Influence of Powder Milling and Annealing Parameters on the Formation of Cubic Li7La3Zr2O12 Compound
Abstract
:1. Introduction
2. Materials and Methods
3. Results and Discussion
4. Conclusions
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- The mechanical milling processes had no induced phase transformations of the starting powder mixture, and a broadening of the diffraction lines was observed only due to structural refinement and the generation of crystal imperfections;
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- The type of ball mill used (with different dominant modes of milling—impact and friction) has no influence on the processing of powders
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- Changes to other milling parameters (ball-to-powder weight ratio BPR, addition of ethanol, prolongation of milling up to 10 h) do not introduce qualitative changes in the powder structure;
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- The formation of c-LLZO was possible only after powder annealing, and the amount of the desired cubic modification of LLZO significantly depended on the annealing parameters. It was found that annealing at 750 °C resulted in a higher amount of c-LLZO than processing at 950 °C, and that the prolongation of annealing time for upward of 3 h was beneficial.
Author Contributions
Funding
Data Availability Statement
Conflicts of Interest
References
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Compound | Weight Content (%) | Cryst. Structure | Space Group | Lattice Parameters (Å) |
---|---|---|---|---|
Li7La3Zr2O12 | 29.4 (3) | cubic | IA–3d | a = 13.025 (1) |
Li7La3Zr2O12 | 58.5 (4) | tetragonal | I41/acd | a = 13.1189 (8), c = 12.6698 (5) |
La2Zr2O7 | 7.9 (2) | cubic | Fd-3m | a = 10.8226 (8) |
La(OH)3 | 4.2 (2) | hexagonal | P63/m | a = 6.5346 (5), c = 3.8579 (5) |
Milling and Annealing Parameters | c-LLZO Content (wt.%) ±2 (%) | Other Phases Detected |
---|---|---|
Fritsch 1h MM + 750 °C/2h | 48 | t-LLZO Li2CO3 ZrO2 La2Zr2O7 LaAlO3 La(OH)3 La2O2CO3 La2O3 LaOOH |
Fritsch 1 h MM + 750 °C/3 h | 90 | |
Fritsch 1 h MM + 950 °C/2 h | 30 | |
Fritsch 1 h MM + 950 °C/3h | 60 | |
SPEX 1 h MM + 750 °C/3 h | 80 |
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Oleszak, D.; Pawlyta, M.; Pikula, T. Influence of Powder Milling and Annealing Parameters on the Formation of Cubic Li7La3Zr2O12 Compound. Materials 2021, 14, 7633. https://doi.org/10.3390/ma14247633
Oleszak D, Pawlyta M, Pikula T. Influence of Powder Milling and Annealing Parameters on the Formation of Cubic Li7La3Zr2O12 Compound. Materials. 2021; 14(24):7633. https://doi.org/10.3390/ma14247633
Chicago/Turabian StyleOleszak, Dariusz, Mirosława Pawlyta, and Tomasz Pikula. 2021. "Influence of Powder Milling and Annealing Parameters on the Formation of Cubic Li7La3Zr2O12 Compound" Materials 14, no. 24: 7633. https://doi.org/10.3390/ma14247633