Authors: E.N. Popova, I.L. Deryagina, E.P. Romanov, E.A. Dergunova, A.E. Vorobyova, S.M. Balaev
Abstract: The structure of Nb3Sn-based, bronze-processed Ti-doped multifilamentary superconducting wires has been studied by TEM and SEM after the first (5750C,100 h) and the second (6500C,100 h) stage of the diffusion annealing. The Nb3Sn layers formation in all the composites proceeds by one and the same mechanism and starts with nucleation of particles and very fine grains of this phase in Nb filaments where Sn diffuses from the bronze matrix. Ti, inserted both in the bronze matrix, or Nb filaments, diffuses into the growing superconducting layer and promotes its more active formation. At the first stage of annealing (5750C, 100 h) Nb3Sn grains have an average size of 40 nm, and at the second stage (6500C, 100 h) they increase by a factor of 1.5 and the grain size distribution gets wider. After the two-stage annealing the amount of the residual niobium is small, and some Nb filaments, especially in doped composites, almost completely transform into Nb3Sn. In the Nb3Sn layers of a zone of columnar grains is adjacent to the residual Nb.
69
Authors: Omar Abbes, Feng Xu, Alain Portavoce, Khalid Hoummada, Vinh Le Thanh, Christophe Girardeaux
Abstract: In recent years, spintronics whose principle is based on controlling the spin of electrons in semiconductor layers is presented as a complementary or even an alternative solution for production of logic devices in microelectronics. It relies on the fact that electric current in a magnetic layer can be spin polarized. Manufacture of such components is based on the use of materials or heterostructures whose electronic properties depend on their magnetic state. The magnetic Mn-Ge system is interesting because of its possible development at high Curie temperature and its integration on Si substrate. Among all of the Mn-Ge phase compounds of the diagram, Mn5Ge3 seems the most interesting one for spintronics applications: it is a stable and ferromagnetic phase at room temperature. In this paper, we present first results of the study, by Reflection High Energy Electron Diffraction (RHEED), X-ray diffraction (XRD) and Atomic Force Microscopy (AFM), of the sequence of formation of the MnxGey phases in the case of reaction of a nanometric-thick Mn film (200nm) deposited by MBE on Ge (111).
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Authors: Masanori Kajihara, Shingo Nakamura
Abstract: The reactive diffusion between Ti and a bronze was experimentally examined using sandwich diffusion couples consisting of Ti and a Cu-9.3Sn-0.3Ti alloy. The diffusion couples were isothermally annealed at temperatures of T = 923-1023 K. During annealing, CuTi, (Cu, Sn)4Ti3 and (Sn, Cu)5Ti6 compounds are formed as layers at the interface in the diffusion couple. The overall growth of the compound layers is controlled by volume diffusion at T = 1023 K but by boundary and volume diffusion at T = 923-973 K. Hence, the interface reaction is not the bottleneck for the growth of the compound layers under the present experimental conditions.
470
Authors: Jaromír Drápala, Alena Struhařová, Daniel Petlák, Vlastimil Vodárek, Petr Kubíček
Abstract: Problems of reactive diffusion at the solid phase and melt contact were studied theoretically and experimentally. The main intention was to calculate the time course of the solid phase dissolving in the case of cylindrical dissolving. These calculations were carried out on the assumption for the rate constant of dissolving K = const. In our work we give heed especially to the dominating process, which is the solid metal A dissolved in the melt B. During the dissolving the melt B saturates with the metal A and the process is influenced by convections which are characteristic for the given experimental configuration. A theoretical description of the kinetics of the solid phase dissolving in the melt will be presented for the case of cylindrical dissolving. The aim is to derive a relation for the interface boundary movement c(t) in dependence on time and a time course of growth of the element A concentration in the melt B. There are problems with accurate determination of the interface boundary movement after certain heating times of specimens, when it is observed experimentally, since intermetallic phases create in the original A metal at both the diffusion and cooling and some phases segregate at the solidifying melt cooling. The main intention was an experimental study of the copper dissolving in the tin melt. Experiments aimed to the determination of the Cu wires (diameters from 0.5 to 3.5 mm) dissolution in the solder melt were carried out at various selected temperatures and times. Rapid growth of phases in the metal A and determination of the thickness of layers with these phases pose considerable time demands to X-ray micro-analyses (WDX, EDX) of specimens after their long-time heating.
