Ball milling enables phase-pure synthesis of a temperature sensitive ternary chloride, MgZrCl$_6$
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arXiv
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| Main Authors: | , , , , , , |
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| Format: | Preprint |
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2025
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| _version_ | 1866911116492275712 |
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| author | Rom, Christopher L. Shotwell, Austin Combs, Sinclair Peters, Autumn Borgia, Lauren Neilson, James R. Maughan, Annalise E. |
| author_facet | Rom, Christopher L. Shotwell, Austin Combs, Sinclair Peters, Autumn Borgia, Lauren Neilson, James R. Maughan, Annalise E. |
| contents | Ball milling is a powerful synthetic tool for discovering new inorganic materials. Inspired by the high ionic conductivity in Li$_2$ZrCl$_6$ synthesized via mechanochemistry, we synthesized MgZrCl$_6$ with a similar method. High resolution synchrotron X-ray diffraction shows that MgZrCl$_6$ is poorly crystalline after ball milling, but crystallizes in a layered hexagonal structure ($P31c$) after heat treatment. In situ synchrotron X-ray diffraction reveals a narrow temperature window around 400 °C in which crystallization occurs. At higher temperatures the phase decomposes. Pair distribution function analysis shows 2D sheets of MgZrCl$_6$ form after milling, with heating driving 3D crystallization. Raman spectroscopy also shows evidence of MgZrCl$_6$ after milling. Electrochemical impedance spectroscopy does not reveal ionic conductivity in MgZrCl$_6$ (limit of detection ca. $1.4 \times 10^{-8}$ S/cm). In addition to supporting existing design rules for Mg-based solid electrolytes, this work shows the power of ball milling to synthesize temperature-sensitive inorganic compounds with high yield. |
| format | Preprint |
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arxiv_https___arxiv_org_abs_2508_16066 |
| institution | arXiv |
| publishDate | 2025 |
| record_format | arxiv |
| spellingShingle | Ball milling enables phase-pure synthesis of a temperature sensitive ternary chloride, MgZrCl$_6$ Rom, Christopher L. Shotwell, Austin Combs, Sinclair Peters, Autumn Borgia, Lauren Neilson, James R. Maughan, Annalise E. Materials Science Ball milling is a powerful synthetic tool for discovering new inorganic materials. Inspired by the high ionic conductivity in Li$_2$ZrCl$_6$ synthesized via mechanochemistry, we synthesized MgZrCl$_6$ with a similar method. High resolution synchrotron X-ray diffraction shows that MgZrCl$_6$ is poorly crystalline after ball milling, but crystallizes in a layered hexagonal structure ($P31c$) after heat treatment. In situ synchrotron X-ray diffraction reveals a narrow temperature window around 400 °C in which crystallization occurs. At higher temperatures the phase decomposes. Pair distribution function analysis shows 2D sheets of MgZrCl$_6$ form after milling, with heating driving 3D crystallization. Raman spectroscopy also shows evidence of MgZrCl$_6$ after milling. Electrochemical impedance spectroscopy does not reveal ionic conductivity in MgZrCl$_6$ (limit of detection ca. $1.4 \times 10^{-8}$ S/cm). In addition to supporting existing design rules for Mg-based solid electrolytes, this work shows the power of ball milling to synthesize temperature-sensitive inorganic compounds with high yield. |
| title | Ball milling enables phase-pure synthesis of a temperature sensitive ternary chloride, MgZrCl$_6$ |
| topic | Materials Science |
| url | https://arxiv.org/abs/2508.16066 |