Colloidal Sol Deposition for Binder-Free Transition Metal Oxide Films

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Solution Overview

Problem

Current methods for depositing thin films of lithiated transition metal oxides, such as cobalt, manganese, or nickel oxides, face challenges including high temperature requirements, slow processing speeds, and the need for expensive equipment, which are incompatible with flexible electronic circuits and industrial production capacities, and result in degraded mass capacity after charge/discharge cycles.

Innovation Solution

A process involving the preparation of a colloidal sol from transition metal oxide powders using a solvent system that excludes carbon residues and binders, allowing for the deposition of pure, adherent transition metal oxide films with improved electrochemical properties through a low-energy, eco-friendly method suitable for industrial microbattery applications.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Reliability

If physical vapor deposition (PVD) or sputtering methods are used to deposit thin films, then film quality and adhesion are improved, but equipment cost and process complexity increase significantly

Engineering Contradiction:
Improvefilm adhesionVSAvoidequipment complexity
Core Design Contradiction:
ReliabilityVSDevice complexity

Solution Approach 1:

The patent replaces complex physical vapor deposition equipment with a simple dip-coating apparatus. Instead of using vacuum chambers, laser systems, or sputtering devices, the invention uses a straightforward liquid deposition method where the substrate is dipped into a colloidal sol containing metal oxide nanoparticles, followed by drying. This substitution of mechanical/physical systems with a chemical solution-based approach dramatically simplifies the equipment while maintaining film quality.

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

2Reliability

If high temperature calcination is applied to sol-gel deposited films, then film adhesion is improved, but energy consumption increases and carbon residues remain

Engineering Contradiction:
Improvefilm adhesionVSAvoidenergy consumption
Core Design Contradiction:
ReliabilityVSUse of energy by moving object

Solution Approach 1:

The patent fundamentally changes the deposition parameters by using pre-formed metal oxide nanoparticles in a colloidal sol instead of requiring high-temperature calcination of organic precursors. The nanoparticles are already in their final oxide form, eliminating the need for thermal decomposition. This parameter change from chemical precursor-based sol-gel to nanoparticle-based colloidal deposition reduces the required processing temperature from typically 500-1000°C to much lower temperatures, thereby reducing energy consumption and avoiding carbon residue formation.

Inventive Principle:
Principle #35Parameter changes

3Stability of the object's composition

If binders are used in sol-gel deposition to ensure film coherence, then film integrity is improved, but material purity decreases due to carbon residues

Engineering Contradiction:
Improvefilm integrityVSAvoidmaterial purity
Core Design Contradiction:
Stability of the object's compositionVSManufacturing precision

Solution Approach 1:

The patent extracts and eliminates the binder component from the deposition system. Instead of using organic binders that leave carbon residues, the invention relies on the natural colloidal stability of metal oxide nanoparticles and their direct adhesion to the substrate. The nanoparticles self-assemble into coherent films through van der Waals forces and surface interactions, achieving film integrity without any organic binding agents, thus maintaining material purity.

Inventive Principle:
Principle #2Taking out (Extraction)

4Manufacturing precision

If grinding of metal oxide powders is performed to achieve desired particle size, then dispersion quality is improved, but electrochemical properties are degraded

Engineering Contradiction:
Improveparticle size controlVSAvoidelectrochemical properties
Core Design Contradiction:
Manufacturing precisionVSReliability

Solution Approach 1:

The patent applies preliminary action by pre-synthesizing metal oxide nanoparticles with controlled size and optimized surface properties before incorporating them into the colloidal sol. Rather than grinding bulk powders which damages the crystal structure, the nanoparticles are prepared through controlled precipitation or hydrothermal methods that preserve the electrochemical activity. The surface of these pre-formed nanoparticles is then functionalized with surface modifiers to ensure colloidal stability and good substrate adhesion, achieving both particle size control and electrochemical performance.

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 achieves high insertion capacity, with films maintaining over 70% of theoretical reversible insertion capacity even after multiple charge/discharge cycles, and ensures stable, binder-free, and carbon-free deposition, enhancing the performance and durability of microbattery electrodes.

Implementation Method 1

the deposition of one or more layers of said sol on said substrate

Methodology Applied
Scientific EffectDeposition: Deposition (physical)

Implementation Method 2

the annealing of said one or several layers formed in step c') to prepare said transition metal oxide film

Methodology Applied
Scientific EffectAnnealing: Annealing

Implementation Method 3

the calcination of said powder obtained after step b')

Methodology Applied
Scientific EffectCalcination: Heat Treatment

Data Source

PatentEP3234222B1Method for the wet deposition of thin films
Publication Date: 2019.07.17 PRAYON SA
  • EP3234222B1 patent drawingFigure 1
  • EP3234222B1 patent drawingFigure 2A~2B
  • EP3234222B1 patent drawingFigure 3~4

AI summary

The invention relates to a method for the deposition of thin films, comprising preparing a solution containing at least one transition metal oxide powder in a solvent, continuously stirring said solution in order to form a sol, and using said sol in the form of said transition metal oxide film, characterised in that the powder is subjected to a preliminary preparation step.