WorldWideScience

Sample records for palladium silicides

  1. Palladium silicide - a new contact for semiconductor radiation detectors

    International Nuclear Information System (INIS)

    Totterdell, D.H.J.

    1981-11-01

    Silicide layers can be used as low resistance contacts in semiconductor devices. The formation of a metal rich palladium silicide Pd 2 Si is discussed. A palladium film 100A thick is deposited at 300 0 C and the resulting silicide layer used as an ohmic contact in an n + p silicon detector. This rugged contact has electrical characteristics comparable with existing evaporated gold contacts and enables the use of more reproducible bonding techniques. (author)

  2. Study of surface segregation of Si on palladium silicide using Auger electron spectroscopy

    International Nuclear Information System (INIS)

    Abhaya, S; Amarendra, G; Gopalan, Padma; Reddy, G L N; Saroja, S

    2004-01-01

    The transformation of Pd/Si to Pd 2 Si/Si is studied using Auger electron spectroscopy over a wide temperature range of 370-1020 K. The Pd film gets totally converted to Pd 2 Si upon annealing at 520 K, and beyond 570 K, Si starts segregating on the surface of silicide. It is found that the presence of surface oxygen influences the segregation of Si. The time evolution study of Si segregation reveals that segregation kinetics is very fast and the segregated Si concentration increases as the temperature is increased. Scanning electron microscopy measurements show that Pd 2 Si is formed in the form of islands, which grow as the annealing temperature is increased

  3. Palladium transport in SiC

    International Nuclear Information System (INIS)

    Olivier, E.J.; Neethling, J.H.

    2012-01-01

    Highlights: ► We investigate the reaction of Pd with SiC at typical HTGR operating temperatures. ► The high temperature mobility of palladium silicides within polycrystalline SiC was studied. ► Corrosion of SiC by Pd was seen in all cases. ► The preferential corrosion and penetration of Pd along grain boundaries in SiC was found. ► The penetration and transport of palladium silicides in SiC along grain boundaries was found. - Abstract: This paper reports on a transmission electron microscopy (TEM) and scanning electron microscopy (SEM) study of Pd corroded SiC. The reaction of Pd with different types of SiC at typical HTGR operating temperatures was examined. In addition the high temperature mobility of palladium silicides within polycrystalline SiC was investigated. The results indicated corrosion of the SiC by Pd in all cases studied. The corrosion leads to the formation of palladium silicides within the SiC, with the predominant phase found being Pd 2 Si. Evidence for the preferential corrosion and penetration of Pd along grain boundaries in polycrystalline SiC was found. The penetration and transport, without significant corrosion, of palladium silicides into polycrystalline SiC along grain boundaries was also observed. Implications of the findings with reference to the use of Tri Isotropic particles in HTGRs will be discussed.

  4. Palladium transport in SiC

    Energy Technology Data Exchange (ETDEWEB)

    Olivier, E.J., E-mail: jolivier@nmmu.ac.za [Centre for High Resolution Transmission Electron Microscopy, Nelson Mandela Metropolitan University, Port Elizabeth (South Africa); Neethling, J.H. [Centre for High Resolution Transmission Electron Microscopy, Nelson Mandela Metropolitan University, Port Elizabeth (South Africa)

    2012-03-15

    Highlights: Black-Right-Pointing-Pointer We investigate the reaction of Pd with SiC at typical HTGR operating temperatures. Black-Right-Pointing-Pointer The high temperature mobility of palladium silicides within polycrystalline SiC was studied. Black-Right-Pointing-Pointer Corrosion of SiC by Pd was seen in all cases. Black-Right-Pointing-Pointer The preferential corrosion and penetration of Pd along grain boundaries in SiC was found. Black-Right-Pointing-Pointer The penetration and transport of palladium silicides in SiC along grain boundaries was found. - Abstract: This paper reports on a transmission electron microscopy (TEM) and scanning electron microscopy (SEM) study of Pd corroded SiC. The reaction of Pd with different types of SiC at typical HTGR operating temperatures was examined. In addition the high temperature mobility of palladium silicides within polycrystalline SiC was investigated. The results indicated corrosion of the SiC by Pd in all cases studied. The corrosion leads to the formation of palladium silicides within the SiC, with the predominant phase found being Pd{sub 2}Si. Evidence for the preferential corrosion and penetration of Pd along grain boundaries in polycrystalline SiC was found. The penetration and transport, without significant corrosion, of palladium silicides into polycrystalline SiC along grain boundaries was also observed. Implications of the findings with reference to the use of Tri Isotropic particles in HTGRs will be discussed.

  5. Refractory silicides for integrated circuits

    International Nuclear Information System (INIS)

    Murarka, S.P.

    1980-01-01

    Transition metal silicides have, in the past, attracted attention because of their usefulness as high temperature materials and in integrated circuits as Schottky barrier and ohmic contacts. More recently, with the increasing silicon integrated circuits (SIC) packing density, the line widths get narrower and the sheet resistance contribution to the RC delay increases. The possibility of using low resistivity silicides, which can be formed directly on the polysilicon, makes these silicides highly attractive. The usefulness of a silicide metallization scheme for integrated circuits depends, not only on the desired low resistivity, but also on the ease with which the silicide can be formed and patterned and on the stability of the silicides throughout device processing and during actual device usage. In this paper, various properties and the formation techniques of the silicides have been reviewed. Correlations between the various properties and the metal or silicide electronic or crystallographic structure have been made to predict the more useful silicides for SIC applications. Special reference to the silicide resistivity, stress, and oxidizability during the formation and subsequent processing has been given. Various formation and etching techniques are discussed

  6. Surface morphology of erbium silicide

    International Nuclear Information System (INIS)

    Lau, S.S.; Pai, C.S.; Wu, C.S.; Kuech, T.F.; Liu, B.X.

    1982-01-01

    The surface of rare-earth silicides (Er, Tb, etc.), formed by the reaction of thin-film metal layers with a silicon substrate, is typically dominated by deep penetrating, regularly shaped pits. These pits may have a detrimental effect on the electronic performance of low Schottky barrier height diodes utilizing such silicides on n-type Si. This study suggests that contamination at the metal-Si or silicide-Si interface is the primary cause of surface pitting. Surface pits may be reduced in density or eliminated entirely through either the use of Si substrate surfaces prepared under ultrahigh vacuum conditions prior to metal deposition and silicide formation or by means of ion irradiation techniques. Silicide layers formed by these techniques possess an almost planar morphology

  7. High temperature structural silicides

    International Nuclear Information System (INIS)

    Petrovic, J.J.

    1997-01-01

    Structural silicides have important high temperature applications in oxidizing and aggressive environments. Most prominent are MoSi 2 -based materials, which are borderline ceramic-intermetallic compounds. MoSi 2 single crystals exhibit macroscopic compressive ductility at temperatures below room temperature in some orientations. Polycrystalline MoSi 2 possesses elevated temperature creep behavior which is highly sensitive to grain size. MoSi 2 -Si 3 N 4 composites show an important combination of oxidation resistance, creep resistance, and low temperature fracture toughness. Current potential applications of MoSi 2 -based materials include furnace heating elements, molten metal lances, industrial gas burners, aerospace turbine engine components, diesel engine glow plugs, and materials for glass processing

  8. Laccases as palladium oxidases.

    Science.gov (United States)

    Mekmouche, Yasmina; Schneider, Ludovic; Rousselot-Pailley, Pierre; Faure, Bruno; Simaan, A Jalila; Bochot, Constance; Réglier, Marius; Tron, Thierry

    2015-02-01

    The first example of a coupled catalytic system involving an enzyme and a palladium(ii) catalyst competent for the aerobic oxidation of alcohol in mild conditions is described. In the absence of dioxygen, the fungal laccase LAC3 is reduced by a palladium(0) species as evidenced by the UV/VIS and ESR spectra of the enzyme. During the oxidation of veratryl alcohol performed in water, at room temperature and atmospheric pressure, LAC3 regenerates the palladium catalyst, is reduced and catalyzes the four-electron reduction of dioxygen into water with no loss of enzyme activity. The association of a laccase with a water-soluble palladium complex results in a 7-fold increase in the catalytic efficiency of the complex. This is the first step in the design of a family of renewable palladium catalysts for aerobic oxidation.

  9. Room temperature ferromagnetic gadolinium silicide nanoparticles

    Science.gov (United States)

    Hadimani, Magundappa Ravi L.; Gupta, Shalabh; Harstad, Shane; Pecharsky, Vitalij; Jiles, David C.

    2018-03-06

    A particle usable as T1 and T2 contrast agents is provided. The particle is a gadolinium silicide (Gd5Si4) particle that is ferromagnetic at temperatures up to 290 K and is less than 2 .mu.m in diameter. An MRI contrast agent that includes a plurality of gadolinium silicide (Gd.sub.5Si.sub.4) particles that are less than 1 .mu.m in diameter is also provided. A method for creating gadolinium silicide (Gd5Si4) particles is also provided. The method includes the steps of providing a Gd5Si4 bulk alloy; grinding the Gd5Si4 bulk alloy into a powder; and milling the Gd5Si4 bulk alloy powder for a time of approximately 20 minutes or less.

  10. Reprocessing of LEU silicide fuel at Dounreay

    International Nuclear Information System (INIS)

    Cartwright, P.

    1996-01-01

    UKAEA have recently reprocessed two LEU silicide fuel elements in their MTR fuel reprocessing plant at Dounreay. The reprocessing was undertaken to demonstrate UKAEA's commitment to the world-wide research reactor communities future needs. Reprocessing of LEU silicide fuel is seen as a waste treatment process, resulting in the production of a liquid feed suitable for conditioning in a stable form of disposal. The uranium product from the reprocessing can be used as a blending feed with the HEU to produce LEU for use in the MTR cycle. (author)

  11. Palladium Nanoparticle Hydrogen Sensor

    Directory of Open Access Journals (Sweden)

    I. Pavlovsky

    2006-12-01

    Full Text Available An innovative hydrogen sensor based on palladium (Pd nanoparticle networks is described in the article. Made by Applied Nanotech Inc. sensor has a fast response time, in the range of seconds, which is increased at 80 °C due to higher hydrogen diffusion rates into the palladium lattice. The low detection limit of the sensor is 10 ppm of H2, and the high limit is 40,000 ppm. This is 100% of a lowest flammability level of hydrogen. This range of sensitivities complies with the requirements that one would expect for a reliable hydrogen sensor.

  12. Synthesis and design of silicide intermetallic materials

    Energy Technology Data Exchange (ETDEWEB)

    Petrovic, J.J.; Castro, R.G.; Butt, D.P. [Los Alamos National Lab., NM (United States)] [and others

    1997-04-01

    The overall objective of this program is to develop structural silicide-based materials with optimum combinations of elevated temperature strength/creep resistance, low temperature fracture toughness, and high temperature oxidation and corrosion resistance for applications of importance to the U.S. processing industry. A further objective is to develop silicide-based prototype industrial components. The ultimate aim of the program is to work with industry to transfer the structural silicide materials technology to the private sector in order to promote international competitiveness in the area of advanced high temperature materials and important applications in major energy-intensive U.S. processing industries. The program presently has a number of developing industrial connections, including a CRADA with Schuller International Inc. targeted at the area of MoSi{sub 2}-based high temperature materials and components for fiberglass melting and processing applications. The authors are also developing an interaction with the Institute of Gas Technology (IGT) to develop silicides for high temperature radiant gas burner applications, for the glass and other industries. Current experimental emphasis is on the development and characterization of MoSi{sub 2}-Si{sub 3}N{sub 4} and MoSi{sub 2}-SiC composites, the plasma spraying of MoSi{sub 2}-based materials, and the joining of MoSi{sub 2} materials to metals.

  13. Silicide formation by Ar/sup +/ ion bombardment of Pd/Si

    Energy Technology Data Exchange (ETDEWEB)

    Lee, R Y; Whang, C N; Kim, H K; Smith, R J

    1988-08-01

    Palladium films, 45 nm thick, evaporated on to Si(111) were irradiated to various doses with 78 keV Ar/sup +/ ions to promote silicide formation. Rutherford backscattering spectroscopy (RBS) shows that intermixing has occurred across the Pd/Si interface at room temperature. The mixing behaviour is increased with dose which coincides well with the theoretical model of cascade mixing. The absence of deep RBS tails for palladium and the small area of this for silicon spectra indicate that short-range mixing occurs. From the calculated damage profiles computed with TRIM code, the dominant diffusion species is found to be silicon atoms in the Pd/Si system. It is also found that the initial compound formed by Ar/sup +/ irradiation is Pd/sub 2/Si which increases with dose. At a dose of 1 x 10/sup 16/ Ar/sup +/ cm/sup -2/, a 48 nm thickness of Pd/sub 2/Si was formed by ion-beam mixing at room temperature.

  14. Irradiation behavior of miniature experimental uranium silicide fuel plates

    International Nuclear Information System (INIS)

    Hofman, G.L.; Neimark, L.A.; Mattas, R.F.

    1983-01-01

    Uranium silicides, because of their relatively high uranium density, were selected as candidate dispersion fuels for the higher fuel densities required in the Reduced Enrichment Research and Test Reactor (RERTR) Program. Irradiation experience with this type of fuel, however, was limited to relatively modest fission densities in the bulk from, on the order of 7 x 10 20 cm -3 , far short of the approximately 20 x 10 20 cm -3 goal established for the RERTR program. The purpose of the irradiation experiments on silicide fuels on the ORR, therefore, was to investigate the intrinsic irradiation behavior of uranium silicide as a dispersion fuel. Of particular interest was the interaction between the silicide particles and the aluminum matrix, the swelling behavior of the silicide particles, and the maximum volume fraction of silicide particles that could be contained in the aluminum matrix

  15. Solvent extraction studies of RERTR silicide fuels

    International Nuclear Information System (INIS)

    Gouge, Anthony P.

    1983-01-01

    Uranium silicide fuels, which are candidate RERTR fuel compositions, may require special considerations in solvent extraction reprocessing. Since Savannah River Plant may be reprocessing RERTR fuels as early as 1985, studies have been conducted at Savannah River Laboratory to demonstrate the solvent extraction behavior of this fuel. Results of solvent extraction studies with both unirradiated and irradiated fuel are presented along with the preliminary RERTR solvent extraction reprocessing flow sheet for Savannah River Plant. (author)

  16. MONTANA PALLADIUM RESEARCH INITIATIVE

    Energy Technology Data Exchange (ETDEWEB)

    Peters, John; McCloskey, Jay; Douglas, Trevor; Young, Mark; Snyder, Stuart; Gurney, Brian

    2012-05-09

    Project Objective: The overarching objective of the Montana Palladium Research Initiative is to perform scientific research on the properties and uses of palladium in the context of the U.S. Department of Energy's Hydrogen, Fuel Cells and Infrastructure Technologies Program. The purpose of the research will be to explore possible palladium as an alternative to platinum in hydrogen-economy applications. To achieve this objective, the Initiatives activities will focus on several cutting-edge research approaches across a range of disciplines, including metallurgy, biomimetics, instrumentation development, and systems analysis. Background: Platinum-group elements (PGEs) play significant roles in processing hydrogen, an element that shows high potential to address this need in the U.S. and the world for inexpensive, reliable, clean energy. Platinum, however, is a very expensive component of current and planned systems, so less-expensive alternatives that have similar physical properties are being sought. To this end, several tasks have been defined under the rubric of the Montana Palladium Research Iniative. This broad swath of activities will allow progress on several fronts. The membrane-related activities of Task 1 employs state-of-the-art and leading-edge technologies to develop new, ceramic-substrate metallic membranes for the production of high-purity hydrogen, and develop techniques for the production of thin, defect-free platinum group element catalytic membranes for energy production and pollution control. The biomimetic work in Task 2 explores the use of substrate-attached hydrogen-producing enzymes and the encapsulation of palladium in virion-based protein coats to determine their utility for distributed hydrogen production. Task 3 work involves developing laser-induced breakdown spectroscopy (LIBS) as a real-time, in situ diagnostic technique to characterize PGEs nanoparticles for process monitoring and control. The systems engineering work in task 4

  17. Uranium silicide activities at Babcock and Wilcox

    International Nuclear Information System (INIS)

    Noel, W.W.; Freim, J.B.

    1983-01-01

    Babcock and Wilcox, Naval Nuclear Fuel Division (NNFD) in conjunction with Argonne National Laboratory (ANL) is actively involved in the Reduced Enrichment Research Test Reactor (RERTR) Program to produce low enriched fuel elements for research reactors. B and W and ANL have undertaken a joint effort in which NNFD will fabricate two low enriched uranium (LEU), Oak Ridge Reactor (ORR) elements with uranium silicide fuel furnished by ANL. These elements are being fabricated for irradiation testing at Oak Ridge National Laboratory (ORNL). Concurrently with this program, NNFD is developing and implementing the uranium silicide and uranium aluminide fuel fabrication technology. NNFD is fabricating the uranium silicide ORR elements in a two-phase program, Development and Production. To summarize: 1. Full size fuel plates can be made with U 3 SiAl but the fabricator must prevent oxidation of the compact prior to hot roll bonding; 2. Providing the ANL U 3 Si x irradiation results are successful, NNFD plans to provide two ORR elements during February 1983; 3. NNFD is developing and implementing U 3 Si x and UAI x fuel fabrication technology to be operational in 1983; 4. NNFD can supply U 3 O 8 high enriched uranium (HEU) or low enriched uranium (LEU) research reactor elements; 5. NNFD is capable of providing high quality, cost competitive LEU or HEU research reactor elements to meet the needs of the customer

  18. Room temperature ferromagnetic gadolinium silicide nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Hadimani, Magundappa Ravi L.; Gupta, Shalabh; Harstad, Shane; Pecharsky, Vitalij; Jiles, David C.

    2018-03-06

    A particle usable as T1 and T2 contrast agents is provided. The particle is a gadolinium silicide (Gd5Si4) particle that is ferromagnetic at temperatures up to 290 K and is less than 2 .mu.m in diameter. An MRI contrast agent that includes a plurality of gadolinium silicide (Gd.sub.5Si.sub.4) particles that are less than 1 .mu.m in diameter is also provided. A method for creating gadolinium silicide (Gd5Si4) particles is also provided. The method includes the steps of providing a Gd5Si4 bulk alloy; grinding the Gd5Si4 bulk alloy into a powder; and milling the Gd5Si4 bulk alloy powder for a time of approximately 20 minutes or less.

  19. Palladium nanoparticle anchored polyphosphazene nanotubes ...

    Indian Academy of Sciences (India)

    607–610. c Indian Academy of Sciences. Palladium ... 2Department of Chemistry, APA College of Arts and Culture, Palani, Tamil Nadu 624 601, India. 3Department of .... K Dinakaran acknowledges the financial support from. Department of ...

  20. Sensitization to palladium in Europe

    DEFF Research Database (Denmark)

    Muris, Joris; Goossens, An; Gonçalo, Margarida

    2015-01-01

    BACKGROUND: Recently, sodium tetrachloropalladate (Na2 PdCl4 ) was found to be a more sensitive palladium patch test allergen than palladium dichloride (PdCl2 ). OBJECTIVES: To determine the optimal test concentration of Na2 PdCl4 , to evaluate the prevalence of palladium sensitization with Na2 P...... patch test concentration. Sensitization to palladium is almost as prevalent as sensitization to nickel. The sex distribution is different between nickel-sensitized and palladium-sensitized patients, suggesting different sources of exposure.......Cl4 and PdCl2 , and to compare the results with nickel sensitization in a European multicentre study. MATERIALS AND METHODS: In addition to the European or national baseline series including NiSO4 ·6H2 0 5% pet., consecutive patients were tested with PdCl2 and Na2 PdCl4 2%, 3% and 4% pet. in eight...... European dermatology clinics. The age and sex distributions were also evaluated in patients sensitized to nickel and palladium. RESULTS: In total, 1651 patients were tested. Relative to 3% Na2 PdCl4 , 4% Na2 PdCl4 did not add any information. Two per cent Na2 PdCl4 resulted in more doubtful reactions...

  1. Molybdenum silicide based materials and their properties

    International Nuclear Information System (INIS)

    Yao, Z.; Stiglich, J.; Sudarshan, T.S.

    1999-01-01

    Molybdenum disilicide (MoSi 2 ) is a promising candidate material for high temperature structural applications. It is a high melting point (2030 C) material with excellent oxidation resistance and a moderate density (6.24 g/cm 3 ). However, low toughness at low temperatures and high creep rates at elevated temperatures have hindered its commercialization in structural applications. Much effort has been invested in MoSi 2 composites as alternatives to pure molybdenum disilicide for oxidizing and aggressive environments. Molybdenum disilicide-based heating elements have been used extensively in high-temperature furnaces. The low electrical resistance of silicides in combination with high thermal stability, electron-migration resistance, and excellent diffusion-barrier characteristics is important for microelectronic applications. Projected applications of MoSi 2 -based materials include turbine airfoils, combustion chamber components in oxidizing environments, missile nozzles, molten metal lances, industrial gas burners, diesel engine glow plugs, and materials for glass processing. On this paper, synthesis, fabrication, and properties of the monolithic and composite molybdenum silicides are reviewed

  2. Subsurface contributions in epitaxial rare-earth silicides

    Energy Technology Data Exchange (ETDEWEB)

    Luebben, Olaf; Shvets, Igor V. [Centre for Research on Adaptive Nanostructures and Nanodevices (CRANN), School of Physics, Trinity College, Dublin (Ireland); Cerda, Jorge I. [Instituto de Ciencia de Materiales de Madrid, ICMM-CSIC, Cantoblanco, Madrid (Spain); Chaika, Alexander N. [Institute of Solid State Physics, RAS, Chernogolovka (Russian Federation)

    2015-07-01

    Metallic thin films of heavy rare-earth silicides epitaxially grown on Si(111) substrates have been widely studied in recent years because of their appealing properties: unusually low values of the Schottky barrier height, an abrupt interface, and a small lattice mismatch. Previous studies also showed that these silicides present very similar atomic and electronic structures. Here, we examine one of these silicides (Gd{sub 3}Si{sub 5}) using scanning tunneling microscopy (STM) image simulations that go beyond the Tersoff-Hamann approach. These simulations strongly indicate an unusual STM depth sensitivity for this system.

  3. Low-cost method for fabricating palladium and palladium-alloy thin films on porous supports

    Science.gov (United States)

    Lee, Tae H; Park, Chan Young; Lu, Yunxiang; Dorris, Stephen E; Balachandran, Uthamalingham

    2013-11-19

    A process for forming a palladium or palladium alloy membrane on a ceramic surface by forming a pre-colloid mixture comprising a powder palladium source, carrier fluid, dispersant and a pore former and a binder. Ultrasonically agitating the precolloid mixture and applying to a substrate with an ultrasonic nozzle and heat curing the coating form a palladium-based membrane.

  4. Production of Mo-99 using low-enriched uranium silicide

    International Nuclear Information System (INIS)

    Hutter, J.C.; Srinivasan, B.; Vicek, M.; Vandegrift, G.F.

    1994-01-01

    Over the last several years, uranium silicide fuels have been under development as low-enriched uranium (LEU) targets for Mo-99. The use of LEU silicide is aimed at replacing the UAl x alloy in the highly-enriched uranium dissolution process. A process to recover Mo-99 from low-enriched uranium silicide is being developed at Argonne National Laboratory. The uranium silicide is dissolved in alkaline hydrogen peroxide. Experiments performed to determine the optimum dissolution procedure are discussed, and the results of dissolving a portion of a high-burnup (>40%) U 3 Si 2 miniplate are presented. Future work related to Mo-99 separation and waste disposal are also discussed

  5. Rare earth silicide nanowires on silicon surfaces

    International Nuclear Information System (INIS)

    Wanke, Martina

    2008-01-01

    The growth, structure and electronic properties of rare earth silicide nanowires are investigated on planar and vicinal Si(001) und Si(111) surfaces with scanning tunneling microscopy (STM), low energy electron diffraction (LEED) and angle-resolved photoelectron spectroscopy (ARPES). On all surfaces investigated within this work hexagonal disilicides are grown epitaxially with a lattice mismatch of -2.55% up to +0.83% along the hexagonal a-axis. Along the hexagonal c-axis the lattice mismatch is essentially larger with 6.5%. On the Si(001)2 x 1 surface two types of nanowires are grown epitaxially. The socalled broad wires show a one-dimensional metallic valence band structure with states crossing the Fermi level. Along the nanowires two strongly dispersing states at the anti J point and a strongly dispersing state at the anti Γ point can be observed. Along the thin nanowires dispersing states could not be observed. Merely in the direction perpendicular to the wires an intensity variation could be observed, which corresponds to the observed spacial structure of the thin nanowires. The electronic properties of the broad erbium silicide nanowires are very similar to the broad dysprosium silicide nanowires. The electronic properties of the DySi 2 -monolayer and the Dy 3 Si 5 -multilayer on the Si(111) surface are investigated in comparison to the known ErSi 2 /Si(111) and Er 3 Si 5 /Si(111) system. The positions and the energetic locations of the observed band in the surface Brillouin zone will be confirmed for dysprosium. The shape of the electron pockets in the vector k parallel space is elliptical at the anti M points, while the hole pocket at the anti Γ point is showing a hexagonal symmetry. On the Si(557) surface the structural and electronic properties depend strongly on the different preparation conditions likewise, in particular on the rare earth coverage. At submonolayer coverage the thin nanowires grow in wide areas of the sample surface, which are oriented

  6. Far-infrared spectroscopy of thermally annealed tungsten silicide films

    International Nuclear Information System (INIS)

    Amiotti, M.; Borghesi, A.; Guizzetti, G.; Nava, F.; Santoro, G.

    1991-01-01

    The far-infrared transmittance spectrum of tungsten silicide has been observed for the first time. WSi 2 polycrystalline films were prepared by coevaporation and chemical-vapour deposition on silicon wafers, and subsequently thermally annealed at different temperatures. The observed structures are interpreted, on the basis of the symmetry properties of the crystal, such as infrared-active vibrational modes. Moreover, the marked lineshape dependence on annealing temperature enables this technique to analyse the formation of the solid silicide phases

  7. Determination of accurate metal silicide layer thickness by RBS

    International Nuclear Information System (INIS)

    Kirchhoff, J.F.; Baumann, S.M.; Evans, C.; Ward, I.; Coveney, P.

    1995-01-01

    Rutherford Backscattering Spectrometry (RBS) is a proven useful analytical tool for determining compositional information of a wide variety of materials. One of the most widely utilized applications of RBS is the study of the composition of metal silicides (MSi x ), also referred to as polycides. A key quantity obtained from an analysis of a metal silicide is the ratio of silicon to metal (Si/M). Although compositional information is very reliable in these applications, determination of metal silicide layer thickness by RBS techniques can differ from true layer thicknesses by more than 40%. The cause of these differences lies in how the densities utilized in the RBS analysis are calculated. The standard RBS analysis software packages calculate layer densities by assuming each element's bulk densities weighted by the fractional atomic presence. This calculation causes large thickness discrepancies in metal silicide thicknesses because most films form into crystal structures with distinct densities. Assuming a constant layer density for a full spectrum of Si/M values for metal silicide samples improves layer thickness determination but ignores the underlying physics of the films. We will present results of RBS determination of the thickness various metal silicide films with a range of Si/M values using a physically accurate model for the calculation of layer densities. The thicknesses are compared to scanning electron microscopy (SEM) cross-section micrographs. We have also developed supporting software that incorporates these calculations into routine analyses. (orig.)

  8. Recent Advances in Nb-silicide in-situ composites

    International Nuclear Information System (INIS)

    Bewlay, B.P.; Jackson, M.R.; Subramanian, P.R.; Briant, C.L.

    2001-01-01

    In-situ composites based on Nb silicides have great potential for future high-temperature applications. These Nb-silicide composites combine a ductile Nb-based matrix with high-strength silicides. With the appropriate combination of alloying elements, such as Ti, Hf, Cr, AI, it is possible to achieve a promising balance of fracture toughness, high-temperature creep performance, and oxidation resistance. This paper will describe the effect of volume fraction of silicide on microstructure, high-temperature creep performance, and oxidation resistance. The ratio of Nb:(W+Ti) is critical in determining both creep rate and oxidation performance. If this ratio goes below ∼1.5, the creep rate increases substantially. In more complex silicide-based systems, other intermetallics, such as laves phases and a boron-rich T-2 phase, are added for oxidation resistance. To understand the role of each phase on the creep resistance and oxidation performance of these composites, we determined the creep and oxidation behavior of the individual phases and composites at temperatures up to 1200 o C. These data allow quantification of the load-bearing capability of the individual phases in the Nb-silicide based in-situ composites. (author)

  9. Influence of impurities on silicide contact formation

    International Nuclear Information System (INIS)

    Kazdaev, Kh.R.; Meermanov, G.B.; Kazdaev, R.Kh.

    2002-01-01

    Research objectives of this work are to investigate the influence of light impurities implantation on peculiarities of the silicides formation in molybdenum monocrystal implanted by silicon, and in molybdenum films sputtered on silicon substrate at subsequent annealing. Implantation of the molybdenum samples was performed with silicon ions (90 keV, 5x10 17 cm -2 ). Phase identification was performed by X ray analysis with photographic method of registration. Analysis of the results has shown the formation of the molybdenum silicide Mo 3 Si at 900 deg. C. To find out the influence of impurities present in the atmosphere (C,N,O) on investigated processes we have applied combined implantation. At first, molybdenum was implanted with ions of the basic component (silicon) and then -- with impurities ions. Acceleration energies (40keV for C, 45 keV for N and 50 keV for O) were chosen to obtain the same distribution profiles for basic and impurities ions. Ion doses were 5x10 17 cm -2 for Si-ions and 5x10 16 cm -2 - for impurities. The most important results are reported here. The first, for all three kinds of impurities the decreased formation temperatures of the phase Mo 3 Si were observed; in the case of C and N it was ∼100 deg. and in the case of nitrogen - ∼200 deg. Further, simultaneously with the Mo 3 Si phase, the appearance of the rich-metal phase Mo 5 Si 3 was registered (not observed in the samples without additional implantation). In case of Mo/Si-structure, the implantation of the impurities (N,O) was performed to create the peak concentration (∼4at/%) located in the middle of the molybdenum film (∼ 150nm) deposited on silicon substrate. Investigation carried out on unimplanted samples showed the formation of the silicide molybdenum MoSi 2 , observed after annealing at temperatures 900/1000 deg. C, higher than values 500-600 deg. C reported in other works. It is discovered that electrical conductivity of Mo 5 Si 3 -films synthesized after impurities

  10. Phase transformations in Higher Manganese Silicides

    Energy Technology Data Exchange (ETDEWEB)

    Allam, A. [MADIREL, UMR 7246 CNRS - Universite Aix-Marseille, av Normandie-Niemen, 13397 Marseille Cedex 20 (France); IM2NP, UMR 7334 CNRS - Universite Aix-Marseille, av Normandie-Niemen, Case 142, 13397 Marseille Cedex 20 (France); Boulet, P. [MADIREL, UMR 7246 CNRS - Universite Aix-Marseille, av Normandie-Niemen, 13397 Marseille Cedex 20 (France); Nunes, C.A. [Departamento de Engenharia de Materiais (DEMAR), Escola de Engenharia de Lorena (EEL), Universidade de Sao Paulo - USP, Caixa Postal 116, 12600-970 Lorena, Sao Paulo (Brazil); Sopousek, J.; Broz, P. [Masaryk University, Faculty of Science, Department of Chemistry, Kolarska 2, 611 37 Brno (Czech Republic); Masaryk University, Central European Institute of Technology, CEITEC, Kamenice 753/5, 625 00 Brno (Czech Republic); Record, M.-C., E-mail: m-c.record@univ-cezanne.fr [IM2NP, UMR 7334 CNRS - Universite Aix-Marseille, av Normandie-Niemen, Case 142, 13397 Marseille Cedex 20 (France)

    2013-02-25

    Highlights: Black-Right-Pointing-Pointer The phase transitions of the Higher Manganese Silicides were investigated. Black-Right-Pointing-Pointer The samples were characterised by XRD, DTA and DSC. Black-Right-Pointing-Pointer Mn{sub 27}Si{sub 47} is the stable phase at room temperature and under atmospheric pressure. Black-Right-Pointing-Pointer At around 800 Degree-Sign C, Mn{sub 27}Si{sub 47} is transformed into Mn{sub 15}Si{sub 26}. Black-Right-Pointing-Pointer The phase transition is of a second order. - Abstract: This work is an investigation of the phase transformations of the Higher Manganese Silicides in the temperature range [100-1200 Degree-Sign C]. Several complementary experimental techniques were used, namely in situ X-ray Diffraction (XRD), Differential Thermal Analysis (DTA) and Differential Scanning Calorimetry (DSC). The evolution of both the lattice parameters and the thermal expansion coefficients was determined from in situ XRD measurements. The stability of the samples was investigated by thermal analysis (DTA) and Cp measurements (DSC). This study shows that Mn{sub 27}Si{sub 47} which is the stable phase at room temperature and under atmospheric pressure undergoes a phase transformation at around 800 Degree-Sign C. Mn{sub 27}Si{sub 47} is transformed into Mn{sub 15}Si{sub 26}. This phase transformation seems to be of a second order one. Indeed it was not evidenced by DTA and by contrast it appears on the Cp curve.

  11. Determination of palladium content in palladium-alumina/palladium-silica/palladium-tin oxide catalyst for nuclear reactor applications

    International Nuclear Information System (INIS)

    Sharma, P.K.; Bassan, M.K.T.; Avhad, D.K.; Singhal, R.K.

    2012-01-01

    Alumina and silica act as support for finely divided palladium metal powder in synthesis of catalyst. These catalyst (Pd-Al 2 O 3 , Pd-SiO 2 and Pd-SnO 2 ) used in nuclear power reactor (moderator cover gas system) for the conversion of hydrogen. In Indian nuclear power programme these catalyst are regularly used in Kaiga 1 and 2 and Rajasthan atomic power plant 3 and 4. The performance of the catalyst, solely depends on the concentration of palladium, which is the active component in this catalyst composition. Therefore it is highly desirable to have rouged analytical methodology for the accurate estimation of palladium. Leaching of Pd from the bulk matrix is tedious due to the less reactive nature of Pd therefore complete solubilization of the matrix is carried out by fusion method

  12. Analyses on Silicide Coating for LOCA Resistant Cladding

    Energy Technology Data Exchange (ETDEWEB)

    Sweidan, Faris B.; Lee, You Ho; Ryu, Ho Jin [KAIST, Daejeon (Korea, Republic of)

    2015-10-15

    A particular focus of accident-tolerant fuel has been cladding due to the rapid high-temperature oxidation of zirconium-based cladding with the evolution of H2 when steam is a reactant. Some key features of the coated cladding include high-temperature resistance to oxidation, lower processing temperatures, and a high melting point of the coating. Zirconium alloys exhibit a reasonably high melting temperature, so a coating for the cladding is appealing if the coating increases the high-temperature resistance to oxidation. In this case, the cladding is protected from complete oxidation. The cladding coating involves the application of zirconium silicide onto Zr-based cladding. Zirconium silicide coating is expected to produce a glassy layer that becomes more protective at elevated temperature. For this reason, silicide coatings on cladding offer the potential for improved reliability at normal operating temperatures and at the higher transient temperatures encountered during accidents. Although ceramic coatings are brittle and may have weak points to be used as coating materials, several ceramic coatings were successful and showed adherent behavior and high resistance to oxidation. In this study, the oxidation behavior of zirconium silicide and its oxidation kinetics are analyzed. Zirconium silicide is a new suggested material to be used as coatings on existing Zr-based cladding alloys, the aim of this study is to evaluate if zirconium silicide is applicable to be used, so they can be more rapidly developed using existing cladding technology with some modifications. These silicide coatings are an attractive alternative to the use of coatings on zirconium claddings or to the lengthy development of monolithic ceramic or ceramic composite claddings and coatings.

  13. Analyses on Silicide Coating for LOCA Resistant Cladding

    International Nuclear Information System (INIS)

    Sweidan, Faris B.; Lee, You Ho; Ryu, Ho Jin

    2015-01-01

    A particular focus of accident-tolerant fuel has been cladding due to the rapid high-temperature oxidation of zirconium-based cladding with the evolution of H2 when steam is a reactant. Some key features of the coated cladding include high-temperature resistance to oxidation, lower processing temperatures, and a high melting point of the coating. Zirconium alloys exhibit a reasonably high melting temperature, so a coating for the cladding is appealing if the coating increases the high-temperature resistance to oxidation. In this case, the cladding is protected from complete oxidation. The cladding coating involves the application of zirconium silicide onto Zr-based cladding. Zirconium silicide coating is expected to produce a glassy layer that becomes more protective at elevated temperature. For this reason, silicide coatings on cladding offer the potential for improved reliability at normal operating temperatures and at the higher transient temperatures encountered during accidents. Although ceramic coatings are brittle and may have weak points to be used as coating materials, several ceramic coatings were successful and showed adherent behavior and high resistance to oxidation. In this study, the oxidation behavior of zirconium silicide and its oxidation kinetics are analyzed. Zirconium silicide is a new suggested material to be used as coatings on existing Zr-based cladding alloys, the aim of this study is to evaluate if zirconium silicide is applicable to be used, so they can be more rapidly developed using existing cladding technology with some modifications. These silicide coatings are an attractive alternative to the use of coatings on zirconium claddings or to the lengthy development of monolithic ceramic or ceramic composite claddings and coatings

  14. Rare earth silicide nanowires on silicon surfaces

    Energy Technology Data Exchange (ETDEWEB)

    Wanke, Martina

    2008-11-10

    The growth, structure and electronic properties of rare earth silicide nanowires are investigated on planar and vicinal Si(001) und Si(111) surfaces with scanning tunneling microscopy (STM), low energy electron diffraction (LEED) and angle-resolved photoelectron spectroscopy (ARPES). On all surfaces investigated within this work hexagonal disilicides are grown epitaxially with a lattice mismatch of -2.55% up to +0.83% along the hexagonal a-axis. Along the hexagonal c-axis the lattice mismatch is essentially larger with 6.5%. On the Si(001)2 x 1 surface two types of nanowires are grown epitaxially. The socalled broad wires show a one-dimensional metallic valence band structure with states crossing the Fermi level. Along the nanowires two strongly dispersing states at the anti J point and a strongly dispersing state at the anti {gamma} point can be observed. Along the thin nanowires dispersing states could not be observed. Merely in the direction perpendicular to the wires an intensity variation could be observed, which corresponds to the observed spacial structure of the thin nanowires. The electronic properties of the broad erbium silicide nanowires are very similar to the broad dysprosium silicide nanowires. The electronic properties of the DySi{sub 2}-monolayer and the Dy{sub 3}Si{sub 5}-multilayer on the Si(111) surface are investigated in comparison to the known ErSi{sub 2}/Si(111) and Er{sub 3}Si{sub 5}/Si(111) system. The positions and the energetic locations of the observed band in the surface Brillouin zone will be confirmed for dysprosium. The shape of the electron pockets in the (vector)k {sub parallel} space is elliptical at the anti M points, while the hole pocket at the anti {gamma} point is showing a hexagonal symmetry. On the Si(557) surface the structural and electronic properties depend strongly on the different preparation conditions likewise, in particular on the rare earth coverage. At submonolayer coverage the thin nanowires grow in wide areas

  15. Palladium alloys for hydrogen diffusion

    International Nuclear Information System (INIS)

    1977-01-01

    A palladium-base alloy with tin and/or a silicon addition and its use in the production of hydrogen from water via a cycle of chemical reactions, of which the decomposition of HI into H 2 and I 2 is the most important, is described

  16. Palladium-Catalysed Coupling Reactions

    NARCIS (Netherlands)

    de Vries, Johannes G.; Beller, M; Blaser, HU

    2012-01-01

    Palladium-catalysed coupling reactions have gained importance as a tool for the production of pharmaceutical intermediates and to a lesser extent also for the production of agrochemicals, flavours and fragrances, and monomers for polymers. In this review only these cases are discussed where it seems

  17. Irradiation behavior of experimental miniature uranium silicide fuel plates

    International Nuclear Information System (INIS)

    Hofman, Gerard L.; Neimark, L.A.; Mattas, R.F.

    1983-01-01

    Uranium silicides, because of their relatively high uranium density, were selected as candidate dispersion fuels for the higher fuel densities required in the Reduced Enrichment Research and Test Reactor (RERTR) Program. Irradiation experience with this type of fuel, however, was limited to relatively modest fission densities in the bulk form, on the order of 7 x 10 20 cm -3 , far short of he approximately 20 x 10 20 cm -3 goal established for the RERTR Program. The purpose of the irradiation experiments on silicide fuels in the ORR, therefore, was to investigate the intrinsic irradiation behavior of uranium silicide as a dispersion fuel. Of particular interest was the interaction between the silicide particles and the aluminum matrix, the swelling behavior of the silicide particles, and the maximum volume fraction of silicide particles that could be contained in the aluminum matrix. The first group of experimental 'mini' fuel plates have recently reached the program's goal burnup and are in various stages of examination. Although the results to date indicate some limitations, it appears that within the range of parameters examined thus far the uranium silicide dispersion holds promise for satisfying most of the needs of the RERTR Program. The twelve experimental silicide dispersion fuel plates that were irradiated to approximately their goal exposure show the 30-vol % U 3 Si-Al plates to be in a stage of relatively rapid fission-gas-driven swelling at a fission density of 2 x 10 20 cm -3 . This fuel swelling will likely result in unacceptably large plate-thickness increases. The U 3 Si plates appear to be superior in this respect; however, they, too, are starting to move into the rapid fuel-swelling stage. Analysis of the currently available post irradiation data indicates that a 40-vol % dispersed fuel may offer an acceptable margin to the onset of unstable thickness changes at exposures of 2 x 10 21 fission/cm 3 . The interdiffusion between fuel and matrix

  18. Ferromagnetic properties of manganese doped iron silicide

    Science.gov (United States)

    Ruiz-Reyes, Angel; Fonseca, Luis F.; Sabirianov, Renat

    We report the synthesis of high quality Iron silicide (FeSi) nanowires via Chemical Vapor Deposition (CVD). The materials exhibits excellent magnetic response at room temperature, especially when doped with manganese showing values of 2.0 X 10-04 emu for the FexMnySi nanowires. SEM and TEM characterization indicates that the synthesized nanowires have a diameter of approximately 80nm. MFM measurements present a clear description of the magnetic domains when the nanowires are doped with manganese. Electron Diffraction and XRD measurements confirms that the nanowires are single crystal forming a simple cubic structure with space group P213. First-principle calculations were performed on (111) FeSi surface using the Vienna ab initio simulation package (VASP). The exchange correlations were treated under the Ceperley-Alder (CA) local density approximation (LDA). The Brillouin Zone was sampled with 8x8x1 k-point grid. A total magnetic moment of about 10 μB was obtained for three different surface configuration in which the Iron atom nearest to the surface present the higher magnetization. To study the effect of Mn doping, Fe atom was replaced for a Mn. Stronger magnetization is presented when the Mn atom is close to the surface. The exchange coupling constant have been evaluated calculating the energy difference between the ferromagnetic and anti-ferromagnetic configurations.

  19. Submicron Features in Higher Manganese Silicide

    Directory of Open Access Journals (Sweden)

    Yatir Sadia

    2013-01-01

    Full Text Available The world energy crisis had increased the demand for alternative energy sources and as such is one of the topics at the forefront of research. One way for reducing energy consumption is by thermoelectricity. Thermoelectric effects enable direct conversion of thermal into electrical energy. Higher manganese silicide (HMS, MnSi1.75 is one of the promising materials for applications in the field of thermoelectricity. The abundance and low cost of the elements, combined with good thermoelectric properties and high mechanical and chemical stability at high temperatures, make it very attractive for thermoelectric applications. Recent studies have shown that Si-rich HMS has improved thermoelectric properties. The most interesting of which is the unusual reduction in thermal conductivity. In the current research, transmission (TEM and scanning (SEM electron microscopy as well as X-ray diffraction methods were applied for investigation of the govern mechanisms resulting in very low thermal conductivity values of an Si-rich HMS composition, following arc melting and hot-pressing procedures. In this paper, it is shown that there is a presence of sub-micron dislocations walls, stacking faults, and silicon and HMS precipitates inside each other apparent in the matrix, following a high temperature (0.9 Tm hot pressing for an hour. These are not just responsible for the low thermal conductivity values observed but also indicate the ability to create complicate nano-structures that will last during the production process and possibly during the application.

  20. Nickel silicide formation in silicon implanted nickel

    Science.gov (United States)

    Rao, Z.; Williams, J. S.; Pogany, A. P.; Sood, D. K.; Collins, G. A.

    1995-04-01

    Nickel silicide formation during the annealing of very high dose (≥4.5×1017 ions/cm2) Si implanted Ni has been investigated, using ion beam analytical techniques, electron microscopy, and x-ray diffraction analysis. An initial amorphous Si-Ni alloy, formed as a result of high dose ion implantation, first crystallized to Ni2Si upon annealing in the temperature region of 200-300 °C. This was followed by the formation of Ni5Si2 in the temperature region of 300-400 °C and then by Ni3Si at 400-600 °C. The Ni3Si layer was found to have an epitaxial relationship with the substrate Ni, which was determined as Ni3Si∥Ni and Ni3Si∥Ni for Ni(100) samples. The minimum channeling yield in the 2 MeV He Rutherford backscattering and channeling spectra of this epitaxial layer improved with higher annealing temperatures up to 600 °C, and reached a best value measured at about 8%. However, the epitaxial Ni3Si dissolved after long time annealing at 600 °C or annealing at higher temperatures to liberate soluble Si into the Ni substrate. The epitaxy is attributed to the excellent lattice match between the Ni3Si and the Ni. The annealing behavior follows the predictions of the Ni-Si phase diagram for this nickel-rich binary system.

  1. Characterization of uranium silicide powder using XRD

    International Nuclear Information System (INIS)

    Garcia, Rafael H.L.; Saliba-Silva, Adonis M.; Carvalho, Elita F.U.; Lima, Nelson B.; Ichikawa, Rodrigo U.; Martinez, Luiz G.

    2013-01-01

    Uranium silicide (U 3 Si 2 ) is an intermetallic used as nuclear fuel in most modern MTR - Materials Test Reactor. Dispersed in aluminum, this fuel allows high uranium densities, up to 4.8 gU/cm 3 . At IPEN, the fabrication of fuel elements based on U 3 Si 2 for the IEA-R1 reactor is carried out in the Nuclear Fuel Center (CCN), by vacuum induction melting of uranium and silicon, followed by grinding. Before employed in a nuclear reactor, U 3 Si 2 must be submitted to a strict quality control, which includes granulometry, density, X-ray radiography for dispersion homogeneity, chemical and crystallographic characterization. Concerning phase composition for a qualified fuel, the fraction of U 3 Si 2 should be higher than 80wt.%. Aiming at the development of a routine methodology for quantification of phases via analysis of XRD data using the Rietved method, six samples from two production baths of CCN were submitted to X-ray diffraction. The data were analyzed using software GSAS and line profile analysis methods. The results suggest that fusion product have preferred orientation and grinding step is important for a better refinement. (author)

  2. Trace metal assay of uranium silicide fuel

    International Nuclear Information System (INIS)

    Kulkarni, M.J.; Argekar, A.A.; Thulasidas, S.K.; Dhawale, B.A.; Rajeswari, B.; Adya, V.C.; Purohit, P.J.; Neelam, G.; Bangia, T.R.; Page, A.G.; Sastry, M.D.; Iyer, R.H.

    1994-01-01

    A comprehensive trace metal assay of uranium silicide, a fuel for nuclear research reactors that employs low-enrichment uranium, is carried out by atomic spectrometry. Of the list of specification elements, 21 metallic elements are determined by a direct current (dc) arc carrier distillation technique; the rare earths yttrium and zirconium are chemically separated from the major matrix followed by a dc arc/inductively coupled argon plasma (ICP) excitation technique in atomic emission spectrometry (AES); silver is determined by electrothermal atomization-atomic absorption spectrometry (ETA-AAS) without prior chemical separation of the major matrix. Gamma radioactive tracers are used to check the recovery of rare earths during the chemical separation procedure. The detection limits for trace metallics vary in the 0.1- to 40-ppm range. The precision of the determinations as evaluated from the analysis of the synthetic sample with intermediate range analyte concentration is better than 25% relative standard deviation (RSD) for most of the elements employing dc arc-AES, while that for silver determination by ETS-AAS is 10% RSD. The precision of the determinations for four crucially important rare earths by ICP-AES is better than 3% RSD

  3. Si-Ge Nano-Structured with Tungsten Silicide Inclusions

    Science.gov (United States)

    Mackey, Jon; Sehirlioglu, Alp; Dynys, Fred

    2014-01-01

    Traditional silicon germanium high temperature thermoelectrics have potential for improvements in figure of merit via nano-structuring with a silicide phase. A second phase of nano-sized silicides can theoretically reduce the lattice component of thermal conductivity without significantly reducing the electrical conductivity. However, experimentally achieving such improvements in line with the theory is complicated by factors such as control of silicide size during sintering, dopant segregation, matrix homogeneity, and sintering kinetics. Samples are prepared using powder metallurgy techniques; including mechanochemical alloying via ball milling and spark plasma sintering for densification. In addition to microstructural development, thermal stability of thermoelectric transport properties are reported, as well as couple and device level characterization.

  4. Magnesium silicide production and silane synthesis on its basis

    International Nuclear Information System (INIS)

    Taurbaev, T.I.; Mukashev, F.A.; Manakov, S.M.; Francev, U.V.; Kalblanbekov, B.M.; Akhter, P.; Abbas, M.; Hussain, A.

    2003-01-01

    We had developed an alternative method of production of magnesium silicide with use of ferroalloys of silicon. Magnesium silicide is raw material for silane synthesis. The essence of the method consist of sintering FS -75 (ferrosilicium with 75 % of silicon and 25 % of iron, made by ferroalloy factories) with metal magnesium at temperature of 650 deg. C. The X-ray analysis has shown formation of magnesium silicide. That is further used for synthesis of silane. The output of silane is 60 % in respect of the contents of silicon. After removing the water vapors the mass-spectrometer analysis has estimated the purity of silane as 99.95 % with no detection of phosphine and diborane. (author)

  5. TiSi2 integrity within a doped silicide process step

    International Nuclear Information System (INIS)

    Crean, G.M.; Cole, P.D.; Stoemenos, J.

    1993-01-01

    Degradation of arsenic implanted titanium silicide (TiSi 2 ) thin films as a result of thermal processing for shallow junction formation is investigated. Significant arsenic diffusion from the silicide overlayer into the silicon substrate has been detected by Rutherford Backscattering Spectrometry at drive-in temperatures > 1,050 C. Cross-sectional transmission electron micrographs have shown the silicide film become increasingly non-uniform as the thermal budget increases, ultimately leading to discontinuities forming in the silicide film. This observed degradation of the titanium silicide film is also supported by sheet resistance measurements which show the film to degrade significantly above a threshold thermal budget

  6. Morphology of Si/tungsten-silicides/Si interlayers

    International Nuclear Information System (INIS)

    Theodore, N.; Secco d'Aragona, F.; Blackstone, S.

    1992-01-01

    Tungsten and tungsten-silicides are of interest for semiconductor technology because of their refractory nature, low electrical-resistivity and high electromigration-resistance. This paper presents the first formation of buried tungsten-silicide layers in silicon, by proximity adhesion. The interlayers, created by a combination of chemical vapor-deposition (CVD) and proximity-adhesion were studied using transmission electron-microscopy (TEM). The behavior of the layers in the presence and absence of an adjacent silicon-dioxide interlayer was also investigated. Buried silicide layers were successfully formed with or without the adjacent silicon-dioxide. The silicide formed continuous layers with single grains encompassing the width of the interlayer. Individual grains were globular, with cusps at grain boundaries. This caused interlayer-thicknesses to be non-uniform, with lower thickness values being present at the cusps. Occasional voids were observed at grain-boundary cusps. The voids were smaller and less frequent in the presence of an adjacent oxide-layer, due to flow of the oxide during proximity adhesion. Electron-diffraction revealed a predominance of tungsten-disilicide in the interlayers, with some free tungsten being present. Stresses in the silicide layers caused occasional glide dislocations to propagate into the silicon substrate beneath the interlayers. The dislocations propagate only ∼100 nm into the substrate and therefore should not be detrimental to use of the buried layers. Occasional precipitates were observed at the end of glide-loops. These possibly arise due to excess tungsten from the interlayer diffusion down the glide dislocation to finally precipitate out as tungsten-silicide

  7. Oxidation behavior of molybdenum silicides and their composites

    International Nuclear Information System (INIS)

    Natesan, K.; Deevi, S. C.

    2000-01-01

    A key materials issue associated with the future of high-temperature structural silicides is the resistance of these materials to oxidation at low temperatures. Oxidation tests were conducted on Mo-based silicides over a wide temperature range to evaluate the effects of alloy composition and temperature on the protective scaling characteristics and testing regime for the materials. The study included Mo 5 Si 3 alloys that contained several concentrations of B. In addition, oxidation characteristics of MoSi 2 -Si 3 N 4 composites that contained 20--80 vol.% Si 3 N 4 were evaluated at 500--1,400 C

  8. Formation of silicides in a cavity applicator microwave system

    International Nuclear Information System (INIS)

    Thompson, D.C.; Kim, H.C.; Alford, T.L.; Mayer, J.W.

    2003-01-01

    Metal silicides of nickel and cobalt are formed in a cavity applicator microwave system with a magnetron power of 1200 W and a frequency of 2.45 GHz. X-ray diffraction, Rutherford backscattering spectrometry, and four-point-probe measurements are used to identify the silicide phase present and layer thicknesses. Additional processing confirmed that the products attained from heating by microwaves do not differ appreciably from those attained in heating by thermal processes. Materials properties are used to explain microwave power absorption and demonstrate how to tailor a robust process in which thin film reactions can be attained and specific products isolated

  9. Making of fission 99Mo from LEU silicide(s): A radiochemists' view

    International Nuclear Information System (INIS)

    Kolar, Z.I.; Wolterbeek, H.Th.

    2005-01-01

    The present-day industrial scale production of 99 Mo is fission based and involves thermal-neutron irradiation in research reactors of highly enriched uranium (HEU, > 20 % 235 U) containing targets, followed by radiochemical processing of the irradiated targets resulting in the final product: a 99 Mo containing chemical compound of molybdenum. In 1978 a program (RERTR) was started to develop a substitute for HEU reactor fuel i.e. a low enriched uranium (LEU, 235 U) one. In the wake of that program studies were undertaken to convert HEU into LEU based 99 Mo production. Both new targets and radiochemical treatments leading to 99 Mo compounds were proposed. One of these targets is based on LEU silicide, U 3 Si 2 . Present paper aims at comparing LEU U 3 Si 2 and LEU U 3 Si with another LEU target i.e. target material and arriving at some preferences pertaining to 99 Mo production. (author)

  10. Silicide Schottky Contacts to Silicon: Screened Pinning at Defect Levels

    Energy Technology Data Exchange (ETDEWEB)

    Drummond, T.J.

    1999-03-11

    Silicide Schottky contacts can be as large as 0.955 eV (E{sub v} + 0.165 eV) on n-type silicon and as large as 1.05 eV (E{sub c} {minus} 0.07 eV) on p-type silicon. Current models of Schottky barrier formation do not provide a satisfactory explanation of occurrence of this wide variation. A model for understanding Schottky contacts via screened pinning at defect levels is presented. In the present paper it is shown that most transition metal silicides are pinned approximately 0.48 eV above the valence band by interstitial Si clusters. Rare earth disilicides pin close to the divacancy acceptor level 0.41 eV below the conduction band edge while high work function silicides of Ir and Pt pin close to the divacancy donor level 0.21 eV above the valence band edge. Selection of a particular defect pinning level depends strongly on the relative positions of the silicide work function and the defect energy level on an absolute energy scale.

  11. The electronic structure of 4d and 5d silicides

    NARCIS (Netherlands)

    Speier, W.; Kumar, L.; Sarma, D.D.; Groot, R.A. de; Fuggle, J.C.

    1989-01-01

    A systematic experimental and theoretical study of the electronic structure of stoichiometric silicides with Nb, Mo, Ta and W is presented. We have employed x-ray photoemission and bremsstrahlung isochromat spectroscopy as experimental techniques and interpreted the measured data by calculation of

  12. Neutronic design of the RSG-GAS silicide core

    Energy Technology Data Exchange (ETDEWEB)

    Sembiring, T.M.; Kuntoro, I.; Hastowo, H. [Center for Development of Research Reactor Technology National Nuclear Energy Agency BATAN, PUSPIPTEK Serpong Tangerang, 15310 (Indonesia)

    2002-07-01

    The objective of core conversion program of the RSG-GAS multipurpose reactor is to convert the fuel from oxide, U{sub 3}O{sub 8}-Al to silicide, U{sub 3}Si{sub 2}-Al. The aim of the program is to gain longer operation cycle by having, which is technically possible for silicide fuel, a higher density. Upon constraints of the existing reactor system and utilization, an optimal fuel density in amount of 3.55 g U/cc was found. This paper describes the neutronic parameter design of the silicide equilibrium core and the design of its transition cores as well. From reactivity control point of view, a modification of control rod system is also discussed. All calculations are carried out by means of diffusion codes, Batan-EQUIL-2D, Batan-2DIFF and -3DIFF. The silicide core shows that longer operation cycle of 32 full power days can be achieved without decreasing the safety criteria and utilization capabilities. (author)

  13. Palladium allergy in relation to dentistry

    NARCIS (Netherlands)

    Muris, J.

    2015-01-01

    Palladium is a metal that is used as alloying metal for dental crowns and bridges. This thesis focusses on the possible impact of oral exposure to this metal on the immune system, and allergy in particular. An alternative skin test allergen for diagnosing palladium allergy is introduced: (di)sodium

  14. Texture in thin film silicides and germanides: A review

    Energy Technology Data Exchange (ETDEWEB)

    De Schutter, B., E-mail: bob.deschutter@ugent.be; De Keyser, K.; Detavernier, C. [Department of Solid State Sciences, Ghent University, Ghent (Belgium); Lavoie, C. [IBM Research Division, T.J. Watson Research Center, P.O. Box 218, Yorktown Heights, New York 10598 (United States)

    2016-09-15

    Silicides and germanides are compounds consisting of a metal and silicon or germanium. In the microelectronics industry, silicides are the material of choice for contacting silicon based devices (over the years, CoSi{sub 2}, C54-TiSi{sub 2}, and NiSi have been adopted), while germanides are considered as a top candidate for contacting future germanium based electronics. Since also strain engineering through the use of Si{sub 1−x}Ge{sub x} in the source/drain/gate regions of MOSFET devices is an important technique for improving device characteristics in modern Si-based microelectronics industry, a profound understanding of the formation of silicide/germanide contacts to silicon and germanium is of utmost importance. The crystallographic texture of these films, which is defined as the statistical distribution of the orientation of the grains in the film, has been the subject of scientific studies since the 1970s. Different types of texture like epitaxy, axiotaxy, fiber, or combinations thereof have been observed in such films. In recent years, it has become increasingly clear that film texture can have a profound influence on the formation and stability of silicide/germanide contacts, as it controls the type and orientation of grain boundaries (affecting diffusion and agglomeration) and the interface energy (affecting nucleation during the solid-state reaction). Furthermore, the texture also has an impact on the electrical characteristics of the contact, as the orientation and size of individual grains influences functional properties such as contact resistance and sheet resistance and will induce local variations in strain and Schottky barrier height. This review aims to give a comprehensive overview of the scientific work that has been published in the field of texture studies on thin film silicide/germanide contacts.

  15. Texture in thin film silicides and germanides: A review

    International Nuclear Information System (INIS)

    De Schutter, B.; De Keyser, K.; Detavernier, C.; Lavoie, C.

    2016-01-01

    Silicides and germanides are compounds consisting of a metal and silicon or germanium. In the microelectronics industry, silicides are the material of choice for contacting silicon based devices (over the years, CoSi_2, C54-TiSi_2, and NiSi have been adopted), while germanides are considered as a top candidate for contacting future germanium based electronics. Since also strain engineering through the use of Si_1_−_xGe_x in the source/drain/gate regions of MOSFET devices is an important technique for improving device characteristics in modern Si-based microelectronics industry, a profound understanding of the formation of silicide/germanide contacts to silicon and germanium is of utmost importance. The crystallographic texture of these films, which is defined as the statistical distribution of the orientation of the grains in the film, has been the subject of scientific studies since the 1970s. Different types of texture like epitaxy, axiotaxy, fiber, or combinations thereof have been observed in such films. In recent years, it has become increasingly clear that film texture can have a profound influence on the formation and stability of silicide/germanide contacts, as it controls the type and orientation of grain boundaries (affecting diffusion and agglomeration) and the interface energy (affecting nucleation during the solid-state reaction). Furthermore, the texture also has an impact on the electrical characteristics of the contact, as the orientation and size of individual grains influences functional properties such as contact resistance and sheet resistance and will induce local variations in strain and Schottky barrier height. This review aims to give a comprehensive overview of the scientific work that has been published in the field of texture studies on thin film silicide/germanide contacts.

  16. Texture in thin film silicides and germanides: A review

    Science.gov (United States)

    De Schutter, B.; De Keyser, K.; Lavoie, C.; Detavernier, C.

    2016-09-01

    Silicides and germanides are compounds consisting of a metal and silicon or germanium. In the microelectronics industry, silicides are the material of choice for contacting silicon based devices (over the years, CoSi2, C54-TiSi2, and NiSi have been adopted), while germanides are considered as a top candidate for contacting future germanium based electronics. Since also strain engineering through the use of Si1-xGex in the source/drain/gate regions of MOSFET devices is an important technique for improving device characteristics in modern Si-based microelectronics industry, a profound understanding of the formation of silicide/germanide contacts to silicon and germanium is of utmost importance. The crystallographic texture of these films, which is defined as the statistical distribution of the orientation of the grains in the film, has been the subject of scientific studies since the 1970s. Different types of texture like epitaxy, axiotaxy, fiber, or combinations thereof have been observed in such films. In recent years, it has become increasingly clear that film texture can have a profound influence on the formation and stability of silicide/germanide contacts, as it controls the type and orientation of grain boundaries (affecting diffusion and agglomeration) and the interface energy (affecting nucleation during the solid-state reaction). Furthermore, the texture also has an impact on the electrical characteristics of the contact, as the orientation and size of individual grains influences functional properties such as contact resistance and sheet resistance and will induce local variations in strain and Schottky barrier height. This review aims to give a comprehensive overview of the scientific work that has been published in the field of texture studies on thin film silicide/germanide contacts.

  17. Evaluation of anomalies during nickel and titanium silicide formation using the effective heat of formation mode

    CSIR Research Space (South Africa)

    Pretorius, R

    1993-11-01

    Full Text Available , as well as the observed sequence of growth of different silicide phases, are not in agree- ment with thermodynamic considerations [26]. In the case of the nickel silicides Ni,Si is nearly always found to be the first... to determine how the oxygen content in the silicon affects phase formation. We also show how the anomalous behaviour of titanium and nickel silicide formation can be explained thermodynamically by using the ?effective heat...

  18. Gas cluster ion beam assisted NiPt germano-silicide formation on SiGe

    Energy Technology Data Exchange (ETDEWEB)

    Ozcan, Ahmet S., E-mail: asozcan@us.ibm.com [IBM Almaden Research Center, 650 Harry Road, San Jose, California 95120 (United States); Lavoie, Christian; Jordan-Sweet, Jean [IBM T. J. Watson Research Center, 1101 Kitchawan Road, Yorktown Heights, New York 10598 (United States); Alptekin, Emre; Zhu, Frank [IBM Semiconductor Research and Development Center, 2070 Route 52, Hopewell Junction, New York 12533 (United States); Leith, Allen; Pfeifer, Brian D.; LaRose, J. D.; Russell, N. M. [TEL Epion Inc., 900 Middlesex Turnpike, Bldg. 6, Billerica, Massachusetts 01821 (United States)

    2016-04-21

    We report the formation of very uniform and smooth Ni(Pt)Si on epitaxially grown SiGe using Si gas cluster ion beam treatment after metal-rich silicide formation. The gas cluster ion implantation process was optimized to infuse Si into the metal-rich silicide layer and lowered the NiSi nucleation temperature significantly according to in situ X-ray diffraction measurements. This novel method which leads to more uniform films can also be used to control silicide depth in ultra-shallow junctions, especially for high Ge containing devices, where silicidation is problematic as it leads to much rougher interfaces.

  19. A study of CoSix silicide formed by recoil implantation

    International Nuclear Information System (INIS)

    Kwok, H.L.

    1989-01-01

    This work investigated the formation of CoSi x silicides on n-Si by recoil implantation through a thin cobalt layer using an inert gas ion beam. The results suggest the formation of a very shallow (35 to 45 nm) silicide surface layer under the specific conditions of preparation. The surface layer resistivity was comparable to values reported for Co 2 Si and CoSi, although below the surface, the resistivity decreased. This appeared to suggest a change-over from cobalt-rich silicides near the surface to a more conducting silicide (CoSi 2 ) at the interface. (author)

  20. Analysis of reactivity accidents of the RSG-GAS core with silicide fuel

    International Nuclear Information System (INIS)

    Tukiran

    2002-01-01

    The fuels of RSG-GAS reactor is changed from uranium oxide to uranium silicide. For time being, the fuel of RSG-GAS core are mixed up between oxide and silicide fuels with 250 gr of loading and 2.96 g U/cm 3 of density, respectively. While, silicide fuel with 300 gr of loading is still under research. The advantages of silicide fuels are can be used in high density, so that, it can be stayed longer in the core at higher burn-up, therefore, the length of cycle is longer. The silicide fuel in RSG-GAS core is used in step-wise by using mixed up core. Firstly, it is used silicide fuel with 250 gr of loading and then, silicide fuel with 300 gr of loading (3.55 g U/cm 3 of density). In every step-wise of fuel loading must be analysed its safety margin. In this occasion, it is analysed the reactivity accident of RSG-GAS core with 300 gr of silicide fuel loading. The calculation was done by using POKDYN code which available at P2TRR. The calculation was done by reactivity insertion at start up and power rangers. From all cases which were have been done, the results of analysis showed that there is no anomaly and safety margin break at RSG-GAS core with 300 gr silicide fuel loading

  1. Fuel-cycle cost comparisons with oxide and silicide fuels

    International Nuclear Information System (INIS)

    Matos, J.E.; Freese, K.E.

    1982-01-01

    This paper addresses fuel cycle cost comparisons for a generic 10 MW reactor with HEU aluminide fuel and with LEU oxide and silicide fuels in several fuel element geometries. The intention of this study is to provide a consistent assessment of various design options from a cost point of view. Fuel cycle cost benefits could result if a number of reactors were to utilize fuel elements with the same number or different numbers of the same standard fuel plate. Data are presented to quantify these potential cost benefits. This analysis shows that there are a number of fuel element designs using LEU oxide or silicide fuels that have either the same or lower total fuel cycle costs than the HEU design. Use of these fuels with the uranium densities considered requires that they are successfully demonstrated and licensed

  2. RA-3 core with uranium silicide fuel elements

    International Nuclear Information System (INIS)

    Abbate, Maximo J.; Sbaffoni, Maria M.

    2000-01-01

    Following on with studies on uranium silicide fuel elements, this paper reports some comparisons between the use of standard ECN [U 3 O 8 ] fuel elements and type P-06 [from U 3 Si 2 ] fuel elements in the RA-3 core.The first results showed that the calculated overall mean burn up is in agreement with that reported for the facility, which gives more confidence to the successive ones. Comparing the mentioned cores, the silicide one presents several advantages such as: -) a mean burn up increase of 18 %; -) an extraction burn up increase of 20 %; -) 37.4 % increase in full power days, for mean burn up. All this is meritorious for this fuel. Moreover, grouped and homogenized libraries were prepared for CITVAP code that will be used for planning experiments and other bidimensional studies. Preliminary calculations were also performed. (author)

  3. Secondary neutral mass spectrometry depth profile analysis of silicides

    International Nuclear Information System (INIS)

    Beckmann, P.; Kopnarski, M.; Oechsner, H.

    1985-01-01

    The Direct Bombardment Mode (DBM) of Secondary Neutral Mass Spectrometry (SNMS) has been applied for depth profile analysis of two different multilayer systems containing metal silicides. Due to the extremely high depth resolution obtained with low energy SNMS structural details down to only a few atomic distances are detected. Stoichiometric information on internal oxides and implanted material is supplied by the high quantificability of SNMS. (Author)

  4. Fracture of niobium-base silicide coated alloy

    International Nuclear Information System (INIS)

    Davydova, A.D.; Zotov, Yu.P.; Ivashchenko, O.V.; Kushnareva, N.P.; Yarosh, I.P.

