Lithium Titanium Sulfide Synthesis via Mechanical Milling

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Solution Overview

Problem

The existing synthesis process for lithium titanium sulfide is limited by the morphology and size control of titanium sulfide powders, which are expensive and difficult to synthesize, restricting the versatility of the process and preventing the achievement of desired electrochemical properties.

Innovation Solution

A process involving the milling of a particulate mixture composed of lithiated powder, transition metal powder, and chalcogen powder, where the powders are mixed and milled to form a material with a crystalline nature and electrochemical properties similar to those obtained from traditional methods, allowing for the synthesis of materials like lithium titanium sulfide with varying stoichiometric coefficients and crystallographic structures.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If titanium sulfide salt is used as precursor, then synthesis is achieved, but particle morphology and size control is limited and cost is high

Engineering Contradiction:
Improveparticle morphology and size controlVSAvoidsynthesis difficulty and cost
Core Design Contradiction:
Manufacturing precisionVSEase of manufacture

Solution Approach 1:

The synthesis is divided into two independent stages: first synthesizing titanium sulfide particles with controlled morphology and size, then reacting them with lithium sulfide. This segmentation allows optimization of each stage independently, enabling better particle control while simplifying the overall manufacturing process.

Inventive Principle:
Principle #1Segmentation

Solution Approach 2:

Titanium sulfide particles are prepared in advance with specific morphology and size control before the final reaction with lithium sulfide. This preliminary preparation enables precise control over the final product's particle characteristics while using commercially available precursors.

Inventive Principle:
Principle #10Preliminary action

2Adaptability or versatility

If transition metal powder is used instead of salt, then versatility is improved, but oxidation risk increases

Engineering Contradiction:
Improvesynthetic process versatilityVSAvoidoxidation and flammability
Core Design Contradiction:
Adaptability or versatilityVSObject-affected harmful factors

Solution Approach 1:

The milling process using transition metal powder is conducted in an inert atmosphere (argon or nitrogen) to prevent oxidation of the reactive metal powder. This allows the use of versatile metal powder precursors while eliminating the harmful oxidation effect.

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

Solution Approach 2:

An inert gas atmosphere acts as an intermediary medium that allows direct contact between reactive metal powder and other precursors during milling without allowing oxidation to occur, thus enabling versatile synthesis while protecting against harmful effects.

Inventive Principle:
Principle #24Intermediary (Mediator)

3Ease of manufacture

If traditional salt-based process is used, then synthesis is achieved, but particle size and morphology modification range is limited

Engineering Contradiction:
Improvesynthesis feasibilityVSAvoidparticle size and morphology range
Core Design Contradiction:
Ease of manufactureVSAdaptability or versatility

Solution Approach 1:

The process parameters (milling time, ball-to-powder ratio, atmosphere conditions, precursor ratios) are systematically varied to achieve a wide range of particle sizes and morphologies. This parameter optimization enables versatile particle engineering while maintaining synthesis feasibility.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The milling-based synthesis process serves multiple functions: it mixes precursors, controls particle size, adjusts morphology, and promotes reaction simultaneously. This multi-functionality allows versatile particle engineering while keeping the process simple and feasible.

Inventive Principle:
Principle #6Universality (Multi-functionality)

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 process achieves materials with high reversible capacity, such as lithium titanium sulfide, with electrochemical properties identical to those produced by traditional methods, while being more versatile and capable of synthesizing materials not feasible with traditional salt-based processes, such as lithium selenium titanium compounds, and offers a wider range of particle size and morphology modifications.

Implementation Method 1

The energy provided by the milling is sufficient for the titanium sulfide to react with the lithium sulfide to form lithium titanium sulfide

Methodology Applied
Scientific EffectMechanical energy input through planetary ball milling: Mechanical Force

Data Source

PatentUS11618076B2Synthesis method
Publication Date: 2023.04.04 COMMISSARIAT A LENERGIE ATOMIQUE ET AUX ENERGIES ALTERNATIVES
  • US11618076B2 patent drawing

AI summary

A process for synthesizing a material, includes:(a) providing a plurality of powders including at least one lithiated powder including lithium, at least one TM powder including, for more than 95.0% of its mass, a transition metal chosen from titanium; cobalt, manganese, nickel, niobium, tin, iron and mixtures thereof, and at least one chalcogen powder including, for more than 95.0% of its mass, a chalcogen element chosen from sulfur, selenium, tellurium and mixtures thereof,(b) preparing a particulate mixture by mixing all the powders of the plurality or by mixing one of the powders of the plurality with a milled material obtained by; milling a particulate assembly formed by mixing at least two of the other powders of the plurality, and(c) milling the particulate fixture to form the material.