Fabrication of thin solid electrolytes containing a small volume of an Li3OCl-type antiperovskite phase by RF magnetron sputtering
<p>Several attempts to synthesize Li<small><sub>3</sub></small>OCl – a lithium-rich antiperovskite compound envisaged as a potential solid electrolyte material for lithium metal batteries – have been reported, but few have yielded convincing results....
| Päätekijät: | , , , , , , |
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| Aineistotyyppi: | Journal article |
| Kieli: | English |
| Julkaistu: |
Royal Society of Chemistry
2021
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| _version_ | 1826309318634373120 |
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| author | Turrell, SJ Lee, HJ Siniscalchi, M Narayanan, S Pasta, M Speller, S Grovenor, C |
| author_facet | Turrell, SJ Lee, HJ Siniscalchi, M Narayanan, S Pasta, M Speller, S Grovenor, C |
| author_sort | Turrell, SJ |
| collection | OXFORD |
| description | <p>Several attempts to synthesize Li<small><sub>3</sub></small>OCl – a lithium-rich antiperovskite compound envisaged as a potential solid electrolyte material for lithium metal batteries – have been reported, but few have yielded convincing results. There are two key challenges associated with this synthesis: the thermodynamic instability of Li<small><sub>3</sub></small>OCl at room temperature and its extreme hygroscopicity. Therefore, the likelihood of inadvertently forming the structurally similar thermodynamically stable hydroxide halide compound Li<small><sub>2</sub></small>OHCl is very high. In this report, we demonstrate the stabilization of a small volume fraction of antiperovskite phase with the characteristics expected for Li<small><sub>3</sub></small>OCl in ∼0.5 to ∼1 μm films fabricated from a Li<small><sub>2</sub></small>O + LiCl powder target by RF magnetron sputtering. Measures were taken to minimize the presence of moisture at all stages of synthesis and characterization. X-ray diffraction (XRD) experiments showed that reaction between the precursor phases occurred within the growing films to form a volume of antiperovskite phase with an identical lattice parameter to that predicted for cubic Li<small><sub>3</sub></small>OCl. This antiperovskite phase decomposed into Li<small><sub>2</sub></small>O and LiCl upon annealing at moderate temperatures. Characterization by Fourier transform infrared spectroscopy (FT-IR) confirmed the absence of O–H bonding in the films, providing further evidence that the antiperovskite phase was Li<small><sub>3</sub></small>OCl rather than Li<small><sub>2</sub></small>OHCl. Deposition of films with similar thicknesses from an Li<small><sub>2</sub></small>OHCl powder target was also performed for comparison. While FT-IR results showed that O–H bonding was present in these films, a small volume fraction of an antiperovskite phase with identical lattice parameter to Li<small><sub>2</sub></small>OHCl was only detected after heating the films to ∼100 °C. Owing to the low phase purities of films deposited from both target types, the Li<small><sup>+</sup></small> conductivities were found to be on the order of 10<small><sup>−8</sup></small> S cm<small><sup>−1</sup></small>. For Li<small><sub>2</sub></small>OHCl in particular, it is expected that further optimization of the processing conditions will lead to a significant increase in Li<small><sup>+</sup></small> conductivity. This is the first reported attempt to synthesize lithium-rich antiperovskite compounds by RF magnetron sputtering.</p> |
| first_indexed | 2024-03-07T07:32:26Z |
| format | Journal article |
| id | oxford-uuid:c0f43043-6e1d-40e1-b9dd-ce37c5a63c00 |
| institution | University of Oxford |
| language | English |
| last_indexed | 2024-03-07T07:32:26Z |
| publishDate | 2021 |
| publisher | Royal Society of Chemistry |
| record_format | dspace |
