Spatially resolved mapping of the relative concentration of dissolved hydrogen using the scanning electrochemical microscope

Schaller, Rebecca; Thomas, Sebastian; Birbilis, Nick; Scully, John R.

doi:10.1016/j.elecom.2014.12.004

Cited by 36 publications

(40 citation statements)

References 30 publications

Supporting

Mentioning

Contrasting

Order By: Relevance

“…Scanning electrochemical microscopy (SECM) has recently been reported as a new technique to detect hydrogen in steel [7]. In this paper, Schaller et al monitored the oxygen reduction reaction at the SECM probe over H-charged regions and over regions with no hydrogen present.…”

Section: Introductionmentioning

confidence: 99%

Hydrogen mapping in an aluminum alloy using an alternating current scanning electrochemical microscope (AC-SECM)

Lafouresse

Bonfils-Lahovary

Laffont

et al. 2017

Electrochemistry Communications

View full text Add to dashboard Cite

OATAO is an open access repository that collects the work of Toulouse researchers and makes it freely available over the web where possible. A B S T R A C TMeasurements using an alternating current scanning electrochemical microscope (AC-SECM) were performed on a 2024 aluminum alloy pre-charged with hydrogen. A gradient in AC current magnitude was observed over several hundreds of microns on the side perpendicular to the charging side. After heat treatment at 130°C for 2 h, the current gradient disappeared. Comparison with scanning Kelvin probe force microscopy (SKPFM) measurements confirmed that the increase in AC current magnitude observed with AC-SECM was due to the presence of hydrogen in the material. Fitting of localized impedance spectra with a suitable equivalent circuit showed the influence of H on the corrosion rate. AC-SECM is thus a powerful new method to detect hydrogen and study its effect on corrosion at the micrometer scale.

show abstract

Section: Introductionmentioning

confidence: 99%

Hydrogen mapping in an aluminum alloy using an alternating current scanning electrochemical microscope (AC-SECM)

Lafouresse

Bonfils-Lahovary

Laffont

et al. 2017

Electrochemistry Communications

View full text Add to dashboard Cite

show abstract

“…KCl), where the electro-reduction of dissolved oxygen (Equation (1)) could be the principle reaction and it can be monitored by SECM. 2 2…”

Section: Secm Measurementsmentioning

confidence: 99%

“…Moreover, the corrosion mechanism is a quite complex process in scratched and coated area of the epoxy coated carbon steel in sat. Ca(OH) 2 containing Cl − ions and depends on the type of metal/alloy, its chemical composition and ability to form a passive film, defect size, concentration of Cl − ions, pH, transport phenomena and the nature of corrosion products [16]. Hence, in the present study, an attempt is made to understand and monitor the local corrosion process of scratched epoxy coated carbon steel in sat.…”

Section: Introductionmentioning

confidence: 99%

See 1 more Smart Citation

<i>In-Situ</i> Corrosion Monitoring of Scratched Epoxy Coated Carbon Steel in Saturated Ca(OH)<sub>2</sub> with or without 3% NaCl by Scanning Electrochemical Microscopy and Electrochemical Impedance Spectroscopy

Balusamy¹,

Nishimura²

2016

AJAC

View full text Add to dashboard Cite

The present work is investigated the in-situ monitoring of local corrosion process of scratched epoxy coated carbon steel in saturated Ca(OH)2 with and without 3% NaCl using SECM and correlated with EIS. The results obtained from EIS analysis showed that the corrosion resistance of scratched epoxy coated carbon steel decreases in Cl − containing solution as the increase in wet/ dry corrosion cycles. This was indicated by decrease in film resistance (Rf) and charge transfer resistance (Rct), while the coated steel maintain the resistance values in saturated Ca(OH)2, most of which recovered after drying. The corrosion process was monitored using SECM by setting the tip potential at −0.70 V vs Ag/AgCl, where the consumption of dissolved oxygen occurred at the surface of test sample. The consumption of dissolved oxygen current (I'oxy-c) values was increased during the immersion in a solution with 3% NaCl. However, in wet/dry corrosion cycles, I'oxy-c was decreased due to the coverage of hydroxides/oxides at scratch area which suppressed the consumption of dissolved O2. It was found that the continuous decrease in corrosion was mainly attributed to continuous formation of corrosion products at anodic spots.

