Ultra high vacuum high precision low background setup with temperature control for thermal desorption mass spectroscopy (TDA-MS) of hydrogen in metals

Merzlikin, Sergiy Vasil ́ović; Borodin, Sergiy; Vogel, Dirk; Rohwerder, Michael

doi:10.1016/j.talanta.2015.01.014

Cited by 18 publications

(8 citation statements)

References 28 publications

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“…However, compared to the non-immersed alloy in the 0.9% NaCl solution, the NiTi archwire indicates arise in the martensite start stress of about 10 MPa. This phenomenon is attributed to the solid-solution hardening during hydrogen charging [ 18 , 19 , 20 , 21 , 22 , 23 , 24 , 25 , 26 , 27 , 28 , 29 , 30 , 31 , 32 ].…”

Section: Resultsmentioning

confidence: 99%

“…All TDA examinations were carried out after 24 h hydrogen charging. The total amount of hydrogen within the specimen was determined to be the sum of desorbed hydrogen within peaks of a hydrogen desorption rate [ 26 , 27 ]. At least two analyses have been done for each cyclic condition, and the experimental errors of the absorbed-hydrogen amount have been estimated between 5% and 10%.…”

Section: Methodsmentioning

confidence: 99%

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Strain Rate Effect upon Mechanical Behaviour of Hydrogen-Charged Cycled NiTi Shape Memory Alloy

Gamaoun

2021

Materials

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The rate dependence of thermo-mechanical responses of superelastic NiTi with different imposed strain rates after cycling from 1 to 50 cycles under applied 10−5s−1, 10−4s−1 and 10−3s−1 strain rates, immersion for 3 h and ageing has been investigated. The loaded and unloaded as-received NiTi alloy under an imposed strain of 7.1% have shown an increase in the residual deformation at zero stress with an increase in strain rates. It has been found that after 13 cycles and hydrogen charging, the amount of absorbed hydrogen (291 mass ppm) was sufficient to cause the embrittlement of the tensile loaded NiTi alloy with 10−5s−1. However, no premature fracture has been detected for the imposed strain rates of 10−4s−1 and 10−3s−1. Nevertheless, after 18 cycles and immersion for 3 h, the fracture has occurred in the plateau of the austenite martensite transformation during loading with 10−4s−1. Despite the higher quantity of absorbed hydrogen, the loaded specimen with a higher imposed strain rate of 10−3s−1 has kept its superelasticity behaviour, even after 20 cycles. We attribute such a behaviour to the interaction between the travelling distance during the growth of the martensitic domains while introducing the martensite phase and the amount of diffused hydrogen.

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Section: Resultsmentioning

confidence: 99%

Section: Methodsmentioning

confidence: 99%

Strain Rate Effect upon Mechanical Behaviour of Hydrogen-Charged Cycled NiTi Shape Memory Alloy

Gamaoun

2021

Materials

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“…With this purpose in mind, the recent molecular-beam thermal desorption spectrometry (MB-TDS) is used in this work [ 12 ]. This technique is a variant of thermal desorption spectrometry which has been developed to detect the hydrogen release by the lowest amounts of solid samples, with several advantages [ 12 , 13 , 14 , 15 , 16 ].…”

Section: Introductionmentioning

confidence: 99%

Hydrogen Nanometrology in Advanced Carbon Nanomaterial Electrodes

2021

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A comparative experimental study between advanced carbon nanostructured electrodes, in similar hydrogen uptake/desorption conditions, is investigated making use of the recent molecular beam-thermal desorption spectrometry. This technique is used for monitoring hydrogen uptake and release from different carbon electrocatalysts: 3D-graphene, single-walled carbon nanotube networks, multi-walled carbon nanotube networks, and carbon nanotube thread. It allows an accurate determination of the hydrogen mass absorbed in electrodes made from these materials, with significant enhancement in the signal-to-noise ratio for trace hydrogen avoiding recourse to ultra-high vacuum procedures. The hydrogen mass spectra account for the enhanced surface capability for hydrogen adsorption in the different types of electrode in similar uptake conditions, and confirm their enhanced hydrogen storage capacity, pointing to a great potential of carbon nanotube threads in replacing the heavier metals or metal alloys as hydrogen storage media.

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“…The detection limit of these techniques strongly depends on the sample volumes because a larger total amount of hydrogen facilitates detection. Therefore, many quantitative hydrogen analyses have been performed on bulk samples with large volumes such as polycrystals and single crystals [9,13]. However, semiconductor device technology is generally based on thin-film deposition and fine-scale processing technologies, for which additional material purification and refinement of processing techniques have been rapidly advancing.…”

Section: Introductionmentioning

confidence: 99%

“…Among the previously discussed hydrogen detection techniques, SIMS and RNRA are the most sensitive quantitative techniques for thin films (hydrogen detection limit ≈ 10 18 atoms/cm 3 ) [11,12]. However, quantitative analyses of extremely low hydrogen concentrations of < 10 18 atoms/cm 3 have only been performed for bulk samples using optical detection [9] and TDS [13]. Thus, the development of hydrogen detection techniques for thin films with much higher sensitivity is strongly needed to better understand the role of hydrogen impurities and accurately control the hydrogen concentration in semiconductor devices.…”

Section: Introductionmentioning

confidence: 99%

Highly hydrogen-sensitive thermal desorption spectroscopy system for quantitative analysis of low hydrogen concentration (∼1 × 1016 atoms/cm3) in thin-film samples

Hanna

Hiramatsu

Sakaguchi

et al. 2017

Review of Scientific Instruments

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We developed a highly hydrogen-sensitive thermal desorption spectroscopy (HHS-TDS) system to detect and quantitatively analyze low hydrogen concentrations in thin films. The system was connected to an in situ sample-transfer chamber system, manipulators, and an rf magnetron sputtering thin-film deposition chamber under an ultra-high-vacuum (UHV) atmosphere of ~10 -8 Pa. The following key requirements were proposed in developing the HHS-TDS: (i) a low hydrogen residual partial pressure,(ii) a low hydrogen exhaust velocity, and (iii) minimization of hydrogen thermal desorption except from the bulk region of the thin films. To satisfy these requirements, appropriate materials and components were selected, and the system was constructed to extract the maximum performance from each component. Consequently, ~2000 times higher sensitivity to hydrogen than that of a commercially available UHV-TDS system was achieved using H

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Ultra high vacuum high precision low background setup with temperature control for thermal desorption mass spectroscopy (TDA-MS) of hydrogen in metals

Cited by 18 publications

References 28 publications

Strain Rate Effect upon Mechanical Behaviour of Hydrogen-Charged Cycled NiTi Shape Memory Alloy

Strain Rate Effect upon Mechanical Behaviour of Hydrogen-Charged Cycled NiTi Shape Memory Alloy

Hydrogen Nanometrology in Advanced Carbon Nanomaterial Electrodes

Highly hydrogen-sensitive thermal desorption spectroscopy system for quantitative analysis of low hydrogen concentration (∼1 × 1016 atoms/cm3) in thin-film samples

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