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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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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issn | 1996-1944 |
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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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