Electron Spectroscopy Research Articles

Synthesis, Crystal Structure, Hirshfeld Surface, Energy Frame Work and DFT Analysis of Ethyl-4-aminobenzoate Oxalate Monohydrate Salt

Using the single crystal X-ray diffraction method, the title molecule ethyl-4-aminobenzoate oxalate monohydrate has been synthesized, crystallized and characterized. The Hirshfeld surfaces computational approach was used to analyze the intermolecular interactions in the crystal structure. The aforementioned compound crystallizes in a monoclinic crystal system of space group P21/c with the following cell parameters: a = 15.475(3), b = 5.7117(9), c = 14.029(3), = 101.764(6)º, V = 1214.0(4) 3 and Z = 4. The molecules in the crystal structure are connected by the N1-H1C···O7, O5-H2···O3, O7-H1···O4 and C8-H8A···Cg type intermolecular interaction, where Cg is the centroid of the ring. For the title molecule, the inter contact O···H (48.4%) contributes more to the Hirshfeld surfaces. The proton transfer from oxalic acid’s phenolic group to ethyl-4-aminobenzoate’s amine group, which results in the creation of salt, is revealed by the crystal structure. The ground state of ethyl-4-aminobenzoate oxalate monohydrate was also studied theoretically using the density functional method (DFT/B3LYP) with a basis set of 6–311++G(d,p). Charge transfer happens within the molecule, as shown by the computed HOMO and LUMO energies, DOS and MESP, as well as by the optimized molecular structure, electronic structural analysis and UV spectrum analysis.

Origins and Importance of Intragranular Cracking in Layered Lithium Transition Metal Oxide Cathodes.

Li-ion batteries have a pivotal role in the transition toward electric transportation. Ni-rich layered transition metal oxide (LTMO) cathode materials promise high specific capacity and lower cost but exhibit faster degradation compared with lower Ni alternatives. Here, we employ high-resolution electron microscopy and spectroscopy techniques to investigate the nanoscale origins and impact on performance of intragranular cracking (within primary crystals) in Ni-rich LTMOs. We find that intragranular cracking is widespread in charged specimens early in cycle life but uncommon in discharged samples even after cycling. The distribution of intragranular cracking is highly inhomogeneous. We conclude that intragranular cracking is caused by local stresses that can have several independent sources: neighboring particle anisotropic expansion/contraction, Li- and TM-inhomogeneities at the primary and secondary particle levels, and interfacing of electrochemically active and inactive phases. Our results suggest that intragranular cracks can manifest at different points of life of the cathode and can potentially lead to capacity fade and impedance rise of LTMO cathodes through plane gliding and particle detachment that lead to exposure of additional surfaces to the electrolyte and loss of electrical contact.

Study on modified graphene oxide-based emulsion cleaner for oily sludge

Abstract Oily sludge is a complex system that is inevitably generated during the process of oil extracting and processing. It will cause serious environmental pollution and waste of resources if untreated sludge is discharged. In this paper, a composite emulsion cleaner based on modified graphite oxide and surfactants was developed for cleaning oily sludge. First, graphite oxide (GO) was functionally modified with butylamine, and its structures were verified by Fourier transform infrared spectroscopy (FTIR), X-ray electron spectroscopy (XPS), thermogravimetric analysis (TGA), and environmental scanning electron microscopy (SEM). Then, the oil-in-water composite emulsion cleaner was prepared by using butylamine modified graphite oxide and surfactants. The conditions for emulsion preparation and oil sludge cleaning were modelled and optimized by the response surface methodology. The obtained optimal formulations were: surfactant content was 2.17 ‰ with SDS/AEO-3 ratio of 9:1, GO-A4 content was 0.96 ‰, water-oil ratio was 5:5, and the oil removal rate was 97.45 %. The optimal cleaning conditions were: liquid-solid ratio of 3.2:1, cleaning time of 32 min, cleaning temperature of 28.7 °C, and oil removal rate of 99.02 %. The solid sediments were characterized by FTIR and SEM, which proved the feasibility of cleaning oily sludge with the emulsion.

