Plasma Exfoliation of Graphite Nanoplatelets

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Solution Overview

Problem

Current methods for processing carbon nanotubes (CNTs) and graphene are inefficient, costly, and result in contaminated, tangled aggregates, limiting their industrial application due to strong agglomeration and structural damage during dispersion in matrix materials.

Innovation Solution

A plasma treatment method using conductive contact bodies in a treatment chamber generates glow plasma to exfoliate, clean, and functionalize graphite particles, producing discrete graphene platelets that can be dispersed in a liquid vehicle or matrix, achieving high yields and uniform functionalization.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Ease of operation

If aggressive mechanical and chemical treatments are used to disperse CNTs, then dispersion is achieved, but structural damage to carbon layers occurs and CNT properties are lost

Engineering Contradiction:
Improvedispersion capabilityVSAvoidstructural integrity of CNTs
Core Design Contradiction:
Ease of operationVSStrength

Solution Approach 1:

The patent replaces aggressive mechanical treatments (milling, grinding, ultrasonication) with a controlled plasma treatment process. The plasma generates ion bombardment and radical reactions that functionalize the CNT surfaces and reduce agglomeration without the severe mechanical stress that damages the carbon structure, thus achieving dispersion while preserving structural integrity.

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

Solution Approach 2:

The patent changes the chemical and physical parameters of the CNT surface through plasma treatment, introducing functional groups and modifying surface energy. This alters the interaction between CNTs and the dispersing medium, enabling effective dispersion without requiring aggressive mechanical force that would damage the structure.

Inventive Principle:
Principle #35Parameter changes

2Stability of the object's composition

If chemical functionalization is used to stabilize CNT dispersions, then dispersion stability is improved, but production cost increases and efficiency decreases

Engineering Contradiction:
Improvedispersion stabilityVSAvoidproduction efficiency
Core Design Contradiction:
Stability of the object's compositionVSProductivity

Solution Approach 1:

The patent replaces multi-step chemical functionalization processes with a single plasma treatment step. The plasma process simultaneously achieves surface activation, functionalization, and dispersion stabilization in one operation, eliminating the need for separate chemical treatment and surfactant addition steps, thereby improving production efficiency while maintaining dispersion stability.

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

Solution Approach 2:

The plasma treatment serves multiple functions simultaneously: it cleans contaminants, functionalizes the surface, stabilizes the dispersion, and prevents re-agglomeration. This multi-functionality consolidates what would otherwise require multiple separate process steps into one operation, significantly improving productivity.

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

3Manufacturing precision

If acid boiling and high-shear milling are used to decompose contaminants and break aggregates, then CNT functionalization is achieved, but severe structural damage and tube shortening occur

Engineering Contradiction:
Improvefunctionalization levelVSAvoidCNT tube length
Core Design Contradiction:
Manufacturing precisionVSLength of moving object

Solution Approach 1:

The patent replaces the combination of chemical acid treatment and mechanical high-shear milling with plasma treatment. The plasma process achieves functionalization through ion and radical reactions at the surface without the mechanical forces that cause tube breakage and shortening, thereby maintaining manufacturing precision while preserving tube length.

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

Solution Approach 2:

The plasma acts as an intermediary that transfers energy and reactive species to the CNT surface for functionalization without requiring direct contact with aggressive chemicals or mechanical stress. This indirect action achieves the desired functionalization while avoiding the structural damage caused by direct acid and mechanical treatment.

Inventive Principle:
Principle #24Intermediary (Mediator)

4Quantity of substance

If conventional dispersion methods are used for CNTs, then agglomerates are dispersed, but the properties of individual CNTs are scarcely made available

Engineering Contradiction:
Improvedispersed materialVSAvoidindividual CNT property utilization
Core Design Contradiction:
Quantity of substanceVSManufacturing precision

Solution Approach 1:

The patent uses plasma treatment to achieve fine-level dispersion of individual CNTs rather than just breaking up large agglomerates. The plasma functionalization creates uniform surface properties that prevent re-agglomeration at the individual tube level, ensuring that dispersed CNTs maintain their individual properties and performance characteristics.

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 effectively separates and functionalizes graphite particles, producing materials with enhanced properties suitable for applications in photovoltaic devices, hydrogen storage, and rechargeable battery electrodes, with improved mechanical and thermal profiles.

Implementation Method 1

the particles for treatment are subject to plasma treatment in a treatment chamber containing or comprising multiple electrically-conductive solid contact bodies or contact formations

Methodology Applied
Scientific EffectPlasma: Plasma

Implementation Method 2

During the treatment, glow plasma forms on the surfaces of the contact bodies or contact formations

Methodology Applied
Scientific EffectGlow plasma: Electric Glow Discharge

Implementation Method 3

the particles for treatment are subject to plasma treatment in a treatment chamber

Methodology Applied
Scientific EffectPlasma: Plasma

Implementation Method 4

plasma treatment... producing discrete graphene platelets that can be dispersed

Methodology Applied
Scientific EffectIon bombardment: Ion Beam

Implementation Method 5

the particles for treatment are subject to plasma treatment... and functionalizing graphite particles

Methodology Applied
Scientific EffectPlasma: Plasma

Implementation Method 6

functionalizing graphite particles, in which the particles for treatment are subject to plasma treatment

Methodology Applied
Scientific EffectChemical reactions: Chemical Bonding

Data Source

PatentEP3000849B1Graphite nanoplatelets, composites comprising them, preparation and uses thereof
Publication Date: 2018.04.04 HAYDALE GRAPHENE IND
  • EP3000849B1 patent drawingFigure 1~5
  • EP3000849B1 patent drawingFigure 6~7
  • EP3000849B1 patent drawingFigure 8~9

AI summary

The application discloses methods of processing particulate carbon material, such as graphitic particles or agglomerates of carbon nanoparticles such as CNTs. The starting material is agitated in a treatment vessel in the presence of low-pressure (glow) plasma generated between electrodes, e.g. between a central electrode and an outer rotating conductive drum containing the material for treatment. Preferably the material is agitated in the presence of conductive contact bodies such as metal balls, or other contact formations with relatively high specific surface area, on the surface of which plasma glow is present and amongst which the material to be treated moves. The methods are found to effectively deagglomerate nanoparticles, and to exfoliate graphitic material to produce very thin (few-layer or monolayer) graphitic sheets showing graphene-type characteristics. The resulting deaggregated or exfoliated carbon nanomaterials are an aspect of the disclosure, as is their use dispersed in composite materials, e.g. conductive polymeric composites for electric or electronic articles and devices. The particle surfaces can be functionalised by choosing appropriate gas in which to form the plasma. The invention is advantageous in using safe, dry and moderate conditions to achieve a high degree of deaggregation or exfoliation compared with previous aggressive chemical methods such as acid treatment.