Facile Synthesis of High Purity Li2S by Titanothermic Reduction
Source abstract
Abstract
Lithium sulfide (Li2S) is indispensable for lithium–sulfur batteries and sulfide solid-state batteries. However, its high preparation cost and strict process conditions represent core bottlenecks restricting large-scale commercial application. To address this issue, a novel process featuring a low-cost, high-safety, and controllable reaction is proposed in this work. Compared with the commercial H2S-based route for Li2S production, the developed process presents distinct advantages, including accessible raw materials, high safety, low overall cost, and low environmental load. Using Li2SO4·H2O as the raw material and Ti as the reducing agent, high-purity T-Li2S (>99.9%) is successfully synthesized via solid-state sintering and purification, yielding a higher purity level than that of commercial C-Li2S (>99.7%). Furthermore, sulfide all-solid-state electrolytes T-Li5.3PS4.3ClBr0.7 and C-Li5.3PS4.3ClBr0.7 are prepared using the as-obtained T-Li2S and commercial C-Li2S as precursors, respectively. The room-temperature Li-ion conductivities are determined to be 14.5 mS/cm and 11.0 mS/cm, revealing faster ion migration and efficient ion transport in T-Li5.3PS4.3ClBr0.7 without high-temperature assistance, which fully validates the feasibility of the proposed strategy. Overall, this work provides a new technical route for the preparation of high-purity Li2S, showing promising application prospects.
Source: crossref · Quality: baseline
Research context
OpenAlex topics: Advanced Battery Materials and Technologies · Extraction and Separation Processes · Molten salt chemistry and electrochemical processes
SciVX discovery tags are terminology-based. OpenAlex topics are source-provided classifications.
Affiliations
Zijin Mining New Energy and New Materials Technology (Changsha) Co., Ltd., Changsha 410000, China
College of Chemistry and Chemical Engineering, Central South University, Changsha 410083, China
Fujian Zijin Lithium Materials Technology Co., Ltd., Longyan 364200, China
References (40)
Show source-provided references
1. Boosting Oxygen Redox Reversibility in Chemo-Mechanically Robust Li-Rich Oxide Cathodes via Multi-Scale Defect Design10.1039/D4EE04266B ↗
2. Eutectic-Based Polymer Electrolyte with the Enhanced Lithium Salt Dissociation for High-Performance Lithium Metal Batteries10.1002/anie.202310006 ↗
3. Chemo-Mechanical Stable Cathode Interphase via Interface in Situ Catalytic-Conversion Integrated Design for All Solid-State Batteries10.1039/D4EE02827A ↗
4. Unraveling the Catalytic Activity of Fe-Based Compounds toward Li2Sx in L-S Chemical System from D-P Bands10.1002/aenm.202100673 ↗
5. Advances in the Development of Single-Atom Catalysts for High-Energy-Density Lithium-Sulfur Batteries10.1002/adma.202200102 ↗
6. Reinventing Phosphorus Anodes: Taming Pulverization via Strain-Induced Interfacial Coupling10.1002/anie.202523513 ↗
7. Guo, K., Yan, W., Liu, Y., Zou, J., Zhu, J., Wang, Z., Tian, Y., and Cui, X. (2026). Unveiling Confined Proton Desolvation Dynamics in Interlayer-Engineered Mxenes. Adv. Funct. Mater., e28186.10.1002/adfm.202528186 ↗
8. Regulating the Co Spin State via Directional Fe Doping to Enhance Sulfur Conversion Catalysis10.1002/adfm.202504753 ↗
9. MoP Quantum Dots Based Multifunctional Efficient Electrocatalyst for Stable and Long-Life Flexible Lithium-Sulfur Batteries10.1016/j.jcis.2024.01.155 ↗
10. The Contact Interface Engineering of All-Sulfide-Based Solid State Batteries via Infiltrating Dissoluble Sulfide Electrolyte10.1002/eem2.12461 ↗
11. In-Situ Synthesis of Carbon-Encapsulated Atomic Cobalt as Highly Efficient Polysulfide Electrocatalysts for Highly Stable Lithium-Sulfur Batteries10.1002/smll.202106640 ↗
