Carbon Nanotube TEM Grids With Hydrogen-Assisted Infiltration

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Solution Overview

Problem

Carbon nanotube forests delaminate upon cooling after additional carbon infiltration, and existing TEM grids made of high-Z metals or expensive, toxic materials like copper, beryllium, or diamond are unsuitable for chemical and biological applications, leading to inaccurate EDXS analysis and structural limitations.

Innovation Solution

Infiltrate carbon nanotubes with carbon using hydrogen during the infiltration process to prevent delamination and create TEM grids composed of low-Z carbon materials, such as boron carbide, alumina, or silicon dioxide, which are chemically resistant and avoid high-Z atom interference.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Quantity of substance

If additional carbon is added to the carbon nanotube forest via chemical deposition, then the carbon content increases, but the nanotubes delaminate from the substrate upon cooling

Engineering Contradiction:
Improvecarbon contentVSAvoidadhesion to substrate
Core Design Contradiction:
Quantity of substanceVSStability of the object's composition

Solution Approach 1:

Hydrogen gas is introduced as an intermediary substance during the carbon infiltration process. The hydrogen atmosphere acts as a mediator that prevents delamination by maintaining thermal stress balance during cooling, allowing carbon to be deposited without compromising substrate adhesion

Inventive Principle:
Principle #24Intermediary (Mediator)

Solution Approach 2:

The chemical composition of the infiltration atmosphere is changed from pure carbon-source gas to a mixture containing hydrogen. This parameter change in the gas composition enables carbon deposition while preventing the thermal stress-induced delamination that occurs with conventional carbon infiltration methods

Inventive Principle:
Principle #35Parameter changes

2Strength

If high-Z metal grids are used for TEM support, then structural strength is provided, but EDXS analysis shows unwanted interference from the support structure

Engineering Contradiction:
Improvestructural strengthVSAvoidEDXS analysis accuracy
Core Design Contradiction:
StrengthVSMeasurement precision

Solution Approach 1:

The high-Z metal support structure is completely removed and replaced with a low-Z carbon nanotube forest structure. This extraction of the problematic metal component eliminates the source of EDXS interference while maintaining the necessary mechanical support function through the carbon nanotube architecture

Inventive Principle:
Principle #2Taking out (Extraction)

Solution Approach 2:

The support structure is made homogeneous in terms of low atomic number materials. Both the support framework and the sample material are composed of low-Z elements (carbon, and potentially boron, nitrogen, or oxygen), creating material homogeneity that eliminates spectral interference in EDXS analysis

Inventive Principle:
Principle #33Homogeneity

3Strength

If metal grids are used for chemical/biological applications, then structural support is provided, but metals react with samples or preparation materials

Engineering Contradiction:
Improvestructural supportVSAvoidchemical reactivity
Core Design Contradiction:
StrengthVSObject-affected harmful factors

Solution Approach 1:

The carbon nanotube support structure serves as a disposable, chemically inert platform that can be used for various chemical and biological applications without contamination concerns. Unlike metals, the carbon structure does not react with samples or preparation chemicals, eliminating the need for extensive cleaning or replacement due to chemical degradation

Inventive Principle:
Principle #27Cheap short-living objects (Disposable)

4Manufacturing precision

If carbon nanotube forests are created on substrate, then the nanotube structure is formed, but additional carbon infiltration causes delamination upon cooling

Engineering Contradiction:
Improvenanotube structure formationVSAvoidadhesion during cooling
Core Design Contradiction:
Manufacturing precisionVSStability of the object's composition

Solution Approach 1:

Hydrogen gas serves as a protective intermediary during the carbon infiltration and subsequent cooling process. The hydrogen atmosphere mediates the thermal stress management, allowing the nanotube structure to be precisely formed and infiltrated with additional carbon while preventing delamination during the cooling phase

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 stable, high-strength, low-Z carbon TEM grids that resist bending and chemical reactions, allowing accurate EDXS analysis without metal interference, and enables scalable production of thin, suspended films for various applications.

Implementation Method 1

These materials generally are 'grown', via chemical deposition of carbon, upon a substrate

Methodology Applied
Scientific EffectChemical Vapour Deposition: Chemical Vapour Deposition

Implementation Method 2

If a researcher attempts to add additional quantities of carbon to the carbon nanotube forest (via a chemical deposition process involving ethylene within a heated furnace), the infiltrated carbon nanotubes will generally delaminate (separate) from the substrate upon cooling

Methodology Applied
Scientific EffectThermal stress reduction:

Data Source

PatentUS12486569B2Infiltrated carbon nanotubes
Publication Date: 2025.12.02 CNT HLDG LLC
  • US12486569B2 patent drawing
  • US12486569B2 patent drawing
  • US12486569B2 patent drawing

AI summary

Described herein are examples of systems, methods, apparatuses, and devices which include a carbon nanotube structure. The carbon nanotube structure may include a first carbon nanotube with a first top surface and a first bottom surface. The carbon nanotube structure may include a second carbon nanotube vertically aligned with the first carbon nanotube. The second carbon nanotube may include a second top surface and a second bottom surface. The first carbon nanotube and the second carbon nanotube may be infiltrated with carbon by a mixture that is flowing. The mixture may include a first amount of ethylene and a second amount of hydrogen. The carbon nanotube structure may include a thin film extending along the first bottom surface and the second bottom surface.