Graphene Flake Production via Oleum Intercalation and Sonication

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Solution Overview

Problem

Current methods for producing graphene are complex, expensive, and often result in graphene flakes with defects due to the use of oxidizing agents and high temperatures, limiting their scalability and application in energy conversion, storage, and composite technologies.

Innovation Solution

A method involving intercalation and exfoliation of graphite using oleum as the liquid medium, with continuous sonication at low temperatures, eliminates the need for oxidizing agents and achieves 100% yield of high-quality graphene flakes without defects by using sulphuric acid and water dilution.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Reliability

If traditional Liquid-Phase Exfoliation methods using oxidizing agents (potassium permanganate, nitric acid, sulphuric acid) are used to produce graphene, then graphene can be obtained, but the process becomes complex, expensive, and produces graphene flakes with defects

Engineering Contradiction:
Improvegraphene qualityVSAvoidproduction process complexity
Core Design Contradiction:
ReliabilityVSDevice complexity

Solution Approach 1:

The patent extracts and eliminates the oxidizing agent step from the traditional Liquid-Phase Exfoliation process. Instead of using potassium permanganate, nitric acid, or sulphuric acid as oxidants, the invention directly exfoliates graphite in a liquid medium without oxidation, thereby simplifying the process and avoiding defect formation while maintaining graphene quality

Inventive Principle:
Principle #2Taking out (Extraction)

Solution Approach 2:

The patent replaces expensive and hazardous oxidizing agents (potassium permanganate, concentrated nitric and sulphuric acids) with a simple liquid medium that can be easily removed by filtration. This substitution reduces costs, eliminates safety hazards, and simplifies the overall production process while maintaining effective graphene exfoliation

Inventive Principle:
Principle #27Cheap short-living objects (Disposable)

2Productivity

If graphite is converted into graphite oxide using strong oxidizing agents, then exfoliation can be achieved, but the process becomes dangerous (explosion risk) and requires removal of manganese salts

Engineering Contradiction:
Improvegraphene production yieldVSAvoidprocess safety hazards
Core Design Contradiction:
ProductivityVSObject-affected harmful factors

Solution Approach 1:

The patent converts the harmful effect of strong oxidizing agents (which cause explosion risks and require careful salt removal) into a beneficial direct exfoliation process. By using a simple liquid medium without oxidation, the method eliminates safety hazards while maintaining high production yield and avoiding the need to remove manganese salts or handle dangerous chemical combinations

Inventive Principle:
Principle #22Blessing in disguise (Convert harm into benefit)

3Manufacturing precision

If graphite is treated with concentrated acids and oxidants at high temperatures, then exfoliation occurs, but the graphene flakes acquire defects and the process becomes costly

Engineering Contradiction:
Improvegraphene flake qualityVSAvoidproduction cost
Core Design Contradiction:
Manufacturing precisionVSLoss of substance

Solution Approach 1:

The patent fundamentally changes the chemical parameters of the exfoliation process by eliminating oxidation and using a simple liquid medium instead of concentrated acids and oxidants. This parameter change allows exfoliation to occur at lower temperatures without introducing defects, while also reducing material costs and eliminating the need for expensive purification steps

Inventive Principle:
Principle #35Parameter changes

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

This method produces graphene flakes with a mean thickness of less than 10 layers, characterized by high quality and minimal defects, as evidenced by Raman and electron microscope images, using only sulphuric acid and water, reducing production costs and increasing yield.

Implementation Method 1

The purpose of the exfoliation is to overcome van der Waals interactions and separate individual layers of graphene from each other. In intercalated graphite, distances between the graphene layers are greater than in graphite and, accordingly, van der Waals forces are smaller.

Methodology Applied
Scientific EffectIntercalation:

Implementation Method 2

This form of graphite is subjected to sonication and is exfoliated.

Methodology Applied
Scientific EffectSonication: Ultrasonic Vibration

Data Source

PatentUS20240228295A1A method for producing flaked graphene by intercalation and exfoliation of graphite
Publication Date: 2024.07.11 POLITECHNIKA WARSZAWSKA
  • US20240228295A1 patent drawing
  • US20240228295A1 patent drawing

AI summary

The object of the invention is a method for producing flaked graphene by intercalation and exfoliation of graphite in a liquid, with continuous stirring of the components by sonication, characterized in that oleum is used as the liquid, wherein the concentration of sulphur trioxide in sulphuric acid is 1-60%.