Electrochemical Surface Nanostructuring of Ti47Cu38Fe2.5Zr7.5Sn2Si1Ag2 Metallic Glass for Improved Pitting Corrosion Resistance

Ti‐based bulk metallic glasses are envisioned for human implant applications. Yet, while their elevated Cu content is essential for a high glass‐forming ability, it poses biocompatibility issues, necessitating a reduction in near‐surface regions. To address this, surface treatments that simultaneously generate protective and bioactive states, based on nanostructured Ti and Zr‐oxide layers are proposed. An electrochemical pseudo‐dealloying process using the bulk glass‐forming Ti47Cu38Fe2.5Zr7.5Sn2Si1Ag2 alloy is defined. Melt‐spun ribbons are immersed in hot concentrated nitric acid solution, monitoring the anodic polarization behavior. From the current density transient measurements, together with surface studies (field‐emission scanning electron microscopy, transmission electron microscopy, and Auger electron spectroscopy), the surface reactions are described. This nanostructuring process is divided into three stages: passivation, Cu dissolution, and slow oxide growth, leading to homogenous nanoporous and ligament structures. By tuning the applied potential, the pore and ligament sizes, and thickness values are adjusted. According to X‐ray photoelectron spectroscopy, these nanoporous structures are Ti and Zr‐oxides rich in hydrous and nonhydrous states. In a simulated physiological solution, for those treated glassy alloy samples, complete suppression of chloride‐induced pitting corrosion in the anodic regime of water stability is achieved. This high corrosion resistance is similar to that of clinically used cp‐Ti.

A Novel Method for Preparation of Al–Ni Reactive Coatings by Incorporation of Ni Nanoparticles into an Al Matrix Fabricated by Electrodeposition in AlCl3:1‐Eethyl‐3‐Methylimidazolium Chloride (1.5:1) Ionic Liquid Containing Ni Nanoparticles

Al/Ni reactive coatings are fabricated via electrochemical deposition (ECD) at different applied voltages for reactive bonding application. :1‐ethyl‐3‐methylimidazolium chloride ([EMIm]Cl) (1.5:1) ionic liquid electrolyte is used as source of Al, whereas Ni is in the bath and incorporated into final coatings as nanoparticles (NPs). Scanning electron microscopy and Auger electron spectroscopy reveal a homogeneous Ni particle dispersion, as well as a high amount of particle incorporation into the Al matrix. A maximum of 37 wt% (22 at%) of Ni is detected via atomic absorption spectroscopy in the Al/Ni coating deposited at −0.1 V from an electrolyte containing 20 g L−1 of Ni NPs. Previous literature show that for bonding application an ideal concentration is around 50 at% of Ni and 50 at% Al. However, this is achieved using high vacuum, time‐consuming processes, and costly techniques like evaporation and magnetron sputtering. The ECD used in this work represents a more cost‐efficient approach which is not reported up to date for the aforementioned application. The reactivity of the coatings is confirmed by Differential scanning calorimetry. Herein, an exothermic reaction is detected upon the mixing of Al and Ni occurring at high temperatures.

Tuning grain boundary cation segregation with oxygen deficiency and atomic structure in a perovskite compositionally complex oxide thin film

