MXene Nanosheet Surface Modification via Selective Etching and Reduction

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Solution Overview

Problem

The existing methods for manufacturing MXene nanosheets often result in surfaces modified with functional groups like O, OH, or F, which can deteriorate the intrinsic properties of the material.

Innovation Solution

A method involving the selective removal of the A atomic layer from an inorganic compound with a formula of Mn+1AXn, followed by a reduction process to form an MXene nanosheet (Mn+1Xn) without substantial surface modification, using acids like hydrofluoric acid and reducing agents such as alkali metals and amines, to preserve the intrinsic properties.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Manufacturing precision

If strong acid conditions are used to exfoliate MAX phase to remove A layers, then the A layers are effectively removed to form MXene, but the surface is modified with functional groups (O, OH, F) which deteriorates the intrinsic properties of MXene

Engineering Contradiction:
Improveremoval of A layersVSAvoidsurface modification with functional groups
Core Design Contradiction:
Manufacturing precisionVSObject-affected harmful factors

Solution Approach 1:

The patent extracts only the necessary action (removal of A layers) while eliminating the harmful side effect (surface functionalization). By using selective etching with HF followed by reduction treatment, the method removes A layers to form MXene while subsequently removing the unwanted functional groups (O, OH, F) from the surface, thereby obtaining MXene with preserved intrinsic properties

Inventive Principle:
Principle #2Taking out (Extraction)

Solution Approach 2:

The patent changes the chemical state of the surface by applying reduction treatment after acid etching. The reduction process transforms the surface from an oxidized state (with functional groups) to a reduced state, removing O, OH, and F groups. This parameter change (oxidation state) allows the same MXene structure to be obtained with different surface properties - the harmful functional groups are eliminated while maintaining the MXene phase

Inventive Principle:
Principle #35Parameter changes

2Ease of manufacture

If general mechanical or chemical exfoliation methods are used on MAX phase, then the process is simple and easy to perform, but the two-dimensional structure cannot be effectively modified due to strong chemical bonding between transition metal M and A element

Engineering Contradiction:
Improveexfoliation processVSAvoidformation of two-dimensional structure
Core Design Contradiction:
Ease of manufactureVSManufacturing precision

Solution Approach 1:

The patent introduces hydrofluoric acid as an intermediary substance that selectively attacks and removes the A layers from MAX phase. HF acts as a chemical mediator that facilitates the separation of A layers from the M-X layers without requiring strong mechanical force. This intermediary approach enables the formation of two-dimensional MXene structure while maintaining a relatively simple and controllable process

Inventive Principle:
Principle #24Intermediary (Mediator)

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

The method produces MXene nanosheets with unmodified surfaces, exhibiting intrinsic properties and maintaining the two-dimensional structure, as evidenced by electron paramagnetic resonance (EPR) spectroscopy showing peaks attributed to unpaired electrons of the transition metal, suitable for various applications including electronic devices and energy storage.

Implementation Method 1

removing an A atomic layer from an inorganic compound having a formula of Mn+1AXn to form a nanosheet

Methodology Applied
Scientific EffectChemical etching:

Implementation Method 2

reducing the nanosheet having a formula of Mn+1XnTs to form an MXene nanosheet

Methodology Applied
Scientific EffectChemical reduction: Reduction

Implementation Method 3

showing a peak attributed to unpaired electrons of 3d orbitals of a transition metal present on the surface upon electron paramagnetic resonance (EPR) spectroscopy

Methodology Applied
Scientific EffectElectron paramagnetic resonance: Electron Paramagnetic Resonance

Data Source

PatentUS10683208B2MXene nanosheet and manufacturing method thereof
Publication Date: 2020.06.16 SAMSUNG ELECTRONICS CO LTD
  • US10683208B2 patent drawing
  • US10683208B2 patent drawing
  • US10683208B2 patent drawing

AI summary

A method of manufacturing a MXene nanosheet includes removing an A atomic layer from an inorganic compound having a formula of Mn+1AXn to form a nanosheet, the nanosheet having a formula of Mn+1XnTs, and reducing the nanosheet having a formula of Mn+1XnTs to form an MXene nanosheet, the MXene nanosheet having a formula of Mn+1Xn, wherein M is at least one of Group 3 transition metal, Group 4 transition metal, Group 5 transition metal, and Group 6 transition metal, A is at least one of a Group 12 element, Group 13 element, Group 14 element, Group 15 element and Group 16 element, X is one of carbon (C), nitrogen (N) and a combination thereof, Ts is one of oxide (O), epoxide, hydroxide (OH), alkoxide having 1-5 carbon atoms, fluoride (F), chloride (Cl), bromide (Br), iodide (I), and a combination thereof, and n is one of 1, 2 and 3.