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Rapid and Tunable Assisted-Microwave Preparation of Glass and Glass-Ceramic Thiophosphate “Li7P3S11” Li-Ion Conductors
- Molleigh B. PreeferMolleigh B. PreeferDepartment of Chemistry and Biochemistry and Materials Research Laboratory, University of California, Santa Barbara, Santa Barbara, California 93106, United StatesMore by Molleigh B. Preefer
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- Jason H. GrebenkemperJason H. GrebenkemperMaterials Research Laboratory, University of California, Santa Barbara, Santa Barbara, California 93106, United StatesMore by Jason H. Grebenkemper
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- Franziska SchroederFranziska SchroederMaterials Research Laboratory, University of California, Santa Barbara, Santa Barbara, California 93106, United StatesMore by Franziska Schroeder
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- Joshua D. BocarslyJoshua D. BocarslyMaterials Research Laboratory and Materials Department, University of California, Santa Barbara, Santa Barbara, California 93106, United StatesMore by Joshua D. Bocarsly
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- Kartik PilarKartik PilarMaterials Research Laboratory, University of California, Santa Barbara, Santa Barbara, California 93106, United StatesMore by Kartik Pilar
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- Joya A. CooleyJoya A. CooleyMaterials Research Laboratory, University of California, Santa Barbara, Santa Barbara, California 93106, United StatesMore by Joya A. Cooley
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- William ZhangWilliam ZhangDepartment of Chemistry and Biochemistry, University of California, Santa Barbara, Santa Barbara, California 93106, United StatesMore by William Zhang
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- Jerry HuJerry HuMaterials Research Laboratory, University of California, Santa Barbara, Santa Barbara, California 93106, United StatesMore by Jerry Hu
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- Sumohan Misra
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- Fabian Seeler
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- Kerstin Schierle-Arndt
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- Ram Seshadri*Ram Seshadri*E-mail: [email protected]Department of Chemistry and Biochemistry, Materials Research Laboratory and Materials Department, University of California, Santa Barbara, Santa Barbara, California 93106, United StatesMore by Ram Seshadri
Abstract
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.
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