Compositionally complex oxides (CCOs) are an emerging class of materials encompassing high entropy and entropy stabilized oxides. These promising advanced materials leverage tunable chemical bond structure, lattice distortion, and chemical disorder for unprecedented properties. Grain boundary (GB) and point defect segregation to GBs are relatively understudied in CCOs even though they can govern macroscopic material properties. For example, GB segregation can govern local chemical (dis)order and point defect distribution, playing a critical role in electrochemical reaction kinetics, and charge and mass transport in solid electrolytes. However, compared with conventional oxides, GBs in multi-cation CCO systems are expected to exhibit more complex segregation phenomena and, thus, prove more difficult to tune through GB design strategies. Here, GB segregation was studied in a model perovskite CCO LaFe0.7Ni0.1Co0.1Cu0.05Pd0.05O3−x textured thin film by (sub-)atomic-resolution scanning transmission electron microscopy imaging and spectroscopy. It is found that GB segregation is correlated with cation reducibility—predicted by an Ellingham diagram—as Pd and Cu segregate to GBs rich in oxygen vacancies (VO··). Furthermore, Pd and Cu segregation is highly sensitive to the concentration and spatial distribution of VO·· along the GB plane, as well as fluctuations in atomic structure and elastic strain induced by GB local disorder, such as dislocations. This work offers a perspective of controlling segregation concentration of CCO cations to GBs by tuning reducibility of CCO cations and oxygen deficiency, which is expected to guide GB design in CCOs.

Synthesis, characterization and column adsorption properties of gum ghatti and water hyacianth derived cellulose grafted poly(vinyl sulfonic acid-co-acrylamide) composites

Vinylsulfonic acid (VSA), acrylamide (AM) and N, N methylene bis acrylamide(MBA) were copolymerized by radical polymerization in the presence of gum ghatti (GG) and treated water hyacianth (WH) in water. Several composite copolymers were prepared by varying the i) AM: VSA molar ratios ii) wt% of GG and iii) wt% of treated WH based on a Box-Behnken Design(BBD) of a response surface methodology (RSM) model with three input variables and the batch adsorption capacity (mg/g) of 100 mg/L Cd (II) from water as response. The composite polymer was characterized by Fourier transform Infrared spectroscopy (FTIR), X-ray diffraction (XRD), thermogravimetric analysis(TGA), X- ray photo electron spectroscopy (XPS), compressive strength, pH reversibility, pH at point zero charge (pHPZC), Brunauer-Emmett-Teller (BET) surface area and scanning electron microscopy (SEM). The network parameters of the composites were determined. The copolymer composite prepared with AM: VSA of 5:1 containing 10 wt% GG and 4 wt% treated WH showed an optimum batch adsorption capacity of 399.15 mg/g Cd (II) from water containing 100 mg/L Cd (II). The same composite showed an adsorption capacity of 170.1 mg/g and a removal% of 31.5 at a feed concentration/feed flow rate/bed height of 150 mgL−1/30mLmin−1/30 mm in a fixed bed column.

Development of fluorosilicon bivalve isocyanate microcapsules for multifunctional coatings with excellent self-repairing properties, enhanced hydrophobicity, and corrosion protection properties

This study first self-made TMP-IPDI tetramer, and then prepared a fluorine-modified silicon dioxide double shell isocyanate type self-healing microcapsule (CBS-X/TMP-IPDI@PU@F-SiO2) using TMP-IPDI tetramer, fluorescent agent 4,4-bis (2-disulfonic acid sodium styrene) biphenyl (CBS-X) as the core material, polyurethane (PU) as the single shell, and fluorine modified silicon dioxide (F-SiO2) as the double shell using interfacial polymerisation method. Then, it was added to waterborne polyurethane (WPU) to prepare self-healing coatings and coatings. The chemical structure, microstructure, self-healing self detection, and mechanical properties of TMP-IPDI, CBS-X/TMP-IPDI@PU@F-SiO2, and composite coatings were characterized by infrared spectroscopy (FTIR), proton nuclear magnetic resonance (1H NMR), scanning electron microscopy (SEM), particle size analysis (PSA), X-ray electron spectroscopy (XPS) analysis, contact angle testing, tensile testing, electrochemical impedance testing, and Ultraviolet photograph. The results showed that the TMP-IPDI tetramer was successfully prepared. The average particle size of CBS-X/TMP-IPDI@PU@F-SiO2 prepared is 29 μm. The contact angle, tensile strength, low-frequency impedance and Nyquist curve radius of the repaired spots increased with the increase of the amount of CBS-X/TMP-IPDI@PU@F-SiO2 in WPUs; the increasing trend slowed down when the amount of CBS-X/TMP-IPDI@PU@F-SiO2 was >5 %. When the CBS-X/TMP-IPDI@PU@F-SiO2 dosage is 5 %, the WPU coating has good self-repair and self-detection performance. The stress before and after repair were 12.89 MPa and 20.11 MPa, respectively, with a repair rate of 80.3 %. The contact angle at the repair site can reach 100.8°, and the coating has good corrosion resistance. The microcapsules prepared based on fluorine-modified silica (F-SiO2) as the wall material have good self-healing performance for WPU coatings, achieving secondary protection of the repaired material.

