Thermal Desorption Spectroscopy Measurements Research Articles

Influence of heating rate and storage condition on thermal desorption of deuterium in tungsten

The retention of hydrogen isotopes in tungsten has been a critical issue in future fusion facilities. Thermal desorption spectroscopy (TDS) is a common method for the studies of hydrogen isotope retention. To explore the effect of heating rate in TDS measurement, a series of deuterium (D) desorption experiments with different heating rates were conducted. The results were compared with TMAP7 (Tritium Migration and Analysis Program, version 7) simulations and Kissinger's theory. An empirical expression for the analysis of desorption spectra with different heating rates was derived. The expression was verified in another set of experiments on helium (He) desorption. Furthermore, the formation of molecules containing D atoms during TDS measurements was investigated. Specimens exposed to D plasma were stored in air and vacuum respectively for three months prior to desorption experiments. Signals of H, H2, HD, D2, HDO and D2O were detected. The reasons for the formation of these species were explored.

Evaluation of hydrogen embrittlement in ODS-Cu, Cu–Cr–Zr, and Cu–Cr alloys using slow strain rate technique test

Precipitation-hardened Cu–Cr–Zr alloy is proposed as a heat sink material for various components of the ITER owing to its high strength, high conductivity, and superior resistance against neutron irradiation. Oxide-dispersion-strengthened copper (ODS-Cu) was selected as the candidate material. Hydrogen embrittlement of Cu–Cr–Zr, Cu–Cr, and ODS-Cu (GlidCop® CuAl60) alloys was evaluated using the slow strain rate technique (SSRT) in 0.1 M sodium sulfate (Na2SO4) solutions under cathodic hydrogen charging or after D2 gas exposure. Thermal desorption spectroscopy (TDS) measurements were performed to estimate the differences in the hydrogen-trapping sites using hydrogen charging methods. According to the TDS results, the quantity of hydrogen retained in ODS-Cu exceeded that in the other alloys by an order of magnitude because of hydrogen trapping at the grain boundaries and the particle/matrix interface. Cu–Cr–Zr alloys tend to trap more hydrogen than Cu–Cr alloys because of the addition of Zr. As a result of the SSRT, no hydrogen embrittlement was observed in any alloy, regardless of the hydrogen charging method. All alloys exhibited excellent hydrogen embrittlement resistance under the conditions adopted in this study.

Effective treatment of hydrogen boride sheets for long-term stabilization.

Two-dimensional hydrogen boride (HB) sheets prepared via the ion-exchange reaction from magnesium diboride (MgB2) are known to possess several intriguing properties for a wide range of applications; however, previous reports have shown that the sheets prepared using this method contain small amounts of reactive components, making them unsuitable for certain applications. Therefore, developing a method for preparing HB sheets that exhibit long-term stability and do not contain reactive species is essential. In this study, we developed an effective treatment method for achieving long-term stabilization of HB sheets. We found that by pre-treating the HB sheets with water and then filtering the dried product from an acetonitrile dispersion, we could achieve excellent long-term stability over nine months. This stability was maintained even outside of a glovebox, with no H2 released by the decomposition and/or reaction. X-ray photoelectron spectroscopy (XPS) and Fourier transform infrared (FT-IR) absorption spectroscopy measurements revealed that the sample exhibited pure HB characteristics with negatively charged boron and B-H-B and terminal B-H bonds, even after nine months of storage. Furthermore, based on thermal desorption spectroscopy (TDS) measurements, the presence of reactive species in the as-prepared HB sheets is attributed to fluctuating B-H bonds with relatively weak binding energies that can be removed using the method developed in this study.

Hydrogen-induced micro-void formation in copper used for spent nuclear fuel disposal canisters

Spent nuclear fuel is planned to be deposited in the 50 mm thick copper canisters at about 500 m depth in the bedrock. Hydrogen uptake may occur in the disposal conditions in copper due to corrosion reactions and effects of irradiation. Therefore, it is important to know in which conditions the hydrogen uptake results in the formation of pressurized hydrogen bubbles near the copper surface. During the thermal desorption spectroscopy (TDS) measurements the existing hydrogen bubbles grow due to accumulation of dissolved hydrogen and build-up of hydrogen gas pressure inside the voids. The further growth of the voids occurs by plastic deformation and results opening of the voids near the copper surface due to increasing temperature. The friction-stir weld metal samples of phosphorous-doped oxygen-free copper were cathodically charged with hydrogen in a 1.0 N H2SO4 solution with added 10 mg/L thiourea at various electrochemical potentials, -0.95…-1.3 VSCE. A threshold potential of -1.10 VSCE was found for the marked increase of hydrogen uptake and hydrogen-induced void formation near the copper surface.

