液相法制备硫化物固体电解质及其在全固态锂电池中的应用

doi:10.3866/PKU.WHXB202309019

物理化学学报 >> 2025, Vol. 41 >> Issue (1): 100004.doi: 10.3866/PKU.WHXB202309019

所属专题：电化学前沿

液相法制备硫化物固体电解质及其在全固态锂电池中的应用

门明阳¹^,², 吴敬华¹^,², 刘高瞻¹^,², 张婧¹^,², 张妮妮¹^,², 姚霞银¹^,²^,*()

¹ 中国科学院宁波材料技术与工程研究所, 浙江省先进燃料电池与电解池技术重点实验室, 浙江宁波 315201
² 中国科学院大学材料科学与光电技术中心, 北京 100049

收稿日期:2023-09-12 修回日期:2023-10-11 录用日期:2023-10-30 发布日期:2023-12-20
通讯作者: Email: yaoxy@nimte.ac.cn; Tel.: +86-574-8632-4359 (姚霞银)
基金资助:
国家自然科学基金(22309194); 国家自然科学基金(52372244); 宁波市重点研发计划(2021Z122); 宁波市重点研发计划(2023Z106); 浙江省重点研发计划(2022C01072); 中国科学院青年创新促进会(Y2021080)

Sulfide Solid Electrolyte Synthesized by Liquid Phase Approach and Application in All-Solid-State Lithium Batteries

Mingyang Men¹^,², Jinghua Wu¹^,², Gaozhan Liu¹^,², Jing Zhang¹^,², Nini Zhang¹^,², Xiayin Yao¹^,²^,*()

¹ Key Laboratory of Advanced Fuel Cells and Electrolyzers Technology of Zhejiang Province, Ningbo Institute of Materials Technology and Engineering, Chinese Academy of Sciences, Ningbo 315201, Zhejiang Province, China
² Center of Materials Science and Optoelectronics Engineering, University of Chinese Academy of Sciences, Beijing 100049, China

Received:2023-09-12 Revised:2023-10-11 Accepted:2023-10-30 Published:2023-12-20
Contact: Email: yaoxy@nimte.ac.cn; Tel.: +86-574-8632-4359 (Xiayin Yao)
Supported by:
the National Natural Science Foundation of China(22309194); the National Natural Science Foundation of China(52372244); the Ningbo S&T Innovation 2025 Major Special Program(2021Z122); the Ningbo S&T Innovation 2025 Major Special Program(2023Z106); the Zhejiang Provincial Key R&D Program of China(2022C01072); the Youth Innovation Promotion Association CAS(Y2021080)

摘要/Abstract

摘要：

硫化物固体电解质具有接近甚至超过液态有机电解质的高室温离子电导率和较好的机械延展性，是一种极具应用潜力的固体电解质。其制备方式主要分为固相烧结法、高能球磨法和液相法三类。其中，固相烧结法和高能球磨法耗时长，能耗高，且合成的电解质颗粒尺寸较大。相比之下，液相法以有机溶剂为介质，可以合成颗粒较小的硫化物固体电解质，工艺简单省时，更适用于规模化生产。有鉴于此，本文总结了近年来液相法制备硫化物固体电解质的研究进展，基于原料在溶剂中的溶解状态，分析了悬浮型、溶液型和混合型三种反应类型的反应机理，并进一步探讨了溶剂对电解质纯度、形貌及结晶性的影响。同时，概述了液相法制备的硫化物固体电解质在全固态锂电池中的应用。最后，对硫化物固体电解质液相法合成的优势与局限性进行了全面的分析，以期为该领域的研究提供方向。

关键词: 全固态电池, 硫化物固体电解质, 液相法, 湿化学合成, 反应机理

Abstract:

Current commercialized lithium ion batteries generally suffer from safety issues due to using flammable organic liquid electrolytes. All-solid-state lithium batteries employing solid electrolytes instead of organic liquid electrolytes and separators possess the advantages of both good safety and high energy density, which is expected to be the most promising energy storage devices for the next generation electric vehicles and smart grid. Sulfide solid electrolytes are regarded as crucial components for all-solid-state rechargeable batteries for the merits of their high room temperature ionic conductivities that approaches or exceeds liquid organic electrolytes and excellent mechanical ductility. The preparation methods of sulfide solid electrolytes are mainly divided into three categories, i.e. solid-state sintering, ball milling and liquid-phase method. However, solid-state sintering and ball milling are time-consuming accompanied by high energy consumption. At the same time, the synthesized electrolyte particles are large in size, which seriously limits the practical application of sulfide electrolytes. In contrast, the liquid-phase method, using organic solvents as the medium, can synthesize sulfide solid electrolytes with controlled particle sizes, which is a simple and time-saving process and more suitable for large-scale production. In this review, we begin by introducing the crystal structures and ion transport mechanisms of major sulfide electrolytes including Li₂S-P₂S₅ binary sulfide solid electrolytes, Li₁₀GeP₂S₁₂ and Li₆PS₅X (X = Cl, Br, I) ternary systems, and summarize the progress of sulfide solid electrolytes prepared by liquid phase method in recent years. Based on the solubility state of the reagents in the solvent, the liquid-phase synthesis of sulfide electrolytes can be categorized into suspension type, solution type and mixed type, and their reaction mechanisms are discussed separately. Subsequently, we summarize the effect of solvents on the properties of liquid-phase synthesized sulfide electrolytes, such as purity, morphology, crystallinity and ionic conductivity. In addition, the application of liquid-phase synthesized sulfide solid electrolytes for all-solid-state lithium batteries is presented from six aspects: sulfide electrolytes coated on active materials, electrolyte-active material composites, electrolyte injection into porous electrodes, interfacial modification at solid-solid contact triple-interfaces within electrode layers, electrolyte elemental doping and electrolyte film preparation, which demonstrates the superior scalability of the liquid-phase method and the diverse application prospects. Finally, according to the current research status of the sulfide solid electrolytes synthesized by liquid phase method, the advantages and limitations of the liquid phase synthesis of sulfide solid electrolytes are also analyzed, providing the development direction for the liquid phase synthesized sulfide solid electrolyte for all-solid-state lithium batteries in future.

