasz Pikula
author_facet Dariusz Oleszak
Mirosława Pawlyta
Tomasz Pikula
author_sort Dariusz Oleszak
collection DOAJ
description Li-ion batteries are widely used as energy storage devices due to their excellent electrochemical performance. The cubic Li<sub>7</sub>La<sub>3</sub>Zr<sub>2</sub>O<sub>12</sub> (c-LLZO) compound is regarded as a promising candidate as a solid-state electrolyte for lithium-ion batteries due to its high bulk Li-ion conductivity, excellent thermal performance, and chemical stability. The standard manufacturing procedure involves the high-temperature and lengthy annealing of powders. However, the formation of the tetragonal modification of LLZO and other undesired side phases results in the deterioration of electrochemical properties. The mechanical milling of precursor powders can enhance the powders’ reactivity and can result in an easier formation of c-LLZO. The aim of this work was to study the influence of selected milling and annealing parameters on c-LLZO compound formation. The starting powders of La(OH)<sub>3,</sub> Li<sub>2</sub>CO<sub>3</sub>, and ZrO<sub>2</sub> were subjected to milling in various ball mills, under different milling conditions. The powders were then annealed at various temperatures for different lengths of times. These studies showed that the phase transformation processes of the powders were not very sensitive to the milling parameters. On the other hand, the final phase composition and microstructure strongly depended on heat treatment conditions. Low temperature annealing (750 °C) for 3 h produced 90% of c-LLZO in the powder structure.
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spelling doaj.art-7f17487290d04060a6bdc07aa5b22bcb2023-11-23T09:20:43ZengMDPI AGMaterials1996-19442021-12-011424763310.3390/ma14247633Influence of Powder Milling and Annealing Parameters on the Formation of Cubic Li<sub>7</sub>La<sub>3</sub>Zr<sub>2</sub>O<sub>12</sub> CompoundDariusz Oleszak0Mirosława Pawlyta1Tomasz Pikula2Faculty of Materials Science and Engineering, Warsaw University of Technology, 02-507 Warsaw, PolandInstitute of Engineering Materials and Biomaterials, Silesian University of Technology, 44-100 Gliwice, PolandFaculty of Electrical Engineering and Computer Science, Lublin University of Technology, 20-618 Lublin, PolandLi-ion batteries are widely used as energy storage devices due to their excellent electrochemical performance. The cubic Li<sub>7</sub>La<sub>3</sub>Zr<sub>2</sub>O<sub>12</sub> (c-LLZO) compound is regarded as a promising candidate as a solid-state electrolyte for lithium-ion batteries due to its high bulk Li-ion conductivity, excellent thermal performance, and chemical stability. The standard manufacturing procedure involves the high-temperature and lengthy annealing of powders. However, the formation of the tetragonal modification of LLZO and other undesired side phases results in the deterioration of electrochemical properties. The mechanical milling of precursor powders can enhance the powders’ reactivity and can result in an easier formation of c-LLZO. The aim of this work was to study the influence of selected milling and annealing parameters on c-LLZO compound formation. The starting powders of La(OH)<sub>3,</sub> Li<sub>2</sub>CO<sub>3</sub>, and ZrO<sub>2</sub> were subjected to milling in various ball mills, under different milling conditions. The powders were then annealed at various temperatures for different lengths of times. These studies showed that the phase transformation processes of the powders were not very sensitive to the milling parameters. On the other hand, the final phase composition and microstructure strongly depended on heat treatment conditions. Low temperature annealing (750 °C) for 3 h produced 90% of c-LLZO in the powder structure.https://www.mdpi.com/1996-1944/14/24/7633lithium-ion batteriessolid-state electrolytesolid-state reactionmechanical millingnanopowdersXRD
spellingShingle Dariusz Oleszak
Mirosława Pawlyta
Tomasz Pikula
Influence of Powder Milling and Annealing Parameters on the Formation of Cubic Li<sub>7</sub>La<sub>3</sub>Zr<sub>2</sub>O<sub>12</sub> Compound
Materials
lithium-ion batteries
solid-state electrolyte
solid-state reaction
mechanical milling
nanopowders
XRD
title Influence of Powder Milling and Annealing Parameters on the Formation of Cubic Li<sub>7</sub>La<sub>3</sub>Zr<sub>2</sub>O<sub>12</sub> Compound
title_full Influence of Powder Milling and Annealing Parameters on the Formation of Cubic Li<sub>7</sub>La<sub>3</sub>Zr<sub>2</sub>O<sub>12</sub> Compound
title_fullStr Influence of Powder Milling and Annealing Parameters on the Formation of Cubic Li<sub>7</sub>La<sub>3</sub>Zr<sub>2</sub>O<sub>12</sub> Compound
title_full_unstemmed Influence of Powder Milling and Annealing Parameters on the Formation of Cubic Li<sub>7</sub>La<sub>3</sub>Zr<sub>2</sub>O<sub>12</sub> Compound
title_short Influence of Powder Milling and Annealing Parameters on the Formation of Cubic Li<sub>7</sub>La<sub>3</sub>Zr<sub>2</sub>O<sub>12</sub> Compound
title_sort influence of powder milling and annealing parameters on the formation of cubic li sub 7 sub la sub 3 sub zr sub 2 sub o sub 12 sub compound
topic lithium-ion batteries
solid-state electrolyte
solid-state reaction
mechanical milling
nanopowders
XRD
url https://www.mdpi.com/1996-1944/14/24/7633
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