A combined thermal desorption spectroscopy and internal friction study on the interaction of hydrogen with microstructural defects and the influence of carbon distribution

Hydrogen interactions with different microstructural defects were analysed in ultra-low carbon steel, with specific focus on the influence of carbon distribution. For this purpose, the steel was cold rolled and subjected to various annealing treatments, obtaining microstructures ranging from as cold rolled, over recovered up to fully recrystallized. Optical microscopy, transmission electron microscopy and hardness measurements were used to obtain information on the grain boundary structure and dislocation density. Positron annihilation spectroscopy measurements revealed metastable open volume defects related to both dislocations and vacancy clusters. The carbon distribution was characterized by internal friction experiments. Hydrogen interactions were studied by thermal desorption spectroscopy and internal friction measurements of samples electrochemically pre-charged with hydrogen.The most dominant contribution in hydrogen trapping in the cold rolled material is provided by dislocations. However, their contribution is strongly reduced after annealing at temperatures in the range between 300 K and 600 K due to dissolution of metastable kink-pairs and small carbon-vacancy clusters. Dissolution of such clusters provides fresh supply of carbon to dislocations, which reduces the dislocation trapping capacity for hydrogen due to carbon-hydrogen repulsion. The presence of carbon also reduces the vacancy mobility, allowing clustering and growth during cold rolling resulting in strong hydrogen trapping sites. Binding energies at dislocations were obtained from thermal desorption spectroscopy and internal friction measurements and compared to various models. The small discrepancy in the activation energy is argued to originate from the quantum effect. Hydrogen release from vacancy clusters is determined by the energy required for complete cluster dissolution.

A comparative study on the hydrogen dissolution and release behaviors in the zirconate proton conductors by TDS and TMAP4 analysis

Proton-conducting oxides are potential materials for electrochemical devices such as fuel cells, hydrogen pumps, hydrogen sensors, and the tritium purification and recovery system in nuclear fusion reactors. The hydrogen concentration in oxide materials is important, but its precise measurement is difficult. In this study, thermal desorption spectroscopy (TDS) was used to investigate hydrogen dissolution and release behavior in proton-conducting oxides, yttrium (Y), and cobalt (Co) doped barium-zirconates in the temperature range of 673-1273 K using deuterium (D2) and heavy water (D2O). Specimens were prepared with conventional powder metallurgy: the powder of three zirconates, BaZr0.9Y0.1O3-a (BZY), BaZr0.955Y0.03Co0.015O3-a (BZYC), and CaZr0.9In0.1O2.95 (CZI) was pressed into discs and fired in the air at 1873 K for 20 h. The densities of the sintered BZY, BZYC, and CZI specimens were 98 percent, 99.7 percent, and 99.5 percent of the theoretical densities respectively. XRD, SEM, and EDX were performed for the structural and morphological analysis of the sintered samples. From TDS measurement, a similar trend of temperature-dependent hydrogen solubility was obtained for all samples compared to the tritium imaging plate (TIP) methods literature data of HT- and DTO-exposed samples. To compare the experimental results of the deuterium desorption profile derived by TDS analysis, the simulation code of the tritium migration analysis program, version 4 (TMAP4) was employed.

In silico screening and experimental study of anion-pillared metal-organic frameworks for hydrogen isotope separation

Deuterium is a key energy source for fusion reaction and widely used in various application fields. Nevertheless, the separation of deuterium from its isotopic mixture with nearly same physicochemical properties is one of the greatest challenging tasks in industry. Compared with cryogenic distillation, quantum sieving effect based on nanoporous materials has been proposed as a promising strategy for isotopes separation, in which metal-organic frameworks (MOFs) are considered as an ideal platform because of their structural diversity and tailorable functionality. In this work, high-throughput molecular simulations were performed to identify optimal structural features of high-performance materials from a recently-constructed database of anion-pillared MOFs. As a proof-of-concept, the identified material SIFSIX-18-Cd was prepared using a proposed direct mixing method, which can achieve a goal of quickly preparation of such material on a large scale. The experimental pure-component adsorption isotherms of D2 and H2 confirmed the preferential adsorption of SIFSIX-18-Cd for D2 over H2 due to the quantum sieving effect. The advanced cryogenic thermal desorption spectroscopy (ACTDS) measurements further showed that the enrichment factor (EF) of an equimolar D2/H2 mixture in SIFSIX-18-Cd can reach 5.1 at 30 K and 1.0 bar, which is higher than the current cryogenic distillation method (1.5 at 24 K). Along with the proposed efficient preparation method, the high hydrophobic property of SIFSIX-18-Cd also demonstrated a broad industrial prospect of this material for hydrogen isotope separation.

