Publication date: 15th December 2025
All-solid-state lithium batteries benefit from scalable routes to sulfide solid electrolytes with controlled phase formation. Here, an in situ Raman spectrometer integrated with a microwave reactor provides real-time vibrational fingerprints of the liquid-phase reaction between Li2S and P4S10 in acetonitrile. We benchmark the cell by tracking P4S10 solubility up to 130 °C and establish analytical performance for the PS stretch at ∼716 cm−1, determining LOD = 0.78 mM and LOQ = 2.60 mM. Time-resolved spectra capture the systematic decay of the 716 cm−1 band during the reaction, consistent with the disruption of the P4S10 cage and formation of thiophosphate intermediates. Early-stage kinetics are quantitatively described by the Finke–Watzky two-step model, and temperature-dependent rate constants yield Arrhenius and Eyring relationships with Ea(mw) = 39.59 kJ mol−1, ΔH‡ = 36.97 kJ mol−1, and ΔS‡ = −178.55 J mol−1 K−1. This combined in situ spectroscopic–kinetic approach offers a direct pathway to mechanistic understanding and parameter extraction in solution-based synthesis of sulfide SSEs.
This research work is a part of the PIE project “Innovative and Designed (Electro)-Chemistry, All-in-One for Lithium Sulfide Solid Electrolytes” (IDEAL-Li), reference 20226AT009, supported by The Spanish National Research Council (CSIC). This work was supported by the ELISA project (ref. CNS2023-145494), funded by MCIN/AEI/10.13039/501100011033 and by the European Union “NextGenerationEU”/PRTR. We also acknowledge the Erasmus Internship support for Thomas Poupeau and Beyza Batu.
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