Failure analysis of heavy ion-irradiated silicon carbide junction barrier Schottky diodes

An analysis of damage, including single event burnout (SEB) and single event leakage current (SELC) caused by heavy ion irradiation in silicon carbide (SiC) junction barrier Schottky diodes (JBSDs), was performed using Auger electron spectroscopy (AES), emission microscope (EMMI), focused ion beam (FIB), transmission electron microscopy (TEM) and other methods. The damage of SEB extending from the Schottky contact through the epitaxial layer to the SiC substrate was observed. The damage causing SELC was related to the micro-burnout of the Schottky contact. It was concluded that the damage of Schottky contact was induced by incident high-energy particles under a large electric field, forming a leakage current path, resulting in SEB and SELC in the SiC device.

Chemical bond reorganization in intramolecular proton transfer revealed by ultrafast X-ray photoelectron spectroscopy

Time-resolved X-ray photoelectron spectroscopy (TR-XPS) is used in a simulation study to monitor the excited state intramolecular proton transfer between oxygen and nitrogen atoms in 2-(iminomethyl)phenol. Real-time monitoring of the chemical bond breaking and forming processes is obtained through the time evolution of excited-state chemical shifts. By employing individual atomic probes of the proton donor and acceptor atoms, we predict distinct signals with opposite chemical shifts of the donor and acceptor groups during proton transfer. Details of the ultrafast bond breaking and forming dynamics are revealed by extending the classical electron spectroscopy chemical analysis to real time. Through a comparison with simulated time-resolved photoelectron spectroscopy at the valence level, the distinct advantage of TR-XPS is demonstrated thanks to its atom specificity.

Effects of Spectrum Loading and break in period using molybdenum disulphide (MoS2) and zinc dialkyl dithiophosphate (ZDDP) as EP additives in lithium based grease

PurposeThe purpose of variable loading conditions (392 N-785N-392N-785N) with break-in period were used to study interactions between zinc dialkyl dithiophosphate (ZDDP) 0.1 P% (phosphorus) and fine-grade molybdenum disulfide (MoS2) 3%, in different mixtures of NLGI 2 lithium stearate grease. Four-ball wear tests were used to evaluate the tribological properties of different grease mixtures such as coefficient of friction and wear. ASTM 2266 as reported by earlier studies is useful, but it is not representative of real-life applications where variable loads and speeds and different break-in periods play a role and could change the results and the nature of tribofilms.Design/methodology/approachIn this study, chemical and mechanical properties of tribofilms were examined. Moreover, design of experiment was used to examine the data and shorten experimentation time. Research described here is investigating variable loading conditions for real-life applications by using a break-in period of 2 min at the start to minimize asperities and establish a clean surface. Design expert (DOE) analyzes responses to reveal those variables that are single factor and those that are multifactor whether synergistically or antagonistically.FindingsThe results indicated that spectrum loading with break-in period showed reduction in wear when tested in greases with ZDDP/MoS2 combinations. Ramping up or down the load every 7.5 min for a rotational speed of 1,200 rpm and a total of 36,000 revolutions or 30-min time slowed the wear properties of lithium-based grease under different MoS2 and ZDDP concentrations. Experiments indicated that wear was largely dependent on the loading condition and ZDDP additives during specific break-in period at 1,200 rotational speed. It is believed that MoS2 greases perform better under spectrum loading and under constant loading when mixed with ZDDP phosphorus.Originality/valueThis research indicates that there is a synergistic interaction between ZDDP, MoS2 and variable loading especially when a break-in period is applied. The results indicated that wear was largely dependent on the specific speed used with spectrum loading as presented in the energy dispersive spectroscopy and the Auger electron spectroscopy analysis, and thus a 3% MoS2 grease with ZDDP (phosphorus: 0.1 Wt.%) are needed to improve the wear resistance and improve the friction characteristics.Peer reviewThe peer review history for this article is available at: https://publons.com/publon/10.1108/ILT-01-2024-0016/