Isotope-selective pore opening in a flexible metal-organic framework.

Flexible metal-organic frameworks that show reversible guest-induced phase transitions between closed and open pore phases have enormous potential for highly selective, energy-efficient gas separations. Here, we present the gate-opening process of DUT-8(Ni) that selectively responds to D2, whereas no response is observed for H2 and HD. In situ neutron diffraction directly reveals this pressure-dependent phase transition. Low-temperature thermal desorption spectroscopy measurements indicate an outstanding D2-over-H2 selectivity of 11.6 at 23.3 K, with high D2 uptake. First-principles calculations coupled with statistical thermodynamics predict the isotope-selective gate opening, rationalized by pronounced nuclear quantum effects. Simulations suggest DUT-8(Ni) to remain closed in the presence of HT, while it also opens for DT and T2, demonstrating gate opening as a highly effective approach for isotopolog separation.

Comparative Studies of Hydrogen Dissolution and Release Behavior in Zirconate Oxides by TDS and TMAP4 Analysis

Proton-conducting oxides are potential materials for electrochemical devices such as fuel cells, hydrogen pumps, hydrogen sensors, and the tritium purification and recovery system in nuclear fusion reactors. The hydrogen concentration in oxide materials is important, but its precise measurement is difficult. In this study, thermal desorption spectroscopy (TDS) was used to investigate hydrogen dissolution and release behavior in proton-conducting oxides, yttrium (Y), and cobalt (Co) doped barium-zirconates in the temperature range of 673-1273 K using deuterium (D2) and heavy water (D2O). Specimens were prepared with conventional powder metallurgy: the powder of three zirconates, BaZr0.9Y0.1O3-a (BZY), BaZr0.955Y0.03Co0.015O3-a (BZYC), and CaZr0.9In0.1O2.95 (CZI) was pressed into discs and fired in the air at 1873 K for 20 h. The densities of the sintered BZY, BZYC, and CZI specimens were 98 percent, 99.7 percent, and 99.5 percent of the theoretical densities respectively. XRD, SEM, and EDX were performed for the structural and morphological analysis of the sintered samples. From TDS measurement, a similar trend of temperature-dependent hydrogen solubility was obtained for all samples compared to the tritium imaging plate (TIP) methods literature data of HT- and DTO-exposed samples. To compare the experimental results of the deuterium desorption profile derived by TDS analysis, the simulation code of the tritium migration analysis program, version 4 (TMAP4) was employed.

Effect of surface quality on hydrogen/helium irradiation behavior in tungsten

As the plasma facing material in the nuclear fusion reactor, tungsten has to bear the irradiation impact of high energy particles. The surface quality of tungsten may affect its irradiation resistance, and even affect the service life of fusion reactor. In this paper, tungsten samples with different surface quality were polished by mechanical processing, subsequently conducted by D2+ implantation and thermal desorption. D2+ implantation was performed at room temperature (RT) with the irradiation dose of 1 × 1021 D2+/m2 by 5 keV D2+ ions, and thermal desorption spectroscopy measurements were done from RT to 900 K. In addition, He irradiation was also performed by 50 eV He+ ions energy with the fluxes of 5.5 × 1021 m−2s−1 and 1.5 × 1022 m−2s−1, respectively. Results reveal that the hydrogen/helium irradiation behavior are both related to surface quality. Samples with high surface quality has superior D2+ retention behavior with less D2 retained after implantation. However, such samples are more likely to generate fuzzes on the surface after helium irradiation. Different morphologies (smooth, wavy, pyramids) after helium irradiation also demonstrates that the surface morphology is related to tungsten crystallographic orientation.

