Lithium Sulfide Powder Process for Fine Particle Solid Electrolytes

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Solution Overview

Problem

Commercially available lithium sulfide (Li2S) powders have low cycling stability, high initial activation potential, and large particle sizes, which hinder their effectiveness as battery components, and existing methods require complex raw materials, high temperatures, and catalysts.

Innovation Solution

A process to produce Li2S powder with a d50-value of less than 10 μm, specific surface area of more than 5 m2/g, and a high percentage of pores below 20 nm, achieved by grinding and heating lithium hydroxide monohydrate to reduce particle size and water content, then reacting it with a sulfide reactant without a catalyst or solvent, at low temperatures.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Ease of manufacture

If conventional methods are used to produce Li2S powder, then the production process is simpler, but the particle size is large (over 100 μm) and requires further processing

Engineering Contradiction:
Improveproduction process simplicityVSAvoidparticle size
Core Design Contradiction:
Ease of manufactureVSLength of moving object

Solution Approach 1:

The patent performs preliminary grinding of lithium hydroxide monohydrate to obtain fine particles (d50 < 10 μm) before the reaction with sulfur source. This preliminary size reduction action ensures that the final Li2S powder has the desired fine particle size without requiring additional processing steps after production.

Inventive Principle:
Principle #10Preliminary action

2Speed

If high temperature processing is used, then the reaction kinetics are improved, but the energy consumption and process complexity increase

Engineering Contradiction:
Improvereaction kineticsVSAvoidenergy consumption
Core Design Contradiction:
SpeedVSUse of energy by stationary object

Solution Approach 1:

The patent changes the particle size parameter of the reactants (using ground LiOH monohydrate with d50 < 10 μm) to increase the reaction surface area. This parameter change allows the reaction to proceed efficiently at lower temperatures (100-260°C), reducing energy consumption while maintaining good reaction kinetics.

Inventive Principle:
Principle #35Parameter changes

3Ease of manufacture

If Li2S powder with large particle size is used, then the manufacturing cost is lower, but the cycling stability and activation potential are poor

Engineering Contradiction:
Improvemanufacturing costVSAvoidcycling stability
Core Design Contradiction:
Ease of manufactureVSReliability

Solution Approach 1:

The patent performs preliminary grinding of lithium hydroxide monohydrate to obtain fine particles (d50 < 10 μm) before the reaction with sulfur source. This preliminary size reduction action ensures that the final Li2S powder has the desired fine particle size without requiring additional processing steps after production.

Inventive Principle:
Principle #10Preliminary action

4Productivity

If complex raw materials and catalysts are used, then the reaction efficiency is improved, but the process complexity and cost increase

Engineering Contradiction:
Improvereaction efficiencyVSAvoidprocess complexity
Core Design Contradiction:
ProductivityVSDevice complexity

Solution Approach 1:

The patent extracts and eliminates the need for catalysts and complex raw materials from the conventional process. By using ground lithium hydroxide monohydrate as the reactant, the process achieves efficient Li2S production without requiring any catalysts, thereby simplifying the overall process while maintaining high reaction efficiency.

Inventive Principle:
Principle #2Taking out (Extraction)

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 resulting Li2S powder exhibits improved agglomeration and dispersion properties, reducing the need for additional processing and making it suitable for high-quality solid electrolytes without increasing process complexity or cost.

Implementation Method 1

heating such LiOH powder C at a temperature of less than 180° C., in order to obtain the LiOH powder A

Methodology Applied
Scientific EffectEvaporation: Evaporation

Implementation Method 2

reacting such LiOH powder A with a sulfide reactant, in order to obtain the Li2S powder

Methodology Applied
Scientific EffectChemical reaction: Chemical Bonding

Data Source

PatentUS20250002342A1Process of obtaining a powder of lithium sulfide, and use thereof to prepare a lps compound
Publication Date: 2025.01.02 SPECIALTY OPERATIONS FRANCE

AI summary

The present disclosure relates to a process of obtaining a powder of lithium sulfide (Li2S powder) having a d50-value of less than 10 μm, a specific surface area of more than 5 m2/g, a total pore volume of more than 0.035 cm3/g and a percentage of total pore volume constituted of pore with diameter below 20 nm of more than 20%, comprising the steps of: a) providing a powder of lithium hydroxide having a d50-value of less than 10 μm and presenting a residual water content below 5 wt. % (LiOH powder A), and b) reacting such LiOH powder A with a sulfide reactant, in order to obtain the Li2S powder. The present disclosure also relates to the powder of lithium sulfide obtained from such process and the use of such Li2S powder to prepare a solid compound of formula (I): LiaPSbXc wherein —X represents at least one halogen element; —a represents a number from 3.0 to 6.0; —b represents a number from 3.5 to 5.0; and —c represents a number from 0 to 3.0.