Electrochemical Graphite Exfoliation for Ultra-Thin Platelets

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Solution Overview

Problem

Existing methods for producing nano-scaled graphene platelets (NGPs) face challenges such as environmental concerns due to undesirable chemical effluents, high exfoliation temperatures leading to graphite oxidation, non-uniformity in exfoliation, and difficulty in achieving ultra-thin thicknesses, which hinder widespread application.

Innovation Solution

A method involving electrochemical intercalation of layered graphite materials with carboxylic acids to form stable graphite intercalation compounds, followed by thermal shock and mechanical shearing to produce uniformly thin NGPs, avoiding high-temperature oxidation and undesirable by-products.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Reliability

If conventional chemical oxidation or electrochemical methods are used to intercalate graphite, then graphite intercalation compounds can be formed, but undesirable chemical effluents are generated causing environmental concerns

Engineering Contradiction:
Improveformation of graphite intercalation compoundVSAvoidchemical effluents
Core Design Contradiction:
ReliabilityVSObject-generated harmful factors

Solution Approach 1:

The invention changes the intercalation method from conventional chemical oxidation or traditional electrochemical methods to a specific electrochemical intercalation process using formic acid as the intercalating agent. This parameter change in the chemical composition and intercalation mechanism eliminates the generation of undesirable chemical effluents while still forming the required graphite intercalation compound.

Inventive Principle:
Principle #35Parameter changes

2Manufacturing precision

If high temperature exposure is used to exfoliate the GIC, then exfoliation occurs, but graphite oxidation happens leading to non-uniformity

Engineering Contradiction:
ImproveexfoliationVSAvoidexfoliation temperature
Core Design Contradiction:
Manufacturing precisionVSTemperature

Solution Approach 1:

The invention changes the exfoliation temperature parameter from conventional high temperatures (800-1100°C) to a lower temperature range (300-600°C). This parameter change is made possible by the specific formic acid intercalation process, which creates a GIC structure that exfoliates at lower temperatures without causing graphite oxidation, thereby achieving uniform exfoliation.

Inventive Principle:
Principle #35Parameter changes

3Manufacturing precision

If conventional exfoliation methods are used, then graphite flakes can be separated, but achieving ultra-thin thicknesses (less than 2 nm or 5 layers) is difficult

Engineering Contradiction:
Improvethickness controlVSAvoidexfoliation process
Core Design Contradiction:
Manufacturing precisionVSEase of manufacture

Solution Approach 1:

The invention changes multiple parameters: the intercalating agent (formic acid), the intercalation method (electrochemical), and the exfoliation temperature (300-600°C). These combined parameter changes enable consistent production of ultra-thin NGPs with average thicknesses less than 2 nm or 5 layers, achieving superior thickness control that was not possible with conventional methods.

Inventive Principle:
Principle #35Parameter changes

4Manufacturing precision

If repeated intercalation and exfoliation cycles are performed to achieve ultra-thin NGPs, then thickness is reduced, but the process becomes more complex and time-consuming

Engineering Contradiction:
ImprovethicknessVSAvoidprocess complexity
Core Design Contradiction:
Manufacturing precisionVSDevice complexity

Solution Approach 1:

The invention changes the fundamental parameters of the intercalation and exfoliation process to achieve ultra-thin NGPs in a single cycle rather than requiring multiple repeated cycles. The electrochemical intercalation with formic acid combined with low-temperature exfoliation (300-600°C) produces such effective separation that ultra-thin platelets are obtained directly, significantly reducing process complexity and time.

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 consistently produces NGPs with average thicknesses less than 2 nm or 5 layers, achieving uniformity and environmental benignity, suitable for various applications, including supercapacitor electrodes.

Implementation Method 1

forming a formic acid-intercalated graphite compound by an electrochemical reaction which uses a formic acid as both an electrolyte and an intercalate source

Methodology Applied
Scientific EffectElectrochemical reaction: Electrolysis

Implementation Method 2

exposing the intercalated graphite compound to a thermal shock to produce exfoliated graphite

Methodology Applied
Scientific EffectThermal shock: Thermal Shock

Data Source

PatentUS9422164B2Electrochemical method of producing nano graphene platelets
Publication Date: 2016.08.23 GLOBAL GRAPHENE GROUP INC
  • US9422164B2 patent drawing
  • US9422164B2 patent drawing
  • US9422164B2 patent drawing

AI summary

A method of producing nano-scaled graphene platelets with an average thickness smaller than 30 nm from a layered graphite material. The method comprises (a) forming a carboxylic acid-intercalated graphite compound by an electrochemical reaction; (b) exposing the intercalated graphite compound to a thermal shock to produce exfoliated graphite; and (c) subjecting the exfoliated graphite to a mechanical shearing treatment to produce the nano-scaled graphene platelets. Preferred carboxylic acids are formic acid and acetic acid. The exfoliation step in the instant invention does not involve the evolution of undesirable species, such as NOx and SOx, which are common by-products of exfoliating conventional sulfuric or nitric acid-intercalated graphite compounds. The nano-scaled platelets are candidate reinforcement fillers for polymer nanocomposites. Nano-scaled graphene platelets are much lower-cost alternatives to carbon nano-tubes or carbon nano-fibers.