Determination of Critical Hydrogen Concentration and Its Effect on Mechanical Performance of 2200 MPa and 600 HBW Martensitic Ultra-High-Strength Steel

The influence of hydrogen on the mechanical performance of a hot-rolled martensitic steel was studied by means of constant extension rate test (CERT) and constant load test (CLT) followed with thermal desorption spectroscopy measurements. The steel shows a reduction in tensile strength up to 25% of ultimate tensile strength (UTS) at critical hydrogen concentrations determined to be about 1.1 wt.ppm and 50% of UTS at hydrogen concentrations of 2 wt.ppm. No further strength degradation was observed up to hydrogen concentrations of 4.8 wt.ppm. It was observed that the interplay between local hydrogen concentrations and local stress states, accompanied with the presence of total average hydrogen reducing the general plasticity of the specimen are responsible for the observed strength degradation of the steel at the critical concentrations of hydrogen. Under CLT, the steel does not show sensitivity to hydrogen at applied loads below 50% of UTS under continuous electrochemical hydrogen charging up to 85 h. Hydrogen enhanced creep rates during constant load increased linearly with increasing hydrogen concentration in the steel.

Effect of brush plating process variables on the microstructures of Cd and ZnNi coatings and hydrogen embrittlement

Brush plated ZnNi coating is evaluated for replacement of Cd coating during repair of sacrificial coatings on high strength steel components. Plating parameters such as deposition voltage, surface preparation and type of anode for coating deposition are used to study the risk of Internal Hydrogen Embrittlement (IHE). Coating characterization using Transmission Electron Microscopy (TEM) is correlated with Incremental Step Load (ISL) testing, permeation measurements and Thermal Desorption Spectroscopy (TDS) to evaluate the effect of microstructure and crystallographic defects within the coating on the risk of internal hydrogen embrittlement (IHE) of the substrate steel. It is observed that the coating microstructure plays an important role in mitigating IHE. Brush plated ZnNi coatings at 6 V deposition voltage with grit blast method of surface preparation and graphite anode, or deposition at 12 V with scotch-brite™ method of surface preparation and either of platinized Ti or graphite anode can suitably replace Cd coating. Presence of twin boundaries within the coating proved to be beneficial to decrease the risk of IHE by minimizing the H diffusion to the substrate. On the other hand, stacking faults and dislocations within the ZnNi coating do not sufficiently trap hydrogen and therefore do not mitigate the IHE risk when plated at 10 V and 12 V. Coating deposited at 6 V generates low amount of hydrogen, and does not cause IHE irrespective of the microstructure. TDS measurements performed to quantify the hydrogen desorption from different plating conditions indicate a direct correlation between the amount of hydrogen generated during plating and degradation of mechanical strength by IHE cannot always be established, principally because of the influence of microstructure.

Deuterium transport and retention properties of representative fusion blanket structural materials

Reduced activation ferritic-martensitic (RAFM) steels have been developed for decades for use as fusion blanket structural materials, and have advantages in both mechanical properties and irradiation resistance following careful engineering of the microstructure. However, the hydrogen isotope behavior in these proposed fusion structural materials is not well understood, but is important to assess since it impacts the fusion reactor safety and self-sufficient tritium fuel cycle. In this work, we investigated deuterium transport and retention in representative advanced RAFM steels, including castable nanostructured alloys (CNAs), and oxide-dispersion-strengthened (ODS) steels. A gas-driven permeation (GDP) system was used to measure the permeability, diffusivity and solubility of the studied materials, covering the temperature range from 623 K to 873 K, and the loading pressures from 1.8×104 to 1.0×105 Pa. The results indicated that the deuterium permeability has little material dependence. In contrast, the deuterium diffusivity of the studied materials showed significant variation. The deuterium diffusivity in ODS steels is one order of magnitude lower than that in RAFM steels and CNAs, and correspondingly, have an effective solubility that is 2–10 times larger than RAFM steels and CNAs. In addition, thermal desorption spectroscopy (TDS) measurements were performed to assess the deuterium retention and desorption of these materials following a static thermal deuterium charging at 723 Kfor 1 hour under the deuterium pressure of 1.0×105Pa. It was found that ODS steels exhibit the highest deuterium retention and have broader desorption peaks. Microstructural features contributing to deuterium retention and impacting deuterium transport are discussed to rationalize the observed deuterium behavior in the studied RAFM steels.

A high temperature dual-mode quartz crystal microbalance technique for erosion and thermal desorption spectroscopy measurements.

An improved quartz crystal microbalance measurement method is described, which allows us to determine erosion, implantation, and release rates of thin films, during changing temperatures and up to 700 K. A quasi-simultaneous excitation of two eigenmodes of the quartz resonator is able to compensate for frequency drifts due to temperature changes. The necessary electronics, the controlling behavior, and the dual-mode temperature compensation are described. With this improved technique, quantitative in situ temperature-programmed desorption measurements are possible and the quartz crystal microbalance can be used for quantification of thermal desorption spectroscopy measurements with a quadrupole mass spectrometer. This is demonstrated by a study of the retention and release behavior of hydrogen isotopes in fusion-relevant materials. We find that more than 90% of the deuterium implanted into a thin film of beryllium is released during a subsequent temperature ramp up to 500 K.

