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Sample records for palladium borides

  1. Kinetics of borided gear steels

    Indian Academy of Sciences (India)

    ration (FeB + Fe2B) due to the high intensity stress states generally situated at the ... performed molten salt boriding of AISI D2 steel with borax (Na2B4O7) as the ... the borided layer thickness; silicon, chromium and aluminium have moderate.

  2. Nanodispersed boriding of titanium alloy

    International Nuclear Information System (INIS)

    Kostyuk, K.O.; Kostyuk, V.O.

    2015-01-01

    The problem of improving the operational reliability of machines is becoming increasingly important due to the increased mechanical, thermal and other loads on the details. There are many surface hardening methods for machines parts which breakdown begins with surface corruption. The most promising methods are chemical-thermal treatment. The aim of this work is to study the impact of boriding on the structure and properties of titanium alloy. Materials and Methods: The material of this study is VT3-1 titanium alloy. The boriding were conducted using nanodispersed powder blend based on boric substances. It is established that boriding of paste compounds allows obtaining the surface hardness within 30 - 29 GPa and with declining to 27- 26 GPa in layer to the transition zone (with total thickness up to 110 μm) owing to changes of the layer phase composition where T 2 B, TiB, TiB 2 titanium borides are formed. The increasing of chemical-thermal treatment time from 15 minutes to 2 hours leads to thickening of the borated layer (30 - 110 μm) and transition zone (30 - 190 μm). Due to usage of nanodispersed boric powder, the boriding duration is decreasing in 2 - 3 times. This allows saving time and electric energy. The developed optimal mode of boriding the VT3-1 titanium alloy allows obtaining the required operational characteristics and to combine the saturation of the surface layer with atomic boron and hardening

  3. Superconductivity in borides and carbides

    International Nuclear Information System (INIS)

    Muranaka, Takahiro

    2007-01-01

    It was thought that intermetallic superconductors do not exhibit superconductivity at temperatures over 30 K because of the Bardeen-Cooper-Schrieffer (BCS) limit; therefore, researchers have been interested in high-T c cuprates. Our group discovered high-T c superconductivity in MgB 2 at 39 K in 2001. This discovery has initiated a substantial interest in the potential of high-T c superconductivity in intermetallic compounds that include 'light' elements (borides, carbides, etc.). (author)

  4. Boride particles in a powder metallurgy superalloy

    Energy Technology Data Exchange (ETDEWEB)

    Witt, M C; Charles, J A

    1985-12-01

    Using optical and electron metallography, the composition, morphology, and distribution of M/sub 3/B/sub 2/ borides in as-hipped (hot isostatically pressed) samples of the powder metallurgy superalloy Nimonic AP1 have been determined. Two types of boride are present depending on the HIP temperature. Hipping below the boride solvus results in low-aspect ratio particles, distributed both inter- and intragranularly. Hipping above the boride solvus produces high-aspect ratio particles which are exclusively intergranular. A small difference in both lattice parameter and composition has been measured. Electron energy loss spectroscopy of the particles has confirmed the presence of boron, and laser ion-induced mass analysis has indicated a low carbon level. The higher susceptibility to edge cracking during forging of material hipped above the boride solvus is related to the boride morphology. Studies of the subsequent recrystallization of the forged samples have indicated that necklace formation is neither inhibited nor accelerated by the presence of grain boundary borides. 18 references.

  5. New superhard boride composite materials. Part 1; Neue superharte Borid-Verbundwerkstoffe. Teil 1

    Energy Technology Data Exchange (ETDEWEB)

    Zachariev, Z.

    2001-07-01

    Contents: Investigations of diffusion coupling between steels and borides (ZrB{sub 2}, TiB{sub 2}, CrB, MoB); Diffusion saturation of armco iron inpowdered borides; Gaseous phase transport intensivation of the transition metal using suitable activators (vapour phase process); boron circonisation of steels; High-temperature oxidation studies on boride composite coatings on iron and steel; Corrosion resistance of boride coated iron base composites; Superhard boride coatings on hard metals and on cermet plates with reduced tungsten contents. [German] Dieser Beitrag ist wie folgt gegliedert: Untersuchung der Diffusionskopplung zwischen Staehlen und den Boriden (ZrB{sub 2}, TiB{sub 2}, CrB, MoB); Diffusionssaettigung von Armcoeisen in Pulverboride; Gasphasentransport-Intensivierung des Uebergangsmetalls mittels geeigneter Akivatoren (vapour phase process); Borzirkonieren von Staehlen; Hochtemperaturoxidationuntersuchungen von Borid-Composite-Schichten auf Eisen und Stahl; Korrosionsbestaendigkeit der boridbeschichteten Verbundwerkstoffe auf Eisenbasis; Superharte Boridbeschichtungen auf Hartmetall und auf Metallkeramikplatten mit reduziertem Wolframgehalt.

  6. Characterization of AISI 4140 borided steels

    International Nuclear Information System (INIS)

    Campos-Silva, I.; Ortiz-Dominguez, M.; Lopez-Perrusquia, N.; Meneses-Amador, A.; Escobar-Galindo, R.; Martinez-Trinidad, J.

    2010-01-01

    The present study characterizes the surface of AISI 4140 steels exposed to the paste-boriding process. The formation of Fe 2 B hard coatings was obtained in the temperature range 1123-1273 K with different exposure times, using a 4 mm thick layer of boron carbide paste over the material surface. First, the growth kinetics of boride layers at the surface of AISI 4140 steels was evaluated. Second, the presence and distribution of alloying elements on the Fe 2 B phase was measured using the Glow Discharge Optical Emission Spectrometry (GDOES) technique. Further, thermal residual stresses produced on the borided phase were evaluated by X-ray diffraction (XRD) analysis. The fracture toughness of the iron boride layer of the AISI 4140 borided steels was estimated using a Vickers microindentation induced-fracture testing at a constant distance of 25 μm from the surface. The force criterion of fracture toughness was determined from the extent of brittle cracks, both parallel and perpendicular to the surface, originating at the tips of an indenter impression. The fracture toughness values obtained by the Palmqvist crack model are expressed in the form K C (π/2) > K C > K C (0) for the different applied loads and experimental parameters of the boriding process.

  7. Characterization of AISI 4140 borided steels

    Science.gov (United States)

    Campos-Silva, I.; Ortiz-Domínguez, M.; López-Perrusquia, N.; Meneses-Amador, A.; Escobar-Galindo, R.; Martínez-Trinidad, J.

    2010-02-01

    The present study characterizes the surface of AISI 4140 steels exposed to the paste-boriding process. The formation of Fe 2B hard coatings was obtained in the temperature range 1123-1273 K with different exposure times, using a 4 mm thick layer of boron carbide paste over the material surface. First, the growth kinetics of boride layers at the surface of AISI 4140 steels was evaluated. Second, the presence and distribution of alloying elements on the Fe 2B phase was measured using the Glow Discharge Optical Emission Spectrometry (GDOES) technique. Further, thermal residual stresses produced on the borided phase were evaluated by X-ray diffraction (XRD) analysis. The fracture toughness of the iron boride layer of the AISI 4140 borided steels was estimated using a Vickers microindentation induced-fracture testing at a constant distance of 25 μm from the surface. The force criterion of fracture toughness was determined from the extent of brittle cracks, both parallel and perpendicular to the surface, originating at the tips of an indenter impression. The fracture toughness values obtained by the Palmqvist crack model are expressed in the form KC( π/2) > KC > KC(0) for the different applied loads and experimental parameters of the boriding process.

  8. Characterization of AISI 4140 borided steels

    Energy Technology Data Exchange (ETDEWEB)

    Campos-Silva, I., E-mail: icampos@ipn.mx [Instituto Politecnico Nacional, Grupo Ingenieria de Superficies, SEPI-ESIME U.P. Adolfo Lopez Mateos, Zacatenco, Mexico D.F., 07738 (Mexico); Ortiz-Dominguez, M.; Lopez-Perrusquia, N.; Meneses-Amador, A. [Instituto Politecnico Nacional, Grupo Ingenieria de Superficies, SEPI-ESIME U.P. Adolfo Lopez Mateos, Zacatenco, Mexico D.F., 07738 (Mexico); Escobar-Galindo, R. [Instituto de Ciencia de Materiales de Madrid (CSIC), E-28049 Cantoblanco, Madrid (Spain); Martinez-Trinidad, J. [Instituto Politecnico Nacional, Grupo Ingenieria de Superficies, SEPI-ESIME U.P. Adolfo Lopez Mateos, Zacatenco, Mexico D.F., 07738 (Mexico)

    2010-02-01

    The present study characterizes the surface of AISI 4140 steels exposed to the paste-boriding process. The formation of Fe{sub 2}B hard coatings was obtained in the temperature range 1123-1273 K with different exposure times, using a 4 mm thick layer of boron carbide paste over the material surface. First, the growth kinetics of boride layers at the surface of AISI 4140 steels was evaluated. Second, the presence and distribution of alloying elements on the Fe{sub 2}B phase was measured using the Glow Discharge Optical Emission Spectrometry (GDOES) technique. Further, thermal residual stresses produced on the borided phase were evaluated by X-ray diffraction (XRD) analysis. The fracture toughness of the iron boride layer of the AISI 4140 borided steels was estimated using a Vickers microindentation induced-fracture testing at a constant distance of 25 {mu}m from the surface. The force criterion of fracture toughness was determined from the extent of brittle cracks, both parallel and perpendicular to the surface, originating at the tips of an indenter impression. The fracture toughness values obtained by the Palmqvist crack model are expressed in the form K{sub C}({pi}/2) > K{sub C} > K{sub C}(0) for the different applied loads and experimental parameters of the boriding process.

  9. Ultra-fast boriding of metal surfaces for improved properties

    Science.gov (United States)

    Timur, Servet; Kartal, Guldem; Eryilmaz, Osman L.; Erdemir, Ali

    2015-02-10

    A method of ultra-fast boriding of a metal surface. The method includes the step of providing a metal component, providing a molten electrolyte having boron components therein, providing an electrochemical boriding system including an induction furnace, operating the induction furnace to establish a high temperature for the molten electrolyte, and boriding the metal surface to achieve a boride layer on the metal surface.

  10. Kinetics of electrochemical boriding of low carbon steel

    International Nuclear Information System (INIS)

    Kartal, G.; Eryilmaz, O.L.; Krumdick, G.; Erdemir, A.; Timur, S.

    2011-01-01

    In this study, the growth kinetics of the boride layers forming on low carbon steel substrates was investigated during electrochemical boriding which was performed at a constant current density of 200 mA/cm 2 in a borax based electrolyte at temperatures ranging from 1123 K to 1273 K for periods of 5-120 min. After boriding, the presence of both FeB and Fe 2 B phases were confirmed by the X-ray diffraction method. Cross-sectional microscopy revealed a very dense and thick morphology for both boride phases. Micro hardness testing of the borided steel samples showed a significant increase in the hardness of the borided surfaces (i.e., up to (1700 ± 200) HV), while the hardness of un-borided steel samples was approximately (200 ± 20) HV. Systematic studies over a wide range of boriding time and temperature confirmed that the rate of the boride layer formation is strongly dependent on boriding duration and has a parabolic character. The activation energy of boride layer growth for electrochemical boriding was determined as (172.75 ± 8.6) kJ/mol.

  11. Boriding with boron carbide base pastes

    International Nuclear Information System (INIS)

    Aliev, A.A.

    1978-01-01

    The aim of this paper is to develop an advanced technique of boriding using pastes under the conditions of furnace heating. The research is carried out on flat specimens of 20 and U8 steels pre-annealed in vacuum. B 4 C base pastes were used as saturating media, and the glue prepared by dissolving of nitrocellulose in the mixture of butylacetate and acetone was used as a bond. Measured was the depth of diffusion layers, produced on the 20 and u8 steels after boriding with the pastes under different temperatures and saturation times. The results of metallographic analysis show that borided layers have a specific needle-like structure. The surface of the specimens is clean and free from any paste residues and traces of partial melting

  12. Production and properties of boride powders

    International Nuclear Information System (INIS)

    Klinskaya, N.A.; Koroleva, E.B.; Petrunichev, V.A.

    1990-01-01

    Results of plasma metallization of boride powders 40-80 μ diam. are presented. Peculiarities of changes of granulometric powder composition and of metallic cover on refractory cores were investigated. There are shown size- and compositional cores effects on metallization level of poders and on cover structure

  13. Preparation of single phase molybdenum boride

    International Nuclear Information System (INIS)

    Camurlu, Hasan Erdem

    2011-01-01

    Highlights: → Formation of Mo and a mixture of molybdenum boride phases take place in preparation of molybdenum borides. → It is intricate to prepare single phase molybdenum borides. → Formation of single phase MoB from MoO 3 + B 2 O 3 + Mg mixtures has not been reported previously. → Single phase MoB was successfully prepared through a combination of mechanochemical synthesis and annealing process. - Abstract: The formation of MoB through volume combustion synthesis (VCS), and through mechanochemical synthesis (MCS) followed by annealing has been investigated. MoO 3 , B 2 O 3 and Mg were used as reactants while MgO and NaCl were introduced as diluents. Products were leached in dilute HCl solution and were subjected to X-ray diffraction (XRD) analysis and scanning electron microscopy (SEM) examinations. Mo was the major phase component in the VCS products under all the experimental conditions. Mo 2 B, MoB, MoB 2 and Mo 2 B 5 were found as minor phases. Products of MCS contained a mixture of Mo 2 B, MoB, MoB 2 and Mo. After annealing the MCS product at 1400 deg. C for 3 h, single phase α-MoB was obtained.

  14. Growth kinetics of boride coatings formed at the surface AISI M2 during dehydrated paste pack boriding

    Energy Technology Data Exchange (ETDEWEB)

    Doñu Ruiz, M.A., E-mail: mdonur0800@alumno.ipn.mx [Universidad Politécnica del Valle de México UPVM, Grupo Ciencia e Ingeniería de Materiales, Av. Mexiquense S/N Esquina Av. Universidad Politécnica, Col Villa Esmeralda, 54910 Tultitlan (Mexico); López Perrusquia, N.; Sánchez Huerta, D. [Universidad Politécnica del Valle de México UPVM, Grupo Ciencia e Ingeniería de Materiales, Av. Mexiquense S/N Esquina Av. Universidad Politécnica, Col Villa Esmeralda, 54910 Tultitlan (Mexico); Torres San Miguel, C.R.; Urriolagoitia Calderón, G.M. [Instituto Politécnico Nacional, SEPI-ESIME, Unidad Profesional Adolfo López Mateos Zacatenco, Edificio 5, 2do. Piso, Col. Lindavista, CP 07738 México, D.F. (Mexico); Cerillo Moreno, E.A. [Universidad Politécnica del Valle de México UPVM, Grupo Ciencia e Ingeniería de Materiales, Av. Mexiquense S/N Esquina Av. Universidad Politécnica, Col Villa Esmeralda, 54910 Tultitlan (Mexico); Cortes Suarez, J.V. [Univerisdad Autónoma Metropolitana Unidad Azcapotzalco, Av. San Pablo 180 Azcapotzalco 02200, Área de Ciencia de los Materiales, México, D.F. (Mexico)

    2015-12-01

    The growth kinetics of the boride coatings (FeB and Fe{sub 2}B) at the surface of AISI M2 high speed steels were studied in this work. Boriding thermochemical treatment was carried out by dehydrated paste pack at three different temperatures 1173, 1223, and 1273 K and four exposure times 1, 3, 5, and 7 h, respectively. The presence of FeB and Fe{sub 2}B phases was identified by scanning electron microscopy with energy dispersive spectroscopy (SEM-EDS) and X-ray diffraction method. In order to obtain the boron diffusion coefficients at the FeB/Fe{sub 2}B boride coatings, a mathematical model based on the mass balance at the growing interfaces was proposed under certain assumptions. Likewise the parabolic growth constants and the boride incubation time were established as a function of the parameters η (T) and ε (T). The activation energy values estimated for the FeB and Fe{sub 2}B layers were 233.42 and 211.89 kJ mol{sup −1} respectively. A good agreement was obtained between the simulated values of boride layer thicknesses and the experimental results. Finally, empirical relationships of boride coating thickness as a function of boriding temperature and time are presented. - Highlights: • Formed boride coatings at the surface of AISI M2 high speed steels by new process dehydrated paste pack boriding. • The model was based on the mass balance equation at the FeB/Fe{sub 2}B and Fe{sub 2}B/Fe interfaces by considering the boride incubation time. • A good agreement was obtained between the simulated values of boride layers coatings and the experimental results.

  15. Preparation of iron boride layers from the gas phase

    International Nuclear Information System (INIS)

    Marx, G.; Plaenitz, H.; Treffer, G.; Koenig, H.; Altenburger, S.

    1980-01-01

    Coating of Armco iron, steel-C100W1, and steel-100Cr6 with borides by decomposition of boron tribromide on the surface of the specimens is described. The experiments were carried out in a laboratory apparatus at temperatures between 923 and 1223 K. The dependence of the thickness of the boride layers on time and temperature is presented in graphs

  16. Low-temperature heat capacity of molybdenum borides

    International Nuclear Information System (INIS)

    Bolgar, A.S.; Klinder, A.V.; Novoseletskaya, L.M.; Turov, V.P.; Klochkov, L.A.; Lyashchenko, A.B.

    1988-01-01

    Heat capacity of molybdenum borides Mo 2 B, MoB, Mo 2 B 5 is studied for the first time in the 60-300 K range using the adiabatic method. Standard (at 298.15 K) thermodynamic functions (enthalpy, heat capacity, entropy, reduced Gibbs energy) of molybdenum borides are calculated

  17. Pulsed nanocrystalline plasma electrolytic boriding as a novel ...

    Indian Academy of Sciences (India)

    Potentiodynamic polarization and electrochemical impedance spectroscopy were employed to test borided CP-Ti, treated by a relatively new method called pulsed plasma electrolytic boriding. The results show excellent corrosion resistance for modified CP-Ti. The effect of frequency and duty cycle of pulsed current was ...

  18. Pulsed nanocrystalline plasma electrolytic boriding as a novel ...

    Indian Academy of Sciences (India)

    WINTEC

    borided CP-Ti, treated by a relatively new method called pulsed plasma electrolytic boriding. The results ... ratio, high stiffness and strength (Donachie 2000; Lutjer- ing and Albrecht ..... both direct current and a.c. techniques. Although the main ...

  19. Investigation of diffusion kinetics of plasma paste borided AISI 8620 ...

    Indian Academy of Sciences (India)

    Henríquez 2009), plasma boriding (Rodríguez et al 1999) and plasma paste boriding (Gunes et al 2011; Yoon et al ... symmetric geometry with monochromatized radiation (Cu Kα, λ = 0.15418 nm). ..... cate the degree of reliability of the predicted results, when compared with that of the experiments. ... low alloy steels. Surf.

  20. Fracture toughness of borides formed on boronized ductile iron

    International Nuclear Information System (INIS)

    Sen, Ugur; Sen, Saduman; Koksal, Sakip; Yilmaz, Fevzi

    2005-01-01

    In this study, fracture toughness properties of boronized ductile iron were investigated. Boronizing was realized in a salt bath consisting of borax, boric acid and ferro-silicon. Boronizing heat treatment was carried out between 850 and 950 deg. C under the atmospheric pressure for 2-8 h. Borides e.g. FeB, Fe 2 B formed on ductile iron was verified by X-ray diffraction (XRD) analysis, SEM and optical microscope. Experimental results revealed that longer boronizing time resulted in thicker boride layers. Optical microscope cross-sectional observation of borided layers showed dentricular morphology. Both microhardness and fracture toughness of borided surfaces were measured via Vickers indenter. The harnesses of borides formed on the ductile iron were in the range of 1160-2140 HV 0.1 and fracture toughness were in the range of 2.19-4.47 MPa m 1/2 depending on boronizing time and temperature

  1. Surface oxidation phenomena of boride coatings grown on iron

    International Nuclear Information System (INIS)

    Carbucicchio, M.; Palombarini, G.; Sambogna, G.

