Rapid and Tunable Assisted-Microwave Preparation of Glass and Glass-Ceramic Thiophosphate 'Li7P3S11' Li-Ion Conductors
| العنوان: | Rapid and Tunable Assisted-Microwave Preparation of Glass and Glass-Ceramic Thiophosphate 'Li7P3S11' Li-Ion Conductors |
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| المؤلفون: | William Zhang, Jason H. Grebenkemper, Joshua D. Bocarsly, Kartik Pilar, Sumohan Misra, Franziska Schroeder, Joya A. Cooley, Fabian Seeler, Molleigh B. Preefer, Kerstin Schierle-Arndt, Jerry Hu, Ram Seshadri |
| المصدر: | ACS Applied Materials & Interfaces. 11:42280-42287 |
| بيانات النشر: | American Chemical Society (ACS), 2019. |
| سنة النشر: | 2019 |
| مصطلحات موضوعية: | Glass-ceramic, Materials science, Rietveld refinement, Analytical chemistry, chemistry.chemical_element, 02 engineering and technology, 010402 general chemistry, 021001 nanoscience & nanotechnology, 01 natural sciences, 0104 chemical sciences, Amorphous solid, law.invention, symbols.namesake, X-ray photoelectron spectroscopy, chemistry, law, symbols, Fast ion conductor, General Materials Science, Lithium, 0210 nano-technology, Raman spectroscopy, Spectroscopy |
| الوصف: | Glass and glass-ceramic samples of metastable lithium thiophosphates with compositions of 70Li2S-30P2S5 and Li7P3S11 were controllably prepared by using a rapid assisted-microwave procedure in under 30 min. The rapid preparation times and weak coupling of the evacuated silica ampules with microwave radiation ensure minimal reactivity of the reactants and the container. The microwave-prepared samples display comparable conductivity values with more conventionally prepared (melt quenched) glass and glass-ceramic samples, on the order of 0.1 and 1 mS cm-1 at room temperature, respectively. Rietveld analysis of synchrotron X-ray diffraction data acquired with an internal standard quantitatively yields phase amounts of the glassy and amorphous components, establishing the tunable nature of the microwave preparation. X-ray photoelectron spectroscopy and Raman spectroscopy confirm the composition and the appropriate ratios of isolated and corner-sharing tetrahedra in these semicrystalline systems. Solid-state 7Li nuclear magnetic resonance (NMR) spectroscopy resolves the seven crystallographic Li sites in the crystalline compound into three main environments. The diffusion behavior of these Li environments as obtained from pulsed-field gradient NMR methods can be separated into one slow and one fast component. The rapid and tunable approach to the preparation of high quality "Li7P3S11" samples presented here coupled with detailed structural and compositional analysis opens the door to new and promising metastable solid electrolytes. |
| تدمد: | 1944-8252 1944-8244 |
| DOI: | 10.1021/acsami.9b15688 |
| URL الوصول: | https://explore.openaire.eu/search/publication?articleId=doi_________::91c4fe42f75851b299cfe475e67f317a https://doi.org/10.1021/acsami.9b15688 |
| Rights: | CLOSED |
| رقم الانضمام: | edsair.doi...........91c4fe42f75851b299cfe475e67f317a |
| قاعدة البيانات: | OpenAIRE |
| تدمد: | 19448252 19448244 |
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| DOI: | 10.1021/acsami.9b15688 |