Comparison of hydrogen diffusivities measured by electrochemical permeation and temperature-programmed desorption in cold-rolled pure iron

Zafra, A.; Harris, Zachary D.; Sun, Chao; Martínez‐Pañeda, Emilio

doi:10.1016/j.jngse.2021.104365

Cited by 24 publications

(16 citation statements)

References 54 publications

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“…During the test, J p describes an exponential rising transient until reaching a maximum permeation current density, which is commonly known as the steady-state permeation current, J ss . Further details regarding the EP procedure as well as a schematic representation of the experimental setup (including the reduction and oxidation reactions) are provided elsewhere [53]. After completing the first permeation transient (J c =5 mA/cm 2 ), a second transient was performed on eight of the samples by increasing J c to 10 mA/cm 2 .…”

Section: Hydrogen Permeation Testsmentioning

confidence: 99%

“…% NaCl solution using a Gamry 1010B potentiostat operated in galvanostatic mode to maintain a constant cathodic current density of 5 mA/cm 2 . The specimens were charged for 3 hours to obtain a nominally uniform hydrogen concentration across the plate thickness, based on the previously reported hydrogen diffusivity for the current material heat [53]. ITDS measurements were performed under ultra-high vacuum (10 −9 mbar) conditions using a previously described TDS system [53] equipped with a regularly calibrated Hiden Analytical RC PIC quadrupole mass spectrometer with a hydrogen detection resolution of 4.4 × 10 −6 wppm/s.…”

Section: Isothermal Tds Tests (Itds)mentioning

confidence: 99%

“…However, recent advances in thermal desorption systems, such as the introduction of conductionbased heating and improved vacuum system design for more rapid sample introduction, now enable the use of ITDS for material/sample combinations that were previously considered incompatible with this technique. For example, Zafra et al [53] recently demonstrated that ITDS and EP methods yielded similar average diffusivities for thin (<1 mm thick) sheet specimens of cold-rolled pure Fe. Critically, this direct comparison revealed that the error in replicate ITDS measurements was noticeably reduced relative to the replicate EP experiments [53].…”

Section: Introductionmentioning

confidence: 99%

“…For example, Zafra et al [53] recently demonstrated that ITDS and EP methods yielded similar average diffusivities for thin (<1 mm thick) sheet specimens of cold-rolled pure Fe. Critically, this direct comparison revealed that the error in replicate ITDS measurements was noticeably reduced relative to the replicate EP experiments [53]. It is well-known that EP experiments are prone to significant scatter, which has been historically attributed to numerous factors: the need for sample conditioning prior to starting the permeation experiment [28,[54][55][56][57][58], surface effects [59,60], trapping effects [61][62][63], concentration-dependent diffusion [64,65], analysis method assumptions [52,[66][67][68], failure to reach true steady-state conditions [69], and test-to-test variations in specimen thickness, environmental parameters, among other [70,71].…”

Section: Introductionmentioning

confidence: 99%

“…It is well-known that EP experiments are prone to significant scatter, which has been historically attributed to numerous factors: the need for sample conditioning prior to starting the permeation experiment [28,[54][55][56][57][58], surface effects [59,60], trapping effects [61][62][63], concentration-dependent diffusion [64,65], analysis method assumptions [52,[66][67][68], failure to reach true steady-state conditions [69], and test-to-test variations in specimen thickness, environmental parameters, among other [70,71]. The work of Zafra et al [53] suggests that this longstanding issue of error in EP experiments may be circumvented via the more widespread adoption of ITDS, but this prior study only performed two experiments per technique. As such, additional experiments are needed to more rigorously compare the ITDS and EP methods for measuring hydrogen diffusivity.…”

Section: Introductionmentioning

confidence: 99%

See 4 more Smart Citations

On the relative efficacy of electropermeation and isothermal desorption approaches for measuring hydrogen diffusivity