Key words: All-solid-state battery, Sulfide solid electrolyte, Liquid phase method, Wet-chemical synthesis, Reaction mechanism

门明阳, 吴敬华, 刘高瞻, 张婧, 张妮妮, 姚霞银. 液相法制备硫化物固体电解质及其在全固态锂电池中的应用[J]. 物理化学学报, 2025, 41(1), 100004. doi: 10.3866/PKU.WHXB202309019

Mingyang Men, Jinghua Wu, Gaozhan Liu, Jing Zhang, Nini Zhang, Xiayin Yao. Sulfide Solid Electrolyte Synthesized by Liquid Phase Approach and Application in All-Solid-State Lithium Batteries[J]. Acta Phys. -Chim. Sin. 2025, 41(1), 100004. doi: 10.3866/PKU.WHXB202309019

链接本文: https://www.whxb.pku.edu.cn/CN/10.3866/PKU.WHXB202309019

https://www.whxb.pku.edu.cn/CN/Y2025/V41/I1/100004

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Sulfide solid electrolyte	Ionic conductivity (S∙cm⁻¹)	Temperature (℃)	Solvent	Synthesis type	Reference
Li₃PS₄	1.6 × 10⁻⁴	25	THF	Suspension type	42
Li₃PS₄	3.3 × 10⁻⁴	25	EA	Suspension type	44
Li₃PS₄	1.2 × 10⁻⁴	30	ACN	Suspension type	53
Li₃PS₄	6.4 × 10⁻⁶	20	DMC	Suspension type	47
Li₃PS₄	2.3 × 10⁻⁶	25	NMF	Suspension type	50
Li₃PS₄	5.0 × 10⁻⁵	25	EDA	Solution type	54
Li₃PS₄	2.0 × 10⁻⁴	30	THF-O-xylene	Solution type	55
Li₇PS₆	1.1 × 10⁻⁴	30	EtOH	Solution type	56
Li₇P₃S₁₁	1.0 × 10⁻³	–	ACN	Suspension type	43
Li₇P₃S₁₁	1.05 × 10⁻³	–	EA	Suspension type	45
Li₇P₃S₁₁	2.7 × 10⁻⁴	25	DME	Solution type	40
Li₄PS₄I	1.0 × 10⁻³	25	EP	Suspension type	57
Li₄PS₄I	1.2 × 10⁻⁴	25	DME	Mixed type	58
Li_3.2P_0.8Sn_0.2S₄	1.9 × 10⁻⁴	30	EDA-EDT-THF	Suspension type	59
Li_3.25Ge_0.25P_0.75S₄	1.82 × 10⁻⁴	30	Hydrazine	Dissolution-precipitation type	60
80Li₂S∙20P₂S₅	2.6 × 10⁻⁶	–	NMF	Dissolution-precipitation type	49
Li₁₀GeP₂S₁₂	1.6 × 10⁻³	–	DME-THF	Suspension type	61
Li₁₀GeP₂S₁₂	1.2 × 10⁻³	30	EDA-ET	Solution type	62
Li₁₀GeP₂S₁₂	1.8 × 10⁻³	25	EtOH-THF	Mixed type	63
Li_5.5PS_4.5Cl_1.5	2.87 × 10⁻³	25	EDA	Mixed type	64
Li₆PS₅Cl	1.3 × 10⁻³	30	EDA-EDT	Solution type	62
Li₆PS₅Cl	2.1 × 10⁻⁴	30	EtOH	Solution type	52
Li₆PS₅Cl	1.1 × 10⁻³	30	EA	Mixed type	65
Li₆PS₅Cl	2.79 × 10⁻³	25	ACN	Mixed type	66
Li₆PS₅Cl	1.4 × 10⁻⁵	–	EtOH	Dissolution-precipitation type	51
Li₆PS₅Br	3.1 × 10⁻³	25	THF-EtOH	Solution type	67
Li₆PS₅Br	1.9 × 10⁻⁴	25	EtOH	Dissolution-precipitation type	68

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液相法制备硫化物固体电解质及其在全固态锂电池中的应用

Sulfide Solid Electrolyte Synthesized by Liquid Phase Approach and Application in All-Solid-State Lithium Batteries

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