| spelling | oxford-uuid:c0f43043-6e1d-40e1-b9dd-ce37c5a63c002023-02-02T14:22:25ZFabrication of thin solid electrolytes containing a small volume of an Li3OCl-type antiperovskite phase by RF magnetron sputteringJournal articlehttp://purl.org/coar/resource_type/c_dcae04bcuuid:c0f43043-6e1d-40e1-b9dd-ce37c5a63c00EnglishSymplectic ElementsRoyal Society of Chemistry2021Turrell, SJLee, HJSiniscalchi, MNarayanan, SPasta, MSpeller, SGrovenor, C<p>Several attempts to synthesize Li<small><sub>3</sub></small>OCl – a lithium-rich antiperovskite compound envisaged as a potential solid electrolyte material for lithium metal batteries – have been reported, but few have yielded convincing results. There are two key challenges associated with this synthesis: the thermodynamic instability of Li<small><sub>3</sub></small>OCl at room temperature and its extreme hygroscopicity. Therefore, the likelihood of inadvertently forming the structurally similar thermodynamically stable hydroxide halide compound Li<small><sub>2</sub></small>OHCl is very high. In this report, we demonstrate the stabilization of a small volume fraction of antiperovskite phase with the characteristics expected for Li<small><sub>3</sub></small>OCl in ∼0.5 to ∼1 μm films fabricated from a Li<small><sub>2</sub></small>O + LiCl powder target by RF magnetron sputtering. Measures were taken to minimize the presence of moisture at all stages of synthesis and characterization. X-ray diffraction (XRD) experiments showed that reaction between the precursor phases occurred within the growing films to form a volume of antiperovskite phase with an identical lattice parameter to that predicted for cubic Li<small><sub>3</sub></small>OCl. This antiperovskite phase decomposed into Li<small><sub>2</sub></small>O and LiCl upon annealing at moderate temperatures. Characterization by Fourier transform infrared spectroscopy (FT-IR) confirmed the absence of O–H bonding in the films, providing further evidence that the antiperovskite phase was Li<small><sub>3</sub></small>OCl rather than Li<small><sub>2</sub></small>OHCl. Deposition of films with similar thicknesses from an Li<small><sub>2</sub></small>OHCl powder target was also performed for comparison. While FT-IR results showed that O–H bonding was present in these films, a small volume fraction of an antiperovskite phase with identical lattice parameter to Li<small><sub>2</sub></small>OHCl was only detected after heating the films to ∼100 °C. Owing to the low phase purities of films deposited from both target types, the Li<small><sup>+</sup></small> conductivities were found to be on the order of 10<small><sup>−8</sup></small> S cm<small><sup>−1</sup></small>. For Li<small><sub>2</sub></small>OHCl in particular, it is expected that further optimization of the processing conditions will lead to a significant increase in Li<small><sup>+</sup></small> conductivity. This is the first reported attempt to synthesize lithium-rich antiperovskite compounds by RF magnetron sputtering.</p> |
| spellingShingle | Turrell, SJ Lee, HJ Siniscalchi, M Narayanan, S Pasta, M Speller, S Grovenor, C Fabrication of thin solid electrolytes containing a small volume of an Li3OCl-type antiperovskite phase by RF magnetron sputtering |
| title | Fabrication of thin solid electrolytes containing a small volume of an Li3OCl-type antiperovskite phase by RF magnetron sputtering |
| title_full | Fabrication of thin solid electrolytes containing a small volume of an Li3OCl-type antiperovskite phase by RF magnetron sputtering |
| title_fullStr | Fabrication of thin solid electrolytes containing a small volume of an Li3OCl-type antiperovskite phase by RF magnetron sputtering |
| title_full_unstemmed | Fabrication of thin solid electrolytes containing a small volume of an Li3OCl-type antiperovskite phase by RF magnetron sputtering |
| title_short | Fabrication of thin solid electrolytes containing a small volume of an Li3OCl-type antiperovskite phase by RF magnetron sputtering |
| title_sort | fabrication of thin solid electrolytes containing a small volume of an li3ocl type antiperovskite phase by rf magnetron sputtering |
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