Publication date: 10th April 2024
Li-garnets, oxide-based ceramics with the structure of Li7La3Zr2O12 (LLZO), are promising solid-state electrolytes for hybrid and solid-state batteries due to their large electrochemical stability window (up to 5.0V vs Li/Li+) and high stability with metallic lithium, and conductivity of greater than 1mS/cm.1 Despite the promise, high sinter temperatures of LLZO above 1100°C in classical processing routes are unbeneficial as they limit co-sintering with Co-reduced cathodes,2 lead to unfavorable aspect-ratios of electrolyte thickness to average grain size, and also are critical in terms of energy consumption and CO2 footprint at production3. In contrast, liquid-to-solid-state manufacturing enables the scalable fabrication of thin electrolyte films from dissolved precursors at significantly reduced processing temperatures, overcoming the aforementioned challenges.3 In this work, we employ a direct liquid-to-solid-state synthesis method, Sequential Decomposition Synthesis (SDS), capable to solidify nano-grained films of LLZO with a thickness of 2-10 micrometers without sintering.4 Such films are after the first synthesis step amorphous and can be crystallized to the cubic higher Li-ion conductive phase at around 500-650°C;4–6 To better understand the crystallization mechanism and structure of LLZO fabricated through SDS, we further study the phase evolution during the crystallization process and compare how the Li‑content influences structure and ionic conductivity in amorphous and crystalline LLZO films. Collectively, our study contributes to the deeper understanding of the role of precursor selection and composition on the phase evolution during the formation process of non-sintered solid Li-oxide electrolyte materials from precursors via nucleation and growth as a gateway to integration of thin and cost-effective electrolytes into hybrid or all-solid-state Li-metal batteries.
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