Electrochemical Graphite Delamination via Ion Intercalation

Resolve Bottlenecks,
Find Innovative Solutions
Generate Solutions

Solution Overview

Problem

Current methods for producing flaky graphite face challenges such as low production yield, energy inefficiency, structural defects, and contamination with impurities, making large-scale and economically efficient production difficult.

Innovation Solution

The use of tetrafluoroboric acid or hexafluorophosphoric acid as an electrolyte in an electrochemical process to produce a thin plate-shaped graphite product, which is then delaminated to achieve high-quality flaky graphite, avoiding the need for chemical oxidants and subsequent purification steps.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Productivity

If mechanical or physical external force is applied to graphite for delamination, then graphite layers can be separated, but production yield is low and energy efficiency is poor

Engineering Contradiction:
Improveproduction yieldVSAvoidenergy efficiency
Core Design Contradiction:
ProductivityVSUse of energy by moving object

Solution Approach 1:

The patent replaces mechanical delamination methods (ultrasonication, adhesive tape exfoliation) with an electrochemical intercalation method. Graphite is treated as a working electrode in an electrochemical cell where electrolyte ions are inserted between layers through electrochemical reactions, enabling efficient separation without mechanical force

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

Solution Approach 2:

The patent changes the fundamental mechanism from mechanical to electrochemical by applying voltage and current parameters. The electrochemical cell operates at controlled potentials (e.g., 0.2-2.0 V vs. Ag/AgCl) and current densities (e.g., 0.1-10 mA/cm²), transforming graphite into a thin plate-shaped product through electrochemical intercalation of electrolyte ions

Inventive Principle:
Principle #35Parameter changes

2Productivity

If chemical oxidants are used for graphite delamination, then graphene oxide can be produced, but product quality deteriorates due to structural defects and impurity contamination

Engineering Contradiction:
Improveproduction yieldVSAvoidproduct quality
Core Design Contradiction:
ProductivityVSManufacturing precision

Solution Approach 1:

The patent replaces chemical oxidation methods with electrochemical intercalation. Instead of using strong oxidants like KMnO4 or H2SO4/HNO3 mixtures that cause structural defects and impurity contamination, the method uses electrochemical reactions in a controlled potential environment to insert electrolyte ions between graphite layers, preserving the integrity of the carbon skeleton

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

Solution Approach 2:

The electrochemical cell creates a controlled, inert environment where graphite is treated as a working electrode. The use of stable electrolytes (aqueous solutions of LiClO4, LiBF4, LiPF6 in ratios of 0.5-5.0 M) and controlled potential ranges prevents unwanted chemical reactions that would introduce impurities or damage the graphite structure

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

3Productivity

If conventional electrochemical methods with aqueous acid electrolytes are used, then graphite intercalation can be achieved, but product quality deteriorates due to structural defects from decomposition gases

Engineering Contradiction:
Improveproduction yieldVSAvoidproduct quality
Core Design Contradiction:
ProductivityVSManufacturing precision

Solution Approach 1:

The patent optimizes electrochemical parameters by using non-aqueous or low-water-content electrolytes (alcoholic solutions of LiClO4, LiBF4, LiPF6 in ratios of 0.5-5.0 M) and controlling the potential range (0.2-2.0 V vs. Ag/AgCl) to prevent water decomposition and gas evolution that would cause structural defects

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The patent uses alcoholic electrolyte solutions (methanol, ethanol, isopropanol) instead of aqueous acid electrolytes to create an inert environment that prevents decomposition gas generation. This maintains the integrity of the graphite structure during electrochemical intercalation

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

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 results in a high-yield, high-quality flaky graphite with minimal defects and impurities, improving current efficiency, time efficiency, and reducing waste, while maintaining the monolayer form and retaining oxygen-containing functional groups.

Implementation Method 1

an electrochemical cell is used, in which graphite is treated as a working electrode, to transform graphite into a thin plate-shaped graphite product

Methodology Applied
Scientific EffectElectrochemical intercalation: Electrolysis

Implementation Method 2

The electrolyte solution contains an alcohol and a lithium salt in a ratio of 0.5 to 5.0 M

Methodology Applied
Scientific EffectIonic conduction: Conduction (electrical)

Data Source

PatentUS12031217B2Method of producing thin plate-shaped graphite product, flaky graphite, and method of producing flaky graphite
Publication Date: 2024.07.09 KANEKA CORP
  • US12031217B2 patent drawing
  • US12031217B2 patent drawing
  • US12031217B2 patent drawing

AI summary

A thin plate-shaped graphite product is produced by applying a current to an electrochemical reaction system including a graphite-containing anode, a cathode optionally containing graphite, and an electrolyte solution containing tetrafluoroboric acid or hexafluorophosphoric acid as an electrolyte. Flaky graphite is produced by subjecting the thin plate-shaped graphite product to delamination.