Hydrogen permeation and retention in deuterium plasma exposed 316L ITER steel

Abstract Fuel permeation and retention in fusion reactor wall materials are important issues for plasma operation and safety reasons in ITER. The austenitic stainless steel 316L(N)-IG will be used as structural material in the first wall components in ITER. The impact of deuterium plasma exposure on the deuterium permeation and retention was studied. Polished 316L(N)-IG steel samples were deuterium plasma exposed with an ion energy of 200 eV and at two different fluences. Deuterium gas-driven permeation and thermal desorption spectroscopy measurements were performed afterwards. By comparison of the exposed samples to an unexposed sample, it is concluded that the surface roughness due to plasma exposure has no significant influence on the deuterium permeation through the samples. The first results of thermal desorption spectroscopy analysis show that the main release of retained deuterium is between 600 ∘ C and 900 ∘ C and the release temperature increases by increasing the plasma fluence.

Influence of neon seeding on the deuterium retention and surface modification of ITER-like forged tungsten

In order to investigate the effect of neon seeding on deuterium retention and surface modification of ITER-like forged tungsten with grains elongated perpendicular to the surface, pure and neon-seeded deuterium plasma exposures were performed in the linear plasma device PSI-2. The ion percentage of neon in the mixed plasma was around 10%. The sample temperature and deuterium ion fluence were kept at 450 K and 1 × 1026 m−2, respectively. The incident ion energy was 40 eV, just reaching the tungsten sputtering threshold for neon. Surface observations show that neon seeding leads to pronounced cracking and erosion of blister caps and a significant reduction of small blisters (<0.8 μm). This is possibly attributed to surface sputtering and the inhibitory effect of neon-induced defects on blister nucleation by hindering dislocation movements. On the other hand, neon seeding increases the total deuterium retention by ∼70% according to the thermal desorption spectroscopy (TDS) measurements. A low-temperature desorption peak (∼660 K) which should be mainly ascribed to deuterium de-trapping from dislocations is observed to be broadened and shifts towards higher temperature in the case of neon seeding, suggesting enhanced inward diffusion and trapping of deuterium. An additional deuterium release peak appears at a higher temperature (∼803 K), indicating the creation of new deuterium-traps induced by neon. A comparison of the results of nuclear reaction analysis and TDS reveals that neon seeding not only increases deuterium retention in the surface region (<7.2 μm) but also in the bulk (>7.2 μm). We ascribe the enhanced deuterium retention to the increased deuterium-traps in the top-surface induced by Ne irradiation and the vertical grain boundary configuration of the forged W promoting the inward diffusion of deuterium.

Atomistic State of Hydrogen in Electrochemically Deposited Cu Films

Electro and electroless deposition of Cu films are widely used in the print circuit boards production. These electrochemical Cu deposition process are accompanied with the simultaneous hydrogen evolution, and the hydrogen co-deposition sometimes causes the voids and blisters1). However, the detail mechanism of such hydrogen-induced phenomena have not been clarified. We previously reported that the primary cause of the room-temperature grain growth observed in electrodeposited Cu films was the formation of superabundant vacancies induced by the hydrogen co-deposition2). In this study, the atomistic state of hydrogen co-deposited in the Cu films obtained by electro and electroless deposition and the influence of hydrogen on the microstructure of Cu films were investigated.Cu films were electrodeposited from six different baths (sulfate bath, additive-containing bath, chloride bath, pyrophosphate bath, EDA bath, and EDTA bath) and electrolessly deposited from an EDTA bath. The amount and atomistic state of hydrogen in the Cu films were analyzed by thermal desorption spectroscopy (TDS). The microstructural analysis of the Cu films was performed by X-ray diffraction (XRD) and transmission electron microscopy (TEM).In the electrodeposited Cu films with high hydrogen concentrations (x = H/Cu = 5.4 ~ 98.2×10-4), the room-temperature grain growth proceeded with the desorption of hydrogen during 7 ~ 21 days after deposition2). A pronounced desorption peak at 600 ~ 700 K due to the break-up of vacancy-hydrogen clusters3) was observed in the thermal desorption spectra of hydrogen from these Cu films.In the thermal desorption spectra of hydrogen from electrolessly deposited Cu films, a pronounced peak at around 420 K and a small peak at 600 ~ 700 K were observed and the hydrogen concentration was x = 13.6×10-3. From the XRD measurements, the lattice expansion of about 0.14% was observed in the as-deposited Cu films, which was reduced with the desorption of hydrogen at room temperature after 7 days. These results suggest that the desorption peak at 420 K may be assigned to the desorption of hydrogen from the regular interstitial sites. In the TEM images of these Cu films, many nano-voids distributed in the crystal grains were observed. We consider that the hydrogen molecules trapped in the nano-voids should be desorbed at high temperature above 900 K. The high-temperature TDS measurements will be performed. References 1) T. Sharma, A. E. Landry, A. Leger, D. A. Brown, T. Bernhard, S. Zarwell, F. Brüning, and R. Brüning, Thin Solid Films, 666, 76 (2018).2) N. Fukumuro, H. Yoshida, T. Yamazaki, Y. Fukai, and S. Yae, J. Japan. Inst. Met. Mater., 80, 736 (2016).3) Y. Fukai, M. Mizutani, S. Yokota, M. Kanazawa, Y. Miura, and T. Watanabe, J. Alloy. Comp., 356-357, 270 (2003).

