Oxidized Graphene Production With Two-Step Milling for Solvent Dispersibility

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Solution Overview

Problem

Current methods for large-scale production of functionalized graphene face challenges in achieving high yield and uniformity, particularly in dispersibility and mixability in various solvents, due to defects concentrated at the edges of graphene materials.

Innovation Solution

A two-step milling process involving a combination of crystalline graphite with electrolyte solutions containing metal hydroxide salts and oxidizers to produce electrostatically charged and hydroxylated graphene sheets, which are then partially oxidized to enhance dispersibility and mixability in both polar and non-polar solvents.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Productivity

If conventional single-step milling methods are used to produce graphene, then the production process is simple, but the yield is low and the dispersibility in solvents is poor

Engineering Contradiction:
Improveproduction yieldVSAvoidprocess complexity
Core Design Contradiction:
ProductivityVSDevice complexity

Solution Approach 1:

The patent divides the graphene production process into two distinct steps: (1) a first milling step using a first electrolyte solution to produce intermediate graphene material, and (2) a second milling step using a second electrolyte solution to produce the final functionalized graphene. This segmentation allows each step to be optimized independently, achieving high yield and good dispersibility while maintaining manageable process complexity through modular design.

Inventive Principle:
Principle #1Segmentation

Solution Approach 2:

The first milling step performs preliminary functionalization by introducing oxygen-containing groups and creating defects at the graphene edges before the second milling step. This preliminary action prepares the graphene structure to receive further functionalization in the second step, enabling cumulative improvement in dispersibility and yield without requiring complete functionalization in a single difficult step.

Inventive Principle:
Principle #10Preliminary action

2Adaptability or versatility

If conventional milling methods are used, then the process is straightforward, but the dispersibility and mixability in various solvents are poor

Engineering Contradiction:
Improvedispersibility in solventsVSAvoidmanufacturing ease
Core Design Contradiction:
Adaptability or versatilityVSEase of manufacture

Solution Approach 1:

The patent changes the chemical parameters of the electrolyte solutions between steps: the first electrolyte solution uses milder conditions to create initial functional groups, while the second electrolyte solution uses stronger oxidizing conditions to enhance dispersibility. This parameter progression allows the graphene to gradually acquire better solvent compatibility without overwhelming the manufacturing process.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent creates functionally composite graphene material by combining different functional groups (oxygen-containing groups from the first step and additional functional groups from the second step) on the graphene structure. This composite functionalization enables the material to interact effectively with both polar and non-polar solvents, achieving universal dispersibility while maintaining manufacturing feasibility through systematic processing.

Inventive Principle:
Principle #40Composite materials

3Adaptability or versatility

If strong oxidation is applied in a single step, then dispersibility improves, but defects become concentrated at edges reducing overall quality

Engineering Contradiction:
Improvemixability in solventsVSAvoiduniformity of functionalization
Core Design Contradiction:
Adaptability or versatilityVSManufacturing precision

Solution Approach 1:

The patent applies periodic functionalization action through two sequential milling steps with different electrolyte solutions. The first step introduces functional groups at a controlled rate, and the second step adds additional functional groups with different characteristics. This periodic approach distributes defects more uniformly throughout the graphene structure rather than concentrating them at edges, while still achieving excellent mixability in both polar and non-polar solvents.

Inventive Principle:
Principle #19Periodic 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 results in high-yield, functionalized graphene sheets with improved dispersibility and mixability, maintaining desirable properties while utilizing defective edges for enhanced performance in applications such as lubricants, composites, and thermal transfer liquids.

Implementation Method 1

produce electrostatically charged and hydroxylated graphene sheets

Methodology Applied
Scientific EffectElectrostatic charging: Electrostatics

Implementation Method 2

produce electrostatically charged and hydroxylated graphene sheets

Methodology Applied
Scientific EffectHydroxylation: Chemical Bonding

Implementation Method 3

The thinned intermediate material is then milled in the presence of the second electrolyte solution that includes a strong oxidizer

Methodology Applied
Scientific EffectOxidation: Oxidation

Data Source

PatentUS20250002354A1Large scale production of oxidized graphene
Publication Date: 2025.01.02 NANOXPLORE INC
  • US20250002354A1 patent drawing
  • US20250002354A1 patent drawing
  • US20250002354A1 patent drawing

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.