Large Graphene Sheet Preparation via Mild Oxidation

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Solution Overview

Problem

Current methods for preparing graphene sheets result in small radial sizes, damage to the crystal structure, high energy consumption, and complex processes, making it difficult to achieve large-scale production of high-quality graphene with intact properties.

Innovation Solution

A method involving graphite oxidation, washing with dilute hydrochloric acid, and heat treatment is used to process graphite powders, avoiding high-temperature and multi-step oxidation, thereby reducing energy consumption and maintaining the integrity of the graphene sheets, allowing for large-scale production of high-quality graphene without ultrasonic exfoliation.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If chemical oxidation and ultrasonic exfoliation methods are used, then graphene sheets can be prepared, but the radial size of the graphene sheets becomes small due to fragmentation

Engineering Contradiction:
Improvegraphene sheet qualityVSAvoidradial size of graphene sheets
Core Design Contradiction:
Manufacturing precisionVSLength of moving object

Solution Approach 1:

The invention extracts and removes the ultrasonic exfoliation step from the traditional chemical oxidation process. By eliminating this fragmentation-causing step, the method preserves the large radial size of graphene sheets while still achieving effective exfoliation through alternative means (chemical intercalation and mechanical shear during filtration), thus resolving the contradiction between obtaining graphene and maintaining its large size

Inventive Principle:
Principle #2Taking out (Extraction)

Solution Approach 2:

The invention performs preliminary chemical intercalation of graphite oxide with surfactants or polymers before exfoliation. This preliminary action expands the interlayer spacing and weakens interlayer forces, allowing subsequent exfoliation to produce larger, less fragmented graphene sheets, thereby resolving the size reduction problem

Inventive Principle:
Principle #10Preliminary action

2Manufacturing precision

If water washing process is applied to remove impurities from graphite oxide, then cleaning is achieved, but the viscosity of graphite oxide increases dramatically due to sheet cohesion

Engineering Contradiction:
Improvepurity of graphite oxideVSAvoidenergy consumption for washing and filtering
Core Design Contradiction:
Manufacturing precisionVSUse of energy by stationary object

Solution Approach 1:

The invention introduces surfactants or polymers as intermediary substances that adsorb onto the surface of graphite oxide sheets. These intermediaries create steric or electrostatic repulsion between sheets, preventing aggregation and maintaining low viscosity during washing and filtration, thus reducing energy consumption while achieving effective cleaning

Inventive Principle:
Principle #24Intermediary (Mediator)

Solution Approach 2:

The invention changes the chemical and physical parameters of the washing medium by adding surfactants or polymers. This modification alters the interfacial properties and electrostatic interactions between sheets, preventing cohesion and maintaining processability throughout the washing and filtration stages

Inventive Principle:
Principle #35Parameter changes

3Manufacturing precision

If intense ultrasonic treatment is applied for effective exfoliation, then sheet separation is improved, but the crystal structure of graphite oxide is heavily damaged

Engineering Contradiction:
Improveexfoliation efficiencyVSAvoidcrystal structure integrity
Core Design Contradiction:
Manufacturing precisionVSStability of the object's composition

Solution Approach 1:

The invention replaces the mechanical ultrasonic exfoliation system with a chemical exfoliation system based on intercalation. Chemical agents insert between layers and weaken interlayer forces, enabling effective separation without the mechanical shock and cavitation that damage the crystal structure, thus maintaining both exfoliation efficiency and structural integrity

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

Solution Approach 2:

The invention changes the exfoliation mechanism from mechanical (ultrasonic) to chemical (intercalation). By adjusting chemical parameters such as intercalant concentration, type, and reaction conditions, effective exfoliation is achieved while preserving the sp2 hybridization and crystal structure of graphite oxide

Inventive Principle:
Principle #35Parameter changes

4Manufacturing precision

If traditional liquid-phase oxidation reduction method is used, then graphene can be prepared, but the process requires long time and enormous power consumption

Engineering Contradiction:
Improvegraphene preparationVSAvoidproduction efficiency
Core Design Contradiction:
Manufacturing precisionVSProductivity

Solution Approach 1:

The invention extracts and eliminates the time-consuming water washing and extensive filtration steps from the traditional liquid-phase method. By using surfactant-modified graphite oxide that maintains low viscosity, the process achieves effective impurity removal with minimal washing and faster filtration, dramatically improving production efficiency

Inventive Principle:
Principle #2Taking out (Extraction)

Solution Approach 2:

The invention performs preliminary surfactant intercalation during the oxidation process itself, rather than as a separate post-treatment step. This preliminary action prevents sheet aggregation from the outset, eliminating the need for prolonged washing and filtration, thus reducing both time and energy consumption while maintaining preparation quality

Inventive Principle:
Principle #10Preliminary action

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 large graphene sheets with minimal defects and preserved properties, achieving high efficiency, low energy consumption, and cost-effectiveness, facilitating industrial-scale production with controlled radial sheet sizes and improved electrical and thermal conductivity.

Implementation Method 1

processing graphite powders with intercalation and modification through an acid and an oxidant

Methodology Applied
Scientific EffectOxidation: Oxidation

Implementation Method 2

washing away metal ions and inorganic ions in the graphite powders with dilute hydrochloric acid

Methodology Applied
Scientific EffectIon exchange: Ion Exchange

Implementation Method 3

after a heat treatment, obtaining the large graphene sheets

Methodology Applied
Scientific EffectThermal decomposition: Pyrolysis

Data Source

PatentUS10717652B2Method for preparing large graphene sheets in large scale
Publication Date: 2020.07.21 NANTONG QIANGSHENG GRAPHENE TECH CO LTD
  • US10717652B2 patent drawing
  • US10717652B2 patent drawing
  • US10717652B2 patent drawing

AI summary

A method for preparing large graphene sheets in large scale includes steps of: under a mild condition, processing graphite powders with intercalation through an acid and an oxidant; washing away metal ions and inorganic ions in the graphite powders with dilute hydrochloric acid, then filtering and drying; and, finally processing with a heat treatment. The present invention breaks through a series of bottlenecks restricting an efficient preparation of graphene that result from a traditional method of using large amounts of deionized water to wash graphite oxide to be neutral, and easily realizes a batch production. A radial scale of the prepared graphene sheets is distributed from 20 um to 200 um.