    1990-01-01

    Mechanical properties and character of fracture of Nb-W-Mo-Zr-C alloy composition with complex by composition and structure silicide coating under different states of stage-by-stage coating are studied. Structural features, character of fracture from ductile to quasibrittle transcrystalline one and, respectively, the composition plasticity level are defined by interrelation of fracture processes in coating, matrix plastic flow and possibility and way of stress relaxation on their boundary

  5. Development of Silicide Coating on Molybdenum Alloy Cladding

    International Nuclear Information System (INIS)

    Lim, Woojin; Ryu, Ho Jin

    2015-01-01

    The molybdenum alloy is considered as one of the accident tolerant fuel (ATF) cladding materials due to its high temperature mechanical properties. However, molybdenum has a weak oxidation resistance at elevated temperatures. To modify the oxidation resistance of molybdenum cladding, silicide coating on the cladding is considered. Molybdenum silicide layers are oxidized to SiO 2 in an oxidation atmosphere. The SiO 2 protective layer isolates the substrate from the oxidizing atmosphere. Pack cementation deposition technique is widely adopted for silicide coating for molybdenum alloys due to its simple procedure, homogeneous coating quality and chemical compatibility. In this study, the pack cementation method was conducted to develop molybdenum silicide layers on molybdenum alloys. It was found that the Mo 3 Si layer was deposited on substrate instead of MoSi 2 because of short holding time. It means that through the extension of holding time, MoSi 2 layer can be formed on molybdenum substrate to enhance the oxidation resistance of molybdenum. The accident tolerant fuel (ATF) concept is to delay the process following an accident by reducing the oxidation rate at high temperatures and to delay swelling and rupture of fuel claddings. The current research for Atf can be categorized into three groups: First, modification of existing zirconium-based alloy cladding by improving the high temperature oxidation resistance and strength. Second, replacing Zirconium based alloys with alternative metallic materials such as refractory elements with high temperature oxidation resistance and strength. Third, designing alternative fuel structures using ceramic and composite systems

  6. Detailed analysis of uranium silicide dispersion fuel swelling

    International Nuclear Information System (INIS)

    Hofmann, G.L.; Ryu, Woo-Seog

    1991-01-01

    Swelling of U 3 Si and U 3 Si 2 is analyzed. The growth of fission gas bubbles appears to be affected by fission rate, fuel loading, and micro structural change taking place in the fuel compounds during irradiation. Several mechanisms are explored to explain the observations. The present work is aimed at a better understanding of the basic swelling phenomenon in order to accurately model irradiation behavior of uranium silicide dispersion fuel. (orig.)

  7. Detailed analysis of uranium silicide dispersion fuel swelling

    International Nuclear Information System (INIS)

    Hofman, G.L.; Ryu, Woo-Seog.

    1989-01-01

    Swelling of U 3 Si and U 3 Si 2 is analyzed. The growth of fission gas bubbles appears to be affected by fission rate, fuel loading, and microstructural change taking place in the fuel compounds during irradiation. Several mechanisms are explored to explain the observations. The present work is aimed at a better understanding of the basic swelling phenomenon in order to accurately model irradiation behavior of uranium silicide disperson fuel. 5 refs., 10 figs

  8. Anionic Palladium(0) and Palladium(II) Ate Complexes.

    Science.gov (United States)

    Kolter, Marlene; Böck, Katharina; Karaghiosoff, Konstantin; Koszinowski, Konrad

    2017-10-16

    Palladium ate complexes are frequently invoked as important intermediates in Heck and cross-coupling reactions, but so far have largely eluded characterization at the molecular level. Here, we use electrospray-ionization mass spectrometry, electrical conductivity measurements, and NMR spectroscopy to show that the electron-poor catalyst [L 3 Pd] (L=tris[3,5-bis(trifluoromethyl)phenyl]phosphine) readily reacts with Br - ions to afford the anionic, zero-valent ate complex [L 3 PdBr] - . In contrast, more-electron-rich Pd catalysts display lower tendencies toward the formation of ate complexes. Combining [L 3 Pd] with LiI and an aryl iodide substrate (ArI) results in the observation of the Pd II ate complex [L 2 Pd(Ar)I 2 ] - . © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  9. Determination of palladium by flame photometry

    International Nuclear Information System (INIS)

    Parellada Bellod, R.

    1964-01-01

    A study on the determination of palladium by lame photometry, fixing the most convent experimental conditions and using solvents to increase the emission of this elements is carried out. Among the organic solvents, acetone has been found the most efficient. The interferences produced by anions and cations have also been studied and an analytical method is related, in which lines of calibration of 0 to 100 ppm palladium re used. (Author) 7 refs

  10. Mechanoactivation of chromium silicide formation in the SiC-Cr-Si system

    Directory of Open Access Journals (Sweden)

    Vlasova M.

    2002-01-01

    Full Text Available The processes of simultaneous grinding of the components of a SiC-Cr-Si mixture and further temperature treatment in the temperature range 1073-1793 K were studied by X-ray phase analysis, IR spectroscopy, electron microscopy, and X-ray microanalysis. It was established that, during grinding of the mixture, chromium silicides form. A temperature treatment completes the process. Silicide formation proceeds within the framework of the diffusion of silicon into chromium. In the presence of SiO2 in the mixture, silicide formation occurs also as a result of the reduction of silica by silicon and silicon carbide. The sintering of synthesized composite SiC-chromium silicides powders at a high temperature under a high pressure (T = 2073 K, P = 5 GPa is accompanied by the destruction of cc-SiC particles, the cc/3 transition in silicon carbide and deformation distortions of the lattices of chromium silicides.

  11. Neutronic Analysis and Radiological Safety of RSG-GAS Reactor on 300 Grams Uranium Silicide Core

    International Nuclear Information System (INIS)

    Pande Made Udiyani; Lily Suparlina; Rokhmadi

    2007-01-01

    As starting of usage silicide U 250 g fuel element in the core of RSG-GAS and will be continued with usage of silicide U 300 g fuel element, hence done beforehand neutronic analyse and radiological safety of RSG-GAS. Calculation done by ORIGEN2.1 code to calculate source term, and also by PC-COSYMA code to calculate radiological safety of radioactive dispersion from RSG-GAS. Calculation of radioactive dispersion done at condition of reactor is postulated be happened an accident of LOCA causing one fuel element to melt. Neutronic analysis indicate that silicide U 250 g full core shall to be operated beforehand during 625 MWD before converted to silicide U 300 g core. During operation of transition core with mixture of silicide U 250 g and 300 g, all parameter fulfill criterion of safety Designed Balance core of silicide U 300 g will be reached at the time of fifth full core. Result of calculation indicate that through mixture core of silicide U 250 and 300 g proposed can form silicide U 300 g balance core of reactor RSG-GAS safely. Calculation of radiology safety by deterministic for silicide U 300 g balance core, and accident postulation which is equal to core of silicide U 250 g yield output in the form of radiation activity (radionuclide concentration in the air and deposition on the ground), radiation dose (collective and individual), radiation effect (short- and long-range), which accepted by society in each perceived sector. Result of calculation indicated that dose accepted by society is not pass permitted boundary for public society if happened accident. (author)

  12. Exploitation of a self-limiting process for reproducible formation of ultrathin Ni1-xPtx silicide films

    International Nuclear Information System (INIS)

    Zhang Zhen; Zhu Yu; Rossnagel, Steve; Murray, Conal; Jordan-Sweet, Jean; Yang, Bin; Gaudet, Simon; Desjardins, Patrick; Kellock, Andrew J.; Ozcan, Ahmet; Zhang Shili; Lavoie, Christian

    2010-01-01

    This letter reports on a process scheme to obtain highly reproducible Ni 1-x Pt x silicide films of 3-6 nm thickness formed on a Si(100) substrate. Such ultrathin silicide films are readily attained by sputter deposition of metal films, metal stripping in wet chemicals, and final silicidation by rapid thermal processing. This process sequence warrants an invariant amount of metal intermixed with Si in the substrate surface region independent of the initial metal thickness, thereby leading to a self-limiting formation of ultrathin silicide films. The crystallographic structure, thickness, uniformity, and morphological stability of the final silicide films depend sensitively on the initial Pt fraction.

  13. Palladium-cobalt particles as oxygen-reduction electrocatalysts

    Science.gov (United States)

    Adzic, Radoslav [East Setauket, NY; Huang, Tao [Manorville, NY

    2009-12-15

    The present invention relates to palladium-cobalt particles useful as oxygen-reducing electrocatalysts. The invention also relates to oxygen-reducing cathodes and fuel cells containing these palladium-cobalt particles. The invention additionally relates to methods for the production of electrical energy by using the palladium-cobalt particles of the invention.

  14. Unexpectedly high uptake of palladium by bituminous coals

    Energy Technology Data Exchange (ETDEWEB)

    Lakatos, J. [Research Lab. for Mining Chemistry, Hungarian Academy of Sciences, Miskolc-Egyetemvaros (Hungary); Brown, S.D.; Snape, C.E. [Univ. of Strathclyde, Dept. of Pure and Applied Chemistry, Glasgow (United Kingdom)

    1997-12-31

    The uptake of palladium as a conversion catalyst onto coals of different rank was investigated. Palladium fixation occurs by a different mode to that for alkaline earth and first row transition metals. Therefore, the dispersion of relatively high concentration of palladium by an ion sorption process is even possible for bituminous coals. (orig.)

  15. : Recyclable, ligand free palladium(II) catalyst for Heck reaction

    Indian Academy of Sciences (India)

    well as heterogeneous palladium catalysts, generated from either palladium(0) compounds or palladium(II) acetate or chloride salts.6 Several ligands such as phosphines, phoshites, carbenes, thioethers have been successfully employed for this reaction.7 However, homogeneous catalysis results in problems of recovery.

  16. Mechanochemical synthesis and spark plasma sintering of the cerium silicides

    Energy Technology Data Exchange (ETDEWEB)

    Alanko, Gordon A.; Jaques, Brian; Bateman, Allyssa [Department of Materials Science and Engineering, College of Engineering, Boise State University, 1910 University Drive, Boise, ID 83725 (United States); Butt, Darryl P., E-mail: darrylbutt@boisestate.edu [Department of Materials Science and Engineering, College of Engineering, Boise State University, 1910 University Drive, Boise, ID 83725 (United States); Center for Advanced Energy Studies, 995 University Boulevard, Idaho Falls, ID 83401 (United States)

    2014-12-15

    Highlights: • Ce{sub 5}Si{sub 3}, Ce{sub 3}Si{sub 2}, CeSi, CeSi{sub 2−x} and CeSi{sub 2} were mechanochemically synthesized. • Temperature and pressure were monitored to investigate reaction progress. • All syntheses proceeded through a MSR event followed by rapid solid-state diffusion. • Milling time before MSR correlates well with effective heat of formation. • Some synthesized material was densified by spark plasma sintering. - Abstract: The cerium silicides, Ce{sub 5}Si{sub 3}, Ce{sub 3}Si{sub 2}, CeSi, CeSi{sub 2−y}, and CeSi{sub 2−x}, have been prepared from the elements by mechanochemical processing in a planetary ball mill. Preparation of the cerium silicide Ce{sub 5}Si{sub 4} was unsuccessfully attempted and potential reasons for this are discussed. Temperature and pressure of the milling vial were monitored in situ to gain insight into the mechanochemical reaction kinetics, which include a mechanically-induced self-propagating reaction (MSR). Some prepared powders were consolidated by spark plasma sintering to high density. Starting materials, as-milled powders, and consolidated samples were characterized by X-ray diffraction, scanning electron microscopy, and energy dispersive spectroscopy. The results obtained help elucidate key questions in mechanochemical processing of intermetallics, showing first phase formation similar to thin films, MSR ignition times that are composition- and milling speed-dependent, and sensitivity of stable compound formation on the impact pressure. The results demonstrate mechanochemical synthesis as a viable technique for rare earth silicides.

  17. Immobilization of Uranium Silicide in Sintered Iron-Phosphate Glass

    International Nuclear Information System (INIS)

    Mateos, Patricia; Russo, Diego; Rodriguez, Diego; Heredia, A; Sanfilippo, M.; Sterba, Mario

    2003-01-01

    This work is a continuation of a previous one performed in vitrification of uranium silicide in borosilicate and iron-silicate glasses, by sintering.We present the results obtained with an iron-phosphate glass developed at our laboratory and we compare this results with those obtained with the above mentioned glasses. The main objective was to develop a method as simple as possible, so as to get a monolithic glass block with the appropriate properties to be disposed in a deep geological repository.The thermal transformation of the uranium silicide was characterized by DTA/TG analysis and X-ray diffraction.We determined the evolution of the crystalline phases and the change in weight.Calcined uranium silicide was mixed with natural U 3 O 8 , the amount of U 3 O 8 was calculated to simulate an isotopic dilution of 4%.This material was mixed with powdered iron-phosphate glass (in wt.%: 64,9 P 2 O 5 ; 22,7 Fe 2 O 3 ; 8,1 Al 2 O 3 ; 4,3 Na 2 O) in different proportions (in wt%): 7%, 10% y 15%.The powders were pressed and sintered at temperatures between 585 y 670 °C. Samples of the sintered pellet were prepared for the lixiviation tests (MCC-1P: monolithic samples; deionised water; 90° C; 7, 14 and 28 days).The samples showed a quite good durability (0,6 g.m -2 .day -1 ), similar to borosilicate glasses.The microstructure of the glass samples showed that the uranium particles are much better integrated to the glass matrix in the iron-phosphate glasses than in the borosilicate or iron-silicate glasses.We can conclude that the sintered product obtained could be a good alternative for the immobilization of nuclear wastes with high content of uranium, as the ones arising from the conditioning of research reactors spent fuels

  18. Neutronic calculations of PARR-1 cores using LEU silicide fuel

    International Nuclear Information System (INIS)

    Arshad, M.; Bakhtyar, S.; Hayat, T.; Salahuddin, A.

    1991-08-01

    Detailed neutronic calculations have been carried out for different PARR-1 cores utilizing low enriched uranium (LEU) silicide fuel and operating at an upgraded power of 9 MW. The calculations include the search for critical loadings in open and stall ends of the pool, neutronic analysis of the first full equilibrium core and calculations cores. The burnup study of inventory have also been carried out. Further, the reactivity coefficients of the first full power operation core are evaluated for use in the accident analysis. 14 figs. (author)

  19. Postirradiation analysis of experimental uranium-silicide dispersion fuel plates

    International Nuclear Information System (INIS)

    Hofman, G.L.; Neimark, L.A.

    1985-01-01

    Low-enriched uranium silicide dispersion fuel plates were irradiated to maximum burnups of 96% of 235 U. Fuel plates containing 33 v/o U 3 Si and U 3 Si 2 behaved very well up to this burnup. Plates containing 33 v/o U 3 Si-Al pillowed between 90 and 96% burnup of the fissile atoms. More highly loaded U 3 Si-Al plates, up to 50 v/o were found to pillow at lower burnups. Plates containing 40 v/o U 3 Si showed an increase swelling rate around 85% burnup. 5 refs., 10 figs

  20. Progress in doping of ruthenium silicide (Ru2Si3)

    International Nuclear Information System (INIS)

    Vining, C.B.; Allevato, C.E.

    1992-01-01

    This paper reports that ruthenium silicide (Ru 2 Si 3 ) is currently under development as a promising thermoelectric material suitable for space power applications. Key to realizing the potentially high figure of merit values of this material is the development of appropriate doping techniques. In this study, manganese and iridium have been identified as useful p- and n-type dopants, respectively. Resistivity values have been reduced by more than 3 orders of magnitude. Anomalous Hall effect results, however, complicate interpretation of some of the results and further effort is required to achieve optimum doping levels

  1. Microstructure and mechanical properties of molybdenum silicides with Al additions

    International Nuclear Information System (INIS)

    Rosales, I.; Bahena, D.; Colin, J.

    2007-01-01

    Several molybdenum silicides alloys with different aluminum additions were produced by the arc-cast method. Microstructure observed in the alloys presented a variation of the precipitated second phase respect to the aluminum content. Evaluation of the compressive behavior at high temperature of the alloys shows an important improvement in its ductility, approximately of 20%. Fracture toughness was increased proportionally with Al content. In addition at room temperature the alloys show a better mechanical behavior in comparison with the sample unalloyed. In general, Al additions result to be a good alternative to improve the resistance of these intermetallic alloys. The results are interpreted on the base of the analysis of second phase strengthening

  2. Californium Recovery from Palladium Wire

    Energy Technology Data Exchange (ETDEWEB)

    Burns, Jon D. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)

    2014-08-01

    The recovery of 252Cf from palladium-252Cf cermet wires was investigated to determine the feasibility of implementing it into the cermet wire production operation at Oak Ridge National Laboratory’s Radiochemical Engineering Development Center. The dissolution of Pd wire in 8 M HNO3 and trace amounts of HCl was studied at both ambient and elevated temperatures. These studies showed that it took days to dissolve the wire at ambient temperature and only 2 hours at 60°C. Adjusting the ratio of the volume of solvent to the mass of the wire segment showed little change in the kinetics of dissolution, which ranged from 0.176 mL/mg down to 0.019 mL/mg. A successful chromatographic separation of 153Gd, a surrogate for 252Cf, from Pd was demonstrated using AG 50x8 cation exchange resin with a bed volume of 0.5 mL and an internal diameter of 0.8 cm.

  3. Structural and electronic properties of rare-earth silicide thin films at Si(111)

    Energy Technology Data Exchange (ETDEWEB)

    Dues, Christof; Schmidt, Wolf Gero; Sanna, Simone [Lehrstuhl fuer Theoretische Physik, Universitaet Paderborn (Germany)

    2016-07-01

    Rare-earth (RE) silicides thin films on silicon surfaces are currently of high interest. They grow nearly defect-free because of the small lattice mismatch, and exhibit very low Schottky-barriers on n-type silicon. They even give rise to the self-organized formation of RE silicide nanowires on the Si(001) and vicinal surfaces. Depending on the amount of deposited RE atoms, a plethora of reconstructions are observed for the RE silicide. While one monolayer leads to the formation of a 1 x 1-reconstruction, several monolayer thick silicides crystallize in a √(3) x √(3) R30 {sup circle} superstructure. Submonolayer RE deposition leads to different periodicities. In this work we investigate the formation of RE silicides thin films on Si(111) within the density functional theory. The energetically favored adsorption site for RE adatoms is determined calculating the potential energy surface. As prototypical RE, Dysprosium is used. Additional calculations are performed for silicides formed by different RE elements. We calculate structural properties, electronic band structures and compare measured and simulated STM images. We consider different terminations for the 5 x 2 reconstruction occurring in the submonolayer regime and investigate their stability by means of ab initio thermodynamics. The same method is employed to predict the stable silicide structure as a function of the deposited RE atoms.

  4. Silver-Palladium Surfaces Inhibit Biofilm Formation

    DEFF Research Database (Denmark)

    Chiang, Wen-Chi; Schroll, Casper; Hilbert, Lisbeth Rischel

    2009-01-01

    Undesired biofilm formation is a major concern in many areas. In the present study, we investigated biofilm-inhibiting properties of a silver-palladium surface that kills bacteria by generating microelectric fields and electrochemical redox processes. For evaluation of the biofilm inhibition...... efficacy and study of the biofilm inhibition mechanism, the silver-sensitive Escherichia coli J53 and the silver-resistant E. coli J53[pMG101] strains were used as model organisms, and batch and flow chamber setups were used as model systems. In the case of the silver-sensitive strain, the silver......-palladium surfaces killed the bacteria and prevented biofilm formation under conditions of low or high bacterial load. In the case of the silver-resistant strain, the silver-palladium surfaces killed surface-associated bacteria and prevented biofilm formation under conditions of low bacterial load, whereas under...

  5. Influence of IR-laser irradiation on α-SiC-chromium silicides ceramics

    International Nuclear Information System (INIS)

    Vlasova, M.; Marquez Aguilar, P.A.; Resendiz-Gonzalez, M.C.; Kakazey, M.; Bykov, A.; Gonzalez Morales, I.

    2005-01-01

    This project investigated the influence of IR-laser irradiation (λ = 1064 nm, P = 240 mW) on composite ceramics SiC-chromium silicides (CrSi 2 , CrSi, Cr 5 Si 3 ) by methods of X-ray diffraction, electron microscopy, atomic force microscopy, and X-ray microanalysis. Samples were irradiated in air. It was established that a surface temperature of 1990 K was required to melt chromium silicides, evaporate silicon from SiC, oxidize chromium silicides, and enrich superficial layer by carbon and chromium oxide

  6. Fuel cycle cost comparisons with oxide and silicide fuels

    Energy Technology Data Exchange (ETDEWEB)

    Matos, J E; Freese, K E [RERTR Program, Argonne National Laboratory (United States)

    1983-09-01

    This paper addresses fuel cycle cost comparisons for a generic 10 MW reactor with HEU aluminide fuel and with LEU oxide and silicide fuels in several fuel element geometries. The intention of this study is to provide a consistent assessment of various design options from a cost point of view. The status of the development and demonstration of the oxide and silicide fuels are presented in several papers in these proceedings. Routine utilization of these fuels with the uranium densities considered here requires that they are successfully demonstrated and licensed. Thermal-hydraulic safety margins, shutdown margins, mixed cores, and transient analyses are not addressed here, but analyses of these safety issues are in progress for a limited number of the most promising design options. Fuel cycle cost benefits could result if a number of reactors were to utilize fuel elements with the same number or different numbers of the same standard fuel plate. Data is presented to quantify these potential cost benefits. This analysis shows that there are a number of fuel element designs using LEU oxide or silicide fuels that have either the same or lower total fuel cycle costs than the HEU design. Use of these fuels with the uranium densities considered requires that they are successfully demonstrated and licensed. All safety criteria for the reactor with these fuel element designs need to be satisfied as well. With LEU oxide fuel, 31 g U/cm{sup 3} 1 and 0.76 mm--thick fuel meat, elements with 18-22 plates 320-391 g {sup 235}U) result in the same or lower total costs than with the HEU element 23 plates, 280 g {sup 235}U). Higher LEU loadings (more plates per element) are needed for larger excess reactivity requirements. However, there is little cost advantage to using more than 20 of these plates per element. Increasing the fuel meat thickness from 0.76 mm to 1.0 mm with 3.1 g U/cm{sup 3} in the design with 20 plates per element could result in significant cost reductions if the

  7. Palladium-Catalyzed Asymmetric Quaternary Stereocenter Formation

    NARCIS (Netherlands)

    Gottumukkala, Aditya L.; Matcha, Kiran; Lutz, Martin; de Vries, Johannes G.; Minnaard, Adriaan J.

    2012-01-01

    An efficient palladium catalyst is presented for the formation of benzylic quaternary stereocenters by conjugate addition of arylboronic acids to a variety of beta,beta-disubstituted carbocyclic, heterocyclic, and acyclic enones. The catalyst is readily prepared from PdCl2, PhBOX, and AgSbF6, and

  8. Palladium-catalyzed asymmetric quaternary stereocenter formation

    NARCIS (Netherlands)

    Gottumukkala, A.L.; Matcha, K.; Lutz, M.; de Vries, J.G.; Minnaard, A.J.

    2012-01-01

    An efficient palladium catalyst is presented for the formation of benzylic quaternary stereocenters by conjugate addition of arylboronic acids to a variety of β,β-disubstituted carbocyclic, heterocyclic, and acyclic enones. The catalyst is readily prepared from PdCl2, PhBOX, and AgSbF6, and provides

  9. Prediction of barrier inhomogeneities and carrier transport in Ni-silicided Schottky diode

    International Nuclear Information System (INIS)

    Saha, A.R.; Dimitriu, C.B.; Horsfall, A.B.; Chattopadhyay, S.; Wright, N.G.; O'Neill, A.G.; Maiti, C.K.

    2006-01-01

    Based on Quantum Mechanical (QM) carrier transport and the effects of interface states, a theoretical model has been developed to predict the anomalous current-voltage (I-V) characteristics of a non-ideal Ni-silicided Schottky diode at low temperatures. Physical parameters such as barrier height, ideality factor, series resistance and effective Richardson constant of a silicided Schottky diode were extracted from forward I-V characteristics and are subsequently used for the simulation of both forward and reverse I-V characteristics using a QM transport model in which the effects of interface state and bias dependent barrier reduction are incorporated. The present analysis indicates that the effects of barrier inhomogeneity caused by incomplete silicide formation at the junction and the interface states may change the conventional current transport process, leading to anomalous forward and reverse I-V characteristics for the Ni-silicided Schottky diode

  10. NMOS contact resistance reduction with selenium implant into NiPt silicide

    Science.gov (United States)

    Rao, K. V.; Khaja, F. A.; Ni, C. N.; Muthukrishnan, S.; Darlark, A.; Lei, J.; Peidous, I.; Brand, A.; Henry, T.; Variam, N.; Erokhin, Y.

    2012-11-01

    A 25% reduction in NMOS contact resistance (Rc) was achieved by Selenium implantation into NiPt silicide film in VIISta Trident high-current single-wafer implanter. The Trident implanter is designed for shallow high-dose implants with high beam currents to maintain high throughput (for low CoO), with improved micro-uniformity and no energy contamination. The integration of Se implant was realized using a test chip dedicated to investigating silicide/junction related electrical properties and testable after silicidation. The silicide module processes were optimized, including the pre-clean (prior to RF PVD NiPt dep) and pre- and post-implant anneals. A 270°C soak anneal was used for RTP1, whereas a msec laser anneal was employed for RTP2 with sufficient process window (800-850°C), while maintaining excellent junction characteristics without Rs degradation.

  11. Further data of silicide fuel for the LEU conversion of JMTR

    International Nuclear Information System (INIS)

    Saito, M.; Futamura, Y.; Nakata, H.; Ando, H.; Sakurai, F.; Ooka, N.; Sakakura, A.; Ugajin, M.; Shirai, E.

    1990-01-01

    Silicide fuel data for the safety assessment of the JMTR LEU fuel conversion are being measured. The data include fission product release, thermal properties, behaviour under accident conditions, and metallurgical characteristics. The methods used in the experiments are discussed. Results of fission products release at high temperature are described. The release of iodine from the silicide fuel is considerably lower than for U-Al alloy fuel

  12. Evaluation of the oxide and silicide fuels reactivity in the RSG-GAS core

    International Nuclear Information System (INIS)

    S, Tukiran; M S, Tagor; S, Lily; Pinem, S.

    2000-01-01

    Fuel exchange of The RSG-GAS reactor core from uranium oxide to uranium silicide in the same loading, density, and enrichment, that is, 250 gr, 2.98 gr/cm 3 , and 19.75 % respectively, will be performed in-step wise. In every cycle of exchange with 5/l mode, it is needed to evaluate the parameter of reactor core operation. One of the important operation parameters is fuel reactivity that gives effect to the core reactivity. The experiment was performed at core no. 36, BOC, low power which exist 2 silicide fuels. The evaluation was done based on the RSG-GAS control rod calibration consisting of 40 fuels and 8 control rod.s. From 40 fuels in the core, there are 2 silicide fuels, RI-225/A-9 and RI-224/C-3. For inserting 2 silicide fuels, the reactivity effect to the core must be know. To know this effect , it was performed fuels reactivity experiment, which based on control rod calibration. But in this case the RSG-GAS has no other fresh oxide fuel so that configuration of the RSG-GAS core was rearranged by taking out the both silicide fuels and this configuration is used as reference core. Then silicide fuel RI-224 was inserted to position F-3 replacing the fresh oxide fuel RI-260 so the different reactivity of the fuels is obtained. The experiment result showed that the fuel reactivity change is in amount of 12.85 cent (0.098 % ) The experiment result was compared to the calculation result, using IAFUEL code which amount to 13.49 cent (0.103 %) The result showed that the reactivity change of oxide to silicide fuel is small so that the fuel exchange from uranium oxide to uranium silicide in the first step can be done without any significant change of the operation parameter

  13. Information for irradiation and post-irradiation of the silicide fuel element prototype P-07

    International Nuclear Information System (INIS)

    Abbate, Maximo J.; Sbaffoni, Maria M.

    2003-01-01

    Included in the 'Silicides' Project, developed by the Nuclear Fuels Department of the National Atomic Energy Commission (CNEA), it is foreseen the qualification of this type of fuel for research reactors in order to be used in the Argentine RA-3 reactor and to confirm the CNEA as an international supplier. The paper presents basic information on several parameters corresponding to the new silicide prototype, called P-07, to be taken into account for its irradiation, postirradiation and qualification. (author)

  14. Thermoelectric characteristics of Pt-silicide/silicon multi-layer structured p-type silicon

    International Nuclear Information System (INIS)

    Choi, Wonchul; Jun, Dongseok; Kim, Soojung; Shin, Mincheol; Jang, Moongyu

    2015-01-01

    Electric and thermoelectric properties of silicide/silicon multi-layer structured devices were investigated with the variation of silicide/silicon heterojunction numbers from 3 to 12 layers. For the fabrication of silicide/silicon multi-layered structure, platinum and silicon layers are repeatedly sputtered on the (100) silicon bulk substrate and rapid thermal annealing is carried out for the silicidation. The manufactured devices show ohmic current–voltage (I–V) characteristics. The Seebeck coefficient of bulk Si is evaluated as 195.8 ± 15.3 μV/K at 300 K, whereas the 12 layered silicide/silicon multi-layer structured device is evaluated as 201.8 ± 9.1 μV/K. As the temperature increases to 400 K, the Seebeck coefficient increases to 237.2 ± 4.7 μV/K and 277.0 ± 1.1 μV/K for bulk and 12 layered devices, respectively. The increase of Seebeck coefficient in multi-layered structure is mainly attributed to the electron filtering effect due to the Schottky barrier at Pt-silicide/silicon interface. At 400 K, the thermal conductivity is reduced by about half of magnitude compared to bulk in multi-layered device which shows the efficient suppression of phonon propagation by using Pt-silicide/silicon hetero-junctions. - Highlights: • Silicide/silicon multi-layer structured is proposed for thermoelectric devices. • Electric and thermoelectric properties with the number of layer are investigated. • An increase of Seebeck coefficient is mainly attributed the Schottky barrier. • Phonon propagation is suppressed with the existence of Schottky barrier. • Thermal conductivity is reduced due to the suppression of phonon propagation

  15. Kinetics of nickel silicide growth in silicon nanowires: From linear to square root growth

    International Nuclear Information System (INIS)

    Yaish, Y. E.; Beregovsky, M.; Katsman, A.; Cohen, G. M.

    2011-01-01

    The common practice for nickel silicide formation in silicon nanowires (SiNWs) relies on axial growth of silicide along the wire that is initiated from nickel reservoirs at the source and drain contacts. In the present work the silicide intrusions were studied for various parameters including wire diameter (25-50 nm), annealing time (15-120 s), annealing temperature (300-440 deg. C), and the quality of the initial Ni/Si interface. The silicide formation was investigated by high-resolution scanning electron microscopy, high-resolution transmission electron microscopy (TEM), and atomic force microscopy. The main part of the intrusion formed at 420 deg. C consists of monosilicide NiSi, as was confirmed by energy dispersive spectroscopy STEM, selected area diffraction TEM, and electrical resistance measurements of fully silicided SiNWs. The kinetics of nickel silicide axial growth in the SiNWs was analyzed in the framework of a diffusion model through constrictions. The model calculates the time dependence of the intrusion length, L, and predicts crossover from linear to square root time dependency for different wire parameters, as confirmed by the experimental data.

  16. Attempt to produce silicide fuel elements in Indonesia

    International Nuclear Information System (INIS)

    Soentono, S.; Suripto, A.

    1991-01-01

    After the successful experiment to produce U 3 Si 2 powder and U 3 Si 2 -Al fuel plates using depleted U and Si of semiconductor quality, silicide fuel was synthesized using x -Al available at the Fuel Element Production Installation (FEPI) at Serpong, Indonesia. Two full-size U 3 Si 2 -Al fuel elements, having similar specifications to the ones of U 3 O 8 -Al for the RSG-GAS (formerly known as MPR-30), have been produced at the FEPI. All quality controls required have been imposed to the feeds, intermediate, as well as final products throughout the production processes of the two fuel elements. The current results show that these fuel elements are qualified from fabrication point of view, therefore it is expected that they will be permitted to be tested in the RSG-GAS, sometime by the end of 1989, for normal (∝50%) and above normal burn-up. (orig.)

  17. Status of the atomized uranium silicide fuel development at KAERI

    Energy Technology Data Exchange (ETDEWEB)

    Kim, C.K.; Kim, K.H.; Park, H.D.; Kuk, I.H. [Korea Atomic Energy Research Institute, Taejon (Korea, Republic of)

    1997-08-01

    While developing KMRR fuel fabrication technology an atomizing technique has been applied in order to eliminate the difficulties relating to the tough property of U{sub 3}Si and to take advantage of the rapid solidification effect of atomization. The comparison between the conventionally comminuted powder dispersion fuel and the atomized powder dispersion fuel has been made. As the result, the processes, uranium silicide powdering and heat treatment for U{sub 3}Si transformation, become simplified. The workability, the thermal conductivity and the thermal compatibility of fuel meat have been investigated and found to be improved due to the spherical shape of atomized powder. In this presentation the overall developments of atomized U{sub 3}Si dispersion fuel and the planned activities for applying the atomizing technique to the real fuel fabrication are described.

  18. Characterization of tungsten silicides formed by rapid thermal annealing

    International Nuclear Information System (INIS)

    Siegal, M.; Santiago, J.J.; VanDerSpiegel, J.

    1986-01-01

    Tungsten silicide samples were formed by sputter depositing 80 nm W metal onto (100) oriented, 5 ohm-cm Si wafers. After deposition, the samples were fast radiatively processed in an RTA system using quartz-halogen tungsten lamps as radiation sources for time intervals ranging from 20 to 60s under high vacuum. Films processed at 22-25 W/cm 2 radiation with the film side of the samples oriented away from the lamps result in films which are metallic or cloudy in color, and have mixed composition as evidenced by x-ray diffraction (W, W 5 Si 3 and WSi 2 ). Films processed with the film side oriented toward the lamps show the occurrence of a phase transformation clearly nucleated at the film edge

  19. Development of molecular dynamics potential for uranium silicide fuels

    Energy Technology Data Exchange (ETDEWEB)

    Yu, Jianguo; Zhang, Yongfeng; Hales, Jason D.

    2016-09-01

    Use of uranium–silicide (U-Si) in place of uranium dioxide (UO2) is one of the promising concepts being proposed to increase the accident tolerance of nuclear fuels. This is due to a higher thermal conductivity than UO2 that results in lower centerline temperatures. U-Si also has a higher fissile density, which may enable some new cladding concepts that would otherwise require increased enrichment limits to compensate for their neutronic penalty. However, many critical material properties for U-Si have not been determined experimentally. For example, silicide compounds (U3Si2 and U3Si) are known to become amorphous under irradiation. There was clear independent experimental evidence to support a crystalline to amorphous transformation in those compounds. However, it is still not well understood how the amorphous transformation will affect on fuel behavior. It is anticipated that modeling and simulation may deliver guidance on the importance of various properties and help prioritize experimental work. In order to develop knowledge-based models for use at the engineering scale with a minimum of empirical parameters and increase the predictive capabilities of the developed model, inputs from atomistic simulations are essential. First-principles based density functional theory (DFT) calculations will provide the most reliable information. However, it is probably not possible to obtain kinetic information such as amorphization under irradiation directly from DFT simulations due to size and time limitations. Thus, a more feasible way may be to employ molecular dynamics (MD) simulation. Unfortunately, so far no MD potential is available for U-Si to discover the underlying mechanisms. Here, we will present our recent progress in developing a U-Si potential from ab initio data. This work is supported by the Nuclear Energy Advanced Modeling and Simulation (NEAMS) program funded by the U.S. Department of Energy, Office of Nuclear Energy.

  20. Nickel silicide thin films as masking and structural layers for silicon bulk micro-machining by potassium hydroxide wet etching

    International Nuclear Information System (INIS)

    Bhaskaran, M; Sriram, S; Sim, L W

    2008-01-01

    This paper studies the feasibility of using titanium and nickel silicide thin films as mask materials for silicon bulk micro-machining. Thin films of nickel silicide were found to be more resistant to wet etching in potassium hydroxide. The use of nickel silicide as a structural material, by fabricating micro-beams of varying dimensions, is demonstrated. The micro-structures were realized using these thin films with wet etching using potassium hydroxide solution on (1 0 0) and (1 1 0) silicon substrates. These results show that nickel silicide is a suitable alternative to silicon nitride for silicon bulk micro-machining

  1. Dendritic surface morphology of palladium hydride produced by electrolytic deposition

    International Nuclear Information System (INIS)

    Julin, Peng; Bursill, L.A.

    1990-01-01

    Conventional and high-resolution electron microscopic studies of electrolytically-deposited palladium hydride reveal a fascinating variety of surface profile morphologies. The observations provide direct information concerning the surface structure of palladium electrodes and the mechanism of electrolytic deposition of palladium black. Both classical electrochemical mechanisms and recent 'modified diffusion-limited-aggregation' computer simulations are discussed in comparison with the experimental results. 13 refs., 9 figs

  2. Adsorption of palladium ions by modified carbons from rice husks

    International Nuclear Information System (INIS)

    Mostafa, M.R.

    1994-01-01

    Steam activated carbon of high surface area does not show palladium ions adsorption. Treatment of this carbon with HF acid increases to a great extent the gas adsorption capacity expressed as nitrogen surface area as well as the adsorption capacity of palladium ions from aqueous solution. HHB was loaded in different amounts on to these carbons. The acid sites represent the active fraction of the surface on which the adsorption palladium ions proceed. The uptake of palladium ions by HHB treated carbons is related to the total number of HHB molecules loaded on the carbon surface. (author)

  3. Development of Separation Materials Containing Palladium for Hydrogen Isotopes Separation

    International Nuclear Information System (INIS)

    Deng Xiaojun; Luo Deli; Qian Xiaojing

    2010-01-01

    Displacement chromatography (DC) is a ascendant technique for hydrogen isotopes separation. The performance of separation materials is a key factor to determine the separation effect of DC. At present,kinds of materials are researched, including palladium materials and non-palladium materials. It is hardly replaceable because of its excellent separation performance, although palladium is expensive. The theory of hydrogen isotopes separation using DC was introduced at a brief manner, while several palladium separation materials were expatiated in detail(Pd/K, Pd-Al 2 O 3 , Pd-Pt alloy). Development direction of separation materials for DC was forecasted elementarily. (authors)

  4. Functionalized Palladium Nanoparticles for Hydrogen Peroxide Biosensor

    Directory of Open Access Journals (Sweden)

    H. Baccar

    2011-01-01

    Full Text Available We present a comparison between two biosensors for hydrogen peroxide (H2O2 detection. The first biosensor was developed by the immobilization of Horseradish Peroxidase (HRP enzyme on thiol-modified gold electrode. The second biosensor was developed by the immobilization of cysteamine functionalizing palladium nanoparticles on modified gold surface. The amino groups can be activated with glutaraldehyde for horseradish peroxidase immobilization. The detection of hydrogen peroxide was successfully observed in PBS for both biosensors using the cyclic voltammetry and the chronoamperometry techniques. The results show that the limit detection depends on the large surface-to-volume ratio attained with palladium nanoparticles. The second biosensor presents a better detection limit of 7.5 μM in comparison with the first one which is equal to 75 μM.

  5. Oxygen isotope exchange on palladium catalysts

    International Nuclear Information System (INIS)

    Kravchuk, L.S.; Beschetvertnaya, T.I.; Novorodskij, V.G.; Novikova, M.G.; Zaretskij, M.V.; Valieva, S.V.

    1983-01-01

    Oxygen heteromolecular isotope exchange on unreduced palladium catalysts, distingushing by metal content is studied. Content of 18 O in gaseous phase is eoual to 46%. Calculations of heteroexchange rates are conducted with decrease of the 18 O in the gaseous phase over solid sample. Method of oxygen thermodesorption has been used to establish that palladium, deposited on γ-Al 2 O 3 during exchange process is in oxidized state; in this case strength of Pd-O bond is determined by content dispersity) of the metal. It is shown that significant increase of exchange rate on the samples with Pd >> 0.5 mass.% content can be induced as by side decomposition reaction of its oxide and corresponding dilution of gaseous mixture by ''light'' oxygen so by possibility of exchange with oxygen of PdO phase

  6. Technology CAD of silicided Schottky barrier MOSFET for elevated source-drain engineering

    International Nuclear Information System (INIS)

    Saha, A.R.; Chattopadhyay, S.; Bose, C.; Maiti, C.K.

    2005-01-01

    Technology CAD has been used to study the performance of a silicided Schottky barrier (SB) MOSFET with gate, source and drain contacts realized with nickel-silicide. Elevated source-drain structures have been used towards the S/D engineering of CMOS devices. A full process-to-device simulation has been employed to predict the performance of sub-micron SB n-MOSFETs for the first time. A model for the diffusion and alloy growth kinetics has been incorporated in SILVACO-ATLAS and ATHENA to explore the processing and design parameter space for the Ni-silicided MOSFETs. The temperature and concentration dependent diffusion model for NiSi have been developed and necessary material parameters for nickel-silicide and epitaxial-Si have been incorporated through the C-interpreter function. Two-dimensional (2D) process-to-device simulations have also been used to study the dc and ac (RF) performance of silicided Schottky barrier (SB) n-MOSFETs. The extracted sheet resistivity, as a function of annealing temperature of the silicided S/D contacts, is found to be lower than the conventional contacts currently in use. It is also shown that the Technology CAD has the full capability to predict the possible dc and ac performance enhancement of a MOSFET with elevated S/D structures. While the simulated dc performance shows a clear enhancement, the RF analyses show no performance degradation in the cut-off frequency/propagation delay and also improve the ac performance due to the incorporation of silicide contacts in the S/D region

  7. Technology CAD of silicided Schottky barrier MOSFET for elevated source-drain engineering

    Energy Technology Data Exchange (ETDEWEB)

    Saha, A.R. [Department of Electronics and ECE, IIT, Kharagpur 721302 (India)]. E-mail: ars.iitkgp@gmail.com; Chattopadhyay, S. [Department of Electronics and ECE, IIT, Kharagpur 721302 (India); School of Electrical, Electronics and Computer Engineering, University of Newcastle, Newcastle upon Tyne (United Kingdom); Bose, C. [Department of Electronics and Telecommunication Engineering, Jadavpur University, Calcutta 700032 (India); Maiti, C.K. [Department of Electronics and ECE, IIT, Kharagpur 721302 (India)

    2005-12-05

    Technology CAD has been used to study the performance of a silicided Schottky barrier (SB) MOSFET with gate, source and drain contacts realized with nickel-silicide. Elevated source-drain structures have been used towards the S/D engineering of CMOS devices. A full process-to-device simulation has been employed to predict the performance of sub-micron SB n-MOSFETs for the first time. A model for the diffusion and alloy growth kinetics has been incorporated in SILVACO-ATLAS and ATHENA to explore the processing and design parameter space for the Ni-silicided MOSFETs. The temperature and concentration dependent diffusion model for NiSi have been developed and necessary material parameters for nickel-silicide and epitaxial-Si have been incorporated through the C-interpreter function. Two-dimensional (2D) process-to-device simulations have also been used to study the dc and ac (RF) performance of silicided Schottky barrier (SB) n-MOSFETs. The extracted sheet resistivity, as a function of annealing temperature of the silicided S/D contacts, is found to be lower than the conventional contacts currently in use. It is also shown that the Technology CAD has the full capability to predict the possible dc and ac performance enhancement of a MOSFET with elevated S/D structures. While the simulated dc performance shows a clear enhancement, the RF analyses show no performance degradation in the cut-off frequency/propagation delay and also improve the ac performance due to the incorporation of silicide contacts in the S/D region.

  8. Extracellular Palladium Nanoparticle Production using Geobacter sulfurreducens

    KAUST Repository

    Yates, Matthew D.

    2013-09-03

    Sustainable methods are needed to recycle precious metals and synthesize catalytic nanoparticles. Palladium nanoparticles can be produced via microbial reduction of soluble Pd(II) to Pd(0), but in previous tests using dissimilatory metal reducing bacteria (DMRB), the nanoparticles were closely associated with the cells, occupying potential reductive sites and eliminating the potential for cell reuse. The DMRB Geobacter sulfurreducens was shown here to reduce soluble Pd(II) to Pd(0) nanoparticles primarily outside the cell, reducing the toxicity of metal ions, and allowing nanoparticle recovery without cell destruction that has previously been observed using other microorganisms. Cultures reduced 50 ± 3 mg/L Pd(II) with 1% hydrogen gas (v/v headspace) in 6 h incubation tests [100 mg/L Pd(II) initially], compared to 8 ± 3 mg/L (10 mM acetate) without H2. Acetate was ineffective as an electron donor for palladium removal in the presence or absence of fumarate as an electron acceptor. TEM imaging verified that Pd(0) nanoparticles were predominantly in the EPS surrounding cells in H2-fed cultures, with only a small number of particles visible inside the cell. Separation of the cells and EPS by centrifugation allowed reuse of the cell suspensions and effective nanoparticle recovery. These results demonstrate effective palladium recovery and nanoparticle production using G. sulfurreducens cell suspensions and renewable substrates such as H2 gas. © 2013 American Chemical Society.

  9. Reclamation and reuse of LEU silicide fuel from manufacturing scrap

    International Nuclear Information System (INIS)

    Gale, G.R.; Pace, B.W.; Evans, R.S.

    2004-01-01

    In order to provide an understanding of the organization which is the sole supplier of United States plate type research and test reactor fuel and LEU core conversions, a brief description of the structure and history is presented. Babcock and Wilcox (B and W) is a part of McDermott International, Inc. which is a large diversified corporation employing over 20,000 people primarily in engineering and construction for the off-shore oil and power generation industries throughout the world. B and W provides many energy related products requiring precision machining and high quality systems. This is accomplished by using state-of-the-art equipment, technology and highly skilled people. The RTRFE group within B and W has the ability to produce various complexly shaped fuel elements with a wide variety of fuels and enrichments. B and W RTRFE has fabricated over 200,000 plates since 1981 and gained the diversified experience necessary to satisfy many customer requirements. This accomplishment was possible with the support of McDermott International and all of its resources. B and W has always had a commitment to high quality and integrity. This is apparent by the success and longevity (125 years) of the company. A lower cost to convert cores to LEU provides direct support to RERTR and demonstrates Babcock and Wilcox's commitment to the program. As a supporter of RERTR reactor conversion from HEU to LEU, B and W has contributed a significant amount of R and D money to improve the silicide fuel process which ultimately lowers the LEU core costs. In the most recent R and D project, B and W is constructing a LEU silicide reclamation facility to re-use the unirradiated fuel scrap generated from the production process. Remanufacturing use of this fuel completes the fuel cycle and provides a contribution to LEU cores by reducing scrap inventory and handling costs, lowering initial purchase of fuel due to increasing the process yields, and lowering the replacement costs. This

  10. Capacitance-voltage characterization of fully silicided gated MOS capacitor

    International Nuclear Information System (INIS)

    Wang Baomin; Ru Guoping; Jiang Yulong; Qu Xinping; Li Bingzong; Liu Ran

    2009-01-01

    This paper investigates the capacitance-voltage (C-V) measurement on fully silicided (FUSI) gated metal-oxide-semiconductor (MOS) capacitors and the applicability of MOS capacitor models. When the oxide leakage current of an MOS capacitor is large, two-element parallel or series model cannot be used to obtain its real C-V characteristic. A three-element model simultaneously consisting of parallel conductance and series resistance or a four-element model with further consideration of a series inductance should be used. We employed the three-element and the four-element models with the help of two-frequency technique to measure the Ni FUSI gated MOS capacitors. The results indicate that the capacitance of the MOS capacitors extracted by the three-element model still shows some frequency dispersion, while that extracted by the four-element model is close to the real capacitance, showing little frequency dispersion. The obtained capacitance can be used to calculate the dielectric thickness with quantum effect correction by NCSU C-V program. We also investigated the influence of MOS capacitor's area on the measurement accuracy. The results indicate that the decrease of capacitor area can reduce the dissipation factor and improve the measurement accuracy. As a result, the frequency dispersion of the measured capacitance is significantly reduced, and real C-V characteristic can be obtained directly by the series model. In addition, this paper investigates the quasi-static C-V measurement and the photonic high-frequency C-V measurement on Ni FUSI metal gated MOS capacitor with a thin leaky oxide. The results indicate that the large tunneling current through the gate oxide significantly perturbs the accurate measurement of the displacement current, which is essential for the quasi-static C-V measurement. On the other hand, the photonic high-frequency C-V measurement can bypass the leakage problem, and get reliable low-frequency C-V characteristic, which can be used to

  11. Microstructure and mechanical properties of metal/oxide and metal/silicide interfaces

    International Nuclear Information System (INIS)

    Shaw, L.; Miracle, D.; Abbaschian, R.

    1995-01-01

    Fracture energies of Al 2 O 3 /Nb interfaces and MoSi 2 /Nb interfaces with and without Al 2 O 3 coating were measured using sandwich-type chevron-notched specimens. The relations between the mechanical properties, microstructures, types of bonds at the interface and processing routes were explored. The fracture energy of the Al 2 O 3 /Nb interface was determined to be 9 J/m 2 and changed to 16 J/m 2 when Nb was pre-oxidized before the formation of the Al 2 O 3 /Nb interface. The fracture energy of the MoSi 2 /Nb interface could not be determined directly because of the formation of the interfacial compounds. However, the fracture energy at the MoSi 2 /Nb interfacial region was found to depend on the interfacial bond strength, roughness of interfaces and microstructure of interfacial compounds. The interfacial fracture energies of Al 2 O 3 with silicides, MoSi 2 , Nb 5 Si 3 , or (Nb, Mo)Si 2 were estimated to be about 16 J/m 2 , while the interfacial fracture energies between two silicides or between Nb and a silicide were larger than 34 J/m 2 . The measured fracture energies between two silicides or between Nb and a silicide were larger than 34 J/m 2 . The measured fracture energies of the various interfaces are discussed in terms of the interfacial microstructures and types of bonds at the interfaces

  12. Improvement of Silicide Coating Method as Diffusion Barrier for U-Mo Dispersion Fuel

    Energy Technology Data Exchange (ETDEWEB)

    Nam, Ji Min; Kim, Sunghwan; Lee, Kyu Hong; Park, Jong Man [Korea Atomic Energy Research Institute, Daejeon (Korea, Republic of)

    2014-10-15

    The excessive interaction between the U-Mo alloys and their surrounding Al matrix lead to excessive local swelling called 'pillowing'. For this reason, KAERI suggested several remedies such as alloying U-Mo with Ti, or Al matrix with Si. In addition, silicide or nitride coatings on the surface of U-Mo particles have also been proposed to hinder the growth of the interaction layer. In this study, centrifugally atomized U-Mo-Ti alloy powders were coated with silicide layers. The coating process was improved when compared to the previous coating in terms of the ball milling and heat treatment conditions. Subsequently, silicide coated U-Mo-Ti powders and pure aluminum powders were mixed and made into a compact for the annealing test. The compacts were annealed at 550 .deg. C for 2hr, and characterized using scanning electron microscopy (SEM) and energy dispersive x-ray spectroscopy (EDS). 1. Uniform, homogeneous, thickness controllable silicide layers were successfully coated on the surface of U-7wt%Mo-1wt%Ti powders. 2. U{sub 3}Si, U{sub 3}Si{sub 2} silicide layers formed on the surface of U-7wt%Mo-1wt%Ti powders, and were identified by XRD and EDS analyses.

  13. Synthesis of molybdenum borides and molybdenum silicides in molten salts and their oxidation behavior in an air-water mixture

    NARCIS (Netherlands)

    Kuznetsov, S.A.; Kuznetsova, S.V.; Rebrov, E.V.; Mies, M.J.M.; Croon, de M.H.J.M.; Schouten, J.C.

    2005-01-01

    The formation of various coatings in molybdenum-boron and molybdenum-silicon systems was investigated. Boronizing and siliciding treatments were conducted in molten salts under inert gas atm. in the 850-1050 DegC temp. range for 7 h. The presence of boride (e.g. Mo2B, MoB, Mo2B5) and silicide

  14. Neutronic design of mixed oxide-silicide cores for the core conversion of rsg-gas reactor

    International Nuclear Information System (INIS)

    Sembiring, Tagor Malem; Tukiran; Pinem surian; Febrianto

    2001-01-01

    The core conversion of rsg-gas reactor from an all-oxide (U 3 O 8 -Al) core, through a series of mixed oxide-silicide core, to an all-silicide (U 3 Si 2 -Al) core for the same meat density of 2.96 g U/cc is in progress. The conversion is first step of the step-wise conversion and will be followed by the second step that is the core conversion from low meat density of silicide core, through a series of mixed lower-higher density of silicide core, to an all-higher meat density of 3.55 g/cc core. Therefore, the objectives of this work is to design the mixed cores on the neutronic performance to achieve safety a first full-silicide core for the reactor with the low uranium meat density of 2.96gU/cc. The neutronic design of the mixed cores was performed by means of Batan-EQUIL-2D and Batan-3DIFF computer codes for 2 and 3 dimension diffusion calculation, respectively. The result shows that all mixed oxide-silicide cores will be feasible to achieve safety a fist full-silicide core. The core performs the same neutronic core parameters as those of the equilibrium silicide core. Therefore, the reactor availability and utilization during the core conversion is not changed

  15. Thermosonic wire bonding of IC devices using palladium wire

    International Nuclear Information System (INIS)

    Shze, J.H.; Poh, M.T.; Tan, R.M.

    1996-01-01

    The feasibility of replacing gold wire by palladium wire in thermosonic wire bonding of CMOS and bipolar devices are studied in terms of the manufacturability, physical, electrical and assembly performance. The results that palladium wire is a viable option for bonding the bipolar devices but not the CMOS devices

  16. Thermodynamics of the hybrid interaction of hydrogen with palladium nanoparticles

    NARCIS (Netherlands)

    Griessen, R.P.; Strohfeldt, N.; Giessen, H.

    2015-01-01

    Palladium-hydrogen is a prototypical metal-hydrogen system. It is therefore not at all surprising that a lot of attention has been devoted to the absorption and desorption of hydrogen in nanosized palladium particles. Several seminal articles on the interaction of H with Pd nanocubes and

  17. Nanoscale investigation of the interface situation of plated nickel and thermally formed nickel silicide for silicon solar cell metallization

    Energy Technology Data Exchange (ETDEWEB)

    Mondon, A., E-mail: andrew.mondon@ise.fraunhofer.de [Fraunhofer ISE, Heidenhofst. 2, D-79110 Freiburg (Germany); Wang, D. [Karlsruhe Nano Micro Facility (KNMF), H.-von-Helmholz-Platz 1, D-76344 Eggenstein-Leopoldshafen (Germany); Zuschlag, A. [Universität Konstanz FB Physik, Jacob-Burckhardt-Str. 27, D-78464 Konstanz (Germany); Bartsch, J.; Glatthaar, M.; Glunz, S.W. [Fraunhofer ISE, Heidenhofst. 2, D-79110 Freiburg (Germany)

    2014-12-30

    Highlights: • Adhesion of metallization of fully plated nickel–copper contacts on silicon solar cells can be achieved by formation of nickel silicide at the cost of degraded cell performance. • Understanding of silicide growth mechanisms and controlled growth may lead to high performance together with excellent adhesion. • Silicide formation is well known from CMOS production from PVD-Ni on flat surfaces. Yet the deposition methods and therefore layer characteristics and the surface topography are different for plated metallization. • TEM analysis is performed for differently processed samples. • A nickel silicide growth model is created for plated Ni on textured silicon solar cells. - Abstract: In the context of nickel silicide formation from plated nickel layers for solar cell metallization, there are several open questions regarding contact adhesion and electrical properties. Nanoscale characterization by transmission electron microscopy has been employed to support these investigations. Interfacial oxides and silicide phases were investigated on differently prepared samples by different analytical methods associated with transmission electron microscopy analysis. Processing variations included the pre-treatment of samples before nickel plating, the used plating solution and the thermal budget for the nickel–silicon solid-state reaction. It was shown that interface oxides of only few nm thickness on both silicon and nickel silicide are present on the samples, depending on the chosen process sequence, which have been shown to play an important role in adhesion of nickel on silicide in an earlier publication. From sample pretreatment variations, conclusions about the role of an interfacial oxide in silicide formation and its influence on phase formation were drawn. Such an oxide layer hinders silicide formation except for pinhole sites. This reduces the availability of Ni and causes a silicide with low Ni content to form. Without an interfacial oxide

  18. Irradiation of an uranium silicide prototype in RA-3 reactor

    International Nuclear Information System (INIS)

    Calabrese, R.; Estrik, G.; Notari, C.

    1996-01-01

    The factibility of irradiation of an uranium silicide (U 3 Si 2 ) prototype in the RA-3 reactor was studied. The standard RA-3 fuel element uses U 3 O 8 as fissible material. The enrichment of both standard and prototype is the same: 20% U 235 and also the frame geometry and number of plates is identical. The differences are in the plate dimensions and the fissile content which is higher in the prototype. The cooling conditions of the core allow the insertion of the prototype in any core position, even near the water trap, if the overall power is kept below 5Mw. Nevertheless, the recommendation was to begin irradiation near the periphery and later on move the prototype towards more central positions in order to increase the burnup rate. The prototype was effectively introduced in a peripheral position and the thermal fluxes were measured between plates with the foil activation technique. These were also evaluated with the fuel management codes and a reasonable agreement was found. (author). 5 refs., 3 figs., 3 tabs

  19. Milling uranium silicide powder for dispersion nuclear fuels

    Energy Technology Data Exchange (ETDEWEB)

    Vieira, E.; Silva, D.G.; Souza, J.A.B.; Durazzo, M. [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil); Riella, H.G. [Universidade Federal de Santa Catarina (UFSC), Florianopolis, SC (Brazil)

    2009-07-01

    Full text: Uranium silicide (U3Si2) is presently considered the best fuel qualified so far in terms of uranium loading and performance. Stability of the U3Si2 fuel with uranium density of 4.8 g/cm3 was confirmed by burnup stability tests performed during the Reduced Enrichment for Research and Test Reactors (RERTR) program. This fuel was chosen to compose the first core of the new Brazilian Multipurpose Research Reactor (RMB), planned to be constructed in the next years. This new reactor will consume bigger quantities of U3Si2 powder, when compared with the small consumption of the IEA-R1 research reactor of IPEN-CNEN/SP, the unique MTR type research reactor operating in the country. At the present time, the milling operation of U3Si2 ingots is made manually. In order to increase the powder production capacity, the manual milling must be replaced by an automated procedure. This paper describes a new milling machine and procedure developed to produce U3Si2 powder with higher efficiency. (author)

  20. Mixing of Al into uranium silicides reactor fuels

    International Nuclear Information System (INIS)

    Ding, F.R.; Birtcher, R.C.; Kestel, B.J.; Baldo, P.M.

    1996-11-01

    SEM observations have shown that irradiation induced interaction of the aluminum cladding with uranium silicide reactor fuels strongly affects both fission gas and fuel swelling behaviors during fuel burn-up. The authors have used ion beam mixing, by 1.5 MeV Kr, to study this phenomena. RBS and the 27 Al(p, γ) 28 Si resonance nuclear reaction were used to measure radiation induced mixing of Al into U 3 Si and U 3 Si 2 after irradiation at 300 C. Initially U mixes into the Al layer and Al mixes into the U 3 Si. At a low dose, the Al layer is converted into UAl 4 type compound while near the interface the phase U(Al .93 Si .07 ) 3 grows. Under irradiation, Al diffuses out of the UAl 4 surface layer, and the lower density ternary, which is stable under irradiation, is the final product. Al mixing into U 3 Si 2 is slower than in U 3 Si, but after high dose irradiation the Al concentration extends much farther into the bulk. In both systems Al mixing and diffusion is controlled by phase formation and growth. The Al mixing rates into the two alloys are similar to that of Al into pure uranium where similar aluminide phases are formed

  1. Simulated Fission Gas Behavior in Silicide Fuel at LWR Conditions

    Energy Technology Data Exchange (ETDEWEB)

    Miao, Yinbin [Argonne National Lab. (ANL), Argonne, IL (United States); Mo, Kun [Argonne National Lab. (ANL), Argonne, IL (United States); Yacout, Abdellatif [Argonne National Lab. (ANL), Argonne, IL (United States); Harp, Jason [Argonne National Lab. (ANL), Argonne, IL (United States)

    2016-09-15

    As a promising candidate for the accident tolerant fuel (ATF) used in light water reactors (LWRs), the fuel performance of uranium silicide (U3Si2) at LWR conditions needs to be well-understood. However, existing experimental post-irradiation examination (PIE) data are limited to the research reactor conditions, which involve lower fuel temperature compared to LWR conditions. This lack of appropriate experimental data significantly affects the development of fuel performance codes that can precisely predict the microstructure evolution and property degradation at LWR conditions, and therefore evaluate the qualification of U3Si2 as an AFT for LWRs. Considering the high cost, long timescale, and restrictive access of the in-pile irradiation experiments, this study aims to utilize ion irradiation to simulate the inpile behavior of the U3Si2 fuel. Both in situ TEM ion irradiation and ex situ high-energy ATLAS ion irradiation experiments were employed to simulate different types of microstructure modifications in U3Si2. Multiple PIE techniques were used or will be used to quantitatively analyze the microstructure evolution induced by ion irradiation so as to provide valuable reference for the development of fuel performance code prior to the availability of the in-pile irradiation data.

  2. Chemical recovery of a palladium-103 from irradiated silver target

    International Nuclear Information System (INIS)

    Lapshina, E.V.; Kokhanyuk, V.M.; Zhuikov, B.L.; Myasoedova, G.V.; Zakhartchenko, E.A.; Phillips, D.R.; Jamriska, D.J.

    2003-01-01

    The goal of this work is to develop an extraction method of no-carrier-added palladium-103 from silver. Metallic silver targets were irradiated by protons with the energy of 60-140 MeV to generate palladium-103. Other radioactive isotopes of rhodium, ruthenium, technetium, palladium and silver are also formed at the same time. Two methods of Pd-103 recovering from irradiated silver target are considered. The first one includes the dissolving of the irradiated silver target in nitric acid followed by adding of hydrochloric acid to the solution. Palladium with rhodium, ruthenium and technetium completely remained in solution while silver was precipitated in the form of silver chloride. Extraction of palladium from the obtained solution was provided by the formation of palladium complex with a chelate sorbent which is specific to palladium in acidic solutions. The sorbent makes it possible to separate palladium from admixtures of rhodium, ruthenium and technetium isotopes. The polymeric complex-forming sorbent of fibrous structure with the groups of 3 (5) - methylpyrazole (POLYORGS-15n) is used. An other possible method has been also studied. It includes again dissolving of metallic silver in nitric acid, but does not need silver chloride precipitation. Silver may be sorbed by the complex-forming sorbents, but its sorption is very sensitive to acid concentration. Chelate sorbents of fibrous structure with the groups of amidoxime and hydrazidine (POLYORGS-33n) have been successfully used in our experiments. A high efficiency of palladium extraction by POLYORGS-33n from 2-4 M nitric acid solutions was achieved. Concentrated hydrochloric acid (without heating) was used for palladium desorption with higher yield than in the first method. (authors)

  3. Nanoscale investigation of the interface situation of plated nickel and thermally formed nickel silicide for silicon solar cell metallization

    Science.gov (United States)

    Mondon, A.; Wang, D.; Zuschlag, A.; Bartsch, J.; Glatthaar, M.; Glunz, S. W.

    2014-12-01

    In the context of nickel silicide formation from plated nickel layers for solar cell metallization, there are several open questions regarding contact adhesion and electrical properties. Nanoscale characterization by transmission electron microscopy has been employed to support these investigations. Interfacial oxides and silicide phases were investigated on differently prepared samples by different analytical methods associated with transmission electron microscopy analysis. Processing variations included the pre-treatment of samples before nickel plating, the used plating solution and the thermal budget for the nickel-silicon solid-state reaction. It was shown that interface oxides of only few nm thickness on both silicon and nickel silicide are present on the samples, depending on the chosen process sequence, which have been shown to play an important role in adhesion of nickel on silicide in an earlier publication. From sample pretreatment variations, conclusions about the role of an interfacial oxide in silicide formation and its influence on phase formation were drawn. Such an oxide layer hinders silicide formation except for pinhole sites. This reduces the availability of Ni and causes a silicide with low Ni content to form. Without an interfacial oxide a continuous nickel silicide of greater depth, polycrystalline modification and expected phase according to thermal budget is formed. Information about the nature of silicide growth on typical solar cell surfaces could be obtained from silicide phase and geometric observations, which were supported by FIB tomography. The theory of isotropic NiSi growth and orientation dependent NiSi2 growth was derived. By this, a very well performing low-cost metallization for silicon solar cells has been brought an important step closer to industrial introduction.

  4. Analysis of impurity effect on Silicide fuels of the RSG-GAS core

    International Nuclear Information System (INIS)

    Tukiran-Surbakti

    2003-01-01

    Simulation of impurity effect on silicide fuel of the RSG-GAS core has been done. The aim of this research is to know impurity effect of the U-234 and U-236 isotopes in the silicide fuels on the core criticality. The silicide fuels of 250 g U loading and 19.75 of enrichment is used in this simulation. Cross section constant of fuels and non-structure material of core are generated by WIMSD/4 computer code, meanwhile impurity concentration was arranged from 0.01% to 2%. From the result of analysis can be concluded that the isotopes impurity in the fuels could make trouble in the core and the core can not be operated at critical after a half of its cycle length (350 MW D)

  5. Self-organized patterns along sidewalls of iron silicide nanowires on Si(110) and their origin

    Energy Technology Data Exchange (ETDEWEB)

    Das, Debolina; Mahato, J. C.; Bisi, Bhaskar; Dev, B. N., E-mail: msbnd@iacs.res.in [Department of Materials Science, Indian Association for the Cultivation of Science, Kolkata 700032 (India); Satpati, B. [Surface Physics and Material Science Division, Saha Institute of Nuclear Physics, 1/AF Bidhannagar, Kolkata 700064 (India)

    2014-11-10

    Iron silicide (cubic FeSi{sub 2}) nanowires have been grown on Si(110) by reactive deposition epitaxy and investigated by scanning tunneling microscopy and scanning/transmission electron microscopy. On an otherwise uniform nanowire, a semi-periodic pattern along the edges of FeSi{sub 2} nanowires has been discovered. The origin of such growth patterns has been traced to initial growth of silicide nanodots with a pyramidal Si base at the chevron-like atomic arrangement of a clean reconstructed Si(110) surface. The pyramidal base evolves into a comb-like structure along the edges of the nanowires. This causes the semi-periodic structure of the iron silicide nanowires along their edges.

  6. Evaluation Of Oxide And Silicide Mixed Fuels Of The RSG-GAS Core

    International Nuclear Information System (INIS)

    Tukiran; Sembiring, Tagor Malem; Suparlina, Lily

    2000-01-01

    Fuel exchange of the RSG-GAS reactor core from uranium oxide to uranium silicide in the same loading, density, and enrichment, that is 250 gr, 2.98 gr/cm 3 , and 19.75%, respectively, will be performed in-step wise. In every cycle of exchange with 5/1 mode, it is needed to evaluate the parameter of reactor core operation. The parameters of the reactor operation observed are criticality mass of fuels, reactivity balance, and fuel reactivity that give effect to the reactor operation. The evaluation was done at beginning of cycle of the first and second transition core with compared between experiment and calculation results. The experiments were performed at transition core I and II, BOC, and low power. At transition core I, there are 2 silicide fuels (RI-224 and R1-225) in the core and then, added five silicide fuels (R1-226, R1-252, R1-263, and R1-264) to the core, so that there are seven silicide fuels in the transition core II. The evaluation was done based on the experiment of criticality, control rod calibration, fuel reactivity of the RSG-GAS transition core. For inserting 2 silicide fuels in the transition core I dan 7 fuels in the transition core II, the operation of RSG-GAS core fulfilled the safety margin and the parameter of reactor operation change is not occur drastically in experiment and calculation results. So that, the reactor was operated during 36 days at 15 MW, 540 MWD at the first transition core. The general result showed that the parameter of reactor operation change is small so that the fuel exchange from uranium oxide to uranium silicide in the next step can be done

  7. A Study on Silicide Coatings as Diffusion barrier for U-7Mo Dispersion Fuel

    Energy Technology Data Exchange (ETDEWEB)

    Won, Ju Jin; Kim, Sung Hwan; Lee, Kyu Hong; Jeong, Yong Jin; Kim, Ki Nam; Park, Jong Man; Lee, Chong Tak [KAERI, Daejeon (Korea, Republic of)

    2016-05-15

    Gamma phase U-Mo alloys are regarded as one of the promising candidates for advanced research reactor fuel when it comes to the irradiation performance. However, it has been reported that interaction layer formation between the UMo alloys and Al matrix degrades the irradiation performance of U-Mo dispersion fuel. The excessive interaction between the U-Mo alloys and their surrounding Al matrix lead to excessive local swelling called 'pillowing'. For this reason, KAERI suggested several remedies such as alloying U-Mo with Al matrix with Si. In addition, silicide or nitride coatings on the surface of U-Mo particles have also been proposed to hinder the growth of the interaction layer. In this study, centrifugally atomized U-7Mo alloy powders were coated with silicide layers at 900 .deg. C for 1hr. U-Mo alloy powder was mixed with MoSi{sub 2}, Si and ZrSi{sub 2} powders and subsequently heat-treated to form uranium-silicide coating layers on the surface of U-Mo alloy particles. Silicide coated U-Mo powders and characterized using scanning electron microscopy (SEM), energy dispersive x-ray spectroscopy (EDS) and X-ray diffractometer (XRD). The ZrSi{sub 2} coating layers has a thickness of about 1∼ 2μm. The surface of a silicide coated particle was very rough and silicide powder attached to the surface of the coating layer. 3. The XRD analysis of the coating layers showed that, they consisted of compounds such as U3Si{sub 2}, USi{sub 2}.