    1992-01-01

    Very hard boride coatings are grown on various metals using thermochemical as well as chemical vapour deposition techniques. In this way many surface properties, and in particular the wear resistance, can be considerably improved. Usually, also the corrosion behaviour of the treated components is important. In particular, oxidizing atmospheres are involved in many applications where, therefore, coating-environment interactions can play a relevant role. In a previous work, the early stages of the oxidation of iron borides were studied by treating single phase compacted powders in flowing oxygen at low temperatures (300-450deg C). In the present paper, the attention is addressed to the oxidation of both single phase and polyphase boride coatings thermochemically grown on iron. The single phase boride coatings were constituted by Fe 2 B, while the polyphase coatings were constituted by an inner Fe 2 B layer and an outer FeB-base layer. All the boride layers displayed strong (002) preferred crystallographic orientations. (orig.)

  2. Hardness of carbides, nitrides, and borides

    International Nuclear Information System (INIS)

    Schroeter, W.

    1981-01-01

    Intermetallic compounds of metals with non-metals such as C, N, and B show different hardness. Wagner's interaction parameter characterizes manner and extent of the interaction between the atoms of the substance dissolved and the additional elements in metallic mixed phases. An attempt has been made to correlate the hardness of carbides, nitrides, and borides (data taken from literature) with certain interaction parameters and associated thermodynamic quantities (ΔH, ΔG). For some metals of periods 4, 5, and 6 corresponding relations were found between microhardness, interaction parameters, heat of formation, and atomic number

  3. Magnesium Aluminum Borides as Explosive Materials

    Science.gov (United States)

    2011-12-20

    pestle and screened -325 mesh to remove the filter paper. However, some of the filter paper remained in this powder. Table 13 Compositions of...Property of Si-B System Ceramics,” J. Japan Soc. Pow. and Pow. Met., 41[11] 1299-1303 (1994). 53. H. Nakamura, K. Murata, T. Anan, and Y. Hara...Oxidation of Zirconium Borides,” J. Japan Explosives Society, 55[4] 142-146 (1994). 54. M. Woerle, R.Nesper, G. Mair, M. Schwarz, and H. G. von Schnering

  4. Platinum boride nanowires: Synthesis and characterization

    International Nuclear Information System (INIS)

    Ding Zhanhui; Qiu Lixia; Zhang Jian; Yao Bin; Cui Tian; Guan Weiming; Zheng Weitao; Wang Wenquan; Zhao Xudong; Liu Xiaoyang

    2012-01-01

    Highlights: ► Platinum boride nanowires have been synthesized via the direct current arc discharge method. ► XRD, TEM and SAED indicate that the nanowires are single-crystal PtB. ► Two broad photoluminescence emission peaks at about 586 nm and 626 nm have been observed in the PL spectroscopy of PtB nanowires. - Abstract: Platinum boride (PtB) nanowires have been successfully fabricated with direct current arc discharge method using a milled mixture of platinum (Pt) and boron nitride (BN) powders. X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) were used to characterize the compositions, morphology, and structures of the samples. The results show that PtB nanowires are 30–50 nm thick and 20–30 μm long. TEM and selected area electron diffraction (SAED) patterns identify that the PtB nanowires are single-crystalline in nature. A growth mechanism based on vapor–liquid–solid (VLS) process is proposed for the formation of nanowires.

  5. Electrochemical boriding and characterization of AISI D2 tool steel

    International Nuclear Information System (INIS)

    Sista, V.; Kahvecioglu, O.; Eryilmaz, O.L.; Erdemir, A.; Timur, S.

    2011-01-01

    D2 is an air-hardening tool steel and due to its high chromium content provides very good protection against wear and oxidation, especially at elevated temperatures. Boriding of D2 steel can further enhance its surface mechanical and tribological properties. Unfortunately, it has been very difficult to achieve a very dense and uniformly thick boride layers on D2 steel using traditional boriding processes. In an attempt to overcome such a deficiency, we explored the suitability and potential usefulness of electrochemical boriding for achieving thick and hard boride layers on this tool steel in a molten borax electrolyte at 850, 900, 950 and 1000 °C for durations ranging from 15 min to 1 h. The microstructural characterization and phase analysis of the resultant boride layers were performed using optical, scanning electron microscopy and X-ray diffraction methods. Our studies have confirmed that a single phase Fe 2 B layer or a composite layer consisting of FeB + Fe 2 B is feasible on the surface of D2 steel depending on the length of boriding time. The boride layers formed after shorter durations (i.e., 15 min) mainly consisted of Fe 2 B phase and was about 30 μm thick. The thickness of the layer formed in 60 min was about 60 μm and composed mainly of FeB and Fe 2 B. The cross sectional micro-hardness values of the boride layers varied between 14 and 22 GPa, depending on the phase composition.

  6. 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.

  7. Borides of the group 1 metals of the periodic system

    International Nuclear Information System (INIS)

    Samsonov, G.V.; Serebryakova, T.I.; Neronov, V.A.

    1975-01-01

    The borides of alkali metals (lithium, sodium, potassium) and the metals of a copper subgroup (copper, silver, gold) are described. Consideration is given to the crystalline structure and state diagrams of the metal systems within the first group of the Periodic Table with boron. Existence, formation conditions and physico-chemical properties of binary boride phases are characterized. Conclusion is made as to the absence of interaction between boron and silver. Information on the interaction between gold and boron is scanty and conflicting. Methods are described suitable for the production of the borides of the metals within the first group of the Periodic Table [ru

  8. Properties of boride-added powder metallurgy magnesium alloys

    Science.gov (United States)

    Tanaka, Atsushi; Yoshimura, Syota; Fujima, Takuya; Takagi, Ken-ichi

    2009-06-01

    Magnesium alloys with metallic borides, magnesium diboride (MgB2) or aluminum diboride (AlB2), were investigated regarding their mechanical properties, transverse rupture strength (TRS) and micro Vickers hardness (HV). The alloys were made from pure Mg, Al and B powders by mechanical alloying and hot pressing to have boride content of between 2.0 and 20 vol%. The alloy with AlB2 exhibited an obvious improvement of HV around a boride content of 6 vol% though the other alloy, with MgB2, did not. TRS showed moderate maxima around the same boride content region for the both alloys. X-ray diffraction measurements indicated an intermetallic compound, Mg17Al12, formed in the alloy with AlB2, which was consistent with its higher hardness.

  9. Properties of boride-added powder metallurgy magnesium alloys

    Energy Technology Data Exchange (ETDEWEB)

    Tanaka, Atsushi; Yoshimura, Syota; Fujima, Takuya; Takagi, Ken-ichi [Department of Mechanical Engineering, Tokyo City University 1-28-1 Tamazutsumi, Setagaya, Tokyo 158-8557 (Japan)], E-mail: ktakagi@tcu.ac.jp

    2009-06-01

    Magnesium alloys with metallic borides, magnesium diboride (MgB{sub 2}) or aluminum diboride (AlB{sub 2}), were investigated regarding their mechanical properties, transverse rupture strength (TRS) and micro Vickers hardness (HV). The alloys were made from pure Mg, Al and B powders by mechanical alloying and hot pressing to have boride content of between 2.0 and 20 vol%. The alloy with AlB{sub 2} exhibited an obvious improvement of HV around a boride content of 6 vol% though the other alloy, with MgB{sub 2}, did not. TRS showed moderate maxima around the same boride content region for the both alloys. X-ray diffraction measurements indicated an intermetallic compound, Mg{sub 17}Al{sub 12}, formed in the alloy with AlB{sub 2}, which was consistent with its higher hardness.

  10. Properties of boride-added powder metallurgy magnesium alloys

    International Nuclear Information System (INIS)

    Tanaka, Atsushi; Yoshimura, Syota; Fujima, Takuya; Takagi, Ken-ichi

    2009-01-01

    Magnesium alloys with metallic borides, magnesium diboride (MgB 2 ) or aluminum diboride (AlB 2 ), were investigated regarding their mechanical properties, transverse rupture strength (TRS) and micro Vickers hardness (HV). The alloys were made from pure Mg, Al and B powders by mechanical alloying and hot pressing to have boride content of between 2.0 and 20 vol%. The alloy with AlB 2 exhibited an obvious improvement of HV around a boride content of 6 vol% though the other alloy, with MgB 2 , did not. TRS showed moderate maxima around the same boride content region for the both alloys. X-ray diffraction measurements indicated an intermetallic compound, Mg 17 Al 12 , formed in the alloy with AlB 2 , which was consistent with its higher hardness.

  11. Tetragonal ternary borides: superconductivity, ferromagnetism and the role of scandium

    International Nuclear Information System (INIS)

    Matthias, B.T.; Patel, C.K.N.; Barz, H.; Corenzwit, E.; Vandenberg, J.M.

    1978-01-01

    The authors report and discuss two discoveries made while studying the condensation phenomena of ternary rhodium borides, MRh 4 B 4 . M is generally a trivalent transition metal, usually a rare earth element RE. An exception is scandium which by itself does not form an isomorphous boride, but in combination with many other elements will do just that. A suprising correlation between ferromagnetic and superconducting transition temperatures has been found. (Auth.)

  12. Structure, microstructure and residual stresses in borided steels

    Czech Academy of Sciences Publication Activity Database

    Pala, Z.; Mušálek, Radek; Kyncl, J.; Harcuba, P.; Stráský, J.; Kolařík, K.

    2013-01-01

    Roč. 20, č. 2 (2013), s. 93-95 ISSN 1211-5894. [Struktura 2013 - Kolokvium Krystalografické společnosti. Češkovice (Blansko), 09.09.2013-13.09.2013] Institutional support: RVO:61389021 Keywords : boriding * surface hardening * iron borides * tooth-shaped microstructure * residual stresses Subject RIV: JK - Corrosion ; Surface Treatment of Materials http://www.xray.cz/ms/bul2013-2/s6.pdf

  13. Formation of boride layers on steel substrates

    International Nuclear Information System (INIS)

    Stergioudis, G.

    2006-01-01

    Boronizing coatings were prepared by means of pack cementation technique. It was found that using the appropriate substrate and controlling parameters of the boribing process such as boron activity of the mixture, temperature and time of treatment, it is possible to obtain a structure predominantly consisting of the Fe 2 B phase. In the present study low alloy ferritic steels were chosen as substrates. Changing the boron carbide concentration in the mixture and the temperature and time of boronizing process the conditions of the boronizing were altered. As a result the formation of the Fe 2 B phase is enhanced. Characterization of the as-borided steels is discussed based on X-ray diffraction and Curie temperature measurements. (copyright 2006 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  14. Synthesis of cobalt boride nanoparticles using radio frequency thermal plasma

    International Nuclear Information System (INIS)

    Lapitan, Jr. Lorico DS.; Ying Ying Chen; Seesoek Choe; Watanabe, Takayuki

    2012-01-01

    Nano size cobalt boride particles were synthesized from vapor phase using a 30 kw-4 MHz radio frequency (RF) thermal plasma. Cobalt and boron powder mixtures used as precursors in different composition and feed rate were evaporated immediately in the high temperature plasma and cobalt boride nanoparticles were produced through the quenching process. The x-ray diffractometry (XRD) patterns of cobalt boride nanoparticles prepared from the feed powder ratio of 1:2 and 1:3 for Co: B showed peaks that are associated with the Co 2 B and CoB crystal phases of cobalt boride. The XRD analysis revealed that increasing the powder feed rate results in a higher mass fraction and a larger crystalline diameter of cobalt boride nanoparticles. The images obtained by field emission scanning electron microscopy (FE-SEM) revealed that cobalt boride nanoparticles have a spherical morphology. The crystallite size of the particles estimated with XRD was found to be 18-22 nm. (author)

  15. Mechanochemically Driven Syntheses of Boride Nanomaterials

    Science.gov (United States)

    Blair, Richard G.

    Solid state metathesis reactions have proven to be a viable route to the production of unfunctionalized nanomaterials. However, current implementations of this approach are limited to self-propagating reactions. We have been investigating mechanically driven metathesis reactions. The use of high-energy ball mills allows control of crystallite sizes without the use of a capping group. Reinforcement materials with crystallite sizes on the order of 5-30 nm can be produced in such a manner. Borides are of particular interest due to their strength, high melting point, and electrical conductivity. The ultimate goal of this work is to prepare oxide and capping group-free nanoparticles suitable for incorporation in thermoelectric, polymer, and ceramic composites. Ultimately this work will facilitate the production of improved thermoelectric materials that will provide robust, deployable, power generation modules to supplement or replace fuel cell, Stirling, and battery-derived power sources. It will also result in scalable, bulk syntheses of tough, refractory, conductive nanomaterials for polymer composites with improved electrical properties, ceramic composites with enhanced fracture toughness, and composites with enhanced neutron reflectance and/or absorbance.

  16. Corrosion behavior of boride layers evaluated by the EIS technique

    Energy Technology Data Exchange (ETDEWEB)

    Campos, I. [Instituto Politecnico Nacional. SEPI-ESIME U.P. Adolfo Lopez Mateos, Zacatenco, Mexico D.F. 07738 (Mexico)], E-mail: icampos@ipn.mx; Palomar-Pardave, M. [Universidad Autonoma Metropolitana-Azcapotzalco, Materials Department, Avenue San Pablo 180 Col. Reynosa Tamaulipas, Mexico D.F. 02200 (Mexico); Amador, A. [Tecnologico de Monterrey, Campus Ciudad de Mexico, Calle del Puente 222 Col. Ejidos de Huipulco, Mexico D.F. 14380 (Mexico); VillaVelazquez, C. [Instituto Politecnico Nacional. SEPI-ESIME U.P. Adolfo Lopez Mateos, Zacatenco, Mexico D.F. 07738 (Mexico); Hadad, J. [Tecnologico de Monterrey, Campus Ciudad de Mexico, Calle del Puente 222 Col. Ejidos de Huipulco, Mexico D.F. 14380 (Mexico)

    2007-09-30

    The corrosion behavior of boride layers at the AISI 304 steel surface is evaluated in the present study. Electrochemical impedance spectroscopy (EIS) technique was used for the evaluation of the polarization resistance at the steel surface, with the aid of AUTOLAB potentiostat. Samples were treated with boron paste thickness of 4 and 5 mm, in the range of temperatures 1123 {<=} T {<=} 1273 K and exposed time of 4 and 6 h. The electrochemical technique employed 10 mV AC with a frequency scan range from 8 kHz to 3 mHz in deaerated 0.1 M NaCl solution. Nyquist diagrams show that the highest values of corrosion resistance are present in the samples borided at the temperature of 1273 K, with treatment time of 4 h and 4 mm of boron paste thickness. The values of corrosion resistance on borided steels are compared with the porosity exhibited in the layers.

  17. Synthesis of Magnesium Nickel Boride Aggregates via Borohydride Autogenous Pressure.

    Science.gov (United States)

    Shahbazi, Mahboobeh; Cathey, Henrietta E; Mackinnon, Ian D R

    2018-03-23

    We demonstrate synthesis of the ternary intermetallic MgNi₃B₂ using autogenous pressure from the reaction of NaBH₄ with Mg and Ni metal powder. The decomposition of NaBH₄ to H₂ and B₂H₆ commences at low temperatures in the presence of Mg and/or Ni and promotes formation of Ni-borides and MgNi₃B₂ with the increase in temperature. MgNi₃B₂ aggregates with Ni-boride cores are formed when the reaction temperature is >670 °C and autogenous pressure is >1.7 MPa. Morphologies and microstructures suggest that solid-gas and liquid-gas reactions are dominant mechanisms and that Ni-borides form at a lower temperature than MgNi₃B₂. Magnetic measurements of the core-shell MgNi₃B₂ aggregates are consistent with ferromagnetic behaviour in contrast to stoichiometric MgNi₃B₂ which is diamagnetic at room temperature.

  18. Laser borided composite layer produced on austenitic 316L steel

    Directory of Open Access Journals (Sweden)

    Mikołajczak Daria

    2016-12-01

    Full Text Available Abstract Austenitic 316L steel is well-known for its good resistance to corrosion and oxidation. Therefore, this material is often used wherever corrosive media or high temperatures are to be expected. The main drawback of this material is very low hardness and low resistance to mechanical wear. In this study, the laser boriding was used in order to improve the wear behavior of this material. As a consequence, a composite surface layer was produced. The microstructure of laser-borided steel was characterized by only two zones: re-melted zone and base material. In the re-melted zone, a composite microstructure, consisting of hard ceramic phases (borides and a soft austenitic matrix, was observed. A significant increase in hardness and wear resistance of such a layer was obtained.

  19. 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.

  20. Thermodynamic properties of molybdenum borides at temperatures above 300 K

    International Nuclear Information System (INIS)

    Bolgar, A.S.; Blinder, A.V.; Serbova, M.I.

    1990-01-01

    Enthalpy of Mo 2 B, MoB, Mo 2 B 5 borides within the range of temperatures above 300 K has been experimentally studied. Parameters of temperature dependences of enthalpy, heat capacity, entropy and the reduced Gibbs energy of the studied substances are calculated within a wide range. It is stated that high-temperature heat capacity of the studied borides can be presented as a sum of the electron component, a harmonic part of the lattice component and a contribution caused by anharmonic oscillations of lattice atoms. Values of coefficients of isothermal compressibility of Mo 2 , MoB, Mo 2 B 5 within the high temperature range are estimated

  1. Swelling and fracturing of borides under neutron irradiation

    International Nuclear Information System (INIS)

    Krainy, A.G.; Ogorodnikov, V.V.; Grinik, E.U.; Chirko, L.I.; Shinakov, A.A.

    1994-01-01

    The neutron irradiation of high temperature borides, which are included in boron-containing reactor materials, results in high internal stresses, leading to considerable swelling and micro- and macro-fracturing. Experimental results over a large range of temperature and fluences, show a change of damage mechanism for borides within 400-530 C: the macro-cracking with formation of annular and radial cracks is observed below this temperature zone. The accumulation of micro-fractures and the process of gas swelling take place at irradiation temperatures above 530 C. The effect of the high internal stresses is compared to external pressure. 12 refs., 4 figs

  2. Development and application of high strength ternary boride base cermets

    International Nuclear Information System (INIS)

    Takagi, Ken-ichi

    2006-01-01

    Reaction boronizing sintering is a novel strategy to form a ternary boride coexisting with a metal matrix in a cermet during liquid phase sintering. This new sintering technique has successfully developed world first ternary boride base cermets with excellent mechanical properties such as Mo 2 FeB 2 , Mo 2 NiB 2 and WCoB base ones. In these cermets Mo 2 FeB 2 and Mo 2 NiB 2 base ones consist of a tetragonal M 3 B 2 (M: metal)-type complex boride as a hard phase and a transition metal base matrix. The cermets have already been applied to wear resistant applications such as injection molding machine parts, can making tools, and hot copper extruding dies, etc. This paper focuses on the characteristics, effects of the additional elements on the mechanical properties and structure, and practical applications of the ternary boride base cermets. - Graphical abstract: TRS and hardness of Ni-5B-51Mo-17.5Cr and Ni-5B-51Mo-12.5Cr-5V-xMn mass% cermets as functions of Mn content (Fig. 17)

  3. Metal Borohydrides synthesized from metal borides and metal hydrides

    DEFF Research Database (Denmark)

    Sommer, Sanna

    2014-01-01

    Aarhus C, Denmark email: gallafogh@hotmail.com / sanna-sommer@hotmail.com Magnesium boride, MgB2, ball milled with MH (M = Li, Na, Ca) followed by hydrogenation under high hydrogen pressure, readily forms the corresponding metal borohydrides, M(BH4)x (M = Li, Na, Ca) and MgH2 according to reaction scheme...

