Oxidized Graphene Production with Edge-Selective Functionalization

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Solution Overview

Problem

Current methods for large-scale production of graphene struggle with achieving functionalized graphene with enhanced mixability and dispersibility in various solvents, particularly due to defects concentrated at the edges of graphene materials, which affect its electrical conductivity and surface properties.

Innovation Solution

A two-step milling process involving the combination of crystalline graphite with electrolyte solutions containing metal hydroxide salts and oxidizers, followed by milling to produce electrostatically charged and hydroxylated graphene sheets, where the edges are selectively functionalized to enhance dispersibility and mixability in both polar and non-polar solvents.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Productivity

If current large-scale production methods are used, then production volume is achieved, but functionalized graphene with enhanced mixability and dispersibility cannot be obtained due to defects concentrated at edges

Engineering Contradiction:
Improveproduction volumeVSAvoidfunctionalization quality
Core Design Contradiction:
ProductivityVSManufacturing precision

Solution Approach 1:

The patent applies local quality by selectively functionalizing the edges of graphene sheets through controlled oxidation. The edge regions, which naturally contain defects, are targeted for oxidation to introduce functional groups (carboxyl, hydroxyl, carbonyl) that enhance dispersibility, while the basal planes are preserved to maintain electrical conductivity and other desirable properties. This localized functionalization approach resolves the contradiction by improving mixability without compromising production volume or overall material quality.

Inventive Principle:
Principle #3Local quality

Solution Approach 2:

The patent employs parameter changes by controlling oxidation potential and exposure time to achieve partial oxidation. By adjusting these parameters, the process selectively modifies edge regions without过度 oxidizing the basal planes, thereby maintaining the balance between productivity and functionalization quality. The controlled oxidation introduces necessary functional groups while preserving the graphitic structure's essential properties.

Inventive Principle:
Principle #35Parameter changes

2Adaptability or versatility

If edges are functionalized to enhance dispersibility, then mixability in solvents is improved, but electrical conductivity may be affected due to defect concentration

Engineering Contradiction:
ImprovedispersibilityVSAvoidelectrical conductivity
Core Design Contradiction:
Adaptability or versatilityVSReliability

Solution Approach 1:

The patent resolves this contradiction through local quality by confining oxidation to edge regions only. The functional groups (carboxyl, hydroxyl, carbonyl) are introduced at the edges to enhance dispersibility and processability, while the extensive basal planes retain their sp2 hybridized carbon structure and high electrical conductivity. This spatial differentiation of properties allows the material to exhibit both improved dispersibility and maintained conductivity.

Inventive Principle:
Principle #3Local quality

Solution Approach 2:

The patent applies partial action by performing controlled oxidation that stops before complete oxidation of the entire graphene structure. The oxidation is deliberately limited to partial modification of edge regions, preserving the majority of the graphitic structure's conductive properties while achieving sufficient functionalization for enhanced dispersibility in various solvents.

Inventive Principle:
Principle #16Partial or excessive 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 effectively produces functionalized graphene with improved dispersibility and mixability, preserving the desirable properties of graphene surfaces while utilizing defective edges for enhanced solubility, resulting in high-quality graphene sheets with increased thermal and electrical conductivity.

Implementation Method 1

milling the crystalline graphite in the presence of the first electrolyte solution for a first time period to produce a thinned intermediate material

Methodology Applied
Scientific EffectElectrostatic charging: Electrostatics

Implementation Method 2

combining the thinned intermediate material with a second electrolyte solution, the second electrolyte solution including a strong oxidizer

Methodology Applied
Scientific EffectOxidation: Oxidation

Implementation Method 3

the strong oxidizer is a chemical agent with an oxidation potential greater than 1.5V

Methodology Applied
Scientific EffectOxidation: Oxidation

Data Source

PatentEP3230386B1Large scale production of oxidized graphene
Publication Date: 2024.02.21 NANOXPLORE INC
  • EP3230386B1 patent drawingFigure 1
  • EP3230386B1 patent drawingFigure 2A~2B
  • EP3230386B1 patent drawingFigure 3(a)~3(f)

AI summary

Embodiments described herein relate generally to the large scale production of functionalized graphene. In some embodiments, a method for producing functionalized graphene includes combining a crystalline graphite with a first electrolyte solution that includes at least one of a metal hydroxide salt, an oxidizer, and a surfactant. The crystalline graphite is then milled in the presence of the first electrolyte solution for a first time period to produce a thinned intermediate material. The thinned intermediate material is combined with a second electrolyte solution that includes a strong oxidizer and at least one of a metal hydroxide salt, a weak oxidizer, and a surfactant. The thinned intermediate material is then milled in the presence of the second electrolyte solution for a second time period to produce functionalized graphene.