Determination of the detrapping energy of tritium in tungsten

Thermal desorption spectroscopy (TDS) measurement of tungsten (W) exposed to tritium (T2) under a series of conditions was conducted, and the peak of T2 desorption reached as high as 895 K at the heating rate of 20 K/min. The detrapping energy of T in W was then determined experimentally to be 2.18 ± 0.22 eV, suggesting that T was mainly trapped by vacancy clusters which may be formed during manufacturing and enhanced by charged T atoms.

In Situ Study of Molecular Doping of Chlorine on MoS2 Field Effect Transistor Device in Ultrahigh Vacuum Conditions.

We report a precise measurement of the sensor behavior of the field effect transistor (FET) formed with the MoS2 channel when the channel part is exposed to Cl2 gas. The gas exposure and the electrical measurement of the MoS2 FET were executed with in situ ultrahigh-vacuum (UHV) conditions in which the surface analysis techniques were equipped. This makes it possible to detect how much sensitivity the MoS2 FET can provide and understand the surface properties. With the Cl2 gas exposure to the channel, the plot of the drain current versus the gate voltage (Id–Vg curve) shifts monotonically toward the positive direction of Vg, suggesting that the adsorbate acts as an electron acceptor. The Id–Vg shifts are numerically estimated by measuring the onset of Id (threshold voltage, Vth) and the mobility as a function of the dosing amounts of the Cl2 gas. The behaviors of both the Vth shift and the mobility with the Cl2 dosing amount can be fitted with the Langmuir adsorption kinetics, which is typically seen in the uptake curve of molecule adsorption onto well-defined surfaces. This can be accounted for by a model where an impinging molecule occupies an empty site with a certain probability, and each adsorbate receives a certain amount of negative charge from the MoS2 surface up to the monolayer coverage. The charge transfer makes the Vth shifts. In addition, the mobility is reduced by the enhancement of the Coulomb scattering for the electron flow in the MoS2 channel by the accumulated charge. From the thermal desorption spectroscopy (TDS) measurement and density functional theory (DFT) calculations, we concluded that the adsorbate that is responsible for the change of the FET property is the Cl atom that is dissociated from the Cl2 molecule. The monotonic shift of Vth with the coverage suggests that the MoS2 device sensor has a good sensitivity to detect 10–3 monolayers (ML) of adsorption corresponding to the ppb level sensor with an activation time of 1 s.

Thermal desorption spectroscopy evaluation of hydrogen-induced damage and deformation-induced defects

ABSTRACT Thermal desorption spectroscopy (TDS) was performed on ultra-low carbon (ULC) steel with various degrees of hydrogen-induced damage and deformation-induced defects. First, the extent to which hydrogen-induced damage manifests itself in TDS measurements was evaluated. Application of multiple test conditions on cold deformed ULC steel with and without the presence of hydrogen-induced damage showed that such damage did not appear as a hydrogen signal on the TDS spectra. Second, interesting features observed on the TDS spectra of cold deformed ULC steel were further investigated by assessing the TDS spectra of recrystallised and annealed ULC steel. As such, the four peaks in the TDS spectra were linked to microstructural features: interstitial lattice positions, grain boundaries, dislocations and microvoids.