  4. Assessment of polyphase sintered iron-cobalt-iron boride cermets

    International Nuclear Information System (INIS)

    Nowacki, J.; Pieczonka, T.

    2004-01-01

    Sintering of iron, cobalt and boron powders has been analysed. As a result iron-iron boride, Fe-Fe 2 B and iron/cobalt boride with a slight admixture of molybdenum, Fe - Co - (FeMoCo) 2 B cermets have been produced. Iron was introduced to the mixture as the Astalloy Mo Hoeganaes grade powder. Elemental amorphous boron powder was used, and formation of borides occurred both during heating and isothermal sintering periods causing dimensional changes of the sintered body. Dilatometry was chosen to control basic phenomena taking place during multiphase sintering of investigated systems. The microstructure and phase constituents of sintered compacts were controlled as well. The cermets produced were substituted to: metallographic tests, X-ray analysis, measurements of hardness and of microhardness, and of wear in the process of sliding dry friction. Cermets are made up of two phases; hard grains of iron - cobalt boride, (FeCo) 2 B (1800 HV) constituting the reinforcement and a relatively soft and plastic eutectic mixture Fe 2 B - Co (400-500 HV) constituting the matrix. (author)

  5. Nanosize boride particles in heat-treated nickel base superalloys

    International Nuclear Information System (INIS)

    Zhang, H.R.; Ojo, O.A.; Chaturvedi, M.C.

    2008-01-01

    Grain boundary microconstituents in aged nickel-based superalloys were studied by transmission electron microscopy techniques. A nanosized M 5 B 3 boride phase, possibly formed by intergranular solute desegregation-induced precipitation, was positively identified. The presence of these intergranular nanoborides provides reasonable clarification of a previously reported reduction of grain boundary liquation temperature during the weld heat affected zone thermal cycle

  6. Bonding and doping of simple icosahedral-boride semiconductors

    International Nuclear Information System (INIS)

    Emin, David

    2004-01-01

    A simple model of the bonding and doping of a series of icosahedral-boride insulators is presented. Icosahedral borides contain clusters of boron atoms that occupy the 12 vertices of icosahedra. This particular series of icosahedral borides share both the stoichiometry B 12 X 2 , where X denotes a group V element (P or As), and a common lattice structure. The inter-icosahedral bonding of these icosahedral borides is contrasted with that of B 12 O 2 and with that of α-rhombohedral boron. Knowledge of the various types of inter-icosahedral bonding is used as a basis to address effects of inter-icosahedral atomic substitutions. The inter-icosahedral bonding is maintained when an atom of a group V element is replaced with an atom of a group IV element, thereby producing a p-type dopant. However, changes of inter-icosahedral bonding occur upon replacing an atom of a group V element with an atom of a group VI element or with a vacancy. As a result, these substitutions do not produce effective n-type dopants. Moreover, partial substitution of boron atoms for atoms of group V elements generally renders these materials p-type semiconductors

  7. Subminiature eddy current transducers for studying boride coatings

    Science.gov (United States)

    Dmitriev, S. F.; Ishkov, A. V.; Malikov, V. N.; Sagalakov, A. M.

    2016-07-01

    Strengthening of parts and units of machines, increased reliability and longer service life is an important task of modern mechanical engineering. The main objects of study in the work were selected steel 65G and 50HGA, wear-resistant boride coatings ternary system Fe-B-Fe n B which were investigated by scanning electron microscopy and eddy-current nondestructive methods.

  8. 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

  9. Borides and vitreous compounds sintered as high-energy fuels

    International Nuclear Information System (INIS)

    Mota, J.M.; Abenojar, J.; Martinez, M.A.; Velasco, F.; Criado, A.J.

    2004-01-01

    Boron was chosen as fuel in view of its excellent thermodynamic values for combustion, as compared to traditional fuels. The problem of the boron in combustion is the formation of a surface layer of oxide, which delays the ignition process, reducing the performance of the rocket engine. This paper presents a high-energy fuel for rocket engines. It is composed of sintered boron (borides and carbides and vitreous compounds) with a reducing chemical agent. Borides and boron carbide were prepared since the combustion heat of the latter is similar to that of the amorphous boron (in: K.K. Kuo (Ed.), Boron-Based Solid Propellant and Solid Fuel, Vol. 427, CRC Press, Boca Raton, FL, 1993). Several chemical reducing elements were used, such as aluminum, magnesium, and coke. As the raw material for boron, different compounds were used: amorphous boron, boric acid and boron oxide

  10. Catalytic activity of metal borides in the reaction of decomposition

    International Nuclear Information System (INIS)

    Labodi, I.; Korablev, L.I.; Tavadyan, L.A.; Blyumberg, Eh.A.

    1982-01-01

    Catalytic effect of CoB, MoB 2 , ZrB 2 and NbB 2 , prepared by the method of self-propagating high-temperature synthesis, on decomposition of tertiary butyl hydroperoxide has been studied. A technigue of determination of action mechanism of heterogeneous catalysts in liquid-phase process is suggested. It is established that CoB in contrast to other metal borides catalyzes only hydroperoxide decomposition into radicals

  11. Novel boride base cermets with very high strength

    International Nuclear Information System (INIS)

    Ken-ichi Takagi; Mari Yonetsu; Yuji Yamasaki

    2001-01-01

    Mo 2 NiB 2 boride base cermets consist of a Mo 2 NiB 2 type complex boride as a hard phase and a Ni base binder. The addition of Cr and V to the cermets changed the boride structure from orthorhombic to tetragonal and resulted in the improvement of mechanical properties and microstructural refinement. The tetragonal Mo 2 NiB 2 was formed through the orthorhombic Mo 2 NiB 2 by the solid state reaction during sintering and not formed directly from the raw material powders. Ni-4.5B-46.9Mo-12.5V-xMn (wt.%) model cermets with five levels of Mn content from 0 to 10 wt.% were prepared to investigate the effects of Mn on the mechanical properties and microstructure Of Mo 2 NiB 2 base cermets. The transverse rupture strength (TRS) of the cermets depended strongly on the microstructure, which varied significantly with Mn content. The maximum TRS obtained at 2.5 wt.%Mn were 3.5 Gpa with hardness of 87 R A . (author)

  12. Characterization and diffusion model for the titanium boride layers formed on the Ti6Al4V alloy by plasma paste boriding

    Energy Technology Data Exchange (ETDEWEB)

    Keddam, Mourad, E-mail: keddam@yahoo.fr [Laboratoire de Technologie des Matériaux, Faculté de Génie Mécanique et Génie des Procédés, USTHB, B.P. No. 32, 16111 El-Alia, Bab-Ezzouar, Algiers (Algeria); Taktak, Sukru [Metallurgical and Materials Engineering, Faculty of Technology, Afyon Kocatepe University, ANS Campus, 03200, Afyonkarahisar (Turkey)

    2017-03-31

    Highlights: • Titanium boride layers were produced by plasma paste boriding on Ti6Al4V at 973–1073 K. • Formation rates of the Ti boride layers have parabolic character at all temperatures. • Boron diffusivities were estimated using a diffusion model including incubation times. • Activation energies of boron in TiB{sub 2} and TiB were 136 and 63 kJ/mol respectively. - Abstract: The present study is focused on the estimation of activation energy of boron in the plasma paste borided Ti6Al4V alloy, which is extensively used in technological applications, using an analytical diffusion model. Titanium boride layers were successfully produced by plasma paste boriding method on the Ti6Al4V alloy in the temperature range of 973–1073 K for a treatment time ranging from 3 to 7 h. The presence of both TiB{sub 2} top-layer and TiB whiskers sub-layer was confirmed by the XRD analysis and SEM observations. The surface hardness of the borided alloy was evaluated using Micro-Knoop indenter. The formation rates of the TiB{sub 2} and TiB layers were found to have a parabolic character at all applied process temperatures. A diffusion model was suggested to estimate the boron diffusivities in TiB{sub 2} and TiB layers under certain assumptions, by considering the effect of boride incubation times. Basing on own experimental data on boriding kinetics, the activation energies of boron in TiB{sub 2} and TiB phases were estimated as 136.24 ± 0.5 and 63.76 ± 0.5 kJ mol{sup −1}, respectively. Finally, the obtained values of boron activation energies for Ti6Al4V alloy were compared with the data available in the literature.

  13. Plasma boriding of a cobalt–chromium alloy as an interlayer for nanostructured diamond growth

    Energy Technology Data Exchange (ETDEWEB)

    Johnston, Jamin M.; Jubinsky, Matthew; Catledge, Shane A., E-mail: catledge@uab.edu

    2015-02-15

    Highlights: • Metal-boride layer creates a compatible surface for NSD deposition. • PECVD boriding on CoCrMo produces robust metal-boride layer. • Deposition temperature comparison shows 750 °C boriding masks surface cobalt. • EDS shows boron diffusion as well as deposition. • Nanoindentation hardness of CoCrMo substantially increases after boriding. - Abstract: Chemical vapor deposited (CVD) diamond coatings can potentially improve the wear resistance of cobalt–chromium medical implant surfaces, but the high cobalt content in these alloys acts as a catalyst to form graphitic carbon. Boriding by high temperature liquid baths and powder packing has been shown to improve CVD diamond compatibility with cobalt alloys. We use the microwave plasma-enhanced (PE) CVD process to deposit interlayers composed primarily of the borides of cobalt and chromium. The use of diborane (B{sub 2}H{sub 6}) in the plasma feedgas allows for the formation of a robust boride interlayer for suppressing graphitic carbon during subsequent CVD of nano-structured diamond (NSD). This metal–boride interlayer is shown to be an effective diffusion barrier against elemental cobalt for improving nucleation and adhesion of NSD coatings on a CoCrMo alloy. Migration of elemental cobalt to the surface of the interlayer is significantly reduced and undetectable on the surface of the subsequently-grown NSD coating. The effects of PECVD boriding are compared for a range of substrate temperatures and deposition times and are evaluated using glancing-angle X-ray diffraction (XRD), cross-sectional scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS), and micro-Raman spectroscopy. Boriding of CoCrMo results in adhered nanostructured diamond coatings with low surface roughness.

  14. Evaluation of High Temperature Particle Erosion Resistance of Vanadium-Boride Coating

    International Nuclear Information System (INIS)

    Lee, E. Y.; Kim, J. H.; Jeong, S. I.; Lee, S. H.; Eum, G. W.

    2015-01-01

    The components in ultra super critical (USC) steam turbine, which is under development for high efficient power generation, are encountering harsher solid particle erosion by iron oxide scales than ones in the existing steam turbines. Therefore, the currently used boride coating will not be able to hold effective protection from particle erosion in USC system and should be replaced by new particle erosion resistant coatings. One of the best protective coatings developed for USC steam turbine parts was found to be vanadium-boride (V-boride) coating which has a hardness of about 3000 HV, much higher than that of boride, 1600∼2000 HV. In order to evaluate particle erosion resistance of the various coatings such as V-boride, boride and Cr-carbide coatings at high temperature, particle erosion test equipment were designed and manufactured. In addition, erosion particle velocity was simulated using FLUENT software based on semi-implicity method for pressure linked equations revised (SIMPLER). Based on experimental results of this work, the vanadium-boride coating was found to be superior to others and to be a candidate coating to replace the boride coating

  15. Evaluation of High Temperature Particle Erosion Resistance of Vanadium-Boride Coating

    Energy Technology Data Exchange (ETDEWEB)

    Lee, E. Y.; Kim, J. H.; Jeong, S. I. [Andong National University, Andong (Korea, Republic of); Lee, S. H.; Eum, G. W. [Corporate R and D Institute Doosan Heavy Industries and Construction Co., Changwon (Korea, Republic of)

    2015-04-15

    The components in ultra super critical (USC) steam turbine, which is under development for high efficient power generation, are encountering harsher solid particle erosion by iron oxide scales than ones in the existing steam turbines. Therefore, the currently used boride coating will not be able to hold effective protection from particle erosion in USC system and should be replaced by new particle erosion resistant coatings. One of the best protective coatings developed for USC steam turbine parts was found to be vanadium-boride (V-boride) coating which has a hardness of about 3000 HV, much higher than that of boride, 1600∼2000 HV. In order to evaluate particle erosion resistance of the various coatings such as V-boride, boride and Cr-carbide coatings at high temperature, particle erosion test equipment were designed and manufactured. In addition, erosion particle velocity was simulated using FLUENT software based on semi-implicity method for pressure linked equations revised (SIMPLER). Based on experimental results of this work, the vanadium-boride coating was found to be superior to others and to be a candidate coating to replace the boride coating.

  16. Standard entropy for borides of non-transition metals, rare-earth metals and actinides

    International Nuclear Information System (INIS)

    Borovikova, M.S.

    1986-01-01

    Using as initial data the most reliable values of standard entropy for 10 compounds, the entropies for 40 compounds of non-transition metals, rare-earth metals and actinides have been evaluated by the method of comparative calculation. Taking into account the features of boride structures, two methods, i.e. additive and proportional, have been selected for the entropy calculations. For the range of borides the entropies were calculated from the linear relation of the latter to the number of boron atoms in the boride. For borides of rare-earth metals allowance has been made for magnetic contributions in conformity with the multiplicity of the corresponding ions. Insignificant differences in the electronic contributions to the entropy for borides and metals have been neglected. For dodecaborides only the additive method has been used. This is specified by the most rigid network that provides the same contribution to compound entropy. (orig.)

  17. Some mechanical properties of borided AISI H13 and 304 steels

    International Nuclear Information System (INIS)

    Taktak, Sukru

    2007-01-01

    In the present study, mechanical properties of borides formed on AISI H13 hot work tool and AISI 304 stainless steels have been investigated. Both steels have high chromium content and have a widespread use in the engineering application. Boriding treatment was carried out in slurry salt bath consisting of borax, boric acid, and ferrosilicon at temperature range of 800-950 deg. C for 3, 5, and 7 h. X-ray diffraction analysis of boride layers on the surface of steels revealed various peaks of FeB, Fe 2 B, CrB, and Ni 3 B. Metallographic studies showed that the boride layer has a flat and smooth morphology in the 304 steel while H13 steel was a ragged morphology. The characterization of the boride layer is also carried out by means of the micro-hardness, surface roughness, adhesion, and fracture toughness studies

  18. 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 ...

  19. 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...

  20. 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.

  1. Borides - a new generation of highly resistant materials?

    International Nuclear Information System (INIS)

    Telle, R.

    1988-01-01

    High-duty ceramics are on advance in all sectors where materials with extremely good resistance to high temperatures and wear are required. The group of oxides, nitrides and carbides in use for quite a time now recently has been increased by the metal borides which offer among others economic advantages in certain applications. The drawbacks of these materials still to be reduced are their brittleness and susceptibility to oxidation and corrosion. Current research work on the thermodynamics of such systems, on the interaction between structure and properties, and on means to improve strength and resistance to wear are expected to soon open up new applications. (orig.) [de

  2. Transition metal borides. Synthesis, characterization and superconducting properties

    Energy Technology Data Exchange (ETDEWEB)

    Kayhan, Mehmet

    2013-07-12

    A systematic study was done on the synthesis and superconducting properties of metal rich transition metal borides. Five different binary systems were investigated including the boride systems of niobium, tantalum, molybdenum, tungsten and rhenium. High temperature solid state methods were used in order to synthesize samples of different transition metal borides of the composition M{sub 2}B, MB, M{sub 3}B{sub 2}, MB{sub 2}, and M{sub 2}B{sub 4}. The reactions were carried out in three different furnaces with different sample containers: the electric arc (copper crucible), the high frequency induction furnace (boron nitride, tantalum or glassy carbon crucibles), and the conventional tube furnace (sealed evacuated quartz ampoules). The products obtained were characterized with X-ray powder diffractometry, scanning electron microscopy and energy-dispersive X-ray spectroscopy. Phase analyses and crystal structure refinements using the Rietveld method and based on structure models known from literature were performed. A neutron diffraction measurement was done for W{sub 2}B{sub 4} to allow for a complete crystal structure determination, because of the presence of a heavy element like tungsten and a light element like boron that made it difficult to determine the accurate determination of the boron atom positions and occupancies from X-ray data. A new structure model for W{sub 2}B{sub 4} was proposed. Magnetic measurements in a SQUID magnetometer down to temperatures as low as 1.8 K were performed to several of the products in order to see if the transition metal borides become superconducting at low temperatures, and the results were compared with data from literature. Superconducting properties were found for the following compounds: NbB{sub 2} (T{sub C} = 3.5 K), β-MoB (T{sub C} = 2.4 K), β-WB (T{sub C} = 2.0 K), α-WB (T{sub C} = 4.3 K), W{sub 2}B{sub 4} (T{sub C} = 5.4 K), Re{sub 7}B{sub 3} (T{sub C} = 2.4 K). A relationship between the superconducting properties

  3. Deposition and characterization of aluminum magnesium boride thin film coatings

    Science.gov (United States)

    Tian, Yun

    Boron-rich borides are a special group of materials possessing complex structures typically comprised of B12 icosahedra. All of the boron-rich borides sharing this common structural unit exhibit a variety of exceptional physical and electrical properties. In this work, a new ternary boride compound AlMgB14, which has been extensively studied in bulk form due to its novel mechanical properties, was fabricated into thin film coatings by pulsed laser deposition (PLD) technology. The effect of processing conditions (laser operating modes, vacuum level, substrate temperature, and postannealing, etc.) on the composition, microstructure evolution, chemical bonding, and surface morphology of AlMgB14 thin film coatings has been investigated by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), transmission electron microscopy (TEM), atomic force microscopy (AFM) and Fourier transform infrared (FTIR) spectrometry; the mechanical, electrical, and optical properties of AlMgB14 thin films have been characterized by nanoindentation, four-point probe, van der Pauw Hall measurement, activation energy measurement, and UV-VIS-NIR spectrophotometer. Experimental results show that AlMgB14 films deposited in the temperature range of 300 K - 873 K are amorphous. Depositions under a low vacuum level (5 x 10-5 Torr) can introduce a significant amount of C and O impurities into AlMgB14 films and lead to a complex oxide glass structure. Orthorhombic AlMgB14 phase cannot be obtained by subsequent high temperature annealing. By contrast, the orthorhombic AlMgB 14 crystal structure can be attained via high temperature-annealing of AlMgB14 films deposited under a high vacuum level (boride films, high vacuum level-as deposited AlMgB14 films also possess a low n-type electrical resistivity, which is a consequence of high carrier concentration and moderate carrier mobility. The operative electrical transport mechanism and doping behavior for high vacuum level-as deposited AlMgB14

  4. Transition metal borides. Synthesis, characterization and superconducting properties

    International Nuclear Information System (INIS)

    Kayhan, Mehmet

    2013-01-01

    A systematic study was done on the synthesis and superconducting properties of metal rich transition metal borides. Five different binary systems were investigated including the boride systems of niobium, tantalum, molybdenum, tungsten and rhenium. High temperature solid state methods were used in order to synthesize samples of different transition metal borides of the composition M 2 B, MB, M 3 B 2 , MB 2 , and M 2 B 4 . The reactions were carried out in three different furnaces with different sample containers: the electric arc (copper crucible), the high frequency induction furnace (boron nitride, tantalum or glassy carbon crucibles), and the conventional tube furnace (sealed evacuated quartz ampoules). The products obtained were characterized with X-ray powder diffractometry, scanning electron microscopy and energy-dispersive X-ray spectroscopy. Phase analyses and crystal structure refinements using the Rietveld method and based on structure models known from literature were performed. A neutron diffraction measurement was done for W 2 B 4 to allow for a complete crystal structure determination, because of the presence of a heavy element like tungsten and a light element like boron that made it difficult to determine the accurate determination of the boron atom positions and occupancies from X-ray data. A new structure model for W 2 B 4 was proposed. Magnetic measurements in a SQUID magnetometer down to temperatures as low as 1.8 K were performed to several of the products in order to see if the transition metal borides become superconducting at low temperatures, and the results were compared with data from literature. Superconducting properties were found for the following compounds: NbB 2 (T C = 3.5 K), β-MoB (T C = 2.4 K), β-WB (T C = 2.0 K), α-WB (T C = 4.3 K), W 2 B 4 (T C = 5.4 K), Re 7 B 3 (T C = 2.4 K). A relationship between the superconducting properties and the compositional and structural features was discussed for metal diborides. Also it was

  5. Anisotropic elastic and thermal properties of titanium borides by first-principles calculations

    Energy Technology Data Exchange (ETDEWEB)

    Sun, Liang; Gao, Yimin [State Key Laboratory for Mechanical Behavior of Materials, Xi’an Jiaotong University, Xi’an 710049 (China); Xiao, Bing [Department of Physics and Quantum Theory Group, School of Science and Engineering, Tulane University, New Orleans, LA 70118 (United States); Li, Yefei, E-mail: yefeili@126.com [State Key Laboratory for Mechanical Behavior of Materials, Xi’an Jiaotong University, Xi’an 710049 (China); Wang, Guoliang [State Key Laboratory for Mechanical Behavior of Materials, Xi’an Jiaotong University, Xi’an 710049 (China)

    2013-12-05

    Highlights: •Elastic properties of titanium borides are calculated by first principles calculation. •Thermodynamical stability of titanium borides is analyzed. •Heat capacity and thermal expansion coefficient for titanium borides are calculated and compared. •Grüneisen parameters of titanium borides are calculated. -- Abstract: The anisotropic elastic and thermal expansions of the titanium borides (TiB{sub 2}, Ti{sub 3}B{sub 4}, TiB{sub P}nma and TiB{sub F}m3{sup ¯}m) are calculated from first-principles using density functional theory. All borides show different anisotropic elastic properties; the bulk, shear and Young’s moduli are consistent with those determined experimentally. The temperature dependence of thermal expansions is mainly caused by the restoration of thermal energy due to phonon excitations at low temperature. When the temperature is higher than 500 K, the volumetric coefficient is increased linearly by increasing temperature. Meanwhile, the heat capacities of titanium borides are obtained based on the knowledge of thermal expansion coefficient and the elasticity, the calculations are in good agreement with the experiments.