  8. Effects of Silicide Coating on the Interdiffusion between U-7Mo and Al

    Energy Technology Data Exchange (ETDEWEB)

    Nam, Ji Min; Kim, Ji Hyun; Kim, Sunghwan; Lee, Kyu Hong; Park, Jong Man; Jeong, Yong Jin; Kim, Ki Nam [Korea Atomic Energy Research Institute, Daejeon (Korea, Republic of)

    2015-05-15

    The excessive interaction between the U-Mo alloys and their surrounding Al matrix lead to and excessive local swelling called 'pillowing'. For this reason, KAERI suggested several remedies such as alloying U-Mo with Ti, or Al matrix with Si. In addition, silicide, or nitride coatings on the surface of U-Mo particles have also been proposed to hinder the growth of interaction layer. In this study, centrifugally atomized U-7Mo alloy powders were coated with silicide layers at varying T (T = 900 and 1000 .deg. C) for 30 min, respectively. U-Mo alloy powder was blended with Si powders and subsequently heat-treated to form uranium-silicide coating layers on the surface of U-Mo alloy particles. For an annealing test, silicide-coated U-Mo alloy powders were made into a compact, and Al powders were used as a matrix. From EDS results, transformed uranium aluminide intermetallic compounds were mainly U(Al,Si)3. U(Al,Si)3 phase left the silicide coating layer behind, and formed inside of U-7Mo particles, as shown in Fig. 3(a) and (b). In the case of sample B, Al could not penetrate the silicide coating layer and the coating layers were remained constant, as shown in Fig. 3(c) and (d). From the results, we made a comparison between the compacts of sample A and B, and it was shown that Al can easily diffuse into unreacted Si and U{sub 3}Si{sub 5} mixed layer while U{sub 3}Si{sub 2} acted as a good diffusion barrier at 550 .deg. C though those layers had the same thickness.

  9. Effects of Silicide Coating on the Interdiffusion between U-7Mo and Al

    International Nuclear Information System (INIS)

    Nam, Ji Min; Kim, Ji Hyun; Kim, Sunghwan; Lee, Kyu Hong; Park, Jong Man; Jeong, Yong Jin; Kim, Ki Nam

    2015-01-01

    The excessive interaction between the U-Mo alloys and their surrounding Al matrix lead to and excessive local swelling called 'pillowing'. For this reason, KAERI suggested several remedies such as alloying U-Mo with Ti, or Al matrix with Si. In addition, silicide, or nitride coatings on the surface of U-Mo particles have also been proposed to hinder the growth of interaction layer. In this study, centrifugally atomized U-7Mo alloy powders were coated with silicide layers at varying T (T = 900 and 1000 .deg. C) for 30 min, respectively. U-Mo alloy powder was blended with Si powders and subsequently heat-treated to form uranium-silicide coating layers on the surface of U-Mo alloy particles. For an annealing test, silicide-coated U-Mo alloy powders were made into a compact, and Al powders were used as a matrix. From EDS results, transformed uranium aluminide intermetallic compounds were mainly U(Al,Si)3. U(Al,Si)3 phase left the silicide coating layer behind, and formed inside of U-7Mo particles, as shown in Fig. 3(a) and (b). In the case of sample B, Al could not penetrate the silicide coating layer and the coating layers were remained constant, as shown in Fig. 3(c) and (d). From the results, we made a comparison between the compacts of sample A and B, and it was shown that Al can easily diffuse into unreacted Si and U 3 Si 5 mixed layer while U 3 Si 2 acted as a good diffusion barrier at 550 .deg. C though those layers had the same thickness

  10. Formation of copper silicides by high dose metal vapor vacuum arc ion implantation

    International Nuclear Information System (INIS)

    Rong Chun; Zhang Jizhong; Li Wenzhi

    2003-01-01

    Si(1 1 1) was implanted by copper ions with different doses and copper distribution in silicon matrix was obtained. The as-implanted samples were annealed at 300 and 540 deg. C, respectively. Formation of copper silicides in as-implanted and annealed samples were studied. Thermodynamics and kinetics of the reaction were found to be different from reaction at copper-silicon interface that was applied in conventional studies of copper-silicon interaction. The defects in silicon induced by implantation and formation of copper silicides were recognized by Si(2 2 2) X-ray diffraction (XRD)

  11. The influence of alloying on the phase formation sequence of ultra-thin nickel silicide films and on the inheritance of texture

    Science.gov (United States)

    Geenen, F. A.; Solano, E.; Jordan-Sweet, J.; Lavoie, C.; Mocuta, C.; Detavernier, C.

    2018-05-01

    The controlled formation of silicide materials is an ongoing challenge to facilitate the electrical contact of Si-based transistors. Due to the ongoing miniaturisation of the transistor, the silicide is trending to ever-thinner thickness's. The corresponding increase in surface-to-volume ratio emphasises the importance of low-energetic interfaces. Intriguingly, the thickness reduction of nickel silicides results in an abrupt change in phase sequence. This paper investigates the sequence of the silicides phases and their preferential orientation with respect to the Si(001) substrate, for both "thin" (i.e., 9 nm) and "ultra-thin" (i.e., 3 nm) Ni films. Furthermore, as the addition of ternary elements is often considered in order to tailor the silicides' properties, additives of Al, Co, and Pt are also included in this study. Our results show that the first silicide formed is epitaxial θ-Ni2Si, regardless of initial thickness or alloyed composition. The transformations towards subsequent silicides are changed through the additive elements, which can be understood through solubility arguments and classical nucleation theory. The crystalline alignment of the formed silicides with the substrate significantly differs through alloying. The observed textures of sequential silicides could be linked through texture inheritance. Our study illustrates the nucleation of a new phase drive to reduce the interfacial energy at the silicide-substrate interface as well as at the interface with the silicide which is being consumed for these sub-10 nm thin films.

  12. Irradiation behavior of uranium-silicide dispersion fuels

    International Nuclear Information System (INIS)

    Hofman, G.L.; Neimark, L.A.

    1984-01-01

    This paper describes and analyzes the irradiation behavior of experimental fuel plates containing U 3 Si, U 3 Si-1.5 w/o Al, and U 3 Si 2 particulate fuel dispersed and clad in aluminum. The fuel is nominally 19.9%-enriched 235 U and the fuel volume fraction in the central ''meat'' section of the plates is approximately 33%. Sets of fuel plates were removed from the Oak Ridge Research reactor at burnup levels of 35, 83, and 94% 235 U depletion and examined at the Alpha-Gamma Hot-Cell Facility at Argonne National Laboratory. The results of the examination may be summarized as follows. The dimensional stability of the U 3 Si 2 and pure U 3 Si fuel was excellent throughout the entire burnup range, with uniform plate thickness increases up to a maximum of 4 mils at the highest burnup level (94% 235 U depletion). This corresponds to a meat volume increase of 11%. The swelling was partially due to solid fission products but to a larger extent to fission gas bubbles. The fission gas bubbles in U 3 Si 2 were small (submicrometer size) and very uniformly distributed, indicating great stability. To a large extent this was also the case for U 3 Si; however, larger bubbles ( 3 Si-1.5 w/o Al fuel became unstable at the higher burnup levels. Fission gas bubbles were larger than in the other two fuels and were present throughout the fuel particles. At 94% 235 U depletion, the formation of fission gas bubbles with diameters up to 20 mils caused the plates to pillow. It is proposed that aluminum in U 3 Si destabilizes fission gas bubble formation to the point of severe breakaway swelling in the prealloyed silicide fuel. (author)

  13. Radiation Re-solution Calculation in Uranium-Silicide Fuels

    International Nuclear Information System (INIS)

    Matthews, Christopher; Andersson, Anders David Ragnar; Unal, Cetin

    2017-01-01

    The release of fission gas from nuclear fuels is of primary concern for safe operation of nuclear power plants. Although the production of fission gas atoms can be easily calculated from the fission rate in the fuel and the average yield of fission gas, the actual diffusion, behavior, and ultimate escape of fission gas from nuclear fuel depends on many other variables. As fission gas diffuses through the fuel grain, it tends to collect into intra-granular bubbles, as portrayed in Figure 1.1. These bubbles continue to grow due to absorption of single gas atoms. Simultaneously, passing fission fragments can cause collisions in the bubble that result in gas atoms being knocked back into the grain. This so called ''re-solution'' event results in a transient equilibrium of single gas atoms within the grain. As single gas atoms progress through the grain, they will eventually collect along grain boundaries, creating inter-granular bubbles. As the inter-granular bubbles grow over time, they will interconnect with other grain-face bubbles until a pathway is created to the outside of the fuel surface, at which point the highly pressurized inter-granular bubbles will expel their contents into the fuel plenum. This last process is the primary cause of fission gas release. From the simple description above, it is clear there are several parameters that ultimately affect fission gas release, including the diffusivity of single gas atoms, the absorption and knockout rate of single gas atoms in intra-granular bubbles, and the growth and interlinkage of intergranular bubbles. Of these, the knockout, or re-solution rate has an particularly important role in determining the transient concentration of single gas atoms in the grain. The re-solution rate will be explored in the following sections with regards to uranium-silicide fuels in order to support future models of fission gas bubble behavior.

  14. Analysis Of Core Management For The Transition Cores Of RSG-GAS Reactor To Full-Silicide Core

    International Nuclear Information System (INIS)

    Malem Sembiring, Tagor; Suparlina, Lily; Tukiran

    2001-01-01

    The core conversion of RSG-GAS reactor from oxide to silicide core with meat density of 2.96 g U/cc is still doing. At the end of 2000, the reactor has been operated for 3 transition cores which is the mixed core of oxide-silicide. Based on previous work, the calculated core parameter for the cores were obtained and it is needed 10 transition cores to achieve a full-silicide core. The objective of this work is to acquire the effect of the increment of the number of silicide fuel on the core parameters such as excess reactivity and shutdown margin. The measurement of the core parameters was carried out using the method of compensation of couple control rods. The experiment shows that the excess reactivity trends lower with the increment of the number of silicide fuel in the core. However, the shutdown margin is not change with the increment of the number of silicide fuel. Therefore, the transition cores can be operated safety to a full-silicide core

  15. The Accident Analysis Due to Reactivity Insertion of RSG GAS 3.55 g U/cc Silicide Core

    International Nuclear Information System (INIS)

    Endiah Puji-Hastuti; Surbakti, Tukiran

    2004-01-01

    The fuels of RSG-GAS reactor was changed from uranium oxide with 250 g U of loading or 2.96 g U/cc of fuel loading to uranium silicide with the same loading. The silicide fuels can be used in higher density, staying longer in the reactor core and hence having a longer cycle length. The silicide fuel in RSG-GAS core was made up in step-wise by using mixed up core Firstly, it was used silicide fuel with 250 g U of loading and then, silicide fuel with 300 g U of loading (3.55 g U/cc of fuel loading). In every step-wise of fuel loading, it must be analyzed its safety margin. In this occasion, the reactivity accident of RSG-GAS core with 300 g U of silicide fuel loading is analyzed. The calculation was done using EUREKA-2/RR code available at P2TRR. The calculation was done by reactivity insertion at start up and power rangers. The worst case accident is transient due to control rod with drawl failure at start up by means of lowest initial power (0.1 W), either in power range. From all cases which have been done, the results of analysis showed that there is no anomaly and safety margin break at RSG-GAS core with 300 g U silicide fuel loading. (author)

  16. Thermal stability of Ni-Pt-Ta alloy silicides on epi-Si{sub 1-x}C{sub x}

    Energy Technology Data Exchange (ETDEWEB)

    Yoo, Jung-Ho; Chang, Hyun-Jin [Department of Ceramic Engineering, Yonsei University, Seoul 120-749 (Korea, Republic of); Min, Byoung-Gi [Department of Ceramic Engineering, Yonsei University, Seoul 120-749 (Korea, Republic of); Jusung Engineering Co., Ltd., 49, Neungpyeong-ri, Opo-eup, Gwangju-Si, Kyunggi-do 464-892 (Korea, Republic of); Ko, Dae-Hong [Department of Ceramic Engineering, Yonsei University, Seoul 120-749 (Korea, Republic of)], E-mail: dhko@yonsei.ac.kr; Cho, Mann-Ho [Institute of Physics and Applied Physics, Yonsei University, Seoul 120-749 (Korea, Republic of); Sohn, Hyunchul [Department of Ceramic Engineering, Yonsei University, Seoul 120-749 (Korea, Republic of); Lee, Tae-Wan [Jusung Engineering Co., Ltd., 49, Neungpyeong-ri, Opo-eup, Gwangju-Si, Kyunggi-do 464-892 (Korea, Republic of)

    2008-12-05

    We investigated the silicide formation in Ni/epi-Si{sub 1-x}C{sub x} systems. Ni-Pt and Ni-Pt-Ta films were deposited on epi-Si{sub 1-x}C{sub x}/Si substrates by DC magnetron sputtering and processed at various temperatures. The sheet resistance of the silicide from the Ni alloy/epi-Si{sub 1-x}C{sub x} systems was maintained at low values compared to that from Ni/Si systems. By TEM and EDS analyses, we confirmed the presence of a Pt alloy layer at the top of the Ni-silicide layer. The stability of the silicide layer in the Ni alloy/epi-Si{sub 1-x}C{sub x} system is explained by not only the Pt rich layer on the top of the Ni-silicide layer, but also by the presence of a small amount of Pt in the Ni-silicide layer or at the grain boundaries. And both the thermal stability and the morphology of silicide were greatly improved by the addition of Ta in Ni-Pt films.

  17. Thermal stability of Ni-Pt-Ta alloy silicides on epi-Si1-xCx

    International Nuclear Information System (INIS)

    Yoo, Jung-Ho; Chang, Hyun-Jin; Min, Byoung-Gi; Ko, Dae-Hong; Cho, Mann-Ho; Sohn, Hyunchul; Lee, Tae-Wan

    2008-01-01

    We investigated the silicide formation in Ni/epi-Si 1-x C x systems. Ni-Pt and Ni-Pt-Ta films were deposited on epi-Si 1-x C x /Si substrates by DC magnetron sputtering and processed at various temperatures. The sheet resistance of the silicide from the Ni alloy/epi-Si 1-x C x systems was maintained at low values compared to that from Ni/Si systems. By TEM and EDS analyses, we confirmed the presence of a Pt alloy layer at the top of the Ni-silicide layer. The stability of the silicide layer in the Ni alloy/epi-Si 1-x C x system is explained by not only the Pt rich layer on the top of the Ni-silicide layer, but also by the presence of a small amount of Pt in the Ni-silicide layer or at the grain boundaries. And both the thermal stability and the morphology of silicide were greatly improved by the addition of Ta in Ni-Pt films

  18. Tritium evolution from various morphologies of palladium

    International Nuclear Information System (INIS)

    Tuggle, D.G.; Claytor, T.N.; Taylor, S.F.

    1994-01-01

    The authors have been able to extend the tritium production techniques to various novel morphologies of palladium. These include small solid wires of various diameters and a type of pressed powder wire and a plasma cell. In most successful experiments, the amount of palladium required, for an equivalent tritium output, has been reduced by a factor of 100 over the older powder methods. In addition, they have observed rates of tritium production (>5 nCi/h) that far exceed most of the previous results. Unfortunately, the methods that they currently use to obtain the tritium are poorly understood and consequently there are numerous variables that need to be investigated before the new methods are as reliable and repeatable as the previous techniques. For instance, it seems that surface and/or bulk impurities play a major role in the successful generation of any tritium. In those samples with total impurity concentrations of >400 ppM essentially no tritium has been generated by the gas loading and electrical simulation methods

  19. Impact of Nickel silicide Rear Metallization on Series Resistance of Crystalline Silicon Solar Cells

    KAUST Repository

    Bahabry, Rabab R; Hanna, Amir N; Kutbee, Arwa T; Gumus, Abdurrahman; Hussain, Muhammad Mustafa

    2018-01-01

    the electrical characteristics of nickel mono-silicide (NiSi)/Cu-Al ohmic contact on the rear side of c-Si solar cells. We observe a significant enhancement in the fill factor of around 6.5% for NiSi/Cu-Al rear contacts leading to increasing the efficiency by 1.2

  20. Pilot plant production at Riso of LEU silicide fuel for the Danish reactor DR3

    International Nuclear Information System (INIS)

    Toft, P.; Borring, J.; Adolph, E.

    1988-01-01

    A pilot plant for fabricating LEU silicide fuel elements has been established at Riso National Laboratory. Three test elements for the Danish reactor DR3 have been fabricated, based on 19.88% enriched U 3 Si 2 powder that has been purchased elsewhere. The pilot plant has been set up and 3 test elements fabricated without any major difficulties

  1. Role of Ti 3 Al/silicides on tensile properties of Timetal 834 at ...

    Indian Academy of Sciences (India)

    Extremely fine coherent precipitates of ordered Ti3Al and relatively coarse incoherent precipitates of 2 silicide exist together in the near -titanium alloy, Timetal 834, in the dual phase matrix of primary and transformed . In order to assess the role of these precipitates, three heat treatments viz. WQ, WQ–A and WQ–OA, ...

  2. Core-hole effects in the x-ray-absorption spectra of transition-metal silicides

    NARCIS (Netherlands)

    WEIJS, PJW; CZYZYK, MT; VANACKER, JF; SPEIER, W; GOEDKOOP, JB; VANLEUKEN, H; HENDRIX, HJM; DEGROOT, RA; VANDERLAAN, G; BUSCHOW, KHJ; WIECH, G; FUGGLE, JC

    1990-01-01

    We report systematic differences between the shape of the Si K x-ray-absorption spectra of transition-metal silicides and broadened partial densities of Si p states. We use a variety of calculations to show that the origin of these discrepancies is the core-hole potential appropriate to the final

  3. Cross-Bridge Kelvin Resistor (CBKR) structures for silicide-semiconductor junctions characterization

    NARCIS (Netherlands)

    Stavitski, N.; van Dal, M.J.H.; Klootwijk, J.H.; Wolters, Robertus A.M.; Kovalgin, Alexeij Y.; Schmitz, Jurriaan

    2006-01-01

    Analyzing the contact geometry factors for the conventional CBKR structures, it appeared that the contact geometries conventionally used for the metal-to-silicide contact resistance measurements were not always satisfactory to reveal the specific contact resistance values. To investigate these

  4. X-ray-emission studies of chemical bonding in transition-metal silicides

    NARCIS (Netherlands)

    Weijs, P.J.W.; Leuken, H. van; Groot, R.A. de; Fuggle, J.C.; Reiter, S.; Wiech, G.; Buschow, K.H.J.

    1991-01-01

    We present Si L2,3 emission-band spectra of a series of 3d and 4d transition-metal (TM) silicides, together wtih Si K emission-band spectra of four 3d TM disilicides. The data are compared with augmented-spherical-wave density-of-states (DOS) calculations, and good agreement is found. The trends we

  5. Kinetics of low pressure chemical vapor deposition of tungsten silicide from dichlorocilane reduction of tungsten hexafluoride

    International Nuclear Information System (INIS)

    Srinivas, D.; Raupp, G.B.; Hillman, J.

    1990-01-01

    The authors report on experiments to determine the intrinsic surface reaction rate dependences and film properties' dependence on local reactant partial pressures and wafer temperature in low pressure chemical vapor deposition (LPCVD) of tungsten silicide from dichlorosilane reduction of tungsten hexafluoride. Films were deposited in a commercial-scale Spectrum CVD cold wall single wafer reactor under near differential, gradientless conditions. Over the range of process conditions investigated, deposition rate was found to be first order in dichlorosillane and negative second order in tungsten hexafluoride partial pressure. The apparent activation energy in the surface reaction limited regime was found to be 70-120 kcal/mol. The silicon to tungsten ratio of as deposited silicide films ranged from 1.1 to 2.4, and increased with increasing temperature and dichlorosillane partial pressure, and decreased with increasing tungsten hexafluoride pressure. These results suggest that the apparent silicide deposition rate and composition are controlled by the relative rates of at least two competing reactions which deposit stoichiometric tungsten silicides and/or silicon

  6. Waste Photovoltaic Panels for Ultrapure Silicon and Hydrogen through the Low-Temperature Magnesium Silicide.

    Czech Academy of Sciences Publication Activity Database

    Dytrych, Pavel; Bumba, Jakub; Kaštánek, František; Fajgar, Radek; Koštejn, Martin; Šolcová, Olga

    Roč. 56, č. 45 ( 2017 ), s. 12863-12869 ISSN 0888-5885 R&D Projects: GA ČR GA15-14228S Institutional support: RVO:67985858 Keywords : magnesium silicide * waste photovoltaic panels * ultrapure silicon Subject RIV: CI - Industrial Chemistry, Chemical Engineering OBOR OECD: Chemical process engineering Impact factor: 2.843, year: 2016

  7. High pressure studies on uranium and thorium silicide compounds: Experiment and theory

    DEFF Research Database (Denmark)

    Yagoubi, S.; Heathman, S.; Svane, A.

    2013-01-01

    The actinide silicides ThSi, USi and USi2 have been studied under high pressure using both theory and experiment. High pressure synchrotron X-ray diffraction experiments were performed on polycrystalline samples in diamond anvil cells at room temperature and for pressures up to 54, 52 and 26 GPa...

  8. Characterising palladium-silver and palladium-nickel alloy membranes using SEM, XRD and PIXE

    International Nuclear Information System (INIS)

    Keuler, J.N.; Lorenzen, L.; Sanderson, R.D.; Prozesky, V.; Przybylowicz, W.J.

    1999-01-01

    Palladium alloy membranes were prepared by successive electroless plating steps on an alumina-zirconia support membrane. Palladium, silver and nickel were deposited in layers and then the metal films were heat treated for 5 h in a hydrogen atmosphere at 650 deg. C. The topography of the metal coatings and cross-sections of the films (before and after heating) were characterised using scanning electron microscopy (SEM). XRD was used to determine the crystal phase of the alloy coatings. Both SEM and XRD provide only surface information and therefore micro-PIXE was used to extract depth information of the alloy coating. Concentration profiles across the thickness of the films were constructed to determine penetration of the coating into the support membrane pores during electroless plating and to investigate diffusion of coated layers during the heating step

  9. Fabrication of palladium-based microelectronic devices by microcontact printing

    International Nuclear Information System (INIS)

    Wolfe, Daniel B.; Love, J. Christopher; Paul, Kateri E.; Chabinyc, Michael L.; Whitesides, George M.

    2002-01-01

    This letter demonstrates the patterning of thin films of metallic palladium by microcontact printing (μCP) of octadecanethiol, and the use of the patterned films in the fabrication of a functional sensor. This technique was also used to prepare templates of palladium for the electroless deposition of copper. The resistivity of the palladium and copper microstructures was 13.8 and 2.8 μΩ cm, respectively; these values are approximately 40% larger than the values for the pure bulk metals. Palladium patterned into serpentine wires using μCP functioned as a hydrogen sensor with sensitivity of 0.03 vol % H 2 in N 2 , and a response time of ∼10 s (at room temperature)

  10. Antibacterial properties of palladium nanostructures sputtered on polyethylene naphthalate

    Czech Academy of Sciences Publication Activity Database

    Polívková, M.; Válová, M.; Siegel, J.; Rimpelová, S.; Hubáček, Tomáš; Lyutakov, O.; Švorčík, V.

    2015-01-01

    Roč. 5, č. 90 (2015), s. 73767-73774 ISSN 2046-2069 Institutional support: RVO:60077344 Keywords : polymer * palladium sputtering * annealing * nanostructure * antibacterial effect Subject RIV: JJ - Other Materials Impact factor: 3.289, year: 2015

  11. Palladium-catalysed arylation of sulfonamide stabilised enolates

    CSIR Research Space (South Africa)

    Zeevaart, JG

    2005-03-07

    Full Text Available Alpha-Arylation of inethanesulfonamides using palladium catalysis is described. For example, treatment of N-benzyl-Nmethylmethanesulfonamide with catalytic Pd (OAc) (2) in the presence of sodium tert-butoxide, triphenylphosphine and toluene afforded...

  12. Near surface silicide formation after off-normal Fe-implantation of Si(001) surfaces

    Energy Technology Data Exchange (ETDEWEB)

    Khanbabaee, B., E-mail: khanbabaee@physik.uni-siegen.de; Pietsch, U. [Solid State Physics, University of Siegen, D-57068 Siegen (Germany); Lützenkirchen-Hecht, D. [Fachbereich C - Physik, Bergische Universität Wuppertal, D-42097 Wuppertal (Germany); Hübner, R.; Grenzer, J.; Facsko, S. [Helmholtz-Zentrum Dresden-Rossendorf, 01314 Dresden (Germany)

    2014-07-14

    We report on formation of non-crystalline Fe-silicides of various stoichiometries below the amorphized surface of crystalline Si(001) after irradiation with 5 keV Fe{sup +} ions under off-normal incidence. We examined samples prepared with ion fluences of 0.1 × 10{sup 17} and 5 × 10{sup 17} ions cm{sup −2} exhibiting a flat and patterned surface morphology, respectively. Whereas the iron silicides are found across the whole surface of the flat sample, they are concentrated at the top of ridges at the rippled surface. A depth resolved analysis of the chemical states of Si and Fe atoms in the near surface region was performed by combining X-ray photoelectron spectroscopy and X-ray absorption spectroscopy (XAS) using synchrotron radiation. The chemical shift and the line shape of the Si 2p core levels and valence bands were measured and associated with the formation of silicide bonds of different stoichiometric composition changing from an Fe-rich silicides (Fe{sub 3}Si) close to the surface into a Si-rich silicide (FeSi{sub 2}) towards the inner interface to the Si(001) substrate. This finding is supported by XAS analysis at the Fe K-edge which shows changes of the chemical environment and the near order atomic coordination of the Fe atoms in the region close to surface. Because a similar Fe depth profile has been found for samples co-sputtered with Fe during Kr{sup +} ion irradiation, our results suggest the importance of chemically bonded Fe in the surface region for the process of ripple formation.

  13. Toward Efficient Palladium-Catalyzed Allylic C-H Alkylation

    DEFF Research Database (Denmark)

    Jensen, Thomas; Fristrup, Peter

    2009-01-01

    Recent breakthroughs have proved that direct palladium (II)-catalyzed allylic C-H alkylation can be achieved. This new procedure shows that the inherent requirement for a leaving group in the Tsuji-Trost palladium-catalyzed allylic alkylation can be lifted. These initial reports hold great promise...... for the development of allylic C-H alkylation into a widely applicable methodology, thus providing a means to enhance synthetic efficiency in these reactions....

  14. Carbon in palladium catalysts: A metastable carbide

    International Nuclear Information System (INIS)

    Seriani, Nicola; Mittendorfer, Florian; Kresse, Georg

    2010-01-01

    The catalytic activity of palladium towards selective hydrogenation of hydrocarbons depends on the partial pressure of hydrogen. It has been suggested that the reaction proceeds selectively towards partial hydrogenation only when a carbon-rich film is present at the metal surface. On the basis of first-principles simulations, we show that carbon can dissolve into the metal because graphite formation is delayed by the large critical nucleus necessary for graphite nucleation. A bulk carbide Pd 6 C with a hexagonal 6-layer fcc-like supercell forms. The structure is characterized by core level shifts of 0.66-0.70 eV in the core states of Pd, in agreement with experimental x-ray photoemission spectra. Moreover, this phase traps bulk-dissolved hydrogen, suppressing the total hydrogenation reaction channel and fostering partial hydrogenation. (author)

  15. Electron spectroscopy in the X-ray range for occupied and free levels and the application to transition metal silicides

    International Nuclear Information System (INIS)

    Speier, W.

    1988-03-01

    Intermetallic compounds of transition metals are investigated by means of XPS, Bremsstrahlung Isochromate Spectroscopy and XAS. Occupied and free levels are characterized and moreover a systematic overview over the electronic structure of the transition element silicides is given. (BHO)

  16. Evaluation of In-Core Fuel Management for the Transition Cores of RSG-GAS Reactor to Full-Silicide Core

    International Nuclear Information System (INIS)

    S, Tukiran; MS, Tagor; P, Surian

    2003-01-01

    The core conversion of RSG-GAS reactor from oxide to silicide core with meat density of 2.96 gU/cc has been done. The core-of RSG-GAS reactor has been operated full core of silicide fuels which is started with the mixed core of oxide-silicide start from core 36. Based on previous work, the calculated core parameter for the cores were obtained and it is needed 9 transition cores (core 36 - 44) to achieve a full-silicide core (core 45). The objective of this work is to acquire the effect of the increment of the number of silicide fuel on the core parameters. Conversion core was achieved by transition cores mixed oxide-silicide fuels. Each transition core is calculated and measured core parameter such as, excess reactivity and shutdown margin. Calculation done by Batan-EQUIL-2D code and measurement of the core parameters was carried out using the method of compensation of couple control rods. The results of calculation and experiment shows that the excess reactivity trends lower with the increment of the number of silicide fuel in the core. However, the shutdown margin is not change with the increment of the number of silicide fuel. Therefore, the transition cores can be operated safely to a full-silicide core

  17. Recovery of Elemental Palladium by Shewanella putrefaciens

    Science.gov (United States)

    Akasaka, S.; Xia, X.; Sawada, K.; Enokida, Y.; Yamamoto, I.; Ohnuki, T.

    2006-12-01

    Microbial reduction of metals plays an important role in environmental behavior and provides a technique for the recovery of metals from industrial wastewater. Recently, demand for platinum group metals (PGMs) increases by their catalytic properties. The extreme rarity of PGMs have led to a growing interest in their recovery. Palladium, one of PGMs, has different oxidation states of Pd(II) and Pd(0). The oxidized form of Pd(II) is soluble, while the reduced form of Pd(0) is insoluble. In this study, microbial reduction of palladium by Fe(III)- reducing bacterium, Shewanella putrefaceins was conducted. This bacterium is known to be capable of reducing metals, such as Mn(IV), U(VI), or Tc(VII) with organic C or H2 as an electron donor. In order to investigate the potential of S. putrefaciens to reduce Pd(II) in solution, resting cells or heat-killed cells were suspended under anaerobic conditions with lactate or H2 as an electron donor. The cells of S. putrefaciens (NBRC3908) were grown in aerobic medium, harvested by centrifugation, and then washed with 25 mmol/dm3 HEPES and 100 mmol/dm3 NaCl (HEPES-NaCl) solution (pH 7.0). The heat-killed cells were autoclaved for 20 min at 121 degrees C. The cell suspension (21.5 mg in dry weight) was resuspended in the HEPES-NaCl solution which contained 1.0 mmol/dm3 Na2PdCl4 (Wako Pure chemical Industries, Ltd). The suspensions were bubbled with N2 for 15 min before 10 mmol/dm3 lactate or 4.8 v/v% H2 was added. The suspensions were then incubated at 30 degrees C. Redox potential (Eh) and pH of the solutions were measured in an inert glove box with Ar gas. Concentration of Pd(II) was measured by Inductively Coupled Plasma Atomic Emission Spectrometer (ICP-AES). Deposited Pd and cells were analyzed by X-ray powder diffraction (XRD) and Scanning Electron Microscope (SEM) with Energy-Dispersive Spectroscopy (EDS). Approximately 86% of Pd(II) of the initial concentration was removed from solution by the resting cells within 24 h when

  18. Reactivity And Neutron Flux At Silicide Fuel Element In The Core Of RSG-GAS

    International Nuclear Information System (INIS)

    Hamzah, Amir

    2000-01-01

    In order to 4.8 and 5.2 gr U/cm exp 3 loading of U 3 Si 2 --Al fuel plates characterization, he core reactivity change and neutron flux depression had been done. Control rod calibration method was used to reactivity change measurement and neutron flux distribution was measured using foil activation method. Measurement of insertion of A-type of testing fuel element with U-loading above cannot be done due to technical reason, so the measurement using full type silicide fuel element of 2.96 gr U/cm exp 3 loading. The reactivity change measurement result of insertion in A-9 and C-3 is + 2.67 cent. The flux depression at silicide fuel in A-9 is 1.69 times bigger than oxide and in C-3 is 0.68 times lower than oxide

  19. Babcock and Wilcox plate fabrication experience with uranium silicide spherical fuel

    International Nuclear Information System (INIS)

    Todd, Lawrence E.; Pace, Brett W.

    1996-01-01

    This report is written to present the fuel fabrication experience of Babcock and Wilcox using atomized spherical uranium silicide powder. The intent is to demonstrate the ability to fabricate fuel plates using spherical powder and to provide useful information proceeding into the next phase of work using this type of fuel. The limited quantity of resources- spherical powder and time, did not allow for much process optimizing in this work scope. However, the information contained within provides optimism for the future of spherical uranium silicide fuel plate fabrication at Babcock and Wilcox.The success of assembling fuel elements with spherical powder will enable Babcock and Wilcox to reduce overall costs to its customers while still maintaining our reputation for providing high quality research and test reactor products. (author)

  20. The formation of magnetic silicide Fe{sub 3}Si clusters during ion implantation

    Energy Technology Data Exchange (ETDEWEB)

    Balakirev, N. [Kazan National Research Technological University, K.Marx st. 68, Kazan 420015 (Russian Federation); Zhikharev, V., E-mail: valzhik@mail.ru [Kazan National Research Technological University, K.Marx st. 68, Kazan 420015 (Russian Federation); Gumarov, G. [Zavoiskii Physico-Technical Institute of Russian Academy of Sciences, 10/7 Sibirskii trakt st., Kazan 420029 (Russian Federation)

    2014-05-01

    A simple two-dimensional model of the formation of magnetic silicide Fe{sub 3}Si clusters during high-dose Fe ion implantation into silicon has been proposed and the cluster growth process has been computer simulated. The model takes into account the interaction between the cluster magnetization and magnetic moments of Fe atoms random walking in the implanted layer. If the clusters are formed in the presence of the external magnetic field parallel to the implanted layer, the model predicts the elongation of the growing cluster in the field direction. It has been proposed that the cluster elongation results in the uniaxial magnetic anisotropy in the plane of the implanted layer, which is observed in iron silicide films ion-beam synthesized in the external magnetic field.

  1. The formation of magnetic silicide Fe3Si clusters during ion implantation

    Science.gov (United States)

    Balakirev, N.; Zhikharev, V.; Gumarov, G.

    2014-05-01

    A simple two-dimensional model of the formation of magnetic silicide Fe3Si clusters during high-dose Fe ion implantation into silicon has been proposed and the cluster growth process has been computer simulated. The model takes into account the interaction between the cluster magnetization and magnetic moments of Fe atoms random walking in the implanted layer. If the clusters are formed in the presence of the external magnetic field parallel to the implanted layer, the model predicts the elongation of the growing cluster in the field direction. It has been proposed that the cluster elongation results in the uniaxial magnetic anisotropy in the plane of the implanted layer, which is observed in iron silicide films ion-beam synthesized in the external magnetic field.

  2. RA-3 reactor core with uranium silicide fuel elements P-07 type

    International Nuclear Information System (INIS)

    Abbate, Maximo J.; Sbaffoni, Maria M.

    2003-01-01

    Following the studies on the utilization of fuel elements (FE) containing uranium silicide, core of the RA-3 was analyzed with several calculation models. At first, the present situation, i.e. the core charged with normal FE (U 3 O 8 ), has been analyzed to validate the simulation methodology comparing with experimental results and to establish reference data to 5 and 10 MW able to be compared with future new situations. Also, CITVAP's nuclear data libraries to be used in irradiation experiment planning were completed. The results were satisfactory and were applied to the study of the core containing P-07 FE [U 3 Si 2 ], in face of a future core change. Comparing with the performance of the U 3 O 8 FE, the silicides ones show the following advantages: - average burnup: 45 % greater; -extraction burnup increase 12 %; and, -the residence time [in full power days] could be a 117 % greater. (author)

  3. The formation of magnetic silicide Fe3Si clusters during ion implantation

    International Nuclear Information System (INIS)

    Balakirev, N.; Zhikharev, V.; Gumarov, G.

    2014-01-01

    A simple two-dimensional model of the formation of magnetic silicide Fe 3 Si clusters during high-dose Fe ion implantation into silicon has been proposed and the cluster growth process has been computer simulated. The model takes into account the interaction between the cluster magnetization and magnetic moments of Fe atoms random walking in the implanted layer. If the clusters are formed in the presence of the external magnetic field parallel to the implanted layer, the model predicts the elongation of the growing cluster in the field direction. It has been proposed that the cluster elongation results in the uniaxial magnetic anisotropy in the plane of the implanted layer, which is observed in iron silicide films ion-beam synthesized in the external magnetic field

  4. A long-term ultrahigh temperature application of layered silicide coated Nb alloy in air

    Science.gov (United States)

    Sun, Jia; Fu, Qian-Gang; Li, Tao; Wang, Chen; Huo, Cai-Xia; Zhou, Hong; Yang, Guan-Jun; Sun, Le

    2018-05-01

    Nb-based alloy possessed limited application service life at ultrahigh temperature (>1400 °C) in air even taking the effective protective coating strategy into consideration for last decades. In this work a long duration of above 128 h at 1500 °C in air was successfully achieved on Nb-based alloy thanked to multi-layered silicide coating. Through optimizing interfaces, the MoSi2/NbSi2 silicide coating with Al2O3-adsorbed-particles layer exhibited three-times higher of oxidation resistance capacity than the one without it. In MoSi2-Al2O3-NbSi2 multilayer coating, the Al2O3-adsorbed-particles layer playing as an element-diffusion barrier role, as well as the formed porous Nb5Si3 layer as a stress transition zone, contributed to the significant improvement.

  5. Study of optical and luminescence properties of silicon — semiconducting silicide — silicon multilayer nanostructures

    International Nuclear Information System (INIS)

    Galkin, N.G.; Galkin, K.N.; Dotsenko, S.A.; Goroshko, D.L.; Shevlyagin, A.V.; Chusovitin, E.A.; Chernev, I.M.

    2017-01-01

    By method of in situ differential spectroscopy it was established that at the formation of monolayer Fe, Cr, Ca, Mg silicide and Mg stannide islands on the atomically clean silicon surface an appearance of loss peaks characteristic for these materials in the energy range of 1.1-2.6 eV is observed. An optimization of growth processes permit to grow monolithic double nanoheterostructures (DNHS) with embedded Fe, Cr and Ca nanocrystals, and also polycrystalline DNHS with NC of Mg silicide and Mg stannide and Ca disilicide. By methods of optical spectroscopy and Raman spectroscopy it was shown that embedded NC form intensive peaks in the reflectance spectra at energies up to 2.5 eV and Raman peaks. In DNS with β-FeSi2 NC a photoluminescence and electroluminescence at room temperature were firstly observed.

  6. High-Temperature Compatible Nickel Silicide Thermometer And Heater For Catalytic Chemical Microreactors

    DEFF Research Database (Denmark)

    Jensen, Søren; Quaade, U.J.; Hansen, Ole

    2005-01-01

    Integration of heaters and thermometers is important for agile and accurate control and measurement of the thermal reaction conditions in microfabricated chemical reactors (microreactors). This paper describes development and operation of nickel silicide heaters and temperature sensors...... for temperatures exceeding 700 °C. The heaters and thermometers are integrated with chemical microreactors for heterogeneous catalytic conversion of gasses, and thermally activated catalytic conversion of CO to CO2 in the reactors is demonstrated. The heaters and thermometers are shown to be compatible...

  7. Optical anisotropy of quasi-1D rare-earth silicide nanostructures on Si(001)

    Energy Technology Data Exchange (ETDEWEB)

    Chandola, S., E-mail: sandhya.chandola@isas.de [Leibniz-Institut für Analytische Wissenschaften – ISAS – e.V., Schwarzschildstraße 8, 12489 Berlin (Germany); Speiser, E.; Esser, N. [Leibniz-Institut für Analytische Wissenschaften – ISAS – e.V., Schwarzschildstraße 8, 12489 Berlin (Germany); Appelfeller, S.; Franz, M.; Dähne, M. [Institut für Festkörperphysik, Technische Universität Berlin, Hardenbergstraße 36, 10623 Berlin (Germany)

    2017-03-31

    Highlights: • Reflectance anisotropy spectroscopy (RAS) is capable of distinguishing optically between the semiconducting wetting layer and the metallic nanowires of rare earth (Tb and Dy) silicide nanostructures grown on vicinal Si(001). • The spectra of the wetting layer show a distinctive line shape with a large peak appearing at 3.8 eV, which is assigned to the formation of 2 × 3 and 2 × 4-like subunits of the 2 × 7 reconstruction. The spectra of the metallic nanowires show peaks at the E{sub 1} and E{sub 2} transitions of bulk Si which is assigned to strong substrate strain induced by the nanowires. • The optical anisotropy of the Tb nanowires is larger than for the Dy nanowires, which is related to the preferential formation of more strained bundles as well as larger areas of clean Si surfaces in the case of Tb. • RAS is shown to be a powerful addition to surface science techniques for studying the formation of rare-earth silicide nanostructures. Its surface sensitivity and rapidity of response make it an ideal complement to the slower but higher resolution of scanning probes of STM and AFM. - Abstract: Rare earth metals are known to interact strongly with Si(001) surfaces to form different types of silicide nanostructures. Using STM to structurally characterize Dy and Tb silicide nanostructures on vicinal Si(001), it will be shown that reflectance anisotropy spectroscopy (RAS) can be used as an optical fingerprint technique to clearly distinguish between the formation of a semiconducting two-dimensional wetting layer and the metallic one-dimensional nanowires. Moreover, the distinctive spectral features can be related to structural units of the nanostructures. RAS spectra of Tb and Dy nanostructures are found to show similar features.

  8. Neutronic study on conversion of SAFARI-1 to LEU silicide fuel

    International Nuclear Information System (INIS)

    Ball, G.; Pond, R.; Hanan, N.; Matos, J.

    1995-01-01

    This paper marks the initial study into the technical and economic feasibility of converting the SAFARI-1 reactor in South Africa to LEU silicide fuel. Several MTR assembly geometries and LEU uranium densities have been studied and compared with MEU and HEU fuels. Two factors of primary importance for conversion of SAFARI-1 to LEU fuel are the economy of the fuel cycle and the performance of the incore and excore irradiation positions

  9. Techno-economic study on conversion of SAFARI-1 to LEU silicide fuel

    International Nuclear Information System (INIS)

    Ball, G.; Malherbe, F.J.

    2004-01-01

    This paper marks the conclusion of the techno-economic study into the conversion of SAFARI-1 reactor in South Africa to LEU silicide fuel. Several different fuel types were studied and their characteristics compared to the current HEU fuel. The technical feasibility of operating SAFARI-1 with the different fuels as well as the overall economic impact of the fuels is discussed and conclusions drawn.(author)

  10. Behavior of silicon in nitric media. Application to uranium silicides fuels reprocessing

    International Nuclear Information System (INIS)

    Cheroux, L.

    2001-01-01

    Uranium silicides are used in some research reactors. Reprocessing them is a solution for their cycle end. A list of reprocessing scenarios has been set the most realistic being a nitric dissolution close to the classic spent fuel reprocessing. This uranium silicide fuel contains a lot of silicon and few things are known about polymerization of silicic acid in concentrated nitric acid. The study of this polymerization allows to point out the main parameters: acidity, temperature, silicon concentration. The presence of aluminum seems to speed up heavily the polymerization. It has been impossible to find an analytical technique smart and fast enough to characterize the first steps of silicic acid polymerization. However the action of silicic species on emulsions stabilization formed by mixing them with an organic phase containing TBP has been studied, Silicon slows down the phase separation by means of oligomeric species forming complex with TBP. The existence of these intermediate species is short and heating can avoid any stabilization. When non irradiated uranium silicide fuel is attacked by a nitric solution, aluminum and uranium are quickly dissolved whereas silicon mainly stands in solid state. That builds a gangue of hydrated silica around the uranium silicide particulates without preventing uranium dissolution. A small part of silicon passes into the solution and polymerize towards the highly poly-condensed forms, just 2% of initial silicon is still in molecular form at the end of the dissolution. A thermal treatment of the fuel element, by forming inter-metallic phases U-Al-Si, allows the whole silicon to pass into the solution and next to precipitate. The behavior of silicon in spent fuels should be between these two situations. (author)

  11. Sputtering induced surface composition changes in copper-palladium alloys

    International Nuclear Information System (INIS)

    Sundararaman, M.; Sharma, S.K.; Kumar, L.; Krishnan, R.

    1981-01-01

    It has been observed that, in general, surface composition is different from bulk composition in multicomponent materials as a result of ion beam sputtering. This compositional difference arises from factors like preferential sputtering, radiation induced concentration gradients and the knock-in effect. In the present work, changes in the surface composition of copper-palladium alloys, brought about by argon ion sputtering, have been studied using Auger electron spectroscopy. Argon ion energy has been varied from 500 eV to 5 keV. Enrichment of palladium has been observed in the sputter-altered layer. The palladium enrichment at the surface has been found to be higher for 500 eV argon ion sputtering compared with argon ion sputtering at higher energies. Above 500 eV, the surface composition has been observed to remain the same irrespective of the sputter ion energy for each alloy composition. The bulk composition ratio of palladium to copper has been found to be linearly related to the sputter altered surface composition ratio of palladium to copper. These results are discussed on the basis of recent theories of alloy sputtering. (orig.)

  12. Ageing of palladium tritide: mechanical characterization, helium state and modelling

    International Nuclear Information System (INIS)

    Segard, M.

    2010-01-01

    Palladium is commonly used for the storage of tritium (the hydrogen radioactive isotope), since it forms a low-equilibrium-pressure and reversible tritide. Tritium decay into helium-3 is responsible for the ageing of the tritide, leading to the apparition of helium-3 bubbles for instance. Both experimental and theoretical aspects of this phenomenon are studied here.Previous works on ageing modelling led to two main models, dealing with:- Helium-3 bubbles nucleation (using a cellular automaton), - Bubbles growth (using continuum mechanics).These models were quite efficient, but their use was limited by the lack of input data and fitting experimental parameters.To get through these limitations, this work has consisted in studying the most relevant experimental data to improve the modelling of the palladium tritide ageing.The first part of this work was focused on the assessment of the mechanical properties of the palladium tritide (yield strength, ultimate strength, mechanical behaviour). They were deduced from the in situ tensile tests performed on palladium hydride and deuteride. In the second part, ageing characterization was undertaken, mainly focusing on: - Bubbles observations in palladium tritide using transmission electron microscopy, - Internal bubble pressure measurements using nuclear magnetic resonance, - Macroscopic swelling measurements using pycno-metry.The present work has led to significant progress in ageing understanding and has brought very valuable improvements to the modelling of such a phenomenon. (author) [fr

  13. Atomistic simulation of helium bubble nucleation in palladium

    Energy Technology Data Exchange (ETDEWEB)

    Wang Liang [Department of Applied Physics, Hunan University, Changsha 410082 (China); Hu, Wangyu [Department of Applied Physics, Hunan University, Changsha 410082 (China)], E-mail: wangyuhu2001cn@yahoo.com.cn; Xiao Shifang [Department of Applied Physics, Hunan University, Changsha 410082 (China)], E-mail: sfxiao@yahoo.com.cn; Yang Jianyu [Department of Maths and Physics, Hunan Institute of Engineering, Xiangtan 411104 (China); Deng Huiqiu [Department of Applied Physics, Hunan University, Changsha 410082 (China)

    2009-09-15

    A palladium crystal has been constructed with 11808 atoms. 55 helium atoms occupied the octahedral position of palladium crystal are introduced and retained in a spherical region. Molecular dynamic simulations are performed in a constant temperature and constant volume ensemble (NVT) with temperature controlled by Nose-Hoover thermostat. The interactions between palladium atoms are described with modified analytic embedded atom method (MAEAM), the interactions between palladium atom and helium atom are in the form of Morse potential, and the interactions between helium atoms are in the form of L-J potential function. With the analysis of the radial distribution function (RDF) and microstructure, it reveals that some of helium atoms form a series of clusters with different size, and the nucleation core is random at low temperature, and which is the embryo of helium bubble. Increasing temperature can accelerate the process of bubble nucleation, and the clusters will aggregate and coalesce into a bigger one in which there are no palladium atoms, and it is considered as a helium bubble.

  14. Metal allergen of the 21st century--a review on exposure, epidemiology and clinical manifestations of palladium allergy

    DEFF Research Database (Denmark)

    Faurschou, Annesofie; Menné, Torkil; Johansen, Jeanne D

    2011-01-01

    Consumers are mainly exposed to palladium from jewellery and dental restorations. Palladium contact allergy is nearly always seen together with nickel allergy, as palladium and nickel tend to cross-react. We aimed to analyse the available palladium patch test data and case reports to determine...

  15. Formation of (Nd,Y)-silicides by sequential channeled implantation of Y and Nd ions

    International Nuclear Information System (INIS)

    Jin, S.; Bender, H.; Wu, M.F.; Vantomme, A.; Langouche, G.

    2000-01-01

    A buried hexagonal Nd 0.32 Y 0.68 Si 1.7 layer is formed by a sequential implantation of Y and Nd ions into (1 1 1)-oriented silicon wafers. The orientation relationship between the epitaxial Nd 0.32 Y 0.68 Si 1.7 and the silicon is (0 0 0 1) Nd 0.32 Y 0.68 Si 1.7 //(1 1 1) Si with Nd 0.32 Y 0.68 Si 1.7 // Si . High temperature annealing (1000 deg. C) results in a gradual transition into an orthorhombic ternary (Nd,Y)-silicide. Between the orthorhombic (Nd,Y)-silicide and the Si a preferential orientation relationship exists: (1 1 0) orth //(1 1(bar) 0) Si with orth // Si . However, as not all orthorhombic silicide grains follow this epitaxial relationship, the minimum yield in the Rutherford backscattering spectrometry (RBS) spectrum increases compared to the results after a low temperature annealing

  16. Formation of (Nd,Y)-silicides by sequential channeled implantation of Y and Nd ions

    Science.gov (United States)

    Jin, S.; Bender, H.; Wu, M. F.; Vantomme, A.; Langouche, G.

    2000-03-01

    A buried hexagonal Nd0.32Y0.68Si1.7 layer is formed by a sequential implantation of Y and Nd ions into (1 1 1)-oriented silicon wafers. The orientation relationship between the epitaxial Nd0.32Y0.68Si1.7 and the silicon is (0 0 0 1)Nd0.32Y0.68Si1.7//(1 1 1)Si with Nd0.32Y0.68Si1.7//Si. High temperature annealing (1000°C) results in a gradual transition into an orthorhombic ternary (Nd,Y)-silicide. Between the orthorhombic (Nd,Y)-silicide and the Si a preferential orientation relationship exists: (1 1 0)orth//(1 1¯ 0)Si with orth//Si. However, as not all orthorhombic silicide grains follow this epitaxial relationship, the minimum yield in the Rutherford backscattering spectrometry (RBS) spectrum increases compared to the results after a low temperature annealing.

  17. Pt silicide/poly-Si Schottky diodes as temperature sensors for bolometers

    Energy Technology Data Exchange (ETDEWEB)

    Yuryev, V. A., E-mail: vyuryev@kapella.gpi.ru; Chizh, K. V.; Chapnin, V. A.; Mironov, S. A.; Dubkov, V. P.; Uvarov, O. V.; Kalinushkin, V. P. [A. M. Prokhorov General Physics Institute of the Russian Academy of Sciences, 38 Vavilov Street, Moscow 119991 (Russian Federation); Senkov, V. M. [P. N. Lebedev Physical Institute of the Russian Academy of Sciences, 53 Leninskiy Avenue, Moscow 119991 (Russian Federation); Nalivaiko, O. Y. [JSC “Integral” – “Integral” Holding Management Company, 121A, Kazintsa I. P. Street, Minsk 220108 (Belarus); Novikau, A. G.; Gaiduk, P. I. [Belarusian State University, 4 Nezavisimosti Avenue, 220030 Minsk (Belarus)

    2015-05-28

    Platinum silicide Schottky diodes formed on films of polycrystalline Si doped by phosphorus are demonstrated to be efficient and manufacturable CMOS-compatible temperature sensors for microbolometer detectors of radiation. Thin-film platinum silicide/poly-Si diodes have been produced by a CMOS-compatible process on artificial Si{sub 3}N{sub 4}/SiO{sub 2}/Si(001) substrates simulating the bolometer cells. Layer structure and phase composition of the original Pt/poly-Si films and the Pt silicide/poly-Si films synthesized by a low-temperature process have been studied by means of the scanning transmission electron microscopy; they have also been explored by means of the two-wavelength X-ray structural phase analysis and the X-ray photoelectron spectroscopy. Temperature coefficient of voltage for the forward current of a single diode is shown to reach the value of about −2%/ °C in the temperature interval from 25 to 50 °C.

  18. Multi-layered silicides coating for vanadium alloys for generation IV reactors

    International Nuclear Information System (INIS)

    Mathieu, S.; Chaia, N.; Vilasi, M.; Le Flem, M.

    2012-01-01

    The halide-activated pack-cementation technique was employed to fabricate a diffusion coating that is resistant both to isothermal and to cyclic oxidation in air at 650 degrees C on the surface of the V-4Cr-4Ti vanadium alloy that is a potential core component of future nuclear systems. A thermodynamic assessment determined the deposit conditions in terms of master alloy, activator, filler and temperature. The partial pressures of the main gaseous species (SiCl 4 , SiCl 2 and VCl 2 ) in the pack were calculated with the master alloy Si and the mixture VSi 2 + Si. The VSi 2 + Si master alloy was used to limit vanadium loss from the surface. The obtained coating consisted of multi-layered V x Si y silicides with an outer layer of VSi 2 . This silicide developed a protective layer of silica at 650 degrees C in air and was not susceptible to the pest phenomenon, unlike other refractory silicides (MoSi 2 , NbSi 2 ). We suggest that VSi 2 exhibits no risk of rapid degradation in the gas fast reactor (GFR) conditions. (authors)

  19. Silicide/Silicon Heterointerfaces, Reaction Kinetics and Ultra-short Channel Devices

    Science.gov (United States)

    Tang, Wei

    Nickel silicide is one of the electrical contact materials widely used on very large scale integration (VLSI) of Si devices in microelectronic industry. This is because the silicide/silicon interface can be formed in a highly controlled manner to ensure reproducibility of optimal structural and electrical properties of the metal-Si contacts. These advantages can be inherited to Si nanowire (NW) field-effect transistors (FET) device. Due to the technological importance of nickel silicides, fundamental materials science of nickel silicides formation (Ni-Si reaction), especially in nanoscale, has raised wide interest and stimulate new insights and understandings. In this dissertation, in-situ transmission electron microscopy (TEM) in combination with FET device characterization will be demonstrated as useful tools in nano-device fabrication as well as in gaining insights into the process of nickel silicide formation. The shortest transistor channel length (17 nm) fabricated on a vapor-liquid-solid (VLS) grown silicon nanowire (NW) has been demonstrated by controlled reaction with Ni leads on an in-situ transmission electron microscope (TEM) heating stage at a moderate temperature of 400 ºC. NiSi2 is the leading phase, and the silicide-silicon interface is an atomically sharp type-A interface. At such channel lengths, high maximum on-currents of 890 (microA/microm) and a maximum transconductance of 430 (microS/microm) were obtained, which pushes forward the performance of bottom-up Si NW Schottky barrier field-effect transistors (SB-FETs). Through accurate control over the silicidation reaction, we provide a systematic study of channel length dependent carrier transport in a large number of SB-FETs with channel lengths in the range of (17 nm -- 3.6 microm). Our device results corroborate with our transport simulations and reveal a characteristic type of short channel effects in SB-FETs, both in on- and off-state, which is different from that in conventional MOSFETs

  20. Superconductivity and the structural phase transitions in palladium hydride and palladium deuteride

    International Nuclear Information System (INIS)

    Standley, R.W.

    1980-01-01

    The results of two experimental studies of the superconducting transition temperature, T/sub c/, of palladium hydride, PdH/sub x/, and palladium deuteride, PdD/sub x/, are presented. In the first study, the superconducting transition temperature of PdH/sub x/(D/sub x/) is studied as a function of H(D) concentration, x, in the temperature range from 0.2 K to 4K. The data join smoothly with those reported previously by Miller and Satterthwaite at higher temperatures, and the composite data are described by the empirical relation T/sub c/ = 150.8 (x-x/sub o/) 2 244 , where x/sub o/ = 0.715 for hydride samples and 0.668 for deuteride samples. The results, when compared with the theoretical predictions of Klein and Papaconstantopoulos, et al., raise questions about the validity of their explanation of the reverse isotope effect, which is based solely on a difference in force constants. In the second study, the effect of the order-disorder structural transition associated with the 50 K anomaly on the superconductivity of PdH/sub x/(D/sub x/) is investigated. Samples were quenched to low temperatures in the disordered state, and their transition temperatures measured. The samples were then annealed just below the anomaly temperature, and the ordering process followed by monitoring the change in sample resistance. The transition temperatures in the ordered state were then measured

  1. Behavior of palladium and its impact on intermetallic growth in palladium-coated Cu wire bonding

    International Nuclear Information System (INIS)

    Xu Hui; Qin, Ivy; Clauberg, Horst; Chylak, Bob; Acoff, Viola L.

    2013-01-01

    This paper describes the behavior of palladium in palladium-coated Cu (PdCu) wire bonding and its impact on bond reliability by utilizing transmission electron microscopy (TEM). A Pd layer approximately 80 nm thick, which is coated on the surface of Cu wire, dissolves into the Cu matrix during ball formation (under N 2 gas protection) when the wire tip is melted to form a ball. As a result of dissolving the very thin Pd layer into the ball, Pd is almost undetectable along the entire bond interface between the ball and the Al pad. The behavior of Pd during thermal aging in air, however, is different for central and peripheral interfaces. At the central interface, less than 5 at.% Pd is present after 168 h aging at 175 °C. At the periphery, however, Pd diffuses back and congregates, reaching a level of ∼12 at.% after 24 h, and a Pd-rich (Cu,Pd) 9 Al 4 layer (>40 at.% Pd) forms after 168 h. Pd acts substitutionally in Cu 9 Al 4 but cannot penetrate into the CuAl 2 or CuAl. By comparison of intermetallic thickness and interfacial morphology between PdCu and bare Cu wire bonds, it is concluded that the presence of Pd reduces intermetallic growth rate, and is associated with numerous nanovoids in PdCu bonds.

  2. Superlattices of platinum and palladium nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    MARTIN,JAMES E.; WILCOXON,JESS P.; ODINEK,JUDY G.; PROVENCIO,PAULA P.

    2000-04-06

    The authors have used a nonionic inverse micelle synthesis technique to form nanoclusters of platinum and palladium. These nanoclusters can be rendered hydrophobic or hydrophilic by the appropriate choice of capping ligand. Unlike Au nanoclusters, Pt nanoclusters show great stability with thiol ligands in aqueous media. Alkane thiols, with alkane chains ranging from C{sub 6} to C{sub 18} were used as hydrophobic ligands, and with some of these they were able to form 2-D and/or 3-D superlattices of Pt nanoclusters as small as 2.7 nm in diameter. Image processing techniques were developed to reliably extract from transmission electron micrographs (TEMs) the particle size distribution, and information about the superlattice domains and their boundaries. The latter permits one to compute the intradomain vector pair correlation function of the particle centers, from which they can accurately determine the lattice spacing and the coherent domain size. From these data the gap between the particles in the coherent domains can be determined as a function of the thiol chain length. It is found that as the thiol chain length increases, the gaps between particles within superlattice domains increases, but more slowly than one might expect, possibly indicating thiol chain interdigitation.

  3. Palladium configuration dependence of hydrogen detection sensitivity based on graphene FET for breath analysis

    Science.gov (United States)

    Sakamoto, Yuri; Uemura, Kohei; Ikuta, Takashi; Maehashi, Kenzo

    2018-04-01

    We have succeeded in fabricating a hydrogen gas sensor based on palladium-modified graphene field-effect transistors (FETs). The negative-voltage shift in the transfer characteristics was observed with exposure to hydrogen gas, which was explained by the change in work function. The hydrogen concentration dependence of the voltage shift was investigated using graphene FETs with palladium deposited by three different evaporation processes. The results indicate that the hydrogen detection sensitivity of the palladium-modified graphene FETs is strongly dependent on the palladium configuration. Therefore, the palladium-modified graphene FET is a candidate for breath analysis.

  4. Microwave-assisted synthesis of palladium nanocubes and nanobars

    International Nuclear Information System (INIS)

    Yu, Yanchun; Zhao, Yanxi; Huang, Tao; Liu, Hanfan

    2010-01-01

    Microwave was employed in the shape-controlled synthesis of palladium nanoparticles. Palladium nanocubes and nanobars with a mean size of about 23.8 nm were readily synthesized with H 2 PdCl 4 as a precursor, tetraethylene glycol (TEG) as both a solvent and a reducing agent in the presence of PVP and CTAB in 80 s under microwave irradiation. The structures of the as-prepared palladium nanoparticles were characterized by transmission electron microscopy (TEM), X-ray powder diffraction (XRD) and ultraviolet-visible (UV-vis) absorption spectroscopy. The formation of PdBr 4 2- due to the coordination replacement of the ligand Cl - ions in PdCl 4 2- ions by Br - ions in the presence of bromide was responsible for the synthesis of Pd nanocubes and nanobars. In addition, a milder reducing power, a higher viscosity and a stronger affinity of TEG were beneficial to the larger sizes of Pd nanocubes and nanobars.

  5. The solubility of palladium(II) bis-dimethylglyoximate

    International Nuclear Information System (INIS)

    Maghzian, R.

    1978-01-01

    The solubility of palladium(II) bis-dimethylglyoximate in different solutions has been determined. Values obtained for the solubility of the palladium complex are tabulated. The solubility is the lowest in water, ammonium acetate and a 25% acetone-water mixture. It is highest in dilute HCl and acetone but precipitation from aqueous acetone should be satisfactory for most purposes if the acetone content of the solvent is roughly less than 50% by volume. The solubility in dilute HCl reflects the concern by previous workers for losses in precipitation from mineral acid. In general, however, the losses are unlikely to be significant unless the quantity of palladium to be precipitated and weighed is small. (T.G.)

  6. Investigation of radiation-chemical behaviour of divalent palladium in perchloric acid solutions

    International Nuclear Information System (INIS)

    Vladimirova, M.V.; Kalinina, S.V.

    1988-01-01

    Gamma-radiolysis of divalent palladium in perchloric acid solutions is studied. Absorption spectra of intermediate palladium compounds formed in the irradiated solution are taken. The analysis of literature data as well as comparative analysis of the absorption spectra obtained under irradiation of palladium (2) perchloric acid solutions with absorption spectra of palladium chlorocomplexes allows to suppose that the mentioned compounds are chlorocomplexes of palladium (2) of different composition depending on HClO 4 concentration in the initial solution and absorbed radiation dose. Radiation-chemical reduction of palladium (2) up to metal is stated to take place in the whole studied range of initial concentrations of components of the system and dose rates. Kinetic dependences of metallic palladium formation are obtained. Values of radiation-chemical yields of metallic palladium formation depending on the initial concentrations of palladium (2) and perchloric acid are given. A mechanism of radiolytic reduction of palladium (2) in the investigated system is suggested based on the experimental data, and a theoretical value of the radiation-chemical yield of palladium (2) reduction being in a good agreement with experimentally found values is calculated

  7. Hydrogen Production via Steam Reforming of Ethyl Alcohol over Palladium/Indium Oxide Catalyst

    Directory of Open Access Journals (Sweden)

    Tetsuo Umegaki

    2009-01-01

    Full Text Available We report the synergetic effect between palladium and indium oxide on hydrogen production in the steam reforming reaction of ethyl alcohol. The palladium/indium oxide catalyst shows higher hydrogen production rate than indium oxide and palladium. Palladium/indium oxide affords ketonization of ethyl alcohol with negligible by-product carbon monoxide, while indium oxide mainly affords dehydration of ethyl alcohol, and palladium affords decomposition of ethyl alcohol with large amount of by-product carbon monoxide. The catalytic feature of palladium/indium oxide can be ascribed to the formation of palladium-indium intermetallic component during the reaction as confirmed by X-ray diffraction and X-ray photoelectron spectroscopic measurements.

  8. Morphological Study Of Palladium Thin Films Deposited By Sputtering

    Energy Technology Data Exchange (ETDEWEB)

    Salcedo, K L; Rodriguez, C A [Grupo Plasma Laser y Aplicaciones, Ingenieria Fisica, Universidad Tecnologica de Pereira (Colombia); Perez, F A [WNANO, West Virginia University (United States); Riascos, H [Grupo Plasma Laser y Aplicaciones, Departamento de Fisica, Universidad Tecnologica de Pereira (Colombia)

    2011-01-01

    This paper presents a morphological analysis of thin films of palladium (Pd) deposited on a substrate of sapphire (Al{sub 2}O{sub 3}) at a constant pressure of 3.5 mbar at different substrate temperatures (473 K, 523 K and 573 K). The films were morphologically characterized by means of an Atomic Force Microscopy (AFM); finding a relation between the roughness and the temperature. A morphological analysis of the samples through AFM was carried out and the roughness was measured by simulating the X-ray reflectivity curve using GenX software. A direct relation between the experimental and simulation data of the Palladium thin films was found.

  9. Morphological Study Of Palladium Thin Films Deposited By Sputtering

    International Nuclear Information System (INIS)

    Salcedo, K L; Rodriguez, C A; Perez, F A; Riascos, H

    2011-01-01

    This paper presents a morphological analysis of thin films of palladium (Pd) deposited on a substrate of sapphire (Al 2 O 3 ) at a constant pressure of 3.5 mbar at different substrate temperatures (473 K, 523 K and 573 K). The films were morphologically characterized by means of an Atomic Force Microscopy (AFM); finding a relation between the roughness and the temperature. A morphological analysis of the samples through AFM was carried out and the roughness was measured by simulating the X-ray reflectivity curve using GenX software. A direct relation between the experimental and simulation data of the Palladium thin films was found.

  10. Chemical recovery of palladium-103 from irradiated silver target

    International Nuclear Information System (INIS)

    Lapshina, E.V.; Kokhanyuk, V.M.; Zhuikov, B.L.; Myasoedova, G.V.; Zakhartchenko, E.A.; Phillips, D.R.; Jamriska, D.J.

    2003-01-01

    The goal of this work is to develop an extraction method of no-carrier-added palladium-103 from silver. Metallic silver targets may be irradiated by protons with energy of 60-200 MeV or more to generate palladium-103 simultaneously with other radioactive isotopes of rhodium, ruthenium, technetium, palladium and silver. According to the dependence experimental production yield of Pd-103 and isotopes of other elements in thick silver target vs. Proton energy the most suitable energy for maximum yield of Pd-103 and minimum yield of other elements is from about 100 to about 140 MeV. Activity of radionuclides produced in silver target depends from many factors (target thickness, irradiation time, etc.). Two methods of Pd-103 recovering from irradiated silver target are considered in this work: (1) Silver target is dissolved in nitric acid followed by silver precipitation in the form of silver chloride by addition of HCl. The solution containing Pd, Rh and other radionuclides is passed through the layer of fibrous sorbent POLYORGS-15n. Then the sorbent is washed and Pd is desorbed by hot 12 M hydrochloric acid; (2) Silver target is dissolved in nitric acid followed by passing of the obtained solution (2 M HNO 3 ) through a disk set of complex forming sorbent POLYORGS-33n. Under these conditions palladium is sorbed by the sorbent while silver, rhodium, ruthenium and technetium are passed through the sorbent. Then the sorbent is washed with 2M nitric acid, and Pd is desorbed by 12 M hydrochloric acid. Extraction of palladium is occurred during the formation of palladium complex with a chelate sorbent specific to palladium in acidic solutions. Such a sorbent makes possible separation of palladium from accompanying radionuclides such as rhodium, ruthenium and technetium. The polymeric complex-forming sorbent of fibrous structure with the groups of 3(5)-methylpyrazole (POLYORGS-15) is used. The distinctive feature of the sorbents in the form of fibrous 'filled' material is

  11. Porous palladium coated conducting polymer nanoparticles for ultrasensitive hydrogen sensors

    Science.gov (United States)

    Lee, Jun Seop; Kim, Sung Gun; Cho, Sunghun; Jang, Jyongsik

    2015-12-01

    Hydrogen, a clean-burning fuel, is of key importance to various industrial applications, including fuel cells and in the aerospace and automotive industries. However, hydrogen gas is odorless, colorless, and highly flammable; thus appropriate safety protocol implementation and monitoring are essential. Highly sensitive hydrogen leak detection and surveillance sensor systems are needed; additionally, the ability to maintain uniformity through repetitive hydrogen sensing is becoming increasingly important. In this report, we detail the fabrication of porous palladium coated conducting polymer (3-carboxylate polypyrrole) nanoparticles (Pd@CPPys) to detect hydrogen gas. The Pd@CPPys are produced by means of facile alkyl functionalization and chemical reduction of a pristine 3-carboxylate polypyrrole nanoparticle-contained palladium precursor (PdCl2) solution. The resulting Pd@CPPy-based sensor electrode exhibits ultrahigh sensitivity (0.1 ppm) and stability toward hydrogen gas at room temperature due to the palladium sensing layer.Hydrogen, a clean-burning fuel, is of key importance to various industrial applications, including fuel cells and in the aerospace and automotive industries. However, hydrogen gas is odorless, colorless, and highly flammable; thus appropriate safety protocol implementation and monitoring are essential. Highly sensitive hydrogen leak detection and surveillance sensor systems are needed; additionally, the ability to maintain uniformity through repetitive hydrogen sensing is becoming increasingly important. In this report, we detail the fabrication of porous palladium coated conducting polymer (3-carboxylate polypyrrole) nanoparticles (Pd@CPPys) to detect hydrogen gas. The Pd@CPPys are produced by means of facile alkyl functionalization and chemical reduction of a pristine 3-carboxylate polypyrrole nanoparticle-contained palladium precursor (PdCl2) solution. The resulting Pd@CPPy-based sensor electrode exhibits ultrahigh sensitivity (0.1 ppm

  12. Safeguarding subcriticality during loading and shuffling operations in the higher density of the RSG-GAS's silicide core

    International Nuclear Information System (INIS)

    Sembiring, T.M.; Kuntoro, I.

