Low-Energy Plasma Graphene Surface Cleaning and Hydrogenation

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Solution Overview

Problem

Graphene's hydrophobic nature and susceptibility to contamination hinder its use as a substrate for electron microscopy of biological molecules, and existing methods to render it usable, such as conversion to graphene oxide, introduce electron scattering and mechanical instability.

Innovation Solution

Partial hydrogenation of graphene using low-energy hydrogen, helium, or neon plasmas to create a hydrophilic surface for biological molecule deposition while maintaining the graphene's crystalline structure, and using these plasmas to clean the surface without damaging it.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Strength

If graphene is used as a support film for electron microscopy, then mechanical strength and conductivity are improved, but hydrophobicity causes poor deposition of biological molecules

Engineering Contradiction:
Improvemechanical strengthVSAvoiddeposition of biological molecules
Core Design Contradiction:
StrengthVSEase of manufacture

Solution Approach 1:

The patent applies plasma treatment (hydrogen, helium, or neon plasma) to modify the surface properties of graphene. This changes the chemical state of the graphene surface by introducing hydrogenation or cleaning effects, transforming it from hydrophobic to hydrophilic, thereby enabling reliable deposition of biological molecules while preserving the underlying graphene structure and its mechanical strength.

Inventive Principle:
Principle #35Parameter changes

2Reliability

If graphene is used as a support film, then conductivity is improved, but susceptibility to contamination reduces reliability

Engineering Contradiction:
ImproveconductivityVSAvoidsurface contamination
Core Design Contradiction:
ReliabilityVSObject-affected harmful factors

Solution Approach 1:

The patent employs plasma cleaning treatment before using graphene as a support film. This preliminary action removes surface contaminants and creates a clean, hydrophilic surface that is more resistant to subsequent contamination. The plasma treatment prepares the graphene surface in advance, ensuring reliable conductivity and reduced contamination susceptibility during biological molecule deposition and imaging.

Inventive Principle:
Principle #10Preliminary action

3Ease of manufacture

If graphene oxide is used to make graphene hydrophilic, then deposition of biological molecules is improved, but electron scattering increases background signal

Engineering Contradiction:
Improvedeposition of biological moleculesVSAvoidelectron scattering
Core Design Contradiction:
Ease of manufactureVSObject-generated harmful factors

Solution Approach 1:

The patent uses plasma treatment (hydrogen or helium plasma) to achieve hydrophilicity through controlled hydrogenation or surface cleaning, rather than converting graphene to graphene oxide. This parameter change modifies the surface chemistry to enable biological molecule deposition while preserving the graphitic structure, thereby avoiding the electron scattering problems that arise with oxygen-containing groups in graphene oxide.

Inventive Principle:
Principle #35Parameter changes

4Ease of manufacture

If graphene oxide is used to make graphene hydrophilic, then deposition of biological molecules is improved, but mechanical strength decreases

Engineering Contradiction:
Improvedeposition of biological moleculesVSAvoidmechanical strength
Core Design Contradiction:
Ease of manufactureVSStrength

Solution Approach 1:

The patent applies plasma treatment to modify the graphene surface properties, achieving hydrophilicity through controlled surface hydrogenation or cleaning without converting the bulk graphene structure to graphene oxide. This preserves the strong sp2-bonded carbon lattice and mechanical strength of graphene while creating a hydrophilic surface that enables reliable deposition of biological molecules.

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

Facilitates reliable deposition of biological molecules on graphene, reduces beam-induced motion, and improves image quality in electron microscopy by minimizing surface charge and contamination, while preserving the mechanical strength and conductivity of graphene.

Implementation Method 1

contacting said graphene surface post-synthesis with a helium plasma or a neon plasma for a time sufficient to remove surface impurities without damage to the graphene lattice

Methodology Applied
Scientific EffectPlasma: Plasma

Implementation Method 2

partial hydrogenation of graphene using low-energy hydrogen, helium, or neon plasmas to create a hydrophilic surface for biological molecule deposition

Methodology Applied
Scientific EffectHydrogenation: Hydrogenation

Implementation Method 3

exposure to a low-energy hydrogen plasma can convert graphene to graphane, its fully hydrogenated form

Methodology Applied
Scientific EffectPlasma: Plasma

Data Source

PatentEP4144691B1Graphene modification
Publication Date: 2024.09.18 UNITED KINGDOM RESEARCH AND INNOVATION
  • EP4144691B1 patent drawingFigure 1~1d
  • EP4144691B1 patent drawingFigure 2~2c
  • EP4144691B1 patent drawingFigure 3a~3d

AI summary

The invention relates to a method for cleaning a graphene surface post-synthesis by contacting the surface with a hydrogen, helium, or neon plasma at an energy up to 21 eV for a time sufficient to remove surface impurities without damage to the graphene lattice. The invention also relates to cleaned graphene obtained by this method. The invention also relates to a method for making a partially hydrogenated graphene, the method comprising applying a hydrogen ion or hydrogen atom to the surface of graphene, characterised in that said hydrogen ion or hydrogen atom is applied at an energy in the range 1 to 21 eV. The invention also relates to partially hydrogenated graphene obtained by this method.