The degree of extraction of silver and copper from solutions of their salts by atomic hydrogen in Pd was studied, as well as the conditions for their most complete extraction. The Ag+ concentration was 12.67 and 0.635 g/L, and that of Cu2+ was 1.145 and 1.527 g/L. The residence time of Pd in solution was 1 h. Electrochemical hydrogenation of Pd was carried out in 1 M NaOH solution at 30 mA/cm2 for 9 min until completely saturated with hydrogen, at which H : Pd was 0.73. It has been established that the PdH system has the ability to efficiently extract silver (and copper) with 100
The process was studied of spontaneous gas evolution (cavitation) at the interface with a Pd electrode saturated cathodically with hydrogen in 1 M NaOH and, then, immersed in one of the following liquids: distilled water (aged for more than 20 days after distillation), the same water after purging with argon, ethyl alcohol, ethyl alcohol after purging with argon, 1 M NaOH, and 3 M NaCl, as well as in the following technical fluids: glycerin (99%), glycerin (50% solution in water), ZIPPO gasoline, TC1 kerosene, and PMS-200 silicone oil brand used in diffusion vacuum pumps. Not only was the amount of gas released during cavitation in different liquids measured, but also the amount of remaining hydrogen in Pd. It is established that the intensity of cavitation is different in all cases. In aqueous solutions, alcohols, and silicone oil, intense "cold boiling " is observed, while the amount of hydrogen in Pd does not change. At the same time, cavitation gas is not released in gasoline and kerosene. In this case, the hydrogen content in Pd sharply decreases. It is likely that the process of hydrogenation of gasoline and kerosene proceeds at a higher rate than cavitation.
The kinetics of changes in the linear dimensions of flat Pd samples during electrochemical hydrogen uptake and subsequent electrochemical or thermal desorption has been studied. The amounts of heat released during thermal desorption of hydrogen from Pd at temperatures of 400 and 600°C in air and in vacuum are measured. The presence of irreversible changes in the crystal lattice of Pd after the hydrogen uptake–hydrogen desorption cycle is shown. Moreover, the nature of these changes depends on the method of desorption with complete removal of hydrogen from Pd. The length of the sample after electrochemical desorption increases compared to the initial length, and on the contrary, it decreases in the case of thermal desorption. The last claim is presumably associated with the pulsed heating of the Pd surface layers (up to their melting) during the thermal desorption of hydrogen from Pd and its subsequent reaction with atmospheric oxygen if the thermal desorption is carried out in the air atmosphere.
A decrease in the excess deformation volume (a kind of “imprint” of the system after the stay of hydrogen in Pd) with an increase in the amount of hydrogen introduced into Pd (starting from H : Pd = 0.25) and then removed electrochemically. In parallel, an increase in the electrical conductivity of electrochemically dihydrogenated palladium hydrides by 12% in comparison with the initial samples of pure palladium in a wide temperature range (75–300 K) was recorded. This means that some of the hydrogen in the Pd (about 5.3 × 10 15 atoms per sample) passed into a more compressed, highly conductive phase. In this case, an increase in electrical conductivity with respect to pure Pd can occur both due to the formation and propagation of highly conductive regions of palladium hydride and due to electron transfer (percolation, tunneling) between individual nanoclusters of quasi-metallic hydrogen, localized in the region of metal structural defects, namely, in vacancy clusters and inside the cores of edge dislocations, where the highest pressures in the lattice are achievable.
The paper reviews results obtained in the course of low energy nuclear reactions experimental study using the HELIS facility (LPI). The analysis of DD-reaction yields in deuterated crystalline structures at deuteron energies of 10–25 keV has shown a significant amplification effect. It was found that the exposure of deuterated targets both to 10–25 keV H+ and Ne+ ion beams and 20–30 keV X-ray radiation beams results in stimulation of DD-reaction yield. For CVD diamond and PdDx targets, it was shown that the magnitude of the neutron yield is affected by the orientation of the sample with respect to the deuteron beam. The possible explanation of the said effect may be attributed to the channeling of deuterium ions and neutron (DD reaction products) in textured targets. It was found that the heat release is much higher when D+ ion beams act upon the TiDx target than in case with H+ and Ne+ beams. The heat release depends upon the deuterium concentration in the target and the deuteron beam current density. “Additional peaks” were observed in the X-ray fluorescence spectra, but those are not related to any element and are seemingly associated with diffraction processes in deuterated palladium and CVD diamond.