387
Authors: E.N. Popova, E.P. Romanov, I.L. Deryagina, S.V. Sudareva, E.A. Dergunova, A.E. Vorobyova, S.M. Balaev
Abstract: Bronze-processed Nb3Sn-based multifilamentary composites with external diameter of 0.8 and 0.5 mm and coupled Nb filaments have been studied by transmission (TEM) and scanning (SEM) electron microscopy. After the two-staged annealing, 575°С, 150 h + 650°С, 200 h, commonly used for ITER conductors, a nanocrystalline layer of superconducting Nb3Sn compound is formed in every Nb filament as a result of solid-state reactive diffusion of Sn from the bronze matrix. It is demonstrated that in the wires of smaller external diameter the Nb filaments transformation into the Nb3Sn compound is more pronounced, that is the amount of the residual Nb is smaller. Besides, the nanocrystalline structure of the Nb3Sn diffusion layers is more perfect in 0.5 mm diameter wires, namely, the Nb3Sn grains are finer (their average size being 60 nm compared to 70 nm in 0.8 mm diameter wires) and are more uniform in sizes (the root mean square deviation of grain size distribution is correspondingly 15 and 17 nm).
289
Authors: Jaromír Drápala, Pavel Jopek, Daniel Petlák, Petr Harcuba, Petr Kubíček
Abstract: Problems of reactive diffusion at a solid phase - melt contact were studied theoretically. The main intention was to calculate the time course of the solid phase dissolving in the case of planar dissolving. In our work we give heed especially to the dominating process, which is the solid metal A dissolving in solder melt B. During the dissolving, melt B saturates with metal A, and the process is influenced by convections which are characteristic for a given experimental configuration. A theoretical description of the kinetics of solid phase dissolving in the melt will be presented for the case of planar dissolving. The aim is to derive a relation for the interphase boundary movement (t) depending on time and a time course of growth of the element A concentration in the melt B. There are difficulties in accurate determination of the interphase boundary movement after heating of specimens for certain time intervals. It should be performed experimentally, since intermetallic phases are formed in original metal A both via diffusion and upon cooling and some phases segregate upon cooling of the solidifying melt. The main intention was to study experimentally the copper dissolving in melts of various solder alloys and the related reactive diffusion. We used pure Sn and Sn-Cu, Sn-Ag-Cu, Sn-Sb, Sn-Zn alloys as solder materials. Experiments aimed at the study of a Cu plate dissolving in the solder melt were carried out at various selected temperatures and times. The problems of reactive diffusion were studied both theoretically and experimentally and the problems that have to be solved preferably were emphasized. Concentration profiles of elements and thickness of layers of phases can be determined with SEM and X-ray microanalyses (WDX, EDX) of specimens after their diffusion heating.
127
Authors: S. Korichi, A. Bensmaili, Mourad Keddam
Abstract: The effect of compaction of bentonite on the diffusion behavior of uranium was studied for the safety assessment of radioactive waste (storage and disposal practices). Since the permeability of the compacted clay is very low, the main mechanism for radionuclide transport is governed by the diffusion phenomenon. The diffusion process of uranium in compacted clay as a porous medium has been modeled by Fick's second law taking into account the effect of sorption and considering the non-steady state. The diffusion coefficients and profiles concentration values were calculated by a computational method using a numerical program based on the Newton-Raphson algorithm. In this simulation, the experimental values were used to determine the uranium concentration profiles versus depth of the clay pellet. It was concluded that the dry density of the compacted clay and the aqueous solution properties (pH and ionic strength of background electrolyte) played an important role in the uranium transport through compacted clays.
