Double-Sealed Sample Holder for Ultra-High Vacuum Hydrogen Permeation
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Solution Overview
Problem
Existing hydrogen permeation and diffusion path observation devices are unsuitable for ultra-high vacuum environments due to the presence of gases like water and nitrogen, requiring heat-resistant materials and air-tight solutions to maintain vacuum integrity and enable electrochemical hydrogen introduction.
Innovation Solution
A sample holder with an electrolyte introduction chamber, retainer plate, double sealing members, and electrodes for electrolysis, ensuring ultra-high vacuum conditions and efficient hydrogen ion introduction by applying voltage to generate and attract hydrogen ions.
Engineering Contradictions & Design Principles
Engineering Contradiction Analysis
1Measurement precision
If hydrogen gas is introduced into the sample to measure hydrogen permeation, then the measurement can be performed, but the signal intensity is low and measurement time becomes long
Solution Approach 1:
The invention changes the physical-chemical state of hydrogen introduction from molecular hydrogen gas (H2) to atomic hydrogen through plasma generation. This parameter change in the form and energy state of hydrogen enables much higher signal intensity for permeation detection, directly resolving the contradiction between measurement precision and time consumption.
Solution Approach 2:
The invention employs periodic pulsed plasma generation instead of continuous hydrogen gas flow. By applying periodic high-voltage pulses to generate plasma, the system achieves concentrated hydrogen introduction moments that significantly enhance signal intensity while reducing overall measurement time compared to continuous low-intensity gas introduction.
2Quantity of substance
If solution cells are used for hydrogen introduction, then hydrogen can be introduced more effectively, but they cannot be used in ultra-high vacuum environments
Solution Approach 1:
The invention extracts and eliminates the electrolyte component from the solution cell concept, replacing it with a plasma generation system that operates directly in the vacuum environment. This extraction of the incompatible electrolyte while retaining the beneficial hydrogen introduction mechanism enables effective hydrogen supply without compromising vacuum integrity.
Solution Approach 2:
The invention uses plasma in vacuum as an inert environment that is compatible with ultra-high vacuum requirements. Unlike aqueous electrolytes that outgas and contaminate the vacuum, the plasma-based hydrogen introduction method maintains the inert vacuum environment while still achieving effective hydrogen supply to the sample.
3Reliability
If conventional sample holders are used in ultra-high vacuum, then vacuum integrity is compromised by water and nitrogen, but heat-resistant materials and air-tight solutions increase device complexity
Solution Approach 1:
The invention designs a sample holder that serves multiple functions: it acts as both the plasma generation electrode and the sample mounting substrate. The holder structure integrates vacuum sealing, heating, and plasma generation capabilities into a single multi-functional component, reducing overall device complexity while maintaining vacuum integrity.
Solution Approach 2:
The invention employs composite material construction for the sample holder, combining materials with different properties to achieve both vacuum compatibility and plasma generation capability. The holder uses materials that can withstand both the vacuum environment and the high-voltage plasma conditions, eliminating the need for separate heat-resistant and air-tight components.
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
Enables accurate measurement of hydrogen permeation and diffusion paths with improved signal intensity and reduced measurement time, suitable for samples that conventional methods cannot detect.
Implementation Method 1
the hydrogen that is discharged from the surface of the sample is excited by the electron beam, and turns into hydrogen ions, which desorb from the surface (referred to as electron-stimulated desorption (ESD))
Implementation Method 2
electrodes made up of a bias application electrode and an opposing electrode for electrolyzing the electrolyte, wherein a voltage is applied between the electrodes to cause electrolysis to occur
Data Source
AI summary
The sample holder 30 comprises: a holder body 31 for holding the sample 17; an electrolyte introduction chamber 31b provided with an opening 31c that opens to a measurement region 17a of the sample; a retainer plate 33, which is provided with a through-hole 33a corresponding to the measurement region of the sample, for retaining the sample from the electron source side around the through-hole to sandwich the sample airtightly with the holder body; double sealing members 32 arranged between the surface of the holder body and the sample so as to surround the periphery of the measurement region of the sample; a differential exhaust pipe 35, which opens to a space between the sealing members on the surface of the holder body, for exhaust the space through the opening; and electrodes 19 for electrolysis made up of a bias application electrode 19a and an opposing electrode 36.