The relationship between the amount of hydrogen electrochemically introduced to Pd and the volume and linear sizes of the formed PdH system, as well as the intensity of cavitation that arises after saturation of Pd with hydrogen, has been determined. The results of the study allows one to describe the mechanism of origin of cavitation on PdH in spite of the impossibility to determine the composition of atmosphere in bulk defects (microvoids, microcracks, and dislocations), which are formed upon hydrogenation of Pd. A Harvey–Knapp model has been employed, which describes well the origin of cavitation on nonwettable surfaces with fine cracks. The model is based on the hypothesis that presence of cavitation cores are present in water in the form of fine air bubbles.
The gas evolution process on fully hydrogenated Pd (H : Pd = 0.73) cathodes is studied in a 1 M solution of NaOH at ambient temperature. A phenomenon of spontaneous gas evolution on the surface of PdH after electrolysis and transfer of the sample into a burette with a 1 M solution of NaOH or distilled water is discovered. The volume of the gas that spontaneously evolved on the surface of PdH is 0.22–0.24 cm3/cm2 in a 1 M solution of NaOH and 0.40–0.43 cm3/cm2 in distilled water. It is proposed that the spontaneously evolving gas is not hydrogen from PdH, but results from the cavitation process.
The emission of X-ray quanta, neutrons, and charged particles from deuterated structures under X-ray irradiation is studied. Targets (deuterated chemical-vapor-deposited (CVD)-diamond, palladium, zirconium, and titanium) are irradiated with the use of an X-ray tube equipped with a polycapillary lens with an energy of up to 30 keV and an X-ray tube equipped with a collimator with an energy of up to 25 keV. Different types of detectors, such as a multichannel neutron detector based on He-3 counters, a CR-39 plastic track detector, and silicon surface barrier detectors, are used. The emission of neutrons with an energy of above 10 MeV and alpha particles with an energy range of 7–15 MeV is revealed. This result indicates the possibility of stimulating multiparticle fusion reactions between deuterium nuclei in solid deuterated structures. The analysis of X-ray fluorescence spectra demonstrate the existence of “additional” peaks, which cannot be identified by any characteristic X-ray fluorescence line. Their appearance cannot be associated with any known element or diffraction process. The nature of the origination of the “additional” peaks requires special study.
Measurements of emission from nuclear reaction products (neutrons and protons) have been carried out appearing in the deuterated structures of textured CVD diamond, palladium, titanium, and zirconium under irradiation with a beam of X rays using independent methods (neutron detector based on He-3 counters, Si surface-barrier semiconductor detectors and CR-39 track detector). The possibility of enhancement of both DD reaction and multi-particle deuterium fusion by the beam of X rays with energy ranging 20–30 keV in solid deuterated targets has been established. Analysis of X-ray fluorescence spectra of the target bombarded by beams of ions has revealed “additional” peaks, the occurrence of which cannot be related to any of the known elements, and requires separate study.
Two independent methods based on a neutron detector with He-3 counters and a CR-39 track detector are used to measure neutron and proton emissions from the nuclear reaction in samples of deuterated structures of textured CVD (chemical vapor deposited) diamond, palladium, and zirconium irradiated with X-ray quantum beams. It is demonstrated that, in solid-state deuterated targets, the DD reaction can be stimulated by X-ray quanta with energies of 20−30 keV.
In this study, we present the results of studies of DD reactions in crystalline heterostructures at low energies using the ion accelerator HELIS. The results of measurements of the DD-reaction yields from the Pd/PdO:D-x and the Ti/TiO2:D-x heterostructures in the energy range of 10-25 keV are presented. The neutron and proton fluxes are measured using a neutron detector based on He-3 counters and a CR-39 plastic track detector. Comparisons with calculations show significant DD-reaction yield enhancement. It was first shown that the impact of the H+ and Ne+ ion beams in the energy range of 10-25 keV at currents of 0.01-0.1 mA on the deuterated heterostructure results in an appreciable DD-reaction yield stimulation. We also studied the neutron yield in DD reactions within a polycrystalline deuterium-saturated CVD diamond, during irradiation of its surface by a deuterium ion beam with energy of less than 30 keV. The measurements of the neutron flux in the beam direction are performed in dependence on the target angle, beta, with respect to the beam axis. A significant anisotropy in neutron yield is observed, it was higher by a factor of 3 at beta = 0 compared to that at beta = +/- 45 degrees. (C) 2016 ISCMNS. All rights reserved.