  6. Electron momentum distribution and electronic response of ceramic borides

    Energy Technology Data Exchange (ETDEWEB)

    Heda, N.L. [Department of Pure and Applied Physics, University of Kota, Kota 324005 (India); Meena, B.S.; Mund, H.S. [Department of Physics, Mohanlal Sukhadia University, Udaipur 313001 (India); Sahariya, Jagrati [Department of Physics, Manipal University, Jaipur 303007 (India); Kumar, Kishor [Department of Physics, Mohanlal Sukhadia University, Udaipur 313001 (India); Ahuja, B.L., E-mail: blahuja@yahoo.com [Department of Physics, Mohanlal Sukhadia University, Udaipur 313001 (India)

    2017-03-15

    Isotropic Compton profiles of transition metal based ceramics TaB and VB have been measured using {sup 137}Cs (661.65 keV) γ-ray Compton spectrometer. The experimental momentum densities are compared with those deduced using linear combination of atomic orbitals (LCAO) with Hartree-Fock (HF), density functional theory (DFT) with Wu-Cohen generalized gradient approximation (WCGGA) and also the hybridization of HF and DFT (namely B3PW and PBE0) schemes. It is found that LCAO-DFT-WCGGA scheme based profiles give an overall better agreement with the experimental data, for both the borides. In addition, we have computed the Mulliken's population (MP) charge transfer data, energy bands, density of states and Fermi surface topology of both the borides using full potential-linearized augmented plane wave (FP-LAPW) and LCAO methods with DFT-WCGGA scheme. Cross-overs of Fermi level by the energy bands corresponding to B-2p and valence d-states of transition metals lead to metallic character in both the compounds. Equal-valence-electron-density profiles and MP analysis suggest more ionic character of VB than that of TaB.

  7. A Simple, General Synthetic Route toward Nanoscale Transition Metal Borides.

    Science.gov (United States)

    Jothi, Palani R; Yubuta, Kunio; Fokwa, Boniface P T

    2018-04-01

    Most nanomaterials, such as transition metal carbides, phosphides, nitrides, chalcogenides, etc., have been extensively studied for their various properties in recent years. The similarly attractive transition metal borides, on the contrary, have seen little interest from the materials science community, mainly because nanomaterials are notoriously difficult to synthesize. Herein, a simple, general synthetic method toward crystalline transition metal boride nanomaterials is proposed. This new method takes advantage of the redox chemistry of Sn/SnCl 2 , the volatility and recrystallization of SnCl 2 at the synthesis conditions, as well as the immiscibility of tin with boron, to produce crystalline phases of 3d, 4d, and 5d transition metal nanoborides with different morphologies (nanorods, nanosheets, nanoprisms, nanoplates, nanoparticles, etc.). Importantly, this method allows flexibility in the choice of the transition metal, as well as the ability to target several compositions within the same binary phase diagram (e.g., Mo 2 B, α-MoB, MoB 2 , Mo 2 B 4 ). The simplicity and wide applicability of the method should enable the fulfillment of the great potential of this understudied class of materials, which show a variety of excellent chemical, electrochemical, and physical properties at the microscale. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  8. Comparative NMR investigation of the Re-based borides

    Science.gov (United States)

    Lue, C. S.; Tao, Y. F.; Su, T. H.

    2008-07-01

    We report a systematic study of the rhenium-based borides, ReB2 , Re7B3 , and Re3B , by means of the B11 nuclear magnetic resonance (NMR) spectroscopy. While Re7B3 and Re3B are superconductors, ReB2 exhibits no superconducting signature but is of current interest due to its superhard mechanical property. Since the major focus of this investigation is their electronic characteristics in the normal states, we performed the measurements at temperatures between 77 and 295 K. For Re7B3 and Re3B , s -character electrons were found to be responsible for the observed B11 NMR Knight shift and spin-lattice relaxation rate (1/T1) . From T1 analysis, we thus deduce the partial Bs Fermi-level density of states (DOS) of both borides. On the other hand, the relaxation rate of ReB2 is mainly associated with p electrons, similar to the cases of OsB2 and RuB2 . In addition, the extracted B2p Fermi-level DOS is in good agreement with the theoretical prediction from band-structure calculations.

  9. 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

  10. Characterisation of Wear Resistant Boride Layers on a Tool Steel by Activity Controlled Pack Boronising

    DEFF Research Database (Denmark)

    Fernandes, Frederico Augusto Pires; Christiansen, Thomas Lundin; Somers, Marcel A. J.

    2015-01-01

    The present work addresses the production and characterisation of iron boride layers by pack boronising of a Vanadis 6 tool steel. The boride layers were produced at 900°C for 2h using different pack compositions in order to obtain a single-phase boride layer. The layers were characterized...... by electron microscopy, glow discharge optical emission spectroscopy, X-ray diffraction, Vickers hardness tests and wear testing with a pin-on-disc tribometer. It was found that the type of boride phases (FeB and/or Fe2B) present in the treated layer can be controlled by changing the boron activity...... by pack boronising for all conditions as compared to the heat treated tool steel....

  11. Hard Surface Layers by Pack Boriding and Gaseous Thermo-Reactive Deposition and Diffusion Treatments

    DEFF Research Database (Denmark)

    Christiansen, Thomas Lundin; Bottoli, Federico; Dahl, Kristian Vinter

    2017-01-01

    ) layers with hardnesses up to 1800 HV. Titanizing of ARNE tool steel results in a surface layer consisting of TiC with a hardness of approximately 4000 HV. Duplex treatments, where boriding is combined with subsequent (TRD) titanizing, result in formation of hard TiB2 on top of a thick layer of Fe......Thermo-reactive deposition and diffusion (TRD) and boriding are thermochemical processes that result in very high surface hardness by conversion of the surface into carbides/nitrides and borides, respectively. These treatments offer significant advantages in terms of hardness, adhesion, tribo...... subjected to TRD (chromizing and titanizing) and boriding treatments. For the steels with low carbon content, chromizing results in surface alloying with chromium, i.e., formation of a (soft) “stainless” surface zone. Steels containing higher levels of carbon form chromium carbide (viz. Cr23C6, Cr7C3...

  12. Quantitative electron probe microanalysis of borides in aluminium

    International Nuclear Information System (INIS)

    Karduck, P.; Schuerhoff, H.J.; Burchard, W.G.

    1983-01-01

    A procedure for the quantitative analysis of borides in aluminium was introduced. For this purpose the optimal apparative boundary conditions for the EPMA of boron were worked out. With these conditions a satisfactory peak to background ratio of 57 could be achieved for B-Kα-radiation. By application of this method the following conclusion should be drawn concerning the kind of nuclei during grain refinement of aluminium with titanium and boron: For grain refinement of aluminium with titanium and boron in the hypoperitectic region of the binary system Al-Ti TiB 2 -particles in clusters provide the high efficiency of refinement. This entails that the TiB 2 -particles already present in the master alloy remain inert in the melt. Hence, the good efficiency of refinement in this region cannot be attributed to the presence of particles like Al 3 Ti, AlB 2 or (Al, Ti) B 2 . (Author)

  13. Synthesis, Structure, and Properties of Refractory Hard-Metal Borides

    Science.gov (United States)

    Lech, Andrew Thomas

    As the limits of what can be achieved with conventional hard compounds, such as tungsten carbide, are nearing reach, super-hard materials are an area of increasing industrial interest. The refractory hard metal borides, such as ReB2 and WB4, offer an increasingly attractive alternative to diamond and cubic boron nitride as a next-generation tool material. In this Thesis, a thorough discussion is made of the progress achieved by our laboratory towards understanding the synthesis, structure, and properties of these extremely hard compounds. Particular emphasis is placed on structural manipulation, solid solution formation, and the unique crystallographic manifestations of what might also be called "super-hard metals".

  14. Boron-Based Hydrogen Storage: Ternary Borides and Beyond

    Energy Technology Data Exchange (ETDEWEB)

    Vajo, John J. [HRL Laboratories, LLC, Malibu, CA (United States)

    2016-04-28

    DOE continues to seek reversible solid-state hydrogen materials with hydrogen densities of ≥11 wt% and ≥80 g/L that can deliver hydrogen and be recharged at moderate temperatures (≤100 °C) and pressures (≤100 bar) enabling incorporation into hydrogen storage systems suitable for transportation applications. Boron-based hydrogen storage materials have the potential to meet the density requirements given boron’s low atomic weight, high chemical valance, and versatile chemistry. However, the rates of hydrogen exchange in boron-based compounds are thus far much too slow for practical applications. Although contributing to the high hydrogen densities, the high valance of boron also leads to slow rates of hydrogen exchange due to extensive boron-boron atom rearrangements during hydrogen cycling. This rearrangement often leads to multiple solid phases occurring over hydrogen release and recharge cycles. These phases must nucleate and react with each other across solid-solid phase boundaries leading to energy barriers that slow the rates of hydrogen exchange. This project sought to overcome the slow rates of hydrogen exchange in boron-based hydrogen storage materials by minimizing the number of solid phases and the boron atom rearrangement over a hydrogen release and recharge cycle. Two novel approaches were explored: 1) developing matched pairs of ternary borides and mixed-metal borohydrides that could exchange hydrogen with only one hydrogenated phase (the mixed-metal borohydride) and only one dehydrogenated phase (the ternary boride); and 2) developing boranes that could release hydrogen by being lithiated using lithium hydride with no boron-boron atom rearrangement.

  15. Thermal properties of zirconium diboride -- transition metal boride solid solutions

    Science.gov (United States)

    McClane, Devon Lee

    This research focuses on the thermal properties of zirconium diboride (ZrB2) based ceramics. The overall goal was to improve the understanding of how different transition metal (TM) additives influence thermal transport in ZrB2. To achieve this, ZrB2 with 0.5 wt% carbon, and 3 mol% of individual transition metal borides, was densified by hot-press sintering. The transition metals that were investigated were: Y, Ti, Hf, V, Nb, Ta, Cr, Mo, W, and Re. The room temperature thermal diffusivities of the compositions ranged from 0.331 cm2/s for nominally pure ZrB2 to 0.105 cm2/s for (Zr,Cr)B2 and converged around 0.155cm2/s at higher temperatures for all compositions. Thermal conductivities were calculated from the diffusivities, using temperature-dependent values for density and heat capacity. The electron contribution to thermal conductivity was calculated from measured electrical resistivity according to the Wiedemann-Franz law. The phonon contribution to thermal conductivity was calculated by subtracting the electron contribution from the total thermal conductivity. Rietveld refinement of x-ray diffraction data was used to determine the lattice parameters of the compositions. The decrease in thermal conductivity for individual additives correlated directly to the metallic radius of the additive. Additional strain appeared to exist for additives when the stable TM boride for that metal had different crystal symmetries than ZrB2. This research provided insight into how additives and impurities affect thermal transport in ZrB2. The research potentially offers a basis for future modeling of thermal conductivity in ultra-high temperature ceramics based on the correlation between metallic radius and the decrease in thermal conductivity.

  16. 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

  17. 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

  18. Preparation of boron-rich aluminum boride nanoparticles by RF thermal plasma

    Energy Technology Data Exchange (ETDEWEB)

    Choi, Sooseok [Inha University, Department of Chemical Engineering and Regional Innovation Center for Environmental Technology of Thermal Plasma (Korea, Republic of); Matsuo, Jiro; Cheng, Yingying [Tokyo Institute of Technology, Department of Environmental Chemistry and Engineering (Japan); Watanabe, Takayuki, E-mail: watanabe@chemenv.titech.ac.jp [Kyushu University, Department of Chemical Engineering (Japan)

    2013-08-15

    Boron-rich compounds of AlB{sub 12} and AlB{sub 10} nanoparticles were synthesized by a radiofrequency thermal plasma. Aluminum and boron raw powders were evaporated in virtue of high enthalpy of the thermal plasma in upstream region, followed by the formation of aluminum boride nanoparticles in the tail region of plasma flame with rapid quenching. A high production rate of aluminum boride was confirmed by the X-ray diffraction measurement in the case of high input power, high boron content in raw material and helium inner gas. Polyhedral nanoparticles of 20.8 nm in mean size were observed by a transmission electron microscope. In the raw powder mixture of aluminum, titanium, and boron, titanium-boride nanoparticles were synthesized preferentially, because the Gibbs free energy for the boridation of titanium is lower than that of aluminum. Since the nucleation temperature of boron is higher than that of aluminum, the condensation of metal monomers onto boron nuclei results in the formation of boron-rich aluminum boride nanoparticles.

  19. Some physical properties of the higher borides of molybdenum and tungsten

    International Nuclear Information System (INIS)

    Koval'chenko, M.S.; Bodrova, L.G.; Nemchenko, V.F.; Kolotun, V.F.

    1979-01-01

    The temperature dependences of the thermal conductivity, the specific electrical resistance, the thermo-e.m.f. and the magnetic susceptibility, together with the variation of magnetic resistance and of Hall constant with the magnetic field strength at liquid nitrogen temperature and at room temperature, for the higher borides Mo 2 B 5 , MoB 4 , W 2 B 5 and WB 4 were studied. Some features of the physical properties of these metallic borides were established. In contrast with the corresponding metals the higher borides are diamagnetic and the Hall constants are negative. The values of the magnetic susceptibility and the Hall constant are larger for the higher borides than for the low borides. As the temperature increased an inversion of the thermo-e.m.f. sign took place and the signs of the thermo-e.m.f. and the Hall constant are different. The values of the magnetic susceptibility of Mo 2 B 5 , MoB 4 and WB 4 were temperature independent. The electronic structure of the compounds studied is discussed briefly. (Auth.)

  20. Characterization and wear performance of boride phases over tool steel substrates

    Directory of Open Access Journals (Sweden)

    Edgar E Vera Cárdenas

    2016-02-01

    Full Text Available This research work was conducted to characterize boride phases, obtained from the powder-pack process, on AISI H13 and D2 steel substrates, and investigate their tribological behavior. The boriding was developed at a temperature of 1273 K with an exposure time of 8 h. X-ray diffraction, scanning electron microscopy, and energy-dispersive X-ray spectroscopy were conducted on the borided material to characterize the presence of the FeB, Fe2B, and CrB phases and the distribution of heavy elements on the surface of the substrates. The adherence of the boride layers was evaluated, in a qualitative form, through the Daimler-Benz Rockwell-C indentation technique. Sliding wear tests were then performed using a reciprocating wear test machine. All tests were conducted in dry conditions at room temperature. A frequency of 10 Hz and 15-mm sliding distance were used. The applied Hertzian pressure was 2.01 GPa. Scanning electron microscopy was used to observe and analyze the wear mechanisms. Additionally, the variation of the friction coefficient versus the number of cycles was obtained. Experimental results showed that the characteristic wear mechanism for the borided surface was plastic deformation and mild abrasive wear; for unborided substrates, cracking and spalling were observed.

  1. Study of microcracks morphology produced by Vickers indentation on AISI 1045 borided steels

    International Nuclear Information System (INIS)

    Campos, I.; Ramirez, G.; VillaVelazquez, C.; Figueroa, U.; Rodriguez, G.

    2008-01-01

    In this work, we analyzed the roughness morphology of indentation microcracks produced by the Vickers microindentation in the iron boride Fe 2 B. Using the paste boriding process, the boride layers were formed at the surface of AISI 1045 steels. The diffusion processes were carried out with 5 mm of boron paste thickness over the substrate surface at three different temperatures (1193, 1223 and 1273 K) with two different time exposures. The indentations in each Fe 2 B layer were made using a constant load of 200 g at four different distances from the surface. The fracture behavior of the Fe 2 B borided phase is found to be brittle in nature. The profiles of microcracks formed at the corners of the indentations were obtained using the scanning electronic microscopy and were analyzed within the framework of fractal geometry. We found that all indentation microcracks display a self-affine invariance characterized by the same roughness (Hurst) exponent H = 0.8 ± 0.1. The effect of the self-affine roughness of indentation microcracks on the measured fracture toughness is discussed within the framework of the mechanics of self-affine cracks. It is pointed out that the arrest of indentation microcracks is controlled by the fractal fracture toughness, which for the Fe 2 B borided phase is found to be K fc = 0.42 ± 0.02 MPa m 0.75 at all distances from the surface

  2. Quantitative electron probe microanalysis of boron in binary borides

    International Nuclear Information System (INIS)

    Bastin, G.F.; Heijligers, H.J.M.

    1986-01-01

    Quantitative electron probe microanalysis has been performed in 27 binary borides in the range of 4-30 keV, both for the metals as well as for Boron. The procedures along which accurate intensity measurements for B-K α must be carried out are discussed in detail. A total of 196 k-ratios with respect to elemental standards for the metal X-ray lines and 180 k-ratios for B-K α relative to elemental Boron have been obtained. These data have been used to arrive at an improved parameterization for the φ(ρz) approach in matrix correction. The resulting new program (BAS861) was compared to 5 other current correction programs. At the same occasion the available set of mass absorption coefficients for Boron was tested on its consistency and better values suggested where necessary. Finally it is shown that the modified version of the Gaussian φ(ρz) approach (BAS861 program) is highly successful in the matrix correction for B-K α : a relative root-mean-square value of 6.30% was obtained. (Auth.)