    2003-01-01

    The core conversion program of the RSG-GAS reactor is to convert the all-oxide to all-silicide core. The silicide equilibrium core with fuel meat density of 3.55 gU cm -3 is an optimal core for RSG-GAS reactor and it can significantly increase the operation cycle length from 25 to 32 full power days. Nevertheless, the subcriticality of the shutdown core and the shutdown margin are lower than of the oxide core. Therefore, the deviation of subcriticality condition in the higher silicide core caused by the fuel loading and shuffling error should be reanalysed. The objective of this work is to analyse the sufficiency of the subcriticality condition of the shutdown core to face the worst condition caused by an error during loading and shuffling operations. The calculations were carried out using the 2-dimensional multigroup neutron diffusion code of Batan-FUEL. In the fuel handling error, the calculated results showed that the subcriticality condition of the shutdown higher density silicide equilibrium core of RSG-GAS can be maintained. Therefore, all fuel management steps are fixed in the present reactor operation manual can be applied in the higher silicide equilibrium core of RSG-GAS reactor. (author)

  13. Local solid phase growth of few-layer graphene on silicon carbide from nickel silicide supersaturated with carbon

    International Nuclear Information System (INIS)

    Escobedo-Cousin, Enrique; Vassilevski, Konstantin; Hopf, Toby; Wright, Nick; O'Neill, Anthony; Horsfall, Alton; Goss, Jonathan; Cumpson, Peter

    2013-01-01

    Patterned few-layer graphene (FLG) films were obtained by local solid phase growth from nickel silicide supersaturated with carbon, following a fabrication scheme, which allows the formation of self-aligned ohmic contacts on FLG and is compatible with conventional SiC device processing methods. The process was realised by the deposition and patterning of thin Ni films on semi-insulating 6H-SiC wafers followed by annealing and the selective removal of the resulting nickel silicide by wet chemistry. Raman spectroscopy and X-ray photoelectron spectroscopy (XPS) were used to confirm both the formation and subsequent removal of nickel silicide. The impact of process parameters such as the thickness of the initial Ni layer, annealing temperature, and cooling rates on the FLG films was assessed by Raman spectroscopy, XPS, and atomic force microscopy. The thickness of the final FLG film estimated from the Raman spectra varied from 1 to 4 monolayers for initial Ni layers between 3 and 20 nm thick. Self-aligned contacts were formed on these patterned films by contact photolithography and wet etching of nickel silicide, which enabled the fabrication of test structures to measure the carrier concentration and mobility in the FLG films. A simple model of diffusion-driven solid phase chemical reaction was used to explain formation of the FLG film at the interface between nickel silicide and silicon carbide.

  14. Hydrogen uptake causes molecular "avalanches" in palladium | Argonne

    Science.gov (United States)

    air cylinders for storing the gas. Palladium, a precious metal closely related to platinum, is that storage or purification, and this research gets us closer to making that a reality. In this study take up hydrogen from the environment. "The ultimate goal is hydrogen storage or purification, and

  15. XPS study of palladium sensitized nano porous silicon thin film

    Indian Academy of Sciences (India)

    Keywords. Porous silicon; passivation; palladium; oxidation; XPS. Abstract. Nano porous silicon (PS) was formed on -type monocrystalline silicon of 2–5 cm resistivity and (100) orientation by electrochemical anodization method using HF and ethanol as the electrolytes. High density of surface states, arising due to its ...

  16. Absorption of hydrogen by vanadium-palladium alloys

    International Nuclear Information System (INIS)

    Artman, D.; Lynch, J.F.; Flanagan, T.B.

    1976-01-01

    Pressure composition isotherms (273-373 K) have been determined for the absorption of hydrogen by a series of six palladium alloys (f.c.c) in the composition range from 1 to 8 at.% vanadium. At a given hydrogen content, the equilibrium hydrogen pressure progressively increases with vanadium content. Thermodynamic parameters for the absorption of hydrogen are reported at infinite dilution of hydrogen and for the formation of the nonstoichiometric hydride from the hydrogen-saturated alloy. The relative, partial molar enthalpy of solution of hydrogen at infinite dilution increases slightly with vanadium content. The presence of vanadium, which absorbs hydrogen itself in its normal b.c.c. structure, greatly inhibits the ability of palladium to absorb hydrogen. For example, the isobaric solubility of hydrogen (1 atm, 298K) decreases from H/Pd=0.7 (palladium) to 0.024 (V(6%)-Pd). The lattice expansion due to the presence of interstitial hydrogen has been determined by X-ray diffraction. From these data it can be concluded that the formation of two non-stoichiometric hydride phases does not occur at vanadium contents greater that 5 at.% (298 K). Electrical resistance has been measured as a function of the hydrogen content of the alloys. The electrical resistance increases more markedly with hydrogen content for these alloys than for any of the palladium alloys previously examined. (Auth.)

  17. Microscopic observations of palladium used for cold fusion

    International Nuclear Information System (INIS)

    Matsumoto, T.

    1991-01-01

    This paper examines the microscopic structures of palladium metals used for cold fusion experiments. Tiny spot defects suggesting cold fusion have been observed in grain boundaries as the Nattoh model predicts. The relationship between these defects and a series of neutron busts and an indirect loop of hydrogen chain reactions are discussed

  18. Palladium-based nanocatalysts for alcohol electrooxidation in alkaline media

    CSIR Research Space (South Africa)

    Modibedi, RM

    2013-01-01

    Full Text Available in the electrocatalytic oxidation of alcohols in alkaline media compared to platinum catalysts. Recent efforts have focused on the discovery of palladium-based electrocatalysts with little or no platinum for oxygen reduction reaction (ORR). This chapter is an overview...

  19. ERRATUM Study of microstructure in vanadium–palladium alloys by ...

    Indian Academy of Sciences (India)

    WINTEC

    ERRATUM. Study of microstructure in vanadium–palladium alloys by X-ray diffraction technique. J Ghosh, S K Chattopadhyay, A K Meikap, S K Chatterjee and P Chatterjee 2007 Bull. Mater. Sci. 30 447–454. In page 448, under §2.1 Warren–Averbach method, after equation (1), the sentence starting with “Then the domain ...

  20. Fractal analysis of electrolytically-deposited palladium hydride dendrites

    International Nuclear Information System (INIS)

    Bursill, L.A.; Julin, Peng; Xudong, Fan.

    1990-01-01

    The fractal scaling characteristics of the surface profile of electrolytically-deposited palladium hydride dendritic structures have been obtained using conventional and high resolution transmission electron microscopy. The results are in remarkable agreement with the modified diffusion-limited aggregation model. 19 refs., 3 tabs., 13 figs

  1. Palladium nanoparticles on InP for hydrogen detection

    Czech Academy of Sciences Publication Activity Database

    Černohorský, Ondřej; Žďánský, Karel; Zavadil, Jiří; Kacerovský, Pavel; Piksová, K.

    2011-01-01

    Roč. 6, č. 410 (2011), s. 4101-4104 ISSN 1931-7573 R&D Projects: GA AV ČR(CZ) KAN401220801; GA ČR GA102/09/1037 Institutional research plan: CEZ:AV0Z20670512 Keywords : palladium * indium phosphide Subject RIV: JA - Electronics ; Optoelectronics, Electrical Engineering Impact factor: 2.726, year: 2011

  2. Palladium-catalyzed allylation of tautomerizable heterocycles with alkynes.

    Science.gov (United States)

    Lu, Chuan-Jun; Chen, Dong-Kai; Chen, Hong; Wang, Hong; Jin, Hongwei; Huang, Xifu; Gao, Jianrong

    2017-07-21

    A method for the allylic amidation of tautomerizable heterocycles was developed by a palladium catalyzed allylation reaction with 100% atom economy. A series of structurally diverse N-allylic substituted heterocycles can be synthesized in good yields with high chemo-, regio-, and stereoselectivities under mild conditions.

  3. Supporting Information Palladium Complexes of a New Type of N ...

    Indian Academy of Sciences (India)

    Prasenjit Ghosh

    Palladium Complexes of a New Type of N-heterocyclic Carbene. Ligand Derived From a Tricyclic Triazolooxazine Framework. Manoj Kumar Gangwar, Alok Ch. Kalita and Prasenjit Ghosh*. Department of Chemistry,. Indian Institute of Technology Bombay, ... 2. Figure S1. 1. H NMR spectrum of the compound 1a in CDCl3.

  4. Electronic structure of palladium and its relation to uv spectroscopy

    DEFF Research Database (Denmark)

    Christensen, N.E.

    1976-01-01

    The electronic-energy-band structure of palladium has been calculated by means of the relativistic augmented-plane-wave method covering energies up to 30 eV above the Fermi level. The optical interband transitions producing structure in the dielectric function up to photon energies of 25 eV have ...

  5. Exposure to nickel and palladium from dental appliances

    NARCIS (Netherlands)

    Ventura Da Cruz Rodrigues Milheiro, A.M.

    2015-01-01

    The application of a dental material into the oral cavity is not free of biological implications, as deterioration of the material will undoubtedly occur. The adverse health effects of palladium and nickel are well known and their immunologic cross-reactivity is well established. The aim of this

  6. Study of electroplated silver-palladium biofouling inhibiting coating

    DEFF Research Database (Denmark)

    Chiang, Wen-Chi; Hilbert, Lisbeth Rischel; Schroll, Casper

    2008-01-01

    Biofouling can cause many undesirable effects in industrial and medical settings. In this study, a new biofouling inhibiting Ag-Pd surface was designed to form an inhibiting effect by itself. This design was based on silver combined with nobler palladium, both with catalytic properties. Owing to ...

  7. Confined palladium colloids in mesoporous frameworks for carbon nanotube growth

    NARCIS (Netherlands)

    Berenguer-Murcia, A.; Rebrov, E.V.; Cabaj, M.; Wheatley, A.E.H.; Johnson, B.F.G.; Robertson, J.; Schouten, J.C.

    2009-01-01

    Palladium colloidal nanoparticles with an average size of approximately 2.4 nm have been incorporated into mesoporous inorganic thin films following a multistep approach. This involves the deposition of mesoporous titania thin films with a thickness of 200 nm by spin-coating on titanium plates with

  8. Post-pulse detail metallographic examinations of low-enriched uranium silicide plate-type miniature fuel

    International Nuclear Information System (INIS)

    Yanagisawa, Kazuaki

    1991-10-01

    Pulse irradiation at Nuclear Safety Research Reactor (NSRR) was performed using low-enriched (19.89 w% 235 U) unirradiated silicide plate-type miniature fuel which had a density of 4.8 gU/cm 3 . Experimental aims are to understand the dimensional stability and to clarify the failure threshold of the silicide plate-type miniature fuel under power transient conditions through post-pulse detail metallographic examinations. A silicide plate-type miniature fuel was loaded into an irradiation capsule and irradiated by a single pulse. Deposited energies given in the experiments were 62, 77, 116 and 154 cal/g·fuel, which lead to corresponding peak fuel plate temperatures, 201 ± 28degC, 187 ± 10degC, 418 ± 74degC and 871 ± 74degC, respectively. Below 400degC, reliability and dimensional stability of the silicide plate fuel was sustained, and the silicide plate fuel was intact. Up to 540degC, wall-through intergranular crackings occurred in the Al-3%Mg alloy cladding. With the increase of the temperature, the melting of the aluminum cladding followed by recrystallization, the denudation of fuel core and the plate-through intergranular cracking were observed. With the increase of the temperature beyond 400degC, the bowing of fuel plate became significant. Above the temperature of 640degC molten aluminum partially reacted with the fuel core, partially flowed downward under the influence of surface tension and gravity, and partially formed agglomerations. Judging from these experimental observations, the fuel-plate above 400degC tends to reduce its dimensional stability. Despite of the apparent silicide fuel-plate failure, neither generation of pressure pulse nor that of mechanical energy occurred at all. (J.P.N.)

  9. Quantitative EPMA of Nano-Phase Iron-Silicides in Apollo 16 Lunar Regolith

    Science.gov (United States)

    Gopon, P.; Fournelle, J.; Valley, J. W.; Pinard, P. T.; Sobol, P.; Horn, W.; Spicuzza, M.; Llovet, X.; Richter, S.

    2013-12-01

    Until recently, quantitative EPMA of phases under a few microns in size has been extremely difficult. In order to achieve analytical volumes to analyze sub-micron features, accelerating voltages between 5 and 8 keV need to be used. At these voltages the normally used K X-ray transitions (of higher Z elements) are no longer excited, and we must rely of outer shell transitions (L and M). These outer shell transitions are difficult to use for quantitative EPMA because they are strongly affected by different bonding environments, the error associated with their mass attenuation coefficients (MAC), and their proximity to absorption edges. These problems are especially prevalent for the transition metals, because of the unfilled M5 electron shell where the Lα transition originates. Previous studies have tried to overcome these limitations by using standards that almost exactly matched their unknowns. This, however, is cumbersome and requires accurate knowledge of the composition of your sample beforehand, as well as an exorbitant number of well characterized standards. Using a 5 keV electron beam and utilizing non-standard X-ray transitions (Ll) for the transition metals, we are able to conduct accurate quantitative analyses of phases down to ~300nm. The Ll transition in the transition metals behaves more like a core-state transition, and unlike the Lα/β lines, is unaffected by bonding effects and does not lie near an absorption edge. This allows for quantitative analysis using standards do not have to exactly match the unknown. In our case pure metal standards were used for all elements except phosphorus. We present here data on iron-silicides in two Apollo 16 regolith grains. These plagioclase grains (A6-7 and A6-8) were collected between North and South Ray Craters, in the lunar highlands, and thus are associated with one or more large impact events. We report the presence of carbon, nickel, and phosphorus (in order of abundance) in these iron-silicide phases

  10. The fabrication and performance of Canadian silicide dispersion fuel for test reactors

    International Nuclear Information System (INIS)

    Sears, D.F.; Wood, J.C.; Berthiaume, L.C.; Herbert, L.N.; Schaefer, J.D.

    1985-01-01

    Fuel fabrication effort is now concentrated on the commissioning of large-scale process equipment, defining product specifications, developing a quality assurance plan, and setting up a mini-computer material accountancy system. In the irradiation testing program, full-size NRU assemblies containing 20% enriched silicide dispersion fuel have been Irradiated successfully to burnups in the range 65-80 atomic percent. Irradiations have also been conducted on mini-elements having 1.2 mm diameter holes In their mid-sections, some drilled before irradiation and others after irradiation to 22-83 atomic percent burnup. Uranium was lost to the coolant in direct proportion to the surface area of exposed core material. Pre-irradiation in the intact condition appeared to reduce in-reactor corrosion. Fuel cores developed for the NRU reactor are dimensionally very stable, swelling by only 6-8% at the very high burnup of 93 atomic percent. Two important factors contributing to this good performance are cylindrical clad restraint and coarse silicide particles. Thermal ramping tests were conducted on irradiated silicide aspersion fuels. Small segments of fuel cores released 85 Kr starting at about 520 deg. C and peaking at about 680 deg C. After a holding period of 1 hour at 720 deg. C a secondary 85 Kr peak occurred during cooling (at about 330 deg. C) probably due to thermal contraction cracking. Whole mini-elements irradiated to 93 atomic percent burnup were also ramped thermally, with encouraging results. After about 0.25 h at 530 deg. C the aluminum cladding developed very localized small blisters, some with penetrating pin-hole cracks preventing gross pillowing or ballooning. (author)

  11. Silicon-germanium and platinum silicide nanostructures for silicon based photonics

    Science.gov (United States)

    Storozhevykh, M. S.; Dubkov, V. P.; Arapkina, L. V.; Chizh, K. V.; Mironov, S. A.; Chapnin, V. A.; Yuryev, V. A.

    2017-05-01

    This paper reports a study of two types of silicon based nanostructures prospective for applications in photonics. The first ones are Ge/Si(001) structures forming at room temperature and reconstructing after annealing at 600°C. Germanium, being deposited from a molecular beam at room temperature on the Si(001) surface, forms a thin granular film composed of Ge particles with sizes of a few nanometers. A characteristic feature of these films is that they demonstrate signs of the 2 x 1 structure in their RHEED patterns. After short-term annealing at 600°C under the closed system conditions, the granular films reconstruct to heterostructures consisting of a Ge wetting layer and oval clusters of Ge. A mixed type c(4x2) + p(2x2) reconstruction typical to the low-temperature MBE (Tgr Ge. The other type of the studied nanostructures is based on Pt silicides. This class of materials is one of the friendliest to silicon technology. But as silicide film thickness reaches a few nanometers, low resistivity becomes of primary importance. Pt3Si has the lowest sheet resistance among the Pt silicides. However, the development of a process of thin Pt3Si films formation is a challenging task. This paper describes formation of a thin Pt3Si/Pt2Si structures at room temperature on poly-Si films. Special attention is paid upon formation of poly-Si and amorphous Si films on Si3N4 substrates at low temperatures.

  12. The fabrication and performance of Canadian silicide dispersion fuel for test reactors

    Energy Technology Data Exchange (ETDEWEB)

    Sears, D F; Wood, J C; Berthiaume, L C; Herbert, L N; Schaefer, J D

    1985-07-01

    Fuel fabrication effort is now concentrated on the commissioning of large-scale process equipment, defining product specifications, developing a quality assurance plan, and setting up a mini-computer material accountancy system. In the irradiation testing program, full-size NRU assemblies containing 20% enriched silicide dispersion fuel have been Irradiated successfully to burnups in the range 65-80 atomic percent. Irradiations have also been conducted on mini-elements having 1.2 mm diameter holes In their mid-sections, some drilled before irradiation and others after irradiation to 22-83 atomic percent burnup. Uranium was lost to the coolant in direct proportion to the surface area of exposed core material. Pre-irradiation in the intact condition appeared to reduce in-reactor corrosion. Fuel cores developed for the NRU reactor are dimensionally very stable, swelling by only 6-8% at the very high burnup of 93 atomic percent. Two important factors contributing to this good performance are cylindrical clad restraint and coarse silicide particles. Thermal ramping tests were conducted on irradiated silicide aspersion fuels. Small segments of fuel cores released {sup 85}Kr starting at about 520 deg. C and peaking at about 680 deg C. After a holding period of 1 hour at 720 deg. C a secondary {sup 85}Kr peak occurred during cooling (at about 330 deg. C) probably due to thermal contraction cracking. Whole mini-elements irradiated to 93 atomic percent burnup were also ramped thermally, with encouraging results. After about 0.25 h at 530 deg. C the aluminum cladding developed very localized small blisters, some with penetrating pin-hole cracks preventing gross pillowing or ballooning. (author)

  13. X-ray photoemission spectromicroscopy of titanium silicide formation in patterned microstructures

    International Nuclear Information System (INIS)

    Singh, S.; Solak, H.; Cerrina, F.

    1997-01-01

    Titanium silicide has the lowest resistivity of all the refractory metal silicides and has good thermal stability as well as excellent compatibility with Al metallization. It is used as an intermediate buffer layer between W vias and the Si substrate to provide good electrical contact in ULSI technology, whose submicron patterned features form the basis of the integrated circuits of today and tomorrow, in the self aligned silicide (salicide) formation process. TiSi 2 exists in two phases: a metastable C49 base-centered orthorhombic phase with specific resistivity of 60-90 μΩ-cm that is formed at a lower temperature (formation anneal) and the stable 12-15 μΩ-cm resistivity face-centered orthorhombic C54 phase into which C49 is transformed with a higher temperature (conversion anneal) step. C54 is clearly the target for low resistivity VLSI interconnects. However, it has been observed that when dimensions shrink below 1/mic (or when the Ti thickness drops below several hundred angstroms), the transformation of C49 into C54 is inhibited and agglomeration often occurs in fine lines at high temperatures. This results in a rise in resistivity due to incomplete transformation to C54 and because of discontinuities in the interconnect line resulting from agglomeration. Spectromicroscopy is an appropriate tool to study the evolution of the TiSi2 formation process because of its high resolution chemical imaging ability which can detect bonding changes even in the absence of changes in the relative amounts of species and because of the capability of studying thick open-quotes as isclose quotes industrial samples

  14. X-ray photoemission spectromicroscopy of titanium silicide formation in patterned microstructures

    Energy Technology Data Exchange (ETDEWEB)

    Singh, S.; Solak, H.; Cerrina, F. [Univ. of Wisconsin-Madison, Stoughton, WI (United States)] [and others

    1997-04-01

    Titanium silicide has the lowest resistivity of all the refractory metal silicides and has good thermal stability as well as excellent compatibility with Al metallization. It is used as an intermediate buffer layer between W vias and the Si substrate to provide good electrical contact in ULSI technology, whose submicron patterned features form the basis of the integrated circuits of today and tomorrow, in the self aligned silicide (salicide) formation process. TiSi{sub 2} exists in two phases: a metastable C49 base-centered orthorhombic phase with specific resistivity of 60-90 {mu}{Omega}-cm that is formed at a lower temperature (formation anneal) and the stable 12-15 {mu}{Omega}-cm resistivity face-centered orthorhombic C54 phase into which C49 is transformed with a higher temperature (conversion anneal) step. C54 is clearly the target for low resistivity VLSI interconnects. However, it has been observed that when dimensions shrink below 1/mic (or when the Ti thickness drops below several hundred angstroms), the transformation of C49 into C54 is inhibited and agglomeration often occurs in fine lines at high temperatures. This results in a rise in resistivity due to incomplete transformation to C54 and because of discontinuities in the interconnect line resulting from agglomeration. Spectromicroscopy is an appropriate tool to study the evolution of the TiSi2 formation process because of its high resolution chemical imaging ability which can detect bonding changes even in the absence of changes in the relative amounts of species and because of the capability of studying thick {open_quotes}as is{close_quotes} industrial samples.

  15. Growth and sedimentation of fine particles produced in aqueous solutions of palladium sulfate and palladium sulfate-silver sulfate induced by gamma-ray irradiation

    International Nuclear Information System (INIS)

    Hatada, Motoyoshi; Jonah, C.D.

    1994-10-01

    It is known that palladium and palladium-silver fine particles were formed from deaerated aqueous solutions of palladium sulfate and palladium sulfate-silver sulfate induced by gamma-ray irradiation. Changes in particle size and with amount of particles in the solution with time during and after irradiation were studied using dynamic light scattering technique and UV spectrophotometer. The particles formed from palladium sulfate solution are found to be water-filled bulky particles of diameter of 200 nm, which grow by mutual coagulation even after irradiation was terminated. Average density depends on concentration of palladium ion in the solution and dose, and the lowest density was about 2 g/cm 3 for particles of 200 nm obtained from 0.06 mM solution by 2.4 kGy irradiation. The average density of the particles obtained from palladium sulfate-silver sulfate solutions was smaller than those obtained for the corresponding palladium sulfate solutions. Supersonic agitation destroyed coagulated precipitates to form fine particles, but did not form clusters of a few atoms. (author)

  16. Palladium-Catalyzed Atom-Transfer Radical Cyclization at Remote Unactivated C(sp3 )-H Sites: Hydrogen-Atom Transfer of Hybrid Vinyl Palladium Radical Intermediates.

    Science.gov (United States)

    Ratushnyy, Maxim; Parasram, Marvin; Wang, Yang; Gevorgyan, Vladimir

    2018-03-01

    A novel mild, visible-light-induced palladium-catalyzed hydrogen atom translocation/atom-transfer radical cyclization (HAT/ATRC) cascade has been developed. This protocol involves a 1,5-HAT process of previously unknown hybrid vinyl palladium radical intermediates, thus leading to iodomethyl carbo- and heterocyclic structures. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  17. Tungsten silicide contacts to polycrystalline silicon and silicon-germanium alloys

    International Nuclear Information System (INIS)

    Srinivasan, G.; Bain, M.F.; Bhattacharyya, S.; Baine, P.; Armstrong, B.M.; Gamble, H.S.; McNeill, D.W.

    2004-01-01

    Silicon-germanium alloy layers will be employed in the source-drain engineering of future MOS transistors. The use of this technology offers advantages in reducing series resistance and decreasing junction depth resulting in reduction in punch-through and SCE problems. The contact resistance of metal or metal silicides to the raised source-drain material is a serious issue at sub-micron dimensions and must be minimised. In this work, tungsten silicide produced by chemical vapour deposition has been investigated as a contact metallization scheme to both boron and phosphorus doped polycrystalline Si 1- x Ge x , with 0 ≤x ≤ 0.3. Cross bridge Kelvin resistor (CKBR) structures were fabricated incorporating CVD WSi 2 and polycrystalline SiGe. Tungsten silicide contacts to control polysilicon CKBR structures have been shown to be of high quality with specific contact resistance ρ c values 3 x 10 -7 ohm cm 2 and 6 x 10 -7 ohm cm 2 obtained to boron and phosphorus implanted samples respectively. The SiGe CKBR structures show that the inclusion of Ge yields a reduction in ρ c for both dopant types. The boron doped SiGe exhibits a reduction in ρ c from 3 x 10 -7 to 5 x 10 -8 ohm cm 2 as Ge fraction is increased from 0 to 0.3. The reduction in ρ c has been shown to be due to (i) the lowering of the tungsten silicide Schottky barrier height to p-type SiGe resulting from the energy band gap reduction, and (ii) increased activation of the implanted boron with increased Ge fraction. The phosphorus implanted samples show less sensitivity of ρ c to Ge fraction with a lowest value in this work of 3 x 10 -7 ohm cm 2 for a Ge fraction of 0.3. The reduction in specific contact resistance to the phosphorus implanted samples has been shown to be due to increased dopant activation alone

  18. The series production in a standardized fabrication line for silicide fuels and commercial aspects

    International Nuclear Information System (INIS)

    Wehner, E.L.; Hassel, H.W.

    1987-01-01

    NUKEM has been responsible for the development and fabrication of LEU fuel elements for MTR reactors under the frame of the German AF program since 1979. The AF program is part of the international RERTR efforts, which were initiated by the INFCE Group in 1978. This paper describes the actual status of development and the transition from the prototype to the series production in a standardized manufacturing line for silicide fuels at NUKEM. Technical provisions and a customer oriented standardized product range aim at an economized manufacturing. (Author)

  19. Current enhancement in crystalline silicon photovoltaic by low-cost nickel silicide back contact

    KAUST Repository

    Bahabry, R. R.; Gumus, A.; Kutbee, A. T.; Wehbe, N.; Ahmed, S. M.; Ghoneim, M. T.; Lee, K. -T.; Rogers, J. A.; Hussain, M. M.

    2016-01-01

    We report short circuit current (Jsc) enhancement in crystalline silicon (C-Si) photovoltaic (PV) using low-cost Ohmic contact engineering by integration of Nickel mono-silicide (NiSi) for back contact metallization as an alternative to the status quo of using expensive screen printed silver (Ag). We show 2.6 mA/cm2 enhancement in the short circuit current (Jsc) and 1.2 % increment in the efficiency by improving the current collection due to the low specific contact resistance of the NiSi on the heavily Boron (B) doped Silicon (Si) interface.

  20. Current enhancement in crystalline silicon photovoltaic by low-cost nickel silicide back contact

    KAUST Repository

    Bahabry, R. R.

    2016-11-30

    We report short circuit current (Jsc) enhancement in crystalline silicon (C-Si) photovoltaic (PV) using low-cost Ohmic contact engineering by integration of Nickel mono-silicide (NiSi) for back contact metallization as an alternative to the status quo of using expensive screen printed silver (Ag). We show 2.6 mA/cm2 enhancement in the short circuit current (Jsc) and 1.2 % increment in the efficiency by improving the current collection due to the low specific contact resistance of the NiSi on the heavily Boron (B) doped Silicon (Si) interface.

  1. Estimations on uranium silicide fuel prototypes for their irradiation and postirradiation

    International Nuclear Information System (INIS)

    Sbaffoni, Maria M.

    2000-01-01

    The 'Silicide' project includes the qualification of this type of research reactor fuel to be used i.e. in the Argentine RA-3 and to confirm CNEA's role as an international supplier. The present paper shows complementary basic information for P-04 prototype post-irradiation, which is already under way, and some parameter values related to the new P-06 prototype to be taken into account for planning its irradiation and post-irradiation. The reliability of these values has been evaluated through comparison with experimental results. The reported results contribute, also, to a parallel study on the nuclear data libraries used in calculations for this type of reactor. (author)

  2. Fexofenadine Suppresses Delayed-Type Hypersensitivity in the Murine Model of Palladium Allergy

    Directory of Open Access Journals (Sweden)

    Ryota Matsubara

    2017-06-01

    Full Text Available Palladium is frequently used in dental materials, and sometimes causes metal allergy. It has been suggested that the immune response by palladium-specific T cells may be responsible for the pathogenesis of delayed-type hypersensitivity in study of palladium allergic model mice. In the clinical setting, glucocorticoids and antihistamine drugs are commonly used for treatment of contact dermatitis. However, the precise mechanism of immune suppression in palladium allergy remains unknown. We investigated inhibition of the immune response in palladium allergic mice by administration of prednisolone as a glucocorticoid and fexofenadine hydrochloride as an antihistamine. Compared with glucocorticoids, fexofenadine hydrochloride significantly suppressed the number of T cells by interfering with the development of antigen-presenting cells from the sensitization phase. Our results suggest that antihistamine has a beneficial effect on the treatment of palladium allergy compared to glucocorticoids.

  3. Effect of Utilization of Silicide Fuel with the Density 4.8 gU/cc on the Kinetic Parameters of RSG-GAS Reactor

    International Nuclear Information System (INIS)

    Setiyanto; Sembiring, Tagor M.; Pinem, Surian

    2007-01-01

    Presently, the RSG-GAS reactor using silicide fuel element of 2.96 gU/cc. For increasing reactor operation time, its planning to change to higher density fuel. The kinetic calculation of silicide core with density 4.8 gU/cc has been carried out, since it has an influence on the reactor operation safety. The calculated kinetic parameters are the effective delayed neutron fraction, the delayed neutron decay constant, prompt neutron lifetime and feedback reactivity coefficient very important for reactor operation safety. the calculation is performed in 2-dimensional neutron diffusion-perturbation method using modified Batan-2DIFF code. The calculation showed that the effective delayed neutron fraction is 7. 03256x10 -03 , total delay neutron time constant is 7.85820x10 -02 s -1 and the prompt neutron lifetime is 55.4900 μs. The result of prompt neutron lifetime smaller 10 % compare with silicide fuel of 4.8 gU/cc. The calculated results showed that all of the feedback reactivity coefficient silicide core 4.8 gU/cc is negative. Totally, the feedback reactivity coefficient of silicide fuel of 4.8 gU/cc is 10% less than that of silicide fuel of 2.96 gU/cc. The results shown that kinetic parameters result decrease compared with the silicide core with density 2.96 gU/cc, but no significant influence in the RSG-GAS reactor operation. (author)

  4. Method for recovering palladium and technetium values from nuclear fuel reprocessing waste solutions

    Science.gov (United States)

    Horwitz, E. Philip; Delphin, Walter H.

    1979-07-24

    A method for recovering palladium and technetium values from nuclear fuel reprocessing waste solutions containing these and other values by contacting the waste solution with an extractant of tricaprylmethylammonium nitrate in an inert hydrocarbon diluent which extracts the palladium and technetium values from the waste solution. The palladium and technetium values are recovered from the extractant and from any other coextracted values with a strong nitric acid strip solution.

  5. Preparation of Palladium/Silver-Coated Polyimide Nanotubes: Flexible, Electrically Conductive Fibers

    OpenAIRE

    Lushi Kong; Guanchun Rui; Guangyu Wang; Rundong Huang; Ran Li; Jiajie Yu; Shengli Qi; Dezhen Wu

    2017-01-01

    A simple and practical method for coating palladium/silver nanoparticles on polyimide (PI) nanotubes is developed. The key steps involved in the process are silver ion exchange/reduction and displacement reactions between silver and palladium ions. With the addition of silver, the conductivity of the PI nanotubes is greatly enhanced. Further, the polyimide nanotubes with a dense, homogeneous coating of palladium nanoparticles remain flexible after heat treatment and show the possibility for u...

  6. Surface topography of a palladium cathode after electrolysis in heavy water

    International Nuclear Information System (INIS)

    Silver, D.S.; Dash, J.; Keefe, P.S.

    1993-01-01

    Electrolysis was performed with a palladium cathode and an electrolyte containing both hydrogen and deuterium ions. The cathode bends toward the anode during this process. Examination of both the concave and the convex surfaces with the scanning electron microscope, scanning tunneling microscope, and atomic force microscope shows unusual surface characteristics. Rimmed craters with faceted crystals inside and multitextural surfaces were observed on an electrolyzed palladium cathode but not on palladium that has not been electrolyzed. 9 refs., 9 figs

  7. Determination of the Debye-Waller Factor of hydrogen in Palladium and Palladium Silver alloy

    International Nuclear Information System (INIS)

    Khodabakhsh, R.

    1986-01-01

    The mean square amplitude of the vibrating hydrogen in metals can be determined by using coherent elastic neutron scattering experiments, inelastic one-phonon scattering measurements. To determine the D.W.F. Debye-Waller Factor from the coherent elastic scattering measurements, information about the positions of atoms within the unit is required, and vice versa. The main difficulty concerning the determination of the D.W.F. from the inelastic experiment is in elimination of multi-phonon contribution from the measured spectrum. However, the D.W.F. of hydrogen in palladium has been usually determined by the intensity of the quasi-elastic line. An integration of the measured scattering law S(Q,W) at constant Q, over a certain energy window ΔE, results in the quasi-elastic intensity. To obtain an accurate result, this window has to be chosen large enough to comprise most of the quasi-elastic line, but sufficiently small so that the phonon contributions are small. The MARX spectrometer is ideally constructed for this type of measurement where the window is about +-1 Mev for incident neutron wavelength, =4.115 A. Thus, the quasi-elastic scattering method was considered the best method of determining the D.W.F. of hydrogen in palladium using the MARX spectrometer. However, if the acoustic part overlaps with the quasi-elastic part, one has to obtain the D.W.F. by fitting the data to a quasi-elastic model. The work to be reported here is the investigation of variations of the D.W.F. of hydrogen in Pd and PdAgsub(0.085) with temperature and extension of the available data to as high a temperature as possible. Therefore the integrated intensity of incoherent quasi-elastic neutron scattering by proton in polycrystallin Pd/H and PdAgsub(0.085)/H was investigated as a function of the scattering vector Q. A quasi-harmonic D.W.F. behaviour was observed at elevated temperatures. The observed Debye-Waller Factor depends strongly on the form of the amplitude weighted frequency

  8. Noise temperature measurements for the determination of the thermodynamic temperature of the melting point of palladium

    Energy Technology Data Exchange (ETDEWEB)

    Edler, F.; Kuhne, M.; Tegeler, E. [Bundesanstalt Physikalisch-Technische, Berlin (Germany)

    2004-02-01

    The thermodynamic temperature of the melting point of palladium in air was measured by noise thermometric methods. The temperature measurement was based on noise comparison using a two-channel arrangement to eliminate parasitic noises of electronic components by cross correlation. Three miniature fixed points filled with pure palladium (purity: {approx}99.99%, mass: {approx}90 g) were used to realize the melts of the fixed point metal. The measured melting temperature of palladium in air amounted to 1552.95 deg C {+-} 0.21 K (k = 2). This temperature is 0.45 K lower than the temperature of the melting point of palladium measured by radiation thermometry. (authors)

  9. Preliminary investigations on the use of uranium silicide targets for fission Mo-99 production

    Energy Technology Data Exchange (ETDEWEB)

    Cols, H.; Cristini, P.; Marques, R.

    1997-08-01

    The National Atomic Energy Commission (CNEA) of Argentine Republic owns and operates an installation for production of molybdenum-99 from fission products since 1985, and, since 1991, covers the whole national demand of this nuclide, carrying out a program of weekly productions, achieving an average activity of 13 terabecquerel per week. At present they are finishing an enlargement of the production plant that will allow an increase in the volume of production to about one hundred of terabecquerel. Irradiation targets are uranium/aluminium alloy with 90% enriched uranium with aluminium cladding. In view of international trends held at present for replacing high enrichment uranium (HEU) for enrichment values lower than 20 % (LEU), since 1990 the authors are in contact with the RERTR program, beginning with tests to adapt their separation process to new irradiation target conditions. Uranium silicide (U{sub 3}Si{sub 2}) was chosen as the testing material, because it has an uranium mass per volume unit, so that it allows to reduce enrichment to a value of 20%. CNEA has the technology for manufacturing miniplates of uranium silicide for their purposes. In this way, equivalent amounts of Molybdenum-99 could be obtained with no substantial changes in target parameters and irradiation conditions established for the current process with Al/U alloy. This paper shows results achieved on the use of this new target.

  10. Microstructure of the irradiated U 3Si 2/Al silicide dispersion fuel

    Science.gov (United States)

    Gan, J.; Keiser, D. D.; Miller, B. D.; Jue, J.-F.; Robinson, A. B.; Madden, J. W.; Medvedev, P. G.; Wachs, D. M.

    2011-12-01

    The silicide dispersion fuel of U 3Si 2/Al is recognized as the best performance fuel for many nuclear research and test reactors with up to 4.8 gU/cm 3 fuel loading. An irradiated U 3Si 2/Al dispersion fuel ( 235U ˜ 75%) from the high-flux side of a fuel plate (U0R040) from the Reduced Enrichment for Research and Test Reactors (RERTR)-8 test was characterized using transmission electron microscopy (TEM). The fuel was irradiated in the Advanced Test Reactor (ATR) for 105 days. The average irradiation temperature and fission density of the U 3Si 2 fuel particles for the TEM sample are estimated to be approximately 110 °C and 5.4 × 10 27 f/m 3. The characterization was performed using a 200-kV TEM. The U/Si ratio for the fuel particle and (Si + Al)/U for the fuel-matrix-interaction layer are approximately 1.1 and 4-10, respectively. The estimated average diameter, number density and volume fraction for small bubbles (<1 μm) in the fuel particle are ˜94 nm, 1.05 × 10 20 m -3 and ˜11%, respectively. The results and their implication on the performance of the U 3Si 2/Al silicide dispersion fuel are discussed.

  11. Prospect of Uranium Silicide fuel element with hypostoichiometric (Si ≤3.7%)

    International Nuclear Information System (INIS)

    Suripto, A.; Sardjono; Martoyo

    1996-01-01

    An attempt to obtain high uranium-loading in silicide dispersion fuel element using the fabrication technology applicable nowadays can reach Uranium-loading slightly above 5 gU/cm 3 . It is difficult to achieve a higher uranium-loading than that because of fabricability constraints. To overcome those difficulties, the use of uranium silicide U 3 Si based is considered. The excess of U is obtained by synthesising U 3 Si 2 in Si-hypostoichiometric stage, without applying heat treatment to the ingot as it can generate undesired U 3 Si. The U U will react with the matrix to form U al x compound, that its pressure is tolerable. This experiment is to consider possibilities of employing the U 3 Si 2 as nuclear fuel element which have been performed by synthesising U 3 Si 2 -U with the composition of 3.7 % weigh and 3 % weigh U. The ingot was obtained and converted into powder form which then was fabricated into experimental plate nuclear fuel element. The interaction between free U and Al-matrix during heat-treatment is the rolling phase of the fuel element was observed. The study of the next phase will be conducted later

  12. CEMS Investigations of Fe-Silicide Phases Formed by the Method of Concentration Controlled Phase Selection

    Energy Technology Data Exchange (ETDEWEB)

    Moodley, M. K.; Bharuth-Ram, K. [University of Durban-Westville, Physics Department (South Africa); Waal, H. de; Pretorius, R. [University of Stellenbosch, Physics Department (South Africa)

    2002-03-15

    Conversion electron Moessbauer spectroscopy (CEMS) measurements have been made on Fe-silicide samples formed using the method of concentration controlled phase selection. To prepare the samples a 10 nm layer of Fe{sub 30}M{sub 70} (M=Cr, Ni) was evaporated onto Si(100) surfaces, followed by evaporation of a 60 nm Fe layer. Diffusion of the Fe into the Si substrate and the formation of different Fe-Si phases was achieved by subjecting the evaporated samples to a series of heating stages, which consisted of (a) a 10 min anneal at 800 deg. C plus etch of the residual surface layer, (b) a further 3 hr anneal at 800 deg. C, (c) a 60 mJ excimer laser anneal to an energy density of 0.8 J/cm{sup 2}, and (d) a final 3 hr anneal at 800 deg. C. CEMS measurements were used to track the Fe-silicide phases formed. The CEMS spectra consisted of doublets which, based on established hyperfine parameters, could be assigned to {alpha}- or {beta}-FeSi{sub 2} or cubic FeSi. The spectra showed that {beta}-FeSi{sub 2} had formed already at the first annealing stage. Excimer laser annealing resulted in the formation of a phase with hyperfine parameters consistent with those of {alpha}-FeSi{sub 2}. A further 3 hr anneal at 800 deg. C resulted in complete reversal to the semiconducting {beta}-FeSi{sub 2} phase.

  13. Mössbauer spectroscopy study of surfactant sputtering induced Fe silicide formation on a Si surface

    Energy Technology Data Exchange (ETDEWEB)

    Beckmann, C.; Zhang, K. [2nd Institute of Physics, University of Göttingen, Friedrich-Hund-Platz 1, 37077 Göttingen (Germany); Hofsäss, H., E-mail: hans.hofsaess@phys.uni-goettingen.de [2nd Institute of Physics, University of Göttingen, Friedrich-Hund-Platz 1, 37077 Göttingen (Germany); Brüsewitz, C.; Vetter, U. [2nd Institute of Physics, University of Göttingen, Friedrich-Hund-Platz 1, 37077 Göttingen (Germany); Bharuth-Ram, K. [Physics Department, Durban University of Technology, Durban 4001 (South Africa)

    2015-12-01

    Highlights: • We study the formation of self-organized nanoscale dot and ripple patterns on Si. • Patterns are created by keV noble gas ion irradiation and simultaneous {sup 57}Fe co-deposition. • Ion-induced phase separation and the formation of a-FeSi{sub 2} is identified as relevant process. - Abstract: The formation of Fe silicides in surface ripple patterns, generated by erosion of a Si surface with keV Ar and Xe ions and simultaneous co-deposition of Fe, was investigated with conversion electron Mössbauer spectroscopy, atomic force microscopy and Rutherford backscattering spectrometry. For the dot and ripple patterns studied, we find an average Fe concentration in the irradiated layer between 6 and 25 at.%. The Mössbauer spectra clearly show evidence of the formation of Fe disilicides with Fe content close to 33 at.%, but very little evidence of the formation of metallic Fe particles. The results support the process of ion-induced phase separation toward an amorphous Fe disilicide phase as pattern generation mechanism. The observed amorphous phase is in agreement with thermodynamic calculations of amorphous Fe silicides.

  14. Impact of Nickel silicide Rear Metallization on Series Resistance of Crystalline Silicon Solar Cells

    KAUST Repository

    Bahabry, Rabab R

    2018-01-11

    The Silicon-based solar cell is one of the most important enablers toward high efficiency and low-cost clean energy resource. Metallization of silicon-based solar cells typically utilizes screen printed silver-Aluminium (Ag-Al) which affects the optimal electrical performance. To date, metal silicide-based ohmic contacts are occasionally used as an alternative candidate only to the front contact grid lines in crystalline silicon (c-Si) based solar cells. In this paper, we investigate the electrical characteristics of nickel mono-silicide (NiSi)/Cu-Al ohmic contact on the rear side of c-Si solar cells. We observe a significant enhancement in the fill factor of around 6.5% for NiSi/Cu-Al rear contacts leading to increasing the efficiency by 1.2% compared to Ag-Al. This is attributed to the improvement of the parasitic resistance in which the series resistance decreased by 0.737 Ω.cm². Further, we complement experimental observation with a simulation of different contact resistance values, which manifests NiSi/Cu-Al rear contact as a promising low-cost metallization for c-Si solar cells with enhanced efficiency.

  15. Magnesium and Manganese Silicides For Efficient And Low Cost Thermo-Electric Power Generation

    Energy Technology Data Exchange (ETDEWEB)

    Trivedi, Sudhir B. [Brimrose Technology Corporation; Kutcher, Susan W. [Brimrose Technology Corporation; Rosemeier, Cory A. [Brimrose Technology Corporation; Mayers, David [Brimrose Technology Corporation; Singh, Jogender [Pennsylvania State University

    2013-12-02

    Thermoelectric Power Generation (TEPG) is the most efficient and commercially deployable power generation technology for harvesting wasted heat from such things as automobile exhausts, industrial furnaces, and incinerators, and converting it into usable electrical power. We investigated the materials magnesium silicide (Mg2Si) and manganese silicide (MnSi) for TEG. MgSi2 and MnSi are environmentally friendly, have constituent elements that are abundant in the earth's crust, non-toxic, lighter and cheaper. In Phase I, we successfully produced Mg2Si and MnSi material with good TE properties. We developed a novel technique to synthesize Mg2Si with good crystalline quality, which is normally very difficult due to high Mg vapor pressure and its corrosive nature. We produced n-type Mg2Si and p-type MnSi nanocomposite pellets using FAST. Measurements of resistivity and voltage under a temperature gradient indicated a Seebeck coefficient of roughly 120 V/K on average per leg, which is quite respectable. Results indicated however, that issues related to bonding resulted in high resistivity contacts. Determining a bonding process and bonding material that can provide ohmic contact from room temperature to the operating temperature is an essential part of successful device fabrication. Work continues in the development of a process for reproducibly obtaining low resistance electrical contacts.

  16. Influence of iron and beryllium additions on heat resistance of silicide coatings on TsMB-30 molybdenum alloy

    International Nuclear Information System (INIS)

    Zajtseva, A.L.; Fedorchuk, N.M.; Lazarev, Eh.M.; Korotkov, N.A.

    1985-01-01

    Alloying of titanium modified silicide coatings on TsMB-30 molybdenum alloy with iron or beryllium is stated to improve their protective properties. Coatings with low content of alloying elements have the best protective properties. Service life of coatings is determined by the formed oxide film and phase transformations taking place in the coating

  17. Aluminium alloyed iron-silicide/silicon solar cells: A simple approach for low cost environmental-friendly photovoltaic technology.

    Science.gov (United States)

    Kumar Dalapati, Goutam; Masudy-Panah, Saeid; Kumar, Avishek; Cheh Tan, Cheng; Ru Tan, Hui; Chi, Dongzhi

    2015-12-03

    This work demonstrates the fabrication of silicide/silicon based solar cell towards the development of low cost and environmental friendly photovoltaic technology. A heterostructure solar cells using metallic alpha phase (α-phase) aluminum alloyed iron silicide (FeSi(Al)) on n-type silicon is fabricated with an efficiency of 0.8%. The fabricated device has an open circuit voltage and fill-factor of 240 mV and 60%, respectively. Performance of the device was improved by about 7 fold to 5.1% through the interface engineering. The α-phase FeSi(Al)/silicon solar cell devices have promising photovoltaic characteristic with an open circuit voltage, short-circuit current and a fill factor (FF) of 425 mV, 18.5 mA/cm(2), and 64%, respectively. The significant improvement of α-phase FeSi(Al)/n-Si solar cells is due to the formation p(+-)n homojunction through the formation of re-grown crystalline silicon layer (~5-10 nm) at the silicide/silicon interface. Thickness of the regrown silicon layer is crucial for the silicide/silicon based photovoltaic devices. Performance of the α-FeSi(Al)/n-Si solar cells significantly depends on the thickness of α-FeSi(Al) layer and process temperature during the device fabrication. This study will open up new opportunities for the Si based photovoltaic technology using a simple, sustainable, and los cost method.

  18. Towards the improvement of the oxidation resistance of Nb-silicides in situ composites: A solid state diffusion approach

    International Nuclear Information System (INIS)

    Mathieu, S.; Knittel, S.; François, M.; Portebois, L.; Mathieu, S.; Vilasi, M.

    2014-01-01

    Highlights: •Local equilibrium is attained during oxidation at phase boundaries (steady state conditions). •A solid state diffusion model explains the oxidation mechanism of Nb-silicides composites. •The Nb ss fraction is not the only parameters governing the oxidation rate of Nb-silicides. •Aluminium increases the thermodynamic activity of Si in the Nb-silicides composites. •The results indicate the need to develop a Nb–Ti–Hf–Al–Cr–Si thermodynamic database. -- Abstract: The present study focuses on the oxidation mechanism of Nb-silicide composites and on the effect of the composition on the oxidation rate at 1100 °C. A theoretical approach is proposed based on experimental results and used to optimise the oxidation resistance. The growth model based on multiphase diffusion was experimentally tested and confirmed by manufacturing seven composites with different compositions. It was also found that the effect of the composition has to be evaluated at 1100 °C within a short time duration (50 h), where the oxide scale and the internal oxidation zone both grow according to parabolic kinetics

  19. Kinetic Characteristics of Hydrogen Transfer Through Palladium-Modified Membrane

    Science.gov (United States)

    Petriev, I. S.; Frolov, V. Yu.; Bolotin, S. N.; Baryshev, M. G.; Kopytov, G. F.

    2018-01-01

    The paper deals with hydrogen transfer through Pd-23%Ag alloy membrane, the surface of which is modified by the electrolytic deposition of highly dispersed palladium. The dependence between the density of hydrogen flow and its excess pressure on the input surface of membrane is well approximated by the first-order curve. This fact indicates that the process of hydrogen permeability is defined by its dissociation on the input surface. Activation energy of this process is 47.9 kJ/mol which considerably exceeds that of the process of hydrogen transfer through palladium (22-30 kJ/mol). This confirms the fact that the chemisorption is a rate-controlling step of the hydrogen transfer through membrane.

  20. Analysis of the anomalous hydrogen solubilities in deformed palladiums

    Energy Technology Data Exchange (ETDEWEB)

    Park, Choong Nyeon; Lee, Ho Jong

    1987-02-01

    The anomalous hydrogen solubilities in the deformed palladiums were analyzed by empolying modified Kirchheim's model with considering the partially coherent strain energy which would induced during hydride precipitation around edge dislocations. The dislocation densities, obtained by this model, of the various cold worked and/or reversible US transformed palladium samples were the order of 10/sup 11/cm/sup -2/. The partially coherent strain energies were about 3 kJ/molH and nearly same in the various samples. This value could be compared with the incoherent strain energy, 0.4kJ/molH, which was obtained from the hysteresis on P-C isotherm, and the coherent strain energy calulated, 9.6kJ/molH.

  1. Hydrogenation of carbon monoxide over supported palladium catalysts

    Energy Technology Data Exchange (ETDEWEB)

    Fujimoto, K.; Hashimoto, H.; Kunugi, T.

    1978-03-01

    An alumina-supported 2% palladium catalyst had higher activity for carbon monoxide hydrogenation than a silica-supported 2% palladium catalyst, at 250/sup 0/-400/sup 0/C and 1 atm. The addition of lanthanum oxide or thorium oxide, but not of potassium oxide, to the silica-supported catalyst increased the conversion at 350/sup 0/C from 1.1% to 81.0% with a selectivity of 56.1% for methane, 1.4% for C/sub 2/ compounds, 0.1% for C/sub 3/ compounds, and 42.5% for carbon dioxide. Temperature-programed desorption of carbon monoxide in a hydrogen stream showed that of two desorption peaks observed for carbon monoxide, the one at higher temperature corresponded to the carbon monoxide species which hydrogenates to methane and that the area of this peak increased with increasing thorium content of the catalyst. Graphs, tables, and 12 references.

  2. Adlayers of palladium particles and their aggregates on porous polypropylene hollow fiber membranes as hydrogenization contractors/reactors

    NARCIS (Netherlands)

    Volkov, V.V.; Lebedeva, V.I.; Petrova, I.V.; Bobyl, A.V.; Konnikov, S.G.; Roldughin, V.I.; Erkel, J. van; Tereshchenko, G.F.

    2011-01-01

    Principal approaches for the preparation of catalytic membrane reactors based on polymer membranes containing palladium nanoparticles and for the description of their characteristics are presented. The method for the development of adlayers composed of palladium nanoparticles and their aggregates on

  3. Co-deposition of palladium with hydrogen isotopes

    International Nuclear Information System (INIS)

    Dash, J.; Ambadkar, A.

    2006-01-01

    Palladium was co-deposited with hydrogen isotopes on a Pd cathode. This resulted in enhanced production of excess thermal power. After electrolysis the Pd Lβ/ Lα ratio was found to be increased in characteristic X-ray spectra from localized, microscopic areas on the surface of the Pd cathode. This suggests the possibility that appreciable amounts of silver are present in these areas. (authors)

  4. Unsupported palladium alloy membranes and methods of making same

    Science.gov (United States)

    Way, J. Douglas; Thoen, Paul; Gade, Sabina K.

    2015-06-02

    The invention provides support-free palladium membranes and methods of making these membranes. Single-gas testing of the unsupported foils produced hydrogen permeabilities equivalent to thicker membranes produced by cold-rolling. Defect-free films as thin as 7.2 microns can be fabricated, with ideal H.sub.2/N.sub.2 selectivities as high as 40,000. Homogeneous membrane compositions may also be produced using these methods.

  5. Interaction of CO with Palladium Supported on Oxidized Tungsten

    Czech Academy of Sciences Publication Activity Database

    Jirka, Ivan; Plšek, Jan; Šutara, F.; Matolín, V.; Cháb, Vladimír; Prince, K. C.

    2006-01-01

    Roč. 110, č. 47 (2006), s. 23837-23844 ISSN 1520-6106 R&D Projects: GA ČR GA202/05/0244; GA AV ČR IAA1010413 Institutional research plan: CEZ:AV0Z40400503; CEZ:AV0Z10100521 Keywords : palladium * WOx surfaces * TPD Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 4.115, year: 2006

  6. Application of Colloidal Palladium Nanoparticles for Labeling in Electron Microscopy

    Czech Academy of Sciences Publication Activity Database

    Vancová, Marie; Šlouf, Miroslav; Langhans, Jan; Pavlová, Eva; Nebesářová, Jana

    2011-01-01

    Roč. 17, č. 5 (2011), s. 810-816 ISSN 1431-9276 R&D Projects: GA AV ČR KAN200520704; GA AV ČR KJB600960906; GA ČR GAP205/10/0348 Institutional research plan: CEZ:AV0Z60220518; CEZ:AV0Z40500505 Keywords : electron microscopy * colloidal palladium * nanoparticles * labeling * salivary glands * Ixodes ricinus Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 3.007, year: 2011

  7. Influence of Al addition on phase transformation and thermal stability of nickel silicides on Si(0 0 1)

    International Nuclear Information System (INIS)

    Huang, Shih-Hsien; Twan, Sheng-Chen; Cheng, Shao-Liang; Lee, Tu; Hu, Jung-Chih; Chen, Lien-Tai; Lee, Sheng-Wei

    2014-01-01

    Highlights: ► The presence of Al slows down the Ni 2 Si–NiSi phase transformation but significantly promotes the NiSi 2−x Al x formation. ► The behavior of phase transformation strongly depends on the Al concentration of the initial Ni 1−x Al x alloys. ► The Ni 0.91 Al 0.09 /Si system exhibits remarkably improved thermal stability, even after high temperature annealing for 1000 s. ► The relationship between microstructures, electrical property, and thermal stability of Ni(Al) silicides is discussed. -- Abstract: The influence of Al addition on the phase transformation and thermal stability of Ni silicides on (0 0 1)Si has been systematically investigated. The presence of Al atoms is found to slow down the Ni 2 Si–NiSi phase transformation but significantly promote the NiSi 2−x Al x formation during annealing. The behavior of phase transformation strongly depends on the Al concentration of the initial Ni 1−x Al x alloys. Compared to the Ni 0.95 Pt 0.05 /Si and Ni 0.95 Al 0.05 /Si system, the Ni 0.91 Al 0.09 /Si sample exhibits remarkably enhanced thermal stability, even after high temperature annealing for 1000 s. The relationship between microstructures, electrical property, and thermal stability of Ni silicides is discussed to elucidate the role of Al during the Ni 1−x Al x alloy silicidation. This work demonstrated that thermally stable Ni 1−x Al x alloy silicides would be a promising candidate as source/drain (S/D) contacts in advanced complementary metal–oxide-semiconductor (CMOS) devices

  8. HE3 outgassing from four working palladium and uranium beds

    International Nuclear Information System (INIS)

    Souers, P. C.; Coronado, P. R.; Fearon, F. M.; Garza, R. G.; Shaw , J. F.; Stump, R. K.; Tsugawa, R. T.

    1988-01-01

    The He 3 output from two palladium and two uranium beds storing T 2 and D-T was studied as a function of time. Three of the beds were started new and watched for a year; the fourth bed was twelve years old. All four were beds used in routine tritium handling. Initial stoichiometries were PdT/sub 0.3/ and UT/sub 0.7/ so that both operated at similar 1 to 130 kPa pressures. The He 3 from palladium ranged from the 0.002 mo1% lower level of sensitivity to 0.01% for PdT 2 at one year of age. The UT system showed 0.1% He 3 at 4 to 62 days and 0.1 to 10% at longer times, with the first cuts being high in He 3 . The palladium bed with 95 to 97% pure T 2 enriches the output to as high as 97 to 99%. 9 refs., 1 fig., 2 tabs

  9. Substoichiometric extraction of traces of gold and palladium

    International Nuclear Information System (INIS)

    Colonat, J.-F.

    1975-01-01

    Several systems for extracting palladium at concentrations ranging from 10 -4 to 10 -6 M/l were studied. Extraction by dithizone is limited by the transformation of the primary complex into a secondary complex which takes place at concentrations around 10 -6 M. This transformation has been demonstrated kinetically. Dimethylglyoxime is an interesting reagent in substoichiometry, in spite of its comparatively low extraction constant. Various complexes which are formed in a highly chlorinated medium have been proposed. Use of copper diethyldithiocarbamate is limited principally by its stability in presence of chlorine ions. The kinetic formation of palladium diethyldithiocarbamate has been studied with greater precision. A direct determination of 100μg of palladium in a copper matrix without preliminary separation has given results comparable in every way with those of other methods. In the case of gold (III) the constants of formation with the diethyldithiocarbamate ion have been determined by an iterative method of calculation, using the influence curves of interfering metals. Finally conditions for an automatization of the substoichiometric extraction, as well as its possibilities for gold determination in the range 200-20ppm, were proposed [fr

  10. Arsenic (III Adsorption Using Palladium Nanoparticles from Aqueous Solution

    Directory of Open Access Journals (Sweden)

    Farzaneh Arsiya

    2017-07-01

    Full Text Available The presence of Arsenic in drinking water is the greatest threat to health effects especially in water. The purpose of this study is application of green palladium nanoparticles for removal of trivalent Arsenic from aqueous solutions and also the impact of some factors such as retention time, pH, concentration of palladium nanoparticles and Arsenic concentrations was studied. The values for Arsenic removal from aqueous solutions were measured by furnace atomic adsorption spectrometry (Conter AA700. In the study, Langmuir and Freundlich isotherm models and pseudo-second order kinetic model were studied. The results of  optimization is shown that 0.5 g of nanoparticles can removed %99.8 of Arsenic with initial concentration of  0.5 g/l, in 5 minutes at pH=4. Langmuir model, Freundlich model (R2=0.94 and pseudo-second order kinetic model (R2=0.99 shown high correlation for removing of Arsenic from aqueous solutions. It was found, palladium nanoparticles can be used as an efficient method to remove Arsenic from aqueous solutions in a short time.

  11. Recovery of hydrogen from impurities using a palladium membrane reactor

    International Nuclear Information System (INIS)

    Willms, R.S.; Okuno, K.

    1993-01-01

    One of the important steps in processing the exhaust from a fusion reactor is recovering tritium which is incorporated into molecules such as water and methane. One device which may prove to be very effective for this purpose is a palladium membrane reactor. This is a reactor which incorporates a Pd/Ag membrane in the reactor geometry. Reactions such as water gas shift, steam reforming and methane cracking can be carried out over the reactor catalyst, and the product hydrogen can be simultaneously removed from the reacting mixture. Because product is removed, greater than usual conversions can be obtained. In addition ultrapure hydrogen is produced, eliminating the need for an additional processing step. A palladium membrane reactor has been built and tested with three different catalysts. Initial results with a Ni-based catalyst show that it is very effective at promoting all three reactions listed above. Under the proper conditions, hydrogen recoveries approaching 100% have been observed. This study serves to experimentally validate the palladium membrane reactor as potentially important tool for fusion fuel processing

  12. Core conversion study from silicide to molybdenum fuel in the Indonesian 30 MW multipurpose reactor G.A. Siwabessy (RSG-GAS)

    International Nuclear Information System (INIS)

    Sembiring, T.M.; Kuntoro, I.

    2005-01-01

    This paper describes the core conversion from silicide to molybdenum core through a series of silicide (2.96 gU cm -3 ) - molybdenum (3.55 gUcm -3 ) mixed transition cores for the Indonesian 30 MW-Multipurpose G.A. Siwabessy (RSGGAS) reactor. The core calculations are carried out using the two-dimensional multigroup neutron diffusion method code of Batan-EQUIL-2D. The calculated results showed that the proposed silicide-molybdenum mixed transition cores, using the same refueling/reshuffling scheme, meet the safety criteria and it can be used in safely converting from an all-silicide core to an all-molybdenum core. (author)

  13. Palladium alloy membrane process for the treatment of hydrogen isotopes

    Energy Technology Data Exchange (ETDEWEB)

    Chung, Hongsuk; Paek, Seungwoo; Lee, Minsoo; Kim, Kwangrag; Yim, Sungpaal; Ahn, Dohee [KAERI, Daejeon (Korea, Republic of); Shim, Myunghwa [Univ. of Science and Technology, Daejeon (Korea, Republic of)

    2005-11-15

    Tritium is a radioactive isotope of hydrogen and it has a half-life of 12.3 years; it decays to He-3 by emitting a low energy beta radiation with an average energy of 5.7 keV and a maximum energy of 18.6 keV. Transfer of environmentally tritiated water to humans takes place via an inhalation, diffusion through the skin and ingestion. Radioactive waste containing tritium is continuously generated by the nuclear industry in, for example, nuclear reactor operations and a radioisotope production, as well as in medical research. Methods for removing tritium from liquid waste provide an alternative to the control of tritium emissions and a personnel exposure. A combined electrolysis and catalytic exchange process is a very effective method to remove small quantities of tritium from light or heavy waste water streams. The process consists of three main steps: (a) A front end step that exchanges the tritium to a less toxic hydrogen phase. This can be performed either through a chemical exchange in the presence of a platinum supported catalyst or through the decomposition of water. (b) A back end process that purifies the tritiated hydrogen gas which evolved from the electrolysis. This can be performed through a palladium alloy membrane separator. (c) A means of storing the concentrated gas safely. Uranium is used if the storage is temporary; titanium is usually employed for long term storage. To gain a better understanding of the tritiated hydrogen gas purification process, a mathematical model of the palladium alloy membrane has been used. This model is described herein, and the representative results of the model calculations are presented. The authors selected the palladium alloy membrane for the hydrogen purification process by considering the membrane properties, such as a chemical resistance, mechanical stability, thermal stability, high permeability, and a stable operation. The solution-diffusion model can be a useful tool for designing a membrane permeator. The

  14. Palladium alloy membrane process for the treatment of hydrogen isotopes

    International Nuclear Information System (INIS)

    Chung, Hongsuk; Paek, Seungwoo; Lee, Minsoo; Kim, Kwangrag; Yim, Sungpaal; Ahn, Dohee; Shim, Myunghwa

    2005-01-01

    Tritium is a radioactive isotope of hydrogen and it has a half-life of 12.3 years; it decays to He-3 by emitting a low energy beta radiation with an average energy of 5.7 keV and a maximum energy of 18.6 keV. Transfer of environmentally tritiated water to humans takes place via an inhalation, diffusion through the skin and ingestion. Radioactive waste containing tritium is continuously generated by the nuclear industry in, for example, nuclear reactor operations and a radioisotope production, as well as in medical research. Methods for removing tritium from liquid waste provide an alternative to the control of tritium emissions and a personnel exposure. A combined electrolysis and catalytic exchange process is a very effective method to remove small quantities of tritium from light or heavy waste water streams. The process consists of three main steps: (a) A front end step that exchanges the tritium to a less toxic hydrogen phase. This can be performed either through a chemical exchange in the presence of a platinum supported catalyst or through the decomposition of water. (b) A back end process that purifies the tritiated hydrogen gas which evolved from the electrolysis. This can be performed through a palladium alloy membrane separator. (c) A means of storing the concentrated gas safely. Uranium is used if the storage is temporary; titanium is usually employed for long term storage. To gain a better understanding of the tritiated hydrogen gas purification process, a mathematical model of the palladium alloy membrane has been used. This model is described herein, and the representative results of the model calculations are presented. The authors selected the palladium alloy membrane for the hydrogen purification process by considering the membrane properties, such as a chemical resistance, mechanical stability, thermal stability, high permeability, and a stable operation. The solution-diffusion model can be a useful tool for designing a membrane permeator. The

  15. New Palladium-Catalyzed Approaches to Heterocycles and Carbocycles

    Energy Technology Data Exchange (ETDEWEB)

    Huang, Qinhua [Iowa State Univ., Ames, IA (United States)

    2004-12-19

    The tert-butylimines of o-(1-alkynyl)benzaldehydes and analogous pyridinecarbaldehydes have been cyclized under very mild reaction conditions in the presence of I2, ICl, PhSeCl, PhSCl and p-O2NC6H4SCl to give the corresponding halogen-, selenium- and sulfur-containing disubstituted isoquinolines and naphthyridines, respectively. Monosubstituted isoquinolines and naphthyridines have been synthesized by the metal-catalyzed ring closure of these same iminoalkynes. This methodology accommodates a variety of iminoalkynes and affords the anticipated heterocycles in moderate to excellent yields. The Pd(II)-catalyzed cyclization of 2-(1-alkynyl)arylaldimines in the presence of various alkenes provides an efficient way to synthesize a variety of 4-(1-alkenyl)-3-arylisoquinolines in moderate to excellent yields. The introduction of an ortho-methoxy group on the arylaldimine promotes the Pd-catalyzed cyclization and stabilizes the resulting Pd(II) intermediate, improving the yields of the isoquinoline products. Highly substituted naphthalenes have been synthesized by the palladium-catalyzed annulation of a variety of internal alkynes, in which two new carbon-carbon bonds are formed in a single step under relatively mild reaction conditions. This method has also been used to synthesize carbazoles, although a higher reaction temperature is necessary. The process involves arylpalladation of the alkyne, followed by intramolecular Heck olefination and double bond isomerization. This method accommodates a variety of functional groups and affords the anticipated highly substituted naphthalenes and carbazoles in good to excellent yields. Novel palladium migratiodarylation methodology for the synthesis of complex fused polycycles has been developed, in which one or more sequential Pd-catalyzed intramolecular migration processes involving C-H activation are employed. The chemistry works best with electron-rich aromatics, which is in agreement

  16. Understanding and Improving High-Temperature Structural Properties of Metal-Silicide Intermetallics

    Energy Technology Data Exchange (ETDEWEB)

    Bruce S. Kang

    2005-10-10

    The objective of this project was to understand and improve high-temperature structural properties of metal-silicide intermetallic alloys. Through research collaboration between the research team at West Virginia University (WVU) and Dr. J.H. Schneibel at Oak Ridge National Laboratory (ORNL), molybdenum silicide alloys were developed at ORNL and evaluated at WVU through atomistic modeling analyses, thermo-mechanical tests, and metallurgical studies. In this study, molybdenum-based alloys were ductilized by dispersing MgAl2O4 or MgO spinel particles. The addition of spinel particles is hypothesized to getter impurities such as oxygen and nitrogen from the alloy matrix with the result of ductility improvement. The introduction of fine dispersions has also been postulated to improve ductility by acting as a dislocation source or reducing dislocation pile-ups at grain boundaries. The spinel particles, on the other hand, can also act as local notches or crack initiation sites, which is detrimental to the alloy mechanical properties. Optimization of material processing condition is important to develop the desirable molybdenum alloys with sufficient room-temperature ductility. Atomistic analyses were conducted to further understand the mechanism of ductility improvement of the molybdenum alloys and the results showed that trace amount of residual oxygen may be responsible for the brittle behavior of the as-cast Mo alloys. For the alloys studied, uniaxial tensile tests were conducted at different loading rates, and at room and elevated temperatures. Thermal cycling effect on the mechanical properties was also studied. Tensile tests for specimens subjected to either ten or twenty thermal cycles were conducted. For each test, a follow-up detailed fractography and microstructural analysis were carried out. The test results were correlated to the size, density, distribution of the spinel particles and processing time. Thermal expansion tests were carried out using thermo

  17. Palladium emissions in the environment: analytical methods, environmental assessment and health effects

    National Research Council Canada - National Science Library

    Alt, Friedrich; Zereini, Fathi

    2006-01-01

    ... (Eds)). But there is a clear lack of information concerning palladium. It is very important to condense the present state of research findings from emission to potential health risks for the environment and humans. Very important is the chapter about analytical determination of palladium, which shows clearly the problems of several analytic...

  18. Carbon nanotubes decorated with palladium nanoparticles : Synthesis, characterization, and catalytic activity

    NARCIS (Netherlands)

    Karousis, Nikolaos; Tsotsou, Georgia-Eleni; Evangelista, Fabrizio; Rudolf, Petra; Ragoussis, Nikitas; Tagmatarchis, Nikos

    2008-01-01

    In this article, the in situ preparation of palladium nanoparticles, as mediated by the self-regulated reduction of palladium acetate with the aid of sodium dodecyl sulfate (SDS), followed by subsequent deposition onto single-walled carbon nanotubes and multimalled carbon nanotubes (MWCNTs), is

  19. Oxygen Activated, Palladium Nanoparticle Catalyzed, Ultrafast Cross-Coupling of Organolithium Reagents

    NARCIS (Netherlands)

    Heijnen, Dorus; Tosi, Filippo; Vila, Carlos; Stuart, Marc C. A.; Elsinga, Philip H.; Szymanski, Wiktor; Feringa, Ben L.