The data on the mechanism of electroless (catalytic) deposition of Co–Re–B coatings are obtained by determining the donor capacitance of dimethylamine borane (DMAB) (CH 3 ) 2 HN · BH 3 reductant and the oxidation level of its hydride hydrogen. From the results of the study of isotopic composition of evolved hydrogen, it is concluded that the oxidation level of DMAB hydride hydrogen depends on the catalytic activity of the alloy. The alloys containing up to 46 at % rhenium were produced by the electroless deposition.
The processes of electrodeposition of rhenium and its alloys with nickel from aqueous solutions are considered. The results of theoretical and experimental studies of the process of perrhenate ion reduction are analyzed: the data on the possible mechanisms of the cathodic process, participation of atomic hydrogen in it, potentials of transition of rhenium to different oxidation degrees. Codeposition of rhenium and nickel is discussed. The effect of complexation on the current efficiency of rhenium deposition is considered. Information of the sources of data discussed in this paper is provided.
The structure and properties of Fe–Mo alloys is studied. It is shown that the iron–molybdenum alloys formed in the electrolysis are highly hydrogenated, and the content of hydrogen in them increases with increasing atomic fraction of molybdenum in the cathodic deposit. The kinetics of hydrogen evolution reaction in the alkaline solutions on the obtained materials is studied.
The currentless deposition of Cu2+, Ag+, and other cations from solutions of their salts takes place on the surface of hydrogen-saturated palladium (Pd-H). It is hypothesized that this process occurs via a catalytic chemical mechanism. It is demonstrated that 80–90% of the copper deposits onto Pd-H from a CuSO4 solution in the first hour of their contact. The Pd-H system with a thin palladium coating can finely purify solutions from Cu2+ when the amount of hydrogen in Pd exceeds the amount of Cu2+ in the solution.
The gaseous products of the oxidation of hydride hydrogen of the dimethylamine borane (DMAB) (CH3)2NH · BH3 reducer used for depositing Ni-Re-B coatings and hydrolysis of DMAB on them were studied by mass spectrometry of the isotope composition of the gas. The oxidation level of hydride hydrogen of the DMAB reducer was found to depend on the catalytic activity of the Ni-Re-B alloy, on which heterogeneous hydrolysis takes place. For Ni-Re-B alloys with low rhenium concentrations (0–13 at %), the heterogeneous hydrolysis of DMAB proceeds with hydride hydrogen oxidation to the atomic state, as it does in the deposition of the Ni-B alloy. In contrast, at high rhenium concentrations (40–46 at %), the oxidation proceeds to the proton H+, leading to an antibatic dependence of the hydrolysis and alloy reduction rates. An analysis of the partial rates of the process and isotope composition of the evolved gas revealed two different mechanisms of the chemical-catalytic reduction of Ni-Re-B alloys at concentrations of potassium perrhenate of 0–4 and 4–16 mM in solution.
The yield of the products of nuclear reactions from deuterated palladium and titanium irradiated by an electron beam and X rays has been studied. Charged particles have been detected by CR-39 track detectors, which are not sensitive to electronic noise, electrons, and X-ray photons. To identify the type of particles and to estimate their energy, three detectors covered by aluminum and copper foils of various thicknesses have been used. It has been established with reliable statistics that 30-keV electrons and X rays initiate the synthesis of deuterons in the Pd/PdO:D x and Ti/TiO 2 :D x systems with the yield of 3-MeV protons.
The composition and structure of the electrochemically synthesized Ni-W-H alloys were studied. The co-deposition of nickel with tungsten mainly led to nickel solid solutions, and nanocrystalline alloys formed if the hydrogen content in them was at least 3 at %. The deposits included ∼2% of all evoluted hydrogen. The lattice constant of the solid solutions was 1.7–1.9% higher than the that of nickel. The tungsten solid solution phase found in a number of alloys was not nanocrystalline. The hardness of the alloys was several times higher than that of pure nickel.