show abstract

“…These include older studies with TEM replica-based tritium microautoradiography technique capable of spatial resolutions of 300 nm pioneered by Tiner and Co-workers [23][24][25] and refined by Lacombe et al at Universite Paris Sud [26][27][28] and secondary ion mass spectrometry (SIMS) ion microscopy 29,30 studies with lateral resolutions limited to 1 μm. Emerging more recently is work using atom probe tomography (APT), which has atomic resolution but samples a much smaller volume (~100,000 nm 3 compared to greater than 1 × 10 9 nm 3 for NanoSIMS), 31,32 as well as scanning probe methods 33,34 that show promise for quantification but whose spatial resolution is of the order of hundreds of microns. NanoSIMS imaging bridges the gap between these two methods, providing a better spatial resolution than tritium autoradiography (and also dispensing with the need to work with radioactive materials) while simultaneously sampling larger volumes than APT, while also offering the potential for absolute quantification of hydrogen concentration using well characterized matrix-matched standards.…”

Section: Introductionmentioning

confidence: 99%

High resolution NanoSIMS imaging of deuterium distributions in 316 stainless steel specimens after fatigue testing in high pressure deuterium environment

2018

View full text Add to dashboard Cite

It is irrefutable that the presence of hydrogen reduces the mechanical performance of many metals and alloys used for structural components. Several mechanisms of hydrogen-assisted cracking (HAC) of steels have been postulated. The direct evidence of the mechanisms by which hydrogen embrittles these materials has remained elusive. This is by virtue of our difficulty to directly observe the hydrogen distribution at spatial resolutions less than 100 nm and analysis volumes greater than 1 × 10 9 atoms at microstructural features such as grain boundaries, dislocations, twins, stacking faults and sub-micron inclusions that are all potential hydrogen trapping sites postulated to be responsible for the degradation of mechanical performance. Here, we report on an experimental methodology combining an elaborate fatigue testing protocol in an enriched gaseous deuterium environment with NanoSIMS (secondary ion mass spectrometry) imaging for detection of deuterium at spatial resolutions as low as 100 nm and accompanying TEM analysis. Type 316 stainless steel compact tension specimens were precharged in deuterium followed by fatigue testing at high stress ratio (0.7), low delta K (~11 MPa √m), and a frequency of 1 cycle per minute using a sawtooth waveform with a rise time of 30 s in high pressure (68.9 MPa) gaseous deuterium (99.999% purity) environment at room temperature. High resolution NanoSIMS imaging was then used to measure the deuterium distribution at the tip of and in the wake of secondary and tertiary fatigue cracks as well as at MnS inclusions. The use of deuterium eliminates the difficulties of interpreting hydrogen measurements by SIMS relating to the ubiquitous presence of hydrogen in all high vacuum systems and guarantees that deuterium measured by the NanoSIMS must be attributed to the fatigue testing protocol. This methodology has allowed us to directly observe the distribution of hydrogen in dislocation tangles ahead and in the wake of fatigue crack tips and at the interface of MnS inclusions. The protocol provides an avenue by which the path and speed with which hydrogen proceeds along its embrittling course of action may be directly followed through modifications of the fatigue testing parameters and/or alloy type and allows a means to validate at least qualitatively recently published models of enhanced hydrogen transport by dislocations.npj Materials Degradation (2018) 2:2 ;

show abstract

Spatially resolved mapping of the relative concentration of dissolved hydrogen using the scanning electrochemical microscope

Cited by 36 publications

References 30 publications

Hydrogen mapping in an aluminum alloy using an alternating current scanning electrochemical microscope (AC-SECM)

Hydrogen mapping in an aluminum alloy using an alternating current scanning electrochemical microscope (AC-SECM)

<i>In-Situ</i> Corrosion Monitoring of Scratched Epoxy Coated Carbon Steel in Saturated Ca(OH)<sub>2</sub> with or without 3% NaCl by Scanning Electrochemical Microscopy and Electrochemical Impedance Spectroscopy

High resolution NanoSIMS imaging of deuterium distributions in 316 stainless steel specimens after fatigue testing in high pressure deuterium environment

Contact Info

Product

Resources

About

Spatially resolved mapping of the relative concentration of dissolved hydrogen using the scanning electrochemical microscope

Cited by 36 publications

References 30 publications

Hydrogen mapping in an aluminum alloy using an alternating current scanning electrochemical microscope (AC-SECM)

Hydrogen mapping in an aluminum alloy using an alternating current scanning electrochemical microscope (AC-SECM)

&lt;i&gt;In-Situ&lt;/i&gt; Corrosion Monitoring of Scratched Epoxy Coated Carbon Steel in Saturated Ca(OH)&lt;sub&gt;2&lt;/sub&gt; with or without 3% NaCl by Scanning Electrochemical Microscopy and Electrochemical Impedance Spectroscopy

High resolution NanoSIMS imaging of deuterium distributions in 316 stainless steel specimens after fatigue testing in high pressure deuterium environment

Contact Info

Product

Resources

About

<i>In-Situ</i> Corrosion Monitoring of Scratched Epoxy Coated Carbon Steel in Saturated Ca(OH)<sub>2</sub> with or without 3% NaCl by Scanning Electrochemical Microscopy and Electrochemical Impedance Spectroscopy