COeCO: A new [formula omitted]-delayed conversion-electron spectroscopy setup for low-energy ISOL beams at the ALTO facility in Orsay

A new β-decay station, COnversion electrons Chasing at Orsay (COeCO), has been developed at ALTO to perform conversion electron spectroscopy studies of neutron-rich nuclei produced by photo-fission of a uranium carbide target. It is based on the collection of a low-energy ISOL beam on a mylar tape, and the transportation of the electrons emitted by the produced radioactive source through a magnetic field induced by two copper coils, towards a cooled Si(Li) detector. In this article, a detailed description of the new decay station and its components is given. The magnetic field induced by the coils was measured and compared to simulations performed with the COMSOL® software. The efficiency of the detection setup was estimated using a 207Bi and a 152Eu source as an off-line commissioning. Finally, the results obtained with a 96Rb radioactive beam for the on-line commissioning are presented.

The Use of Sargassum spp. Ashes Like a Raw Material for Mortar Production: Composite Performance and Environmental Outlook.

The accumulation of brown algae from the genus Sargassum has been increasing over the years in coastal regions of the Caribbean, Africa, Brazil, and Mexico. This causes harmful effects to the ecosystem, human health, the economy, and the climate due to gas emissions from its decomposition process. There is the possibility of this biomass being reused in civil construction, and some studies have been carried out on its application to common Portland cement mortar. As such, the objective of this study is to evaluate the potential of sargassum ash as a mineral addition to partially replace fine aggregates in Portland cement mortar. Characterization of the raw materials was carried out through X-ray fluorescence spectroscopy, loss on ignition, particle size distribution, Brunauer-Emmett-Teller (BET) analysis, real density, X-ray diffraction, scanning electron microscopy, and dispersion spectroscopy of electrons. The mortars were prepared by partially replacing the fine aggregate (sand) with sargassum ash at 0%, 5%, 10%, and 20%. Mortar performance was evaluated through water absorption, apparent porosity, apparent specific mass, and compressive strength 7, 28, and 63 days after curing. Lastly, a life cycle assessment was conducted in accordance with ISO standards 14040:2006 and 14044:2006. The results showed that replacing sand with sargassum ash increases water absorption and apparent porosity, and decreases the apparent specific mass and compressive strength as replacement increases. Nevertheless, the compressive strength results after 63 days for 5 and 10% replacement did not differ statistically from reference values. The life cycle assessment indicated that mortars with partial replacement of sand by sargassum ash show positive environmental impacts when compared to reference values for most categories, regardless of the scenario analyzed, especially for mortar with 10% replacement. As such, the use of sargassum ash at 10% does not alter the mortar's compressive strength values after 63 days, but does reduce its environmental impact. The application of this biomass in civil construction materials provides a destination for this algae, and that can be a solution to mitigate the social, environmental, and economic problems it has been causing.

