Random-Structure GIC Production via Polar Protic Solvent

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Solution Overview

Problem

Existing methods for producing exfoliated graphite with a small number of stacked layers struggle to achieve stability and sufficient exfoliation due to retained regularity in alkali metal-GIC structures, even after exposure to air or polar aprotic solvents.

Innovation Solution

A method involving the contact of alkali metal-GIC with a polar protic solvent in a non-oxidizing atmosphere to collapse stage structures, followed by potential exposure to an oxygen-containing atmosphere, results in a random-structure GIC, which is then exfoliated using ultrasonic or shear treatments in a solvent, preferably with a surfactant, to obtain exfoliated graphite with reduced regularity and improved conductivity.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Stability of the object's composition

If alkali metal-GIC is exposed to air or polar aprotic solvent, then the structure changes and stage 2/3 peaks appear, but the regularity of graphene stacked state is not eliminated and stable exfoliation cannot be achieved

Engineering Contradiction:
Improvestability of exfoliated graphiteVSAvoidregularity of graphene stacked state
Core Design Contradiction:
Stability of the object's compositionVSManufacturing precision

Solution Approach 1:

The invention changes the chemical parameter by introducing a polar protic solvent (water or alcohol) instead of polar aprotic solvent, and controls the oxidation state by using non-oxidizing atmosphere initially. This parameter change enables the collapse of stage structures while maintaining regularity, achieving stable exfoliation with controlled oxidation later.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The invention uses non-oxidizing atmosphere (inert atmosphere) during the initial contact of polar protic solvent with alkali metal-GIC to prevent unwanted oxidation reactions. This protects the integrity of the GIC structure during the critical solvation process, allowing controlled structure collapse without premature oxidation.

Inventive Principle:
Principle #39Inert atmosphere (Inert environment)

2Ease of manufacture

If alkali metal-GIC is dissolved in polar aprotic solvent such as THF, then GIC dissolves, but sufficient exfoliation cannot be achieved and exfoliated graphite with small number of stacked layers cannot be obtained

Engineering Contradiction:
Improvedissolution of GICVSAvoidexfoliation degree
Core Design Contradiction:
Ease of manufactureVSManufacturing precision

Solution Approach 1:

The invention changes the solvent parameter from polar aprotic (THF) to polar protic (water or alcohol). This parameter change enables both dissolution and sufficient exfoliation simultaneously, achieving the dual goal of ease of manufacture and high exfoliation degree that was not possible with polar aprotic solvents.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The polar protic solvent acts as an intermediary that facilitates both dissolution and exfoliation processes. The protic nature of the solvent enables stronger interaction with the alkali metal-GIC structure, mediating the collapse of stage structures and achieving complete exfoliation while maintaining solubility.

Inventive Principle:
Principle #24Intermediary (Mediator)

3Manufacturing precision

If stage structure is collapsed to obtain random-structure GIC, then regularity is reduced and exfoliation is facilitated, but oxidation may occur and affect the quality of exfoliated graphite

Engineering Contradiction:
Improveregularity of graphene stacked stateVSAvoidoxidation
Core Design Contradiction:
Manufacturing precisionVSObject-affected harmful factors

Solution Approach 1:

The invention uses non-oxidizing atmosphere during the critical step of polar protic solvent contact to prevent oxidation while enabling structure collapse. This inert environment protects against harmful oxidation during the vulnerable stage when the GIC structure is most susceptible to degradation.

Inventive Principle:
Principle #39Inert atmosphere (Inert environment)

Solution Approach 2:

The invention later exposes the random-structure GIC to oxygen-containing atmosphere after the structure has collapsed and regularity has been reduced. By timing the oxidation exposure after the critical structure collapse, the harmful oxidation effect is converted into a beneficial process that can be controlled to achieve the desired exfoliated graphite quality.

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

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 approach effectively reduces the regularity of graphene stacked states, allowing for the stable production of exfoliated graphite with a small number of layers, maintaining excellent electrical and thermal conductivity, and enabling the formation of tape-shaped or networked exfoliated graphite structures.

Implementation Method 1

bringing a polar erotic solvent into contact with the alkali metal-GIC

Methodology Applied
Scientific EffectSolvation: Solvation

Implementation Method 2

graphite is exfoliated by ultrasonic treatment

Methodology Applied
Scientific EffectUltrasonic vibration: Ultrasonic Vibration

Implementation Method 3

graphite is exfoliated by ultrasonic treatment, heat treatment, or the like

Methodology Applied
Scientific EffectHeat treatment: Heat Treatment

Data Source

PatentUS9919926B2Method for producing random-structure GIC, method for producing exfoliated graphite dispersion liquid, exfoliated graphite dispersion liquid, and exfoliated graphite
Publication Date: 2018.03.20 SEKISUI CHEMICAL CO LTD
  • US9919926B2 patent drawing
  • US9919926B2 patent drawing
  • US9919926B2 patent drawing

AI summary

The present invention provides a method for producing a random-structure GIC in which exfoliated graphite having a low regularity of a graphene stacked state and a small number of stacked graphene layers can be easily obtained by exfoliation treatment. The method includes the steps of providing an alkali metal-GIC having an alkali metal intercalated between graphene layers and bringing a polar protic solvent into contact with the alkali metal-GIC in a non-oxidizing atmosphere.