    2017-01-01

    The discovery of an ultrafast cross-coupling of alkyland aryllithium reagents with a range of aryl bromides is presented. The essential role of molecular oxygen to form the active palladium catalyst was established; palladium nanoparticles that are highly active in cross-coupling reactions with

  20. Palladium(II)-Stabilized Pyridine-2-Diazotates: Synthesis, Structural Characterization, and Cytotoxicity Studies.

    Science.gov (United States)

    Tskhovrebov, Alexander G; Vasileva, Anna A; Goddard, Richard; Riedel, Tina; Dyson, Paul J; Mikhaylov, Vladimir N; Serebryanskaya, Tatiyana V; Sorokoumov, Viktor N; Haukka, Matti

    2018-02-05

    Well-defined diazotates are scarce. Here we report the synthesis of unprecedented homoleptic palladium(II) diazotate complexes. The palladium(II)-mediated nitrosylation of 2-aminopyridines with NaNO 2 results in the formation of metal-stabilized diazotates, which were found to be cytotoxic to human ovarian cancer cells.

  1. A DFT study of arsine adsorption on palladium doped graphene: Effects of palladium cluster size

    International Nuclear Information System (INIS)

    Kunaseth, Manaschai; Mudchimo, Tanabat; Namuangruk, Supawadee; Kungwan, Nawee; Promarak, Vinich; Jungsuttiwong, Siriporn

    2016-01-01

    Graphical abstract: The relationship between charge difference and adsorption strength demonstrates that charge migration from Pd_n-SDG to AsH_x significantly enhanced adsorption strength, the Pd_6 clusters doped SDG with a steep slope is recommended as a superior adsorbent material for AsH_3 removal from gas stream. - Highlights: • Pd atom and Pd clusters bind strongly onto the defective graphene surface. • Larger size of Pd cluster adsorbs arsine and its hydrogenated products stronger. • Order of adsorption strength on Pd_n doped graphene: As > AsH > AsH_2 > > AsH_3. • Charge migration characterizes the strong adsorption of AsH_2, AsH, and As. • Pd cluster doped graphene is thermodynamically preferable for arsine removal. - Abstract: In this study, we have investigated the size effects of palladium (Pd) doped single-vacancy defective graphene (SDG) surface to the adsorption of AsH_3 and its dehydrogenated products on Pd using density functional theory calculations. Here, Pd cluster binding study revealed that Pd_6 nanocluster bound strongest to the SDG surface, while adsorption of AsH_x (x = 0–3) on the most stable Pd_n doped SDG showed that dehydrogenated arsine compounds adsorbed onto the surface stronger than the pristine AsH_3 molecule. Charge analysis revealed that considerable amount of charge migration from Pd to dehydrogenated arsine molecules after adsorption may constitute strong adsorption for dehydrogenated arsine. In addition, study of thermodynamic pathways of AsH_3 dehydrogenation on Pd_n doped SDG adsorbents indicated that Pd cluster doping on SDG adsorbent tends to be thermodynamically favorable for AsH_3 decomposition than the single-Pd atom doped SDG. Hence, our study has indicated that Pd_6 clusters doped SDG is more advantageous as adsorbent material for AsH_3 removal.

  2. Purification in the interaction between yttria mould and Nb-silicide-based alloy during directional solidification: A novel effect of yttrium

    International Nuclear Information System (INIS)

    Ma, Limin; Tang, Xiaoxia; Wang, Bin; Jia, Lina; Yuan, Sainan; Zhang, Hu

    2012-01-01

    Nb-silicide-based alloys were directionally solidified in yttria moulds. As a result of thermal dissociation of yttria, the alloys were slightly contaminated with oxygen, which caused a competitive oxidation between yttrium and hafnium. The addition of 0.15 at.% yttrium reduced the oxygen increment by 42%, because the buoyant inclusions concentrated around the top surface. The yttrium addition caused a significant purification of the interaction between the yttria mould and the Nb-silicide-based alloys during the directional solidification.

  3. Development of anodic stripping voltametry for the determination of palladium in high level nuclear waste

    Energy Technology Data Exchange (ETDEWEB)

    Bhardwaj, T. K. [North Carolina State University, Raleigh (United States); Sharma, H. S.; Affarwal, S. K. [Bhabha Atomic Research Centre, Mumbai (India); Jain, P. C. [Meerut College, Meerut (India)

    2012-12-15

    Deposition potential, deposition time, square wave frequency, rotation speed of the rotating disc electrode, and palladium concentration were studied on a Glassy Carbon Electrode (GCE) in 0.01M HCl for the determination of palladium in High Level Nuclear Waste (HLNW) by anodic stripping voltammetry. Experimental conditions were optimized for the determination of palladium at two different, 10-8 and 10-7 M, levels. Error and standard deviation of this method were under 1% for all palladium standard solutions. The developed technique was successfully applied as a subsidiary method for the determination of palladium in simulated high level nuclear waste with very good precision and high accuracy (under 1 % error and standard deviation).

  4. The Leakage Current Improvement of a Ni-Silicided SiGe/Si Junction Using a Si Cap Layer and the PAI Technique

    International Nuclear Information System (INIS)

    Chang Jian-Guang; Wu Chun-Bo; Ji Xiao-Li; Ma Hao-Wen; Yan Feng; Shi Yi; Zhang Rong

    2012-01-01

    We investigate the leakage current of ultra-shallow Ni-silicided SiGe/Si junctions for 45 nm CMOS technology using a Si cap layer and the pre-amorphization implantation (PAI) process. It is found that with the conventional Ni silicide method, the leakage current of a p + (SiGe)—n(Si) junction is large and attributed to band-to-band tunneling and the generation-recombination process. The two leakage contributors can be suppressed quite effectively when a Si cap layer is added in the Ni silicide method. The leakage reduction is about one order of magnitude and could be associated with the suppression of the agglomeration of the Ni germano-silicide film. In addition, the PAI process after the application of a Si cap layer has little effect on improving the junction leakage but reduces the sheet resistance of the silicide film. As a result, the novel Ni silicide method using a Si cap combined with PAI is a promising choice for SiGe junctions in advanced technology. (cross-disciplinary physics and related areas of science and technology)

  5. Interaction of copper metallization with rare-earth metals and silicides

    International Nuclear Information System (INIS)

    Molnar, G. L.; Peto, G.; Zsoldos, E.; Horvath, Z. E.

    2001-01-01

    Solid-phase reactions of copper films with underlying gadolinium, erbium, and erbium - silicide layers on Si(100) substrates were investigated. For the phase analysis, x-ray diffraction and cross-sectional transmission electron microscopy were used. In the case of Cu/Gd/Si(100), an orthorhombic GdSi 2 formed, and, at higher temperatures, copper aggregated into islands. Annealed Cu/Er/Si(100) samples resulted in a hexagonal Er 5 Si 3 phase. In the Cu/ErSi 2-x /Si system, the copper catalyzes the transformation of the highly oriented hexagonal ErSi 2-x phase into hexagonal Er 5 Si 3 . Diverse phase developments of the samples with Gd and Er are based on reactivity differences of the two rare-earth metals. [copyright] 2001 American Institute of Physics

  6. A study of strain in thin epitaxial films of yttrium silicide on Si(111)

    Science.gov (United States)

    Siegal, Michelle F.; Martínez-Miranda, L. J.; Santiago-Avilés, J. J.; Graham, W. R.; Siegal, M. P.

    1994-02-01

    We present the results of an x-ray diffraction analysis of epitaxial yttrium silicide films grown on Si(111), with thicknesses ranging from 14 to 100 Å. The macroscopic strain along the out-of-plane direction for films containing pits or pinholes follows the trend observed previously in films of thicknesses up to 510 Å. The out-of-plane lattice parameter decreases linearly with film thickness. We show preliminary evidence that pinhole-free films do not follow the above trend, and that strain in these films has the opposite sign than in films with pinholes. Finally, our results also indicate that the mode of growth, coupled to the interfacial thermal properties of the films, affects the observed value for the strain in the films.

  7. A study of strain in thin epitaxial films of yttrium silicide on Si(111)

    International Nuclear Information System (INIS)

    Siegal, M.F.; Martinez-Miranda, L.J.; Santiago-Aviles, J.J.; Graham, W.R.; Siegal, M.P.

    1994-01-01

    We present the results of an x-ray diffraction analysis of epitaxial yttrium silicide films grown on Si(111), with thicknesses ranging from 14 to 100 A. The macroscopic strain along the out-of-plane direction for films containing pits or pinholes follows the trend observed previously in films of thicknesses up to 510 A. The out-of-plane lattice parameter decreases linearly with film thickness. We show preliminary evidence that pinhole-free films do not follow the above trend, and that strain in these films has the opposite sign than in films with pinholes. Finally, our results also indicate that the mode of growth, coupled to the interfacial thermal properties of the films, affects the observed value for the strain in the films

  8. Safety analysis of RSG-GAS Silicide core using one line cooling system

    International Nuclear Information System (INIS)

    Endiah-Puji-Hastuti

    2003-01-01

    In the frame of minimizing the operation-cost, operation mode using one line cooling system is being evaluated. Maximum reactor has been determined and to continuing this program, steady state and transient analysis were done. The analysis was done by means of a core thermal hydraulic code, COOLOD-N, and PARET. The codes solves core thermal hydraulic equation at steady state conditions and transient, respectively. By using silicide core data and coast down flow rate as the input, thermal hydraulics parameters such as fuel cladding and fuel meat temperatures as well as safety margin against flow instability were calculated. Imposing the safety criteria to the results of steady state and transient analysis, maximum permissible power for this operation was obtained as much as 17.1 MW

  9. The fabrication of metal silicide nanodot arrays using localized ion implantation

    International Nuclear Information System (INIS)

    Han, Jin; Kim, Tae-Gon; Min, Byung-Kwon; Lee, Sang Jo

    2010-01-01

    We propose a process for fabricating nanodot arrays with a pitch size of less than 25 nm. The process consists of localized ion implantation in a metal thin film on a Si wafer using a focused ion beam (FIB), followed by chemical etching. This process utilizes the etching resistivity changes of the ion beam irradiated region that result from metal silicide formation by ion implantation. To control the nanodot diameter, a threshold ion dose model is proposed using the Gaussian distribution of the ion beam intensities. The process is verified by fabricating nanodots with various diameters. The mechanism of etching resistivity is investigated via x-ray photoelectron spectroscopy (XPS) and Auger electron spectroscopy (AES).

  10. Hydrogen generation systems utilizing sodium silicide and sodium silica gel materials

    Science.gov (United States)

    Wallace, Andrew P.; Melack, John M.; Lefenfeld, Michael

    2015-07-14

    Systems, devices, and methods combine reactant materials and aqueous solutions to generate hydrogen. The reactant materials can sodium silicide or sodium silica gel. The hydrogen generation devices are used in fuels cells and other industrial applications. One system combines cooling, pumping, water storage, and other devices to sense and control reactions between reactant materials and aqueous solutions to generate hydrogen. Multiple inlets of varied placement geometries deliver aqueous solution to the reaction. The reactant materials and aqueous solution are churned to control the state of the reaction. The aqueous solution can be recycled and returned to the reaction. One system operates over a range of temperatures and pressures and includes a hydrogen separator, a heat removal mechanism, and state of reaction control devices. The systems, devices, and methods of generating hydrogen provide thermally stable solids, near-instant reaction with the aqueous solutions, and a non-toxic liquid by-product.

  11. Contributions to the preparation of 241americium metal and a few 241americium silicides

    International Nuclear Information System (INIS)

    Wittmann, F.D.

    1980-01-01

    In order to take a closer look at the americium-silicon system, three further silicides of americium: Am 5 Si 3 , Am 2 Si 3 and AmSi 2 were prepared in addition to the already known americium monosilicide and starting from the knowledge gained from the latters preparation. Radiographic investigations were carried out into the temperature region of 900 0 C. They showed no change of structure in the three compounds. It was possible to prepare residue-free americium metal by reducing AmF 3 with Si, whereby the SiF 4 formed can be easily separated off as volatile compound, and the Am metal is brought into a very pure form by sublimation suitable for spectrochemical investigations. Attempts to prepare binary germanides and gallides of 241 americium were unsuccessful. (RB) [de

  12. First-principles investigations of the physical properties of binary uranium silicide alloys

    International Nuclear Information System (INIS)

    Yang, Jin; Long, Jianping; Yang, Lijun; Li, Dongmei

    2013-01-01

    Graphical abstract: Total density of states for USi 2 . Display Omitted -- Abstract: The structural, elastic properties and the Debye temperature of binary Uranium Silicide (U-Si) alloys are investigated by using the first-principles plane-wave pseudopotential density function theory within the generalized gradient approximation (GGA). The ground states properties are found to agree with the available experimental data. The mechanical properties like shear modulus, Young’s modulus, Poisson’s ratio σ and ratio B/G are also calculated. Finally, The averaged sound velocity (v m ), the longitudinal sound velocity (v l ), transverse sound velocity (v t ) and the Debye temperature (θ D ) are obtained. However, the theoretical values are slightly different from few existed experiment data because the latter was obtained at room temperature while the former one at 0 K

  13. Hydrogen generation systems and methods utilizing sodium silicide and sodium silica gel materials

    Energy Technology Data Exchange (ETDEWEB)

    Wallace, Andrew P.; Melack, John M.; Lefenfeld, Michael

    2017-12-19

    Systems, devices, and methods combine thermally stable reactant materials and aqueous solutions to generate hydrogen and a non-toxic liquid by-product. The reactant materials can sodium silicide or sodium silica gel. The hydrogen generation devices are used in fuels cells and other industrial applications. One system combines cooling, pumping, water storage, and other devices to sense and control reactions between reactant materials and aqueous solutions to generate hydrogen. Springs and other pressurization mechanisms pressurize and deliver an aqueous solution to the reaction. A check valve and other pressure regulation mechanisms regulate the pressure of the aqueous solution delivered to the reactant fuel material in the reactor based upon characteristics of the pressurization mechanisms and can regulate the pressure of the delivered aqueous solution as a steady decay associated with the pressurization force. The pressure regulation mechanism can also prevent hydrogen gas from deflecting the pressure regulation mechanism.

  14. X-ray absorption fine structure (XAFS) studies of cobalt silicide thin films

    International Nuclear Information System (INIS)

    Naftel, S.J.; Coulthard, I.; Hu, Y.; Sham, T.K.; Zinke-Allmang, M.

    1998-01-01

    Cobalt silicide thin films, prepared on Si(100) wafers, have been studied by X-ray absorption near edge structures (XANES) at the Si K-, L 2,3 - and Co K-edges utilizing both total electron (TEY) and fluorescence yield (FLY) detection as well as extended X-ray absorption fine structure (EXAFS) at the Co K-edge. Samples made using DC sputter deposition on clean Si surfaces and MBE were studied along with a bulk CoSi 2 sample. XANES and EXAFS provide information about the electronic structure and morphology of the films. It was found that the films studied have essentially the same structure as bulk CoSi 2 . Both the spectroscopy and materials characterization aspects of XAFS (X-ray absorption fine structures) are discussed

  15. Burn-up analysis of uranium silicide fuels 20% 235U, in the LFR facility

    International Nuclear Information System (INIS)

    Amor, Ricardo A.; Bouza, Edgardo; Cabrejas, Julian L.; Devida, Claudio A.; Gil, Daniel A.; Stankevicius, Alejandro; Gautier, Eduardo; Garavaglia, Ricardo N.; Lobo, Alfredo

    2003-01-01

    The LFR Facility is a laboratory designed and constructed with a Hot-Cells line, a Globe-Box and a Fume-Hood, all of them suited to work with radioactive materials such as samples of irradiated silicide MTR fuel elements. A series of dissolutions of this material was performed. From the resulting solutions, two fractions were separated by HPLC. One contained U + Pu, and other the fission product Nd. The concentrations of these elements were obtained by isotopic dilution and mass spectrometry (IDMS). It is concluded that this technique is very powerful and accurate when properly applied, and makes the validation of burn-up calculation codes possible. It is worth remarking the Lfr capacity to carry on different Research and Development (R + D) tasks in the Nuclear Fuel Cycle field. (author)

  16. Intermetallic nickel silicide nanocatalyst-A non-noble metal-based general hydrogenation catalyst.

    Science.gov (United States)

    Ryabchuk, Pavel; Agostini, Giovanni; Pohl, Marga-Martina; Lund, Henrik; Agapova, Anastasiya; Junge, Henrik; Junge, Kathrin; Beller, Matthias

    2018-06-01

    Hydrogenation reactions are essential processes in the chemical industry, giving access to a variety of valuable compounds including fine chemicals, agrochemicals, and pharmachemicals. On an industrial scale, hydrogenations are typically performed with precious metal catalysts or with base metal catalysts, such as Raney nickel, which requires special handling due to its pyrophoric nature. We report a stable and highly active intermetallic nickel silicide catalyst that can be used for hydrogenations of a wide range of unsaturated compounds. The catalyst is prepared via a straightforward procedure using SiO 2 as the silicon atom source. The process involves thermal reduction of Si-O bonds in the presence of Ni nanoparticles at temperatures below 1000°C. The presence of silicon as a secondary component in the nickel metal lattice plays the key role in its properties and is of crucial importance for improved catalytic activity. This novel catalyst allows for efficient reduction of nitroarenes, carbonyls, nitriles, N-containing heterocycles, and unsaturated carbon-carbon bonds. Moreover, the reported catalyst can be used for oxidation reactions in the presence of molecular oxygen and is capable of promoting acceptorless dehydrogenation of unsaturated N-containing heterocycles, opening avenues for H 2 storage in organic compounds. The generality of the nickel silicide catalyst is demonstrated in the hydrogenation of over a hundred of structurally diverse unsaturated compounds. The wide application scope and high catalytic activity of this novel catalyst make it a nice alternative to known general hydrogenation catalysts, such as Raney nickel and noble metal-based catalysts.

  17. The ability of silicide coating to delay the catastrophic oxidation of vanadium under severe conditions

    Energy Technology Data Exchange (ETDEWEB)

    Chaia, N., E-mail: nabil.chaia@univ-lorraine.fr [Université de Lorraine, Institut Jean Lamour – UMR7198, Boulevard des Aiguillettes, BP70239, 54506 Vandoeuvre-lès-Nancy Cedex (France); Mathieu, S., E-mail: stephane.mathieu@univ-lorraine.fr [Université de Lorraine, Institut Jean Lamour – UMR7198, Boulevard des Aiguillettes, BP70239, 54506 Vandoeuvre-lès-Nancy Cedex (France); Rouillard, F., E-mail: fabien.rouillard@cea.fr [CEA, DEN, DPC, SCCME, Laboratoire d’Etude de la Corrosion Non Aqueuse, F-91191 Gif-sur-Yvette (France); Vilasi, M., E-mail: michel.vilasi@univ-lorraine.fr [Université de Lorraine, Institut Jean Lamour – UMR7198, Boulevard des Aiguillettes, BP70239, 54506 Vandoeuvre-lès-Nancy Cedex (France)

    2015-02-15

    Highlights: • Oxidation protection is due to the formation of a pure silica layer. • V–4Cr–4Ti with V{sub x}Si{sub y} silicide coating withstands 400 1-h cycles (1100 °C-T{sub amb}) in air. • Three-point flexure testing at 950 °C and 75 MPa does not induce coating breakdown. • No delamination between coating and substrate is observed in any test. - Abstract: V–4Cr–4Ti vanadium alloy is a potential cladding material for sodium-cooled fast-neutron reactors (SFRs). However, its affinity for oxygen and the subsequent embrittlement that oxygen induces causes a need for an oxygen diffusion barrier, which can be obtained by manufacturing a multi-layered silicide coating. The present work aims to evaluate the effects of thermal cycling (using a cyclic oxidation device) and tensile and compressive stresses (using the three-point flexure test) on the coated alloy system. Tests were performed in air up to 1100 °C, which is 200 °C higher than the accidental temperature for SFR applications. The results showed that the VSi{sub 2} coating was able to protect the vanadium substrate from oxidation for more than 400 1-h cycles between 1100 °C and room temperature. The severe bending applied to the coated alloy at 950 °C using a load of 75 MPa did not lead to specimen breakage. It can be suggested that the VSi{sub 2} coating has mechanical properties compatible with the V–4Cr–4Ti alloy for SFR applications.

  18. A DFT study of arsine adsorption on palladium doped graphene: Effects of palladium cluster size

    Energy Technology Data Exchange (ETDEWEB)

    Kunaseth, Manaschai, E-mail: manaschai@nanotec.or.th [National Nanotechnology Center (NANOTEC), National Science and Technology Development Agency (NSTDA) , Pathum Thani 12120 (Thailand); Mudchimo, Tanabat [Department of Chemistry and Center of Excellence for Innovation in Chemistry, Faculty of Science, Ubon Ratchathani University, Ubon Ratchathani 34190 (Thailand); Namuangruk, Supawadee [National Nanotechnology Center (NANOTEC), National Science and Technology Development Agency (NSTDA) , Pathum Thani 12120 (Thailand); Kungwan, Nawee [Department of Chemistry, Faculty of Science, Chiang Mai University, Chiang Mai 50200 (Thailand); Promarak, Vinich [Department of Material Science and Engineering, School of Molecular Science and Engineering, Vidyasirimedhi Institute of Science and Technology, Rayong 21201 (Thailand); Jungsuttiwong, Siriporn, E-mail: siriporn.j@ubu.ac.th [Department of Chemistry and Center of Excellence for Innovation in Chemistry, Faculty of Science, Ubon Ratchathani University, Ubon Ratchathani 34190 (Thailand)

    2016-03-30

    Graphical abstract: The relationship between charge difference and adsorption strength demonstrates that charge migration from Pd{sub n}-SDG to AsH{sub x} significantly enhanced adsorption strength, the Pd{sub 6} clusters doped SDG with a steep slope is recommended as a superior adsorbent material for AsH{sub 3} removal from gas stream. - Highlights: • Pd atom and Pd clusters bind strongly onto the defective graphene surface. • Larger size of Pd cluster adsorbs arsine and its hydrogenated products stronger. • Order of adsorption strength on Pd{sub n} doped graphene: As > AsH > AsH{sub 2} > > AsH{sub 3}. • Charge migration characterizes the strong adsorption of AsH{sub 2}, AsH, and As. • Pd cluster doped graphene is thermodynamically preferable for arsine removal. - Abstract: In this study, we have investigated the size effects of palladium (Pd) doped single-vacancy defective graphene (SDG) surface to the adsorption of AsH{sub 3} and its dehydrogenated products on Pd using density functional theory calculations. Here, Pd cluster binding study revealed that Pd{sub 6} nanocluster bound strongest to the SDG surface, while adsorption of AsH{sub x} (x = 0–3) on the most stable Pd{sub n} doped SDG showed that dehydrogenated arsine compounds adsorbed onto the surface stronger than the pristine AsH{sub 3} molecule. Charge analysis revealed that considerable amount of charge migration from Pd to dehydrogenated arsine molecules after adsorption may constitute strong adsorption for dehydrogenated arsine. In addition, study of thermodynamic pathways of AsH{sub 3} dehydrogenation on Pd{sub n} doped SDG adsorbents indicated that Pd cluster doping on SDG adsorbent tends to be thermodynamically favorable for AsH{sub 3} decomposition than the single-Pd atom doped SDG. Hence, our study has indicated that Pd{sub 6} clusters doped SDG is more advantageous as adsorbent material for AsH{sub 3} removal.

  19. Detecting Airborne Mercury by Use of Palladium Chloride

    Science.gov (United States)

    Ryan, Margaret; Shevade, Abhijit; Kisor, Adam; Homer, Margie; Jewell, April; Manatt, Kenneth; Torres, Julia; Soler, Jessica; Taylor, Charles

    2009-01-01

    Palladium chloride films have been found to be useful as alternatives to the gold films heretofore used to detect airborne elemental mercury at concentrations of the order of parts per billion (ppb). Somewhat more specifically, when suitably prepared palladium chloride films are exposed to parts-per-billion or larger concentrations of airborne mercury, their electrical resistances change by amounts large enough to be easily measurable. Because airborne mercury adversely affects health, it is desirable to be able to detect it with high sensitivity, especially in enclosed environments in which there is a risk of leakage of mercury from lamps or other equipment. The detection of mercury by use of gold films involves the formation of gold/mercury amalgam. Gold films offer adequate sensitivity for detection of airborne mercury and could easily be integrated into an electronic-nose system designed to operate in the temperature range of 23 to 28 C. Unfortunately, in order to regenerate a gold-film mercury sensor, one must heat it to a temperature of 200 C for several minutes in clean flowing air. In preparation for an experiment to demonstrate the present sensor concept, palladium chloride was deposited from an aqueous solution onto sets of gold electrodes and sintered in air to form a film. Then while using the gold electrodes to measure the electrical resistance of the films, the films were exposed, at a temperature of 25 C, to humidified air containing mercury at various concentrations from 0 to 35 ppb (see figure). The results of this and other experiments have been interpreted as signifying that sensors of this type can detect mercury in room-temperature air at concentrations of at least 2.5 ppb and can readily be regenerated at temperatures <40 C.

  20. Oxidation-resistant Ge-doped silicide coating on Cr-Cr2Nb alloys by pack cementation

    International Nuclear Information System (INIS)

    He Yirong

    1997-01-01

    The halide-activated pack cementation process was modified to produce a Ge-doped silicide diffusion coating on Cr-Cr 2 Nb alloys in a single processing step. The morphology and composition of the coating depended both on the pack composition and processing schedule and also on the composition and microstructure of the substrate. Higher Ge content in the pack suppressed the formation of CrSi 2 and reduced the growth kinetics of the coating. Ge was not homogeneously distributed in the coatings. Under cyclic and isothermal oxidation conditions, the Ge-doped silicide coating protected the Cr-Nb alloys from significant oxidation and from pesting by the formation of a Ge-doped silica film. (orig.)

  1. Optical metrology of Ni and NiSi thin films used in the self-aligned silicidation process

    International Nuclear Information System (INIS)

    Kamineni, V. K.; Bersch, E. J.; Diebold, A. C.; Raymond, M.; Doris, B. B.

    2010-01-01

    The thickness-dependent optical properties of nickel metal and nickel monosilicide (NiSi) thin films, used for self-aligned silicidation process, were characterized using spectroscopic ellipsometry. The thickness-dependent complex dielectric function of nickel metal films is shown to be correlated with the change in Drude free electron relaxation time. The change in relaxation time can be traced to the change in grain boundary (GB) reflection coefficient and grain size. A resistivity based model was used as the complementary method to the thickness-dependent optical model to trace the change in GB reflection coefficient and grain size. After silicidation, the complex dielectric function of NiSi films exhibit non-Drude behavior due to superimposition of interband absorptions arising at lower frequencies. The Optical models of the complete film stack were refined using x-ray photoelectron spectroscopy, Rutherford backscattered spectroscopy, and x-ray reflectivity (XRR).

  2. Palladium-Catalyzed alpha-Arylation of Tetramic Acids

    DEFF Research Database (Denmark)

    Storgaard, Morten; Dorwald, F. Z.; Peschke, B.

    2009-01-01

    A mild, racemization-free, palladium-Catalyzed alpha-arylation of tetramic acids (2,4-pyrrolidinediones) has been developed. Various amino acid-derived tetramic acids were cleanly arylated by treatment with 2 mol % of Pd(OAc)(2), 4 mol % of a sterically demanding biaryl phosphine, 2.3 equiv of K2CO...... no effect on their reactivity: both electron-rich and electron-poor aryl chlorides and bromides or triflates led to good yields. Ortho-substituted aryl halides and heteroaryl halides, however, did not undergo the title reaction....

  3. Growth of nanoparticles in hydrogen-implanted palladium subsurfaces

    International Nuclear Information System (INIS)

    Okuyama, F.

    2010-01-01

    Solid particles with nanometric dimensions are shown to grow in the opened subsurface of a polycrystalline palladium (Pd) hydrogen-implanted at around 500 C. The particles are Pd in main composition and densely grown on sloping walls of fissured grain boundaries or cracks. The average grain size increases from deeper to shallow regions, suggesting that a negative temperature gradient toward the surface existed along the crack walls. The nanoparticles are certain to arise from the condensation of Pd vapors on the walls, forcing us to assume that hydrogen atoms implanted in an overpopulation heated their implantation zone so strongly as to vaporize Pd. (orig.)

  4. Growth of nanoparticles in hydrogen-implanted palladium subsurfaces

    Energy Technology Data Exchange (ETDEWEB)

    Okuyama, F. [Nagoya Institute of Technology, Graduate School of Engineering, Nagoya (Japan)

    2010-07-15

    Solid particles with nanometric dimensions are shown to grow in the opened subsurface of a polycrystalline palladium (Pd) hydrogen-implanted at around 500 C. The particles are Pd in main composition and densely grown on sloping walls of fissured grain boundaries or cracks. The average grain size increases from deeper to shallow regions, suggesting that a negative temperature gradient toward the surface existed along the crack walls. The nanoparticles are certain to arise from the condensation of Pd vapors on the walls, forcing us to assume that hydrogen atoms implanted in an overpopulation heated their implantation zone so strongly as to vaporize Pd. (orig.)

  5. Palladium nanoparticles on InP for hydrogen detection

    Directory of Open Access Journals (Sweden)

    Zdansky Karel

    2011-01-01

    Full Text Available Abstract Layers of palladium (Pd nanoparticles on indium phosphide (InP were prepared by electrophoretic deposition from the colloid solution of Pd nanoparticles. Layers prepared by an opposite polarity of deposition showed different physical and morphological properties. Particles in solution are separated and, after deposition onto the InP surface, they form small aggregates. The size of the aggregates is dependent on the time of deposition. If the aggregates are small, the layer has no lateral conductance. Forward and reverse I-V characteristics showed a high rectification ratio with a high Schottky barrier height. The response of the structure on the presence of hydrogen was monitored.

  6. Determination of palladium in biological samples applying nuclear analytical techniques

    International Nuclear Information System (INIS)

    Cavalcante, Cassio Q.; Sato, Ivone M.; Salvador, Vera L. R.; Saiki, Mitiko

    2008-01-01

    This study presents Pd determinations in bovine tissue samples containing palladium prepared in the laboratory, and CCQM-P63 automotive catalyst materials of the Proficiency Test, using instrumental thermal and epithermal neutron activation analysis and energy dispersive X-ray fluorescence techniques. Solvent extraction and solid phase extraction procedures were also applied to separate Pd from interfering elements before the irradiation in the nuclear reactor. The results obtained by different techniques were compared against each other to examine sensitivity, precision and accuracy. (author)

  7. Acoustic emission during hydrogen absorption and desorption in palladium

    International Nuclear Information System (INIS)

    Ramesh, R.; Mukhopadhyay, C.K.; Jayakumar, T.; Baldev Raj

    1996-01-01

    Acoustic emission technique has been used to study charging and discharging of hydrogen in palladium. During charging, breaking of oxide film due to surface activation and saturation of hydrogen absorption have been identified by acoustic emission. In the discharging cycle, the desorption of hydrogen from the specimen leads to high AE activity immediately after initiation of discharging, followed by gradual decrease in the acoustic activity, which reaches a minimum upon completion of the desorption. The potential of the acoustic emission technique for studying the kinetics of hydrogen absorption and desorption in metals has been shown. (author)

  8. Synthesis of Dihydrobenzofurans via Palladium-Catalyzed Heteroannulations

    Energy Technology Data Exchange (ETDEWEB)

    Rozhkov, Roman Vladimirovich [Iowa State Univ., Ames, IA (United States)

    2004-01-01

    Palladium-catalyzed heteroannulation of 1,3-dienes with 3-iodo-2-alkenols, and 2-iodo-2-alkenols, as well as their amino analogs, affords the corresponding cyclic ethers and amines respectively. The presence of a β-hydrogen in the vinylic halide results in β-hydride elimination giving the corresponding alkyne. The presence of a bulky group in the α-position of the vinylic halide results in failure or reduced amounts of annulation products. A chloride source, pyridine base and electron-rich phosphine are essential for this reaction.

  9. Palladium coated fibre Bragg grating based hydrogen sensor

    International Nuclear Information System (INIS)

    Kasinathan, M.; Sosamma, S.; Kishore, S.; Elumalai, V.; Krishnan, R.; Babu Rao, C.; Dash, Sitaram; Murali, N.; Jayakumar, T.

    2011-01-01

    Detection of steam generator leaks in fast nuclear reactors is carried out by monitoring hydrogen in argon cover-gas. Hydrogen released during sodium cleaning of fast reactor components is required to be monitored. Hydrogen sensors with good sensitivity, stability and response time are required for all the above applications. We report a new type of hydrogen sensor with a Fibre Bragg Grating (FBG) coated with palladium thin film which is used to detect the leak of hydrogen gas in the Steam Generator (SG) module of the Fast Breeder Reactor (FBR). If water leaks into sodium, it results in sodium-water reaction. In this reaction hydrogen and sodium hydroxide are formed. Due to the explosive risk of hydrogen system, hydrogen sensors are of great interest in this case. It is known that hydrogen forms an explosive mixture with air once its concentration exceeds beyond the explosion limit of four percent. The advantages of FBG based hydrogen sensor over the other hydrogen sensors are its inherent property of safety from sparking, immunity to ambient electromagnetic interference. The sensing mechanism in this device is based on mechanical strain that is induced in the palladium coating when it absorbs hydrogen. This process physically stretches the grating and causes the grating period and grating's refractive index, to change. The Bragg wavelength shift is directly proportional to the strain induced and can be directly related to the percentage of hydrogen exposure. The online monitoring of palladium thin film coating on FBG is carried out and recorded the wavelength change and strain induced on the FBG. A hydrogen sensor set up have been fabricated which consists of SS vessel of capacity 10 litres, provided with pressure gauge, Argon filling line with a valve, Hydrogen injection line with flange, a vent line with valve and Hydrogen sensor fixing point. The Palladium coated FBG based Hydrogen sensor is tested in this experimental facility in the exposure of hydrogen in

  10. Fuel element burnup measurements for the equilibrium LEU silicide RSG GAS (MPR-30) core under a new fuel management strategy

    International Nuclear Information System (INIS)

    Pinem, Surian; Liem, Peng Hong; Sembiring, Tagor Malem; Surbakti, Tukiran

    2016-01-01

    Highlights: • Burnup measurement of fuel elements comprising the new equilibrium LEU silicide core of RSG GAS. • The burnup measurement method is based on a linear relationship between reactivity and burnup. • Burnup verification was conducted using an in-house, in-core fuel management code BATAN-FUEL. • A good agreement between the measured and calculated burnup was confirmed. • The new fuel management strategy was confirmed and validated. - Abstract: After the equilibrium LEU silicide core of RSG GAS was achieved, there was a strong need to validate the new fuel management strategy by measuring burnup of fuel elements comprising the core. Since the regulatory body had a great concern on the safety limit of the silicide fuel element burnup, amongst the 35 burnt fuel elements we selected 22 fuel elements with high burnup classes i.e. from 20 to 53% loss of U-235 (declared values) for the present measurements. The burnup measurement method was based on a linear relationship between reactivity and burnup where the measurements were conducted under subcritical conditions using two fission counters of the reactor startup channel. The measurement results were compared with the declared burnup evaluated by an in-house in-core fuel management code, BATAN-FUEL. A good agreement between the measured burnup values and the calculated ones was found within 8% uncertainties. Possible major sources of differences were identified, i.e. large statistical errors (i.e. low fission counters’ count rates), variation of initial U-235 loading per fuel element and accuracy of control rod indicators. The measured burnup of the 22 fuel elements provided the confirmation of the core burnup distribution planned for the equilibrium LEU silicide core under the new fuel management strategy.

  11. Evaluation of powder metallurgical processing routes for multi-component niobium silicide-based high-temperature alloys

    Energy Technology Data Exchange (ETDEWEB)

    Seemueller, Hans Christoph Maximilian

    2016-03-22

    Niobium silicide-based composites are potential candidates to replace nickel-base superalloys for turbine applications. The goal of this work was to evaluate the feasibility and differences in ensuing properties of various powder metallurgical processing techniques that are capable of manufacturing net-shape turbine components. Two routes for powder production, mechanical alloying and gas atomization were combined with compaction via hot isostatic pressing and powder injection molding.

  12. Controlling the formation and stability of ultra-thin nickel silicides - An alloying strategy for preventing agglomeration

    Science.gov (United States)

    Geenen, F. A.; van Stiphout, K.; Nanakoudis, A.; Bals, S.; Vantomme, A.; Jordan-Sweet, J.; Lavoie, C.; Detavernier, C.

    2018-02-01

    The electrical contact of the source and drain regions in state-of-the-art CMOS transistors is nowadays facilitated through NiSi, which is often alloyed with Pt in order to avoid morphological agglomeration of the silicide film. However, the solid-state reaction between as-deposited Ni and the Si substrate exhibits a peculiar change for as-deposited Ni films thinner than a critical thickness of tc = 5 nm. Whereas thicker films form polycrystalline NiSi upon annealing above 450 ° C , thinner films form epitaxial NiSi2 films that exhibit a high resistance toward agglomeration. For industrial applications, it is therefore of utmost importance to assess the critical thickness with high certainty and find novel methodologies to either increase or decrease its value, depending on the aimed silicide formation. This paper investigates Ni films between 0 and 15 nm initial thickness by use of "thickness gradients," which provide semi-continuous information on silicide formation and stability as a function of as-deposited layer thickness. The alloying of these Ni layers with 10% Al, Co, Ge, Pd, or Pt renders a significant change in the phase sequence as a function of thickness and dependent on the alloying element. The addition of these ternary impurities therefore changes the critical thickness tc. The results are discussed in the framework of classical nucleation theory.

  13. A Study on Characterization of Light-Induced Electroless Plated Ni Seed Layer and Silicide Formation for Solar Cell Application

    Science.gov (United States)

    Takaloo, Ashkan Vakilipour; Joo, Seung Ki; Es, Firat; Turan, Rasit; Lee, Doo Won

    2018-03-01

    Light-induced electroless plating (LIEP) is an easy and inexpensive method that has been widely used for seed layer deposition of Nickel/Copper (Ni/Cu)-based metallization in the solar cell. In this study, material characterization aspects of the Ni seed layer and Ni silicide formation at different bath conditions and annealing temperatures on the n-side of a silicon diode structure have been examined to achieve the optimum cell contacts. The effects of morphology and chemical composition of Ni film on its electrical conductivity were evaluated and described by a quantum mechanical model. It has been found that correlation exists between the theoretical and experimental conductivity of Ni film. Residual stress and phase transformation of Ni silicide as a function of annealing temperature were evaluated using Raman and XRD techniques. Finally, transmission line measurement (TLM) technique was employed to determine the contact resistance of Ni/Si stack after thermal treatment and to understand its correlation with the chemical-structural properties. Results indicated that low electrical resistive mono-silicide (NiSi) phase as low as 5 mΩ.cm2 was obtained.

  14. Electrical and optical properties of sub-10 nm nickel silicide films for silicon solar cells

    International Nuclear Information System (INIS)

    Brahmi, Hatem; Ravipati, Srikanth; Yarali, Milad; Wang, Weijie; Ryou, Jae-Hyun; Mavrokefalos, Anastassios; Shervin, Shahab

    2017-01-01

    Highly conductive and transparent films of ultra-thin p-type nickel silicide films have been prepared by RF magnetron sputtering of nickel on silicon substrates followed by rapid thermal annealing in an inert environment in the temperature range 400–600 °C. The films are uniform throughout the wafer with thicknesses in the range of 3–6 nm. The electrical and optical properties are presented for nickel silicide films with varying thickness. The Drude–Lorentz model and Fresnel equations were used to calculate the dielectric properties, sheet resistance, absorption and transmission of the films. These ultrathin nickel silicide films have excellent optoelectronic properties for p-type contacts with optical transparencies up to 80% and sheet resistance as low as ∼0.15 µΩ cm. Furthermore, it was shown that the use of a simple anti-reflection (AR) coating can recover most of the reflected light approaching the values of a standard Si solar cell with the same AR coating. Overall, the combination of ultra-low thickness, high transmittance, low sheet resistance and ability to recover the reflected light by utilizing standard AR coating makes them ideal for utilization in silicon based photovoltaic technologies as a p-type transparent conductor. (paper)

  15. Electrical and optical properties of sub-10 nm nickel silicide films for silicon solar cells

    Science.gov (United States)

    Brahmi, Hatem; Ravipati, Srikanth; Yarali, Milad; Shervin, Shahab; Wang, Weijie; Ryou, Jae-Hyun; Mavrokefalos, Anastassios

    2017-01-01

    Highly conductive and transparent films of ultra-thin p-type nickel silicide films have been prepared by RF magnetron sputtering of nickel on silicon substrates followed by rapid thermal annealing in an inert environment in the temperature range 400-600 °C. The films are uniform throughout the wafer with thicknesses in the range of 3-6 nm. The electrical and optical properties are presented for nickel silicide films with varying thickness. The Drude-Lorentz model and Fresnel equations were used to calculate the dielectric properties, sheet resistance, absorption and transmission of the films. These ultrathin nickel silicide films have excellent optoelectronic properties for p-type contacts with optical transparencies up to 80% and sheet resistance as low as ~0.15 µΩ cm. Furthermore, it was shown that the use of a simple anti-reflection (AR) coating can recover most of the reflected light approaching the values of a standard Si solar cell with the same AR coating. Overall, the combination of ultra-low thickness, high transmittance, low sheet resistance and ability to recover the reflected light by utilizing standard AR coating makes them ideal for utilization in silicon based photovoltaic technologies as a p-type transparent conductor.

  16. Palladium sulphide (PdS) films as a new thermoelectric sulphide compound

    Energy Technology Data Exchange (ETDEWEB)

    Ares, J.R.; Diaz-Chao, P.; Clamagirand, J.; Macia, M.D.; Ferrer, I.J.; Sanchez, C. [Universidad Autonoma de Madrid (Spain). Lab. de Materiales de Interes en Energias Renovables

    2010-07-01

    Palladium sulphide (PdS) films have been prepared by direct sulphuration of 20 nm thick palladium films at different temperatures (200 C < T < 450 C). Sulphurated films exhibit an unique crystalline phase: PdS. Seebeck coefficient and electrical resistivity of these films are between -110 and -150 {mu}V/K and {proportional_to} 0.08 to 0.8 {omega}cm depending on the sulphuration temperature. Negative sign of Seebeck coefficient indicates an n type conduction in all films. Discussion is focused on the influence of atomic ratio between sulphur and palladium as well as impurities arising from the substrate on transport properties. (orig.)

  17. Interaction between Palladium Nanoparticles and Surface-Modified Carbon Nanotubes: Role of Surface Functionalities

    DEFF Research Database (Denmark)

    Zhang, Bingsen; Shao, Lidong; Zhang, Wei

    2014-01-01

    degrees C. We focus on probing the effects of oxygen and nitrogen-containing functional groups on supported palladium nanoparticles (NPs) in the model catalytic system. The stability of palladium NPs supported on CNTs depends strongly on the surface properties of CNTs. Moreover, the oxygen...... feature, instability, and subtle response of the components upon application of an external field. Herein, we use insitu TEM, electron energy loss spectroscopy, and X-ray photoelectron spectroscopy techniques to record the interaction in palladium on carbon nanotubes (CNTs) from room temperature to 600...

  18. Supported palladium nanoparticles synthesized by living plants as a catalyst for Suzuki-Miyaura reactions.

    Directory of Open Access Journals (Sweden)

    Helen L Parker

    Full Text Available The metal accumulating ability of plants has previously been used to capture metal contaminants from the environment; however, the full potential of this process is yet to be realized. Herein, the first use of living plants to recover palladium and produce catalytically active palladium nanoparticles is reported. This process eliminates the necessity for nanoparticle extraction from the plant and reduces the number of production steps compared to traditional catalyst palladium on carbon. These heterogeneous plant catalysts have demonstrated high catalytic activity in Suzuki coupling reactions between phenylboronic acid and a range of aryl halides containing iodo-, bromo- and chloro- moieties.

  19. Investigation of mechanical and structural characteristics of platinum and palladium at high temperatures

    Energy Technology Data Exchange (ETDEWEB)

    Trumie, B. T.; Gomidzelovie, L.; Marjanovic, S. R.; Krstic, V. R.

    2015-03-30

    In order to broaden future application of products based on platinum and palladium a comparative analysis of their high-temperature mechanical properties was performed. Platinum and palladium are of great importance and are widely used in chemical industry, electronics, for making laboratory dishes, to name a few. Mechanical properties of pure metals, such as: tensile strength, creep rate and rupture time were investigated using universal testing machine for tensile testing of materials. Microstructure of samples was investigated by optical microscopy. Based on obtained results it can be concluded that the platinum, compared to palladium, is superior for high-temperature applications. (Author)

  20. Investigation of mechanical and structural characteristics of platinum and palladium at high temperatures

    International Nuclear Information System (INIS)

    Trumie, B. T.; Gomidzelovie, L.; Marjanovic, S. R.; Krstic, V. R.

    2015-01-01

    In order to broaden future application of products based on platinum and palladium a comparative analysis of their high-temperature mechanical properties was performed. Platinum and palladium are of great importance and are widely used in chemical industry, electronics, for making laboratory dishes, to name a few. Mechanical properties of pure metals, such as: tensile strength, creep rate and rupture time were investigated using universal testing machine for tensile testing of materials. Microstructure of samples was investigated by optical microscopy. Based on obtained results it can be concluded that the platinum, compared to palladium, is superior for high-temperature applications. (Author)

  1. Carbonylation of 1-hexene in the presence of palladium-anion-exchange resin catalysts

    Energy Technology Data Exchange (ETDEWEB)

    Lapidus, A.L.; Pirozhkov, S.D.; Buiya, M.A.; Lunin, A.F.; Karapetyan, L.P.; Saldadze, K.M.

    1986-06-20

    Activated charcoal, silica gel, and zeolites containing palladium are active in the carbonylation of lower olefins by carbon monoxide. In the present work, they studied the carbonylation of 1-hexene in the presence of a series of palladium catalysts containing An-221, An-251, and AN-511 anion-exchange catalysts produced in the USSR as the supports. A catalyst obtained by the deposition of palladium(II) on weakly basic anion-exchange resins displays high efficiency in the carbonylation of 1-hexene with the formation of a nixture of enanthoic and 2-methylcaproic acids.

  2. Preliminary design of fusion reactor fuel cleanup system by palladium alloy membrane method

    International Nuclear Information System (INIS)

    Yoshida, Hiroshi; Konishi, Satoshi; Naruse, Yuji

    1981-10-01

    A design of palladium diffuser and Fuel Cleanup System (FCU) for D-T fusion reactor is proposed. Feasibility of palladium alloy membrane method is discussed based on the early studies by the authors. Operating conditions of the palladium diffuser are determined experimentally. Dimensions of the diffuser are estimated from computer simulation. FCU system is designed under the feed conditions of Tritium Systems Test Assembly (TSTA) at Los Alamos Scientific Laboratory. The system is composed of Pd-diffusers, catalytic oxidizer, freezer and zink beds, and has some advantages in system layout and operation. This design can readily be extended to other conditions of plasma exhaust gases. (author)

  3. Hydrogen sensor based on palladium-yttrium alloy nanosheet

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Boyi [Queensland Micro- and Nanotechnology Centre, Griffith University, Nathan, QLD 4111 (Australia); Zhu, Yong, E-mail: y.zhu@griffith.edu.au [Queensland Micro- and Nanotechnology Centre, Griffith University, Nathan, QLD 4111 (Australia); Chen, Youping; Song, Han; Huang, Pengcheng [School of Mechanical Science and Engineering, Huazhong University of Science and Technology, Wuhan, 430074 (China); Dao, Dzung Viet [Queensland Micro- and Nanotechnology Centre, Griffith University, Nathan, QLD 4111 (Australia)

    2017-06-15

    This paper presents a hydrogen sensor based on palladium-yttrium (Pd-Y) alloy nanosheet. Zigzag-shaped Pd-Y nanosheet with a thickness of 19.3 nm was deposited on a quartz substrate by using an ultrahigh-vacuum magnetron sputtering system and shadow mask. The atomic ratio of palladium to yttrium in the nanosheet was 0.92/0.08. The fabrication process was simple and low-cost, and the sensor can be mass-produced. The experimental results show the sensor has a superior sensitivity, reversibility, and reproducibility. The resistive-based hydrogen detection mechanism in this research is much simpler and more compact compared to the optical-based detection method. - Highlights: • Pd-Y sensing element was fabricated using a magnetron sputtering system and shadow mask. • The Pd-Y compound consisted of 92% Pd and 8% Y. • The fabrication process was simple, low-cost, and mass-production compatible. • The sensor showed superior sensitivity, reversibility, and reproducibility to hydrogen gas. • The device is more compact than the optical-based counterpart.

  4. Chlorodifluoromethane-triggered formation of difluoromethylated arenes catalysed by palladium

    Science.gov (United States)

    Feng, Zhang; Min, Qiao-Qiao; Fu, Xia-Ping; An, Lun; Zhang, Xingang

    2017-09-01

    Difluoromethylated aromatic compounds are of increasing importance in pharmaceuticals, agrochemicals and materials. Chlorodifluoromethane (ClCF2H), an inexpensive, abundant and widely used industrial raw material, represents the ideal and most straightforward difluoromethylating reagent, but introduction of the difluoromethyl group (CF2H) from ClCF2H into aromatics has not been reported. Here, we describe a direct palladium-catalysed difluoromethylation method for coupling ClCF2H with arylboronic acids and esters to generate difluoromethylated arenes with high efficiency. The reaction exhibits a remarkably broad substrate scope, including heteroarylboronic acids, and was used for difluoromethylation of a range of pharmaceuticals and biologically active compounds. Preliminary mechanistic studies revealed that a palladium difluorocarbene intermediate is involved in the reaction. Although numerous metal-difluorocarbene complexes have been prepared, the catalytic synthesis of difluoromethylated or difluoromethylenated compounds involving metal-difluorocarbene complexes has not received much attention. This new reaction therefore also opens the door to understand metal-difluorocarbene complex catalysed reactions.

  5. Hydrogen sensor based on palladium-yttrium alloy nanosheet

    International Nuclear Information System (INIS)

    Wang, Boyi; Zhu, Yong; Chen, Youping; Song, Han; Huang, Pengcheng; Dao, Dzung Viet

    2017-01-01

    This paper presents a hydrogen sensor based on palladium-yttrium (Pd-Y) alloy nanosheet. Zigzag-shaped Pd-Y nanosheet with a thickness of 19.3 nm was deposited on a quartz substrate by using an ultrahigh-vacuum magnetron sputtering system and shadow mask. The atomic ratio of palladium to yttrium in the nanosheet was 0.92/0.08. The fabrication process was simple and low-cost, and the sensor can be mass-produced. The experimental results show the sensor has a superior sensitivity, reversibility, and reproducibility. The resistive-based hydrogen detection mechanism in this research is much simpler and more compact compared to the optical-based detection method. - Highlights: • Pd-Y sensing element was fabricated using a magnetron sputtering system and shadow mask. • The Pd-Y compound consisted of 92% Pd and 8% Y. • The fabrication process was simple, low-cost, and mass-production compatible. • The sensor showed superior sensitivity, reversibility, and reproducibility to hydrogen gas. • The device is more compact than the optical-based counterpart.

  6. Rate Theory Modeling and Simulations of Silicide Fuel at LWR Conditions

    Energy Technology Data Exchange (ETDEWEB)

    Miao, Yinbin [Argonne National Lab. (ANL), Argonne, IL (United States); Ye, Bei [Argonne National Lab. (ANL), Argonne, IL (United States); Mei, Zhigang [Argonne National Lab. (ANL), Argonne, IL (United States); Hofman, Gerard [Argonne National Lab. (ANL), Argonne, IL (United States); Yacout, Abdellatif [Argonne National Lab. (ANL), Argonne, IL (United States)

    2015-12-10

    Uranium silicide (U3Si2) fuel has higher thermal conductivity and higher uranium density, making it a promising candidate for the accident-tolerant fuel (ATF) used in light water reactors (LWRs). However, previous studies on the fuel performance of U3Si2, including both experimental and computational approaches, have been focusing on the irradiation conditions in research reactors, which usually involve low operation temperatures and high fuel burnups. Thus, it is important to examine the fuel performance of U3Si2 at typical LWR conditions so as to evaluate the feasibility of replacing conventional uranium dioxide fuel with this silicide fuel material. As in-reactor irradiation experiments involve significant time and financial cost, it is appropriate to utilize modeling tools to estimate the behavior of U3Si2 in LWRs based on all those available research reactor experimental references and state-of-the-art density functional theory (DFT) calculation capabilities at the early development stage. Hence, in this report, a comprehensive investigation of the fission gas swelling behavior of U3Si2 at LWR conditions is introduced. The modeling efforts mentioned in this report was based on the rate theory (RT) model of fission gas bubble evolution that has been successfully applied for a variety of fuel materials at devious reactor conditions. Both existing experimental data and DFT-calculated results were used for the optimization of the parameters adopted by the RT model. Meanwhile, the fuel-cladding interaction was captured by the coupling of the RT model with simplified mechanical correlations. Therefore, the swelling behavior of U3Si2 fuel and its consequent interaction with cladding in LWRs was predicted by the rate theory modeling, providing valuable information for the development of U3Si2 fuel as an accident

  7. Studies of valence of selected rare earth silicides determined using Si K and Pd/Rh L{sub 2,3} XANES and LAPW numerical studies

    Energy Technology Data Exchange (ETDEWEB)

    Zajdel, P., E-mail: pawel.zajdel@us.edu.pl [Institute of Physics, University of Silesia, ul. Uniwersytecka 4, 40-007 Katowice (Poland); Kisiel, A., E-mail: andrzej.kisiel@uj.edu.pl [M. Smoluchowski Institute of Physics, Jagiellonian University, ul. Lojasiewicza 11, 30-348 Kraków (Poland); Szytuła, A., E-mail: andrzej.szytula@uj.edu.pl [M. Smoluchowski Institute of Physics, Jagiellonian University, ul. Lojasiewicza 11, 30-348 Kraków (Poland); Goraus, J., E-mail: jerzy.goraus@us.edu.pl [Institute of Physics, University of Silesia, ul. Uniwersytecka 4, 40-007 Katowice (Poland); Balerna, A., E-mail: antonella.balerna@lnf.infn.it [Laboratori Nazionali di Frascati, INFN, Lab DAPHINE-Light, Via E. Fermi 40, I-00044 Frascati (Italy); Banaś, A., E-mail: slsba@nus.edu.sg [Singapore Synchrotron Light Source, National University of Singapore, 5 Research Link, Singapore 117603 (Singapore); Starowicz, P., E-mail: pawel.starowicz@uj.edu.pl [M. Smoluchowski Institute of Physics, Jagiellonian University, ul. Lojasiewicza 11, 30-348 Kraków (Poland); Konior, J., E-mail: jerzy.konior@uj.edu.pl [M. Smoluchowski Institute of Physics, Jagiellonian University, ul. Lojasiewicza 11, 30-348 Kraków (Poland); Cinque, G., E-mail: gianfelice.cinque@diamond.ac.uk [Diamond Light Source, Harwell Campus, OX11 0DE Chilton-Didcot (United Kingdom); Grilli, A., E-mail: antonio.grilli@lnf.infn.it [Laboratori Nazionali di Frascati, INFN, Lab DAPHINE-Light, Via E. Fermi 40, I-00044 Frascati (Italy)

    2015-12-01

    Highlights: • The Si K and Pd L{sub 3} edges of R{sub 2}PdSi{sub 3} (R = Ce, Nd, Tb, Dy, Ho, Er) and HoRh{sub 2−x}Pd{sub x}Si{sub 2} are reported. • The R–Si bonds possess polar and 4d5s bands of Pd and Rh metallic characters. • There is no indication of Ce having a different valence than the other rare earths. • The positions and features of the calculated edges exhibit a fair agreement up to ≈10 eV. • The supercell used for Ho{sub 2}PdSi{sub 3} is good enough to reproduce the Si K edge. - Abstract: We report on the investigation of Si and Pd/Rh chemical environments using X-ray Absorption Near Edge Spectroscopy in two different families of rare earth silicides R{sub 2}PdSi{sub 3} (R = Ce, Nd, Tb, Dy, Ho, Er) and HoRh{sub 2−x}Pd{sub x}Si{sub 2} (x = 0, 0.5, 0.75, 1.0, 1.5, 1.8, 2.0). The Si K, Pd L{sub 3} and Rh L{sub 3} absorption edges were recorded in order to follow their changes upon the variation of 4f and 4d5s electron numbers. In both cases it was found that the Si K edge was shifted ≈0.5 eV toward lower energies, relative to pure silicon. In the first family, the shift decreases with increasing number of f-electrons, while the Si K edge remains constant upon rhodium–palladium substitution. In all cases the Pd L{sub 3} edge was shifted to higher energies relative to metallic Pd. No visible change in the Pd L{sub 3} position was observed either with a varying 4f electron count or upon Pd/Rh substitution. Also, the Rh L{sub 3} edge did not change. For two selected members, Ho{sub 2}PdSi{sub 3} and HoPd{sub 2}Si{sub 2}, the Wien2K’09 (LDA + U) package was used to calculate the electronic structure and the absorption edges. Si K edges were reproduced well for both compounds, while Pd L{sub 3} only exhibited a fair agreement for the second compound. This discrepancy between the Pd L{sub 3} theory and experiment for the Ho{sub 2}PdSi{sub 3} sample can be attributed to the specific ordered superstructure used in the numerical calculations

  8. Insertion of molecular oxygen into a palladium(II) methyl bond: a radical chain mechanism involving palladium(III) intermediates.

    Science.gov (United States)

    Boisvert, Luc; Denney, Melanie C; Hanson, Susan Kloek; Goldberg, Karen I

    2009-11-04

    The reaction of (bipy)PdMe(2) (1) (bipy = 2,2'-bipyridine) with molecular oxygen results in the formation of the palladium(II) methylperoxide complex (bipy)PdMe(OOMe) (2). The identity of the product 2 has been confirmed by independent synthesis. Results of kinetic studies of this unprecedented oxygen insertion reaction into a palladium alkyl bond support the involvement of a radical chain mechanism. Reproducible rates, attained in the presence of the radical initiator 2,2'-azobis(2-methylpropionitrile) (AIBN), reveal that the reaction is overall first-order (one-half-order in both [1] and [AIBN], and zero-order in [O(2)]). The unusual rate law (half-order in [1]) implies that the reaction proceeds by a mechanism that differs significantly from those for organic autoxidations and for the recently reported examples of insertion of O(2) into Pd(II) hydride bonds. The mechanism for the autoxidation of 1 is more closely related to that found for the autoxidation of main group and early transition metal alkyl complexes. Notably, the chain propagation is proposed to proceed via a stepwise associative homolytic substitution at the Pd center of 1 with formation of a pentacoordinate Pd(III) intermediate.

  9. Development of polymeric palladium-nanoparticle membrane-installed microflow devices and their application in hydrodehalogenation.

    Science.gov (United States)

    Yamada, Yoichi M A; Watanabe, Toshihiro; Ohno, Aya; Uozumi, Yasuhiro

    2012-02-13

    We have developed a variety of polymeric palladium-nanoparticle membrane-installed microflow devices. Three types of polymers were convoluted with palladium salts under laminar flow conditions in a microflow reactor to form polymeric palladium membranes at the laminar flow interface. These membranes were reduced with aqueous sodium formate or heat to create microflow devices that contain polymeric palladium-nanoparticle membranes. These microflow devices achieved instantaneous hydrodehalogenation of aryl chlorides, bromides, iodides, and triflates by 10-1000 ppm within a residence time of 2-8 s at 50-90 °C by using safe, nonexplosive, aqueous sodium formate to quantitatively afford the corresponding hydrodehalogenated products. Polychlorinated biphenyl (10-1000 ppm) and polybrominated biphenyl (1000 ppm) were completely decomposed under similar conditions, yielding biphenyl as a fungicidal compound. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  10. Nano-palladium is a cellular catalyst for in vivo chemistry

    Science.gov (United States)

    Miller, Miles A.; Askevold, Bjorn; Mikula, Hannes; Kohler, Rainer H.; Pirovich, David; Weissleder, Ralph

    2017-07-01

    Palladium catalysts have been widely adopted for organic synthesis and diverse industrial applications given their efficacy and safety, yet their biological in vivo use has been limited to date. Here we show that nanoencapsulated palladium is an effective means to target and treat disease through in vivo catalysis. Palladium nanoparticles (Pd-NPs) were created by screening different Pd compounds and then encapsulating bis[tri(2-furyl)phosphine]palladium(II) dichloride in a biocompatible poly(lactic-co-glycolic acid)-b-polyethyleneglycol platform. Using mouse models of cancer, the NPs efficiently accumulated in tumours, where the Pd-NP activated different model prodrugs. Longitudinal studies confirmed that prodrug activation by Pd-NP inhibits tumour growth, extends survival in tumour-bearing mice and mitigates toxicity compared to standard doxorubicin formulations. Thus, here we demonstrate safe and efficacious in vivo catalytic activity of a Pd compound in mammals.

  11. Dinuclear Tetrapyrazolyl Palladium Complexes Exhibiting Facile Tandem Transfer Hydrogenation/Suzuki Coupling Reaction of Fluoroarylketone

    KAUST Repository

    Dehury, Niranjan; Maity, Niladri; Tripathy, Suman Kumar; Basset, Jean-Marie; Patra, Srikanta

    2016-01-01

    Herein, we report an unprecedented example of dinuclear pyrazolyl-based Pd complexes exhibiting facile tandem catalysis for fluoroarylketone: Tetrapyrazolyl di-palladium complexes with varying Pd-Pd distances efficiently catalyze the tandem reaction

  12. Synthesis of pyrrolo(2,3-b)quinolines by palladium-catalyzed heteroannulation

    International Nuclear Information System (INIS)

    Gee, Moon Bae; Lee, Won Jung; Yum, Eul Kgun

    2003-01-01

    Palladium-catalyzed heteroannulation of 2-amino-3-iodoquinoline derivatives and 1-trimethylsilyl internal alkynes provided highly regioselective pyrrolo(2,3-b)quinolines with trimethylsilyl group next to the nitrogen atom in the pyrrole ring

  13. Novel O N N Pyrazolyl-imine and Imidazolyl-imine Pincer Palladium ...

    African Journals Online (AJOL)

    NICO

    pincer palladium complexes in Heck coupling reactions. The general form of .... while single crystals suitable for X-ray analyses of complexes 1–4 were grown by ...... non-hydrogen atoms were refined with anisotropic displacement coefficients.

  14. Development of chiral terminal-alkene-phosphine hybrid ligands for palladium-catalyzed asymmetric allylic substitutions.

    Science.gov (United States)

    Liu, Zhaoqun; Du, Haifeng

    2010-07-02

    A variety of novel chiral terminal-alkene-phosphine hybrid ligands were successfully developed from diethyl L-tartrate for palladium-catalyzed asymmetric allylic alkylations, etherifications, and amination to give the desired products in excellent yields and ee's.

  15. Preparation of fluorinated biaryls through direct palladium-catalyzed coupling of polyfluoroarenes with aryltrifluoroborates

    KAUST Repository

    Fang, Xin; Huang, Yuanyuan; Chen, Xiaoqing; Lin, Xiaoxi; Bai, Zhengshuai; Huang, Kuo-Wei; Yuan, Yaofeng; Weng, Zhiqiang

    2013-01-01

    The direct palladium-catalyzed coupling of polyfluoroarenes with aryltrifluoroborates gave the desired products of fluorinated biaryls in good to excellent yields. A diverse set of important functional groups including methoxy, aldehyde, ester

  16. Nanocomposite catalyst with palladium nanoparticles encapsulated in a polymeric acid: A model for tandem environmental catalysis

    KAUST Repository

    Isimjan, Tayirjan T.; He, Quan; Liu, Yong; Zhu, Jesse; Puddephatt, Richard J.; Anderson, Darren Jason

    2013-01-01

    The synthesis and characterization of a novel hybrid nanocomposite catalyst comprised of palladium nanoparticles embedded in polystyrene sulfonic acid (PSSH) and supported on metal oxides is reported. The catalysts are intended for application

  17. Radiochemical neutron activation analysis of high pure palladium and platinum by ion exchange chromatography

    International Nuclear Information System (INIS)

    Sadikov, I.I.; Zinov'ev, V.G.; Sadikova, Z.O.; Salimov, M.I.

    2006-01-01

    Full text: The palladium and platinum are widely used for jewel manufacture because of their beautiful white color. However the most part of these metals are widely adopted in the world as catalysts. Many works on analytical chemistry of platinum group elements published during last years are devoted to determination of platinum and palladium in other materials. There are no articles on analysis technique of the palladium and platinum purity published during last 20 years. Available publications are very old and are published till 70th of the last century, and implement chemical and spectral methods. At the same time, the palladium and platinum are very suitable for NAA. Therefore the purpose of our research was development of high-sensitivity and multielement techniques of radiochemical neutron activation analysis of a high pure palladium and platinum. Research of nuclear characteristics of palladium and platinum has shown that radioactive nuclides with different yields are formed under the reactor neutrons. 109 , 111 , 111m Pd, 109m , 111 Ag, 191 , 197 , 199 Pt, 199 Au are the most important among them. 109Pd separation factor is equal to 1*10 5 at palladium analysis, whereas 197 Pt and 199 Au separation factor is equal to 1*10 4 at the platinum analysis every other day after irradiation. Palladium and platinum can be separated by precipitation, extraction and ion exchange methods. For separation of radioactive nuclide of the matrix elements from the impurity elements we used ion exchange chromatography system Dowex-1x8 - 1 M HNO 3 for palladium and Dowex-1x8 - 0.1 M HNO 3 for platinum. At the HNO 3 acid concentrations variation from 0,1 M to 1 M more then 25 elements have distribution factors less than 1 and 10 elements have distribution factors 5 while matrix elements have distribution factors higher than 100. It allows an effective separation of these elements from palladium and platinum. Optimum sizes of the chromatographic column and the column effluent

  18. Reactivity management and burn-up management on JRR-3 silicide-fuel-core

    International Nuclear Information System (INIS)

    Kato, Tomoaki; Araki, Masaaki; Izumo, Hironobu; Kinase, Masami; Torii, Yoshiya; Murayama, Yoji

    2007-08-01

    On the conversion from uranium-aluminum-dispersion-type fuel (aluminide fuel) to uranium-silicon-aluminum-dispersion-type fuel (silicide fuel), uranium density was increased from 2.2 to 4.8 g/cm 3 with keeping uranium-235 enrichment of 20%. So, burnable absorbers (cadmium wire) were introduced for decreasing excess reactivity caused by the increasing of uranium density. The burnable absorbers influence reactivity during reactor operation. So, the burning of the burnable absorbers was studied and the influence on reactor operation was made cleared. Furthermore, necessary excess reactivity on beginning of operation cycle and the time limit for restart after unplanned reactor shutdown was calculated. On the conversion, limit of fuel burn-up was increased from 50% to 60%. And the fuel exchange procedure was changed from the six-batch dispersion procedure to the fuel burn-up management procedure. The previous estimation of fuel burn-up was required for the planning of fuel exchange, so that the estimation was carried out by means of past operation data. Finally, a new fuel exchange procedure was proposed for effective use of fuel elements. On the procedure, burn-up of spent fuel was defined for each loading position. The average length of fuel's staying in the core can be increased by two percent on the procedure. (author)

  19. The whole-core LEU silicide fuel demonstration in the JMTR

    Energy Technology Data Exchange (ETDEWEB)

    Aso, Tomokazu; Akashi, Kazutomo; Nagao, Yoshiharu [Japan Atomic Energy Research Institute, Ibaraki-ken (Japan)] [and others

    1997-08-01

    The JMTR was fully converted to LEU silicide (U{sub 3}Si{sub 2}) fuel with cadmium wires as burnable absorber in January, 1994. The reduced enrichment program for the JMTR was initiated in 1979, and the conversion to MEU (enrichment ; 45%) aluminide fuel was carried out in 1986 as the first step of the program. The final goal of the program was terminated by the present LEU conversion. This paper describes the results of core physics measurement through the conversion phase from MEU fuel core to LEU fuel core. Measured excess reactivities of the LEU fuel cores are mostly in good agreement with predicted values. Reactivity effect and burnup of cadmium wires, therefore, were proved to be well predicted. Control rod worth in the LEU fuel core is mostly less than that in the MEU fuel core. Shutdown margin was verified to be within the safety limit. There is no significant difference in temperature coefficient of reactivity between the MEU and LEU fuel cores. These results verified that the JMTR was successfully and safely converted to LEU fuel. Extension of the operating cycle period was achieved and reduction of spend fuel elements is expected by using the fuel with high uranium density.

  20. Status of core conversion with LEU silicide fuel in JRR-4

    Energy Technology Data Exchange (ETDEWEB)

    Nakajima, Teruo; Ohnishi, Nobuaki; Shirai, Eiji [Japan Atomic Energy Research Institute, Ibaraki-ken (Japan)

    1997-08-01

    Japan Research Reactor No.4 (JRR-4) is a light water moderated and cooled, 93% enriched uranium ETR-type fuel used and swimming pool type reactor with thermal output of 3.5MW. Since the first criticality was achieved on January 28, 1965, JRR-4 has been used for shielding experiments, radioisotope production, neutron activation analyses, training for reactor engineers and so on for about 30 years. Within the framework of the RERTR Program, the works for conversion to LEU fuel are now under way, and neutronic and thermal-hydraulic calculations emphasizing on safety and performance aspects are being carried out. The design and evaluation for the core conversion are based on the Guides for Safety Design and Evaluation of research and testing reactor facilities in Japan. These results show that the JRR-4 will be able to convert to use LEU fuel without any major design change of core and size of fuel element. LEU silicide fuel (19.75%) will be used and maximum neutron flux in irradiation hole would be slightly decreased from present neutron flux value of 7x10{sup 13}(n/cm{sup 2}/s). The conversion works are scheduled to complete in 1998, including with upgrade of the reactor building and utilization facilities.