Si(111) islands on β-phase Si(111)√3 × √3R30°-Bi

β-phase √3 × √3R30°-bismuth (Bi) on silicon (Si)(111)7 × 7 surface has been exploited as a template for growing Si films. Two-dimensional Si islands with √3 × √3 reconstruction, parallel to that of Si(111)√3 × √3R30°-Bi, have been resolved by means of scanning tunneling microscopy, grazing-incidence X-ray diffraction (XRD) and low electron energy diffraction. Auger electron spectroscopy and scanning tunneling spectroscopy gave interesting electronic features on two-dimensional Si islands, with the evidence of a reduced band gap to ~0.55 eV, related to the presence of the underneath Bi layer, and atomic structural properties typical of Si(111). These experimental findings fully confirm the recently reported calculation based on the first-principles density functional theory, on the prediction of Si(111) growth on top of β-phase √3 × √3R30°-Bi/Si(111)7 × 7 reconstruction, shedding new light on silicon structures.

Weakening surface hydrogen to enhance permeation in hydrogen selective membranes

Hydrogen selective metallic membranes made of palladium and its alloys are superior to membranes made of other metallic materials due to their unique surface properties. However, the prohibitive cost of Pd has prevented their widespread application. Although the basic mechanisms are known, the link between hydrogen at the surface and that in the bulk has been missing to explain the prominent position of Pd. To provide the missing link between surface and bulk, we measured the hydrogen concentration and depth distribution on the downstream side of a Pd membrane at realistic permeation conditions (temperature and pressure) using a membrane electron spectroscopy setup. We find hydrogen in the vicinity of the surface with intermediate stability. In general, hydrogen on the surface is more stable and thus more concentrated than in the bulk. Subsurface hydrogen with intermediate stability mitigates the difference between surface and bulk concentration and thereby facilitates overall hydrogen permeation. The observations link the results of UHV-compatible hydrogen adsorption experiments with observations made on hydrogen permeation in membranes under technical conditions. This link enables the application of the wealth of surface science based knowledge to the optimization of hydrogen permeable membrane materials.

Formation of thin Crsi2 films by the solid-phase ion-plasma method and their thermoelectric properties

ABSTRACT CrSi2 thin films with different thicknesses obtained on the Si(111) surface by magnetron sputtering method have been investigated using complex of electron spectroscopy and microscopy methods. The thin films’ composition, surface morphology, and cross-section, as well as the resistivity’s, Seebeck coefficient’s, and power factor’s temperature dependences have been studied for the first time. It has been established that, starting from a thickness of ~ 400 Å (deposition time ~ 60 sec), the SiO2/Si(111) surface is completely covered with an amorphous CrSi2 film. After heating the CrSi2/SiO2/Si(111) system at T ≈ 750 K, a homogeneous polycrystalline CrSi2/SiO2/Si(111) film is formed. It is shown that the resistivity ρ, the Seebeck coefficient S, and the power factor P of a CrSi2/SiO2/Si(111) film of different thicknesses (80 and 180 nm) change nonlinearly with increasing temperature. Their values for CrSi2 films of different thicknesses differ slightly from each other.

Spin-orbit coupling induced Van Hove singularity in proximity to a Lifshitz transition in Sr4Ru3O10

Van Hove singularities (VHss) in the vicinity of the Fermi energy often play a dramatic role in the physics of strongly correlated electron materials. The divergence of the density of states generated by VHss can trigger the emergence of phases such as superconductivity, ferromagnetism, metamagnetism, and density wave orders. A detailed understanding of the electronic structure of these VHss is therefore essential for an accurate description of such instabilities. Here, we study the low-energy electronic structure of the trilayer strontium ruthenate Sr4Ru3O10, identifying a rich hierarchy of VHss using angle-resolved photoemission spectroscopy and millikelvin scanning tunneling microscopy. Comparison of k-resolved electron spectroscopy and quasiparticle interference allows us to determine the structure of the VHss and demonstrate the crucial role of spin-orbit coupling in shaping them. We use this to develop a minimal model from which we identify a mechanism for driving a field-induced Lifshitz transition in ferromagnetic metals.

Development of High-Performance Polyindole/Silicon Carbide Nanocomposites for Optoelectrical and Sensing Applications.

