Atom Probe Gas Charge Container for Atomic Hydrogen Positioning

Resolve Bottlenecks,
Find Innovative Solutions
Generate Solutions

Solution Overview

Problem

Conventional methods for observing hydrogen in steel materials lack the necessary spatial resolution to determine its exact position, leading to difficulties in understanding hydrogen embrittlement and developing materials with improved hydrogen resistance.

Innovation Solution

A gas charge container and atom probe apparatus that rapidly cool and convey a needle-shaped sample in a deuterium gas atmosphere, allowing for precise measurement of hydrogen positions at an atomic level by preventing deuterium escape and contamination, enabling efficient hydrogen isotope charging and analysis.

Engineering Contradictions & Design Principles

VSEngineering Contradiction Analysis

1Measurement precision

If conventional thermal desorption methods are used to investigate hydrogen in steel, then the amount of hydrogen can be estimated, but the exact existence position of hydrogen cannot be determined

Engineering Contradiction:
Improvehydrogen position detection precisionVSAvoiddifficulty of hydrogen detection
Core Design Contradiction:
Measurement precisionVSDifficulty of detecting and measuring

Solution Approach 1:

The invention changes the detection parameter from bulk hydrogen amount to spatially-resolved hydrogen position by using atom probe tomography. The method transforms the undetectable hydrogen atoms into detectable ions through field evaporation, enabling precise positional measurement at atomic scale while overcoming the limitations of conventional thermal desorption methods.

Inventive Principle:
Principle #35Parameter changes

Solution Approach 2:

The invention replaces the thermal desorption mechanism with field evaporation mechanism. Instead of using thermal energy to release hydrogen, a high electric field is applied to the needle-shaped sample tip to evaporate atoms and ions, allowing direct observation of hydrogen positions with nanometer-scale spatial resolution.

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

2Productivity

If deuterium gas is introduced into the analysis container before sample measurement, then hydrogen charging can be performed, but deuterium escapes from the sample and contaminates the container

Engineering Contradiction:
Improvehydrogen charging efficiencyVSAvoiddeuterium contamination
Core Design Contradiction:
ProductivityVSObject-generated harmful factors

Solution Approach 1:

The invention performs preliminary cooling of the sample to liquid nitrogen temperature before introducing deuterium gas into the analysis container. This preliminary action prevents deuterium escape during the charging process, as the low temperature suppresses hydrogen diffusion and outgassing, thereby preventing contamination while maintaining charging efficiency.

Inventive Principle:
Principle #10Preliminary action

Solution Approach 2:

The invention creates an inert cold environment by cooling the sample to liquid nitrogen temperature and maintaining vacuum conditions in the analysis container. This inert environment prevents deuterium gas from escaping and contaminating the container, while still allowing efficient deuterium charging of the sample through field evaporation.

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

3Object-generated harmful factors

If the sample is cooled to liquid nitrogen temperature before deuterium charging, then deuterium escape is prevented, but the charging process becomes less efficient

Engineering Contradiction:
Improvedeuterium escapeVSAvoidcharging efficiency
Core Design Contradiction:
Object-generated harmful factorsVSProductivity

Solution Approach 1:

The invention uses periodic pulsed voltage application during field evaporation to achieve efficient deuterium charging. The pulsed action allows sufficient time for deuterium incorporation at low temperature while maintaining high charging efficiency through repeated evaporation and detection cycles, resolving the contradiction between preventing escape and maintaining efficiency.

Inventive Principle:
Principle #19Periodic 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 approach allows for clear visualization of hydrogen positions in materials with high spatial resolution, enhancing the development of materials with improved hydrogen embrittlement resistance and reliability.

Implementation Method 1

a cooling portion for cooling the sample holder; the needle-shaped material is rapidly cooled to -50°C or lower within 10 seconds

Methodology Applied
Scientific EffectRapid cooling: Cooling

Implementation Method 2

a heating portion for heating the needle-shaped material; heating the needle-shaped material to a temperature of 100°C or higher

Methodology Applied
Scientific EffectThermal heating: Heating

Implementation Method 3

carries out field evaporation of sample surface atoms sequentially by a high electric field formed on the surface of the needle

Methodology Applied
Scientific EffectField evaporation:

Implementation Method 4

since the flight time until an evaporated ion reaches the detector is determined depending on the mass of the ion, this measurement then allows the element species of the ion to be determined

Methodology Applied
Scientific EffectTime of flight measurement: Time of Flight

Data Source

PatentEP2302349B1Gas charge container, atom probe apparatus, and method for analyzing hydrogen position in material
Publication Date: 2018.12.19 NIPPON STEEL CORPORATION
  • EP2302349B1 patent drawingFigure 1~2
  • EP2302349B1 patent drawingFigure 3~4
  • EP2302349B1 patent drawingFigure 5~6

AI summary

A gas charge container includes a sample holder which holds a needle-shaped material, a deutrium gas supply portion which charges a deutrium gas into the needle-shaped material held by the sample holder, and a heating portion which heats the needle-shaped material held by the sample holder. The needle-shaped material is cooled by blocking the heat generated by the heating portion after the needle-shaped material is heated by the heating portion.