Sulfide Solid Electrolyte Two-Stage Solvent Synthesis

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Solution Overview

Problem

The high temperature dependency of ion conductivity in sulfide-based solid electrolytes hinders their performance in solid secondary batteries, requiring a method to reduce activation energy and improve conductivity while also addressing the energy and cost inefficiencies of current synthesis methods.

Innovation Solution

A method involving a two-stage solution process using specific solvents, where Li2S, P2S5, and LiI are mixed in a first solvent with a C1-C3 alkyl group or cyclic ether, followed by a second solvent with a C1-C10 hydrocarbon substituted with an alkoxy group, to produce a sulfide-based solid electrolyte with low activation energy and high ion conductivity.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Reliability

If a mechanical milling process is used for solid-phase synthesis, then the sulfide-based solid electrolyte can be prepared, but the input energy is large and synthesis time is long

Engineering Contradiction:
Improvesynthesis feasibilityVSAvoidinput energy
Core Design Contradiction:
ReliabilityVSUse of energy by moving object

Solution Approach 1:

The patent replaces the mechanical milling process with a solution-phase synthesis method using organic solvents. The starting materials are dissolved in a first organic solvent, reacted to form a precursor, then treated with a second organic solvent to obtain the sulfide-based solid electrolyte. This chemical solution approach substitutes the high-energy mechanical grinding process, significantly reducing input energy requirements while maintaining synthesis feasibility.

Inventive Principle:
Principle #28Mechanics substitution (Replace mechanical system)

Solution Approach 2:

The patent changes the synthesis parameters by introducing specific organic solvents (first solvent with C1-C3 alkyl group or cyclic ether, second solvent with C1-C10 hydrocarbon and alkoxy group) and controlling reaction conditions. This parameter optimization enables the synthesis to proceed under milder conditions with lower energy input compared to mechanical milling, while achieving the desired product with good ion conductivity.

Inventive Principle:
Principle #35Parameter changes

2Reliability

If a mechanical milling process is used for solid-phase synthesis, then the sulfide-based solid electrolyte can be prepared, but the synthesis time is long

Engineering Contradiction:
Improvesynthesis feasibilityVSAvoidsynthesis time
Core Design Contradiction:
ReliabilityVSLoss of time

Solution Approach 1:

The patent replaces the time-consuming mechanical milling process with a solution-phase synthesis method. The chemical reactions in solution proceed more rapidly than solid-state mechanical reactions, significantly reducing synthesis time while maintaining the ability to produce the sulfide-based solid electrolyte with desired properties.

Inventive Principle:
Principle #28Mechanics substitution (Replace mechanical system)

Solution Approach 2:

By optimizing reaction parameters such as solvent selection, temperature, and reaction time in the solution-phase process, the patent achieves faster synthesis kinetics compared to mechanical milling. The use of appropriate organic solvents facilitates rapid dissolution and reaction of starting materials, reducing overall synthesis time.

Inventive Principle:
Principle #35Parameter changes

3Reliability

If a mechanical milling process is used for solid-phase synthesis, then the sulfide-based solid electrolyte can be prepared, but it is difficult to increase the scale of the process

Engineering Contradiction:
Improvesynthesis feasibilityVSAvoidscale-up capability
Core Design Contradiction:
ReliabilityVSProductivity

Solution Approach 1:

The patent replaces the mechanical milling process with a solution-phase synthesis that is more amenable to scale-up. Solution chemistry allows for easier control of reaction conditions, better heat and mass transfer, and simpler scaling from laboratory to production scale compared to mechanical grinding processes, thereby improving productivity and scale-up capability.

Inventive Principle:
Principle #28Mechanics substitution (Replace mechanical system)

4Reliability

If a mechanical milling process is used for solid-phase synthesis, then the sulfide-based solid electrolyte can be prepared, but it is difficult to lower the cost of synthesis

Engineering Contradiction:
Improvesynthesis feasibilityVSAvoidsynthesis cost
Core Design Contradiction:
ReliabilityVSEase of manufacture

Solution Approach 1:

The patent replaces the energy-intensive mechanical milling process with a solution-phase synthesis method that consumes less energy and uses readily available organic solvents. This substitution reduces both direct material costs and energy costs, making the synthesis more cost-effective while maintaining the ability to produce the sulfide-based solid electrolyte.

Inventive Principle:
Principle #28Mechanics substitution (Replace mechanical system)

Solution Approach 2:

By optimizing synthesis parameters including solvent selection, reaction conditions, and purification steps, the patent reduces overall manufacturing costs. The use of common organic solvents and simplified processing steps lowers both material and operational expenses compared to mechanical milling methods.

Inventive Principle:
Principle #35Parameter changes

Applied Scientific Principles

This section explains which scientific principles are used to turn an abstract innovation direction into a practical engineering solution.

Function Achieved in This Case

The method efficiently produces a sulfide-based solid electrolyte with improved ion conductivity and reduced temperature dependency, lowering synthesis energy and costs, and enabling the creation of solid secondary batteries with enhanced performance.

Implementation Method 1

first contacting a starting material including Li2S, P2S5, and LiI in a first solvent to provide a precursor

Methodology Applied
Scientific EffectSolvation: Solvation

Implementation Method 2

second contacting the precursor with a second solvent to prepare the sulfide solid electrolyte

Methodology Applied
Scientific EffectSolvation: Solvation

Data Source

PatentUS11127974B2Method of preparing sulfide-based solid electrolyte, sulfide-based solid electrolyte prepared therefrom, and solid secondary battery including the sulfide electrolyte
Publication Date: 2021.09.21 SAMSUNG ELECTRONICS CO LTD
  • US11127974B2 patent drawing
  • US11127974B2 patent drawing
  • US11127974B2 patent drawing

AI summary

A method of preparing a sulfide solid electrolyte, the method including: first contacting a starting materials including Li2S, P2S5, and LiI in a first solvent to provide a precursor; and second contacting the precursor with a second solvent to prepare the sulfide solid electrolyte, wherein the first solvent includes a C1-C3 alkyl group or a cyclic ether compound which is unsubstituted or substituted with a C1-C3 alkoxy group, and the second solvent includes a C1-C10 hydrocarbon substituted with a C1 to C6 alkoxy group.