Zafra¹,

Harris²,

Korec³

et al. 2022

Preprint

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The relative efficacy of electrochemical permeation (EP) and isothermal desorption spectroscopy (ITDS) methods for determining the hydrogen diffusivity is investigated using cold-rolled pure iron. The diffusivities determined from 13 first transient and 8 second transient EP experiments, evaluated using the conventional lag and breakthrough time methods, are compared to the results of 10 ITDS experiments. Results demonstrate that the average diffusivity is similar between the second EP transient and ITDS, which are distinctly increased relative to the first EP transient.However, the coefficient of variation for the ITDS experiments is reduced by 2 and 3-fold relative to the first and second EP transients, confirming the improved repeatability of ITDS diffusivity measurements. The source of the increased error in EP measurements is systematically evaluated, revealing an important influence of assumed electrochemical boundary conditions on the analysis and interpretation of EP experiments.

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Section: Hydrogen Permeation Testsmentioning

confidence: 99%

Section: Isothermal Tds Tests (Itds)mentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

See 3 more Smart Citations

On the relative efficacy of electropermeation and isothermal desorption approaches for measuring hydrogen diffusivity

Zafra¹,

Harris²,

Korec³

et al. 2022

Preprint

View full text Add to dashboard Cite

show abstract

Effect of Tensile Loading and Temperature on the Hydrogen Solubility of Steels at High Gas Pressure

Drexler,

Konert,

Nietzke

et al. 2023

steel research int.

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The hydrogen solubility in ferritic and martensitic steels is affected by hydrostatic stress, pressure and temperature. In general, compressive stresses decrease but tensile stresses increase the hydrogen solubility. This important aspect must be considered when qualifying materials for high‐pressure hydrogen applications (e.g., for pipelines or tanks) by using autoclave systems. This work proposes a pressure equivalent for compensating the effect of compressive stresses on the hydrogen solubility inside of closed autoclaves, to achieve solubilities that are equivalent to those in pipelines and tanks subjected to tensile stresses. Moreover, it is shown that the temperature effect becomes critical at low temperatures (e.g., under cryogenic conditions for storing liquid hydrogen). Trapping of hydrogen in the microstructure can increase the hydrogen solubility with decreasing temperature, having a solubility minimum at about room temperature. In order to demonstrate this effect, the generalized law of the hydrogen solubility is parametrized for different steels using measured contents of gaseous hydrogen. The constant parameter sets are verified and critically discussed with respect to the high‐pressure hydrogen experiments.This article is protected by copyright. All rights reserved.

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Analysis of hydrogen diffusion in the three stage electro-permeation test

Raina

Deshpande

Martínez‐Pañeda

et al. 2023

Continuum Mech. Thermodyn.

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The presence of hydrogen traps within a metallic alloy influences the rate of hydrogen diffusion. The electro-permeation (EP) test can be used to assess this: the permeation of hydrogen through a thin metallic sheet is measured by suitable control of hydrogen concentration on the front face and by recording the flux of hydrogen that exits the rear face. Additional insight is achieved by the more sophisticated three stage EP test: the concentration of free lattice hydrogen on the front face is set to an initial level, is then dropped to a lower intermediate value and is then restored to the initial level. The flux of hydrogen exiting the rear face is measured in all three stages of the test. In the present study, a transient analysis is performed of hydrogen permeation in a three stage EP test, assuming that lattice diffusion is accompanied by trapping and de-trapping. The sensitivity of the three stage EP response to the depth and density of hydrogen traps is quantified. A significant difference in permeation response can exist between the first and third stages of the EP test when the alloy contains a high number density of deep traps.

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Comparison of hydrogen diffusivities measured by electrochemical permeation and temperature-programmed desorption in cold-rolled pure iron

Cited by 24 publications

References 54 publications

On the relative efficacy of electropermeation and isothermal desorption approaches for measuring hydrogen diffusivity

On the relative efficacy of electropermeation and isothermal desorption approaches for measuring hydrogen diffusivity

Effect of Tensile Loading and Temperature on the Hydrogen Solubility of Steels at High Gas Pressure

Analysis of hydrogen diffusion in the three stage electro-permeation test

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