Sonication-Assisted Graphene Production via Carbide Etching

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Solution Overview

Problem

Current methods for large-scale production of high-quality graphene materials face challenges such as limited control over graphene layers, high energy consumption, costly processes, and the presence of defects, which affect the electrical conductivity and mechanical properties of the final product.

Innovation Solution

A direct sonication-assisted method involving a mixture of carbide compounds and etching compounds, where sonication is used to form graphene-based materials at frequencies above 15 kHz, allowing for the production of high-quality graphene sheets, including nanoporous 2D graphene, without the need for further reduction steps or harsh conditions.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Productivity

If conventional top-down methods (mechanical/chemical exfoliation) are used for large-scale production, then production quantity increases, but the number of graphene layers cannot be sufficiently controlled and defects increase

Engineering Contradiction:
Improveproduction quantityVSAvoidcontrol over graphene layers
Core Design Contradiction:
ProductivityVSManufacturing precision

Solution Approach 1:

The patent replaces conventional mechanical exfoliation methods with a chemical etching approach using iron carbide and hydrochloric acid. This substitution enables precise control over graphene layer formation through chemical reaction mechanisms rather than mechanical force, achieving both large-scale production and controlled layer structure simultaneously

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

Solution Approach 2:

The patent utilizes parameter changes in the chemical etching process, specifically controlling etching time, temperature, and acid concentration to precisely regulate the number of graphene layers formed. By adjusting these parameters, the method achieves controlled layer formation while maintaining high production efficiency

Inventive Principle:
Principle #35Parameter changes

2Productivity

If conventional top-down methods are used, then production scale increases, but electrical conductivity decreases due to oxide groups and defects

Engineering Contradiction:
Improveproduction scaleVSAvoidelectrical conductivity
Core Design Contradiction:
ProductivityVSReliability

Solution Approach 1:

The patent replaces mechanical exfoliation with chemical etching followed by in-situ reduction, eliminating the need for separate reduction steps. This integrated approach produces graphene with fewer oxide groups and defects, maintaining high electrical conductivity while enabling large-scale production

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

Solution Approach 2:

The iron carbide serves a dual function: as both the carbon source and the reducing agent in the process. The iron metal released during carbide etching automatically reduces the graphene oxide formed, creating high-quality conductive graphene without requiring additional reducing agents or steps

Inventive Principle:
Principle #25Self-service

3Manufacturing precision

If bottom-up processes (chemical vapor deposition) are used, then graphene quality improves, but energy consumption increases and production scale is limited

Engineering Contradiction:
Improvegraphene qualityVSAvoidenergy consumption
Core Design Contradiction:
Manufacturing precisionVSUse of energy by moving object

Solution Approach 1:

The patent dramatically reduces the energy input parameters compared to CVD methods. The etching process occurs at room temperature or near-ambient temperatures, eliminating the need for high-temperature furnaces (200-1200°C) required in conventional bottom-up approaches, thereby reducing energy consumption while maintaining graphene quality

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent replaces the high-energy thermal field of CVD with a chemical reaction field using hydrochloric acid etching. This substitution enables graphene synthesis at much lower energy levels while achieving comparable or superior quality through controlled chemical reactions rather than thermal decomposition

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

4Manufacturing precision

If bottom-up processes are used, then graphene quality improves, but production cost increases

Engineering Contradiction:
Improvegraphene qualityVSAvoidproduction cost
Core Design Contradiction:
Manufacturing precisionVSEase of manufacture

Solution Approach 1:

The patent employs inexpensive, readily available materials: iron carbide (a common industrial material) and hydrochloric acid (a standard laboratory reagent). These cheap starting materials replace the expensive specialized substrates and high-purity precursors required in CVD methods, significantly reducing production costs while maintaining graphene quality

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

Solution Approach 2:

The iron carbide provides both carbon atoms for graphene formation and iron metal for in-situ reduction of graphene oxide. This self-contained system eliminates the need for separate reduction steps and additional reducing agents, simplifying the process and reducing material costs while ensuring high graphene quality

Inventive Principle:
Principle #25Self-service

5Manufacturing precision

If epitaxial growth is used, then graphene quality improves, but substrate requirements become harsh and production flexibility decreases

Engineering Contradiction:
Improvegraphene qualityVSAvoidsubstrate requirements
Core Design Contradiction:
Manufacturing precisionVSAdaptability or versatility

Solution Approach 1:

The patent replaces the substrate-dependent epitaxial growth mechanism with a substrate-independent chemical etching approach. Graphene is formed directly in solution through carbide etching, eliminating the need for specialized high-temperature substrates and enabling production on various surfaces including flexible substrates, thereby increasing adaptability while maintaining quality

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

Solution Approach 2:

The patent changes the fundamental parameters of graphene synthesis from high-temperature vapor-phase deposition to low-temperature solution-phase chemical reactions. This parameter change enables the use of diverse substrates with lower temperature tolerances and expands the range of applicable substrates beyond the limited high-temperature materials required for epitaxial growth

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 enables the production of high-porosity graphene materials with excellent electrical conductivity, suitable for industrial-scale production, under mild conditions, reducing environmental impact and chemical usage, and eliminating the need for templates or substrate transfer processes.

Implementation Method 1

subjecting the mixture of step (i) to sonication at at least one frequency above 15 kHz for forming the graphene-based material

Methodology Applied
Scientific EffectSonication: Ultrasonic Vibration

Implementation Method 2

subjecting the mixture of step (i) to sonication at at least one frequency above 15 kHz for forming the graphene-based material

Methodology Applied
Scientific EffectAcoustic cavitation: Acoustic Cavitation

Implementation Method 3

etching at least one carbide compound in the presence of at least one etching compound

Methodology Applied
Scientific EffectChemical etching: Ablation

Data Source

PatentUS10160653B2Method of producing graphene-based materials, obtainable materials and their use
Publication Date: 2018.12.25 CITY UNIVERSITY OF HONG KONG
  • US10160653B2 patent drawing

AI summary

A method of producing a graphene-based material, namely a direct sonication assisted method for producing a graphene-based material, in particular comprising 2D porous graphene includes subjecting a mixture of at least one carbide compound and at least one etching compound to sonication. This method enables the production of large amounts of a graphene-based material in a short time at ambient temperature and pressure and without the need for toxic reactants. The obtained porous graphene-based material has excellent electrical conductivity, due to the direct chemical synthesis, and is free of any template and not attached to any substrate. The 2D porous graphene can be directly used without transfer processes. The invention further relates to the graphene-based material obtained or obtainable by the method and the use of the graphene-based material.