KR-102962195-B1 - MANUFACTURING METHOD OF SOLID ELECTROLYTE FOR ALL SOLID STATE BATTERY USING LIQUID STIRRING

KR102962195B1KR 102962195 B1KR102962195 B1KR 102962195B1KR-102962195-B1

Abstract

The present invention relates to a method for manufacturing a solid electrolyte for an all-solid-state battery by reacting the starting materials by stirring in a liquid phase without grinding them.

Inventors

장용준
송인우
최선호
김사흠
이상헌

Assignees

현대자동차주식회사
기아 주식회사

Dates

Publication Date: 20260507
Application Date: 20210203

Claims (12)

A step of preparing starting materials including elemental lithium powder, elemental sulfur powder, and a phosphorus compound; A step of introducing the above starting material into a solvent and stirring to cause a reaction; A step of drying the reactants; and The method includes the step of heat-treating the dried reaction product; The above-mentioned lithium powder and sulfur powder are not soluble in the solvent, and A method for manufacturing a solid electrolyte characterized by stirring the above-mentioned lithium powder and sulfur powder without dissolving them in a solvent to cause collisions between the powders and trigger a reaction.
In paragraph 1, A method for manufacturing a solid electrolyte comprising the above starting material further including a lithium halogen compound (LiX, where X is Br, Cl, or I).
In paragraph 1, A method for manufacturing a solid electrolyte characterized in that the above-mentioned starting material does not contain a lithium sulfur compound.
In paragraph 1, A method for manufacturing a solid electrolyte in which the weight ratio of the starting material to the solvent is 1:20 to 1:50.
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In paragraph 1, The above reaction is carried out using a stirrer, and The above stirrer A container in which a space is formed to accommodate a solvent and a starting material; A stirring blade disposed inside the above container; and A method for manufacturing a solid electrolyte comprising a stirring rod connected to the stirring blade and extended along the longitudinal direction of the container.
In paragraph 6, A method for manufacturing a solid electrolyte in which a reaction occurs by rotating the stirring rod and inducing collision or contact between starting materials within the solvent by the rotational force of the stirring blade.
In paragraph 1, A method for manufacturing a solid electrolyte, wherein the above drying is performed in a vacuum atmosphere at a temperature of 25°C to 250°C for 5 to 15 hours.
In paragraph 1, The above drying is performed in a vacuum atmosphere, Primary drying at a temperature of 25℃ or higher and less than 50℃ for 1 to 3 hours; Secondary drying at a temperature of 50℃ or higher and less than 100℃ for 1 to 3 hours; Third drying at a temperature of 100℃ or higher and less than 150℃ for 1 to 3 hours; Fourth drying at a temperature of 150℃ or higher and less than 200℃ for 1 to 3 hours; and A method for manufacturing a solid electrolyte, comprising: fifth drying at a temperature of 200℃ to 250℃ for 1 to 3 hours.
In Paragraph 9, A method for manufacturing a solid electrolyte, wherein the above first to fifth drying is performed under conditions of continuously or discontinuously increasing the temperature from 25°C to a temperature within the range of 200°C to 250°C.
In paragraph 1, A method for manufacturing a solid electrolyte, wherein the above heat treatment is performed at 400°C to 600°C for 1 hour to 5 hours.
In paragraph 1, A method for manufacturing a solid electrolyte in which the above solid electrolyte has crystallinity.

Description

Manufacturing Method of Solid Electrolyte for All Solid State Batteries Using Liquid Stirring The present invention relates to a method for manufacturing a solid electrolyte for an all-solid-state battery by reacting the starting materials by stirring in a liquid phase without grinding them. Rechargeable batteries are used as high-capacity power storage batteries for electric vehicles and battery energy storage systems, as well as as high-performance energy sources for small portable electronic devices such as mobile phones, camcorders, and laptops. Research is currently underway to reduce component weight and power consumption with the goal of miniaturizing portable electronic devices and enabling long-term continuous use; in this context, there is a demand for rechargeable batteries that are compact yet capable of achieving high capacity. As a secondary battery, lithium-ion batteries have a higher energy density, larger capacity per unit area, a lower self-discharge rate, and a longer lifespan than nickel-manganese or nickel-cadmium batteries. Furthermore, they have no memory effect, offering convenience of use and long lifespan characteristics. However, as batteries for next-generation electric vehicles, lithium-ion batteries face various problems such as safety issues due to overheating, low energy density, and low power output. In particular, safety issues caused by liquid electrolytes can lead to accidents resulting in fires. To overcome the problems associated with lithium-ion batteries using liquid electrolytes, research and development of all-solid-state lithium-ion batteries using solid electrolytes has recently been actively underway. All-solid-state lithium-ion batteries have the advantage of being able to increase volumetric energy density by about five times compared to conventional batteries because they use a solid electrolyte, thereby eliminating the ignition problem that occurs with liquid electrolytes, and because a bipolar structure is possible. However, solid electrolytes used in all-solid-state lithium-ion batteries are very expensive, difficult to mass-produce, and have limitations in particle size control. These are the biggest obstacles to the commercialization of all-solid-state lithium-ion batteries. Therefore, it is necessary to develop new solid electrolyte synthesis methods that can overcome these limitations. FIG. 1 is a flowchart illustrating a method for manufacturing a solid electrolyte according to the present invention. FIG. 2 schematically illustrates a stirrer according to the present invention. Figure 3a is the X-ray diffraction (XRD) analysis result of the solid electrolyte according to Example 1. Figure 3b is the result of X-ray diffraction analysis of the solid electrolyte according to Example 2. Figure 3c is the result of X-ray diffraction analysis of the solid electrolyte according to Example 3. The above objects, other objects, features, and advantages of the present invention will be easily understood through the following preferred embodiments associated with the accompanying drawings. However, the present invention is not limited to the embodiments described herein and may be embodied in other forms. Rather, the embodiments introduced herein are provided to ensure that the disclosed content is thorough and complete and to ensure that the spirit of the invention is sufficiently conveyed to a person skilled in the art. In describing each drawing, similar reference numerals have been used for similar components. In the attached drawings, the dimensions of the structures are depicted enlarged from their actual size for clarity of the invention. Terms such as "first," "second," etc., may be used to describe various components, but said components should not be limited by said terms. These terms are used solely for the purpose of distinguishing one component from another. For example, without departing from the scope of the invention, the first component may be named the second component, and similarly, the second component may be named the first component. A singular expression includes a plural expression unless the context clearly indicates otherwise. In this specification, terms such as "comprising" or "having" are intended to specify the existence of the features, numbers, steps, actions, components, parts, or combinations thereof described in the specification, and should be understood as not precluding the existence or addition of one or more other features, numbers, steps, actions, components, parts, or combinations thereof. Furthermore, when a part such as a layer, film, region, or plate is described as being "on" another part, this includes not only the case where it is "immediately above" the other part, but also the case where there is another part in between. Conversely, when a part such as a layer, film, region, or plate is described as being "below" another part, this includes not only the case where it is "immediately below" the other part, but also