  1. Status of core conversion with LEU silicide fuel in JRR-4

    International Nuclear Information System (INIS)

    Nakajima, Teruo; Ohnishi, Nobuaki; Shirai, Eiji

    1997-01-01

    Japan Research Reactor No.4 (JRR-4) is a light water moderated and cooled, 93% enriched uranium ETR-type fuel used and swimming pool type reactor with thermal output of 3.5MW. Since the first criticality was achieved on January 28, 1965, JRR-4 has been used for shielding experiments, radioisotope production, neutron activation analyses, training for reactor engineers and so on for about 30 years. Within the framework of the RERTR Program, the works for conversion to LEU fuel are now under way, and neutronic and thermal-hydraulic calculations emphasizing on safety and performance aspects are being carried out. The design and evaluation for the core conversion are based on the Guides for Safety Design and Evaluation of research and testing reactor facilities in Japan. These results show that the JRR-4 will be able to convert to use LEU fuel without any major design change of core and size of fuel element. LEU silicide fuel (19.75%) will be used and maximum neutron flux in irradiation hole would be slightly decreased from present neutron flux value of 7x10 13 (n/cm 2 /s). The conversion works are scheduled to complete in 1998, including with upgrade of the reactor building and utilization facilities

  2. Experimental studies of thermal and chemical interactions between oxide and silicide nuclear fuels with water

    Energy Technology Data Exchange (ETDEWEB)

    farahani, A.A.; Corradini, M.L. [Univ. of Wisconsi, Madison, WI (United States)

    1995-09-01

    Given some transient power/cooling mismatch is a nuclear reactor and its inability to establish the necessary core cooling, energetic fuel-coolant interactions (FCI`s commonly called `vapor explosions`) could occur as a result of the core melting and coolant contact. Although a large number of studies have been done on energetic FCI`s, very few experiments have been performed with the actual fuel materials postulated to be produced in severe accidents. Because of the scarcity of well-characterized FCI data for uranium allows in noncommercial reactors (cermet and silicide fuels), we have conducted a series of experiments to provide a data base for the foregoing materials. An existing 1-D shock-tube facility was modified to handle depleted radioactive materials (U{sub 3}O{sub 8}-Al, and U{sub 3}Si{sub 2}-Al). Our objectives have been to determine the effects of the initial fuel composition and temperature and the driving pressure (triggering) on the explosion work output, dynamic pressures, transient temperatures, and the hydrogen production. Experimental results indicate limited energetics, mainly thermal interactions, for these fuel materials as compared to aluminum where more chemical reactions occur between the molten aluminum and water.

  3. Oxidation behavior of niobium aluminide intermetallics protected by aluminide and silicide diffusion coatings

    International Nuclear Information System (INIS)

    Li, Y.; Soboyejo, W.; Rapp, R.A.

    1999-01-01

    The isothermal and cyclic oxidation behavior of a new class of damage-tolerant niobium aluminide (Nb 3 Al-xTi-yCr) intermetallics is studied between 650 C and 850 C. Protective diffusion coatings were deposited by pack cementation to achieve the siliciding or aluminizing of substrates with or without intervening Mo or Ni layers, respectively. The compositions and microstructures of the resulting coatings and oxidized surfaces were characterized. The isothermal and cyclic oxidation kinetics indicate that uncoated Nb-40Ti-15Al-based intermetallics may be used up to ∼750 C. Alloying with Cr improves the isothermal oxidation resistance between 650 C and 850 C. The most significant improvement in oxidation resistance is achieved by the aluminization of electroplated Ni interlayers. The results suggest that the high-temperature limit of niobium aluminide-based alloys may be increased to 800 C to 850 C by aluminide-based diffusion coatings on ductile Ni interlayers. Indentation fracture experiments also indicate that the ductile nickel interlayers are resistant to crack propagation in multilayered aluminide-based coatings

  4. The Comparison Of Silicon Analysis For The Uranium Silicide Fuel Using Spectrophotometrical And Gravimetrical Methods

    International Nuclear Information System (INIS)

    Putro, P. K.; Suripto, A.; Putra, S.; Gunanjar

    1996-01-01

    The analysis of silicon content in the uranium silicide fuel spectro-photometrical and gravimetrical method have been performed. The nitrous oxide-acetylene was used in the atomic absorption spectrophotometry (AAS) on the wave length of 251.6 nm, and the mixture of ammonium hepta molybdate complexes and SnC1 2 as reductor were applied during analysis by UV-VIS spectrophotometry (UV-VIS) on the wave length of 757.5 mm. The reagent of HCLO 4 and HNO 3 were used for determining Si content by gravimetrical methods. The results of this comparison is as follows: the accuracy result is around 96.37 % + 0.24 % for the Si concentration up to 300 ppm (the AAS), is 138.60 % = 0.43 % for the Si concentration range between 0.1-1.5 ppm (UV-VIS), and is 51.13 % + 0.8 % for 1 gram of Si (gravimetry). The results also show that the lowest analytical error is obtained by AAS method

  5. Analysis Of Temperature Effects On Reactivity Of The Rsg-Gas Core Using Silicide Fuels

    International Nuclear Information System (INIS)

    Surbakti, Tukiran; Pinem, Surian

    2001-01-01

    RSG-GAS has been operating using new silicide fuels so that it is necessary to estimate and to measure the effect of temperature on reactivity of the core. The parameters to be determined due to temperature effect are reactivity coefficient of moderator temperature, temperature coefficient of fuel element and power reactivity coefficient. By doing a couple compensation method, determination of reactivity coefficient as well as the reactivity coefficient of moderator temperature can be obtained. Furthermore, coefficient of the reactivity was successfully estimated using the combination of WIMS-D4 and Batan-2DIFF. The cell calculation was done by using WIMS-D4 code to get macroscopic cross section and Batan-2DIFF code is used for core calculation. The calculation and experimental results of reactivity coefficient do not show any deviation from RSG-GAS safety margin. The results are -2,84 sen/ o C, -1,29 sen/MW and -0,64 sen/ o C for reactivity coefficients of temperature, power, fuel element and moderator temperature, respectively. All of 3 parameters are absolutely met with safety criteria

  6. Prompt Neutron Decay Constant Determination Of Silicide Transition Core Using Noise Method

    International Nuclear Information System (INIS)

    Jujuratisbela, Uju; Yulianto, Yusi Eko; Cahyana

    2001-01-01

    Chairman of BATAN had decided to replace the Oxide fuel element type of RSG-GAS into silicide element type step by step. The replacement will create core transitions. Kinetic characteristic of the transition cores have to be monitored in order to know the deviation of core behavior. For that reason, the kinetic parameters have to be measured. Prompt neutron decay constant (alpha) is one of the kinetic parameters that has to be monitored continuously in the transition cores. In order not to disturb the normal operation of reactor, alpha parameter should be measured by using noise analysis method. The voltage of neutron flux at power of 15 MW is connected to preamplifier and filter then to the Dynamic Signal Analyzer Version-2 and then the auto power spectral density (APSD) was determined by using Fast Fourier transform. From the APSD curve of each channel of JKT03, the cut off frequency of each channel can be determined by using linear regression technique such that the prompt neutron decay constant can be estimated

  7. Large-format platinum silicide microwave kinetic inductance detectors for optical to near-IR astronomy.

    Science.gov (United States)

    Szypryt, P; Meeker, S R; Coiffard, G; Fruitwala, N; Bumble, B; Ulbricht, G; Walter, A B; Daal, M; Bockstiegel, C; Collura, G; Zobrist, N; Lipartito, I; Mazin, B A

    2017-10-16

    We have fabricated and characterized 10,000 and 20,440 pixel Microwave Kinetic Inductance Detector (MKID) arrays for the Dark-speckle Near-IR Energy-resolved Superconducting Spectrophotometer (DARKNESS) and the MKID Exoplanet Camera (MEC). These instruments are designed to sit behind adaptive optics systems with the goal of directly imaging exoplanets in a 800-1400 nm band. Previous large optical and near-IR MKID arrays were fabricated using substoichiometric titanium nitride (TiN) on a silicon substrate. These arrays, however, suffered from severe non-uniformities in the TiN critical temperature, causing resonances to shift away from their designed values and lowering usable detector yield. We have begun fabricating DARKNESS and MEC arrays using platinum silicide (PtSi) on sapphire instead of TiN. Not only do these arrays have much higher uniformity than the TiN arrays, resulting in higher pixel yields, they have demonstrated better spectral resolution than TiN MKIDs of similar design. PtSi MKIDs also do not display the hot pixel effects seen when illuminating TiN on silicon MKIDs with photons with wavelengths shorter than 1 µm.

  8. Characterization of titanium silicide thin films by X-ray diffraction techniques

    International Nuclear Information System (INIS)

    Morimoto, N.J.

    1987-01-01

    This thesis deals with characterization techniques of thin films by means of X-ray diffraction. This includes phase identification and residual stress, microstress and crystallite size calculations. The techniques developed were applied on the study of the titanium silicide formation obtained by means of Rapidy Thermal Processing (RTP) pf Ti films deposited on silicon substratum. The different phases were studied in relation with processing temperature and time in one and two anneling steps. The low resistivity TiSi 2 phase was observed for temperature of 700 0 C and higher. The experimental results indicate that the residual stress of TiSi 2 films doesn't vary significantly with the annealing conditions. On the other hand, the microstress is reduced with annealing time at 800 0 C, while the crystallite size is almost not affected. For the microstress and the crystallite size determination technique, two methods were implemented and compared. The Riella's method appeared to be very efficient, while the Gangulle's method seemed to be inadequate, because the results oscillate too much [pt

  9. Neutron irradiated uranium silicides studied by neutron diffraction and Rietveld analysis

    International Nuclear Information System (INIS)

    Birtcher, R.C.; Mueller, M.H.; Richardson, J.W. Jr.; Faber, J. Jr.

    1989-11-01

    Uranium silicides have been considered for use as reactor fuels in both high power and low enrichment applications. However, U 3 Si was found to become amorphous under irradiation and to become mechanically unstable to rapid growth by plastic flow. U 2 Si 2 appears to be stable against amorphization at low displacement rates, but the extent of this stability is uncertain. Although the mechanisms responsible for plastic flow in U 3 Si and other amorphous systems are unknown, as is the importance of crystal structure for amorphization, it may not be surprising that these materials amorphize, in light of the fact that many radioactive nuclide - containing minerals are known to metaminctize (lose crystallinity) under irradiation. The present experiment follows the detailed changes in the crystal structures of U 3 Si and U 3 Si 2 introduced by neutron bombardment and subsequent uranium fission at room temperature. U-Si seems the ideal system for a neutron diffraction investigation since the crystallographic and amorphous forms can be studied simultaneously by combining conventional Rietveld refinement of the crystallographic phases with Fourier-filtering of the non-crystalline scattering component

  10. Determination of palladium by flame photometry; Determinacion de paladio por fotometria de llama

    Energy Technology Data Exchange (ETDEWEB)

    Parallada Bellod, R

    1964-07-01

    A study on the determination of palladium by lame photometry, fixing the most convent experimental conditions and using solvents to increase the emission of this elements is carried out. Among the organic solvents, acetone has been found the most efficient. The interferences produced by anions and cations have also been studied and an analytical method is related, in which lines of calibration of 0 to 100 ppm palladium re used. (Author) 7 refs.

  11. Facile synthesis of bacitracin-templated palladium nanoparticles with superior electrocatalytic activity

    Science.gov (United States)

    Li, Yanji; Wang, Zi; Li, Xiaoling; Yin, Tian; Bian, Kexin; Gao, Faming; Gao, Dawei

    2017-02-01

    Palladium nanomaterials have attracted great attention on the development of electrocatalysts for fuel cells. Herein, we depicted a novel strategy in the synthesis of palladium nanoparticles with superior electrocatalytic activity. The new approach, based on the self-assembly of bacitracin biotemplate and palladium salt for the preparation of bacitracin-palladium nanoparticles (Bac-PdNPs), was simple, low-cost, and green. The complex, composed by a series of spherical Bac-PdNPs with a diameter of 70 nm, exhibited a chain-liked morphology in TEM and a face-centered cubic crystal structure in X-Ray diffraction and selected area electron diffraction. The palladium nanoparticles were mono-dispersed and stable in aqueous solution as shown in TEM and zeta potential. Most importantly, compared to the commercial palladium on carbon (Pd/C) catalyst (8.02 m2 g-1), the Bac-PdNPs showed a larger electrochemically active surface area (47.57 m2 g-1), which endowed the products an excellent electrocatalytic activity for ethanol oxidation in alkaline medium. The strategy in synthesis of Bac-PdNPs via biotemplate approach might light up new ideas in anode catalysts for direct ethanol fuel cells.

  12. Crystal size effect on the electrochemical oxidation of formate on carbon-supported palladium nanoparticles

    International Nuclear Information System (INIS)

    Santos, Rayana Marcela Izidoro da Silva; Nakazato, Roberto Zenhei; Ciapina, Eduardo Goncalves

    2016-01-01

    Full text: The electrochemical oxidation of formate in alkaline electrolytes has emerged an a promising anodic reaction in the Direct Formate Fuel Cells[1]. Although palladium is considered to be one of the best electro catalyst for the oxidation of formate, important structure-activity relationships are still not understood. In the present work, we investigated the effect of the size of the palladium crystals in the electrochemical oxidation of formate in 0.1 mol L -1 KOH. Carbon-supported palladium nanoparticles (Pd/C) were prepared by chemical reduction of palladium (II) chloride in aqueous media by sodium borohydride in the presence of varying quantities of sodium citrate in the reaction media to obtain metallic crystals with distinct sizes. Analysis of the X-ray diffraction profile revealed the presence of palladium crystals in the range of 6 to 19 nm. Potentiostatic oxidation of formate on the distinct Pd/C samples revealed a volcano-like dependence of the specific activity with the size of the palladium crystals, presenting the highest activity for crystals around 7.5 nm. Reference: [1] A.M. Bartrom, J.L. Haan, The direct formate fuel cell with an alkaline anion exchange membrane, J. Power Sources. 214 (2012) 68-74. (author)

  13. Mechanism of the palladium-catalyzed hydrothiolation of alkynes to thioethers: a DFT study.

    Science.gov (United States)

    Zhang, Xing-hui; Geng, Zhi-yuan; Wang, Ke-tai; Li, Shan-shan

    2014-09-01

    The mechanisms of the palladium-catalyzed hydrothiolation of alkynes with thiols were investigated using density functional theory at the B3LYP/6-31G(d, p) (SDD for Pd) level. Solvent effects on these reactions were explored using the polarizable continuum model (PCM) for the solvent tetrahydrofuran (THF). Markovnikov-type vinyl sulfides or cis-configured anti-Markovnikov-type products were formed by three possible pathways. Our calculation results suggested the following: (1) the first step of the cycle is a proton-transfer process from thiols onto the palladium atom to form a palladium-thiolate intermediate. The palladium-thiolate species is attacked on alkynes to obtain an elimination product, liberating the catalyst. (2) The higher activation energies for the alkyne into the palladium-thiolate bond indicate that this step is the rate-determining step. The Markovnikov-type vinyl sulfide product is favored. However, for the aromatic alkyne, the cis-configured anti-Markovnikov-type product is favored. (3) The activation energy would reduce when thiols are substituted with an aromatic group. Our calculated results are consistent with the experimental observations of Frech and colleagues for the palladium-catalyzed hydrothiolation of alkynes to thiols.

  14. Preparation of Palladium-Impregnated Ceria by Metal Complex Decomposition for Methane Steam Reforming Catalysis

    Directory of Open Access Journals (Sweden)

    Worawat Wattanathana

    2017-01-01

    Full Text Available Palladium-impregnated ceria materials were successfully prepared via an integrated procedure between a metal complex decomposition method and a microwave-assisted wetness impregnation. Firstly, ceria (CeO2 powders were synthesized by thermal decomposition of cerium(III complexes prepared by using cerium(III nitrate or cerium(III chloride as a metal source to form a metal complex precursor with triethanolamine or benzoxazine dimer as an organic ligand. Palladium(II nitrate was consequently introduced to the preformed ceria materials using wetness impregnation while applying microwave irradiation to assist dispersion of the dopant. The palladium-impregnated ceria materials were obtained by calcination under reduced atmosphere of 10% H2 in He stream at 700°C for 2 h. Characterization of the palladium-impregnated ceria materials reveals the influences of the metal complex precursors on the properties of the obtained materials. Interestingly, the palladium-impregnated ceria prepared from the cerium(III-benzoxazine dimer complex revealed significantly higher BET specific surface area and higher content of the more active Pdδ+ (δ > 2 species than the materials prepared from cerium(III-triethanolamine complexes. Consequently, it exhibited the most efficient catalytic activity in the methane steam reforming reaction. By optimization of the metal complex precursors, characteristics of the obtained palladium-impregnated ceria catalysts can be modified and hence influence the catalytic activity.

  15. Development of a second generation palladium-catalyzed cycloalkenylation and its application to bioactive natural product synthesis.

    Science.gov (United States)

    Toyota, Masahiro

    2013-07-01

    A novel palladium-catalyzed intramolecular oxidative alkylation of unactivated olefins is described. This protocol was devised to solve one of the drawbacks of the original palladium-catalyzed cycloalkenylation that we developed. We call this new procedure the 'second generation palladium-catalyzed cycloalkenylation'. This protocol has been applied to the total syntheses of cis-195A, trans-195A, boonein, scholareins A, C, D, and alpha-skytanthine.

  16. Controlled immobilization of palladium nanoparticles in two different fluorinated polymeric aggregate cores and their application in catalysis

    DEFF Research Database (Denmark)

    Kijima, Tetsushi; Javakhishvili, Irakli; Jankova Atanasova, Katja

    2012-01-01

    Fluoroalkyl end-capped betaine-type cooligomeric nanocomposites-immobilized palladium nanoparticles were prepared by the reactions of palladium chloride with sodium acetate in the presence of sodium chloride and the corresponding fluorinated cooligomers. Outer blocks of poly(2,3,4,5,6-pentafluoro....... These fluorinated nanocomposites-immobilized palladium nanoparticles were also applied to the catalysts for Suzuki-Miyaura cross-coupling reaction, and the different reactivity between these nanocomposites was observed....

  17. Potential application of palladium nanoparticles as selective recyclable hydrogenation catalysts

    International Nuclear Information System (INIS)

    Mukherjee, DebKumar

    2008-01-01

    The search for more efficient catalytic systems that might combine the advantages of both homogeneous (catalyst modulation) and heterogeneous (catalyst recycling) catalysis is one of the most exciting challenges of modern chemistry. More recently with the advances of nanochemistry, it has been possible to prepare soluble analogues of heterogeneous catalysts. These nanoparticles are generally stabilized against aggregation into larger particles by electrostatic or steric protection. Herein we demonstrate the use of room temperature ionic liquid for the stabilization of palladium nanoparticles that are recyclable catalysts for the hydrogenation of carbon-carbon double bonds and application of these catalysts to the selective hydrogenation of internal or terminal C=C bonds in unsaturated primary alcohols. The particles suspended in room temperature ionic liquid show no metal aggregation or loss of catalytic activity even on prolonged use

  18. Superparamagnetic bimetallic iron-palladium nanoalloy: synthesis and characterization

    Energy Technology Data Exchange (ETDEWEB)

    Nazir, Rabia; Mazhar, Muhammad [Department of Chemistry, Quaid-i-Azam University, Islamabad 45320 (Pakistan); Akhtar, M Javed; Nadeem, M; Siddique, Muhammad [Physics Division, PINSTECH, PO Nilore, Islamabad 44000 (Pakistan); Shah, M Raza [HEJ Research Institute of Chemistry, University of Karachi, Karachi 75270 (Pakistan); Khan, Nawazish A [Material Science Laboratory, Department of Physics, Quaid-i-Azam University, Islamabad 45320 (Pakistan); Mehmood, Mazhar [National Centre for Nanotechnology, PIEAS, Islamabad 45650 (Pakistan); Butt, N M [Pakistan Science Foundation, Islamabad 44000 (Pakistan)], E-mail: mazhar42pk@yahoo.com

    2008-05-07

    Iron-palladium nanoalloy in the particle size range of 15-30 nm is synthesized by the relatively low temperature thermal decomposition of coprecipitated [Fe(Bipy){sub 3}]Cl{sub 2} and [Pd(Bipy){sub 3}]Cl{sub 2} in an inert ambient of dry argon gas. The silvery black Fe-Pd alloy nanoparticles are air-stable and have been characterized by EDX-RF, XRD, AFM, TEM, magnetometry, {sup 57}Fe Moessbauer and impedance spectroscopy. This Fe-Pd nanoalloy is in single phase and contains iron sites having up to 11 nearest-neighboring atoms. It is superparamagnetic in nature with high magnetic susceptibility, low coercivity and hyperfine field.

  19. Divergent unprotected peptide macrocyclisation by palladium-mediated cysteine arylation.

    Science.gov (United States)

    Rojas, Anthony J; Zhang, Chi; Vinogradova, Ekaterina V; Buchwald, Nathan H; Reilly, John; Pentelute, Bradley L; Buchwald, Stephen L

    2017-06-01

    Macrocyclic peptides are important therapeutic candidates due to their improved physicochemical properties in comparison to their linear counterparts. Here we detail a method for a divergent macrocyclisation of unprotected peptides by crosslinking two cysteine residues with bis-palladium organometallic reagents. These synthetic intermediates are prepared in a single step from commercially available aryl bis-halides. Two bioactive linear peptides with cysteine residues at i , i + 4 and i , i + 7 positions, respectively, were cyclised to introduce a diverse array of aryl and bi-aryl linkers. These two series of macrocyclic peptides displayed similar linker-dependent lipophilicity, phospholipid affinity, and unique volume of distributions. Additionally, one of the bioactive peptides showed target binding affinity that was predominantly affected by the length of the linker. Collectively, this divergent strategy allowed rapid and convenient access to various aryl linkers, enabling the systematic evaluation of the effect of appending unit on the medicinal properties of macrocyclic peptides.

  20. Spectroscopic study of low-temperature hydrogen absorption in palladium

    Energy Technology Data Exchange (ETDEWEB)

    Ienaga, K., E-mail: ienaga@issp.u-tokyo.ac.jp; Takata, H.; Onishi, Y.; Inagaki, Y.; Kawae, T. [Department of Applied Quantum Physics, Faculty of Engineering, Kyushu University, Motooka, Nishi-Ku, Fukuoka 819-0395 (Japan); Tsujii, H. [Department of Physics, Faculty of Education, Kanazawa University, Kakuma-machi, Kanazawa 920-1192 (Japan); Kimura, T. [Department of Physics, Kyushu University, Hakozaki, Higashi-Ku, Fukuoka 812-8581 (Japan)

    2015-01-12

    We report real-time detection of hydrogen (H) absorption in metallic palladium (Pd) nano-contacts immersed in liquid H{sub 2} using inelastic electron spectroscopy (IES). After introduction of liquid H{sub 2}, the spectra exhibit the time evolution from the pure Pd to the Pd hydride, indicating that H atoms are absorbed in Pd nano-contacts even at the temperature where the thermal process is not expected. The IES time and bias voltage dependences show that H absorption develops by applying bias voltage 30 ∼ 50 mV, which can be explained by quantum tunneling. The results represent that IES is a powerful method to study the kinetics of high density H on solid surface.

  1. Palladium-based electrocatalysts for ethanol oxidation reaction in DEFC

    International Nuclear Information System (INIS)

    Moraes, L.P.R. de; Elsheikh, A.; Silva, E. L. da; Radtke, C.; Amico, S.C.; Malfatti, C.F.

    2014-01-01

    Direct ethanol fuel cells require the use of electrocatalysts to promote bond cleavage of the ethanol molecule in an efficient way. Currently, most electrocatalysts contain platinum, which enables improved catalytic activity and stability in acidic media. However platinum presents high cost and low availability. Based on that, novel catalysts have been developed, such as those based on palladium and its alloys, which have attained excellent results in the oxidation of ethanol in alkaline media. In this work, Pd, PdSn and PdNiSn catalysts supported on Vulcan XC72R carbon were synthesized via impregnation/reduction. The electrocatalysts were characterized by RBS, XRD and cyclic voltammetry. The X-ray diffraction results showed the formation of an alloy and not the deposition of isolated elements. The synthesized catalysts displayed good catalytic activity, as observed by cyclic voltammetry, being the best electrochemical performance achieved by the ternary alloy. (author)

  2. Reactivity indexes for different geometries of palladium leads

    Energy Technology Data Exchange (ETDEWEB)

    Gomez-Carrillo, S C; Bolcatto, P G [Departamento de Fisica, Facultad de Ingenieria Quimica, Universidad Nacional de Litoral, Santiago del Estero 2829 S3000AOM Santa Fe Argentina (Argentina); Ortega, J, E-mail: scgomez@fiq.unl.edu.a [Departamento de Fisica Teorica de la Materia Condensada, Universidad Autonoma de Madrid (Spain)

    2009-05-01

    Electronic transport through metallic break junctions or molecules is clearly dependent not only on the electronic structure of the central nanodevice connecting the leads, but also the shape and crystalline orientation of the contacts which can define the possible conduction channels. In this work we examine different geometries of contacts of palladium characterizing them through global and local reactivity indexes as electrophilicity, chemical hardness and Fukui functions. In molecules, these indicators are essentially defined by the energies of the frontier molecular orbitals and in solids they are related with the local and partial density of states. We use for this purpose an ab-initio based code (FIREBALL), applied to plane contacts with (001) fcc faces and also pyramidal tips grown following a (001) and (111) packaging. The results allow us to have an insight about the chemical features of this type of nanojunctions.

  3. Palladium complexes with simple iminopyridines as catalysts for polyketone synthesis.

    Science.gov (United States)

    Rosar, V; Dedeic, D; Nobile, T; Fini, F; Balducci, G; Alessio, E; Carfagna, C; Milani, B

    2016-10-07

    Four iminopyridines (N-N') differing in the nature of the substituents on the iminic carbon and on the ortho positions of the aryl ring (H or CH3) on the iminic nitrogen were used for the synthesis of neutral and monocationic palladium(ii) complexes of general formulae [Pd(CH3)Cl(N-N')] and [Pd(CH3)(NCCH3)(N-N')][PF6]. The detailed NMR characterization in solution highlighted that: (i) for both series of complexes, the Pd-CH3 signal is progressively shifted to a lower frequency on increasing the number of methyl groups on the ligand skeleton; (ii) for the neutral derivatives, the chemical shift of the (15)N NMR signals, determined through {(1)H,(15)N}-HMBC spectra, is significantly affected by the coordination to palladium; (iii) the coordination induced shift (CIS) of the nitrogen atom trans to the CH3 ligand is smaller than the other. The structure in the solid state for the neutral derivatives with all the four ligands was solved, pointing out that: (iv) the Pd-C bond distance increases with the basicity of the nitrogen-donor ligand; (v) the Pd-N bond distance correlates well with the CIS value. The combining of the solution and solid state structural features allows stating that: (vi) the Pd-CH3 singlet is a good probe for the electron donor capability of the ligand; (vii) the CIS value might be used as a probe for the strength of the Pd-N bond. All monocationic complexes generated active catalysts for the CO/vinyl arene copolymerization, leading to prevailingly syndiotactic polyketones. The catalyst performances, both in terms of catalyst productivity and polymer molecular weight, correlate well with the precatalyst structural features.

  4. Migration behavior of palladium in UO2, (3)

    International Nuclear Information System (INIS)

    Yoneyama, Mitsuru; Sato, Seichi; Ohashi, Hiroshi; Ogawa, Toru; Ito, Akinori; Fukuda, Kousaku.

    1992-08-01

    Palladium (Pd) is easily released from UO 2 kernels in HTGR coated fuel particles, and reacts with SiC coating layer. In addition, Pd is one of metallic fission products in irradiation UO 2 , which constitutes in dissoluble residue in reprocessing of LWR fuels. In the present investigation, the migration of palladium in UO 2 was examined by heating diffusion pairs sandwiched Pd foil between UO 2 wafers at 1300 ∼ 1800degC. Experiments were also carried out on affinity of Pd to UP 2 and a formation of U-Pd alloy. Pd was found mainly in the pores of UO 2 . The maximum depth intruded by Pd in fairly large amount was more than 100 μm for UO 2 with 90%TD and 50μm for UO 2 with 95%TD, while the maximum length of open pores was 330 μm for UO 2 with 90%TD, and 50 m for that with 95%TD. Fused Pd wetted UO 2 very much. Pd intruded deeply into UO 2 , especially in the edge of Pd droplet. Furthermore, U was detected either in precipitates or the Pd source with α-Pd phase of U-Pd alloy containing Pd at about 10at%. This fact indicates that Pd highly reacts with UO 2 . From the above results, the transport of Pd in UO 2 was explained by the model of gaseous diffusion through pores in UO 2 , which is retarded by formation of U-Pd alloy. It is also indicated that UPd 3 forms even at the oxygen potential condition of O/U ratio, which is a little higher than 2.00 on the basis of thermodynamic calculation. (author)

  5. Electrophysical properties of silicon doped by palladium-103 isotope

    International Nuclear Information System (INIS)

    Makhkamov, Sh.; Tursunov, N.A.; Sattiev, A.R.; Normurodov, A.B.

    2007-01-01

    The work is devoted to study of radiation physical processes taking place in Si under nuclear transmutation, Identification and determination of defects microstructure and homogeneities and their distribution, study of interactions of nuclear-transformed phosphorus isotopes with palladium atoms, and its effect on crystal properties. For examination monocrystalline silicon of n- and p-type conductivity with specific resistance from 1 to 40 Ω·cm, dislocation density ∼10 4 cm -2 and oxygen content ∼10 17 cm -3 has been applied. Doping of silicon plates by examined admixture has been carried out by thermal diffusion method within temperature range 1000-1250 deg. C for 0.5- 5 h. Irradiation of doped silicon was conducted by reactor neutron fluences 5·10 18 - 5·10 19 cm -2 with subsequent annealing at 1000 deg. C for 30 min. Efficiency of mixture centers formation in silicon, effect of concentration of formed mixture-defect centers on electro-physical, photoelectric and recombination parameters of doped silicon and revealing of type and state of generated defects have been controlled by electric, volume and X-ray fluorescent methods. On the base of spectroscopic researches it is shown, that in silicon forbidden zone after Pd diffusion in DLTS spectra peaks related with acceptor (E c -0.18 and E v +0.34 eV) levels, and peak responsible for level E v +0.32 eV of donor character caused by palladium impurity. It is shown, that irradiation of doped silicon samples by neutrons lead to nuclear transmutation of 102 Pd, 104 Pd in 103 Pd isotopes in the crystal volume with following electron capture in stable isotope 103m Rh

  6. Pore surface fractal analysis of palladium-alumina ceramic membrane using Frenkel-Halsey-Hill (FHH) model.

    Science.gov (United States)

    Ahmad, A L; Mustafa, N N N

    2006-09-15

    The alumina ceramic membrane has been modified by the addition of palladium in order to improve the H(2) permeability and selectivity. Palladium-alumina ceramic membrane was prepared via a sol-gel method and subjected to thermal treatment in the temperature range 500-1100 degrees C. Fractal analysis from nitrogen adsorption isotherm is used to study the pore surface roughness of palladium-alumina ceramic membrane with different chemical composition (nitric acid, PVA and palladium) and calcinations process in terms of surface fractal dimension, D. Frenkel-Halsey-Hill (FHH) model was used to determine the D value of palladium-alumina membrane. Following FHH model, the D value of palladium-alumina membrane increased as the calcinations temperature increased from 500 to 700 degrees C but decreased after calcined at 900 and 1100 degrees C. With increasing palladium concentration from 0.5 g Pd/100 ml H(2)O to 2 g Pd/100 ml H(2)O, D value of membrane decreased, indicating to the smoother surface. Addition of higher amount of PVA and palladium reduced the surface fractal of the membrane due to the heterogeneous distribution of pores. However, the D value increased when nitric acid concentration was increased from 1 to 15 M. The effect of calcinations temperature, PVA ratio, palladium and acid concentration on membrane surface area, pore size and pore distribution also studied.

  7. Steady-state thermal hydraulic analysis and flow channel blockage accident analysis of JRR-3 silicide core

    International Nuclear Information System (INIS)

    Kaminaga, Masanori

    1997-03-01

    JRR-3 is a light water moderated and cooled, beryllium and heavy water reflected pool type research reactor using low enriched uranium (LEU) plate-type fuels. Its thermal power is 20 MW. The core conversion program from uranium-aluminum (UAl x -Al) dispersion type fuel (aluminide fuel) to uranium-silicon-aluminum (U 3 Si 2 -Al) dispersion type fuel (silicide fuel) is currently conducted at the JRR-3. This report describes about the steady-state thermal hydraulic analysis results and the flow channel blockage accident analysis result. In JRR-3, there are two operation mode. One is high power operation mode up to 20 MW, under forced convection cooling using the primary and the secondary cooling systems. The other is low power operation mode up to 200 kW, under natural circulation cooling between the reactor core and the reactor pool without the primary and the secondary cooling systems. For the analysis of the flow channel blockage accident, COOLOD code was used. On the other hand, steady-state thermal hydraulic analysis for both of the high power operation mode under forced convection cooling and low power operation under natural convection cooling, COOLOD-N2 code was used. From steady-state thermal hydraulic analysis results of both forced and natural convection cooling, fuel temperature, minimum DNBR etc. meet the design criteria and JRR-3 LEU silicide core has enough safety margin under normal operation conditions. Furthermore, flow channel blockage accident analysis results show that one channel flow blockage accident meet the safety criteria for accident conditions which have been established for JRR-3 LEU silicide core. (author)

  8. On the interdiffusion in multilayered silicide coatings for the vanadium-based alloy V-4Cr-4Ti

    Energy Technology Data Exchange (ETDEWEB)

    Chaia, N., E-mail: nabil.chaia@usp.br [Escola de Engenharia de Lorena, Universidade de São Paulo, Pólo Urbo-Industrial Gleba AI-6, 12602-810 Lorena, SP (Brazil); Portebois, L., E-mail: leo.portebois@univ-lorraine.fr [Université de Lorraine, Institut Jean Lamour, UMR7198, Boulevard des Aiguillettes, BP70239, 54506 Vandoeuvre-lès-Nancy, Cedex (France); Mathieu, S., E-mail: stephane.mathieu@univ-lorraine.fr [Université de Lorraine, Institut Jean Lamour, UMR7198, Boulevard des Aiguillettes, BP70239, 54506 Vandoeuvre-lès-Nancy, Cedex (France); David, N., E-mail: nicolas.david@univ-lorraine.fr [Université de Lorraine, Institut Jean Lamour, UMR7198, Boulevard des Aiguillettes, BP70239, 54506 Vandoeuvre-lès-Nancy, Cedex (France); Vilasi, M., E-mail: michel.vilasi@univ-lorraine.fr [Université de Lorraine, Institut Jean Lamour, UMR7198, Boulevard des Aiguillettes, BP70239, 54506 Vandoeuvre-lès-Nancy, Cedex (France)

    2017-02-15

    To provide protection against corrosion at high temperatures, silicide diffusion coatings were developed for the V-4Cr-4Ti alloy, which can be used as the fuel cladding in next-generation sodium-cooled fast breeder reactors. The multilayered coatings were prepared by halide-activated pack cementation using MgF{sub 2} as the transport agent and pure silicon (high activity) as the master alloy. Coated pure vanadium and coated V-4Cr-4Ti alloy were studied and compared as substrates. In both cases, the growth of the silicide layers (V{sub 3}Si, V{sub 5}Si{sub 3}, V{sub 6}Si{sub 5} and VSi{sub 2}) was controlled exclusively by solid-state diffusion, and the growth kinetics followed a parabolic law. Wagner's analysis was adopted to calculate the integrated diffusion coefficients for all silicides. The estimated values of the integrated diffusion coefficients range from approximately 10{sup −9} to 10{sup −13} cm{sup 2} s{sup −1}. Then, a diffusion-based numerical approach was used to evaluate the growth and consumption of the layers when the coated substrates were exposed at critical temperatures. The estimated lifetimes of the upper VSi{sub 2} layer were 400 h and 280 h for pure vanadium and the V-4Cr-4Ti alloy, respectively. The result from the numeric simulation was in good agreement with the layer thicknesses measured after aging the coated samples at 1150 °C under vacuum. - Highlights: • The pack cementation technique is implemented to study interdiffusion in V/Si and V-4Cr-4Ti/Si couples. • Interdiffusion coefficients of vanadium silicides were experimentally determined within the range 1100–1250 °C. • For either V/Si or V-4Cr-4Ti/Si couples, the VSi{sub 2} layer has the highest growth rate. • The Cr and Ti alloying elements mainly modified the V{sub 5}Si{sub 3} and V{sub 6}Si{sub 5} growth rate. • Numerical simulation allows for a confident assessment of the VSi{sub 2} coating lifetime on V-4Cr-4Ti.

  9. Low-temperature solution processing of palladium/palladium oxide films and their pH sensing performance.

    Science.gov (United States)

    Qin, Yiheng; Alam, Arif U; Pan, Si; Howlader, Matiar M R; Ghosh, Raja; Selvaganapathy, P Ravi; Wu, Yiliang; Deen, M Jamal

    2016-01-01

    Highly sensitive, easy-to-fabricate, and low-cost pH sensors with small dimensions are required to monitor human bodily fluids, drinking water quality and chemical/biological processes. In this study, a low-temperature, solution-based process is developed to prepare palladium/palladium oxide (Pd/PdO) thin films for pH sensing. A precursor solution for Pd is spin coated onto pre-cleaned glass substrates and annealed at low temperature to generate Pd and PdO. The percentages of PdO at the surface and in the bulk of the electrodes are correlated to their sensing performance, which was studied by using the X-ray photoelectron spectroscope. Large amounts of PdO introduced by prolonged annealing improve the electrode's sensitivity and long-term stability. Atomic force microscopy study showed that the low-temperature annealing results in a smooth electrode surface, which contributes to a fast response. Nano-voids at the electrode surfaces were observed by scanning electron microscope, indicating a reason for the long-term degradation of the pH sensitivity. Using the optimized annealing parameters of 200°C for 48 h, a linear pH response with sensitivity of 64.71±0.56 mV/pH is obtained for pH between 2 and 12. These electrodes show a response time shorter than 18 s, hysteresis less than 8 mV and stability over 60 days. High reproducibility in the sensing performance is achieved. This low-temperature solution-processed sensing electrode shows the potential for the development of pH sensing systems on flexible substrates over a large area at low cost without using vacuum equipment. Copyright © 2015 Elsevier B.V. All rights reserved.

  10. Loading rate and test temperature effects on fracture of in situ niobium silicide-niobium composites

    International Nuclear Information System (INIS)

    Rigney, J.D.; Lewandowski, J.J.

    1996-01-01

    Arc cast, extruded, and heat-treated in situ composites of niobium silicide (Nb 5 Si 3 ) intermetallic with niobium phases (primary--Nb p and secondary--Nb s ) exhibited high fracture resistance in comparison to monolithic Nb 5 Si 3 . In toughness tests conducted at 298 K and slow applied loading rates, the fracture process proceeded by the microcracking of the Nb 5 Si 3 and plastic deformation of the Nb p and Nb s phases, producing resistance-curve behavior and toughnesses of 28 MPa√m with damage zone lengths less than 500 microm. The effects of changes in the Nb p yield strength and fracture behavior on the measured toughnesses were investigated by varying the loading rates during fracture tests at both 77 and 298 K. Quantitative fractography was utilized to completely characterize each fracture surface created at 298 K in order to determine the type of fracture mode (i.e., dimpled, cleavage) exhibited by the Nb p . Specimens tested at either higher loading rates or lower test temperatures consistently exhibited a greater amount of cleavage fracture in the Nb p , while the Nb s always remained ductile. However, the fracture toughness values determined from experiments spanning six orders of magnitude in loading rate at 298 and 77 K exhibited little variation, even under conditions when the majority of Nb p phases failed by cleavage at 77 K. The changes in fracture mode with increasing loading rate and/or decreasing test temperature and their effects on fracture toughness are rationalized by comparison to existing theoretical models

  11. Effects of ball milling on microstructures and thermoelectric properties of higher manganese silicides

    International Nuclear Information System (INIS)

    Chen, Xi; Shi, Li; Zhou, Jianshi; Goodenough, John B.

    2015-01-01

    Highlights: • The already low κ L of HMS can be suppressed further by decreasing the grain size. • The ball milling process can lead to the formation of secondary MnSi and W/C-rich phases. • The formation of the MnSi ad W/C rich phases is found to suppress the thermoelectric power factor. - Abstract: Bulk nanostructured higher manganese silicide (HMS) samples with different grain size are prepared by melting, subsequent ball milling (BM), and followed by spark plasma sintering (SPS). The effects of BM time on the microstructures and thermoelectric properties of these samples are investigated. It is found that BM effectively reduces the grain size to about 90 nm in the sample after SPS, which leads to a decrease in both the thermal conductivity and electrical conductivity. By prolonging the BM time, MnSi and tungsten/carbon-rich impurity phases are formed due to the impact-induced decomposition of HMS and contamination from the tungsten carbide jar and balls during the BM, respectively. These impurities result in a reduced Seebeck coefficient and increased thermal conductivity above room temperature. The measured size-dependent lattice thermal conductivities agree qualitatively with the reported calculation results based on a combined phonon and diffuson model. The size effects are found to be increasingly significant as temperature decreases. Because of the formation of the impurity phases and a relatively large grain size, the ZT values are not improved in the ball-milled HMS samples. These findings suggest the need of alternative approaches for the synthesis of pure HMS with further reduced grain size and controlled impurity doping in order to enhance the thermoelectric figure-of-merit of HMS via nanostructuring

  12. Development of silicide coating over molybdenum based refractory alloy and its characterization

    International Nuclear Information System (INIS)

    Chakraborty, S.P.; Banerjee, S.; Sharma, I.G.; Suri, A.K.

    2010-01-01

    Molybdenum based refractory alloys are potential candidate materials for structural applications in high temperature compact nuclear reactors and fusion reactors. However, these alloys being highly susceptible to oxidation in air or oxygen at elevated temperature, undergoes severe losses from highly volatile molybdenum trioxide species. Present investigation, therefore, examines the feasibility of development of silicide type of coating over molybdenum base TZM alloy shape (Mo > 99 wt.%) using pack cementation coating technique. TZM alloy was synthesized in this laboratory from oxide intermediates of MoO 2 , TiO 2 and ZrO 2 in presence of requisite amount of carbon, by alumino-thermic reduction smelting technique. The arc melted and homogenized samples of TZM alloy substrate was then embedded in the chosen and intimately mixed pack composition consisting of inert matrix (Al 2 O 3 ), coating powder (Si) and activator (NH 4 Cl) taken in the judicious proportion. The sealed charge packs contained in an alumina crucible were heated at temperatures of 1000 o C for 8-16 h heating cycle to develop the coating. The coating phase was confirmed to be of made of MoSi 2 by XRD analysis. The morphology of the coating was studied by SEM characterization. It had revealed that the coating was diffusion bonded where Si from coating diffused inward and Mo from TZM substrate diffused outward to form the coating. The coating was found to be resistant to oxidation when tested in air up to 1200 o C. A maximum 100 μm of coating thickness was achieved on each side of the substrate.

  13. Fuel loading and homogeneity analysis of HFIR design fuel plates loaded with uranium silicide fuel

    International Nuclear Information System (INIS)

    Blumenfeld, P.E.

    1995-08-01

    Twelve nuclear reactor fuel plates were analyzed for fuel loading and fuel loading homogeneity by measuring the attenuation of a collimated X-ray beam as it passed through the plates. The plates were identical to those used by the High Flux Isotope Reactor (HFIR) but were loaded with uranium silicide rather than with HFIR's uranium oxide fuel. Systematic deviations from nominal fuel loading were observed as higher loading near the center of the plates and underloading near the radial edges. These deviations were within those allowed by HFIR specifications. The report begins with a brief background on the thermal-hydraulic uncertainty analysis for the Advanced Neutron Source (ANS) Reactor that motivated a statistical description of fuel loading and homogeneity. The body of the report addresses the homogeneity measurement techniques employed, the numerical correction required to account for a difference in fuel types, and the statistical analysis of the resulting data. This statistical analysis pertains to local variation in fuel loading, as well as to ''hot segment'' analysis of narrow axial regions along the plate and ''hot streak'' analysis, the cumulative effect of hot segment loading variation. The data for all twelve plates were compiled and divided into 20 regions for analysis, with each region represented by a mean and a standard deviation to report percent deviation from nominal fuel loading. The central regions of the plates showed mean values of about +3% deviation, while the edge regions showed mean values of about -7% deviation. The data within these regions roughly approximated random samplings from normal distributions, although the chi-square (χ 2 ) test for goodness of fit to normal distributions was not satisfied

  14. Electronic structure and bonding in the ternary silicide YNiSi3

    International Nuclear Information System (INIS)

    Sung, Gi Hong; Kang, Dae Bok

    2003-01-01

    An analysis of the electronic structure and bonding in the ternary silicide YNiSi 3 is made, using extended Hueckel tight-binding calculations. The YNiSi 3 structure consists of Ni-capped Si 2 dimer layers and Si zigzag chains. Significant bonding interactions are present between the silicon atoms in the structure. The oxidation state formalism of (Y 3+ )(Ni 0 )(Si 3 ) 3- for YNiSi 3 constitutes a good starting point to describe its electronic structure. Si atoms receive electrons form the most electropositive Y in YNiSi 3 , and Ni 3d and Si 3p states dominate below the Fermi level. There is an interesting electron balance between the two Si and Ni sublattices. Since the π orbitals in the Si chain and the Ni d and s block levels are almost completely occupied, the charge balance for YNiSi 3 can be rewritten as (Y 3+ )(Ni 2- )(Si 2- )(Si-Si) + , making the Si 2 layers oxidized. These results suggest that the Si zigzag chain contains single bonds and the Si 2 double layer possesses single bonds within a dimer with a partial double bond character. Stronger Si-Si and Ni-Si bonding interactions are important for giving stability to the structure, while essentially no metal-metal bonding exists at all. The 2D metallic behavior of this compound is due to the Si-Si interaction leading to dispersion of the several Si 2 π bands crossing the Fermi level in the plane perpendicular to the crystallographic b axis

  15. Rate Theory Modeling and Simulation of Silicide Fuel at LWR Conditions

    Energy Technology Data Exchange (ETDEWEB)

    Miao, Yinbin [Argonne National Lab. (ANL), Argonne, IL (United States). Nuclear Engineering Division; Ye, Bei [Argonne National Lab. (ANL), Argonne, IL (United States). Nuclear Engineering Division; Hofman, Gerard [Argonne National Lab. (ANL), Argonne, IL (United States). Nuclear Engineering Division; Yacout, Abdellatif [Argonne National Lab. (ANL), Argonne, IL (United States). Nuclear Engineering Division; Gamble, Kyle [Idaho National Lab. (INL), Idaho Falls, ID (United States). Fuel Modeling and Simulation; Mei, Zhi-Gang [Argonne National Lab. (ANL), Argonne, IL (United States). Nuclear Engineering Division

    2016-08-29

    As a promising candidate for the accident tolerant fuel (ATF) used in light water reactors (LWRs), the fuel performance of uranium silicide (U3Si2) at LWR conditions needs to be well understood. In this report, rate theory model was developed based on existing experimental data and density functional theory (DFT) calculations so as to predict the fission gas behavior in U3Si2 at LWR conditions. The fission gas behavior of U3Si2 can be divided into three temperature regimes. During steady-state operation, the majority of the fission gas stays in intragranular bubbles, whereas the dominance of intergranular bubbles and fission gas release only occurs beyond 1000 K. The steady-state rate theory model was also used as reference to establish a gaseous swelling correlation of U3Si2 for the BISON code. Meanwhile, the overpressurized bubble model was also developed so that the fission gas behavior at LOCA can be simulated. LOCA simulation showed that intragranular bubbles are still dominant after a 70 second LOCA, resulting in a controllable gaseous swelling. The fission gas behavior of U3Si2 at LWR conditions is benign according to the rate theory prediction at both steady-state and LOCA conditions, which provides important references to the qualification of U3Si2 as a LWR fuel material with excellent fuel performance and enhanced accident tolerance.

  16. Synthesis and characterization of β-phase iron silicide nano-particles by chemical reduction

    International Nuclear Information System (INIS)

    Sen, Sabyasachi; Gogurla, Narendar; Banerji, Pallab; Guha, Prasanta K.; Pramanik, Panchanan

    2015-01-01

    Graphical abstract: - Highlights: • β-FeSi 2 nano-particle was synthesized by reducing with Mg and by diluting with MgO. • XRD profile shows the iron di-silicide phase to be semiconducting β-FeSi 2 . • HRTEM and FESEM images indicate the β-FeSi 2 average particle size to be 60–70 nm. • Absorption, reflectance and PL spectroscopy show band gap to be direct 0.87 eV. • Nano-β-FeSi 2 is p-type with hole density of 4.38 × 10 18 cm −3 and mobility 8.9 cm 2 /V s. - Abstract: Nano-particles of β-FeSi 2 have been synthesized by chemical reduction of a glassy phase of [Fe 2 O 3 , 4SiO 2 ] by Mg-metal where MgO is used as diluent to prevent the agglomeration of nano crystallites into micro-particles and also act as a negative catalyst for the formation of other phases. The sample is characterized by XRD, FESEM, HRTEM, EDX, ultra-violet-visible-infrared and PL spectroscopy and electronic properties have been investigated by Hall measurement. XRD profile shows that the synthesized powder consists of purely β-FeSi 2 semiconducting phase. The average crystallite size of β-FeSi 2 is determined to be around 65.4 nm from XRD peaks as well as from FESEM also. The optical absorption and PL spectroscopy shows that synthesized β-FeSi 2 phase is a direct band gap semiconductor with a value of 0.87 eV. Hall measurements show that β-FeSi 2 nano-particles is p-type with hole concentration of 4.38 × 10 18 cm −3 and average hole mobility of 8.9 cm 2 /V s at 300 K

  17. Effects of ball milling on microstructures and thermoelectric properties of higher manganese silicides

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Xi [Materials Science and Engineering Program, Texas Materials Institute, The University of Texas at Austin, Austin, TX 78712 (United States); Shi, Li, E-mail: lishi@mail.utexas.edu [Materials Science and Engineering Program, Texas Materials Institute, The University of Texas at Austin, Austin, TX 78712 (United States); Department of Mechanical Engineering, The University of Texas at Austin, Austin, TX 78712 (United States); Zhou, Jianshi; Goodenough, John B. [Materials Science and Engineering Program, Texas Materials Institute, The University of Texas at Austin, Austin, TX 78712 (United States); Department of Mechanical Engineering, The University of Texas at Austin, Austin, TX 78712 (United States)

    2015-08-25

    Highlights: • The already low κ{sub L} of HMS can be suppressed further by decreasing the grain size. • The ball milling process can lead to the formation of secondary MnSi and W/C-rich phases. • The formation of the MnSi ad W/C rich phases is found to suppress the thermoelectric power factor. - Abstract: Bulk nanostructured higher manganese silicide (HMS) samples with different grain size are prepared by melting, subsequent ball milling (BM), and followed by spark plasma sintering (SPS). The effects of BM time on the microstructures and thermoelectric properties of these samples are investigated. It is found that BM effectively reduces the grain size to about 90 nm in the sample after SPS, which leads to a decrease in both the thermal conductivity and electrical conductivity. By prolonging the BM time, MnSi and tungsten/carbon-rich impurity phases are formed due to the impact-induced decomposition of HMS and contamination from the tungsten carbide jar and balls during the BM, respectively. These impurities result in a reduced Seebeck coefficient and increased thermal conductivity above room temperature. The measured size-dependent lattice thermal conductivities agree qualitatively with the reported calculation results based on a combined phonon and diffuson model. The size effects are found to be increasingly significant as temperature decreases. Because of the formation of the impurity phases and a relatively large grain size, the ZT values are not improved in the ball-milled HMS samples. These findings suggest the need of alternative approaches for the synthesis of pure HMS with further reduced grain size and controlled impurity doping in order to enhance the thermoelectric figure-of-merit of HMS via nanostructuring.

  18. Significant enhancement in thermoelectric performance of nanostructured higher manganese silicides synthesized employing a melt spinning technique.

    Science.gov (United States)

    Muthiah, Saravanan; Singh, R C; Pathak, B D; Avasthi, Piyush Kumar; Kumar, Rishikesh; Kumar, Anil; Srivastava, A K; Dhar, Ajay

    2018-01-25

    The limited thermoelectric performance of p-type Higher Manganese Silicides (HMS) in terms of their low figure-of-merit (ZT), which is far below unity, is the main bottle-neck for realising an efficient HMS based thermoelectric generator, which has been recognized as the most promising material for harnessing waste-heat in the mid-temperature range, owing to its thermal stability, earth-abundant and environmentally friendly nature of its constituent elements. We report a significant enhancement in the thermoelectric performance of nanostructured HMS synthesized using rapid solidification by optimizing the cooling rates during melt-spinning followed by spark plasma sintering of the resulting melt-spun ribbons. By employing this experimental strategy, an unprecedented ZT ∼ 0.82 at 800 K was realized in spark plasma sintered 5 at% Al-doped MnSi 1.73 HMS, melt spun at an optimized high cooling rate of ∼2 × 10 7 K s -1 . This enhancement in ZT represents a ∼25% increase over the best reported values thus far for HMS and primarily originates from a nano-crystalline microstructure consisting of a HMS matrix (20-40 nm) with excess Si (3-9 nm) uniformly distributed in it. This nanostructure, resulting from the high cooling rates employed during the melt-spinning of HMS, introduces a high density of nano-crystallite boundaries in a wide spectrum of nano-scale dimensions, which scatter the low-to-mid-wavelength heat-carrying phonons. This abundant phonon scattering results in a significantly reduced thermal conductivity of ∼1.5 W m -1 K -1 at 800 K, which primarily contributes to the enhancement in ZT.

  19. Evaluation of steam corrosion and water quenching behavior of zirconium-silicide coated LWR fuel claddings

    Science.gov (United States)

    Yeom, Hwasung; Lockhart, Cody; Mariani, Robert; Xu, Peng; Corradini, Michael; Sridharan, Kumar

    2018-02-01

    This study investigates steam corrosion of bulk ZrSi2, pure Si, and zirconium-silicide coatings as well as water quenching behavior of ZrSi2 coatings to evaluate its feasibility as a potential accident-tolerant fuel cladding coating material in light water nuclear reactor. The ZrSi2 coating and Zr2Si-ZrSi2 coating were deposited on Zircaloy-4 flats, SiC flats, and cylindrical Zircaloy-4 rodlets using magnetron sputter deposition. Bulk ZrSi2 and pure Si samples showed weight loss after the corrosion test in pure steam at 400 °C and 10.3 MPa for 72 h. Silicon depletion on the ZrSi2 surface during the steam test was related to the surface recession observed in the silicon samples. ZrSi2 coating (∼3.9 μm) pre-oxidized in 700 °C air prevented substrate oxidation but thin porous ZrO2 formed on the coating. The only condition which achieved complete silicon immobilization in the oxide scale in aqueous environments was the formation of ZrSiO4 via ZrSi2 coating oxidation in 1400 °C air. In addition, ZrSi2 coatings were beneficial in enhancing quenching heat transfer - the minimum film boiling temperature increased by 6-8% in the three different environmental conditions tested. During repeated thermal cycles (water quenching from 700 °C to 85 °C for 20 s) performed as a part of quench tests, no spallation and cracking was observed and the coating prevented oxidation of the underlying Zircaloy-4 substrate.

  20. The study of hydrogen electrosorption in layered nickel foam/palladium/carbon nanofibers composite electrodes

    International Nuclear Information System (INIS)

    Skowronski, J.M.; Czerwinski, A.; Rozmanowski, T.; Rogulski, Z.; Krawczyk, P.

    2007-01-01

    In the present work, the process of hydrogen electrosorption occurring in alkaline KOH solution on the nickel foam/palladium/carbon nanofibers (Ni/Pd/CNF) composite electrodes is examined. The layered Ni/Pd/CNF electrodes were prepared by a two-step method consisting of chemical deposition of a thin layer of palladium on the nickel foam support to form Ni/Pd electrode followed by coating the palladium layer with carbon nanofibers layer by means of the CVD method. The scanning electron microscope was used for studying the morphology of both the palladium and carbon layer. The process of hydrogen sorption/desorption into/from Ni/Pd as well as Ni/Pd/CNF electrode was examined using the cyclic voltammetry method. The amount of hydrogen stored in both types of composite electrodes was shown to increase on lowering the potential of hydrogen sorption. The mechanism of the anodic desorption of hydrogen changes depending on whether or not CNF layer is present on the Pd surface. The anodic peak corresponding to the removal of hydrogen from palladium is lower for Ni/Pd/CNF electrode as compared to that measured for Ni/Pd one due to a partial screening of the Pd surface area by CNF layer. The important feature of Ni/Pd/CNF electrode is anodic peak appearing on voltammetric curves at potential ca. 0.4 V more positive than the peak corresponding to hydrogen desorption from palladium. The obtained results showed that upon storing the hydrogen saturated Ni/Pd/CNF electrode at open circuit potential, diffusion of hydrogen from carbon to palladium phase occurs due to interaction between carbon fibers and Pd sites on the nickel foam support

  1. The electrocatalytical reduction of m-nitrophenol on palladium nanoparticles modified glassy carbon electrodes

    International Nuclear Information System (INIS)

    Shi Qiaofang; Diao Guowang

    2011-01-01

    Highlights: ► The deposition of palladium on a GC electrode was performed by cyclic voltammetry. ► SEM images showed palladium nanoparticles deposited on a glassy carbon (GC) electrode. ► The Pd/GC electrode can effectively catalyze m-nitrophenol in aqueous media. ► The reduction of m-nitrophenol on the Pd/GC electrode depended on potential and pH. ► XPS spectra of the Pd/GC electrodes demonstrated the presence of palladium. - Abstract: Palladium nanoparticles modified glassy carbon electrodes (Pd/GC) were prepared via the electrodeposition of palladium on a glassy carbon (GC) electrode using cyclic voltammetry in different sweeping potential ranges. The scanning electron microscope images of palladium particles on the GC electrodes indicate that palladium particles with diameters of 20–50 nm were homogeneously dispersed on the GC electrode at the optimal deposition conditions, which can effectively catalyze the reduction of m-nitrophenol in aqueous solutions, but their catalytic activities are strongly related to the deposition conditions of Pd. The X-ray photoelectron spectroscopy spectra of the Pd/GC electrode confirmed that 37.1% Pd was contained in the surface composition of the Pd/GC electrode. The cyclic voltammograms of the Pd/GC electrode in the solution of m-nitrophenol show that the reduction peak of m-nitrophenol shifts towards the more positive potentials, accompanied with an increase in the peak current compared to the bare GC electrode. The electrocatalytic activity of the Pd/GC electrode is affected by pH values of the solution. In addition, the electrolysis of m-nitrophenol under a constant potential indicates that the reduction current of m-nitrophenol on the Pd/GC electrode is approximately 20 times larger than that on the bare GC electrode.

  2. Observation of Binuclear Palladium Clusters Upon ESI-MS Monitoring of the Suzuki-Miyaura Cross-Coupling Catalyzed by a Dichloro-bis(aminophosphine) Complex of Palladium

    Czech Academy of Sciences Publication Activity Database

    Agrawal, Divya; Schröder, Detlef; Frech, C. M.

    2011-01-01

    Roč. 30, č. 13 (2011), s. 3579-3587 ISSN 0276-7333 Institutional research plan: CEZ:AV0Z40550506 Keywords : catalysis * C-C coupling * electrospray ionization * palladium * Suzuki-Miyaura coupling Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 3.963, year: 2011

  3. Hot wire chemical vapor deposition: limits and opportunities of protecting the tungsten catalyzer from silicide with a cavity

    International Nuclear Information System (INIS)

    Frigeri, P.A.; Nos, O.; Bengoechea, S.; Frevert, C.; Asensi, J.M.; Bertomeu, J.

    2009-01-01

    Hot Wire Chemical Vapor Deposition (HW-CVD) is one of the most promising techniques for depositing the intrinsic microcrystalline silicon layer for the production of micro-morph solar cells. However, the silicide formation at the colder ends of the tungsten wire drastically reduces the lifetime of the catalyzer, thus limiting its industrial exploitation. A simple but interesting strategy to decrease the silicide formation is to hide the electrical contacts of the catalyzer in a long narrow cavity which reduces the probability of the silane molecules to reach the colder ends of the wire. In this paper, the working mechanism of the cavity is elucidated. Measurements of the thickness profile of the silicon deposited in the internal walls of the cavity have been compared with those predicted using a simple diffusion model based on the assumption of Knudsen flow. A lifetime study of the protected and unprotected wires has been carried out. The different mechanisms which determine the deterioration of the catalyzer have been identified and discussed.

  4. Silicide induced surface defects in FePt nanoparticle fcc-to-fct thermally activated phase transition

    International Nuclear Information System (INIS)

    Chen, Shu; Lee, Stephen L.; André, Pascal

    2016-01-01

    Magnetic nanoparticles (MnPs) are relevant to a wide range of applications including high density information storage and magnetic resonance imaging to name but a few. Among the materials available to prepare MnPs, FePt is attracting growing attention. However, to harvest the strongest magnetic properties of FePt MnPs, a thermal annealing is often required to convert face-centered cubic as synthesized nPs into its tetragonal phase. Rarely addressed are the potential side effects of such treatments on the magnetic properties. In this study, we focus on the impact of silica shells often used in strategies aiming at overcoming MnP coalescence during the thermal annealing. While we show that this shell does prevent sintering, and that fcc-to-fct conversion does occur, we also reveal the formation of silicide, which can prevent the stronger magnetic properties of fct-FePt MnPs from being fully realised. This report therefore sheds lights on poorly investigated and understood interfacial phenomena occurring during the thermal annealing of MnPs and, by doing so, also highlights the benefits of developing new strategies to avoid silicide formation.

  5. Silicide induced surface defects in FePt nanoparticle fcc-to-fct thermally activated phase transition

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Shu; Lee, Stephen L. [School of Physics and Astronomy, SUPA, University of St Andrews, St Andrews KY16 9SS (United Kingdom); André, Pascal, E-mail: pjpandre@riken.jp [School of Physics and Astronomy, SUPA, University of St Andrews, St Andrews KY16 9SS (United Kingdom); RIKEN, Wako 351-0198 (Japan); Department of Physics, CNRS-Ewha International Research Center (CERC), Ewha W. University, Seoul 120-750 (Korea, Republic of)

    2016-11-01

    Magnetic nanoparticles (MnPs) are relevant to a wide range of applications including high density information storage and magnetic resonance imaging to name but a few. Among the materials available to prepare MnPs, FePt is attracting growing attention. However, to harvest the strongest magnetic properties of FePt MnPs, a thermal annealing is often required to convert face-centered cubic as synthesized nPs into its tetragonal phase. Rarely addressed are the potential side effects of such treatments on the magnetic properties. In this study, we focus on the impact of silica shells often used in strategies aiming at overcoming MnP coalescence during the thermal annealing. While we show that this shell does prevent sintering, and that fcc-to-fct conversion does occur, we also reveal the formation of silicide, which can prevent the stronger magnetic properties of fct-FePt MnPs from being fully realised. This report therefore sheds lights on poorly investigated and understood interfacial phenomena occurring during the thermal annealing of MnPs and, by doing so, also highlights the benefits of developing new strategies to avoid silicide formation.

  6. Surface effect on the electronic and the magnetic properties of rock-salt alkaline-earth metal silicides

    International Nuclear Information System (INIS)

    Bialek, Beata; Lee, Jaeil

    2011-01-01

    An all electron ab-initio method was employed to study the electronic and the magnetic properties of the (001) surface of alkaline-earth metal silicides, CaSi, SrSi, and BaSi, in the rock-salt structure. The three compounds retain their ferromagnetic metallic properties at the surface. Due to the surface effects, the magnetism of the topmost layer is changed as compared with the bulk. This is a short-range effect. In CaSi, the magnetism of the surface layer is noticeably reduced, as compared with the bulk: magnetic moments (MMs) on both Ca and Si atoms are reduced. In SrSi (001), the polarization of electrons in the surface atoms is similar to that in the bulk atoms, and the values of MMs on the component atoms in the topmost layer do not change as much as in CaSi. In BaSi (001), the magnetic properties of Si surface atoms are enhanced slightly, and the magnetism of Ba atoms is not affected considerably by the surface effect. The calculated densities of states confirm the short-range effect of the surface on the electronic properties of the metal silicides.

  7. Ytterbium silicide (YbSi{sub 2}). A promising thermoelectric material with a high power factor at room temperature

    Energy Technology Data Exchange (ETDEWEB)

    Tanusilp, Sora-at; Ohishi, Yuji; Muta, Hiroaki [Graduate School of Engineering, Osaka University, Suita, Osaka (Japan); Yamanaka, Shinsuke [Graduate School of Engineering, Osaka University, Suita, Osaka (Japan); Research Institute of Nuclear Engineering, University of Fukui, Tsuruga (Japan); Nishide, Akinori [Graduate School of Engineering, Osaka University, Suita, Osaka (Japan); Center for Exploratory Research, Research and Development Group, Hitachi, Ltd., Kokubunji, Tokyo (Japan); Hayakawa, Jun [Center for Exploratory Research, Research and Development Group, Hitachi, Ltd., Kokubunji, Tokyo (Japan); Kurosaki, Ken [Graduate School of Engineering, Osaka University, Suita, Osaka (Japan); Research Institute of Nuclear Engineering, University of Fukui, Tsuruga (Japan); JST, PRESTO, Kawaguchi, Saitama (Japan)

    2018-02-15

    Metal silicide-based thermoelectric (TE) materials have attracted attention in the past two decades, because they are less toxic, with low production cost and high chemical stability. Here, we study the TE properties of ytterbium silicide YbSi{sub 2} with a specific layered structure and the mixed valence state of Yb{sup 2+} and Yb{sup 3+}. YbSi{sub 2} exhibits large Seebeck coefficient, S, accompanied by high electrical conductivity, σ, leading to high power factor, S{sup 2}σ, of 2.2 mW m{sup -1} K{sup -2} at room temperature, which is comparable to those of state-of-the-art TE materials such as Bi{sub 2}Te{sub 3} and PbTe. Moreover, YbSi{sub 2} exhibits high Grueneisen parameter of 1.57, which leads to relatively low lattice thermal conductivity, κ{sub lat}, of 3.0 W m{sup -1} K{sup -1} at room temperature. The present study reveals that YbSi{sub 2} can be a good candidate of TE materials working near room temperature. (copyright 2017 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  8. Technical report: technical development on the silicide plate-type fuel experiment at nuclear safety research reactor

    International Nuclear Information System (INIS)

    Yanagisawa, Kazuaki; Soyama, Kazuhiko; Ichikawa, Hiroki

    1991-08-01

    According to a reduction of fuel enrichment from 45 w/o 235 U to 20 w/o, an aluminide plate-type fuel used currently in the domestic research and material testing reactors will be replaced by a silicide plate-type one. One of the major concern arisen from this alternation is to understand the fuel behavior under simulated reactivity initiated accident (RIA) conditions, this is strongly necessary from the safety and licensing point of view. The in-core RIA experiments are, therefore, carried out at Nuclear Safety Research Reactor (NSRR) in Japan Atomic Energy Research Institute (JAERI). The silicide plate-type fuel consisted of the ternary alloy of U-Al-Si as a meat with uranium density up to 4.8 g/cm 3 having thickness by 0.51 mm and the binary alloy of Al-3%Mg as a cladding by thickness of 0.38 mm. Comparison of the physical properties of this metallic plate fuel with the UO 2 -zircaloy fuel rod used conventionally in commercial light water reactors shows that the heat conductivity of the former is of the order of about 13 times greater than the latter, however the melting temperature is only one-half (1570degC). Prior to in-core RIA experiments, there were some difficulties lay in our technical path. This report summarized the technical achievements obtained through our four years work. (J.P.N.)

  9. Separation of Hydrogen Isotopes by Palladium Alloy Membranes Separator

    International Nuclear Information System (INIS)

    Jiangfeng, S.; Deli, L.; Yifu, X.; Congxian, L.; Zhiyong, H.

