Transition Metal Oxyfluoride Cathodes With Low-Temperature Stabilization

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Solution Overview

Problem

Current disordered rocksalt oxyfluoride cathode materials for alkali metal ion cells suffer from metastability and short lifespan due to structural anomalies and surface defects, despite their potential for high capacities and environmental friendliness, with previous stabilization attempts being unsuccessful.

Innovation Solution

A process involving the synthesis of transition metal oxyfluorides through a low-temperature heat treatment under reducing conditions, combined with cold pressing and multiple heat treatments, to achieve structural and surface stabilization, resulting in homogenous and defect-mitigated materials with enhanced crystallite size and electrochemical stability.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Reliability

If conventional high-temperature synthesis methods are used to create disordered rocksalt oxyfluorides, then the materials can be synthesized, but they suffer from structural anomalies, surface defects, and metastability leading to short lifespan

Engineering Contradiction:
Improveelectrochemical stabilityVSAvoidbattery lifespan
Core Design Contradiction:
ReliabilityVSDuration of action of stationary object

Solution Approach 1:

The patent applies parameter changes by conducting heat treatment at low temperatures (150-400°C) under reducing atmosphere conditions, rather than using conventional high-temperature synthesis. This change in temperature and atmospheric parameters stabilizes the disordered rocksalt structure, reduces surface defects, and eliminates structural anomalies, thereby improving electrochemical stability and extending battery lifespan to over 200 cycles

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent uses a reducing atmosphere (inert environment) during heat treatment to prevent oxidation and stabilize the transition metal oxyfluoride structure. This controlled atmospheric environment protects the material from degradation, reduces surface defects, and maintains the metastable disordered rocksalt phase, leading to improved reliability and longer battery operation

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

2Stability of the object's composition

If multiple heat treatments are performed to stabilize the structure, then structural stability improves, but the manufacturing process becomes more complex

Engineering Contradiction:
Improvestructural stabilityVSAvoidprocess complexity
Core Design Contradiction:
Stability of the object's compositionVSDevice complexity

Solution Approach 1:

The patent merges multiple heat treatment steps into a single integrated process where precursors are mixed, cold-pressed, and then subjected to one comprehensive heat treatment at 150-400°C under reducing atmosphere. This consolidation achieves the same structural stabilization effect as multiple separate heat treatments but simplifies the manufacturing process, reducing operational complexity while maintaining compositional stability

Inventive Principle:
Principle #5Merging (Combining)

3Manufacturing precision

If cold pressing is applied to induce faster crystallite growth, then structural stabilization improves, but the equipment requirements and process complexity increase

Engineering Contradiction:
Improvecrystallite growth controlVSAvoidmanufacturing ease
Core Design Contradiction:
Manufacturing precisionVSEase of manufacture

Solution Approach 1:

The patent applies preliminary cold pressing at 100-300 MPa to the precursor mixture before heat treatment. This preliminary mechanical action densifies the powder, improves particle contact, and promotes faster crystallite growth during subsequent low-temperature heat treatment. While cold pressing adds a step, it enables the use of lower temperatures and shorter times, overall simplifying the manufacturing process compared to high-temperature prolonged heating

Inventive Principle:
Principle #10Preliminary 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 process significantly improves the long-term electrochemical stability and capacity retention of alkali metal ion batteries, achieving notable stability over 200 cycles with reduced capacity fading, and allows for large-scale industrial production.

Implementation Method 1

carrying out a first heat treatment

Methodology Applied
Scientific EffectHeat treatment: Heating

Implementation Method 2

low temperature sintering in contrast to spinel-like oxyfluorides

Methodology Applied
Scientific EffectSintering: Sintering

Implementation Method 3

heat treatment under reducing conditions

Methodology Applied
Scientific EffectReduction: Reduction

Implementation Method 4

cold-pressed, preferably with a pressure in the range of between 100 MPa and 300 MPa

Methodology Applied
Scientific EffectCompression: Compression

Data Source

PatentEP4289788A1Process for making transition metal oxyfluorides as electrode materials for alkali metal ion cells
Publication Date: 2023.12.13 KARLSRUHER INST FUR TECH
  • EP4289788A1 patent drawingFigure 1(a)~1(c)
  • EP4289788A1 patent drawingFigure 2~3
  • EP4289788A1 patent drawingFigure 4(a)~4(b)

AI summary

The present invention refers to a process for making a transition metal oxyfluorides, as battery grade electrode materials, comprising the following steps: (a) providing an alkali metal compound and at least one transition metal compound as precursors (b) mixing the precursors (c) adding an alkali metal fluoride (d) carrying out a first heat treatment (e) cooling down to room temperature.