275
Authors: E.N. Popova, Vladimir V. Popov, E.P. Romanov, S.V. Sudareva, L.V. Elohina, A.E. Vorobyova, A.K. Shikov, V.I. Pantsyrny, S.V. Sudiev
Abstract: Multifilamentary Nb3Sn-based superconducting composites manufactured by an internal-tin method have been studied by transmission (TEM) and scanning (SEM) electron microscopy. The main goal of this study is to reveal the effect of diffusion annealing regimes as well as the external diameter of the wires on the structure of nanocrystalline Nb3Sn layers (average grain size, grain size distribution, layer thickness, amount of Sn, etc.). It is demonstrated that multistep diffusion annealing results in quite a complete transformation of Nb filaments into Nb3Sn though some amount of the residual Nb remains in the filaments center. With an external diameter decrease the superconducting layers structure has been found to refine and get somewhat more uniform. An additional high-temperature annealing results in marked growth of Nb3Sn grain sizes and their scattering in sizes, which may negatively affect the current-carrying capacity of a wire.
126
Authors: Jaromír Drápala, Petr Kubíček
Abstract: In this work we give heed especially to the dominating process which is the solid metal A dissolving in the melt B. During the dissolving, the melt B saturates with the metal A and the process is influenced by convections which are characteristic for the given experimental configuration. A theoretical description of the kinetics of the solid phase dissolving in melt will be presented for the case of planar and cylindrical dissolving. The aim is to derive a relation for the interface boundary (t) movement in dependence on time and a time course of growth of the element A concentration in the melt B. There are problems with an accurate determination of the interface boundary movement after certain heating times of specimens, when it is observed experimentally, since intermetallic phases create in the original A metal at both the diffusion and cooling and some phases segregate at the solidifying melt cooling. The rate constant is a fundamental parameter characterizing the dissolving rate at a certain configuration. We present a theoretical description of dissolving of a long metallic cylinder submerged into a melt column and relations for the rate constant determination from the time of the whole metallic cylinder dissolution are derived. In our experiments were performed in which Cu was dissolving in the Sn melt for a Cu cylinder (wire) diameters 0.8÷2.5 mm and the rate constant K (T = 350°C) was determined. Relationships between the solid phase dissolving rate, i.e. the solid phase interface boundary movement (t) in the melt and rates of growth of intermetallic phases in the metal A will be observed. This procedure enables to create surface and subsurface layers of regulated thickness in metallic materials by means of reactive diffusion.
8
Authors: Akio Nishimoto, Katsuya Akamatsu
Abstract: The intermetallic compound Nb3Al is widely investigated because of its high temperature strength, superior superconductivity and relatively small density. As Nb3Al has an extremely high melting point and lack of deformability, it is impossible to prepare it by using the conventional metallurgy. In this study, a Nb-Al intermetallic compound was prepared by multi-layered roll-bonding of elemental Nb and Al foils. The process consisted of the accumulative roll-bonding (ARB) for making a laminated Nb/Al sheet and the subsequent heat treatment promoting a solid-phase reaction in the laminated Nb/Al sheet. Accumulated foils were roll-bonded at 573 K. The rolling reduction at 1 pass was ~50%, and the final rolling reduction at 4 passes was ~94%. A pulsed electric current sintering (PECS) process was used for the subsequent heat treatment. The microstructures produced at each processing stage were characterized by X-ray diffraction (XRD), optical microscopy and scanning electron microscopy (SEM) equipped with energy-dispersive X-ray spectroscopy (EDS). A homogeneous intermetallic compound of Nb3Al could be obtained after the subsequent heat treatment for 1.8 ks at 873 K and for 0.9 ks at 1673 K.
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