    2007-01-01

    Full text of publication follows: Separation of hydrogen isotope with palladium alloy membranes is one of the promising methods for hydrogen isotope separation. It has several advantages, such as high separation efficiency, smaller tritium inventory, simple separation device, ect. Limited by the manufacture of membrane and cost of gas transportation pump, this method is still at the stage of conceptual study. The relationship between separation factors and temperatures, feed gas components, split ratios have not been researched in detail, and the calculated results of cascade separation have not been validated with experimental data. In this thesis, a palladium alloy membrane separator was designed to further study its separation performance between H 2 and D 2 . The separation factor of the single stage was affected by the temperature, the feed gas component, the split ratio and the gas flow rate, etc. The experimental results showed that the H 2 -D 2 separation factor decreased with the increasing of temperature. On the temperature from 573 K to 773 K, when the feed rate was 5 L/min, the separation factor of 66.2%H 2 - 33.8%D 2 decreased from 2.09 to 1.85 when the split ratio was 0.1 and from 1.74 to 1.52 when the split ratio was 0.2.The separation factor also decreased with the increasing of split ratio. At 573 K and the feed rate of 5 L/min, the separation factor of 15.0%H 2 and 85.0%D 2 decreased from 2.43 to 1.35 with the increasing of split ratio from 0.050 to 0.534,and for 66.2%H 2 -33.8%D 2 , the separation factor decreased from 2.87 to 1.30 with the increasing of split ratio from 0.050 to 0.688. When the separation factor was the biggest, the flow rate of feed gas was in a perfect value. To gain a best separation performance, perfect flow rate, lower temperature and reflux ratio should be chosen. (authors)

  10. Influence of residual catalyst on the properties of conjugated polyphenylenevinylene materials: Palladium nanoparticles and poor electrical performance

    DEFF Research Database (Denmark)

    Krebs, Frederik C; Nyberg, R.B.; Jørgensen, M.

    2004-01-01

    polymer material prepared by two different routes: the palladium route and the condensation route. The performance in a device application of the two polymer materials was, however, very different, and the palladium route was demonstrated to give poor films with low breakdown voltages and short circuits....

  11. Chiral separation of substituted phenylalanine analogues using chiral palladium phosphine complexes with enantioselective liquid-liquid extraction

    NARCIS (Netherlands)

    Verkuijl, B.J.V.; Schuur, B.; Minnaard, A.J.; Vries, de J.G.; Feringa, B.L.

    2010-01-01

    Chiral palladium phosphine complexes have been employed in the chiral separation of amino acids and phenylalanine analogues in particular. The use of (S)-xylyl-BINAP as a ligand for the palladium complex in enantioselective liquid–liquid extraction allowed the separation of the phenylalanine

  12. Palladium on Carbon-Catalyzed Suzuki-Miyaura Coupling Reaction Using an Efficient and Continuous Flow System

    Directory of Open Access Journals (Sweden)

    Tomohiro Hattori

    2015-01-01

    Full Text Available The continuous flow Suzuki-Miyaura reaction between various haloarenes and arylboronic acids was successfully achieved within only ca. 20 s during the single-pass through a cartridge filled with palladium on carbon (Pd/C. No palladium leaching was observed in the collected reaction solution by atomic absorption spectrometry (detection limit: 1 ppm.

  13. High-temperature oxidation of silicide-aluminide layer on the TiAl6V4 alloy prepared by liquid-phase siliconizing

    Czech Academy of Sciences Publication Activity Database

    Kubatík, Tomáš František

    2016-01-01

    Roč. 50, č. 2 (2016), s. 257-261 ISSN 1580-2949 Institutional support: RVO:61389021 Keywords : TiAl6V4 * silicides * high-temperature oxidation * liquid-phase silicon izing Subject RIV: JG - Metallurgy Impact factor: 0.436, year: 2016

  14. Palladium-Catalyzed Cross-Coupling Reactions of Perfluoro Organic Compounds

    Directory of Open Access Journals (Sweden)

    Masato Ohashi

    2014-09-01

    Full Text Available In this review, we summarize our recent development of palladium(0-catalyzed cross-coupling reactions of perfluoro organic compounds with organometallic reagents. The oxidative addition of a C–F bond of tetrafluoroethylene (TFE to palladium(0 was promoted by the addition of lithium iodide, affording a trifluorovinyl palladium(II iodide. Based on this finding, the first palladium-catalyzed cross-coupling reaction of TFE with diarylzinc was developed in the presence of lithium iodide, affording α,β,β-trifluorostyrene derivatives in excellent yield. This coupling reaction was expanded to the novel Pd(0/PR3-catalyzed cross-coupling reaction of TFE with arylboronates. In this reaction, the trifluorovinyl palladium(II fluoride was a key reaction intermediate that required neither an extraneous base to enhance the reactivity of organoboronates nor a Lewis acid additive to promote the oxidative addition of a C–F bond. In addition, our strategy utilizing the synergetic effect of Pd(0 and lithium iodide could be applied to the C–F bond cleavage of unreactive hexafluorobenzene (C6F6, leading to the first Pd(0-catalyzed cross-coupling reaction of C6F6 with diarylzinc compounds.

  15. Factors affecting the corrosion of SiC layer by fission product palladium

    International Nuclear Information System (INIS)

    Dewita, E.

    2000-01-01

    HTR is one of the advanced nuclear reactors which has inherent safety system, graphite moderated and helium gas cooled. In general, these reactors are designed with the TRISO coated particle consist of four coating layers that are porous pyrolytic carbon (PyC). inner dense PyC (IPyC), silicon carbide (SiC), and outer dense PyC (OPyC). Among the four coating layers, the SiC plays an important role beside in retaining metallic fission products, it also provides mechanical strength to fuel particle. However, results of post irradiation examination indicate that fission product palladium can react with and corrode SiC layer, This assessment is conducted to get the comprehension about resistance of SiC layer on irradiation effects, especially in order to increase the fuel bum-up. The result of this shows that the corrosion of SiC layer by fission product palladium is beside depend on the material characteristics of SiC, and also there are other factors that affect on the SiC layer corrosion. Fuel enrichment, bum-up, and irradiation time effect on the palladium flux in fuel kernel. While, the fuel density, vapour pressure of palladium (the degree depend on the irradiation temperature and kernel composition) effect on palladium migration in fuel particle. (author)

  16. Some remarks on the neutron elastic- and enelastic-scattering cross sections of palladium

    International Nuclear Information System (INIS)

    Chiba, S.; Guenther, P.T.; Smith, A.B.

    1989-05-01

    The cross sections for the elastic-scattering of 5.9, 7.1 and 8.0 MeV neutrons from elemental palladium were measured at forty scattering angles distributed between ∼15/degree/ and 160/degree/. The inelastic-scattering cross sections for the excitation of palladium levels at energies of 260 keV to 560 keV were measured with high resolution at the same energies, and at a scattering angle of 80/degree/. The experimental results were combined with lower-energy values previously obtained by this group to provide a comprehensive data base extending from near the inelastic-scattering threshold to 8 MeV. That data base was interpreted in terms of a coupled-channel model, including the inelastic excitation of one- and two-phonon vibrational levels of the even isotopes of palladium. It was concluded that the palladium inelastic-scattering cross section, at the low energies of interest in assessment of fast-fission-reactor performance, are large (∼50% greater than given in widely used evaluated fission-product data files). They primarily involve compound-nucleus processes, with only a small direct-reaction component attributable to the excitation of the one-phonon, 2 + , vibrational levels of the even isotopes of palladium. 24 refs., 6 figs

  17. Phase analyses of silicide or nitride coated U–Mo and U–Mo–Ti particle dispersion fuel after out-of-pile annealing

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Woo Jeong [Korea Atomic Energy Research Institute, 989-111 Daedeok-daero, Yuseong, Daejeon 305-353 (Korea, Republic of); Palancher, Hervé [CEA, DEN, DEC, F-13108 Saint Paul Lez Durance Cedex (France); Ryu, Ho Jin, E-mail: hojinryu@kaist.ac.kr [Korea Advanced Institute of Science and Technology, 291 Daehak-ro, Yuseong, Daejeon 305-701 (Korea, Republic of); Park, Jong Man; Nam, Ji Min [Korea Atomic Energy Research Institute, 989-111 Daedeok-daero, Yuseong, Daejeon 305-353 (Korea, Republic of); Bonnin, Anne [CEA, DEN, DEC, F-13108 Saint Paul Lez Durance Cedex (France); ESRF, 6, rue J. Horowitz, F-38000 Grenoble Cedex (France); Honkimäki, Veijo [ESRF, 6, rue J. Horowitz, F-38000 Grenoble Cedex (France); Charollais, François [CEA, DEN, DEC, F-13108 Saint Paul Lez Durance Cedex (France); Lemoine, Patrick [CEA, DEN, DISN, 91191 Gif sur Yvette (France)

    2014-03-15

    Highlights: • Silicide or nitride layers were coated on atomized U–Mo or U–Mo–Ti powder. • The constituent phases after annealing were identified through high-energy XRD. • U{sub 3}Si{sub 5} and U{sub 4}Mo(Mo{sub x}Si{sub 1−x})Si{sub 2} were identified in the silicide coating layers. • UN was identified for U–Mo particles and UN and U{sub 4}N{sub 7} formed on U–Mo–Ti particles. -- Abstract: The coating of silicide or nitride layers on U–7 wt%Mo or U–7 wt%Mo–1 wt%Ti particles has been proposed for the minimization of the interaction phase growth in U–Mo/Al dispersion fuel during irradiation. Out-of-pile annealing tests show reduced inter-diffusion by forming silicide or nitride protective layers on U–Mo and U–Mo–Ti particles. To characterize the constituent phases of the coated layers on U–Mo and U–Mo–Ti particles and the interaction phases of coated U–Mo and U–Mo–Ti particle dispersed Al matrix fuel, synchrotron X-ray diffraction experiments have been performed. It was identified that silicide coating layers consisted mainly of U{sub 3}Si{sub 5} and U{sub 4}Mo(Mo{sub x}Si{sub 1−x})Si{sub 2}, and nitride coating layers were composed of mainly UN and U{sub 4}N{sub 7}. The interaction phases obtained after annealing of coated U–Mo and U–Mo–Ti particle dispersion samples were identical to those found in U–Mo/Al–Si and U–Mo/Al systems. Nitride-coated particles showed less interaction formation than silicide-coated particles after annealing at 580 °C for 1 h owing to the higher susceptibility to breakage of the silicide coating layers during hot extrusion.

  18. Evidence for hydrogen-assisted recovery of cold-worked palladium: hydrogen solubility and mechanical properties studies

    Directory of Open Access Journals (Sweden)

    Maria Ferrer

    2017-07-01

    Full Text Available The influence of hydrogen as an agent to accelerate the thermal recovery of cold-worked palladium has been investigated. The techniques used to characterize the effects of hydrogen on the thermal recovery of palladium were hydrogen solubility and mechanical property measurements. Results show that the presence of modest amounts of hydrogen during annealing of cold-worked palladium does enhance the degree of thermal recovery, with a direct correlation between the amount of hydrogen during annealing and the degree of recovery. The results indicate that the damage resulting from cold-working palladium can be more effectively and efficiently reversed by suitable heat treatments in the presence of appropriate amounts of hydrogen, as compared to heat treatment in vacuum. The somewhat novel technique of using changes in the hydrogen solubility of palladium as an indicator of thermal recovery has been validated and complements the more traditional technique of mechanical property measurements.

  19. In situ synthesis of carbon nanotubes decorated with palladium nanoparticles using arc-discharge in solution method

    International Nuclear Information System (INIS)

    Bera, Debasis; Kuiry, Suresh C.; McCutchen, Matthew; Seal, Sudipta; Heinrich, Helge; Slane, Grady C.

    2004-01-01

    A unique, simple, inexpensive, and one-step synthesis route to produce carbon nanotubes (CNTs) decorated with palladium nanoparticles using a simplified dc arc-discharge in solution is reported. Zero-loss energy filtered transmission electron microscopy and scanning transmission electron microscopy confirm the presence of 3 nm palladium nanoparticles. Such palladium nanoparticles form during the reduction of palladium tetra-chloro-square-planar complex. The deconvoluted x-ray photoelectron spectroscopy envelope shows the presence of palladium on the decorated CNTs. The energy dispersive spectroscopy suggests no functionalization of atomic chlorine to the sidewall of the CNTs. The presence of dislodged graphene sheets with wavy morphology supports the formation of CNTs through the 'scroll mechanism'

  20. Thermal expansion and elastic moduli of the silicide based intermetallic alloys Ti5Si3(X) and Nb5Si3

    International Nuclear Information System (INIS)

    Zhang, L.; Wu, J.

    1997-01-01

    Silicides are among those potential candidates for high temperature application because of their high melting temperature, low density and good oxidation resistance. Recent interest is focused on molybdenum silicides and titanium silicides. Extensive investigation has been carried out on MoSi 2 , yet comparatively less work was performed on titanium silicides such as Ti 5 Si 3 and Ti 3 and TiSi 2 which are of lower density than MoSi 2 . Fundamental understanding of the titanium silicides' properties for further evaluation their potential for practical application are thus needed. The thermal expansion coefficients and elastic moduli of intermetallic compounds are two properties important for evaluation as a first step. The thermal expansion determines the possible stress that might arise during cooling for these high melting point compounds, which is crucial to the preparation of defect free specimens; and the elastic moduli are usually reflections of the cohesion in crystal. In Frommeyer's work and some works afterwards, the coefficients of thermal expansion were measured on both polycrystalline and single crystal Ti 5 Si 3 . The elastic modulus of polycrystalline Ti 5 Si 3 was measured by Frommeyer and Rosenkranz. However, in the above works, the referred Ti 5 Si 3 was the binary one, no alloying effect has been reported on this matter. Moreover, the above parameters (coefficient of thermal expansion and elastic modulus) of Nb 5 Si 3 remain unreported so far. In this paper, the authors try to extend the knowledge of alloyed Ti 5 Si 3 compounds with Nb and Cr additions. Results on the coefficients of thermal expansion and elastic moduli of Ti 5 Si 3 compounds and Nb 5 Si 3 are presented and the discussion is focused on the alloying effect

  1. Dislocation/hydrogen interaction mechanisms in hydrided nanocrystalline palladium films

    International Nuclear Information System (INIS)

    Amin-Ahmadi, Behnam; Connétable, Damien; Fivel, Marc; Tanguy, Döme; Delmelle, Renaud; Turner, Stuart; Malet, Loic; Godet, Stephane; Pardoen, Thomas; Proost, Joris; Schryvers, Dominique

    2016-01-01

    The nanoscale plasticity mechanisms activated during hydriding cycles in sputtered nanocrystalline Pd films have been investigated ex-situ using advanced transmission electron microscopy techniques. The internal stress developing within the films during hydriding has been monitored in-situ. Results showed that in Pd films hydrided to β-phase, local plasticity was mainly controlled by dislocation activity in spite of the small grain size. Changes of the grain size distribution and the crystallographic texture have not been observed. In contrast, significant microstructural changes were not observed in Pd films hydrided to α-phase. Moreover, the effect of hydrogen loading on the nature and density of dislocations has been investigated using aberration-corrected TEM. Surprisingly, a high density of shear type stacking faults has been observed after dehydriding, indicating a significant effect of hydrogen on the nucleation energy barriers of Shockley partial dislocations. Ab-initio calculations of the effect of hydrogen on the intrinsic stable and unstable stacking fault energies of palladium confirm the experimental observations.

  2. Palladium-catalysed electrophilic aromatic C-H fluorination

    Science.gov (United States)

    Yamamoto, Kumiko; Li, Jiakun; Garber, Jeffrey A. O.; Rolfes, Julian D.; Boursalian, Gregory B.; Borghs, Jannik C.; Genicot, Christophe; Jacq, Jérôme; van Gastel, Maurice; Neese, Frank; Ritter, Tobias

    2018-02-01

    Aryl fluorides are widely used in the pharmaceutical and agrochemical industries, and recent advances have enabled their synthesis through the conversion of various functional groups. However, there is a lack of general methods for direct aromatic carbon-hydrogen (C-H) fluorination. Conventional methods require the use of either strong fluorinating reagents, which are often unselective and difficult to handle, such as elemental fluorine, or less reactive reagents that attack only the most activated arenes, which reduces the substrate scope. A method for the direct fluorination of aromatic C-H bonds could facilitate access to fluorinated derivatives of functional molecules that would otherwise be difficult to produce. For example, drug candidates with improved properties, such as increased metabolic stability or better blood-brain-barrier penetration, may become available. Here we describe an approach to catalysis and the resulting development of an undirected, palladium-catalysed method for aromatic C-H fluorination using mild electrophilic fluorinating reagents. The reaction involves a mode of catalysis that is unusual in aromatic C-H functionalization because no organometallic intermediate is formed; instead, a reactive transition-metal-fluoride electrophile is generated catalytically for the fluorination of arenes that do not otherwise react with mild fluorinating reagents. The scope and functional-group tolerance of this reaction could provide access to functional fluorinated molecules in pharmaceutical and agrochemical development that would otherwise not be readily accessible.

  3. Synthesis, crystal structure and applications of palladium thiosalicylate complexes

    Directory of Open Access Journals (Sweden)

    S.B. Moosun

    2017-05-01

    Full Text Available Three palladium thiosalicylate complexes [Pd(tb(bipy]·3H2O (1, [Pd2(tb2(bipy2]·(dtdb2 (2 and [Pd2(tb2(phen2]·dtdb·H2O (3 (bipy = bipyridine; phen = phenanthroline were prepared from the reaction of PdCl2(CH3CN2 with dithiosalicylic acid (dtdb which underwent cleavage to form thiobenzoate anion (tb in DMF/MeOH. Square planar geometries of the complexes with a N2SO coordination type were proposed on the basis of single crystal X-ray structural study. The presence of trapped and uncoordinated dtdb was observed in complexes 2 and 3. Complexes 1–3 were evaluated as catalysts for Heck coupling reactions of methyl acrylate with iodobenzene, and showed moderate activities at a very low catalyst loading. Complex 1 was found to inhibit the growth of bacteria and scavenge free radicals efficiently.

  4. Biotemplated Palladium Catalysts Can Be Stabilized on Different Support Materials

    KAUST Repository

    Yates, Matthew D.; Logan, Bruce E.

    2014-01-01

    © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim. Sustainably biotemplated palladium catalysts generated on different carbon-based support materials are examined for durability under electrochemical (oxidative) and mechanical-stress conditions. Biotemplated catalysts on carbon paper under both stresses retain 95% (at 0.6V) of the initial catalytic activity as opposed to 70% for carbon cloth and 60% for graphite. Graphite electrodes retain 95% of initial catalytic activity under a single stress. Using electrodeposited polyaniline (PANI) and polydimethylsiloxane binder increases the current density after the stress tests by 22%, as opposed to a 30% decrease for Nafion. PANI-coated electrodes retain more activity than carbon-paper electrodes under elevated mechanical (94 versus 70%) or increased oxidative (175 versus 62%) stress. Biotemplated catalytic electrodes may be useful alternatives to synthetically produce catalysts for some electrochemical applications. Sustainable electrode fabrication: The biotemplated synthesis of catalytic porous electrodes is a sustainable process and, according to the results of durability tests under electrochemical and mechanical stress, these electrodes (e.g. the Pd/carbon paper electrode shown in the picture) are durable enough to replace catalytic electrodes based on synthetic materials in certain applications.

  5. Biotemplated Palladium Catalysts Can Be Stabilized on Different Support Materials

    KAUST Repository

    Yates, Matthew D.

    2014-07-30

    © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim. Sustainably biotemplated palladium catalysts generated on different carbon-based support materials are examined for durability under electrochemical (oxidative) and mechanical-stress conditions. Biotemplated catalysts on carbon paper under both stresses retain 95% (at 0.6V) of the initial catalytic activity as opposed to 70% for carbon cloth and 60% for graphite. Graphite electrodes retain 95% of initial catalytic activity under a single stress. Using electrodeposited polyaniline (PANI) and polydimethylsiloxane binder increases the current density after the stress tests by 22%, as opposed to a 30% decrease for Nafion. PANI-coated electrodes retain more activity than carbon-paper electrodes under elevated mechanical (94 versus 70%) or increased oxidative (175 versus 62%) stress. Biotemplated catalytic electrodes may be useful alternatives to synthetically produce catalysts for some electrochemical applications. Sustainable electrode fabrication: The biotemplated synthesis of catalytic porous electrodes is a sustainable process and, according to the results of durability tests under electrochemical and mechanical stress, these electrodes (e.g. the Pd/carbon paper electrode shown in the picture) are durable enough to replace catalytic electrodes based on synthetic materials in certain applications.

  6. Green Chemistry Approach for Synthesis of Effective Anticancer Palladium Nanoparticles.

    Science.gov (United States)

    Gurunathan, Sangiliyandi; Kim, EunSu; Han, Jae Woong; Park, Jung Hyun; Kim, Jin-Hoi

    2015-12-15

    The purpose of this study was to design and synthesize Palladium nanoparticles (PdNPs) using an environmentally friendly approach and evaluate the in vitro efficacy of PdNPs in human ovarian cancer A2780 cells. Ultraviolet-Visible (UV-Vis) spectroscopy was used to monitor the conversion of Pd(II) ions to Pd(0)NPs. X-ray diffraction (XRD) revealed the crystallinity of the as-synthesized PdNPs and Fourier transform infrared spectroscopy (FTIR) further confirmed the role of the leaf extract of Evolvulus alsinoides as a reducing and stabilizing agent for the synthesis of PdNPs. Dynamic light scattering (DLS) and transmission electron microscopy (TEM) showed that the average size of the NPs was 5 nm. After a 24-h exposure to PdNPs, cell viability and light microscopy assays revealed the dose-dependent toxicity of the PdNPs. Furthermore, the dose-dependent cytotoxicity of the PdNPs was confirmed by lactate dehydrogenase (LDH), increased reactive oxygen species (ROS) generation, activation of PdNPs-induced autophagy, impairment of mitochondrial membrane potential (MMP), enhanced caspase-3 activity, and detection of TUNEL-positive cells. Our study demonstrates a single, simple, dependable and green approach for the synthesis of PdNPs using leaf extracts of Evolvulus alsinoides. Furthermore, the in vitro efficacy of PdNPs in human ovarian cancer cells suggests that it could be an effective therapeutic agent for cancer therapy.

  7. Green Chemistry Approach for Synthesis of Effective Anticancer Palladium Nanoparticles

    Directory of Open Access Journals (Sweden)

    Sangiliyandi Gurunathan

    2015-12-01

    Full Text Available The purpose of this study was to design and synthesize Palladium nanoparticles (PdNPs using an environmentally friendly approach and evaluate the in vitro efficacy of PdNPs in human ovarian cancer A2780 cells. Ultraviolet-Visible (UV-Vis spectroscopy was used to monitor the conversion of Pd(II ions to Pd(0NPs. X-ray diffraction (XRD revealed the crystallinity of the as-synthesized PdNPs and Fourier transform infrared spectroscopy (FTIR further confirmed the role of the leaf extract of Evolvulus alsinoides as a reducing and stabilizing agent for the synthesis of PdNPs. Dynamic light scattering (DLS and transmission electron microscopy (TEM showed that the average size of the NPs was 5 nm. After a 24-h exposure to PdNPs, cell viability and light microscopy assays revealed the dose-dependent toxicity of the PdNPs. Furthermore, the dose-dependent cytotoxicity of the PdNPs was confirmed by lactate dehydrogenase (LDH, increased reactive oxygen species (ROS generation, activation of PdNPs-induced autophagy, impairment of mitochondrial membrane potential (MMP, enhanced caspase-3 activity, and detection of TUNEL-positive cells. Our study demonstrates a single, simple, dependable and green approach for the synthesis of PdNPs using leaf extracts of Evolvulus alsinoides. Furthermore, the in vitro efficacy of PdNPs in human ovarian cancer cells suggests that it could be an effective therapeutic agent for cancer therapy.

  8. Catalytic hydrolysis of ammonia borane via cobalt palladium nanoparticles.

    Science.gov (United States)

    Sun, Daohua; Mazumder, Vismadeb; Metin, Önder; Sun, Shouheng

    2011-08-23

    Monodisperse 8 nm CoPd nanoparticles (NPs) with controlled compositions were synthesized by the reduction of cobalt acetylacetonate and palladium bromide in the presence of oleylamine and trioctylphosphine. These NPs were active catalysts for hydrogen generation from the hydrolysis of ammonia borane (AB), and their activities were composition dependent. Among the 8 nm CoPd catalysts tested for the hydrolysis of AB, the Co(35)Pd(65) NPs exhibited the highest catalytic activity and durability. Their hydrolysis completion time and activation energy were 5.5 min and 27.5 kJ mol(-1), respectively, which were comparable to the best Pt-based catalyst reported. The catalytic performance of the CoPd/C could be further enhanced by a preannealing treatment at 300 °C under air for 15 h with the hydrolysis completion time reduced to 3.5 min. This high catalytic performance of Co(35)Pd(65) NP catalyst makes it an exciting alternative in pursuit of practical implementation of AB as a hydrogen storage material for fuel cell applications. © 2011 American Chemical Society

  9. Palladium-catalysed anti-Markovnikov selective oxidative amination

    Science.gov (United States)

    Kohler, Daniel G.; Gockel, Samuel N.; Kennemur, Jennifer L.; Waller, Peter J.; Hull, Kami L.

    2018-03-01

    In recent years, the synthesis of amines and other nitrogen-containing motifs has been a major area of research in organic chemistry because they are widely represented in biologically active molecules. Current strategies rely on a multistep approach and require one reactant to be activated prior to the carbon-nitrogen bond formation. This leads to a reaction inefficiency and functional group intolerance. As such, a general approach to the synthesis of nitrogen-containing compounds from readily available and benign starting materials is highly desirable. Here we present a palladium-catalysed oxidative amination reaction in which the addition of the nitrogen occurs at the less-substituted carbon of a double bond, in what is known as anti-Markovnikov selectivity. Alkenes are shown to react with imides in the presence of a palladate catalyst to generate the terminal imide through trans-aminopalladation. Subsequently, olefin isomerization occurs to afford the thermodynamically favoured products. Both the scope of the transformation and mechanistic investigations are reported.

  10. Determination of palladium in various samples by atomic absorption spectrometry after preconcentration with dimethylglyoxime on silica gel

    International Nuclear Information System (INIS)

    Tokalioglu, Serife; Oymak, Tuelay; Kartal, Senol

    2004-01-01

    A preconcentration method based on the adsorption of palladium-dimethylglyoxime (DMG) complex on silica gel for the determination of palladium at trace levels by atomic absorption spectrometry (AAS) has been developed. The retained palladium as Pd(DMG) 2 complex was eluted with 1 mol l -1 HCl in acetone. The effect of some analytical parameters such as pH, amount of reagent and the sample volume on the recovery of palladium was examined in synthetic solutions containing street dust matrix. The influence of some matrix ions on the recovery of palladium was investigated by using the developed method when the elements were present both individually and together. The results showed that 2500 μg ml -1 Na + , K + , Mg 2+ , Al 3+ and Fe 3+ ; 5000 μg ml -1 Ca 2+ ; 500 μg ml -1 Pb 2+ ; 125 μg ml -1 Zn 2+ ; 50 μg ml -1 Cu 2+ and 25 μg ml -1 Ni 2+ did not interfere with the palladium signal. At the optimum conditions determined experimentally, the recovery for palladium was found to be 95.3±1.2% at the 95% confidence level. The relative standard deviation and limit of detection (3s/b) of the method were found to be 1.7% and 1.2 μg l -1 , respectively. In order to determine the adsorption behaviour of silica gel, the adsorption isotherm of palladium was studied and the binding equilibrium constant and adsorption capacity were calculated to be 0.38 l mg -1 and 4.06 mg g -1 , respectively. The determination of palladium in various samples was performed by using both flame AAS and graphite furnace AAS. The proposed method was successfully applied for the determination of palladium in the street dust, anode slime, rock and catalytic converter samples

  11. Investigation of high temperature reactions on solid substrates with Rutherford backscattering spectrometry: interaction of palladium with selenium on heated graphite surfaces

    International Nuclear Information System (INIS)

    Majidi, V.; Robertson, J.D.

    1991-01-01

    Selenium and palladium interactions on heated pyrolytically coated graphite substrates were investigated using Rutherford backscattering spectrometry. The studies were performed using selenium alone, palladium alone, and a combination of selenium and palladium deposited on the graphite substrates. The results indicate that palladium instantaneously stabilizes selenium at ambient temperatures and prevents the diffusion of selenium into the graphite. As the substrate is heated, temperature dependent diffusion of all analytes into the graphite is observed. Furthermore, it appears that the stabilization of selenium is due to the formation of a stoichiometric compound with palladium and oxygen. This compound decomposes at a temperature between 1070 and 1770 K. (author)

  12. Investigation of high temperature reactions on solid substrates with Rutherford backscattering spectrometry: interaction of palladium with selenium on heated graphite surfaces

    Energy Technology Data Exchange (ETDEWEB)

    Majidi, V.; Robertson, J.D. (Kentucky Univ., Lexington, KY (United States). Dept. of Chemistry)

    1991-01-01

    Selenium and palladium interactions on heated pyrolytically coated graphite substrates were investigated using Rutherford backscattering spectrometry. The studies were performed using selenium alone, palladium alone, and a combination of selenium and palladium deposited on the graphite substrates. The results indicate that palladium instantaneously stabilizes selenium at ambient temperatures and prevents the diffusion of selenium into the graphite. As the substrate is heated, temperature dependent diffusion of all analytes into the graphite is observed. Furthermore, it appears that the stabilization of selenium is due to the formation of a stoichiometric compound with palladium and oxygen. This compound decomposes at a temperature between 1070 and 1770 K. (author).

  13. Effects of (Al,Ge) double doping on the thermoelectric properties of higher manganese silicides

    Energy Technology Data Exchange (ETDEWEB)

    Chen, Xi; Salta, Daniel; Zhang, Libin [Materials Science and Engineering Program, Texas Materials Institute, The University of Texas at Austin, Austin, Texas 78712 (United States); Weathers, Annie [Department of Mechanical Engineering, The University of Texas at Austin, Austin, Texas 78712 (United States); Zhou, Jianshi; Goodenough, John B.; Shi, Li [Materials Science and Engineering Program, Texas Materials Institute, The University of Texas at Austin, Austin, Texas 78712 (United States); Department of Mechanical Engineering, The University of Texas at Austin, Austin, Texas 78712 (United States)

    2013-11-07

    Experiments and analysis have been carried out to investigate the effects of Al and (Al,Ge) doping on the microstructure and thermoelectric properties of polycrystalline higher manganese silicide (HMS) samples, which were prepared by solid-state reaction, ball milling, and followed by spark plasma sintering. It has been found that Al doping effectively increases the hole concentration, which leads to an increase in the electrical conductivity and power factor. By introducing the second dopant Ge into Al-doped HMS, the electrical conductivity is increased, and the Seebeck coefficient is decreased as a result of further increased hole concentration. The peak power factor is found to occur at a hole concentration between 1.8 × 10{sup 21} and 2.2 × 10{sup 21} cm{sup −3} measured at room temperature. The (Al,Ge)-doped HMS samples show lower power factors owing to their higher hole concentrations. The mobility of Mn(Al{sub 0.0035}Ge{sub y}Si{sub 0.9965-y}){sub 1.8} with y = 0.035 varies approximately as T{sup −3/2} above 200 K, suggesting acoustic phonon scattering is the dominant scattering mechanism. The thermal conductivity of HMS does not change appreciably by Al or (Al,Ge) doping. The maximum ZT of (Al,Ge)-doped HMS is 0.57 at 823 K, which is similar to the highest value found in the Al-doped HMS samples. The ZT values were reduced in the Mn(Al{sub 0.0035}Ge{sub y}Si{sub 0.9965-y}){sub 1.8} samples with high Ge concentration of y = 0.025 and 0.035, because of reduced power factor. In addition, a two-band model was employed to show that the hole contribution to the thermal conductivity dominates the bipolar and electron contributions for all samples from 300 to 823 K and accounts for about 12% of the total thermal conductivity at about 800 K.

  14. Effects of (Al,Ge) double doping on the thermoelectric properties of higher manganese silicides

    International Nuclear Information System (INIS)

    Chen, Xi; Salta, Daniel; Zhang, Libin; Weathers, Annie; Zhou, Jianshi; Goodenough, John B.; Shi, Li

    2013-01-01

    Experiments and analysis have been carried out to investigate the effects of Al and (Al,Ge) doping on the microstructure and thermoelectric properties of polycrystalline higher manganese silicide (HMS) samples, which were prepared by solid-state reaction, ball milling, and followed by spark plasma sintering. It has been found that Al doping effectively increases the hole concentration, which leads to an increase in the electrical conductivity and power factor. By introducing the second dopant Ge into Al-doped HMS, the electrical conductivity is increased, and the Seebeck coefficient is decreased as a result of further increased hole concentration. The peak power factor is found to occur at a hole concentration between 1.8 × 10 21 and 2.2 × 10 21  cm −3 measured at room temperature. The (Al,Ge)-doped HMS samples show lower power factors owing to their higher hole concentrations. The mobility of Mn(Al 0.0035 Ge y Si 0.9965-y ) 1.8 with y = 0.035 varies approximately as T −3/2 above 200 K, suggesting acoustic phonon scattering is the dominant scattering mechanism. The thermal conductivity of HMS does not change appreciably by Al or (Al,Ge) doping. The maximum ZT of (Al,Ge)-doped HMS is 0.57 at 823 K, which is similar to the highest value found in the Al-doped HMS samples. The ZT values were reduced in the Mn(Al 0.0035 Ge y Si 0.9965-y ) 1.8 samples with high Ge concentration of y = 0.025 and 0.035, because of reduced power factor. In addition, a two-band model was employed to show that the hole contribution to the thermal conductivity dominates the bipolar and electron contributions for all samples from 300 to 823 K and accounts for about 12% of the total thermal conductivity at about 800 K

  15. Nanostructured palladium tailored via carbonyl chemical route towards oxygen reduction reaction

    International Nuclear Information System (INIS)

    Luo, Y.; Mora-Hernández, J.M.; Estudillo-Wong, L.A.; Arce-Estrada, E.M.; Alonso-Vante, N.

    2015-01-01

    Graphical Abstract: Mass-depending morphologies of nanostructured Palladium obtained via the carbonyl chemical route. Display Omitted -- Highlights: •Mass-depending morphology was observed in nanostructured palladium supported on carbon prepared by the carbonyl chemical route. •The Morphological effect of carbon supported Pd was investigated towards ORR. -- Abstract: Carbon supported palladium nanostructures were synthesized via the carbonyl chemical route. Compared with nanostructured platinum, prepared via carbonyl chemical route, Pd nanomaterials showed mass-loading morphology, whereas particle size and morphology of Pt nanostructures was constant. The oxygen reduction reaction (ORR) on nanostructured Pd, with different morphology in both acid and alkaline medium was investigated. A relationship, based on X-ray diffraction structural analysis pattern, transmission electron microscope, with the Pd morphological effect on ORR activity was identified

  16. γ-Diimine palladium(II based complexes mediated polymerization of methyl methacrylate

    Directory of Open Access Journals (Sweden)

    Mahmoud Sunjuk

    2017-02-01

    Full Text Available The synthesis of new palladium(II complexes of the type [Pd(A–NC–ph–CN–ACl2] (4a–e (A = cyclohexyl (a, 2-isoprpropyl (b, pyrenyl (c, naphthyl (d, and 2,6-diisopropyl (e is described. The isolated γ-diimine ligands and their corresponding palladium(II complexes were characterized by their physical properties, elemental analysis, 1H NMR-, 13C NMR, and infrared spectroscopy. The palladium(II complexes (4a–e were employed successfully as catalysts for atom transfer radical polymerization (ATRP of methyl methacrylate (MMA in the presence of ethyl-2-bromoisobutyrate (EBIB as initiator at 90 °C. Polymerization with these catalyst systems afforded polymers with low molecular weight distribution (Mw/Mn and syndio-rich atactic poly (MMA with relatively higher [rr] diads.

  17. Study on a multi-component palladium alloy membrane for the fusion fuel cycle

    International Nuclear Information System (INIS)

    Yoshida, Hiroshi; Okuno, Kenji; Nagasaki, Takanori; Noda, Kenji; Ishii, Yoshinobu; Takeshita, Hidefumi.

    1985-11-01

    A feasibility study on the material integrity with respect to the hydride formation and helium damage of the palladium alloy membrane was performed for an application of the palladium diffuser to a fusion fuel cleanup process. This study was conducted under the Japan/US Fusion Cooperation Program. Experimental works on the crystallography, hydrogen solubility and 3 He release characteristics were carried out with a multi-component palladium alloy(Pd-25Ag.Au.Ru). The excellent hydrogen permeability and mechanical properties of the membrane made of this alloy had been confirmed by authors' previous study. Based on the present study, this alloy membrane has high resistivity to the hydrogen embrittlement, and swelling and fracture due to the helium bubble formation under the practical operating conditions of the diffuser. (author)

  18. A dataset for preparing pristine graphene-palladium nanocomposites using swollen liquid crystal templates

    Science.gov (United States)

    Vats, Tripti; Siril, Prem Felix

    2017-12-01

    Pristine graphene (G) has not received much attention as a catalyst support, presumably due to its relative inertness as compared to reduced graphene oxide (RGO). In the present work, we used swollen liquid crystals (SLCs) as nano-reactors for graphene-palladium nanocomposites synthesis. The 'soft' confinement of SLCs directs the growth of palladium (Pd) nanoparticles over the G sheets. In this dataset we include all the parameters and details of different techniques used for the characterization of G, SLCs and synthesized G-Pd nanocomposites. The synthesized G-palladium nanocomposites (Pd-G) exhibited improved catalytic activity compared with Pd-RGO and Pd nanoparticles, in the hydrogenation of nitrophenols and C-C coupling reactions.

  19. Preparation of Palladium/Silver-Coated Polyimide Nanotubes: Flexible, Electrically Conductive Fibers.

    Science.gov (United States)

    Kong, Lushi; Rui, Guanchun; Wang, Guangyu; Huang, Rundong; Li, Ran; Yu, Jiajie; Qi, Shengli; Wu, Dezhen

    2017-11-02

    A simple and practical method for coating palladium/silver nanoparticles on polyimide (PI) nanotubes is developed. The key steps involved in the process are silver ion exchange/reduction and displacement reactions between silver and palladium ions. With the addition of silver, the conductivity of the PI nanotubes is greatly enhanced. Further, the polyimide nanotubes with a dense, homogeneous coating of palladium nanoparticles remain flexible after heat treatment and show the possibility for use as highly efficient catalysts. The approach developed here is applicable for coating various noble metals on a wide range of polymer matrices, and can be used for obtaining polyimide nanotubes with metal loaded on both the inner and outer surface.

  20. Preparation of Palladium/Silver-Coated Polyimide Nanotubes: Flexible, Electrically Conductive Fibers

    Directory of Open Access Journals (Sweden)

    Lushi Kong

    2017-11-01

    Full Text Available A simple and practical method for coating palladium/silver nanoparticles on polyimide (PI nanotubes is developed. The key steps involved in the process are silver ion exchange/reduction and displacement reactions between silver and palladium ions. With the addition of silver, the conductivity of the PI nanotubes is greatly enhanced. Further, the polyimide nanotubes with a dense, homogeneous coating of palladium nanoparticles remain flexible after heat treatment and show the possibility for use as highly efficient catalysts. The approach developed here is applicable for coating various noble metals on a wide range of polymer matrices, and can be used for obtaining polyimide nanotubes with metal loaded on both the inner and outer surface.

  1. Low Temperature Steam Methane Reforming Over Ni Based Catalytic Membrane Prepared by Electroless Palladium Plating.

    Science.gov (United States)

    Lee, Sang Moon; Hong, Sung Chang; Kim, Sung Su

    2018-09-01

    A Pd/Ni-YSZ porous membrane with different palladium loadings and hydrazine as a reducing reagent was prepared by electroless plating and evaluated for the steam methane reforming activity. The steam-reforming activity of a Ni-YSZ porous membrane was greatly increased by the deposition of 4 g/L palladium in the low-temperature range (600 °C). With an increasing amount of reducing reagent, the Pd clusters were well dispersed on the Ni-YSZ surface and were uniform in size (∼500 nm). The Pd/Ni-YSZ catalytic porous membrane prepared by 1 of Pd/hydrazine ratio possessed an abundant amount of metallic Pd. The optimal palladium loadings and Pd/hydrazine ratio increased the catalytic activity in both the steam-reforming reaction and the Pd dispersion.

  2. Shaping surface of palladium nanospheres through the control of reaction parameters

    International Nuclear Information System (INIS)

    Wang Lianmeng; Tan Enzhong; Guo Lin; Wang Lihua; Han Xiaodong

    2011-01-01

    Solid, cracked, and flower-shaped surfaces of palladium nanospheres with high yields and good uniformity were successfully prepared by a wet chemical method. On the basis of the experimental data, the same size of palladium nanosphere with different surface morphologies can be regulated only by changing the amount of ammonium hydroxide and reductant in one experimental system. The as-prepared products were studied by transmission electron microscopy (TEM), scanning electron microscopy (SEM) and x-ray diffraction (XRD). In addition, surface-enhanced Raman scattering (SERS) spectra on the as-prepared different surface of palladium nanospheres exhibit high activity towards p-aminothiophenol (PATP) detection, and the result further reveals that the predominance of the a1 vibration mode in the SERS spectra via an electromagnetic (EM) mechanism is significant.

  3. Recovery of nonradioactive palladium and rhodium from high-level radioactive wastes

    International Nuclear Information System (INIS)

    McDuffie, H.F.

    1979-01-01

    A possible method for recovering significant quantities of nonradioactive palladium from fission-product wastes requires essentially complete separation of the fission-product (radioactive) palladium from fission-product ruthenium. After the decay of 106 Ru via 106 Rh to 106 Pd, this nonradioactive palladium is recovered for normal commercial use. The U.S. production of palladium has never been above 1000 kg per year vs consumption of about 46,000 kg per year. Most of the supply comes from Russia and South Africa. It has been estimated that a 400-GW(e) nuclear reactor economy will make available 2000 kg per year of 106 Ru at reactor fuel discharge. A substantial increase might be achieved if plutonium were recycled as fissionable material because of the higher yields of the 106 chain from plutonium. A literature search has uncovered support for three promising approaches to the required separation of palladium from ruthenium: (1) recrystallization from solution in bismuth or in zinc; (2) selective precipitation of a titanium--ruthenium intermetallic compound from bismuth, followed by precipitation of a zinc--palladium intermetallic compound; and (3) dissolution in molten magnesium followed by partitioning between molten magnesium and a molten uranium-5 wt % chromium eutectic at a temperature above 870 0 C. Liquid-liquid extraction appears to be the most promising method from a technological point of view, although intermetallic compound formation is much more interesting chemically. Recovery of some nonradioactive 103 Rh may be possible by liquid-liquid extraction of the fuel before the decay of the 39.8-d 103 Ru has gone substantially to completion. Demonstration of the practicality of these separations will contribute a positive factor to the evaluation of resumption in the United States of nuclear fuel reprocessing and plutonium recycle in light-water-moderated reactors

  4. Morphology of one-time coated palladium-alumina composite membrane prepared by sol-gel process and electroless plating technique

    Science.gov (United States)

    Sari, R.; Dewi, R.; Pardi; Hakim, L.; Diana, S.

    2018-03-01

    Palladium coated porous alumina ceramic membrane tube was obtained using a combination of sol-gel process and electroless plating technique. The thickness, structure and composition of palladium-alumina composite membrane were analyzed by transmission electron microscopy (TEM), scanning electron microscopy (SEM), energy-dispersive X-ray (EDX), and atomic force microscopy (AFM). Palladium particle size was 6.18 to 7.64 nm. Palladium membrane with thickness of approximately 301.5 to 815.1 nm was formed at the outer surface of the alumina layer. EDX data confirmed the formation of palladium-alumina membrane containing 45% of palladium. From this research it shows the combination of sol-gel process and electroless plating technique with one-time coating can produce a homogeneous and smoother palladium nano layer film on alumina substrate.

  5. Method for palladium activating molybdenum metallized features on a ceramic substrate

    International Nuclear Information System (INIS)

    Kumar, A.H.; Schwartz, B.

    1985-01-01

    A molybdenum or tungsten metallurgical pattern is formed on or in a dielectric green sheet. Palladium, nickel, platinum or rhodium is coated on a layer of polyvinyl butyral which is carried on a polyester film. The metal layer of this assembly is laminated to a dielectric green sheet which carries the molybdenum or tungsten metallurgy. The polyester film is stripped off. The resulting assembly is sintered to a fired structure, whereby the polyvinyl butyral is volatilized off and the palladium, nickel, platinum or rhodium is alloyed with the molybdenum or tungsten metallurgy to provide a densified metallurgy whose surface is free of glass

  6. Fabrication of Polybenzimidazole/Palladium Nanoparticles Hollow Fiber Membranes for Hydrogen Purification

    KAUST Repository

    Villalobos, Luis Francisco

    2017-09-13

    A novel scheme to fabricate polybenzimidazole (PBI) hollow fiber membranes with a thin skin loaded with fully dispersed palladium nanoparticles is proposed for the first time. Palladium is added to the membrane during the spinning process in the form of ions that coordinate to the imidazole groups of the polymer. This is attractive for membrane production because agglomeration of nanoparticles is minimized and the high-cost metal is incorporated in only the selective layer—where it is required. Pd-containing membranes achieve three orders of magnitude higher H2 permeances and a twofold improvement in H2/CO2 selectivity compared to pure PBI hollow fiber membranes.

  7. Palladium-catalysed arylation of acetoacetate esters to yield 2-arylacetic acid esters

    CSIR Research Space (South Africa)

    Zeevaart, JG

    2004-05-24

    Full Text Available , was developed simultaneously by Hart- wig and Buchwald.5 Typically the tert-butyl ester of propionic acid is treated with an aryl halide (bromide or chloride) in the presence of a strong base, palladium and a bulky phosphine ligand or a bulky imidazolinium CO2t... novel palladium- catalysed conditions for the arylation of acetoacetate esters resulting in the formation of 2-arylacetic acid esters. When we attempted the arylation of tert-butyl aceto- acetate 1a with bromobenzene 2a using mild reaction conditions (K3...

  8. Neutron activation determination of gold and palladium using extraction by organic sulfides

    International Nuclear Information System (INIS)

    Gil'berg, Eh.N.; Torgov, V.G.; Verevkin, G.V.; AN SSSR, Novosibirsk. Inst. Neorganicheskoj Khimii)

    1978-01-01

    Compared are methods of gold determination in standard rock samples of the USA National Geological Service: a) extraction by solutions of dioctylsulfide and oil sulfides from irradiated samples; b) preliminary extraction by the above solfides with the following extract radiation; c) the method of isotope dilution with substoichiometry extraction. A possibility is studied to determine palladium in the sulfide extract with gold using the NaI(Tl) thin crystal scintillators. It is established that joint palladium and gold extraction permits to determine them in many natural products simultaneously

  9. Watermelon rind-mediated green synthesis of noble palladium nanoparticles: catalytic application

    Science.gov (United States)

    Lakshmipathy, R.; Palakshi Reddy, B.; Sarada, N. C.; Chidambaram, K.; Khadeer Pasha, Sk.

    2015-02-01

    The present study reports the feasibility of synthesis of palladium nanoparticles (Pd NPs) by watermelon rind. The aqueous extract prepared from watermelon rind, an agro waste, was evaluated as capping and reducing agent for biosynthesis of palladium nanoparticles. The formation of Pd NPs was visually monitored with change in color from pale yellow to dark brown and later monitored with UV-Vis spectroscopy. The synthesized Pd NPs were further characterized by XRD, FTIR, DLS, AFM and TEM techniques. The synthesized Pd NPs were employed in Suzuki coupling reaction as catalyst. The results reveal that watermelon rind, an agro waste, is capable of synthesizing spherical-shaped Pd NPs with catalytic activity.

  10. Efficiency of Al2O3 supported palladium sorbents in the process of hydrogen isotope exchange

    International Nuclear Information System (INIS)

    Andreev, B.M.; Perevezentsev, A.N.; Yasenkov, V.I.

    1981-01-01

    It is found that in the hydrogen-palladium system while applying the metal to aluminium oxide a considerable increase of the heterogeneous hydrogen isotopic exchange rate is observed due to the increase of its specific surface at 167-298 K temperatures and 350-500 Torr hydrogen pressures. It is shown that in the process of thermal treatment of the supported palladium sorbent resulting in reconstruction of the carrier porous structure, as well as in increasing the metal crystal size, the change of the stage, limiting the isotopic exchange process, occurs. The values of the rate and energy of activation of the hydrogen isotopic exchange are presented [ru

  11. Insights into functional-group-tolerant polymerization catalysis with phosphine-sulfonamide palladium (II) complexes

    KAUST Repository

    Jian, Zhongbao; Falivene, Laura; Wucher, Philipp; Roesle, Philipp; Caporaso, Lucia; Cavallo, Luigi; Gç ttker-Schnetmann, Inigo; Mecking, Stefan

    2014-01-01

    Two series of cationic palladium(II) methyl complexes {[(2-MeOC6H4)2PC6H4SO2NHC6H3(2,6-R1,R2)]PdMe}2[A]2 (X1+-A: R1=R2=H: H1+-A; R1=R2=CH(CH3)2: DIPP1+-A; R1=H, R2=CF3: CF31+-A; A=BF4 or SbF6) and neutral palladium(II) methyl complexes {[(2-MeOC6H4

  12. Progress in excess of power experiments with electrochemical loading of deuterium in palladium

    International Nuclear Information System (INIS)

    Violante, V.; Moretti, S.; Bertolotti, M.

    2006-01-01

    A research activity has been carried out, during the last 3 years, in the field of triggering anomalous heat effects in palladium deuteride. An enhancement of the excess of power reproducibility in deuterated palladium was obtained by using He-Ne Laser irradiation during electrochemical loading. A preliminary correlation between excess of energy and 4 He concentration increasing above the background was found. The continuation of the experimental program confirmed that Laser triggering produce an interesting gain of reproducibility. An upgrade of the experimental set-up has been realized. (author)

  13. Construction of a four tip scanning tunneling microscope/scanning electron microscope combination and conductivity measurements of silicide nanowires

    International Nuclear Information System (INIS)

    Zubkov, Evgeniy

    2013-01-01

    In this work the combination of a four-tip scanning tunneling microscope with a scanning electron microscope is presented. By means of this apparatus it is possible to perform the conductivity measurements on the in-situ prepared nanostructures in ultra-high vacuum. With the aid of a scanning electron microscope (SEM), it becomes possible to position the tunneling tips of the four-tip scanning tunneling microscope (STM), so that an arrangement for a four-point probe measurement on nanostructures can be obtained. The STM head was built according to the novel coaxial Beetle concept. This concept allows on the one hand, a very compact arrangement of the components of the STM and on the other hand, the new-built STM head has a good mechanical stability, in order to achieve atomic resolution with all four STM units. The atomic resolution of the STM units was confirmed by scanning a Si(111)-7 x 7 surface. The thermal drift during the STM operation, as well as the resonant frequencies of the mechanical structure of the STM head, were determined. The scanning electron microscope allows the precise and safe navigation of the tunneling tips on the sample surface. Multi tip spectroscopy with up to four STM units can be performed synchronously. To demonstrate the capabilities of the new-built apparatus the conductivity measurements were carried out on metallic yttrium silicide nanowires. The nanowires were prepared by the in-situ deposition of yttrium on a heated Si(110) sample surface. Current-voltage curves were recorded on the nanowires and on the wetting layer in-between. The curves indicate an existence of the Schottky barrier between the yttrium silicide nanowires and the silicon bulk. By means of the two-tip measurements with a gate, the insulating property of the Schottky barrier has been confirmed. Using this Schottky barrier, it is possible to limit the current to the nanowire and to prevent it from flowing through the silicon bulk. A four-tip resistance measurement

  14. Study on the determination of palladium in biological samples by the method of neutron activation analysis

    International Nuclear Information System (INIS)

    Cavalcante, Cassio Queiroz

    2007-01-01

    Palladium is one of platinum group elements present in the nature at very low concentrations. However with the use of this element in the automobile catalyzers Pd became a new pollutant. Besides, Pd has been studied in the preparation of new antitumour drugs. Consequently, there is a need to determine Pd concentrations in biological and environmental samples. This study presents palladium results obtained in the analysis of biological samples and reference materials using instrumental thermal and epithermal neutron activation analysis (INAA and ENAA). The solvent extraction and solid phase extraction separation methods were also applied before ENAA. The samples analyzed in this study were, reference material BCR 723 - Palladium, Platinum and Rhodium in road dust, CCQM-P63 automotive catalyst material of the Proficiency Test and bovine tissue samples containing palladium prepared in the laboratory. Samples and palladium synthetic standard were irradiated at the IEA-R1 nuclear research reactor under thermal neutron flux of about 4 x 10 12 n cm-2 s-1, during a period of 4 and 16 h for INAA and ENAA, respectively. The induced gamma activity of 109 Pd to the sample and standard was measured using a hyper pure Ge detector coupled to a gamma ray spectrometer. The palladium concentration was calculated by comparative method. The gamma ray energy of 109 Pd radioisotope measured was of 88.0 keV, located in a spectrum region of low energy where occurs the interference of X rays, 'Bremsstrahlung' radiations, as well as Compton effect of 24 Na. The pre-separation of palladium from interfering elements by solvent extraction was performed using dimethylglyoxime complexant and chloroform as diluent. In the case of the pre separation procedure using solid reversed phase column, the palladium was retained using N,N-diethyl-N'-benzoyl thiourea complexant and eluted using ethanol. Aliquots of the resulting solutions from the pre-separations, free of interfering elements, were

  15. Sol-gel synthesized of nanocomposite palladium-alumina ceramic membrane for H{sub 2} permeability: Preparation and characterization

    Energy Technology Data Exchange (ETDEWEB)

    Ahmad, A.L.; Mustafa, N.N.N. [School of Chemical Engineering, Engineering Campus, Universiti Sains Malaysia, Seri Ampangan, 14300 Nibong Tebal, Penang (Malaysia)

    2007-08-15

    Palladium-alumina membrane with mesopore and narrow pore size distribution was prepared by the sol-gel method. Effect of the finely dispersed metal on the microstructure and the characteristic properties of the palladium-alumina membrane were investigated. Observations were made on membrane weight loss, morphology, pore structure, pore size, surface area, pore surface fractal and membrane's crystal structure. Autosorb analysis, X-ray Diffraction (XRD), Scanning Electron Microscopy (SEM) and Fourier Transform Infrared (FTIR) analysis were employed in the membrane characterization. Autosorb analysis found that, BET surface area decreased and pore size of the membrane increased with the increasing of calcinations temperature (500-1100{sup o}C) and with the increasing of palladium amount in the membrane. FTIR and TG/DTA analysis show that the suitable temperature for calcinations of palladium-alumina membrane is at 700{sup o}C. Palladium metals are highly dispersed at calcinations temperature of 700{sup o}C as observed by TEM analysis. The fine crystallinity of the palladium and {gamma}-alumina phase was obtained after calcined at 700{sup o}C. The SEM morphology shows a smooth and free crack layer of palladium-alumina membrane after repeating the process of dipping, drying and calcinations at temperature of 700{sup o}C. The membrane also successfully coated with a good adhesion on support. The thickness of the final membrane layer was estimated as 9{mu} m. (author)

  16. Accelerating Palladium Nanowire H2 Sensors Using Engineered Nanofiltration.

    Science.gov (United States)

    Koo, Won-Tae; Qiao, Shaopeng; Ogata, Alana F; Jha, Gaurav; Jang, Ji-Soo; Chen, Vivian T; Kim, Il-Doo; Penner, Reginald M

    2017-09-26

    The oxygen, O 2 , in air interferes with the detection of H 2 by palladium (Pd)-based H 2 sensors, including Pd nanowires (NWs), depressing the sensitivity and retarding the response/recovery speed in air-relative to N 2 or Ar. Here, we describe the preparation of H 2 sensors in which a nanofiltration layer consisting of a Zn metal-organic framework (MOF) is assembled onto Pd NWs. Polyhedron particles of Zn-based zeolite imidazole framework (ZIF-8) were synthesized on lithographically patterned Pd NWs, leading to the creation of ZIF-8/Pd NW bilayered H 2 sensors. The ZIF-8 filter has many micropores (0.34 nm for gas diffusion) which allows for the predominant penetration of hydrogen molecules with a kinetic diameter of 0.289 nm, whereas relatively larger gas molecules including oxygen (0.345 nm) and nitrogen (0.364 nm) in air are effectively screened, resulting in superior hydrogen sensing properties. Very importantly, the Pd NWs filtered by ZIF-8 membrane (Pd NWs@ZIF-8) reduced the H 2 response amplitude slightly (ΔR/R 0 = 3.5% to 1% of H 2 versus 5.9% for Pd NWs) and showed 20-fold faster recovery (7 s to 1% of H 2 ) and response (10 s to 1% of H 2 ) speed compared to that of pristine Pd NWs (164 s for response and 229 s for recovery to 1% of H 2 ). These outstanding results, which are mainly attributed to the molecular sieving and acceleration effect of ZIF-8 covered on Pd NWs, rank highest in H 2 sensing speed among room-temperature Pd-based H 2 sensors.

  17. Enhancing the performance of single-chambered microbial fuel cell using manganese/palladium and zirconium/palladium composite cathode catalysts.

    Science.gov (United States)

    Jadhav, Dipak A; Deshpande, Parag A; Ghangrekar, Makarand M

    2017-08-01

    Application of ZrO 2 , MnO 2 , palladium, palladium-substituted-zirconium oxide (Zr 0.98 Pd 0.02 O 2 ) and palladium-substituted-manganese oxide (Mn 0.98 Pd 0.02 O 2 ) cathode catalysts in a single-chambered microbial fuel cell (MFC) was explored. The highest power generation (1.28W/m 3 ) was achieved in MFC with Mn 0.98 Pd 0.02 O 2 catalyst, which was higher than that with MnO 2 (0.58W/m 3 ) alone; whereas, MFC having Zr 0.98 Pd 0.02 O 2 catalyzed cathode and non-catalyzed cathode produced powers of 1.02 and 0.23W/m 3 , respectively. Also, low-cost zirconium-palladium-composite showed better catalytic activity and capacitance over ZrO 2 with 20A/m 3 current production and demonstrated its suitability for MFC applications. Cyclic voltammetry analyses showed higher well-defined redox peaks in composite catalysts (Mn/Zr-Pd-C) over other catalyzed MFCs containing MnO 2 or ZrO 2 . Electrochemical behaviour of composite catalysts on cathode showed higher availability of adsorption sites for oxygen reduction and, hence, enhanced the rate of cathodic reactions. Thus, Mn/Zr-Pd-C-based composite catalysts exhibited superior cathodic performance and could be proposed as alternatives to costly Pd-catalyst for field applications. Copyright © 2017 Elsevier Ltd. All rights reserved.

  18. In-situ observation of deuteride formation in palladium electrochemical cathode by X-ray diffraction method

    International Nuclear Information System (INIS)

    Yamamoto, Takao; Oka, Takashi; Taniguchi, Ryoichi

    1990-01-01

    In-situ X-ray diffraction observation of palladium foil cathode (10 μm) was carried out during electrolysis of 0.1N-LiOD heavy water solution in order to estimate the deuterium content in palladium during the detection of charged particles in our previous work. A complete transformation into β-palladium deuteride phase was observed, and its maximum lattice constant 4.06 A was evaluated as corresponding to D/Pd = 0.73. The deuterium concentration in the previous work was estimated as higher than this considering the difference in cell conditions. (author)

  19. Synergistic dual activation catalysis by palladium nanoparticles for epoxide ring opening with phenols.

    Science.gov (United States)

    Seth, Kapileswar; Roy, Sudipta Raha; Pipaliya, Bhavin V; Chakraborti, Asit K

    2013-07-04

    Synergistic dual activation catalysis has been devised for epoxide phenolysis wherein palladium nanoparticles induce electrophilic activation via coordination with the epoxide oxygen followed by nucleophilic activation through anion-π interaction with the aromatic ring of the phenol, and water (reaction medium) also renders assistance through 'epoxide-phenol' dual activation.

  20. REMOVAL OF NICKEL(II) AND PALLADIUM(II) FROM SURFACE ...

    African Journals Online (AJOL)

    Preferred Customer

    Nickel is widely used in electroplating, in the manufacture of Ni-Cd batteries, in rods for arc welding, in pigments for ... Palladium has an extensive use in electrical industry as grids for ... It is also used as catalytic converter in motor vehicles.

  1. Copper-based electrochemical sensor with palladium electrode for cathodic stripping voltammetry of manganese.

    Science.gov (United States)

    Kang, Wenjing; Pei, Xing; Bange, Adam; Haynes, Erin N; Heineman, William R; Papautsky, Ian

    2014-12-16

    In this work, we report on the development of a palladium-based, microfabricated point-of-care electrochemical sensor for the determination of manganese using square wave cathodic stripping voltammetry. Heavy metals require careful monitoring, yet current methods are too complex for a point-of-care system. Voltammetry offers an attractive approach to metal detection on the microscale, but traditional carbon, gold, or platinum electrodes are difficult or expensive to microfabricate, preventing widespread use. Our sensor uses palladium working and auxiliary electrodes and integrates them with a copper-based reference electrode for simple fabrication and compatibility with microfabrication and printed circuit board processing, while maintaining competitive performance in electrochemical detection. Copper electrodes were prepared on glass substrate using a combination of microfabrication procedures followed by electrodeposition of palladium. The disposable sensor system was formed by bonding a poly(dimethylsiloxane) (PDMS) well to the glass substrate. Cathodic stripping voltammetry of manganese using our new disposable palladium-based sensors exhibited 334 nM (18.3 ppb) limit of detection in borate buffer. The sensor was used to demonstrate manganese determination in natural water samples from a pond in Burnet Woods, located in Cincinnati, OH, and the Ohio River.

  2. Thin film platinum–palladium thermocouples for gas turbine engine applications

    Energy Technology Data Exchange (ETDEWEB)

    Tougas, Ian M.; Gregory, Otto J., E-mail: gregory@egr.uri.edu

    2013-07-31

    Thin film platinum:palladium thermocouples were fabricated on alumina and mullite surfaces using radio frequency sputtering and characterized after high temperature exposure to oxidizing environments. The thermoelectric output, hysteresis, and drift of these sensors were measured at temperatures up to 1100 °C. Auger electron spectroscopy was used to follow the extent of oxidation in each thermocouple leg and interdiffusion at the metallurgical junction. Minimal oxidation of the platinum and palladium thermoelements was observed after high temperature exposure, but considerable dewetting and faceting of the films were observed in scanning electron microscopy. An Arrhenius temperature dependence on the drift rate was observed and later attributed to microstructural changes during thermal cycling. The thin film thermocouples, however, did exhibit excellent stability at 1000 °C with drift rates comparable to commercial type-K wire thermocouples. Based on these results, platinum:palladium thin film thermocouples have considerable potential for use in the hot sections of gas turbine engines. - Highlights: • Stable thin film platinum:palladium thermocouples for gas turbine engines • Little oxidation but significant microstructural changes from thermal cycling • Minimal hysteresis during repeated thermal cycling • Drift comparable to commercial wire thermocouples.

  3. Green synthesis of palladium nanoparticles with carboxymethyl cellulose for degradation of azo-dyes

    Energy Technology Data Exchange (ETDEWEB)

    Li, Gang; Li, Yun; Wang, Zhengdong; Liu, Huihong, E-mail: huihongliu@126.com

    2017-02-01

    Palladium nanoparticles (PdNPs) were synthesized through friendly environmental method using PdCl{sub 2} and carboxymethyl cellulose (CMC) in an aqueous solution (pH 6) at controlled water bath (80 °C) for 30 min. CMC functioned as both reducing and stabilizing agent. The characterization through high resolution-transmission electron microscopic (HRTEM) and X-ray Fluorescence Spectrometry (XRF) inferred that the as-synthesized PdNPs were spherical in shape with a face cubic crystal (FCC) structure. The results from dynamic light scattering (DLS) suggested the PdNPs had the narrow size distribution with an average size of 2.5 nm. The negative zeta potential (−52.6 mV) kept the as-synthesized PdNPs stable more than one year. The PdNPs showed the excellent catalytic activity by reducing degradation of azo-dyes, such as p-Aminoazobenzene, acid red 66, acid orange 7, scarlet 3G and reactive yellow 179, in the present of sodium borohydride. - Highlights: • Green synthesis of palladium nanoparticles using carboxymethyl cellulose. • The synthesis of palladium nanoparticles were performed easily. • Carboxymethyl cellulose acts as both reducing and stabilization agents. • The as-synthesized palladium nanoparticles show excellent catalytic activity.

  4. Reversible, high molecular weight palladium and platinum coordination polymers based on phosphorus ligands

    NARCIS (Netherlands)

    Paulusse, J.M.J.; Huijbers, J.P.J.; Sijbesma, R.P.

    2005-01-01

    A general strategy for the preparation and characterization of high molecular weight coordination polymers based on bifunctional phosphorus ligands and palladium or platinum dichloride is described. Metal-to-ligand stoichiometry is of key importance for the formation of linear coordination polymers

  5. Reversible, High Molecular Weight Palladium and Platinum Coordination Polymers Based on Phosphorus Ligands

    NARCIS (Netherlands)

    Paulusse, Jos Marie Johannes; Huijbers, Jeroen P.J.; Sijbesma, Rint P.

    2005-01-01

    A general strategy for the preparation and characterization of high molecular weight coordination polymers based on bifunctional phosphorus ligands and palladium or platinum dichloride is described. Metal-to-ligand stoichiometry is of key importance for the formation of linear coordination polymers

  6. PALLADIUM-FACILITATED ELECTROLYTIC DECHLORINATION OF 2-CHLOROBIPHENYL USING A GRANULAR-GRAPHITE ELECTRODE.

    Science.gov (United States)

    Palladium-assisted electrocatalytic dechlorination of 2-chlorobiphenyl (2-Cl BP) in aqueous solutions was conducted in a membrane-separated electrochemical reactor with granular-graphite packed electrodes. The dechlorination took place at a granular-graphite cathode while Pd was ...

  7. Preparation of palladium impregnated alumina adsorbents: Thermal and neutron activation analysis

    Energy Technology Data Exchange (ETDEWEB)

    Mukherjee, Sumanta; Gupta, N.K.; Roy, S.P.; Dash, S.; Kumar, A.; Bamankar, Y.R.; Rao, T.V. Vittal [Product Development Division, Bhabha Atomic Research Centre, Mumbai 400085 (India); Kumar, N. [Fuel Chemistry Division, Bhabha Atomic Research Centre, Mumbai 400085 (India); Naik, Y., E-mail: ynaik@barc.gov.in [Product Development Division, Bhabha Atomic Research Centre, Mumbai 400085 (India)

    2016-02-10

    Highlights: • Pd/Al{sub 2}O{sub 3} composite microspheres particles with high surface area were prepared sol–gel process. • Scanning electron microscopy (SEM) studies on silver coated particle. • Content of the palladium was determined using Neutron Activation Analysis (NAA). • Decomposition study has been done by quadrupole mass analyser. - Abstract: Pd/Al{sub 2}O{sub 3} composite microspheres particles with high surface area were prepared sol–gel process. The decomposition of dried gel-particles was studied by TGA/DTA and FT-IR technique. TGA studies indicated that formation of palladium is marked by a broad exothermic peak with a loss of water and oxidation of trapped HMTA/Urea nitrate mixture. The main decomposition reaction took place in the temperature range of 660–1250 K in helium and relatively lower temperature of 400 K to 1250 K in oxygen. Optical microscopy indicated that the distribution of palladium is uniform. SEM studies on silver coated particle indicated that there was surface erosion of some gel spheres while in few of them micro cracks were seen at high resolution. Content of the palladium was determined using Neutron Activation Analysis (NAA). Decomposition at various temperatures was studied using Residual gas analyser and decomposition species were identified using quadrupole mass analyser.

  8. Chalcogen-containing oxazolines in the palladium-catalyzed asymmetric allylic alkylation

    Directory of Open Access Journals (Sweden)

    Braga Antonio L.

    2006-01-01

    Full Text Available A comparative study about the ability of chiral chalcogen-containing oxazolines to act as chiral ligands in the palladium-catalyzed allylic alkylation of rac-1,3-diphenyl-2-propenyl acetate with dimethyl malonate is reported. Differences in the catalytic performance are observed with sulfur, selenium and tellurium analogues.

  9. Halide-Enhanced Catalytic Activity of Palladium Nanoparticles Comes at the Expense of Catalyst Recovery

    Directory of Open Access Journals (Sweden)

    Azzedine Bouleghlimat

    2017-09-01

    Full Text Available In this communication, we present studies of the oxidative homocoupling of arylboronic acids catalyzed by immobilised palladium nanoparticles in aqueous solution. This reaction is of significant interest because it shares a key transmetallation step with the well-known Suzuki-Miyaura cross-coupling reaction. Additives can have significant effects on catalysis, both in terms of reaction mechanism and recovery of catalytic species, and our aim was to study the effect of added halides on catalytic efficiency and catalyst recovery. Using kinetic studies, we have shown that added halides (added as NaCl and NaBr can increase the catalytic activity of the palladium nanoparticles more than 10-fold, allowing reactions to be completed in less than half a day at 30 °C. However, this increased activity comes at the expense of catalyst recovery. The results are in agreement with a reaction mechanism in which, under conditions involving high concentrations of chloride or bromide, palladium leaching plays an important role. Considering the evidence for analogous reactions occurring on the surface of palladium nanoparticles under different reaction conditions, we conclude that additives can exert a significant effect on the mechanism of reactions catalyzed by nanoparticles, including switching from a surface reaction to a solution reaction. The possibility of this switch in mechanism may also be the cause for the disagreement on this topic in the literature.