In this study, silicon carbide (SiC)-reinforced polyindole (PIn) nanocomposites were prepared by a simple in situ polymerization method. The successful reinforcement of the nanofiller within the host matrix was characterized using different analytical techniques. The chemical bonding of SiC in the polymer was identified by the characteristic peak around 800 cm1 using Fourier transform infrared spectroscopy (FT-IR). The increment in intensity of the absorption and enhanced crystallinity of the samples upon the addition of nanofillers were analyzed using UV-vis spectroscopy and X-ray diffraction (XRD). The prepared specimens showed reduced optical bandgap energy (3.188 eV) and Urbach energy (2.315 meV) with an improved refractive index (2.348). The effect of nanoparticles on the surface morphology of the nanocomposites was studied using scanning electron microscopy (SEM), and a uniform dispersion of fillers in the matrix was found for PInSiC7. A high-resolution transmission electron microscopy (HR-TEM) revealed the shape and average particle size of the sample. X-ray electron spectroscopy (XPS) measurements confirmed the formation of the nanocomposite by exhibiting the presence of all elements in the corresponding spectra. The thermal stability and glass transition temperature of the nanocomposites were significantly improved with the addition of SiC. The temperature-dependent AC conductivity, dielectric parameters, complex impedance, and electrical modulus were also evaluated using an impedance analyzer. The increased electrical characteristics of the PInSiC7 sample can be attributed to the uniform spread and strong synergetic interaction of SiC with PIn. The results thus showcased the potential of the samples for use in optical and energy storage applications. This study was also extended to understand the ammonia sensing properties, which make it possible to design and develop gas sensors using the PInSiC nanocomposites.

Phase transformation sequence of amorphous nickel-molybdenum electrodeposit

In this paper, the amorphous Ni-Mo alloy with cauliflower-like morphology is successfully prepared by electrodeposition, and the effects of heat treatment on its morphology, element content and structure are studied. The results of scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS) and Auger electron spectroscopy (AES) show that, when the temperature is higher than 600 ℃, the fine grains gradually appear and then cover the entire surface of Ni-Mo alloy. The Ni-Mo alloy occurs simultaneously the segregation phenomenon and the Mo content increases on the surface. Differential scanning calorimetry (DSC) and X-ray diffraction (XRD) analysis illustrate that the Ni-Mo alloy gradually transfers from amorphous into crystalline structure, and the first phase MoNi4 and the second phase MoNi precipitate near 633℃ and 707℃ respectively. The apparent activation energy is 234.1 kJ/mol (ΔEa1) for the first phase crystallization and 819.9 kJ/mol (ΔEa2) for the second phase crystallization. The HER catalytic activity of Ni-Mo alloy increases first and then decreases with the increase of heat treatment temperature.

Deuterium permeation of low-activation vanadium alloys possible for reuse in a short time in fusion reactors

Low-activation vanadium (V) alloys are alternative to reduced-activation ferritic/martensitic steels for the blanket structural material. To make the reusage of the alloys possible in a short time, new-design concepts of V alloy have been suggested in National Institute for Fusion Science. In the present study, the deuterium permeation properties of the new-designed V alloys were investigated.The new-designed V-4Cr-4Ti alloy samples with high and low purity, named H44 and L44, respectively, were used. For comparison, the NIFS-HEAT-2 V alloy samples, named NH2 were also used.It was found from the permeation experiments that deuterium permeability coefficient of L44 was smaller than that of NH2, while the permeability coefficient of H44 was comparable with NH2. These results suggest the permeation coefficient of D of the new-designed V alloy was similar to those of the conventional V alloy, if Ti and O content was the same. Estimated activation energies of diffusion and permeation indicated that the permeation behaviors significantly depended on titanium oxides at the surface and in the bulk. Data obtained by a microscope with Auger electron spectroscopy indicated that the concentration and the composition of the oxide must change with air exposure during the maintenance and with hydrogen isotope exposure during the reactor operation. The obtained results suggest these changes of the concentration and the composition result in the change in the permeation characteristics of hydrogen isotopes.