  3. 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

  4. Metal Immiscibility Route to Synthesis of Ultrathin Carbides, Borides, and Nitrides.

    Science.gov (United States)

    Wang, Zixing; Kochat, Vidya; Pandey, Prafull; Kashyap, Sanjay; Chattopadhyay, Soham; Samanta, Atanu; Sarkar, Suman; Manimunda, Praveena; Zhang, Xiang; Asif, Syed; Singh, Abhisek K; Chattopadhyay, Kamanio; Tiwary, Chandra Sekhar; Ajayan, Pulickel M

    2017-08-01

    Ultrathin ceramic coatings are of high interest as protective coatings from aviation to biomedical applications. Here, a generic approach of making scalable ultrathin transition metal-carbide/boride/nitride using immiscibility of two metals is demonstrated. Ultrathin tantalum carbide, nitride, and boride are grown using chemical vapor deposition by heating a tantalum-copper bilayer with corresponding precursor (C 2 H 2 , B powder, and NH 3 ). The ultrathin crystals are found on the copper surface (opposite of the metal-metal junction). A detailed microscopy analysis followed by density functional theory based calculation demonstrates the migration mechanism, where Ta atoms prefer to stay in clusters in the Cu matrix. These ultrathin materials have good interface attachment with Cu, improving the scratch resistance and oxidation resistance of Cu. This metal-metal immiscibility system can be extended to other metals to synthesize metal carbide, boride, and nitride coatings. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  5. Hardness optimization of boride diffusion layer on Astm F-75 alloy using response surface methodology

    Energy Technology Data Exchange (ETDEWEB)

    Arguelles O, J. L.; Corona R, M. A. [Universidad Autonoma de San Luis Potosi, Doctorado Institucional en Ingenieria y Ciencia de Materiales, San Luis Potosi 78000, SLP (Mexico); Marquez H, A.; Saldana R, A. L.; Saldana R, A. [Universidad de Guanajuato, Ingenieria Mecanica Agricola DICIVA, Irapuato, Guanajuato 36500 (Mexico); Moreno P, J., E-mail: amarquez@ugto.mx [Universidad de Guanajuato, Departamento de Minas, Metalurgia y Geologia, Ex-Hacienda San Matias s/n, Guanajuato, Guanajuato 36020 (Mexico)

    2017-11-01

    In this study, the Response Surface Methodology (Rsm) and Central Composite Design (Ccd) were used to optimize the hardness of boride diffusion layer on Astm F-75 alloy (also called Haynes alloy). A boronizing thermochemical treatment was carried out at different temperatures and for different time periods. Hardness tests were conducted. The boride diffusion layer was verified by the X-ray diffraction (XRD) analysis indicating the formation of Co B, Co{sub 2}B, Cr B and Mo{sub 2}B phases. An optimal hardness of 3139.7 Hv was obtained for the samples subjected to the boriding process for a duration of 6.86 h at 802.4 degrees Celsius. (Author)

  6. Wear behavior of tempered and borided tool steels under various conditions

    International Nuclear Information System (INIS)

    Al-Haidary, T. J.; Faleh, M. N.

    2000-01-01

    . Tool steel 61CrV5, 50 NiCr13 and X1000Cr MoV51 were used in the first stage of this investigation. They have been treated as follows: boriding, boriding and tempering and hardening and tempering. The wear tests were conducted under fixed conditions (150 N/mm 2 , 0.48m/sec) with and without lubricant. The wear rate and coefficient of friction of 61Cr Si V5 steel have been studied in the second stage hoping to find the influence of working conditions on these parameters and then to compare these results with the case of hardening and tempering which is the usual case in the actual working field. The study gives a good indication about the improvement achieved in boriding and tempering cases (∼ 30%) as compared with hardening tempering cases in dry sliding conditions -∼5% with lubricating ones. (authors). 13 refs., 19 figs., 1 table

  7. The effect of boriding on wear resistance of cold work tool steel

    International Nuclear Information System (INIS)

    Anzawa, Y; Koyama, S; Shohji, I

    2017-01-01

    Recently, boriding has attracted extensive attention as surface stiffening processing of plain steel. In this research, the influence of processing time on the formation layer of cold work tool steel (KD11MAX) by Al added fused salt bath was examined. In addition, in order to improve the abrasion resistance of KD11MAX, the effect of the treatment of boronization on the formation layer has been investigated. Boriding were performed in molten borax which contained about 10 mass% Al at processing time of 1.8 ∼ 7.2 ks (processing temperature of 1303 K). As a result of the examination, the hardness of the boriding layer becomes about 1900 HV when the processing time of 3.6 ks. Also the abrasion resistance has improved remarkably. Furthermore, it was revealed that the formation layer was boronized iron from the Vickers hardness and analysis of the X-ray diffraction measurement. (paper)

  8. Metal-boride phase formation on tungsten carbide (WC-Co) during microwave plasma chemical vapor deposition

    Energy Technology Data Exchange (ETDEWEB)

    Johnston, Jamin M.; Catledge, Shane A., E-mail: catledge@uab.edu

    2016-02-28

    Graphical abstract: - Highlights: • A detailed phase analysis after PECVD boriding shows WCoB, CoB and/or W{sub 2}CoB{sub 2}. • EDS of PECVD borides shows boron diffusion into the carbide grain structure. • Nanoindentation hardness and modulus of borides is 23–27 GPa and 600–780 GPa. • Scratch testing shows hard coating with cracking at 40N and spallation at 70N. - Abstract: Strengthening of cemented tungsten carbide by boriding is used to improve the wear resistance and lifetime of carbide tools; however, many conventional boriding techniques render the bulk carbide too brittle for extreme conditions, such as hard rock drilling. This research explored the variation in metal-boride phase formation during the microwave plasma enhanced chemical vapor deposition process at surface temperatures from 700 to 1100 °C. We showed several well-adhered metal-boride surface layers consisting of WCoB, CoB and/or W{sub 2}CoB{sub 2} with average hardness from 23 to 27 GPa and average elastic modulus of 600–730 GPa. The metal-boride interlayer was shown to be an effective diffusion barrier against elemental cobalt; migration of elemental cobalt to the surface of the interlayer was significantly reduced. A combination of glancing angle X-ray diffraction, electron dispersive spectroscopy, nanoindentation and scratch testing was used to evaluate the surface composition and material properties. An evaluation of the material properties shows that plasma enhanced chemical vapor deposited borides formed at substrate temperatures of 800 °C, 850 °C, 900 °C and 1000 °C strengthen the material by increasing the hardness and elastic modulus of cemented tungsten carbide. Additionally, these boride surface layers may offer potential for adhesion of ultra-hard carbon coatings.

  9. Metal-boride phase formation on tungsten carbide (WC-Co) during microwave plasma chemical vapor deposition

    International Nuclear Information System (INIS)

    Johnston, Jamin M.; Catledge, Shane A.

    2016-01-01

    Graphical abstract: - Highlights: • A detailed phase analysis after PECVD boriding shows WCoB, CoB and/or W_2CoB_2. • EDS of PECVD borides shows boron diffusion into the carbide grain structure. • Nanoindentation hardness and modulus of borides is 23–27 GPa and 600–780 GPa. • Scratch testing shows hard coating with cracking at 40N and spallation at 70N. - Abstract: Strengthening of cemented tungsten carbide by boriding is used to improve the wear resistance and lifetime of carbide tools; however, many conventional boriding techniques render the bulk carbide too brittle for extreme conditions, such as hard rock drilling. This research explored the variation in metal-boride phase formation during the microwave plasma enhanced chemical vapor deposition process at surface temperatures from 700 to 1100 °C. We showed several well-adhered metal-boride surface layers consisting of WCoB, CoB and/or W_2CoB_2 with average hardness from 23 to 27 GPa and average elastic modulus of 600–730 GPa. The metal-boride interlayer was shown to be an effective diffusion barrier against elemental cobalt; migration of elemental cobalt to the surface of the interlayer was significantly reduced. A combination of glancing angle X-ray diffraction, electron dispersive spectroscopy, nanoindentation and scratch testing was used to evaluate the surface composition and material properties. An evaluation of the material properties shows that plasma enhanced chemical vapor deposited borides formed at substrate temperatures of 800 °C, 850 °C, 900 °C and 1000 °C strengthen the material by increasing the hardness and elastic modulus of cemented tungsten carbide. Additionally, these boride surface layers may offer potential for adhesion of ultra-hard carbon coatings.

  10. Boride-based nano-laminates with MAX-phase-like behaviour

    International Nuclear Information System (INIS)

    Telle, Rainer; Momozawa, Ai; Music, Denis; Schneider, Jochen M.

    2006-01-01

    MAX-phases being usually composed of transition metals, group A elements and carbon/nitrogen are considered interesting materials for many applications because of their tremendous bulk modulus, 'reversible' plasticity, and machinability. This is mainly due to their unique kind of bonding comprising covalent, ionic as well as metallic bonds providing 'easy' planes of rupture and deformability due to the layered crystal structures. In transition metal boride systems, similar types of bonding are available. In particular the W 2 B 5 -structure type and its stacking variations allow the synthesis of strongly layered crystal structures exhibiting unique delamination phenomena. The paper presents ab initio calculations showing the similarities of bonding between the ternary carbides and the corresponding ternary or quaternary borides. Formation of boride-based nano-laminates from auxiliary liquid phases, from the melt as well as during sintering and precipitation from supersaturated solid solutions will be discussed by means of SEM and TEM studies. The role of impurities weakening the interlayer bonding will be addressed in particular. The pronounced cleavage parallel to the basal plane gives rise for crack deflection and pull-out mechanisms if the laminates are dispersed in brittle matrices such as boron carbide, silicon carbide or other transition metal borides. - Graphical abstract: Some transition metal borides crystallise in a layered structure of alternating stacks of metal and boron atoms giving rise for strongly anisotropic properties. Their preferred cleavage parallel and the deformability perpendicular to the basal plan are similar to the peculiar mechanical behaviour recently described for MAX-phases. Ab initio calculations of the crystal structure prove the weak bonds between the layers for a variety of borides which can be used to reinforce ceramic materials on a nano-scale level

  11. Electrosynthesis of tantalum borides in oxygen-free and oxygen-containing fluoride melts

    DEFF Research Database (Denmark)

    Polyakova, L.P.; Polyakov, E.G.; Makarova, O.V.

    2001-01-01

    Results of electrosynthesis of tantalum borides in fluoride and oxyfluoride melts are compared. It is shown that the single-phase X-ray-amorphous micro-layered coatings form only in the latter case. Linear and square-wave voltammetry, complemented by X-ray diffraction analysis, IR spectroscopy...

  12. Micro-Abrasion Wear Resistance of Borided 316L Stainless Steel and AISI 1018 Steel

    Science.gov (United States)

    Reséndiz-Calderon, C. D.; Rodríguez-Castro, G. A.; Meneses-Amador, A.; Campos-Silva, I. E.; Andraca-Adame, J.; Palomar-Pardavé, M. E.; Gallardo-Hernández, E. A.

    2017-11-01

    The 316L stainless steel has high corrosion resistance but low tribological performance. In different industrial sectors (biomedical, chemical, petrochemical, and nuclear engineering), improvement upon wear resistance of 316L stainless steel components using accessible and inexpensive methods is critical. The AISI 1018 steel is widely used in industry, but its tribological performance is not the best among steels. Therefore, in this study the behavior of the borided 316L stainless steel and 1018 steel is evaluated under micro-abrasion wear. The boriding was carried out at 1223 K over 6 h of exposure time, resulting in a biphase layer composed of FeB/Fe2B phases. In order to evaluate Fe2B phase with no influence from FeB phase, AISI 1018 steel samples were borided at 1273 K for over 20 min and then diffusion annealed at 1273 K over 2 h to obtain a Fe2B mono-phase layer. Micro-abrasion wear resistance was evaluated by a commercial micro-abrasion testing rig using a mix of F-1200 SiC particles with deionized water as abrasive slurry. The obtained wear rates for FeB and Fe2B phases and for the 316L stainless steel were compared. Wear resistance of 316L stainless steel increases after boriding. The wear mechanisms for both phases and for the stainless steel were identified. Also, transient conditions for rolling and grooving abrasion were determined for the FeB and Fe2B phases.

  13. Growth kinetics of boride layers formed on 99.0% purity nickel

    Indian Academy of Sciences (India)

    abrasion wear, corrosion and high oxidation resistance com- pared with other ... Ni and Ni-base alloys are used in various industrial plants and equipment for their high ... with 1000-grit emery paper before the boronizing process. The boriding ...

  14. Kinetics of boride layers formed on the surface of AISI 4140 steel

    International Nuclear Information System (INIS)

    Sen, S.; Sen, U.; Bindal, C.

    2004-01-01

    The present study reports on boride layer growth kinetics of borided AISI 4140 steel. Steels were boronized in molten borax, boric acid and ferro-silicon bath at 1123 K 1173 K and 1223 K for 2, 4, 6 and 8 hours. Boride layer thickness ranged from 38.4 to 225 μm. Layer growth kinetics were analysed by measuring the extent of penetration of FeB and Fe 2 B sublayers as a function of boronizing time and temperature in the range of 1123-1223 K. The depth of the tips of the most deeply penetrated FeB and Fe 2 B needles are taken as measures for diffusion in the fast directions. The kinetics of the reaction, K=K 0 exp(-Q/RT) have also been determined by varying the boriding temperature and time. The results showed that K increase with boronizing temperature. Activation energy (Q) for present study was determined as 215 kj.mol -1 . The diffusion coefficient (K) ranged from 3 x 10 -9 cm 2 s -1 to 2 x 10 -8 cm 2 s -1 . Also temperature-dependent constant (K 0 ) at temperatures 1123 K, 1173 K and 1223 K was 179.4 cm 2 s -1 . (orig.)

  15. Kinetics of boride layers formed on the surface of AISI 4140 steel

    Energy Technology Data Exchange (ETDEWEB)

    Sen, S.; Sen, U. [Sakarya Univ., Dept. of Metal Education, Sakarya (Turkey); Bindal, C. [Sakarya Univ., Dept. of Materials and Metallurgy, Sakarya (Turkey)

    2004-07-01

    The present study reports on boride layer growth kinetics of borided AISI 4140 steel. Steels were boronized in molten borax, boric acid and ferro-silicon bath at 1123 K 1173 K and 1223 K for 2, 4, 6 and 8 hours. Boride layer thickness ranged from 38.4 to 225 {mu}m. Layer growth kinetics were analysed by measuring the extent of penetration of FeB and Fe{sub 2}B sublayers as a function of boronizing time and temperature in the range of 1123-1223 K. The depth of the tips of the most deeply penetrated FeB and Fe{sub 2}B needles are taken as measures for diffusion in the fast directions. The kinetics of the reaction, K=K{sub 0} exp(-Q/RT) have also been determined by varying the boriding temperature and time. The results showed that K increase with boronizing temperature. Activation energy (Q) for present study was determined as 215 kj.mol{sup -1}. The diffusion coefficient (K) ranged from 3 x 10{sup -9} cm{sup 2}s{sup -1} to 2 x 10{sup -8} cm{sup 2}s{sup -1}. Also temperature-dependent constant (K{sub 0}) at temperatures 1123 K, 1173 K and 1223 K was 179.4 cm{sup 2}s{sup -1}. (orig.)

  16. 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.

  17. Additive-assisted synthesis of boride, carbide, and nitride micro/nanocrystals

    International Nuclear Information System (INIS)

    Chen, Bo; Yang, Lishan; Heng, Hua; Chen, Jingzhong; Zhang, Linfei; Xu, Liqiang; Qian, Yitai; Yang, Jian

    2012-01-01

    General and simple methods for the syntheses of borides, carbides and nitrides are highly desirable, since those materials have unique physical properties and promising applications. Here, a series of boride (TiB 2 , ZrB 2 , NbB 2 , CeB 6 , PrB 6 , SmB 6 , EuB 6 , LaB 6 ), carbide (SiC, TiC, NbC, WC) and nitride (TiN, BN, AlN, MgSiN 2 , VN) micro/nanocrystals were prepared from related oxides and amorphous boron/active carbon/NaN 3 with the assistance of metallic Na and elemental S. In-situ temperature monitoring showed that the reaction temperature could increase quickly to ∼850 °C, once the autoclave was heated to 100 °C. Such a rapid temperature increase was attributed to the intense exothermic reaction between Na and S, which assisted the formation of borides, carbides and nitrides. The as-obtained products were characterized by XRD, SEM, TEM, and HRTEM techniques. Results in this report will greatly benefit the future extension of this approach to other compounds. - Graphical abstract: An additive-assisted approach is successfully developed for the syntheses of borides, carbides and nitrides micro/nanocrystals with the assistance of the exothermic reaction between Na and S. Highlights: ► An additive-assisted synthesis strategy is developed for a number of borides, carbides and nitrides. ► The reaction mechanism is demonstrated by the case of SiC nanowires. ► The formation of SiC nanowires is initiated by the exothermic reaction of Na and S.

  18. 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

  19. Ni/boride interfaces and environmental embrittlement in Ni-based superalloys: A first-principles study

    International Nuclear Information System (INIS)

    Sanyal, Suchismita; Waghmare, Umesh V.; Hanlon, Timothy; Hall, Ernest L.

    2011-01-01

    Highlights: ► Fracture strengths of Ni/boride interfaces through first-principles calculations. ► Fracture strengths of Ni/boride interfaces are higher than Ni/Ni 3 Al and NiΣ5 grain boundaries. ► Ni/boride interfaces have higher resistance to O-embrittlement than Ni/Ni 3 Al and NiΣ5 grain boundaries. ► CrMo-borides are more effective than Cr-borides in resisting O-embrittlement. ► Electronegativity differences between alloying elements correlate with fracture strengths. - Abstract: Motivated by the vital role played by boride precipitates in Ni-based superalloys in improving mechanical properties such as creep rupture strength, fatigue crack growth rates and improved resistance towards environmental embrittlement , we estimate fracture strength of Ni/boride interfaces through determination of their work of separation using first-principles simulations. We find that the fracture strength of Ni/boride interfaces is higher than that of other commonly occurring interfaces in Ni-alloys, such as Ni Σ-5 grain boundaries and coherent Ni/Ni 3 Al interfaces, and is less susceptible to oxygen-induced embrittlement. Our calculations show how the presence of Mo in Ni/M 5 B 3 (M = Cr, Mo) interfaces leads to additional reduction in oxygen-induced embrittlement. Through Electron-Localization-Function based analyses, we identify the electronic origins of effects of alloying elements on fracture strengths of these interfaces and observe that chemical interactions stemming from electronegativity differences between different atomic species are responsible for the trends in calculated strengths. Our findings should be useful towards designing Ni-based alloys with higher interfacial strengths and reduced oxygen-induced embrittlement.

  20. 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.

  1. 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.)

  2. : 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.

  3. A crossover from high stiffness to high hardness. The case of osmium and its borides

    International Nuclear Information System (INIS)

    Bian, Yongming; Li, Anhu; Liu, Xiaomei; Shanghai Univ. of Engineering Science; Liang, Yongcheng

    2016-01-01

    Transition-metal light-element compounds are currently raising great expectations for hard and superhard materials. Using the widely attracting osmium (Os) and its borides (OsB, Os_2B_3 and OsB_2) as prototypes, we demonstrate by first-principles calculations that heavy transition metals, which possess high stiffness but low hardness, can be converted into highly hard materials by incorporating of light elements to form compounds. Such a crossover is a manifestation that the underlying sources of high stiffness and high hardness are fundamentally different. The stiffness is related to elastic deformation that is closely associated with valence electron density, whereas the hardness depends strongly on plastic deformation that is determined by bonding nature. Therefore, the incorporation of light atoms into transition metal should be a valid pathway of designing hard and superhard materials. This strategy is in principle also applicable to other transition-metal borides, carbides, and nitrides.

