Preparation method of high-purity lithium sulfide and sulfide solid electrolyte, and solid-state battery

By introducing sulfur powder into lithium sulfate and a highly reactive carbon source, and combining wet ball milling, spray drying, and deep purification steps, the problem of high impurity content in lithium sulfide preparation was solved, resulting in high-purity lithium sulfide and improving the conductivity and battery performance of the sulfide solid electrolyte.

CN122118100APending Publication Date: 2026-05-29SHENZHEN ZHISHENG ENERGY TECHNOLOGY CO LTD
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Patent Information

Application Number
CN202610183870.X
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2026-02-09
Publication Date
2026-05-29

AI Technical Summary

Technical Problem

In the existing technology, the carbon reduction capacity in the preparation process of lithium sulfide is limited, resulting in a high impurity content, especially the formation of impurities such as lithium oxide and lithium carbonate, which affects the ionic conductivity and battery performance of sulfide solid electrolytes.

Method used

Lithium sulfate, a highly reactive carbon source, and sulfur powder were mixed in deionized water and then wet-milled and spray-dried to form microsphere precursors. These precursors were then subjected to reduction calcination and dissolution evaporation crystallization, followed by deep purification with strontium nitrate to obtain high-purity lithium sulfide.

Benefits of technology

It significantly reduces oxygen and carbon residues in lithium sulfide, improves the purity and conductivity of lithium sulfide, ensures the stability and consistency of mass production, and enhances the electrochemical performance of solid-state batteries.

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Abstract

The invention provides a preparation method of high-purity lithium sulfide and sulfide solid electrolyte and a solid-state battery. The preparation method of the high-purity lithium sulfide comprises the following steps: adding lithium sulfate, a high-reaction-activity carbon source and sulfur powder into water, and carrying out wet ball-milling treatment to obtain homogeneous slurry; carrying out spray drying treatment on the homogeneous slurry to obtain a microsphere precursor; reducing and calcining the microsphere precursor to obtain coarsened lithium sulfide; adding water into the coarsened lithium sulfide for dissolving, filtering, evaporating and concentrating to obtain crystallized lithium sulfide; and calcining and crushing the crystalline lithium sulfide to obtain the high-purity lithium sulfide. Sulfur powder is introduced into lithium sulfate and a high-reaction-activity carbon source, so that deep reduction of sulfate ions is promoted, side reaction and generation of Li2O are inhibited, and the oxygen content and carbon residues are reduced, so that lithium sulfide with few oxygen-containing impurities and high purity is obtained; through combination of wet ball milling and spray drying, a microsphere precursor with uniform components is obtained, and subsequent high-temperature solid-phase reaction is facilitated.
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