12. Self-Supported and Flexible Sulfur Cathode Enabled via Synergistic Confinement for High-Energy-Density Lithium-Sulfur Batteries10.1002/adma.201902228 ↗
13. Designing with Li2S in Lithium-Sulfur Batteries: From Fundamental Chemistry to Practical Architectures10.1002/smll.202513644 ↗
14. Interface Engineering of All-Solid-State Batteries Based on Inorganic Solid Electrolytes10.1002/cssc.202202158 ↗
15. Advances in Sulfide Solid-State Electrolytes for Lithium Batteries10.1016/j.ensm.2025.104018 ↗
16. Superior Lithium-Stable Li7P2S8I Solid Electrolyte for All-Solid-State Lithium Batteries10.1016/j.jpowsour.2021.229565 ↗
17. Cost-Effective and High Ionic Conductivity Sulfide Solid Electrolyte Li7.3P2.9S10.75X0.3 (X = F, Cl, Br, and I) for All-Solid-State Lithium Batteries10.1021/acsaem.4c02595 ↗
18. Low-Cost and Scalable Synthesis of High-Purity Li2S for Sulfide Solid Electrolyte10.1021/acssuschemeng.2c02238 ↗
19. Advancing Sulfide Solid Electrolytes via Green Li2S Synthesis10.1038/s41467-025-64924-8 ↗
20. Research Progress on Lithium Sulfide Synthesis: A Review10.1021/acsaem.5c02015 ↗
21. Low-Cost Preparation and Purification of Li2S for Sulfide Solid Electrolytes10.1016/j.est.2024.114180 ↗
22. Facile Synthesis of Lithium Sulfide Nanocrystals for Use in Advanced Rechargeable Batteries10.1021/acsami.5b09367 ↗
23. Challenges and Opportunities of Practical Sulfide-Based All-Solid-State Batteries10.1016/j.etran.2023.100272 ↗
24. Environmentally Friendly, Non-Glove Box, Closed-System and Continuously Massive Production of Lithium Sulfide for Battery Applications10.1016/j.jclepro.2022.135221 ↗
25. Investigation of the Carbothermic Reduction of Lithium Sulfate for the Production of Lithium Sulfide10.1007/s40831-025-01203-2 ↗
26. “One Stone Two Birds” Strategy of Synthesizing the Battery Material Lithium Sulfide: Aluminothermal Reduction of Lithium Sulfate10.1021/acs.inorgchem.3c00087 ↗
27. Preparation of High-Quality Lithium Sulfide by Reducing Lithium Sulfate with Hydrogen: A Green and Cost-Effective Method10.1039/D4GC01017E ↗
28. Harnessing Strengthening-Metastability Synergy for Extreme Work Hardening in Additively Manufactured Titanium Alloys10.1038/s41467-025-67683-8 ↗
29. Achieving “True” Selective Hydrogenation by Co Treatment of the Pt/TiO2 Catalyst10.1021/jacs.5c04699 ↗
30. A Mechanochemical Synthesis of Submicron-Sized Li2S and a Mesoporous Li2S/C Hybrid for High Performance Lithium/Sulfur Battery Cathodes10.1039/C7TA00557A ↗
31. A Process for Fabrication of Li2TiO3 Ceramic Pebbles with High Mechanical Properties via Non-Hydrolytic Sol-Gel Method10.1016/j.ceramint.2020.07.266 ↗
32. A Green Method of Synthesizing Battery-Grade Lithium Sulfide: Hydrogen Reduction of Lithium Sulfate10.1021/acssuschemeng.3c07872 ↗
33. Lithium Sulfide: Magnesothermal Synthesis and Battery Applications10.1021/acsami.2c11196 ↗
34. Enhanced Ion Conduction by Enforcing Structural Disorder in Li-Deficient Argyrodites Li6−XPS5−XCl1+X10.1016/j.ensm.2020.04.042 ↗
35. Clean Synthesis of Oxide Electrolytes via a Boiling Water-Assisted Solid-Phase Sintering Route10.1021/acsami.5c01869 ↗
36. Anion Spatial Confinement via Amide Functionalization Induces LiF/Li3N-Rich Interphase for Stable All-Solid-State Lithium Metal Batteries10.1016/j.ensm.2025.104538 ↗
37. Engineering Electronic Radial Effects for Fast Li+ Transport in Solid-State Electrolytes10.1002/adma.202520337 ↗
38. Superionic Fluorinated Halide Solid Electrolytes for Highly Stable Li-Metal in All-Solid-State Li Batteries10.1002/aenm.202101915 ↗
39. Single-Step Ball Milling Synthesis of Highly Li+ Conductive Li5.3PS4.3ClBr0.7 Glass Ceramic Electrolyte Enables Low-Impedance All-Solid-State Batteries10.1039/D1MA00784J ↗
40. Synthesis of High-Purity Li2S Nanocrystals via Metathesis for Solid-State Electrolyte Applications10.1039/D3TA00076A ↗