  4. A crossover from high stiffness to high hardness. The case of osmium and its borides

    Energy Technology Data Exchange (ETDEWEB)

    Bian, Yongming; Li, Anhu [Tongji Univ., Shanghai (China). School of Mechanical Engineering; Liu, Xiaomei [Tongji Univ., Shanghai (China). School of Mechanical Engineering; Shanghai Univ. of Engineering Science (China). College of Mechanical Engineering; Liang, Yongcheng [Shanghai Ocean Univ. (China). College of Engineering Science and Technology

    2016-07-01

    Transition-metal light-element compounds are currently raising great expectations for hard and superhard materials. Using the widely attracting osmium (Os) and its borides (OsB, Os{sub 2}B{sub 3} and OsB{sub 2}) as prototypes, we demonstrate by first-principles calculations that heavy transition metals, which possess high stiffness but low hardness, can be converted into highly hard materials by incorporating of light elements to form compounds. Such a crossover is a manifestation that the underlying sources of high stiffness and high hardness are fundamentally different. The stiffness is related to elastic deformation that is closely associated with valence electron density, whereas the hardness depends strongly on plastic deformation that is determined by bonding nature. Therefore, the incorporation of light atoms into transition metal should be a valid pathway of designing hard and superhard materials. This strategy is in principle also applicable to other transition-metal borides, carbides, and nitrides.

  5. 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.

  6. 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.

  7. Preparation of molybdenum borides by combustion synthesis involving solid-phase displacement reactions

    International Nuclear Information System (INIS)

    Yeh, C.L.; Hsu, W.S.

    2008-01-01

    Preparation of molybdenum borides of five different phases in the Mo-B binary system (including Mo 2 B, MoB, MoB 2 , Mo 2 B 5 , and MoB 4 ) was performed by self-propagating high-temperature synthesis (SHS) with two kinds of the reactant samples. When elemental powder compacts with an exact stoichiometry corresponding to the boride phase were employed, self-sustaining reaction was only achieved in the sample with Mo:B = 1:1 and nearly single-phase MoB was yielded. Therefore, the other four boride compounds were prepared from the reactant compacts composed of MoO 3 , Mo, and B powders, within which the displacement reaction of MoO 3 with boron was involved in combustion synthesis. Experimental evidence shows that the extent of displacement reaction in the overall reaction has a significant impact on sustainability of the synthesis reaction, combustion temperature, reaction front velocity, and composition of the end product. An increase in the solid-phase displacement reaction taking place during the SHS process contributes more heat flux to the synthesis reaction, thus resulting in the increase of combustion temperature and enhancement of the reaction front velocity. Based upon the XRD analysis, formation of Mo 2 B, MoB 2 , and Mo 2 B 5 as the dominant boride phase in the end product was successful through the SHS reaction with powder compacts under appropriate stoichiometries between MoO 3 , Mo, and B. However, a poor conversion was observed in the synthesis of MoB 4 . The powder compact prepared for the production of MoB 4 yielded mostly Mo 2 B 5

  8. Growth kinetics of borided layers: Artificial neural network and least square approaches

    Science.gov (United States)

    Campos, I.; Islas, M.; Ramírez, G.; VillaVelázquez, C.; Mota, C.

    2007-05-01

    The present study evaluates the growth kinetics of the boride layer Fe 2B in AISI 1045 steel, by means of neural networks and the least square techniques. The Fe 2B phase was formed at the material surface using the paste boriding process. The surface boron potential was modified considering different boron paste thicknesses, with exposure times of 2, 4 and 6 h, and treatment temperatures of 1193, 1223 and 1273 K. The neural network and the least square models were set by the layer thickness of Fe 2B phase, and assuming that the growth of the boride layer follows a parabolic law. The reliability of the techniques used is compared with a set of experiments at a temperature of 1223 K with 5 h of treatment time and boron potentials of 2, 3, 4 and 5 mm. The results of the Fe 2B layer thicknesses show a mean error of 5.31% for the neural network and 3.42% for the least square method.

  9. Structure of superhard tungsten tetraboride: A missing link between MB2 and MB12 higher borides

    Science.gov (United States)

    Lech, Andrew T.; Turner, Christopher L.; Mohammadi, Reza; Tolbert, Sarah H.; Kaner, Richard B.

    2015-01-01

    Superhard metals are of interest as possible replacements with enhanced properties over the metal carbides commonly used in cutting, drilling, and wear-resistant tooling. Of the superhard metals, the highest boride of tungsten—often referred to as WB4 and sometimes as W1–xB3—is one of the most promising candidates. The structure of this boride, however, has never been fully resolved, despite the fact that it was discovered in 1961—a fact that severely limits our understanding of its structure–property relationships and has generated increasing controversy in the literature. Here, we present a new crystallographic model of this compound based on refinement against time-of-flight neutron diffraction data. Contrary to previous X-ray–only structural refinements, there is strong evidence for the presence of interstitial arrangements of boron atoms and polyhedral bonding. The formation of these polyhedra—slightly distorted boron cuboctahedra—appears to be dependent upon the defective nature of the tungsten-deficient metal sublattice. This previously unidentified structure type has an intermediary relationship between MB2 and MB12 type boride polymorphs. Manipulation of the fractionally occupied metal and boron sites may provide insight for the rational design of new superhard metals. PMID:25733870

  10. Synthesis of borides in molybdenum implanted by B+ ions under thermal and electron annealing

    International Nuclear Information System (INIS)

    Kazdaev, Kh.R.; Akchulakov, M.T.; Bayadilov, E.M.; Ehngel'ko, V.I.; Lazarenko, A.V.; Chebukov, E.S.

    1989-01-01

    The possibility of formation of borides in the near surface layers of monocrystalline molybdenum implanted by boron ions at 35 keV energy under thermal and pulsed electron annealing by an electon beam at 140 keV energy is investigated. It is found that implantation of boron ions into molybdenum with subsequent thermal annealing permits to produce both molybdenum monoboride (α-MoB) and boride (γ-Mo 2 B) with rather different formation mechanisms. Formation of the α-MoB phase occurs with the temperature elevation from the centers appeared during implantation, while the γ-Mo 2 B phase appears only on heating the implanted layers up to definite temperature as a result of the phase transformation of the solid solution into a chemical compound. Pulsed electron annealing instead of thermal annealing results mainly in formation of molybdenum boride (γ-Mo 2 B), the state of structure is determined by the degree of heating of implanted layers and their durable stay at temperatures exceeding the threshold values

  11. 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.

  12. 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...

  13. 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

  14. 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

  15. Identification of an eta boride phase as a crystallization product of a NiMoFeB amorphous alloy

    International Nuclear Information System (INIS)

    Kim, Y.W.; Rabenberg, L.; Bourell, D.L.

    1988-01-01

    A new, apparently metastable, Mo--Ni boride phase has been observed in transmission electron microscope samples of rapidly consolidated MoNiFeB metallic glass powders. The phase is cubic with lattice parameter 1.083 nm. Its space group as determined by electron diffraction is Fd3-barm and its approximate composition is Mo 3 Ni 3 B. Because its structure, its composition, and its role as a transition phase are analogous to those of eta carbide (M 6 C) in steels and cemented carbides, this phase has tentatively been named ''eta boride.''

  16. Successive determinations of metals and boron in metal borides by chelatometric and alkalimetric titrations

    International Nuclear Information System (INIS)

    Takahashi, Yasuo; Higashi, Iwami; Atoda, Tetzuzo

    1976-01-01

    Based on the investigation of chemical reactivities of metal borides and of the metal chelate effects on the alkalimetric titration of boron, a method of successive determinations of metals and boron of Mn-, Fe-, Cu- and Al-borides has been developed. The procedure is as follows: (1) Mn-, Fe- and Cu-borides: Dissolve 10 to 30 mg of a sample in a mixture of 3 ml of 3N HNO 3 , 3 ml of 3N H 2 SO 4 and 0.3 ml of 10% H 2 O 2 by heating in a quartz flask equipped with a reflux condenser. Cool the solution obtained, add 0.02M CyDTA solution in excess and neutralize to pH 3 with 2N NaOH solution. Boil the solution for several minutes to ensure the formation of the metal chelate. After cooling, adjust the pH exactly to 6.7 with 0.5 M NaHCO 3 solution, and then determine the metal concentration by back-titrating the excess CyDTA with 0.01M ZnSO 4 solution using MTB as an indicator. After the titration is over, make the solution to pH 3 with 2N H 2 SO 4 and boil for several minutes to expel CO 2 . Cool the solution, adjust the pH exactly to 7.0 with 0.1N CO 2 -free NaOH solution and add 5 g of mannite and ten drops of 0.1% phenolphthalein solution. Finally, titrate the mannite-boric acid complex with 0.05N NaOH solution until the pink tinge is observed (pH 8.2). (2) Al-boride: Fuse 10 to 30 mg of a sample with a mixture of 1.5 g of Na 2 CO 3 and 0.3 g of KNO 3 in a nickel crucible. Digest the melt with water and filter off the residue (nickel oxide). Add 0.01 M EDTA solution in excess to the filterate and make it to pH 3 with 2N H 2 SO 4 . Analytical Results obtained by the present method agree well with those by other methods. The present method takes only 40 minutes, whereas several hours are required to determine metal and boron by other methods. (auth.)

  17. 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

  18. 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)

  19. 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)

  20. 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.

  1. 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

  2. Boron-dependency of molybdenum boride electrocatalysts for the hydrogen evolution reaction

    Energy Technology Data Exchange (ETDEWEB)

    Park, Hyounmyung; Encinas, Andrew; Fokwa, Boniface P.T. [Department of Chemistry, University of California, Riverside, CA (United States); Department of Chemical and Environmental Engineering, University of California, Riverside, CA (United States); Scheifers, Jan P.; Zhang, Yuemei [Department of Chemistry, University of California, Riverside, CA (United States)

    2017-05-08

    Molybdenum-based materials have been considered as alternative catalysts to noble metals, such as platinum, for the hydrogen evolution reaction (HER). We have synthesized four binary bulk molybdenum borides Mo{sub 2}B, α-MoB, β-MoB, and MoB{sub 2} by arc-melting. All four phases were tested for their electrocatalytic activity (linear sweep voltammetry) and stability (cyclic voltammetry) with respect to the HER in acidic conditions. Three of these phases were studied for their HER activity and by X-ray photoelectron spectroscopy (XPS) for the first time; MoB{sub 2} and β-MoB show excellent activity in the same range as the recently reported α-MoB and β-Mo{sub 2}C phases, while the molybdenum richest phase Mo{sub 2}B show significantly lower HER activity, indicating a strong boron-dependency of these borides for the HER. In addition, MoB{sub 2} and β-MoB show long-term cycle stability in acidic solution. (copyright 2017 Wiley-VCH Verlag GmbH and Co. KGaA, Weinheim)

  3. Characterization of boride-based powders and detonation gun sprayed cermet coatings

    International Nuclear Information System (INIS)

    Keraenen, J.; Stenberg, T.; Maentylae, T.

    1995-01-01

    Detonation gun sprayed (DGS) cermet coatings containing complex ternary transition metal boride as hard particles dispersed in a stainless steel or nickel based superalloy matrix have been characterized. Microstructure of the coatings, as well as powders, were studied with optical microscopy, scanning electron microscopy (SEM), X-ray diffraction (XRD) and analytical transmission electron microscopy (AEM). X-ray microanalysis of the coatings were carried out using energy dispersive X-ray spectrometer (EDS) attached to the SEM and AEM. Moreover, abrasion wear resistance of the coatings was evaluated with a rubber wheel abrasion test equipment. The general microstructure of studied coatings appeared to be heterogeneous in the terms of the distribution, size and crystallographic nature of the phases. Nonetheless, very low porosities were obtained and in the coatings the oxide phase as well as the unmelted particles and the formation of oxide phase were avoided by optimization of DGS parameters. So far the abrasive wear resistance of boride-based cermet coatings is not so good as that of the WC-12Co coatings

  4. Boron-dependency of molybdenum boride electrocatalysts for the hydrogen evolution reaction

    International Nuclear Information System (INIS)

    Park, Hyounmyung; Encinas, Andrew; Fokwa, Boniface P.T.; Scheifers, Jan P.; Zhang, Yuemei

    2017-01-01

    Molybdenum-based materials have been considered as alternative catalysts to noble metals, such as platinum, for the hydrogen evolution reaction (HER). We have synthesized four binary bulk molybdenum borides Mo_2B, α-MoB, β-MoB, and MoB_2 by arc-melting. All four phases were tested for their electrocatalytic activity (linear sweep voltammetry) and stability (cyclic voltammetry) with respect to the HER in acidic conditions. Three of these phases were studied for their HER activity and by X-ray photoelectron spectroscopy (XPS) for the first time; MoB_2 and β-MoB show excellent activity in the same range as the recently reported α-MoB and β-Mo_2C phases, while the molybdenum richest phase Mo_2B show significantly lower HER activity, indicating a strong boron-dependency of these borides for the HER. In addition, MoB_2 and β-MoB show long-term cycle stability in acidic solution. (copyright 2017 Wiley-VCH Verlag GmbH and Co. KGaA, Weinheim)

  5. 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.

  6. 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

  7. Elevated temperature tensile properties of borated 304 stainless steel: Effect of boride dispersion on strength and ductility

    International Nuclear Information System (INIS)

    Stephens, J.J.; Sorenson, K.B.; McConnell, P.

    1991-01-01

    This paper has documented the increase in strain to fracture and yield strength obtained with Grade A versions of types 304B5 and 304B7 relative to their respective Grade B, counterparts. The apparent microstructural reason for these property increases is the finer dispersion of boride in the Grade A material, obtained by means of a Powder Metallurgy process, relative to the conventional Grade B material which is produced using an Ingot Metallurgy process. The area size distribution of borides can be well approximated using a log-normal distribution, with the largest boride particles in the Grade B material having areas in the range of 450--600 μm 2 . By comparison, the largest boride particles in the Grade A material have areas nearly an order of magnitude smaller than the largest particles in their Grade B counterparts. A Section III ASME B ampersand PV code case inquiry has been initiated for non-welded versions of 304B4A, 3045A and 3046A ,material

  8. Wear resistance of laser-deposited boride reinforced Ti-Nb-Zr-Ta alloy composites for orthopedic implants

    International Nuclear Information System (INIS)

    Samuel, Sonia; Nag, Soumya; Scharf, Thomas W.; Banerjee, Rajarshi

    2008-01-01

    The inherently poor wear resistance of titanium alloys limits their application as femoral heads in femoral (hip) implants. Reinforcing the soft matrix of titanium alloys (including new generation β-Ti alloys) with hard ceramic precipitates such as borides offers the possibility of substantially enhancing the wear resistance of these composites. The present study discusses the microstructure and wear resistance of laser-deposited boride reinforced composites based on Ti-Nb-Zr-Ta alloys. These composites have been deposited using the LENS TM process from a blend of elemental Ti, Nb, Zr, Ta, and boron powders and consist of complex borides dispersed in a matrix of β-Ti. The wear resistance of these composites has been compared with that of Ti-6Al-4V ELI, the current material of choice for orthopedic femoral implants, against two types of counterfaces, hard Si 3 N 4 and softer SS440C stainless steel. Results suggest a substantial improvement in the wear resistance of the boride reinforced Ti-Nb-Zr-Ta alloys as compared with Ti-6Al-4V ELI against the softer counterface of SS440. The presence of an oxide layer on the surface of these alloys and composites also appears to have a substantial effect in terms of enhanced wear resistance

  9. Effect of borides on hot deformation behavior and microstructure evolution of powder metallurgy high borated stainless steel

    Energy Technology Data Exchange (ETDEWEB)

    Zhou, Xuan [State Key Laboratory of Metastable Materials Science and Technology, College of Materials Science and Engineering, Yanshan University, Qinhuangdao 066004 (China); Wang, Mingjia, E-mail: mingjiawangysu@126.com [State Key Laboratory of Metastable Materials Science and Technology, College of Materials Science and Engineering, Yanshan University, Qinhuangdao 066004 (China); Fu, Yifeng [State Key Laboratory of Metastable Materials Science and Technology, College of Materials Science and Engineering, Yanshan University, Qinhuangdao 066004 (China); Wang, Zixi; Li, Yanmei [Yanming Alloy Roll Co. Ltd, Qinhuangdao 066004 (China); Yang, Shunkai; Zhao, Hongchang; Li, Hangbo [State Key Laboratory of Metastable Materials Science and Technology, College of Materials Science and Engineering, Yanshan University, Qinhuangdao 066004 (China)

    2017-02-15

    To investigate borides effect on the hot deformation behavior and microstructure evolution of powder metallurgy high borated stainless steel, hot compression tests at the temperatures of 950– 1150 °C and the strain rates of 0.01– 10 s{sup −1} were performed. Flow stress curves indicated that borides increased the material's stress level at low temperature but the strength was sacrificed at temperatures above 1100 °C. A hyperbolic-sine equation was used to characterize the dependence of the flow stress on the deformation temperature and strain rate. The hot deformation activation energy and stress exponent were determined to be 355 kJ/mol and 3.2, respectively. The main factors leading to activation energy and stress exponent of studied steel lower than those of commercial 304 stainless steel were discussed. Processing maps at the strains of 0.1, 0.3, 0.5, and 0.7 showed that flow instability mainly concentrated at 950– 1150 °C and strain rate higher than 0.6 s{sup −1}. Results of microstructure illustrated that dynamic recrystallization was fully completed at both high temperature-low strain rate and low temperature-high strain rate. In the instability region cracks were generated in addition to cavities. Interestingly, borides maintained a preferential orientation resulting from particle rotation during compression. - Highlights: •The decrement of activation energy was affected by boride and boron solution. •The decrease of stress exponent was influenced by composition and Cottrell atmosphere. •Boride represented a preferential orientation caused by particle rotation.

