Sulfide Solid Electrolyte Slurry Circulation to Prevent Halide Settling

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Solution Overview

Problem

The liquid-phase method for producing sulfide solid electrolytes faces challenges in achieving high ionic conductivity due to issues like precipitation of lithium halides during stirring, which reduces reaction efficiency and shifts the composition of the resultant electrolyte.

Innovation Solution

A method involving the use of a reactor with a discharging and returning port to circulate the contents, preventing lithium halides with high specific gravity from precipitating at the bottom, while stirring raw materials like lithium sulfide, phosphorus compounds, and halogen compounds with a complexing agent, such as tetramethylethylenediamine, to promote reaction without pulverization.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Productivity

If lithium halides are stirred in a reactor during sulfide solid electrolyte production, then reaction efficiency is improved, but lithium halides precipitate at the bottom due to high specific gravity, causing compositional shifts and reduced ionic conductivity

Engineering Contradiction:
Improvereaction efficiencyVSAvoidcompositional uniformity
Core Design Contradiction:
ProductivityVSStability of the object's composition

Solution Approach 1:

The patent introduces a circulation system that dynamically moves the reaction mixture between the reactor and a circulation tank, preventing static precipitation of lithium halides while maintaining continuous reaction efficiency. The system transitions from a static mixing process to a dynamic circulation process, ensuring uniform composition throughout the reaction.

Inventive Principle:
Principle #15Dynamics

Solution Approach 2:

The circulation tank acts as an intermediary component between the reactor and the discharge system. It receives the reaction mixture, allows for uniform mixing without direct precipitation in the reactor, and returns the well-mixed slurry to the reactor, thereby mediating the contradiction between reaction efficiency and compositional uniformity.

Inventive Principle:
Principle #24Intermediary (Mediator)

2Stability of the object's composition

If strong stirring is applied to prevent lithium halide precipitation, then compositional uniformity is improved, but fluid splashes and adheres to reactor walls, causing loss of material and potential safety issues

Engineering Contradiction:
Improvecompositional uniformityVSAvoidmaterial loss from splashing
Core Design Contradiction:
Stability of the object's compositionVSLoss of substance

Solution Approach 1:

Instead of using intense stirring that causes splashing, the patent employs a gentle circulation dynamic where the slurry is pumped at controlled rates. This dynamic approach achieves uniform mixing without the harmful effects of violent agitation, preventing material loss while maintaining compositional uniformity.

Inventive Principle:
Principle #15Dynamics

Solution Approach 2:

The patent extracts the mixing function from the reactor itself and relocates it to the circulation tank. The reactor focuses solely on the chemical reaction, while the circulation tank handles the mixing and uniform distribution, separating the functions to avoid splashing and material loss.

Inventive Principle:
Principle #2Taking out (Extraction)

3Loss of substance

If lithium halides remain at the bottom of the reactor, then less material is lost from splashing, but reaction efficiency decreases due to reduced contact between reactants

Engineering Contradiction:
Improvematerial retentionVSAvoidreaction efficiency
Core Design Contradiction:
Loss of substanceVSProductivity

Solution Approach 1:

The circulation system ensures continuous movement of the reaction mixture, preventing lithium halides from settling and remaining inactive at the bottom. The continuous circulation maintains constant contact between reactants, ensuring sustained reaction efficiency without material loss from splashing.

Inventive Principle:
Principle #20Continuity of useful action

Solution Approach 2:

The system creates a dynamic equilibrium where lithium halides are continuously suspended and circulated rather than statically settled. This dynamic approach prevents both precipitation loss and reaction inefficiency by maintaining optimal reactant contact throughout the process.

Inventive Principle:
Principle #15Dynamics

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

This approach efficiently produces sulfide solid electrolytes with high ionic conductivity by maintaining a uniform dispersion of reactants and preventing compositional shifts, enhancing the production efficiency of both amorphous and crystalline sulfide solid electrolytes.

Implementation Method 1

raw material having a large specific gravity such as a lithium halide can be prevented from going down to the bottom of the reactor

Methodology Applied
Scientific EffectGravity: Gravitation

Implementation Method 2

stirring raw materials like lithium sulfide, phosphorus compounds, and halogen compounds with a complexing agent, such as tetramethylethylenediamine, to promote reaction

Methodology Applied
Scientific EffectStirring: Stirring

Data Source

PatentUS20250006987A1Method for producing sulfide solid electrolyte
Publication Date: 2025.01.02 IDEMITSU KOSAN CO LTD
  • US20250006987A1 patent drawing
  • US20250006987A1 patent drawing
  • US20250006987A1 patent drawing

AI summary

[Problem] To provide a method for efficiently producing a sulfide solid electrolyte using a liquid-phase method.[Solution to Problem] A method for producing a sulfide solid electrolyte not using a pulverizer in reacting raw materials, wherein a raw material that contains lithium sulfide, a phosphorus compound and a halogen compound, and a complexing agent are stirred in a reactor while a fluid that contains the contents in the reactor is discharged outside the reactor through a discharging port arranged in the reactor and the fluid that contains the discharged contents is returned back to the reactor through a returning port arranged in the reactor to thereby make the contents-containing fluid circulate therethrough.