Halogen Vapor Exfoliation of Graphite for Nano-Platelets

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Solution Overview

Problem

Current methods for producing nano-scaled platelets, such as graphene and inorganic platelets, rely on undesirable chemicals and high-temperature processes, leading to contamination, high costs, and limited scalability due to the use of strong acids and labor-intensive washing steps, as well as incomplete exfoliation and varying platelet thickness.

Innovation Solution

A method involving the use of halogen vapors to intercalate and exfoliate layered materials at room temperature, allowing for the production of nano-scaled platelets with controlled thickness, which can be dispersed in liquids for nanocomposite formation, and utilizing ultrasonication for exfoliation without high temperatures, thereby reducing environmental impact and increasing production efficiency.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Reliability

If conventional methods using strong acids and high temperatures are used to exfoliate layered materials, then exfoliation can be achieved, but contamination occurs, washing steps become labor-intensive, and environmental impact increases

Engineering Contradiction:
Improveexfoliation completenessVSAvoidchemical contamination
Core Design Contradiction:
ReliabilityVSObject-affected harmful factors

Solution Approach 1:

The patent changes the chemical parameters by replacing strong acids with halogen vapors (Cl2, Br2, I2) as intercalation agents. This parameter change eliminates chemical contamination while maintaining exfoliation effectiveness, as the halogen vapors can be easily removed by sublimation without leaving harmful residues

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent substitutes the mechanical washing steps with a thermal sublimation process. Instead of mechanically removing contaminants through extensive washing, the halogen intercalation compound undergoes sublimation to release the halogen and produce uniform nano-platelets, eliminating the need for labor-intensive washing

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

2Reliability

If high-temperature processes are used for exfoliation, then complete separation of layers is achieved, but oxidation of carbon materials occurs and production costs increase

Engineering Contradiction:
Improveexfoliation completenessVSAvoidprocess temperature
Core Design Contradiction:
ReliabilityVSTemperature

Solution Approach 1:

The patent utilizes phase transitions of halogen vapors (sublimation and deposition) to achieve exfoliation at room temperature. The halogen vapor penetrates the layered material, and upon deposition, the phase change releases the halogen and creates expansion pressure that separates layers without requiring high temperatures

Inventive Principle:
Principle #36Phase transitions

Solution Approach 2:

The patent introduces halogen vapor as an intermediary substance that mediates the exfoliation process. The halogen vapor acts as a temporary intercalation agent that enables layer separation at low temperatures, avoiding direct high-temperature treatment of the carbon material and preventing oxidation

Inventive Principle:
Principle #24Intermediary (Mediator)

3Productivity

If conventional exfoliation methods are used, then platelets can be produced, but varying thickness and incomplete exfoliation occur

Engineering Contradiction:
Improveproduction rateVSAvoidplatelet thickness uniformity
Core Design Contradiction:
ProductivityVSManufacturing precision

Solution Approach 1:

The patent performs preliminary intercalation of halogen vapor into the layered material structure before exfoliation. This preliminary action ensures uniform distribution of the intercalation agent throughout the material, which subsequently leads to uniform platelet thickness and complete exfoliation when the halogen is removed

Inventive Principle:
Principle #10Preliminary action

Solution Approach 2:

The patent controls the intercalation parameters (halogen vapor pressure, temperature, time) to achieve uniform distribution of the intercalation agent. By optimizing these parameters, the patent ensures that all layers are treated uniformly, resulting in platelets with consistent thickness and complete exfoliation

Inventive Principle:
Principle #35Parameter changes

4Reliability

If carbon nano-tubes are produced using current methods, then high-quality material is obtained, but production costs are extremely high and yield is low

Engineering Contradiction:
Improvematerial qualityVSAvoidproduction yield
Core Design Contradiction:
ReliabilityVSProductivity

Solution Approach 1:

Instead of assembling carbon structures into nano-tubes through complex processes, the patent inverts the approach by starting with layered graphite material and exfoliating it into individual nano-platelets. This inversion simplifies the process, increases yield, and maintains material quality by avoiding the complex tube-forming steps

Inventive Principle:
Principle #13The other way round (Inversion)

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 nano-scaled platelets with uniform thickness, efficient dispersion in liquids, and reduced environmental impact, facilitating the creation of nanocomposites while avoiding high-temperature oxidation and chemical reactions, thus offering a cost-effective and scalable solution for producing nano-scaled platelets.

Implementation Method 1

subjecting the layered material in a powder form to a halogen vapor... to cause the halogen to penetrate an interlayer space of the layered material, forming a stable halogen-intercalated compound

Methodology Applied
Scientific EffectIntercalation: Absorption (physical)

Implementation Method 2

heating the halogen-intercalated compound at a second temperature above the boiling point of the halogen, allowing halogen atoms or molecules residing in the interlayer space to exfoliate the layered material to produce the platelets

Methodology Applied
Scientific EffectThermal expansion: Thermal Expansion

Implementation Method 3

mixing the halogen-intercalated compound in a liquid medium which is subjected to ultrasonication for exfoliating the halogen-intercalated compound to produce the platelets, which are also well-dispersed in the liquid medium due to ultrasonic effects

Methodology Applied
Scientific EffectUltrasonication: Ultrasound

Data Source

PatentUS7892514B2Method of producing nano-scaled graphene and inorganic platelets and their nanocomposites
Publication Date: 2011.02.22 GLOBAL GRAPHENE GROUP INC
  • US7892514B2 patent drawing
  • US7892514B2 patent drawing
  • US7892514B2 patent drawing

AI summary

Disclosed is a method of exfoliating a layered material (e.g., graphite and graphite oxide) to produce nano-scaled platelets having a thickness smaller than 100 nm, typically smaller than 10 nm, and often between 0.34 nm and 1.02 nm. The method comprises: (a) subjecting the layered material in a powder form to a halogen vapor at a first temperature above the melting point or sublimation point of the halogen at a sufficient vapor pressure and for a duration of time sufficient to cause the halogen molecules to penetrate an interlayer space of the layered material, forming a stable halogen-intercalated compound; and (b) heating the halogen-intercalated compound at a second temperature above the boiling point of the halogen, allowing halogen atoms or molecules residing in the interlayer space to exfoliate the layered material to produce the platelets. Alternatively, rather than heating, step (a) is followed by a step of dispersing the halogen-intercalated compound in a liquid medium which is subjected to ultrasonication for exfoliating the halogen-intercalated compound to produce the platelets, which are dispersed in the liquid medium. The halogen can be readily captured and re-used, thereby significantly reducing the impact of halogen to the environment. The method can further include a step of dispersing the platelets in a polymer or monomer solution or suspension as a precursor step to nanocomposite fabrication.