A facile synthesis of bulk LiPON in solution for solid-state electrolytes

Osma J. Gomez; Adam Antar; Alex T. Hall; Leopoldo Tapia-Aracayo; Joshua Seo; Nam Kim; Zihan Sun; Ryan Lim; Fu Chen; Yue Li; John Cumings; Gary Rubloff; Sang Bok Lee; David Stewart; Yang Wang

doi:10.1039/D5TA03196F

A facile synthesis of bulk LiPON in solution for solid-state electrolytes†

Osma J. Gomez,

^a Adam Antar,^b Alex T. Hall,^c Leopoldo Tapia-Aracayo,^c Joshua Seo,^a Nam Kim,^a Zihan Sun,^a Ryan Lim,^a Fu Chen,^a Yue Li,

^a John Cumings,^c Gary Rubloff,

^cd Sang Bok Lee,

*^a David Stewart

*^c and Yang Wang

*^a

Author affiliations

* Corresponding authors

^a Department of Chemistry and Biochemistry, University of Maryland, College Park, MD 20742, USA
E-mail: ywang16@umd.edu

^b Department of Mechanical Engineering, University of Maryland, College Park, MD 20742, USA
E-mail: steward@umd.edu

^c Department of Materials Science and Engineering, University of Maryland, College Park, MD 20742, USA
E-mail: slee@umd.edu

^d Institute for Systems Research, University of Maryland, College Park, MD 20742, USA

Abstract

We present a facile, solution-based approach to prepare bulk lithium phosphorus oxynitride (LiPON) utilizing a stepwise reduction between lithium tert-butoxide (LiO^tBu) and a phosphazene base, diethyl phosphoramidate (DEPA), which are also precursors used in LiPON synthesis by atomic layer deposition (ALD). The study finds that the two ALD LiPON precursors can readily react upon mixing in THF at room temperature, which yields an ionically conductive solid powder that may be used as a solid-state electrolyte in solid-state batteries or as a material for surface coating. We conducted comprehensive characterization studies using solid-state nuclear magnetic resonance (SSNMR) spectroscopy, cryogenic transmission electron microscopy (cryo-TEM), matrix-assisted laser desorption ionization mass spectroscopy (MALDI-MS), X-ray diffraction spectroscopy (XRD), and X-ray photoelectron spectroscopy (XPS) to study the structure of this bulk LiPON material, which exhibits a composition closely resembling LiPO₂N. We propose a reaction mechanism of this bulk synthesized LiPON in a solution system.

Journal of Materials Chemistry A

A facile synthesis of bulk LiPON in solution for solid-state electrolytes†

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A facile synthesis of bulk LiPON in solution for solid-state electrolytes

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