LLTO Solid Electrolyte Particle Synthesis via Low-Temperature Heat Treatment

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Solution Overview

Problem

Existing methods for preparing solid electrolyte particles for lithium secondary batteries involve high-temperature, long-duration processes, resulting in large particle diameters and non-uniform distributions, which limit the contact area with electrodes and ion mobility, posing safety concerns and performance issues.

Innovation Solution

A method involving a precursor solution of titanium, lanthanum, and lithium precursors in an aqueous or organic solvent, heat-treated at lower temperatures for shorter durations to produce solid electrolyte particles with an average diameter of 20 nm to 100 nm and uniform distribution, enhancing specific surface area and lithium ion mobility.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Reliability

If high-temperature heat treatment (1200°C or more) is used to synthesize LLTO solid electrolyte, then the chemical stability and lithium ion conductivity are improved, but the manufacturing cost increases and energy consumption increases

Engineering Contradiction:
Improvechemical stability and lithium ion conductivityVSAvoidenergy consumption
Core Design Contradiction:
ReliabilityVSUse of energy by stationary object

Solution Approach 1:

The patent changes the heat treatment temperature parameter from conventional 1200°C or more to 900-1100°C, and adjusts the heat treatment time parameter to achieve optimal balance between product quality and energy consumption. This parameter optimization resolves the contradiction by maintaining chemical stability and lithium ion conductivity while significantly reducing energy consumption.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent uses preliminary calcination of precursors before the final heat treatment to pre-form the perovskite structure. This preliminary action allows the main heat treatment to be conducted at lower temperatures (900-1100°C) while still achieving the desired chemical stability and lithium ion conductivity, thereby reducing energy consumption.

Inventive Principle:
Principle #10Preliminary action

2Reliability

If high-temperature heat treatment (1200°C or more) is used for a long period of time to synthesize LLTO, then the chemical stability is improved, but the manufacturing time increases and productivity decreases

Engineering Contradiction:
Improvechemical stabilityVSAvoidmanufacturing time
Core Design Contradiction:
ReliabilityVSProductivity

Solution Approach 1:

The patent optimizes the heat treatment temperature parameter to 900-1100°C and adjusts the time parameter to 1-24 hours, creating an optimized parameter combination that achieves chemical stability faster than conventional methods. This resolves the contradiction by maintaining reliability while reducing manufacturing time to enhance productivity.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The preliminary calcination step prepares the precursors in advance, allowing the final heat treatment to be completed in 1-24 hours at lower temperatures. This preliminary action reduces the total manufacturing time while ensuring chemical stability, thereby improving productivity.

Inventive Principle:
Principle #10Preliminary action

3Reliability

If conventional heat treatment is used to prepare LLTO solid electrolyte, then the material is obtained, but the particle diameter is large (few hundred nm to few μm) resulting in limited contact area with electrodes

Engineering Contradiction:
Improvematerial stabilityVSAvoidcontact area with electrode
Core Design Contradiction:
ReliabilityVSArea of stationary object

Solution Approach 1:

The patent changes the heat treatment temperature parameter to a lower range (900-1100°C) and optimizes the time parameter to control particle growth. This parameter optimization produces particles with diameter of 100 nm or less while maintaining material stability, thereby increasing the contact area with electrodes.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The preliminary calcination of precursors creates a fine precursor structure that limits particle growth during final heat treatment. This preliminary action ensures that the resulting LLTO particles have small diameters (100 nm or less) with large specific surface area, increasing contact area with electrodes while maintaining stability.

Inventive Principle:
Principle #10Preliminary action

4Length of moving object

If grinding is used to decrease the particle diameter of LLTO solid electrolyte, then the particle diameter is reduced, but the particle diameter distribution becomes non-uniform

Engineering Contradiction:
Improveparticle diameterVSAvoidparticle diameter distribution uniformity
Core Design Contradiction:
Length of moving objectVSManufacturing precision

Solution Approach 1:

The patent uses preliminary calcination of precursors to establish a fine and uniform precursor structure before final heat treatment. This preliminary action controls nucleation and growth during heat treatment, producing uniform particle diameter distribution (standard deviation of 10 nm or less) without requiring grinding, thereby maintaining manufacturing precision.

Inventive Principle:
Principle #10Preliminary action

Solution Approach 2:

The patent replaces the mechanical grinding system with a chemical-thermal system (controlled heat treatment at 900-1100°C). This substitution achieves particle size reduction through controlled crystallization rather than mechanical force, resulting in uniform particle diameter distribution without the non-uniformity caused by grinding.

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

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 allows for the production of solid electrolyte particles with improved ionic conductivity and increased contact area, leading to enhanced charge and discharge performance and safety in lithium secondary batteries.

Implementation Method 1

heat treating the precursor solution to form solid electrolyte particles

Methodology Applied
Scientific EffectSolid-state reaction: Chemical Bonding

Data Source

PatentUS10128531B2Solid electrolyte particles, preparation method thereof, and lithium secondary battery comprising the same
Publication Date: 2018.11.13 LG ENERGY SOLUTION LTD
  • US10128531B2 patent drawing
  • US10128531B2 patent drawing
  • US10128531B2 patent drawing

AI summary

Provided are a method of preparing solid electrolyte particles of Chemical Formula 1 including preparing a precursor solution by mixing a titanium precursor, a lanthanum precursor, and a lithium precursor in an aqueous or organic solvent, and heat treating the precursor solution, solid electrolyte particles prepared thereby, and a lithium secondary battery including the solid electrolyte particles:Li3xLa(2/3-x)TiO3(0<x<0.16).  <Chemical Formula 1>According to a method of preparing solid electrolyte particles according to an embodiment of the present invention, solid electrolyte particles may be easily prepared by heat treating at low temperature for a short period of time.