High-sensitivity hydrogen gas permeation: system development, sample preparation, and influence of testing variables
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Published version
Author(s)
Li, R
Zafra, A
Harris, ZD
Martínez-Pañeda, E
Type
Journal Article
Abstract
Background
There is a need to develop quantitative, high-resolution hydrogen gas (H₂) permeation techniques to provide a better understanding of hydrogen-material interactions, from hydrogen uptake and diffusion to embrittlement.
Objective
This study aims to develop and validate a high-sensitivity H₂ permeation system, which is then leveraged to systematically quantify the influence of surface condition and key testing variables (surface oxides, residual gas impurities, pressure, and temperature) on hydrogen permeation.
Methods
A gas permeation system capable of operating at pressures up to 50 bar and temperatures up to 250 ° C was developed, incorporating high-sensitivity mass spectrometric detection and controlled surface preparation protocols. Permeation transients were analysed in a model material (annealed pure Fe) to determine hydrogen diffusivity and permeability under systematically varied surface states, oxygen contents, pressures and temperatures.
Results
Surface oxides are shown to play a dominant role in controlling hydrogen permeation at room temperature. The presence of oxide layers can severely hinder or completely suppress hydrogen uptake, with measurable permeation requiring oxide removal via pickling and Pd coating on both surfaces, or activation through hydrogen-assisted reduction at elevated temperature. Residual oxygen present prior to hydrogen exposure further reduces permeability by modifying surface boundary conditions, indicating strongly surface-controlled kinetics. Under optimised surface conditions, hydrogen transport follows bulk diffusion-controlled behaviour, with steady-state flux obeying Sieverts’ law at 25 ° C (1-5 bar) and diffusivity and permeability exhibiting Arrhenius behaviour between 25 and 150 ° C at 5 bar, indicating bulk diffusion-controlled transport.
Conclusions
The developed high-sensitivity permeation system resolves hydrogen fluxes as low as 1.98 x 10⁻⁹ mol/(m² ⋅s) and provides a robust platform for investigating surface, mechanical and environmental effects on hydrogen permeation under realistic service conditions.
There is a need to develop quantitative, high-resolution hydrogen gas (H₂) permeation techniques to provide a better understanding of hydrogen-material interactions, from hydrogen uptake and diffusion to embrittlement.
Objective
This study aims to develop and validate a high-sensitivity H₂ permeation system, which is then leveraged to systematically quantify the influence of surface condition and key testing variables (surface oxides, residual gas impurities, pressure, and temperature) on hydrogen permeation.
Methods
A gas permeation system capable of operating at pressures up to 50 bar and temperatures up to 250 ° C was developed, incorporating high-sensitivity mass spectrometric detection and controlled surface preparation protocols. Permeation transients were analysed in a model material (annealed pure Fe) to determine hydrogen diffusivity and permeability under systematically varied surface states, oxygen contents, pressures and temperatures.
Results
Surface oxides are shown to play a dominant role in controlling hydrogen permeation at room temperature. The presence of oxide layers can severely hinder or completely suppress hydrogen uptake, with measurable permeation requiring oxide removal via pickling and Pd coating on both surfaces, or activation through hydrogen-assisted reduction at elevated temperature. Residual oxygen present prior to hydrogen exposure further reduces permeability by modifying surface boundary conditions, indicating strongly surface-controlled kinetics. Under optimised surface conditions, hydrogen transport follows bulk diffusion-controlled behaviour, with steady-state flux obeying Sieverts’ law at 25 ° C (1-5 bar) and diffusivity and permeability exhibiting Arrhenius behaviour between 25 and 150 ° C at 5 bar, indicating bulk diffusion-controlled transport.
Conclusions
The developed high-sensitivity permeation system resolves hydrogen fluxes as low as 1.98 x 10⁻⁹ mol/(m² ⋅s) and provides a robust platform for investigating surface, mechanical and environmental effects on hydrogen permeation under realistic service conditions.
Date Issued
2026-09-01
Date Acceptance
2026-06-12
Citation
Experimental mechanics, 2026, 66 (7), pp.1273-1302
ISSN
0014-4851
Publisher
Springer
Start Page
1273
End Page
1302
Journal / Book Title
Experimental mechanics
Volume
66
Issue
7
Copyright Statement
©The Author(s) 2026 Open Access This article is licensed under a Creative Commons Attribution 4.0 International License, which permits use, sharing, adaptation, distribution and reproduction in any medium or format, as long as you give appropriate credit to the original author(s) and the source, provide a link to the Creative Commons licence, and indicate if changes were made. The images or other third party material in this article are included in the article's Creative Commons licence, unless indicated otherwise in a credit line to the material. If material is not included in the article's Creative Commons licence and your intended use is not permitted by statutory regulation or exceeds the permitted use, you will need to obtain permission directly from the copyright holder. To view a copy of this licence, visit http://creativecommons.org/licenses/by/4.0/.
License URL
Identifier
10.1007/s11340-026-01339-6
Subjects
Hydrogen permeation
Gas permeation testing
Diffusion
Surface oxides
Oxygen content
Publication Status
Published
Date Publish Online
2026-06-30
