Graphene Oxide Reduction via Moderate Heating for Polymer Composites

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Solution Overview

Problem

Current methods for fabricating graphene-containing composites face challenges in achieving high yields and maintaining the unique mechanical, electrical, and thermal properties of graphene while avoiding the use of high temperatures, inert gases, and surfactants, which are necessary for large-scale production and compatibility with polymers.

Innovation Solution

A method involving the mixing of graphene oxide with a medium and heating it above 40°C to reduce graphene oxide to graphene, optimizing particle-polymer interfacial forces without the need for high temperatures, inert gases, or surfactants, allowing for controlled temperature and time processing to achieve atomic carbon to oxygen ratios similar to pure graphene.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If graphite oxide is exfoliated thermally at very high temperature (e.g., 1050°C) in a tube furnace in an inert gas, then single-layer graphene sheets can be produced, but the process consumes high energy and requires complex equipment and inert gas atmosphere

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

Solution Approach 1:

The patent changes the temperature parameter from very high (1050°C) to moderate (30-200°C) and introduces chemical reducing agents to enable reduction under milder conditions, thereby reducing energy consumption while maintaining graphene quality

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent introduces chemical reducing agents (hydrazine, ascorbic acid, sodium borohydride, etc.) as intermediaries to facilitate the reduction of graphite oxide to graphene, replacing the need for high-thermal-energy environments and inert gas atmospheres

Inventive Principle:
Principle #24Intermediary (Mediator)

2Manufacturing precision

If graphite oxide is exfoliated thermally to produce graphene, then the sheets are chemically similar to pure graphene, but they become very hydrophobic and difficult to handle in liquid processing

Engineering Contradiction:
Improvegraphene sheet purityVSAvoidliquid processing ease
Core Design Contradiction:
Manufacturing precisionVSEase of operation

Solution Approach 1:

The patent uses chemical reducing agents as intermediaries that not only reduce graphite oxide to graphene but also leave functional groups on the graphene surface that maintain hydrophilicity, enabling easy liquid processing while achieving high purity

Inventive Principle:
Principle #24Intermediary (Mediator)

Solution Approach 2:

The patent creates local quality differences by retaining oxygen-containing functional groups at the graphene surface while reducing the bulk graphite oxide structure, resulting in graphene that is both pure and hydrophilic

Inventive Principle:
Principle #3Local quality

3Ease of operation

If graphite oxide is exfoliated acoustically in solvents to retain functional surface groups, then stable dispersions can be achieved in a large range of solvents, but the sheets do not have the advantageous mechanical and thermal properties or conductivity as does graphene

Engineering Contradiction:
Improvedispersion stabilityVSAvoidmechanical properties
Core Design Contradiction:
Ease of operationVSStrength

Solution Approach 1:

The patent performs preliminary exfoliation of graphite oxide to create stable dispersions with functional groups, then subsequently reduces the exfoliated sheets to graphene while maintaining dispersion stability, thereby achieving both ease of operation and improved mechanical properties

Inventive Principle:
Principle #10Preliminary action

Solution Approach 2:

The patent maintains continuous useful action by keeping graphene sheets in stable dispersion throughout the reduction process, ensuring that the sheets remain accessible and do not aggregate, thus preserving both processing ease and final material properties

Inventive Principle:
Principle #20Continuity of useful action

4Manufacturing precision

If methods of reducing graphene oxide while in aqueous dispersions are used, then the atomic carbon to oxygen ratio increases, but surfactants need to be added in considerable amounts to avoid collapse of the dispersion

Engineering Contradiction:
Improvecarbon to oxygen ratioVSAvoidsurfactant amount
Core Design Contradiction:
Manufacturing precisionVSQuantity of substance

Solution Approach 1:

The patent uses chemical reducing agents as intermediaries that simultaneously reduce graphite oxide to graphene and maintain dispersion stability without requiring additional surfactants, thereby achieving high carbon-to-oxygen ratios without surfactant contamination

Inventive Principle:
Principle #24Intermediary (Mediator)

Solution Approach 2:

The patent extracts the need for surfactants by using reducing agents that inherently maintain dispersion stability through their chemical action on graphite oxide, eliminating the requirement for separate surfactant additives

Inventive Principle:
Principle #2Taking out (Extraction)

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 large-scale production of graphene-containing materials with enhanced performance properties, such as mechanical, electrical, and thermal properties, suitable for applications in gas barrier, high-strength, and electrically conductive materials, while avoiding the limitations of conventional methods.

Implementation Method 1

heating it above 40°C to reduce graphene oxide to graphene

Methodology Applied
Scientific EffectThermal reduction: Thermolysis

Implementation Method 2

the energy released during the exothermic reduction process of the graphene oxide to graphene transformation

Methodology Applied
Scientific EffectExothermic reaction: Exothermic Reaction

Implementation Method 3

the energy released during the exothermic reduction process of the graphene oxide to graphene transformation can be further used to heat up the graphene-medium nanocomposite

Methodology Applied
Scientific EffectExothermic reaction: Exothermic Reaction

Implementation Method 4

The tube furnace exfoliation simultaneously exfoliates and reduces graphite oxide, thereby removing the vast majority of the functional groups from the oxidized material. These functional groups are released primarily as CO2 and H2O gas

Methodology Applied
Scientific EffectThermal decomposition: Pyrolysis

Data Source

PatentUS9162896B2Method for making polymer composites containing graphene sheets
Publication Date: 2015.10.20 COLLEGE OF WILLIAM & MARY
  • US9162896B2 patent drawing
  • US9162896B2 patent drawing
  • US9162896B2 patent drawing

AI summary

In one embodiment, a method for producing a graphene-containing composition is provided, the method comprising: (i) mixing a graphene oxide with a medium to form a mixture; and (ii) heating the mixture to a temperature above about 40° C., whereby a graphene-containing composition is formed from the mixture. Composites of polymers with disperse functionalized graphene sheets and the applications thereof are also described.