Sulfur-Containing Complex for Solid Electrolyte Purity

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Solution Overview

Problem

The existing method for producing sulfide solid electrolytes results in the formation of impurities like oxygen-containing lithium halide compounds, which reduces the conversion efficiency of lithium compounds and affects battery performance.

Innovation Solution

A sulfur-containing complex is developed, characterized by a shift in the diffraction angle of lithium halide peaks towards lithium sulfide peaks in X-ray diffractometry, using a method that involves heating a solution of lithium hydrosulfide and lithium halide in the presence of hydrogen sulfide, eliminating oxygen-containing lithium halides and improving purity and efficiency.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Productivity

If conventional methods are used to produce lithium sulfide and lithium halide separately and then combine them, then the production process is simple, but oxygen-containing lithium halide impurities are formed and conversion efficiency decreases

Engineering Contradiction:
Improveconversion efficiencyVSAvoidpurity of lithium sulfide
Core Design Contradiction:
ProductivityVSManufacturing precision

Solution Approach 1:

The patent combines the production of lithium sulfide and lithium halide into a single integrated reaction system. Lithium hydroxide reacts with hydrogen sulfide to form lithium sulfide in situ, while lithium halide is simultaneously present in the solution. This merging of previously separate production steps eliminates the formation of oxygen-containing impurities and achieves high purity lithium sulfide with complete conversion efficiency.

Inventive Principle:
Principle #5Merging (Combining)

Solution Approach 2:

The patent utilizes temperature control as a key parameter to manage the reaction process. By heating the solution to evaporate water and control the reaction conditions, the system achieves complete conversion of lithium hydroxide to lithium sulfide while preventing impurity formation. The temperature parameter change enables the simultaneous achievement of high purity and high conversion efficiency.

Inventive Principle:
Principle #35Parameter changes

2Productivity

If drying equipment and energy are used to remove solvent and water from lithium sulfide and lithium halide, then the materials can be used as raw materials, but production efficiency decreases and equipment complexity increases

Engineering Contradiction:
Improveproduction efficiencyVSAvoiddrying equipment
Core Design Contradiction:
ProductivityVSDevice complexity

Solution Approach 1:

The patent extracts and eliminates the drying step from the production process. By designing the reaction system to produce lithium sulfide and lithium halide in a form that can be directly used as raw materials without requiring solvent removal, the patent removes the need for drying equipment and associated energy consumption, thereby improving production efficiency and reducing device complexity.

Inventive Principle:
Principle #2Taking out (Extraction)

Solution Approach 2:

The patent performs preliminary action by pre-dissolving lithium halide in the reaction solution before the sulfurization reaction occurs. This preliminary preparation ensures that when lithium sulfide is formed in situ, both components are already in the correct form and concentration for direct use as raw materials, eliminating the need for subsequent drying or purification steps.

Inventive Principle:
Principle #10Preliminary action

3Manufacturing precision

If lithium hydroxide is sulfurized using hydrogen sulfide in a heating environment, then lithium sulfide is produced, but oxygen-containing lithium halide impurities are formed

Engineering Contradiction:
Improvepurity of lithium sulfideVSAvoidoxygen-containing lithium halide impurities
Core Design Contradiction:
Manufacturing precisionVSObject-generated harmful factors

Solution Approach 1:

The patent creates an inert sulfur-rich environment by saturating the solution with hydrogen sulfide gas before and during the heating process. This inert atmosphere prevents oxidation reactions that would otherwise form oxygen-containing lithium halide impurities. The hydrogen sulfide atmosphere protects the lithium halide from reacting with oxygen while allowing complete sulfurization of lithium hydroxide to lithium sulfide.

Inventive Principle:
Principle #39Inert atmosphere (Inert environment)

Solution Approach 2:

The patent applies preliminary anti-action by pre-saturating the solution with hydrogen sulfide before initiating the sulfurization reaction. This preliminary action creates a protective sulfur-rich environment that prevents the formation of oxygen-containing impurities during the heating process, thereby eliminating the harmful side reactions before they can occur.

Inventive Principle:
Principle #9Preliminary anti-action

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 approach results in a sulfur-containing complex with fewer impurities, enhancing the production efficiency and battery performance by reducing oxygen-containing lithium halide formation and improving the conversion of lithium compounds.

Implementation Method 1

hydrogen sulfide is made to circulate through a solution containing a lithium hydroxide and a lithium halide in a heating environment to sulfurize the lithium hydroxide into a lithium hydrosulfide

Methodology Applied
Scientific EffectChemical reaction: Chemical Bonding

Implementation Method 2

exhibiting, in X-ray diffractometry using a CuKα ray, the diffraction angle of the peak of lithium halide shifting toward the diffraction angle of the peak of lithium sulfide

Methodology Applied
Scientific EffectX-ray diffraction: X-Ray

Data Source

PatentUS10865108B2Complex comprising sulfur, a method for manufacturing the same, and a method for manufacturing a solid electrolyte
Publication Date: 2020.12.15 IDEMITSU KOSAN CO LTD
  • US10865108B2 patent drawing
  • US10865108B2 patent drawing
  • US10865108B2 patent drawing

AI summary

To provide a sulfur-containing complex having few impurities, a method for producing the complex at a higher production efficiency, and a method for producing a solid electrolyte using the complex, a sulfur-containing complex, containing a lithium sulfide and a lithium halide, exhibiting, in X-ray diffractometry using a CuKα ray, the diffraction angle of the peak of lithium halide shifting toward the diffraction angle of the peak of lithium sulfide, and not containing an oxygen-containing lithium halide represented by Li3OX (where X represents a halogen element) is provided. And a production method for a sulfur-containing complex including heating a solution containing a lithium hydrosulfide and a lithium halide in the presence of hydrogen sulfide is also provided.