  10. 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

  11. 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

  12. 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)

  13. High Temperature Sliding Wear of NiAl-based Coatings Reinforced by Borides

    Directory of Open Access Journals (Sweden)

    Oleksandr UMANSKYI

    2016-05-01

    Full Text Available The development of composite materials (CM in the systems “metal-refractory compound” is one of the up-to-date trends in design of novel materials aimed at operating under the conditions of significant loads at high temperature. To design such material, NiAl, which is widely used for deposition of protective coatings on parts of gas-turbine engines, was selected for a matrix. To strengthen a NiAl under the conditions of intense wear and a broad temperature range (up to 1000 °C, it is reasonable to add refractory inclusions. Introduction of refractory borides into matrix leads to a marked increase in metal wear resistance. In order to research the behavior of the designed composites at high temperatures and to study the influence of oxides on the friction processes, the authors carried out high temperature oxidation of CM of the above systems at 1000 °С for 90 min. It was determined that all of the composites were oxidized selectively and that the thickness of oxide layers formed on the boride inclusions is 3 – 7 times that on the oxides formed on the NiAl matrix. The mechanism of wear of gas-thermal coatings of the NiAl – МеB2 systems was studied for conditions of high temperature tribotests using the «pin-on-disc» technique. The obtained results indicate that introduction of TiB2, CrB2 and ZrB2 leads to their more intense oxidation during high temperature tribotests as compared to the matrix. The oxides formed on refractory borides act as solid lubricants, which promote a decrease in wear of the contact friction pairs. For more detailed investigation of the effect of tribo-oxidation products on the friction processes, tribotests were conducted for prior oxidized (at 900 °С coatings NiAl – 15 wt.% CrB2 (TiB2, ZrB2.DOI: http://dx.doi.org/10.5755/j01.ms.22.1.8093

  14. Electronic Structure Properties and a Bonding Model of Thermoelectric Half-Heusler and Boride Phases

    Science.gov (United States)

    Simonson, Jack William

    Half-Heusler alloys MNiSn and MCoSb (M = Ti, Zr, Hf) and layered boride intermetallics with structure types YCrB4 and Er 3CrB7 were designed, synthesized, and characterized. The thermoelectric properties of these two classes of alloys were measured from room temperature to 1100 K with the intent of indirectly studying their electronic structure properties and gauging not only their suitability but that of related alloys for high temperature thermoelectric power generation. In the case of the half-Heusler alloys, transition metals were substituted to both the M and Ni/Co sites to study the resultant modifications of the d-orbital-rich portion of the electronic structure near the Fermi energy. This modification and subsequent pinning of the Fermi energy within the gap is discussed herein in terms of first principles electronic structure calculations from the literature. In the half-Heusler alloys, it was found that substitution of transition metals invariably led to a decrease in the thermopower, while the resistivity typically maintained its semiconducting trend. On the other hand, Sn doping in MCoSb type alloys -- a dopant that has been known for some time to be efficient -- was shown to result in high ZT at temperatures in excess of 1000 K. Moreover, the band gaps of the transition metal-doped alloys measured in this work offer insight into the discrepancy between the predicted and measured band gaps in the undoped parent compositions. In the case of the layered boride alloys, on the other hand, few electronic calculations have been published, thus prompting the generalization of a well-known electron counting rule -- which is typically used to study molecular organometallics, boranes, and metallocenes -- to predict the trends in the densities of states of crystalline solids that possess the requisite deltahedral bonding geometry. In accordance with these generalized electronic counting rules, alloys of the form RMB4 (R = Y, Gd, Ho; M = Cr, Mo, W) were measured to

  15. Thermo-emf of cermet films based on rare earth borides

    International Nuclear Information System (INIS)

    Islamgaliev, R.K.; Zyrin, A.V.; Shulishova, O.I.; Shcherbak, I.A

    1987-01-01

    Thermo-emf and electric conductivity of granulated films which contain a solid solution of europium and praseodymium borides Eu 0.5 Pr 0.5 B 6 as a conducting phase, and glass-crystal binder on the base of alummomagnesial fluosilicates as a dielectric phase are studied within the temperature range of 100-1100 K. Thermo-emf of films has a negative sign within the temperature range of 100-500 K and does not exceed 5 μkV/K according to the absolute value which is close to the value of the conducting phase thermo-emf. A negative sign and a small value of thermo-emf are indicative of the charge transfer in granulated films by electrons. Contribution of each of the components into the general thermo-emf is different at high temperatures in different temperature ranges and depends on the individual physico-chemical properties of the used materials

  16. New ternary transition metal borides containing uranium and rare earth elements

    International Nuclear Information System (INIS)

    Rogl, P.; Delong, L.

    1983-01-01

    The new ternary actinide metal diborides U 2 MoB 6 , U 2 ReB 6 , U 2 OsB 6 , URuB 4 and UOsB 4 were prepared and found to crystallize with either the Y 2 ReB 6 or the ThMoB 4 type of structure. LuRuB 4 and LuOsB 4 crystallize with the YCrB 4 type of structure. In a ternary series of solid solutions YRh 3 Bsub(1-x) (0 0 C), boron was found to stabilize a Cu 3 Au type of structure. The superconductivity of the new uranium compounds and of a series of ternary transition metal borides was investigated; no superconductivity was observed for temperatures as low at 1.3-1.5 K. The cubic perovskite or filled Cu 3 Au structure is discussed as a type which is very unfavorable for the occurrence of superconductivity. (Auth.)

  17. Structure-chemical and metallurgical investigations in boride- and boron nitride systems

    International Nuclear Information System (INIS)

    Smid, I.

    1987-01-01

    Thermodynamic phase equilibria in the systems (Ti, Zv, Hf)-B-N were determined in an isothermal cut at 1500 O C and 1 atm. The phase field separation is dominated by the high stability of the metal mononitrides and metal diborides. No ternery compounds were found. There are varying solubilities of B and N in the nitrides and borides. The system Cr-B-N was investigated at 1000 O C under 1 atm argon and vacuum, and at 1400 O C at 1 atm argon and 1 atm nitrogen. For the system Mn-B-N the phase field separation was determined at 900 O C under 1 atm Ar and under vacuum. The properties of hard metals with various binding phases and TiBr as hard constituents were investigated. 6 refs., 6 figs., 6 tabs. (qui)

  18. Structural, electronic and thermal properties of super hard ternary boride, WAlB

    Science.gov (United States)

    Rajpoot, Priyanka; Rastogi, Anugya; Verma, U. P.

    2018-04-01

    A first principle study of the structural, electronic and thermal properties of Tungsten Aluminum Boride (WAlB) using full-potential linearized augmented plane wave (FP-LAPW) in the frame work of density function theory (DFT) have been calculated. The calculated equilibrium structural parameters are in excellent agreement with available experimental results. The calculated electronic band structure reveals that WAlB is metallic in nature. The quasi-harmonic Debye model is applied to study of the temperature and pressure effect on volume, Debye temperature, thermal expansion coefficient and specific heat at constant volume and constant pressure. To the best of our knowledge theoretical investigation of these properties of WAlB is reported for the first time.

  19. PREFACE: The 16th International Symposium on Boron, Borides and Related Materials (ISBB 2008)

    Science.gov (United States)

    Tanaka, Takaho

    2009-07-01

    This volume of Journal of Physics: Conference Series contains invited and contributed peer-reviewed papers that were presented at the 16th International Symposium on Boron, Borides and Related Materials (ISBB 2008), which was held on 7-12 September 2008, at Kunibiki Messe, Matsue, Japan. This triennial symposium has a half-century long history starting from the 1st meeting in 1959 at Asbury Park, New Jersey. We were very pleased to organize ISBB 2008, which gathered chemists, physicists, materials scientists as well as diamond and high-pressure researchers. This meeting had a strong background in the boron-related Japanese research history, which includes the discovery of superconductivity in MgB2 and development of Nd-Fe-B hard magnets and of YB66 soft X-ray monochromator. The scope of ISBB 2008 spans both basic and applied interdisciplinary research that is centered on boron, borides and related materials, and the collection of articles defines the state of the art in research on these materials. The topics are centered on: 1. Preparation of new materials (single crystals, thin films, nanostructures, ceramics, etc) under normal or extreme conditions. 2. Crystal structure and chemical bonding (new crystal structures, nonstoichiometry, defects, clusters, quantum-chemical calculations). 3. Physical and chemical properties (band structure, phonon spectra, superconductivity; optical, electrical, magnetic, emissive, mechanical properties; phase diagrams, thermodynamics, catalytic activity, etc) in a wide range of temperatures and pressures. 4. Applications and prospects (thermoelectric converters, composites, ceramics, coatings, etc) There were a few discoveries of new materials, such as nanomaterials, and developments in applications. Many contributions were related to 4f heavy Fermion systems of rare-earth borides. Exotic mechanisms of magnetism and Kondo effects have been discussed, which may indicate another direction of development of boride. Two special sessions

  20. Interlayer utilization (including metal borides) for subsequent deposition of NSD films via microwave plasma CVD on 316 and 440C stainless steels

    Science.gov (United States)

    Ballinger, Jared

    Diamond thin films have promising applications in numerous fields due to the extreme properties of diamonds in conjunction with the surface enhancement of thin films. Biomedical applications are numerous including temporary implants and various dental and surgical instruments. The unique combination of properties offered by nanostructured diamond films that make it such an attractive surface coating include extreme hardness, low obtainable surface roughness, excellent thermal conductivity, and chemical inertness. Regrettably, numerous problems exist when attempting to coat stainless steel with diamond generating a readily delaminated film: outward diffusion of iron to the surface, inward diffusion of carbon limiting necessary surface carbon precursor, and the mismatch between the coefficients of thermal expansion yielding substantial residual stress. While some exotic methods have been attempted to overcome these hindrances, the most common approach is the use of an intermediate layer between the stainless steel substrate and the diamond thin film. In this research, both 316 stainless steel disks and 440C stainless steel ball bearings were tested with interlayers including discrete coatings and graded, diffusion-based surface enhancements. Titanium nitride and thermochemical diffusion boride interlayers were both examined for their effectiveness at allowing for the growth of continuous and adherent diamond films. Titanium nitride interlayers were deposited by cathodic arc vacuum deposition on 440C bearings. Lower temperature diamond processing resulted in improved surface coverage after cooling, but ultimately, both continuity and adhesion of the nanostructured diamond films were unacceptable. The ability to grow quality diamond films on TiN interlayers is in agreement with previous work on iron and low alloy steel substrates, and the similarly seen inadequate adhesion strength is partially a consequence of the lacking establishment of an interfacial carbide phase

  1. 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

  2. Quantity, size and distribution of borides for aluminium grain refinement by neutron-induced autoradiography (NIAR). Pt. 2

    International Nuclear Information System (INIS)

    Rachlitz, R.; Gaertner, S.; Holze, J.; Krumnacker, M.

    1990-01-01

    Al-Ti-B grain refiners improve the cast structure of aluminium and its alloys, but also cause problems related to the great hardness of the borides and their tendency to agglomerate and settle. Accurate information about the distribution, quantity and size of the TiB 2 particles is needed if material properties are to be improved and the quantity of additives minimized. This information is obtained mostly by NIAR. In laboratory-scale tests Al 99.8 and Al 99.5 were refined using different master alloys added in various quantities. In all cases the commercial master alloy gave the best refining effect. Besides boride particle size distribution and the presence of nuclei and nucleus stabilizers, morphological properties (duplex particles) are obviously of essential importance. It has been demonstrated that the TiB 2 size distribution values determined by NIAR are comparable with those established by optical microscopy measurements. (orig.) [de

  3. Effects of process parameters on tungsten boride production from WO{sub 3} by self propagating high temperature synthesis

    Energy Technology Data Exchange (ETDEWEB)

    Yazici, Sertac [Metallurgical and Materials Engineering Department, Istanbul Technical University, Maslak, Istanbul 34469 (Turkey); Derin, Bora, E-mail: bderin@itu.edu.tr [Metallurgical and Materials Engineering Department, Istanbul Technical University, Maslak, Istanbul 34469 (Turkey)

    2013-01-01

    Highlights: Black-Right-Pointing-Pointer We produced tungsten boride compounds by SHS method. Black-Right-Pointing-Pointer Mg containing byproducts were leached out by using a hot aqueous HCl media. Black-Right-Pointing-Pointer The ratio of W{sub 2}B{sub 5}/WB was found to be {approx}2.0 containing minor phases of W{sub 2}B and W. - Abstract: In the present study, the production parameters of tungsten boride compounds by self-propagating high-temperature synthesis (SHS) method and following leaching process were investigated. In the SHS stage, the products consisting of tungsten borides, magnesium oxide, magnesium borate, and also minor compounds were obtained by using different initial molar ratios of WO{sub 3}, Mg and B{sub 2}O{sub 3} as starting materials. In the leaching step, Mg containing byproducts, i.e. MgO and Mg{sub 3}B{sub 2}O{sub 6}, existed in the selected SHS product synthesized at 1:8:2.5 initial molar ratio of WO{sub 3}:Mg:B{sub 2}O{sub 3} were leached out by using aqueous HCl solution to obtain clean tungsten boride compounds at different experimental parameters which are time, acid concentration and temperature. The acid leaching experiments of the SHS product showed that optimum leaching conditions could be achieved by using 5.8 M HCl at 1/10 S/L ratio and the temperature of 80 Degree-Sign C for 60 min.

  4. On magnetic properties of thorium and uranium borides and Usub(1-x)Thsub(x)Bsub(4) solid solutions

    International Nuclear Information System (INIS)

    Chachkhiani, Z.B.; Chachkhiani, L.G.; Chechernikov, V.I.; Slovyanskikh, V.K.

    1982-01-01

    The dependence of magnetic susceptibility on temperature of UB 4 compound and Usub(1-x)Thsub(x)Bsub(4) alloy system in the 140-1300 K temperature range is investigated. It has been found that paramagnetic susceptibility does not obeys the Curie-Weiss law. The interpretation of experimental results is performed on the basis of Stoner model of collectivized electrons which permits also to explain the magnetic properites of other thorium and uranium borides

  5. 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

  6. 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)

  7. 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

  8. 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...

  9. 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)

  10. 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....

  11. 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)

  12. Suppression of Boride Formation in Transient Liquid Phase Bonding of Pairings of Parent Superalloy Materials with Different Compositions and Grain Structures and Resulting Mechanical Properties

    Science.gov (United States)

    Steuer, Susanne; Singer, Robert F.

    2014-07-01

    Two Ni-based superalloys, columnar grained Alloy 247 and single-crystal PWA1483, are joined by transient liquid phase bonding using an amorphous brazing foil containing boron as a melting point depressant. At lower brazing temperatures, two different morphologies of borides develop in both base materials: plate-like and globular ones. Their ratio to each other is temperature dependent. With very high brazing temperatures, the deleterious boride formation in Alloy 247 can be totally avoided, probably because the three-phase-field moves to higher alloying element contents. For the superalloy PWA1483, the formation of borides cannot be completely avoided at high brazing temperatures as incipient melting occurs. During subsequent solidification of these areas, Chinese-script-like borides precipitate. The mechanical properties (tensile tests at room and elevated temperatures and short-term creep rupture tests at elevated temperatures) for brazed samples without boride precipitation are very promising. Tensile strengths and creep times to 1 pct strain are comparable, respectively, higher than the ones of the weaker parent material for all tested temperatures and creep conditions (from 90 to 100 pct rsp. 175 to 250 pct).

  13. A superconducting battery material: Lithium gold boride (LiAu3B)

    Science.gov (United States)

    Aydin, Sezgin; Şimşek, Mehmet

    2018-04-01

    The superconducting and potential cathode material properties of ternary boride of LiAu3B have been investigated by density functional first principles. The Li-concentration effects on the actual electronic and structural properties, namely the properties of LixAu9B3 (x = 0, 1, 2) sub-systems are studied. It is remarkably shown that the existence of Li-atoms has no considerable effect on the structural properties of Au-B skeleton in LiAu3B. Then, it can be offered as a potential cathode material for Li-ion batteries with the very small volume deviation of 0.42%, and the suitable average open circuit voltage of ∼1.30 V. Furthermore, the vibrational and superconducting properties such as electron-phonon coupling constant (λ) and critical temperature (Tc) of LiAu3B are studied. The calculated results suggest that LiAu3B should be a superconductor with Tc ∼5.8 K, also.

  14. Boride Formation Induced by pcBN Tool Wear in Friction-Stir-Welded Stainless Steels

    Science.gov (United States)

    Park, Seung Hwan C.; Sato, Yutaka S.; Kokawa, Hiroyuki; Okamoto, Kazutaka; Hirano, Satoshi; Inagaki, Masahisa

    2009-03-01

    The wear of polycrystalline cubic boron nitride (pcBN) tool and its effect on second phase formation were investigated in stainless steel friction-stir (FS) welds. The nitrogen content and the flow stress were analyzed in these welds to examine pcBN tool wear. The nitrogen content in stir zone (SZ) was found to be higher in the austenitic stainless steel FS welds than in the ferritic and duplex stainless steel welds. The flow stress of austenitic stainless steels was almost 1.5 times larger than that of ferritic and duplex stainless steels. These results suggest that the higher flow stress causes the severe tool wear in austenitic stainless steels, which results in greater nitrogen pickup in austenitic stainless steel FS welds. From the microstructural observation, a possibility was suggested that Cr-rich borides with a crystallographic structure of Cr2B and Cr5B3 formed through the reaction between the increased boron and nitrogen and the matrix during FS welding (FSW).

  15. Computer simulation of monolayer growth kinetics of Fe2B phase during the paste-boriding process: Influence of the paste thickness

    International Nuclear Information System (INIS)

    Keddam, M.

    2006-01-01

    This paper deals with the effect of boron paste thickness on the study of the monolayer growth kinetics of Fe 2 B phase forming on AISI 1045 steel by the paste-boriding process. A mathematical diffusion model based on the Fick's phenomenological equations was applied in order to estimate the growth rate constant at (Fe 2 B/γ-Fe) interface, the layer thickness of iron boride as well as the associated mass gain depending on the boriding parameters such as time, temperature and surface boron concentration related to the boron paste thickness. The simulation results are found to be in a fairly good agreement with the experimental data derived from the literature

  16. 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

  17. 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.)

  18. 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

  19. 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.

  20. 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...

  1. Synthesis of Binary Transition Metal Nitrides, Carbides and Borides from the Elements in the Laser-Heated Diamond Anvil Cell and Their Structure-Property Relations

    Directory of Open Access Journals (Sweden)

    Lkhamsuren Bayarjargal

    2011-09-01

    Full Text Available Transition metal nitrides, carbides and borides have a high potential for industrial applications as they not only have a high melting point but are generally harder and less compressible than the pure metals. Here we summarize recent advances in the synthesis of binary transition metal nitrides, carbides and borides focusing on the reaction of the elements at extreme conditions generated within the laser-heated diamond anvil cell. The current knowledge of their structures and high-pressure properties like high-(p; T stability, compressibility and hardness is described as obtained from experiments.

  2. Synthesis of Binary Transition Metal Nitrides, Carbides and Borides from the Elements in the Laser-Heated Diamond Anvil Cell and Their Structure-Property Relations

    Science.gov (United States)

    Friedrich, Alexandra; Winkler, Björn; Juarez-Arellano, Erick A.; Bayarjargal, Lkhamsuren

    2011-01-01

    Transition metal nitrides, carbides and borides have a high potential for industrial applications as they not only have a high melting point but are generally harder and less compressible than the pure metals. Here we summarize recent advances in the synthesis of binary transition metal nitrides, carbides and borides focusing on the reaction of the elements at extreme conditions generated within the laser-heated diamond anvil cell. The current knowledge of their structures and high-pressure properties like high-(p,T) stability, compressibility and hardness is described as obtained from experiments. PMID:28824101

  3. 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

  4. 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.

  5. 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.

  6. 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.

  7. Possible multigap type-I superconductivity in the layered boride RuB2

    Science.gov (United States)

    Singh, Jaskaran; Jayaraj, Anooja; Srivastava, D.; Gayen, S.; Thamizhavel, A.; Singh, Yogesh

    2018-02-01

    The structure of the layered transition-metal borides A B2 (A =Os,Ru ) is built up by alternating T and B layers with the B layers forming a puckered honeycomb. Here we report superconducting properties of RuB2 with a Tc≈1.5 K using measurements of the magnetic susceptibility versus temperature T , magnetization M versus magnetic field H , resistivity versus T , and heat capacity versus T at various H . We observe a reduced heat capacity anomaly at Tc given by Δ C /γ Tc≈1.1 suggesting multigap superconductivity. Strong support for this is obtained by the successful fitting of the electronic specific heat data to a two-gap model with gap values Δ1/kBTc≈1.88 and Δ2/kBTc≈1.13 . Additionally, M versus H measurements reveal a behavior consistent with type-I superconductivity. This is confirmed by comparing the experimental critical field ≈122 Oe obtained from extrapolation to T =0 of the H -T phase diagram, with an estimate of the T =0 thermodynamic critical field ≈114 Oe. Additionally, the Ginzburg-Landau parameter was estimated to be κ ≈0.1 -0.66 . These results strongly suggest multigap type-I superconductivity in RuB2. We also calculate the band structure and obtain the Fermi surface for RuB2. The Fermi surface consists of one quasi-two-dimensional sheet and two concentric ellipsoidal sheets very similar to OsB2. An additional small fourth sheet is also found for RuB2. RuB2 could thus be an example of a multigap type-I superconductor.

  8. 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.

  9. 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.)

  10. 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

  11. 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.

  12. 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.

  13. 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.