  10. Electrochemical behavior of fission palladium in 1-butyl-3-methylimidazolium chloride

    Energy Technology Data Exchange (ETDEWEB)

    Jayakumar, M.; Venkatesan, K.A.; Srinivasan, T.G. [Fuel Chemistry Division, Indira Gandhi Centre for Atomic Research, Kalpakkam 603102 (India)

    2007-08-01

    Electrochemical behavior of palladium (II) chloride in 1-butyl-3-methylimidazolium chloride has been investigated by various electrochemical transient techniques using glassy carbon working electrode at different temperatures (343-373 K). Cyclic voltammogram consisted of a prominent reduction wave at -0.61 V (vs. Pd) due to the reduction of Pd(II) to Pd, and two oxidation waves at -0.26 and 0.31 V. A nucleation loop is observed at -0.53 V. The diffusion coefficient of palladium (II) in bmimCl ({proportional_to}10{sup -7} cm{sup 2}/s) was determined and the energy of activation (63 kJ/mol) was deduced from the cyclic voltammograms at various temperatures. Nucleation and growth of palladium on glassy carbon working electrode has been investigated by chronoamperometry and chronopotentiometry. The growth and decay of chronocurrents measured for palladium deposition has been found to follow the instantaneous nucleation model with three-dimensional growth of nuclei. The surface morphology of the deposit obtained at various applied potentials revealed the formation of dendrites immediately after nucleation and spread in all the directions with time. (author)

  11. Alternative products to carbazoles in the oxidation of diphenylamines with palladium (II) acetate

    OpenAIRE

    Raposo, M. Manuela M.; Campos, Ana M. F. Oliveira; Shannon, Patrick V. R.

    1997-01-01

    Although simple diphenylamines are conveniently oxidised with Palladium (II) acetate to give carbazoles, for more complex examples, carbazoles are minor products amongst many. CRUP (Portugal). British Council - Treaty of Windsor Programme. Junta Nacional de Investigação Científica e Tecnológica.

  12. Oxidative addition of aryl chlorides to monoligated palladium(0): A DFT-SCRF study

    DEFF Research Database (Denmark)

    Ahlquist, Mårten Sten Gösta; Norrby, Per-Ola

    2007-01-01

    Oxidative addition of aryl chlorides to palladium has been investigated by hybrid density functional theory methods (B3LYP), including a continuum model describing the solvent implicitly. A series of para-substituted aryl chlorides were studied to see the influence of electronic effects...

  13. Definition of the size of nanoclusters of silver and palladium in carbon fiber

    International Nuclear Information System (INIS)

    Volobuev, V.S.; Bashmakov, I.A.; Lukashevich, S.M.; Tolkacheva, E.A.; Tikhonova, T.F.; Lukashevich, M.G.; Kaputskij, F.N.

    2008-01-01

    Size of palladium and silver nanoclusters is carbon matrix prepared by heart treatment of metal-polymer precursor has been determined by means of XR diffractions study. It was shown that the cluster size increases with increasing annealing temperature from 700 to 900 degree Celsius by factor two. No structuring of carbon matrix was observed under clusters forming. (authors)

  14. Sensitization to palladium and nickel in Europe and the relationship with oral disease and dental alloys

    NARCIS (Netherlands)

    Muris, J.; Goossens, A.; Gonçalo, M.; Bircher, A.J.; Giménez-Arnau, A.; Foti, C.; Rustemeyer, T.; Feilzer, A.J.; Kleverlaan, C.J.

    2015-01-01

    Background The role of palladium and nickel sensitization in oral disease and dermatitis is not fully understood. Objectives To investigate whether sensitization to these metals was associated with exposure to dental alloys and oral and skin complaints/symptoms in a European multicentre study.

  15. Controlled deposition of palladium nanodendrites on the tips of gold nanorods and their enhanced catalytic activity.

    Science.gov (United States)

    Su, Gaoxing; Jiang, Huaqiao; Zhu, Hongyan; Lv, Jing-Jing; Yang, Guohai; Yan, Bing; Zhu, Jun-Jie

    2017-08-31

    Plasmonic Au-Pd nanostructures have drawn significant attention for use in heterogeneous catalysis. In this study, palladium nanodendrite-tipped gold nanorods (PdND-T-AuNRs) were subjected to a facile fabrication under mild reaction conditions. The palladium amounts on the two tips were tunable. In the preparation of PdND-T-AuNRs, dense capped AuNRs, a low reaction temperature, and suitable stabilizing agents were identified as critical reaction parameters for controlling palladium nanodendrites deposited on both ends of AuNRs. After overgrowth with palladium nanodendrites, the longitudinal surface plasmonic resonance peaks of PdND-T-AuNRs were red-shifted from 810 nm to 980 nm. The electrocatalytic activity of PdND-T-AuNRs for ethanol oxidation was examined, which was a bit weaker than that of cuboid core-shell Au-Pd nanodendrites; however, PdND-T-AuNRs were more stable in ethanol electrooxidation. Moreover, the photocatalytic activity of PdND-T-AuNRs for Suzuki cross-coupling reactions was investigated. At room temperature, nearly 100% yield was obtained under laser irradiation. The results can further enhance our capability of fine-tuning the optical, electronic, and catalytic properties of the bimetallic Au-Pd nanostructures.

  16. Sonogashira Coupling Reaction with Palladium Powder and Potassium Fluoride in Methanol

    Institute of Scientific and Technical Information of China (English)

    王磊; 李品华

    2003-01-01

    A Sonogashira coupling reaction of aromatic halides with terminal alkynes in the presence of palladium powder,potassium fluoride,cuprous iodide and triphenylphosphine in methanol,giving the corresponding coupling products aryl alkynes in good to excellent yiekls,was investigated.

  17. Palladium-catalyzed aerobic oxidative cross-coupling of arylhydrazines with terminal alkynes.

    Science.gov (United States)

    Zhao, Yingwei; Song, Qiuling

    2015-09-04

    The palladium-catalyzed Sonogashira-type aerobic oxidative coupling of arylhydrazines with terminal alkynes via C-N bond cleavage has been developed; internal alkynes were afforded with a broad substrate scope. This reaction proceeds under copper- and base-free conditions with molecular oxygen as the sole oxidant and nitrogen and water as the only by-products.

  18. Practical and General Palladium-Catalyzed Synthesis of Ketones from Internal Olefins

    KAUST Repository

    Morandi, Bill; Wickens, Zachary K.; Grubbs, Robert H.

    2013-01-01

    Make it simple! A convenient and general palladium-catalyzed oxidation of internal olefins to ketones is reported. The transformation occurs at room temperature and shows wide substrate scope. Applications to the oxidation of seed-oil derivatives and a bioactive natural product (see scheme) are described, as well as intriguing mechanistic features.

  19. Reactivation of a Palladium Catalyst during Glucose Oxidation by Molecular Oxygen

    Czech Academy of Sciences Publication Activity Database

    Gogová, Zuzana; Hanika, Jiří

    2009-01-01

    Roč. 63, č. 5 (2009), s. 520-526 ISSN 0366-6352 R&D Projects: GA ČR(CZ) GD203/08/H032 Institutional research plan: CEZ:AV0Z40720504 Keywords : glucose * palladium catalyst * deactivation Subject RIV: CI - Industrial Chemistry, Chemical Engineering Impact factor: 0.791, year: 2009

  20. Metal Palladium Dispersed Inside Macroporous Ion-Exchange Resins: Textural Characterization and Accessibility to Gaseou Reactants

    Czech Academy of Sciences Publication Activity Database

    Biffis, A.; Jeřábek, Karel; D'Archivio, A. A.; Galantini, L.; Corain, B.

    2000-01-01

    Roč. 130, - (2000), s. 2327-2332 ISSN 0167-2991. [International Congress on Catalysis /12./. Granada, 09.07.2000-14.07.2000] Institutional research plan: CEZ:AV0Z4072921 Keywords : metal palladium * dispersed * ion-exchange resins Subject RIV: CI - Industrial Chemistry, Chemical Engineering Impact factor: 0.513, year: 2000

  1. Practical and General Palladium-Catalyzed Synthesis of Ketones from Internal Olefins

    KAUST Repository

    Morandi, Bill

    2013-01-16

    Make it simple! A convenient and general palladium-catalyzed oxidation of internal olefins to ketones is reported. The transformation occurs at room temperature and shows wide substrate scope. Applications to the oxidation of seed-oil derivatives and a bioactive natural product (see scheme) are described, as well as intriguing mechanistic features.

  2. Palladium-Catalysed Direct Cross-Coupling of Organolithium Reagents with Aryl and Vinyl Triflates

    NARCIS (Netherlands)

    Vila, Carlos; Hornillos, Valentin; Giannerini, Massimo; Fananas-Mastral, Martin; Feringa, Bernard L.

    2014-01-01

    Carbon-Carbon Bond Formation Carbon-carbon bond formation by the cross-coupling of highly reactive organolithium reagents is a major challenge. Recently, it was demonstrated that palladium catalysts are able to couple organic halides with various organolithium species under mild conditions in a

  3. Palladium-catalysed direct cross-coupling of secondary alkyllithium reagents

    NARCIS (Netherlands)

    Vila, Carlos; Giannerini, Massimo; Hornillos, Valentin; Fananas-Mastral, Martin; Feringa, Ben L.

    2014-01-01

    Palladium-catalysed cross-coupling of secondary C(sp(3)) organometallic reagents has been a long-standing challenge in organic synthesis, due to the problems associated with undesired isomerisation or the formation of reduction products. Based on our recently developed catalytic C-C bond formation

  4. Preparation of fluorinated biaryls through direct palladium-catalyzed coupling of polyfluoroarenes with aryltrifluoroborates

    KAUST Repository

    Fang, Xin

    2013-07-01

    The direct palladium-catalyzed coupling of polyfluoroarenes with aryltrifluoroborates gave the desired products of fluorinated biaryls in good to excellent yields. A diverse set of important functional groups including methoxy, aldehyde, ester, nitro and halide can be well tolerated in the protocol. © 2013 Elsevier B.V. All rights reserved.

  5. Silver-palladium catalysts for the direct synthesis of hydrogen peroxide

    Science.gov (United States)

    Khan, Zainab; Dummer, Nicholas F.; Edwards, Jennifer K.

    2017-11-01

    A series of bimetallic silver-palladium catalysts supported on titania were prepared by wet impregnation and assessed for the direct synthesis of hydrogen peroxide, and its subsequent side reactions. The addition of silver to a palladium catalyst was found to significantly decrease hydrogen peroxide productivity and hydrogenation, but crucially increase the rate of decomposition. The decomposition product, which is predominantly hydroxyl radicals, can be used to decrease bacterial colonies. The interaction between silver and palladium was characterized using scanning electron microscopy, X-ray diffraction, X-ray photoelectron spectroscopy (XPS) and temperature programmed reduction (TPR). The results of the TPR and XPS indicated the formation of a silver-palladium alloy. The optimal 1% Ag-4% Pd/TiO2 bimetallic catalyst was able to produce approximately 200 ppm of H2O2 in 30 min. The findings demonstrate that AgPd/TiO2 catalysts are active for the synthesis of hydrogen peroxide and its subsequent decomposition to reactive oxygen species. The catalysts are promising for use in wastewater treatment as they combine the disinfectant properties of silver, hydrogen peroxide production and subsequent decomposition. This article is part of a discussion meeting issue 'Providing sustainable catalytic solutions for a rapidly changing world'.

  6. Bulk and Surface Structures of Palladium-Modified Copper-Zinc Oxides ex Hydroxycarbonate Precursors

    NARCIS (Netherlands)

    López Granados, M.; Melián-Cabrera, I.; Fierro, J.L.G.

    2002-01-01

    (Pd)-Cu-Zn ex hydroxycarbonate precursors were prepared and characterized by several bulk and surface techniques. A palladium-free Cu-Zn precursor (CZ) was prepared by coprecipitation. Two Pd-Cu-Zn samples were prepared by coprecipitation (PCZ-CP) and sequential precipitation (PCZ-SP). It is shown

  7. Synthesis of Nitriles via Palladium-Catalyzed Water Shuffling from Amides to Acetonitrile

    OpenAIRE

    Zhang, Wandi; Haskins, Christopher W.; Yang, Yang; Dai, Mingji

    2014-01-01

    Palladium-catalyzed synthesis of nitriles from amides has been described. Two similar, but complementary reaction conditions have been identified to convert various amides including α,β,γ,δ-unsaturated amides, cinnamides, aromatic amides and alkyl amides to the corresponding nitriles in good to excellent yield.

  8. Synthesis of nitriles via palladium-catalyzed water shuffling from amides to acetonitrile.

    Science.gov (United States)

    Zhang, Wandi; Haskins, Christopher W; Yang, Yang; Dai, Mingji

    2014-12-07

    Palladium-catalyzed synthesis of nitriles from amides has been described. Two similar, but complementary reaction conditions have been identified to convert various amides including α,β,γ,δ-unsaturated amides, cinnamides, aromatic amides and alkyl amides to the corresponding nitriles in good to excellent yield.

  9. Palladium(II)-catalyzed ortho-olefination of arenes applying sulfoxides as remote directing groups.

    Science.gov (United States)

    Wang, Binjie; Shen, Chuang; Yao, Jinzhong; Yin, Hong; Zhang, Yuhong

    2014-01-03

    A novel palladium-catalyzed ortho-C(sp(2))-H olefination protocol has been developed by the use of sulfoxide as the directing group. Importantly, relatively remote coordination can be accessed to achieve the ortho olefination of benzyl, 2-arylethyl, and 3-arylpropenyl sulfoxide substrates, and the olefinated sulfoxide can be easily transformed to other functionalities.

  10. Palladium Hydride Promoted Stereoselective Isomerization of Unactivated Di(exo)methylenes to Endocyclic Dienes

    OpenAIRE

    Jung, Michael E.; Lee, Gloria S.; Pham, Hung V.; Houk, K. N.

    2014-01-01

    The exomethylenes of 2,6-disubstituted bicyclo[3.3.1]nonan-9-ones 2 are readily isomerized over a palladium catalyst under an atmosphere of hydrogen to predominantly form the isomer 3 with C 2 symmetry with very little formation of the analogous product with C s symmetry. A hydrogen source is essential to effect the rearrangement.

  11. Memory effects in palladium-catalyzed allylic Alkylations of 2-cyclohexen-1-yl acetate

    DEFF Research Database (Denmark)

    Svensen, Nina; Fristrup, Peter; Tanner, David Ackland

    2007-01-01

    The objective of this work was to characterize the enantiospecificity of the allylic alkylation of enantioenriched 2-cyclohexen-1-yl acetate with the enolate ion of dimethyl malonate catalyzed by unsymmetrical palladium catalysts. The precatalysts employed were (eta(3)-allyl)PdLCl, where L...

  12. Assembling strategy to synthesize palladium modified kaolin nanocomposites with different morphologies

    OpenAIRE

    Li, Xiaoyu; Ouyang, Jing; Zhou, Yonghua; Yang, Huaming

    2015-01-01

    Nanocomposites of aluminosilicate minerals, kaolins (kaolinite and halloysite) with natural different morphologies assembling with palladium (Pd) nanoparticles have been successfully synthesized through strong electrostatic adsorption and chemical bonding after surface modification with 3-aminopropyl triethoxysilane (APTES). Meanwhile, the influence of different morphologies supports on catalytic hydrogenation properties was explored. The surface concentration of amino groups on the kaolins w...

  13. Preparation of palladium nanoparticles on alumina surface by chemical co-precipitation method and catalytic applications

    Energy Technology Data Exchange (ETDEWEB)

    Kumar, Avvaru Praveen; Kumar, B. Prem; Kumar, A.B.V. Kiran; Huy, Bui The [Department of Chemistry, Changwon National University, Changwon 641-773 (Korea, Republic of); Lee, Yong-Ill, E-mail: yilee@changwon.ac.kr [Department of Chemistry, Changwon National University, Changwon 641-773 (Korea, Republic of)

    2013-01-15

    Highlights: Black-Right-Pointing-Pointer Facile synthesis of palladium nanoparticles on alumina surface. Black-Right-Pointing-Pointer The surface morphology and properties of the nanocrystalline powders were characterized. Black-Right-Pointing-Pointer The catalytic activities of palladium nanoparticles were investigated. - Abstract: The present work reports a chemical co-precipitation process to synthesize palladium (Pd) nanoparticles using alumina as a supporting material. The optimized temperature for the formation of nanocrystalline palladium was found to be 600 Degree-Sign C. The X-ray diffraction (XRD) and Raman spectroscopy were used to study the chemical nature of the Pd in alumina matrix. The surface morphology and properties of the nanocrystalline powders were examined using thermogravimetric analysis (TG-DTA), XRD, Raman spectroscopy, transmission electron microscopy (TEM), scanning electron microscopy (SEM) and atomic force microscopy (AFM). The calcinations in different atmospheres including in the inert medium forms the pure nano Pd{sup 0} while in the atmospheric air indicates the existence pure Pd{sup 0} along with PdO nanoparticles. The catalytic activities of the as-synthesized nanocrystalline Pd nanoparticles in the alumina matrix were investigated in Suzuki coupling, Hiyama cross-coupling, alkene and alkyne hydrogenation, and aerobic oxidation reactions.

  14. Micromachined Dense Palladium Electrodes for Thin-film Solid Acid Fuel Cells

    NARCIS (Netherlands)

    Unnikrishnan, S.

    2009-01-01

    This thesis paves the way towards the microfabrication of a solid acid electrolyte based fuel cell (µSAFC), which has a membrane electrode assembly (MEA) consisting of a thin-film of water soluble electrolyte encapsulated between two dense palladium electrode membranes. This project work

  15. A Palladium-Catalyzed Vinylcyclopropane (3 + 2) Cycloaddition Approach to the Melodinus Alkaloids

    KAUST Repository

    Goldberg, Alexander F. G.

    2011-08-19

    A palladium-catalyzed (3+2) cycloaddition of a vinylcyclopropane and a β-nitrostyrene is employed to rapidly assemble the cyclopentane core of the Melodinus alkaloids. The ABCD ring system of the natural product family is prepared in six steps from commercially available materials.

  16. GREEN SYNTHESIS OF SILVER AND PALLADIUM NANOPARTICLES AT ROOM TEMPERATURE USING COFFEE AND TEA EXTRACT

    Science.gov (United States)

    An extremely simple green approach that generates bulk quantities of nanocrystals of noble metals such as silver (Ag) and palladium (Pd) using coffee and tea extract at room temperature is described. The single-pot method uses no surfactant, capping agent, and/or template. The ob...

  17. DTDGA impregnated XAD-16 beads for separation and recovery of palladium from acidic wastes

    International Nuclear Information System (INIS)

    Singh, Krishan Kant; Kanagare, Anant B.; Bairwa, K.K.; Manmohan Kumar; Bajaj, Parma N.; Ruhela, Ritesh; Singh, Ajoy K.; Hubli, Rajendra C.

    2014-01-01

    In the present study DTDGA extractant impregnated XAD16 polymeric beads (DTDGA- XAD16) were synthesized by wet chemical method and the beads were characterized by various techniques viz. FT-IR, Optical microscopy, SEM and TGA. The DTDGA-XAD 16 beads were evaluated for separation and recovery of palladium from high level waste solutions (HLW)

  18. Characterization of intracellular palladium nanoparticles synthesized by Desulfovibrio desulfuricans and Bacillus benzeovorans

    Energy Technology Data Exchange (ETDEWEB)

    Omajali, Jacob B., E-mail: JBO037@bham.ac.uk, E-mail: jbomajali@gmail.com; Mikheenko, Iryna P. [University of Birmingham, Unit of Functional Bionanomaterials, School of Biosciences, Institute of Microbiology and Infection (United Kingdom); Merroun, Mohamed L. [University of Granada, Department of Microbiology, Faculty of Sciences (Spain); Wood, Joseph [University of Birmingham, School of Chemical Engineering (United Kingdom); Macaskie, Lynne E. [University of Birmingham, Unit of Functional Bionanomaterials, School of Biosciences, Institute of Microbiology and Infection (United Kingdom)

    2015-06-15

    Early studies have focused on the synthesis of palladium nanoparticles within the periplasmic layer or on the outer membrane of Desulfovibrio desulfuricans and on the S-layer protein of Bacillus sphaericus. However, it has remained unclear whether the synthesis of palladium nanoparticles also takes place in the bacterial cell cytoplasm. This study reports the use of high-resolution scanning transmission electron microscopy with a high-angle annular dark field detector and energy dispersive X-ray spectrometry attachment to investigate the intracellular synthesis of palladium nanoparticles (Pd NPs). We show the intracellular synthesis of Pd NPs within cells of two anaerobic strains of D. desulfuricans and an aerobic strain of B. benzeovorans using hydrogen and formate as electron donors. The Pd nanoparticles were small and largely monodispersed, between 0.2 and 8 nm, occasionally from 9 to 12 nm with occasional larger nanoparticles. With D. desulfuricans NCIMB 8307 (but not D. desulfuricans NCIMB 8326) and with B. benzeovorans NCIMB 12555, the NPs were larger when made at the expense of formate, co-localizing with phosphate in the latter, and were crystalline, but were amorphous when made with H{sub 2,} with no phosphorus association. The intracellular Pd nanoparticles were mainly icosahedrons with surfaces comprising {111} facets and about 5 % distortion when compared with that of bulk palladium. The particles were more concentrated in the cell cytoplasm than the cell wall, outer membrane, or periplasm. We provide new evidence for synthesis of palladium nanoparticles within the cytoplasm of bacteria, which were confirmed to maintain cellular integrity during this synthesis.

  19. Influence of layout parameters on snapback characteristic for a gate-grounded NMOS device in 0.13-μm silicide CMOS technology

    International Nuclear Information System (INIS)

    Jiang Yuxi; Li Jiao; Ran Feng; Cao Jialin; Yang Dianxiong

    2009-01-01

    Gate-grounded NMOS (GGNMOS) devices with different device dimensions and layout floorplans have been designed and fabricated in 0.13-μm silicide CMOS technology. The snapback characteristics of these GGNMOS devices are measured using the transmission line pulsing (TLP) measurement technique. The relationships between snapback parameters and layout parameters are shown and analyzed. A TCAD device simulator is used to explain these relationships. From these results, the circuit designer can predict the behavior of the GGNMOS devices under high ESD current stress, and design area-efficient ESD protection circuits to sustain the required ESD level. Optimized layout rules for ESD protection in 0.13-μm silicide CMOS technology are also presented. (semiconductor devices)

  20. Program description for the qualification of CNEA - Argentina as a supplier of LEU silicide fuel and post-irradiation examinations plan for the first prototype irradiated in Argentina

    International Nuclear Information System (INIS)

    Rugirello, Gabriel; Adelfang, Pablo; Denis, Alicia; Zawerucha, Andres; Marco, Agustin di; Guillaume, Eduardo; Sbaffoni, Monica; Lacoste, Pablo

    1998-01-01

    In this report we present a description of the ongoing and future stages of the program for the qualification of CNEA, Argentina, as a supplier of low enriched uranium silicide fuel elements for research reactor. Particularly we will focus on the characteristics of the future irradiation experiment on a new detachable prototype, the post-irradiation examinations (PIE) plan for the already irradiated prototype PO4 and an overview of the recently implemented PIE facilities and equipment. The program is divided in several steps, some of which have been already completed. It concludes: development of the uranium silicide fissile material, irradiation and PIE of several full-scale prototypes. Important investments have been already carried out in the facilities for the FE production and PIE. (author)

  1. In-pile test results of U-silicide or U-nitride coated U-7Mo particle dispersion fuel in Al

    Science.gov (United States)

    Kim, Yeon Soo; Park, J. M.; Lee, K. H.; Yoo, B. O.; Ryu, H. J.; Ye, B.

    2014-11-01

    U-silicide or U-nitride coated U-Mo particle dispersion fuel in Al (U-Mo/Al) was in-pile tested to examine the effectiveness of the coating as a diffusion barrier between the U-7Mo fuel kernels and Al matrix. This paper reports the PIE data and analyses focusing on the effectiveness of the coating in terms of interaction layer (IL) growth and general fuel performance. The U-silicide coating showed considerable success, but it also provided evidence for additional improvement for coating process. The U-nitride coated specimen showed largely inefficient results in reducing IL growth. From the test, important observations were also made that can be utilized to improve U-Mo/Al fuel performance. The heating process for coating turned out to be beneficial to suppress fuel swelling. The use of larger fuel particles confirmed favorable effects on fuel performance.

  2. In-pile test results of U-silicide or U-nitride coated U-7Mo particle dispersion fuel in Al

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Yeon Soo, E-mail: yskim@anl.gov [Argonne National Laboratory, 9700 South Cass Avenue, Argonne, IL 60439 (United States); Park, J.M.; Lee, K.H.; Yoo, B.O. [Korea Atomic Energy Research Institute, 989-111 Daedeokdaero, Yuseong-gu, Daejeon 305-353 (Korea, Republic of); Ryu, H.J. [Dept. of Nuclear and Quantum Engineering, Korea Advanced Institute of Science and Technology, 291 Daehak-ro, Yuseong-gu, Daejeon 305-701 (Korea, Republic of); Ye, B. [Argonne National Laboratory, 9700 South Cass Avenue, Argonne, IL 60439 (United States)

    2014-11-15

    U-silicide or U-nitride coated U-Mo particle dispersion fuel in Al (U-Mo/Al) was in-pile tested to examine the effectiveness of the coating as a diffusion barrier between the U-7Mo fuel kernels and Al matrix. This paper reports the PIE data and analyses focusing on the effectiveness of the coating in terms of interaction layer (IL) growth and general fuel performance. The U-silicide coating showed considerable success, but it also provided evidence for additional improvement for coating process. The U-nitride coated specimen showed largely inefficient results in reducing IL growth. From the test, important observations were also made that can be utilized to improve U-Mo/Al fuel performance. The heating process for coating turned out to be beneficial to suppress fuel swelling. The use of larger fuel particles confirmed favorable effects on fuel performance.

  3. Vertically grown multiwalled carbon nanotube anode and nickel silicide integrated high performance microsized (1.25 μl) microbial fuel cell

    KAUST Repository

    Mink, Justine E.

    2012-02-08

    Microbial fuel cells (MFCs) are an environmentally friendly method for water purification and self-sustained electricity generation using microorganisms. Microsized MFCs can also be a useful power source for lab-on-a-chip and similar integrated devices. We fabricated a 1.25 μL microsized MFC containing an anode of vertically aligned, forest type multiwalled carbon nanotubes (MWCNTs) with a nickel silicide (NiSi) contact area that produced 197 mA/m 2 of current density and 392 mW/m 3 of power density. The MWCNTs increased the anode surface-to-volume ratio, which improved the ability of the microorganisms to couple and transfer electrons to the anode. The use of nickel silicide also helped to boost the output current by providing a low resistance contact area to more efficiently shuttle electrons from the anode out of the device. © 2012 American Chemical Society.

  4. Moissanite (SiC) with metal-silicide and silicon inclusions from tuff of Israel: Raman spectroscopy and electron microscope studies

    Science.gov (United States)

    Dobrzhinetskaya, Larissa; Mukhin, Pavel; Wang, Qin; Wirth, Richard; O'Bannon, Earl; Zhao, Wenxia; Eppelbaum, Lev; Sokhonchuk, Tatiana

    2018-06-01

    Here, we present studies of natural SiC that occurs in situ in tuff related to the Miocene alkaline basalt formation deposited in northern part of Israel. Raman spectroscopy, SEM and FIB-assisted TEM studies revealed that SiC is primarily hexagonal polytypes 4H-SiC and 6H-SiC, and that the 4H-SiC polytype is the predominant phase. Both SiC polytypes contain crystalline inclusions of silicon (Sio) and inclusions of metal-silicide with varying compositions (e.g. Si58V25Ti12Cr3Fe2, Si41Fe24Ti20Ni7V5Zr3, and Si43Fe40Ni17). The silicides crystal structure parameters match Si2TiV5 (Pm-3m space group, cubic), FeSi2Ti (Pbam space group, orthorhombic), and FeSi2 (Cmca space group, orthorhombic) respectively. We hypothesize that SiC was formed in a local ultra-reduced environment at respectively shallow depths (60-100 km), through a reaction of SiO2 with highly reducing fluids (H2O-CH4-H2-C2H6) arisen from the mantle "hot spot" and passing through alkaline basalt magma reservoir. SiO2 interacting with the fluids may originate from the walls of the crustal rocks surrounding this magmatic reservoir. This process led to the formation of SiC and accompanied by the reducing of metal-oxides to native metals, alloys, and silicides. The latter were trapped by SiC during its growth. Hence, interplate "hot spot" alkali basalt volcanism can now be included as a geological environment where SiC, silicon, and silicides can be found.

  5. Behavior of silicon in nitric media. Application to uranium silicides fuels reprocessing; Comportement du silicium en milieu nitrique. Application au retraitement des combustibles siliciures d'uranium

    Energy Technology Data Exchange (ETDEWEB)

    Cheroux, L

    2001-07-01

    Uranium silicides are used in some research reactors. Reprocessing them is a solution for their cycle end. A list of reprocessing scenarios has been set the most realistic being a nitric dissolution close to the classic spent fuel reprocessing. This uranium silicide fuel contains a lot of silicon and few things are known about polymerization of silicic acid in concentrated nitric acid. The study of this polymerization allows to point out the main parameters: acidity, temperature, silicon concentration. The presence of aluminum seems to speed up heavily the polymerization. It has been impossible to find an analytical technique smart and fast enough to characterize the first steps of silicic acid polymerization. However the action of silicic species on emulsions stabilization formed by mixing them with an organic phase containing TBP has been studied, Silicon slows down the phase separation by means of oligomeric species forming complex with TBP. The existence of these intermediate species is short and heating can avoid any stabilization. When non irradiated uranium silicide fuel is attacked by a nitric solution, aluminum and uranium are quickly dissolved whereas silicon mainly stands in solid state. That builds a gangue of hydrated silica around the uranium silicide particulates without preventing uranium dissolution. A small part of silicon passes into the solution and polymerize towards the highly poly-condensed forms, just 2% of initial silicon is still in molecular form at the end of the dissolution. A thermal treatment of the fuel element, by forming inter-metallic phases U-Al-Si, allows the whole silicon to pass into the solution and next to precipitate. The behavior of silicon in spent fuels should be between these two situations. (author)

  6. Morphological and electrical properties of self-assembled iron silicide nanoparticles on Si(0 0 1) and Si(1 1 1) substrates

    International Nuclear Information System (INIS)

    Molnár, G.; Dózsa, L.; Erdélyi, R.; Vértesy, Z.; Osváth, Z.

    2015-01-01

    Highlights: • Epitaxial iron silicide nanostructures were grown on Si(1 1 1) and Si(0 0 1) substrates. • The size and shape of the particles are the function of the thickness and annealing. • The local current–voltage characteristics were measured by conductive AFM. • The different size and shape nanoparticles show similar I–V characteristics. • The tip current is dominated in few nm size sites, visible in the AFM phase image. - Abstract: Epitaxial iron silicide nanostructures are grown by solid phase epitaxy on Si(0 0 1) and Si(1 1 1), and by reactive deposition epitaxy on Si(0 0 1) substrates. The formation process is monitored by reflection high-energy electron diffraction. The morphology, size, and electrical properties of the nanoparticles are investigated by scanning electron microscopy, by electrically active scanning probe microscopy, and by confocal Raman spectroscopy. The results show that the shape, size, orientation, and density of the nanoobjects can be tuned by self-assembly, controlled by the lattice misfit between the substrates and iron silicides. The size distribution and shape of the grown nanoparticles depend on the substrate orientation, on the initial thickness of the evaporated iron, on the temperature and time of the annealing, and on the preparation method. The so-called Ostwald ripening phenomena, which state that the bigger objects develop at the expense of smaller ones, controls the density of the nanoparticles. Raman spectra show the bigger objects do not contain β-FeSi 2 phase. The different shape nanoparticles exhibit small, about 100 mV barrier compared to the surrounding silicon. The local leakage current of the samples measured by conductive AFM using a Pt coated Si tip is localized in a few nanometers size sites, and the sites which we assume are very small silicide nanoparticles or point defects.

  7. Evaluation Of Radioactivity Concentration In The Primary Cooling Water System Of The RSG-GAS During Operation With 30% Silicide Fuels

    International Nuclear Information System (INIS)

    Hartoyo, Unggul; Udiyani, P.M.; Setiawanto, Anto

    2001-01-01

    The evaluating radioactivity concentration in the primary cooling water of the RSG-GAS during operation with 30% silicide fuels has been performed. The method of the research is sampling of primary cooling water during operation of the reactor and calculation of its radioactivity concentration. Based on the data obtained from calculation, the identified nuclides in the water are, Mn-56, Sb-124, Sb-122 and Na-24, under the limit of safety value

  8. Soluble Polymer-supported Synthesis of Indoles via Palladium-mediat -ed Heteroannulation of Terminal Alkynes with o-Iodoanilines

    Institute of Scientific and Technical Information of China (English)

    2002-01-01

    A soluble polymer-supported synthesis of indoles via palladium-mediated hetero- annulation of terminal alkynes with o-iodoanilines has been described. The protocol provides a useful tool for constructing combinatorial indole libraries.

  9. Stereoselective synthesis of tricyclic compounds by intramolecular palladium-catalyzed addition of aryl iodides to carbonyl groups

    Directory of Open Access Journals (Sweden)

    Jakub Saadi

    2016-06-01

    Full Text Available Starting from γ-ketoesters with an o-iodobenzyl group we studied a palladium-catalyzed cyclization process that stereoselectively led to bi- and tricyclic compounds in moderate to excellent yields. Four X-ray crystal structure analyses unequivocally defined the structure of crucial cyclization products. The relative configuration of the precursor compounds is essentially transferred to that of the products and the formed hydroxy group in the newly generated cyclohexane ring is consistently in trans-arrangement with respect to the methoxycarbonyl group. A transition-state model is proposed to explain the observed stereochemical outcome. This palladium-catalyzed Barbier-type reaction requires a reduction of palladium(II back to palladium(0 which is apparently achieved by the present triethylamine.

  10. Camphyl-based α-diimine palladium complexes: highly efficient precatalysts for direct arylation of thiazoles in open-air.

    Science.gov (United States)

    Chen, Fu-Min; Lu, Dong-Dong; Hu, Li-Qun; Huang, Ju; Liu, Feng-Shou

    2017-07-21

    Based on the strategy of the development of phosphine-free palladium-catalyzed direct C-H arylation, a series of camphyl-based α-diimine palladium complexes bearing sterically bulky substituents were synthesized and characterized. The palladium complexes were applied for the cross-coupling of thiazole derivatives with aryl bromides. The effect of the sterically bulky substituent on the N-aryl moiety as well as the reaction conditions was screened. Under the optimal protocols, a wide range of aryl bromides can be smoothly coupled with thiazoles in good to excellent yields in the presence of a low palladium loading of 0.2 mol% under open-air conditions.

  11. Simultaneous aluminizing and chromizing of steels to form (Fe,Cr){sub 3}Al coatings and Ge-doped silicide coatings of Cr-Zr base alloys

    Energy Technology Data Exchange (ETDEWEB)

    Zheng, M.; He, Y.R.; Rapp, R.A. [Ohio State Univ., Columbus, OH (United States). Dept. of Materials Science and Engineering

    1997-12-01

    A halide-activated cementation pack involving elemental Al and Cr powders has been used to achieve surface compositions of approximately Fe{sub 3}Al plus several percent Cr for low alloy steels (T11, T2 and T22) and medium carbon steel (1045 steel). A two-step treatment at 925 C and 1150 C yields the codeposition and diffusion of aluminum and chromium to form dense and uniform ferrite coatings of about 400 {micro}m thickness, while preventing the formation of a blocking chromium carbide at the substrate surfaces. Upon cyclic oxidation in air at 700 C, the coated steel exhibits a negligible 0.085 mg/cm{sup 2} weight gain for 1900 one-hour cycles. Virtually no attack was observed on coated steels tested at ABB in simulated boiler atmospheres at 500 C for 500 hours. But coatings with a surface composition of only 8 wt% Al and 6 wt% Cr suffered some sulfidation attack in simulated boiler atmospheres at temperatures higher than 500 C for 1000 hours. Two developmental Cr-Zr based Laves phase alloys (CN129-2 and CN117(Z)) were silicide/germanide coated. The cross-sections of the Ge-doped silicide coatings closely mimicked the microstructure of the substrate alloys. Cyclic oxidation in air at 1100 C showed that the Ge-doped silicide coating greatly improved the oxidation resistance of the Cr-Zr based alloys.

  12. Analysis Influence of Mixing Gd2O3 in the Silicide Fuel Element to Core Excess Reactivity of RSG-GAS

    International Nuclear Information System (INIS)

    Susilo, Jati

    2004-01-01

    Gadolinium (Gd 2 O 3 ) is a burnable poison material mixed in the pin fuel element of the LWR core used to decrease core excess reactivity. In this research, analysis influence of mixing Gd 2 O 3 in the silicide fuel element to excess reactivity of the RSG-GAS core had been done. Equivalent cell of the equilibrium core developed by L.E.Strawbridge from Westing House Co. burn-up calculation has been done using SRAC-PIJ computer code achieve infinite multiplication factor (k x ). Value of Gd 2 O 3 concentration in the fuel element (pcm) showed by mass ratio of Gd 2 O 3 (gram) to that U 3 Si 2 (gram) times 10 5 , that is 0 pcm ∼ 100 pcm. From the calculation results analysis showed that Gd 2 O 3 concentration added should be considered. because a large number of Gd 2 O 3 will result in not achieving criticality at the Beginning Of Cycle. The maximum concentration of Gd 2 O 3 for RSG-GAS equilibrium fueled silicide 2.96 grU/cc is 80 pcm or 52.02 mgram/fuel plate. Maximum reduction of core excess reactivity due to mixing of Gd 2 O 3 in the RSG-GAS silicide fuels was around 1.502 %Δk/k, and hence not achieving the standard nominal excess reactivity for RSG-GAS core using high density of U 3 Si 2 -Al fuel. (author)

  13. Development of Self-Healing Zirconium-Silicide Coatings for Improved Performance Zirconium-Alloy Fuel Cladding

    Energy Technology Data Exchange (ETDEWEB)

    Sridharan, Kumar [University of Wisconsin-Madison; Mariani, Robert [Idaho National Lab. (INL), Idaho Falls, ID (United States); Bai, Xianming [Idaho National Lab. (INL), Idaho Falls, ID (United States); Xu, Peng [Westinghouse Electric Company; Lahoda, Ed [Westinghouse Electric Company

    2018-03-31

    Given the long-term goal of developing such coatings for use with nuclear reactor fuel cladding, this work describes results of oxidation and corrosion behavior of bulk zirconium-silicide and fabrication of zirconium-silicide coatings on zirconium-alloy test flats, tube configurations, and SiC test flats. In addition, boiling heat transfer of these modified surfaces (including ZrSi2 coating) during clad quenching experiments is discussed in detail. Oxidation of bulk ZrSi2 was found to be negligible compared to Zircaloy-4 (a common Zr-alloy cladding material) and mechanical integrity of ZrSi2 was superior to that of bulk Zr2Si at high temperatures in ambient air. Very interesting and unique multi-nanolayered composite of ZrO2 and SiO2 were observed. Physical model for the oxidation has been proposed wherein Zr–Si–O mixture undergoes a spinodal phase decomposition into ZrO2 and SiO2, which is manifested as a nanoscale assembly of alternating layer of the two oxides. Steam corrosion at high pressure (10.3 MPa) led to weight loss of ZrSi2 and produced oxide scale with depletion of silicon, possibly attributed to volatile silicon hydroxide, gaseous silicon monoxide, and a solubility of silicon dioxide in water. Only Zircon phase (ZrSiO4) formed during oxidation of ZrSi2 at 1400°C in air, and allowed for immobilization silicon species in oxide scale in the aqueous environments. Zirconium-silicide coatings (on zirconium-alloy substrates) investigated in this study were deposited primarily using magnetron sputter deposition method and slurry method, although powder spray deposition processes cold spray and thermal spray methods were also investigated. The optimized ZrSi2 sputtered coating exhibited a highly protective nature at elevated temperatures in ambient air by mitigating oxygen permeation to the underlying zirconium alloy substrate. The high oxidation resistance of the coating has been shown to be due to nanocrystalline SiO2 and ZrSiO4 phases in the amorphous

  14. Palladium nanoparticles supported on layered hydroxide salts and their use in carbon-carbon coupling organic reactions

    OpenAIRE

    Martínez,Maby; Ocampo,Rogelio; Rios,Luz Amalia; Ramírez,Alfonso; Giraldo,Oscar

    2011-01-01

    Palladium nanoparticles supported on zinc hydroxide salts were prepared by intercalation of [PdCl6]2- and its further reduction with ethanol under reflux. All the materials were completely characterized by atomic absorption spectroscopy (AAS), X-ray diffraction (XRD), thermogravimetric/derivative thermogravimetric (TG/DTG) analyses, scanning electron microscopy (SEM), UV-Visible spectrometry and transmission electron microscopy (TEM). TEM analysis confirmed that the palladium nanoparticles we...

  15. Temperature and thickness dependence of the grain boundary scattering in the Ni–Si silicide films formed on silicon substrate at 500 °C by RTA

    International Nuclear Information System (INIS)

    Utlu, G.; Artunç, N.; Selvi, S.

    2012-01-01

    Highlights: ► It is a systematic study of various thicknesses (18–290 nm) of Ni–Si silicide films. ► The temperature-dependent resistivity measurements of the films are studied. ► Resistivity variation of the films with temperature exhibits an unusual behavior. ► Parallel-resistor formula is reduced to Matthiessen's rule in this study. ► Reflection coefficients have been found in a wide temperature and thickness range. - Abstract: The temperature-dependent resistivity measurements of Ni–Si silicide films with 18–290 nm thicknesses are studied as a function of temperature and film thickness over the temperature range of 100–900 K. The most striking behavior is that the variation of the resistivity of the films with temperature exhibits an unusual behavior. The total resistivity of the Ni–Si silicide films in this work increases linearly with temperature up to a T m temperature, thereafter decreases rapidly and finally reaches zero. Our analyses have shown that in the temperature range of 100 to T m (K), parallel-resistor formula reduces to Matthiessen's rule and θ D Debye temperature becomes independent of the temperature for the given thickness range, whereas at high temperatures (above T m ) it increases slightly with thickness. θ D Debye temperature have been found to be about 400–430 K for the films. We have also shown that for temperature range of 100 to T m (K), linear variation of the resistivity of the silicide films with temperature has been caused from both grain-boundary scattering and electron–phonon scattering. That is why, resistivity data could have been analyzed in terms of the Mayadas–Schatzkes (M–S) model successfully. Theoretical and experimental values of reflection coefficients have been calculated by analyzing resistivity data using M–S model. According to our analysis, R increases with decreasing film thickness for a given temperature, while it is almost constant for the thickness range of 200–67 nm and 47

  16. Dosimetric study of a new polymer encapsulated palladium-103 seed

    International Nuclear Information System (INIS)

    Bernard, S; Vynckier, S

    2005-01-01

    The use of low-energy photon emitters for brachytherapy applications, as in the treatment of prostate or ocular tumours, has increased significantly over the last few years. Several new seed models utilizing 103 Pd and 125 I have recently been introduced. Following the TG43U1 recommendations of the AAPM (American Association of Physicists in Medicine) (Rivard et al 2004 Med. Phys. 31 633), dose distributions around these low-energy photon emitters are characterized by the dose rate constant, the radial dose function and the anisotropy function in water. These functions and constants can be measured for each new seed in a solid phantom (i.e. solid water such as WT1) using high spatial resolution detectors such as very small thermoluminescent detectors. These experimental results in solid water must then be converted into liquid water by using Monte Carlo simulations. This paper presents the dosimetric parameters of a new palladium seed, OptiSeed TM (produced by International Brachytherapy (IBt), Seneffe, Belgium), made with a biocompatible polymeric shell and with a design that differs from the hollow titanium encapsulated seed, InterSource 103 , produced by the same company. A polymer encapsulation was chosen by the company IBt in order to reduce the quantity of radioactive material needed for a given dose rate, and to improve the symmetry of the radiation field around the seed. The necessary experimental data were obtained by measurements with LiF thermoluminescent dosimeters (1 mm 3 ) in a solid water phantom (WT1) and then converted to values in liquid water using Monte Carlo calculations (MCNP-4C). Comparison of the results with a previous study by Reniers et al (2002 Appl. Radiat. Isot. 57 805) shows very good agreement for the dose rate constant and for the radial dose function. In addition, the results also indicate an improvement in isotropy compared to a conventional titanium encapsulated seed. The relative dose (anisotropy value relative to 90 deg.) from

  17. Experimental Observation of Nuclear Reactions in Palladium and Uranium

    International Nuclear Information System (INIS)

    J. Dufour; D. Murat; X. Dufour; J. Foos

    2001-01-01

    By submitting various metals (Pd, U) containing hydrogen (from 2000 to 700 000 atoms of hydrogen for 1 000 000 atoms of the host metal) to the combined action of electrical currents and magnetic fields, we have observed a sizeable exothermal effect (from 0.1 to 8 W for 500 mg of metal used). This effect is beyond experimental errors, the energy output being typically 130 to 250% of the energy input and not of chemical origin (exothermal effect in the range of 7000 MJ/mol of metal in the case of palladium and of 60 MJ/mol in the case of uranium). New chemical species also appear in the processes metals. It has been shown by a QED calculation that resonances of long lifetime (s), nuclear dimensions (fm), and low energy of formation (eV) could exist. This concept seems to look like the 'shrunken hydrogen atoms' proposed by various authors. It is indeed very different in two ways (a) being a metastable state, it needs energy to be formed (a few eV) and reverts to normal hydrogen after a few seconds, liberating back its energy of formation (it is thus not the source of the energy observed); (b) its formation can be described as the electron spin/proton nuclear spin interaction becoming first order in the lattice environment (whereas it is third order in a normal hydrogen atom). Moreover, we consider that the hydrex cannot yield a neutron because this reaction is strongly endothermic. To explain our results, we put forward the following working hypothesis: In a metal lattice and under proper conditions, the formation of such resonances (metastable state) could be favored. We propose to call them HYDREX, and we assume that they are actually formed in cold fusion (CF) and low-energy nuclear reaction (LENR) experiments. Once formed, a number of HYDREX could gather around a nucleus of the lattice to form a cluster of nuclear size and of very long life time compared to nuclear time (10 -22 s). In this cluster, nuclear rearrangements could take place, yielding mainly 4 He

  18. FY 1997 report on the improvement of toughness of silicide system intermetallic compounds by complex texture; 1997 nendo chosa hokokusho (fukugo soshikika ni yoru silicide kei kinzokukan kagobutsu no kyojinsei kaizen)

    Energy Technology Data Exchange (ETDEWEB)

    NONE

    1998-03-01

    In order to develop new materials superior in both room- temperature ductility and high-temperature strength, the basic data on MoSi2 intermetallic compounds with complex texture were stored. Intermetallic compound is one of the promising candidates of new super heat-resistant materials superior to conventional super heat-resistant alloys, however, it is extremely poor in ductility at room temperature. Based on available information on isothermal sectional phase diagrams of ternary system (Mo-Si-X system) composed of Mo silicide and the third element (X), some alloy systems were selected in consideration of use of carbide and nitride stably existing as dispersed phase of deposits at high temperature. A knowledge on phase diagrams of ternary system specimens with various compositions was obtained through arc melting, X-ray diffraction and texture observation, and heat treatment conditions for obtaining target complex textures were also determined. Storage of the basic data suggested that improvement of the ductility is possible by forming fine texture through addition of the third element and teat treatment. 21 refs., 58 figs., 15 tabs.

  19. On the possibility of deuteron disintegration in electrochemically compressed D+ in a palladium cathode

    International Nuclear Information System (INIS)

    Ragheb, M.; Miley, G.H.

    1989-01-01

    The possibility of deuteron disintegration due to polarization in the coulomb field of a target nucleus according to an Oppenheimer-Phillips process is discussed within the context of electrochemically compressed D + in a palladium cathode. This reaction is possible between deuterons and palladium isotopes, as well as between the deuterons themselves. In the last case, the equivalent of the proton branch of the deuterium-deuterium fusion reaction occurs in preference to the neutron branch. The process provides a possible explanation for the observed energy release, tritium production, and neutron suppression in the Fleischmann and Pons experiment. If such a process can be experimentally verified, analogous processes leading to the disintegration of the 9 Be nucleus may be achievable

  20. Synthesis of phenanthridines via palladium-catalyzed picolinamide-directed sequential C–H functionalization

    Directory of Open Access Journals (Sweden)

    Ryan Pearson

    2013-05-01

    Full Text Available We report a new synthesis of phenanthridines based on palladium-catalyzed picolinamide-directed sequential C–H functionalization reactions starting from readily available benzylamine and aryl iodide precursors. Under the catalysis of Pd(OAc2, the ortho-C–H bond of benzylpicolinamides is first arylated with an aryl iodide. The resulting biaryl compound is then subjected to palladium-catalyzed picolinamide-directed intramolecular dehydrogenative C–H amination with PhI(OAc2 oxidant to form the corresponding cyclized dihydrophenanthridines. The benzylic position of these dihydrophenanthridines could be further oxidized with Cu(OAc2, removing the picolinamide group and providing phenathridine products. The cyclization and oxidation could be carried out in a single step and afford phenathridines in moderate to good yields.

  1. Immobilization of Highly Effective Palladium Catalyst onto Poly(4-Vinylpyridine): Synthesis and Characterization

    International Nuclear Information System (INIS)

    Siti Kamilah Che Soh; Intan Shafinass Kassim; Siti Aminah Jusoh; Mustaffa Samsuddin

    2016-01-01

    A commonly known weakness of homogeneous catalysts is the difficulty to recover the active catalyst from the product. Due to the disadvantage, the designing of supported catalyst has been approached to overcome the separation difficulty of the palladium-based homogeneous catalyst. New polymer supported N 2 O 2 metal complex was successfully immobilized by mixing of poly(4-vinylpyridine) with palladium(II) complex in the presence of ethyl acetate as solvent. Then, the reaction was stirred for 72 hours at room temperature to form corresponding P 4 VP-Pd catalyst. The properties of immobilized catalyst were characterized by various techniques such as fourier transform infrared (FTIR), thermogravimetric (TGA), X-ray diffraction (XRD), scanning electron microscopy/ energy dispersive X-ray (SEM/ EDX) and inductively coupled plasma-optical emission (ICP-OES) spectroscopy. (author)

  2. Enhancement in photovoltaic properties of silicon solar cells by surface plasmon effect of palladium nanoparticles

    Science.gov (United States)

    Atyaoui, Malek; Atyaoui, Atef; Khalifa, Marwen; Elyagoubi, Jalel; Dimassi, Wissem; Ezzaouia, Hatem

    2016-04-01

    This work presents the surface Plasmon effect of Palladium nanoparticles (Pd NPs) on the photovoltaic properties of silicon solar cells. Pd NPs were deposited on the p-type silicon base of the n+/p junction using a chemical deposition method in an aqueous solution containing Palladium (II) Nitrate (PdNO3)2 and Ammonium Hydroxide (NH4OH) followed by a thermal treatment at 500 °C under nitrogen atmosphere. Chemical composition and surface morphology of the treated silicon base were examined by energy dispersive X-ray (EDX) spectroscopy, scanning electronic microscopy (SEM) and Atomic Force Microscopy (AFM). The effect of the deposited Pd NPs on the electrical properties was evaluated by the internal quantum efficiency (IQE) and current-voltage (I-V) measurements. The results indicate that the formation of the Pd NPs is accompanied by an enhanced light absorption and improved photovoltaic parameters.

  3. Polystyrene-Supported Acyclic Diaminocarbene Palladium Complexes in Sonogashira Cross-Coupling: Stability vs. Catalytic Activity

    Directory of Open Access Journals (Sweden)

    Vladimir N. Mikhaylov

    2018-04-01

    Full Text Available Two types of immobilized on the amino-functionalized polystyrene-supported acyclic diaminocarbene palladium complexes (ADC-PdII are investigated under Sonogashira cross-coupling conditions. Depending on substituents in the diaminocarbene fragment immobilized ADC-PdII, systems are found to have different catalytic activity and stability regarding Pd-leaching. PdII-diaminocarbenes possessing protons at both nitrogen atoms smoothly decompose into Pd0-containing species providing a catalytic “cocktail system” with high activity and ability to reuse within nine runs. Polymer-supported palladium (II complex bearing NBn–Ccarbene–NH-moiety exhibits greater stability while noticeably lower activity under Sonogashira cross-coupling. Four molecular ADC-PdII complexes are also synthesized and investigated with the aim of confirming proposed base-promoted pathway of ADC-PdII conversion through carbodiimide into an active Pd0 forms.

  4. PVP-Stabilized Palladium Nanoparticles in Silica as Effective Catalysts for Hydrogenation Reactions

    Directory of Open Access Journals (Sweden)

    Caroline Pires Ruas

    2013-01-01

    Full Text Available Palladium nanoparticles stabilized by poly (N-vinyl-2-pyrrolidone (PVP can be synthesized by corresponding Pd(acac2 (acac = acetylacetonate as precursor in methanol at 80°C for 2 h followed by reduction with NaBH4 and immobilized onto SiO2 prepared by sol-gel process under acidic conditions (HF or HCl. The PVP/Pd molar ratio is set to 6. The effect of the sol-gel catalyst on the silica morphology and texture and on Pd(0 content was investigated. The catalysts prepared (ca. 2% Pd(0/SiO2/HF and ca. 0,3% Pd(0/SiO2/HCl were characterized by TEM, FAAS, and SEM-EDS. Palladium nanoparticles supported in silica with a size 6.6 ± 1.4 nm were obtained. The catalytic activity was tested in hydrogenation of alkenes.

  5. Palladium polypyridyl complexes: synthesis, characterization, DNA interaction and biological activity on Leishmania (L.) mexicana

    Energy Technology Data Exchange (ETDEWEB)

    Navarro, Maribel [Instituto Venezolano de Investigaciones Cientificas, Caracas (Venezuela). Centro de Quimica; Betancourt, Adelmo [Universidad de Carabobo, Valencia (Venezuela). Facultad Experimental de Ciencia y Tecnologia. Dept. de Quimica; Hernandez, Clara [Universidad de Carabobo Sede Aragua, Maracay (Venezuela). Facultad de Ciencias de la Salud. Dept. de Ciencias Basicas; Marchan, Edgar [Universidad de Oriente, Cumana (Venezuela). Inst. de Investigaciones en Biomedicina y Ciencias Aplicadas. Nucleo de Sucre

    2008-07-01

    This paper describes the search for new potential chemotherapeutic agents based on transition metal complexes with planar ligands. In this study, palladium polypyridyl complexes were synthesized and characterized by elemental analysis, NMR, UV-VIS and IR spectroscopies. The interaction of the complexes with DNA was also investigated by spectroscopic methods. All metal-to-ligand charge transfer (MLCT) bands of the palladium polypyridyl complexes exhibited hypochromism and red shift in the presence of DNA. The binding constant and viscosity data suggested that the complexes [PdCl{sub 2}(phen)] and [PdCl{sub 2}(phendiamine)] interact with DNA by electrostatic forces. Additionally, these complexes induced an important leishmanistatic effect on L. (L.) mexicana promastigotes at the final concentration of 10 {mu}mol L{sup -1} in 48 h. (author)

  6. Studies on nickel (II and palladium (II complexes with some tetraazamacrocycles containing tellurium

    Directory of Open Access Journals (Sweden)

    Rathee Nitu

    2012-01-01

    Full Text Available The synthesis of 10-membered and 12-membered tellurium containing tetraazamacrocyclic complexes of divalent nickel and palladium by template condensation of diaryltellurium dichlorides, (aryl = p-hydroxyphenyl, 3-methyl-4-hydroxyphenyl, p-methoxyphenyl with 1,2-diaminoethane and 1,3-diaminopropane in the presence of metal dichloride is reported. The resulting complexes have been subjected to elemental analyses, magnetic measurements, electronic absorption, infra-red, and proton magnetic resonance spectral studies. The formation of proposed macrocyclic skeletons and their donor sites have been identified on the basis of spectral studies. Distorted octahedral structure for the nickel complexes in the solid state and squareplanar structure for the palladium complexes have been suggested.

  7. Effects of impurities on hydrogen permeability through palladium alloy membrane at comparatively high pressure and temperature

    International Nuclear Information System (INIS)

    Yoshida, Hiroshi; Konishi, Satoshi; Katsuta, Hiroji; Naruse, Yuji

    1982-02-01

    Palladium alloy membrane method is considered to be a useful technique for fusion reactor fuel purification process. To study the feasibility of this method, the effects of impurities on permeation characteristics of palladium alloy membrane were examined. Experiments were carried out at practical conditions: pressure; 120 - 1200 kPa, temperature; about 700 K. No poisoning effect on hydrogen permeability of commercial Pd-Ag (Au.Ru) alloy was observed for impurities such as NH 3 , CH 4 , CO, CO 2 , O 2 and N 2 , which were mixed with hyper-pure H 2 at low concentration level (10 - 10000 ppm). Deterioration occurred by contamination with oil vapor. However, regeneration of the membrane was easily performed by air baking followed by hydrogen reduction. Chemical reactions in the permeation cell were also examined. (author)

  8. Experiments on a ceramic electrolysis cell and a palladium diffuser at the tritium systems test assembly

    International Nuclear Information System (INIS)

    Konishi, Satoshi; Yoshida, Hiroshi; Ohno, Hideo; Naruse, Yuji; Coffin, D.O.; Walthers, C.R.; Binning, K.E.

    1985-01-01

    A ceramic electrolysis cell and a palladium diffuser are developed in Japan and is tested with tritium in Tritium Systems Test Assembly (TSTA) of the Los Alamos National Laboratory, in order to confirm the feasibility as possible upgrades for the fuel cleanup system (PCU). The ceramic electrolysis cell made of stabilized zirconia was operated at 630 0 C for an extended period with a mixture of 3% T 2 O in He carrier gas in the circulation system with oxidizing catalyst bed. The palladium diffuser was tested with circulated pure tritium gas at 280 0 C to verify the compatibility of the alloy with tritium, since the 3 He produced in the metal could cause a degradation. The isotopic effects were also measured for both devices

  9. A Palladium-Tin Modified Microband Electrode Array for Nitrate Determination

    Directory of Open Access Journals (Sweden)

    Yexiang Fu

    2015-09-01

    Full Text Available A microband electrode array modified with palladium-tin bimetallic composite has been developed for nitrate determination. The microband electrode array was fabricated by Micro Electro-Mechanical System (MEMS technique. Palladium and tin were electrodeposited successively on the electrode, forming a double-layer structure. The effect of the Pd-Sn composite was investigated and its enhancement of catalytic activity and lifetime was revealed. The Pd-Sn modified electrode showed good linearity (R2 = 0.998 from 1 mg/L to 20 mg/L for nitrate determination with a sensitivity of 398 μA/(mg∙L−1∙cm2. The electrode exhibited a satisfying analytical performance after 60 days of storage, indicating a long lifetime. Good repeatability was also displayed by the Pd-Sn modified electrodes. The results provided an option for nitrate determination in water.

  10. Palladium polypyridyl complexes: synthesis, characterization, DNA interaction and biological activity on Leishmania (L.) mexicana

    International Nuclear Information System (INIS)

    Navarro, Maribel; Betancourt, Adelmo; Hernandez, Clara; Marchan, Edgar

    2008-01-01

    This paper describes the search for new potential chemotherapeutic agents based on transition metal complexes with planar ligands. In this study, palladium polypyridyl complexes were synthesized and characterized by elemental analysis, NMR, UV-VIS and IR spectroscopies. The interaction of the complexes with DNA was also investigated by spectroscopic methods. All metal-to-ligand charge transfer (MLCT) bands of the palladium polypyridyl complexes exhibited hypochromism and red shift in the presence of DNA. The binding constant and viscosity data suggested that the complexes [PdCl 2 (phen)] and [PdCl 2 (phendiamine)] interact with DNA by electrostatic forces. Additionally, these complexes induced an important leishmanistatic effect on L. (L.) mexicana promastigotes at the final concentration of 10 μmol L -1 in 48 h. (author)

  11. Synthesis of heterocyclic compounds through palladium-catalyzed C-H cyclization processes.

    Science.gov (United States)

    Inamoto, Kiyofumi

    2013-01-01

    Herein, we describe our development of synthetic methods for heterocyclic compounds based on the palladium-catalyzed carbon-hydrogen bond (C-H) functionalization/intramolecular carbon-heteroatom (nitrogen or sulfur) bond formation process. By this C-H cyclization method, we efficiently prepared various N-heterocycles, including indazoles, indoles, and 2-quinolinones, as well as S-heterocycles such as benzothiazoles and benzo[b]thiophenes. Yields are typically good to high and good functional-group tolerance is observed for each process, thereby indicating that the method provides a novel, highly applicable synthetic route to the abovementioned biologically important heterocyclic frameworks. As an application of this approach, an auto-tandem-type, one-pot process involving the oxidative Heck reaction and subsequent C-H cyclization using cinnamamides and arylboronic acids as starting materials in the presence of a palladium catalyst was also developed for the rapid construction of the 2-quinolinone nucleus.

  12. Thermogravimetric determination of the enthalpy of astatine and radon adsorption on palladium surfaces

    International Nuclear Information System (INIS)

    Eichler, B.; Son Chun, K.

    1985-01-01

    In order to investigate the adsorption of astatine and radon on a palladium surface some on- and off-line thermochromatographic experiments were carried out with 210 At and 220 Rn tracers. The partial molar adsorption enthalpy for zero covering was found to be ΔH/sub a//sup 0, loc./(At) = -(15S +- 10) kJ mole -1 and ΔH/sub a//sup 0, mob./(Rn) = -(37 +- 4) kJ mole -1 . The results are compared with theoretical and experimental values for other elements of the sixth period. The adsorption behaviour of At is in conformity with that of the p-metals on a palladium surface. (author)

  13. Palladium-catalyzed aryl C-H olefination with unactivated, aliphatic alkenes.

    Science.gov (United States)

    Deb, Arghya; Bag, Sukdev; Kancherla, Rajesh; Maiti, Debabrata

    2014-10-01

    Palladium-catalyzed coupling between aryl halides and alkenes (Mizoroki-Heck reaction) is one of the most popular reactions for synthesizing complex organic molecules. The limited availability, problematic synthesis, and higher cost of aryl halide precursors (or their equivalents) have encouraged exploration of direct olefination of aryl carbon-hydrogen (C-H) bonds (Fujiwara-Moritani reaction). Despite significant progress, the restricted substrate scope, in particular noncompliance of unactivated aliphatic olefins, has discouraged the use of this greener alternative. Overcoming this serious limitation, we report here a palladium-catalyzed chelation-assisted ortho C-H bond olefination of phenylacetic acid derivatives with unactivated, aliphatic alkenes in good to excellent yields with high regio- and stereoselectivities. The versatility of this operationally simple method has been demonstrated through drug diversification and sequential C-H olefination for synthesizing divinylbenzene derivatives.

  14. Methanofullerene-Based Palladium Bis(amino)aryl Complexes and Applications in Lewis Acid Catalysis

    NARCIS (Netherlands)

    Koten, G. van; Meijer, M.D.; Ronde, N.; Vogt, D.; Klink, G.P.M. van

    2001-01-01

    Synthetic routes have been developed for the attachment of palladium(II) bis(amino)aryl (NCN or C6H2{CH2NMe2}2-2,6)- complexes to C60. Using diazo and Bingel addition reactions, various methanofullerene NCN-SiMe3 compounds (C60-L-NCN-SiMe3, L = C(Me), C(CO2Et)CO2CH2, and C(Me)C6H4CC) have been

  15. Sulphur containing novel extractants for extraction-separation of palladium (II)

    International Nuclear Information System (INIS)

    Shukla, J.P.; Sawant, S.R.; Anil Kumar; Singh, R.K.

    1995-01-01

    Extraction performance of palladium (II) by sulphur containing extragents has unequivocally established their strong extraction ability toward this thiophilic soft metal. Hence a comprehensive investigative study was initiated by us to examine selective reversible extraction-separation of trace and macro amounts of palladium (II) from both aqueous nitric acid as well as hydrochloric acid media into 1,2-dichloroethane by 1,10-dithia-18 crown-6 (1,10-DT18C6), S 6 -pentano-36 (S 6 -P-36) and bis (2-ethylhexyl) sulphoxide (BESO) dissolved in toluene. From the study of aqueous phase acidity, reagent concentration, period of equilibration, diluent, strippant and diverse ions, conditions are established from its quantitative and reversible extraction. Recovery of Pd(II) from loaded thiacrown and sulphoxide phase is easily accomplished by using sodium thiocyanate, ammonium thiocyanate, thiourea, sodium thiosulphate and mixture of (2M Na 2 CO 3 + 0.5 NH 4 OH) (only for BESO) as the strippants. The lack of interference from even appreciable amounts of contaminants like 137 Cs, 106 Ru, 233 U and 239 Pu may be considered as one of the outstanding advantages of the method. Application of these extractants has been successfully tested for the recovery of palladium from high active waste matrix. The extracted complex from both the thiacrowns has been characterized by elemental analyses and UV-Visible spectra, confirmed to be PdA 2 .T (A = NO - 3 , Cl - ) from dilute (pH ∼ 2) acid solutions while composition of organic species with palladium for the sulphoxide, has also been confirmed to be disolvate of the type Pd(NO 3 ) 2 .2BESO. (author). 52 refs., 6 tabs., 6 figs

  16. Neutron measurements in deuterated palladium cathodes subjected to pulsed electrolytic currents

    International Nuclear Information System (INIS)

    Granada, J.R.; Mayer, R.E.; Guido, G.; Florido, P.C.; Patino, N.E.; Gillette, V.H.; Sobehart, L.; Gomez, S.; Larreteguy, A.; Universidad Nacional de Cuyo, San Carlos de Bariloche

    1989-01-01

    We report on neutron measurements performed on electrolytic cells using a high efficiency (22%) detection system in combination with a procedure involving a non-stationary current through the cell's circuit. Under these conditions, neutron production was observed in cells containing LiH dissolved in heavy water with a Palladium cathode. Characteristic patterns showing one or two bumps were obtained in a repeatable fashion, depending on the previous charging history of the cathode. (orig.)

  17. Palladium-catalyzed, asymmetric Baeyer–Villiger oxidation of prochiral cyclobutanones with PHOX ligands

    KAUST Repository

    Petersen, Kimberly S.

    2011-06-01

    Described in this report is a general method for the conversion of prochiral 3-substituted cyclobutanones to enantioenriched γ-lactones through a palladium-catalyzed Baeyer-Villiger oxidation using phosphinooxazoline ligands in up to 99% yield and 81% ee. Lactones of enantiopurity ≥93% could be obtained through a single recrystallization step. Importantly, 3,3-disubtituted cyclobutanones produced enantioenriched lactones containing a β-quaternary center. © 2011 Elsevier Ltd. All rights reserved.

  18. Ester versus polyketone formation in the palladium-diphosphine catalyzed carbonylation of ethene.

    Science.gov (United States)

    Zuidema, Erik; Bo, Carles; van Leeuwen, Piet W N M

    2007-04-04

    The origin of the chemoselectivity of palladium catalysts containing bidentate phosphine ligands toward either methoxycarbonylation of ethene or the copolymerization of ethene and carbon monoxide was investigated using density functional theory based calculations. For a palladium catalyst containing the electron-donating bis(dimethylphosphino)ethane (dmpe) ligand, the rate determining step for chain propagation is shown to be the insertion of ethene into the metal-acyl bond. The high barrier for chain propagation is attributed to the low stability of the ethene intermediate, (dmpe)Pd(ethene)(C(O)CH3). For the competing methanolysis process, the most likely pathway involves the formation of (dmpe)Pd(CH3OH)(C(O)CH3) via dissociative ligand exchange, followed by a solvent mediated proton-transfer/reductive- elimination process. The overall barrier for this process is higher than the barrier for ethene insertion into the palladium-acetyl bond, in line with the experimentally observed preference of this type of catalyst toward the formation of polyketone. Electronic bite angle effects on the rates of ethene insertion and ethanoyl methanolysis were evaluated using four electronically and sterically related ligands (Me)2P(CH2)nP(Me)2 (n = 1-4). Steric effects were studied for larger tert-butyl substituted ligands using a QM/MM methodology. The results show that ethene coordination to the metal center and subsequent insertion into the palladium-ethanoyl bond are disfavored by the addition of steric bulk around the metal center. Key intermediates in the methanolysis mechanism, on the other hand, are stabilized because of electronic effects caused by increasing the bite angle of the diphosphine ligand. The combined effects explain successfully which ligands give polymer and which ones give methyl propionate as the major products of the reaction.

  19. Polymer producing palladium complexes of unidentate phosphines in the methoxycarbonylation of ethene.

    Science.gov (United States)

    Smith, Graeme; Vautravers, Nicolas R; Cole-Hamilton, David J

    2009-02-07

    A wide range of unidentate phosphines have been studied as ligands for the palladium-catalysed methoxycarbonylation of ethene in the presence of methanesulfonic acid using methanol as the solvent. At high phosphine to Pd ratios, methyl propanoate is formed at a low rate. However, at P-Pd ratios of 4 : 1, some unidentate phosphines promote the formation of polyketone with moderate rates. Analysis of all the phosphines shows that good electron donating power, combined with small size, favours polyketone formation.

  20. Continuous flow hydrogenation using polysilane-supported palladium/alumina hybrid catalysts

    Directory of Open Access Journals (Sweden)

    Shū Kobayashi

    2011-05-01

    Full Text Available Continuous flow systems for hydrogenation using polysilane-supported palladium/alumina (Pd/(PSi–Al2O3 hybrid catalysts were developed. Our original Pd/(PSi–Al2O3 catalysts were used successfully in these systems and the hydrogenation of unsaturated C–C bonds and a nitro group, deprotection of a carbobenzyloxy (Cbz group, and a dehalogenation reaction proceeded smoothly. The catalyst retained high activity for at least 8 h under neat conditions.