  14. 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

  15. 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

  16. Microstructural evaluation of a low carbon steel submitted to boriding treatment pre and post GTAW welding; Avaliacao microestrutural de um aco de baixo carbono submetido ao tratamento de boretacao pre e pos-soldagem GTAW

    Energy Technology Data Exchange (ETDEWEB)

    Pollnow, Edilson Nunes; Osorio, Alice Goncalves, E-mail: edilson.pollnow@hotmail.com, E-mail: osorio.alice@gmail.com [Universidade Federal de Pelotas (CDTec/UFPel), Pelotas, RS (Brazil). Centro de Desenvolvimento Tecnologico; Araujo, Douglas Bezerra de, E-mail: dbaraujo@ufu.br [Universidade Federal de Uberlandia (FEMEC/UFU), Uberlandia, MG (Brazil). Faculdade de Engenharia Mecanica; Passos, Thais Andrezza dos; Souza, Daniel, E-mail: thais.andrezza.passos@gmail.com, E-mail: danielsouza@furg.br [Universidade Federal do Rio Grande (EE/FURG), Rio Grande, RS (Brazil). Escola de Engenharia

    2017-04-15

    Studies on surface engineering area are given great importance due to the improvement that surface modifications provide to materials. With a global market that has the need to provide parts and equipment with extended service life and low cost, to support stringent requests and thus maintain its high performance, surface treatments may bring what was impossible into reality. Among the surface treatments that have received attention recently, we have the thermochemical process of boriding. The boriding process consists of saturate the surface of steels and metal alloys with boron. This saturation provides an increase in the surface properties not inherent to the base metal, such as hardness, resistance to abrasion and corrosion. Although the properties of boriding steels have already been studied, the effects that the boriding process perform on the steel during or after the welding processes are not known. Hence, it is the purpose of this study to evaluate the microstructure of a low carbon steel treated with boriding before and after GTAW welding. The results indicated poor metallurgical weldability of low carbon steel with boride layer, with the presence of solidification cracks. Nonetheless, the steel welded previous to boring treatment presented a more ductile nucleus, with harder surface. Although the values of hardness within the nucleus of the steel had dropped drastically at the welded zone after the boring, the surface of this steel showed higher values of hardness due to the boriding layer. This fact should be considered when applications where wear resistance is needed. (author)

  17. Surface decoration through electrostatic interaction leading to enhanced reactivity: Low temperature synthesis of nanostructured chromium borides (CrB and CrB2)

    International Nuclear Information System (INIS)

    Menaka,; Kumar, Bharat; Kumar, Sandeep; Ganguli, A.K.

    2013-01-01

    The present study describes a novel low temperature route at ambient pressure for the synthesis of nanocrystalline chromium borides (CrB and CrB 2 ) without using any flux or additives. The favorable and intimate mixing of nanoparticles of chromium acetate (Cr source) and boron forms an active chromium–boron precursor which decomposes at much lower temperature (400 °C) to form CrB (which is ∼1000 °C less than the known ambient pressure synthesis). The chromium acetate nanoparticles (∼5 nm) decorate the larger boron particles (150–200 nm) due to electrostatic interactions resulting from opposing surface charges of boron (zeta potential:+48.101 mV) and chromium acetate (zeta potential:−4.021 mV) in ethanolic medium and is evident in the TEM micrographs. The above method leads to the formation of pure CrB film like structure at 400 °C and nanospheres (40–60 nm) at 600 °C. Also, chromium diboride (CrB 2 ) nanoparticles (25 nm) could be obtained at 1000 °C. - Graphical abstract: Variation of surface charge of reactants, precursor and the products, chromium borides (CrB and CrB 2 ). Highlights: ► Novel borothermal reduction process for synthesis of chromium boride. ► Significant lowering of reaction temperature to obtain nanocrystalline chromium boride. ► Enhanced reactivity due to appropriate surface interactions

  18. 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

  19. 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 ...

  20. 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.)

  1. 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

  2. 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...

  3. 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 ...

  4. 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

  5. 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

  6. 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.

  7. 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.

  8. 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 ...

  9. 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

  10. 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 ...

  11. 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

  12. 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)

  13. 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.

  14. 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.

  15. Thermodynamic modelling of phase equilibrium in system Ti-B-Si-C, synthesis and phases composition of borides and carbides layers on titanic alloyVT-1 at electron beam treatment in vacuum

    Science.gov (United States)

    Smirnyagina, N. N.; Khaltanova, V. M.; Lapina, A. E.; Dasheev, D. E.

    2017-01-01

    Composite layers on the basis of carbides and borides the titan and silicon on titanic alloy VT-1 are generated at diffused saturation in vacuum. Formation in a composite of MAX phase Ti3SiC2 is shown. Thermodynamic research of phase equilibrium in systems Ti-Si-C and Ti-B-C in the conditions of high vacuum is executed. The thermodynamics, formation mechanisms of superfirm layers borides and carbides of the titan and silicon are investigated.

  16. 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.

  17. 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...

  18. 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

  19. Tunable field emission characteristics of ZnO nanowires coated with varied thickness of lanthanum boride thin films

    International Nuclear Information System (INIS)

    Zhao, C.X.; Li, Y.F.; Chen, Jun; Deng, S.Z.; Xu, N.S.

    2013-01-01

    Lanthanum boride (LaB x ) thin films with various thicknesses were deposited on ZnO nanowire arrays by electron beam evaporation. Field emission characteristics of ZnO nanowires show close dependence on LaB x coating thickness. The turn-on field increases with increasing LaB x coating thickness from 10 nm to 50 nm. The observed phenomena were explained by a model that the tunneling at ZnO/LaB x interface dominates the emission process. - Highlights: ► Coating thickness dependence of field emission characteristics of ZnO nanowires was observed from LaB x coated ZnO nanowires. ► More stable field emission was observed from ZnO nanowires with LaB x coating. ► A model was proposed that the tunneling at ZnO/LaB x interface dominates the emission process

  20. The low-lying quartet electronic states of group 14 diatomic borides XB (X = C, Si, Ge, Sn, Pb)

    Science.gov (United States)

    Pontes, Marcelo A. P.; de Oliveira, Marcos H.; Fernandes, Gabriel F. S.; Da Motta Neto, Joaquim D.; Ferrão, Luiz F. A.; Machado, Francisco B. C.

    2018-04-01

    The present work focuses in the characterization of the low-lying quartet electronic and spin-orbit states of diatomic borides XB, in which X is an element of group 14 (C, Si, Ge, Sn, PB). The wavefunction was obtained at the CASSCF/MRCI level with a quintuple-ζ quality basis set. Scalar relativistic effects were also taken into account. A systematic and comparative analysis of the spectroscopic properties for the title molecular series was carried out, showing that the (1)4Π→X4Σ- transition band is expected to be measurable by emission spectroscopy to the GeB, SnB and PbB molecules, as already observed for the lighter CB and SiB species.

  1. 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

  2. Synthesis, characterization and investigation of thermoelectric properties of selected metal borides; Synthese, Charakterisierung und Untersuchung thermoelektrischer Eigenschaften ausgewaehlter Metallboride

    Energy Technology Data Exchange (ETDEWEB)

    Stober, Frederick

    2012-06-04

    The present work deals with the high-temperature thermoelectric properties of transition metal [eg V, Cr, Mn, Ni, Cu] and lanthanide [e.g. Sc, Y, Gd, Er, Dy]-borides. In particular, intercalation compounds of beta-rhombohedral boron, compounds of the type MB{sub 66}, dodecaborides and hexaborides were examined. In the case of intercalation compounds of beta-rhombohedral boron it was found that the incorporation of metals such as Sc, Mn or Cu result in favorable thermoelectric properties. The reason is most likely the preferred occupation of the metal position M2 instead of M4. Composites, for example, DyB{sub 66}-DyB{sub 12} show high electrical conductivities, high Seebeck effects at high temperatures due to the presence of DyB{sub 12} and low thermal conductivities as a result of the DyB{sub 66} matrix. At 1100K the composite DyB{sub 66}-DyB{sub 12} shows a ZT value of 0.55, thus exceeding the ZT of boron carbide (B{sub 13}C{sub 2}) at this temperature which is considered the best p-type boride material. A composite of ErB{sub 12}-ErB{sub 4}-ErB{sub 2} has negative Seebeck coefficients and shows a ZT value of 0.5 at 840K. Furthermore, the structure of tetragonal Scandiumdodecaboride ScB{sub 12} was solved on the basis of synchrotron data from a crystalline powder, after it has been debated for decades but never fully resolved.

  3. Co3O4 nanoneedle@electroactive nickel boride membrane core/shell arrays: A novel hybrid for enhanced capacity

    International Nuclear Information System (INIS)

    Li, Tingting; Zhu, Congxu; Yang, Xiaogang; Gao, Yuanhao; He, Weiwei; Yue, Hongwei; Zhao, Hongxiao

    2017-01-01

    Graphical abstract: Active nickel boride membrane anchored Co 3 O 4 nanoneedle arrays hybrid is synthesized via rapid interface reaction. The optimized core/shell nanostructure demonstrates greatly enhanced electrochemical properties. Display Omitted -- Highlights: •Active nickel boride membrane anchored Co 3 O 4 nanoneedle arrays core-shell hybrid architectures was fabricated via rapid interface reaction. •Specific capacity was improved by synergy between highly active components and optimized electron transfer microstructure. •The assembled asymmetric supercapacitor device exhibited excellent electrochemical performance. -- Abstract: Exploring novel hybrid materials with efficient microstructure using facile approaches is highly urgent in designing supercapacitor electrodes. Here, the Ni-B membrane was used for coating the porous Co 3 O 4 nanoneedle arrays which supported on the nickel foam (NF) frameworks through a rapid chemical reduction process (denoted as NF/Co 3 O 4 @NiB). The Ni-B membrane both provided sufficient active sites for redox reactions and inhibited the aggregation of formed hybrid architectures. Benefiting from the unique structural design and strongly coupled effects between porous Co 3 O 4 arrays and Ni-B membrane, the resulted NF/Co 3 O 4 @NiB electrode exhibited high areal capacitance of 3.47 F cm −2 (0.48 mAh cm −2 ) at a current density of 2.5 mA cm −2 , an excellent rate capability while maintaining 95.5% capacity retention after 2000 cycles. The asymmetric supercapacitor constructed with the NF/Co 3 O 4 @NiB as positive electrode and hierarchical porous carbon (HPC) as negative electrode also showed ideal capacitive behavior, and simultaneously delivered high energy and power densities. The easily decoration of Ni-B membrane on various active nanoarrays may arouse more novel design about hybrid architectures for large-scale applications.

  4. 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)

  5. 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.

  6. 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.

  7. 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.

  8. 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

  9. 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)

  10. 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.

  11. 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

  12. 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

  13. 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

  14. 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

  15. 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.

  16. 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

  17. 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

  18. 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

  19. 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

  20. 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...

  1. 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

  2. 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

  3. 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.

  4. 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.

  5. 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).

  6. 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.

  7. 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.

  8. 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....

  9. 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.)

  10. 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.)

  11. 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.

  12. 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)

  13. 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)

  14. 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.

  15. 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

  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. A novel route to nanosized molybdenum boride and carbide and/or metallic molybdenum by thermo-synthesis method from MoO3, KBH4, and CCl4

    International Nuclear Information System (INIS)

    Li Yuanzhi; Fan Yining; Chen Yi

    2003-01-01

    Nanosized molybdenum boride and carbide were synthesized from MoO 3 , KBH 4 , and CCl 4 by thermo-synthesis method at lower temperature. The relative content of Mo, Mo 2 C, and molybdenum boride in the product was decided by the molar ratio between MoO 3 , KBH 4 , and CCl 4 . Increasing the molar ratio of CCl 4 to MoO 3 was favorable to the production of Mo 2 C. Increasing the molar ratio of KBH 4 to MoO 3 was favorable to the production of molybdenum boride. By carefully adjusting the reaction conditions and annealing in Ar at 900 deg. C, a single phase of MoB could be obtained

  4. 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.

  5. 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.

  6. 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.

  7. 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.

  8. 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.

  9. 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.

  10. 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

  11. 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

  12. 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.

  13. 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.

  14. 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

  15. 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

  16. Elevated temperature tensile properties of borated 304 stainless steel: Effect of boride dispersion on strength and ductility

    International Nuclear Information System (INIS)

    Stephens, J.J.; Sorenson, K.B.; McConnell, P.

    1992-01-01

    Conventional cast and wrought (open-quotes Ingot Metallurgyclose quotes) borated 304 stainless steel has been used for a number of years in spent fuel storage applications where a combination of structural integrity and neutron criticality control are required. Similar requirements apply for materials used in transport cask baskets. However, in the high boron contents (>1.0 wt. %) which are most useful for criticality control, the conventional cast and wrought material suffers from low ductility as well as low impact toughness. The microstructural reason for these poor properties is the relatively coarse size of the boride particles in these alloys, which act as sites for crack initiation. Recently, a open-quotes premiumclose quotes grade of borated 304 stainless steel has been introduced (Strober and Smith, 1988) which is made by a Powder Metallurgy (PM) process. This material has greatly improved ductility and impact properties relative to the conventional cast and wrought product. In addition, an ASTM specification (ATSM A887) has been developed for borated stainless steel, containing 8 different material Types with respect to boron content - with the highest level (Type B7) having permissible range from 1.75 to 2.25 wt. % boron - and each Type contains two different Grades of material based on tensile and impact properties. While the ASTM specification is properties-based and does not require a specific production process for a particular grade of material, the PM material qualifies as open-quotes Grade Aclose quotes material while the conventional Ingot Metallurgy (IM) material generally qualifies as open-quotes Grade Bclose quotes material. This paper presents a comparison of the tensile properties of PM open-quotes Grade Aclose quotes material with that of the conventional IM open-quotes Grade Bclose quotes material for two selected Types (i.e., boron contents) as defined by the ASTM A887 specification: Types 304B5 and 304B7

  17. The effect of lanthanum boride on the sintering, sintered microstructure and mechanical properties of titanium and titanium alloys

    International Nuclear Information System (INIS)

    Yang, Y.F.; Luo, S.D.; Qian, M.

    2014-01-01

    An addition of ≤0.5 wt% lanthanum boride (LaB 6 ) to powder metallurgy commercially pure Ti (CP-Ti), Ti–6Al–4V and Ti–10V–2Fe–3Al (all in wt%) resulted in improved sintered density, substantial microstructural refinement, and noticeably increased tensile elongation. The addition of LaB 6 led to scavenging of both oxygen (O) and chlorine (Cl) from the titanium powder during sintering, evidenced by the formation of La 2 O 3 and LaCl x O y . The pinning effect of La 2 O 3 , LaCl x O y and TiB inhibited prior-β grain growth and resulted in subsequent smaller α-laths. The formation of nearly equiaxed α-Ti phase is partially attributed to the nucleation effect of α-Ti on TiB. The improved sintered density was caused by B from LaB 6 rather than La, while excessive formation of La 2 O 3 and TiB with an addition of >0.5 wt% LaB 6 resulted in a noticeable decrease in sintered density. The improved tensile elongation with an addition of ≤0.5 wt% LaB 6 was mainly attributed to the scavenging of oxygen by LaB 6 , partially assisted by the improved sintered density. However, an addition of >0.5 wt% LaB 6 led to the formation of large La 2 O 3 aggregates and more brittle TiB whiskers and therefore decreased tensile elongation. Balanced scavenging of O is thus important. The optimal addition of LaB 6 was 0.5 wt% but this may change depending on the powder size of the LaB 6 to be used

  18. 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

  19. 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.

  20. 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.

  1. 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)

  2. 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.

  3. 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.

  4. 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.

  5. 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....

  6. 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

  7. 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.

  8. 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.

  9. 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.

  10. 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)

  11. 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.

  12. 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.

  13. 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)

  14. 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

  15. 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.

  16. 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.

  17. 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

  18. 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.

  19. The effect of lanthanum boride on the sintering, sintered microstructure and mechanical properties of titanium and titanium alloys

    Energy Technology Data Exchange (ETDEWEB)

    Yang, Y.F. [RMIT University, Centre for Additive Manufacturing, School of Aerospace, Mechanical and Manufacturing Engineering, GPO Box 2476, Melbourne VIC 3001 (Australia); Luo, S.D. [The University of Queensland, School of Mechanical and Mining Engineering, Brisbane, QLD 4072 (Australia); Qian, M., E-mail: ma.qian@rmit.edu.au [RMIT University, Centre for Additive Manufacturing, School of Aerospace, Mechanical and Manufacturing Engineering, GPO Box 2476, Melbourne VIC 3001 (Australia)

    2014-11-17

    An addition of ≤0.5 wt% lanthanum boride (LaB{sub 6}) to powder metallurgy commercially pure Ti (CP-Ti), Ti–6Al–4V and Ti–10V–2Fe–3Al (all in wt%) resulted in improved sintered density, substantial microstructural refinement, and noticeably increased tensile elongation. The addition of LaB{sub 6} led to scavenging of both oxygen (O) and chlorine (Cl) from the titanium powder during sintering, evidenced by the formation of La{sub 2}O{sub 3} and LaCl{sub x}O{sub y}. The pinning effect of La{sub 2}O{sub 3}, LaCl{sub x}O{sub y} and TiB inhibited prior-β grain growth and resulted in subsequent smaller α-laths. The formation of nearly equiaxed α-Ti phase is partially attributed to the nucleation effect of α-Ti on TiB. The improved sintered density was caused by B from LaB{sub 6} rather than La, while excessive formation of La{sub 2}O{sub 3} and TiB with an addition of >0.5 wt% LaB{sub 6} resulted in a noticeable decrease in sintered density. The improved tensile elongation with an addition of ≤0.5 wt% LaB{sub 6} was mainly attributed to the scavenging of oxygen by LaB{sub 6}, partially assisted by the improved sintered density. However, an addition of >0.5 wt% LaB{sub 6} led to the formation of large La{sub 2}O{sub 3} aggregates and more brittle TiB whiskers and therefore decreased tensile elongation. Balanced scavenging of O is thus important. The optimal addition of LaB{sub 6} was 0.5 wt% but this may change depending on the powder size of the LaB{sub 6} to be used.

  20. 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

  1. 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)

  2. 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....

  3. 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

  4. 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.

  5. 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.

  6. 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)

  7. 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

  8. New ternary tantalum borides containing boron dumbbells: Experimental and theoretical studies of Ta2OsB2 and TaRuB

    International Nuclear Information System (INIS)

    Mbarki, Mohammed; Touzani, Rachid St.; Rehorn, Christian W.G.; Gladisch, Fabian C.; Fokwa, Boniface P.T.

    2016-01-01

    The new ternary transition metal-rich borides Ta 2 OsB 2 and TaRuB have been successfully synthesized by arc-melting the elements in a water-cooled crucible under an argon atmosphere. The crystal structures of both compounds were solved by single-crystal X-ray diffraction and their metal compositions were confirmed by EDX analysis. It was found that Ta 2 OsB 2 and TaRuB crystallize in the tetragonal Nb 2 OsB 2 (space group P4/mnc, no. 128) and the orthorhombic NbRuB (space group Pmma, no. 51) structure types with lattice parameters a=5.878(2) Å, c=6.857(2) Å and a=10.806(2) Å, b=3.196(1) Å, c=6.312(2) Å, respectively. Furthermore, crystallographic, electronic and bonding characteristics have been studied by density functional theory (DFT). Electronic structure relaxation has confirmed the crystallographic parameters while COHP bonding analysis indicates that B 2 -dummbells are the strongest bonds in both compounds. Moreover, the formation of osmium dumbbells in Ta 2 OsB 2 through a Peierls distortion along the c-axis, is found to be the origin of superstructure formation. Magnetic susceptibility measurements reveal that the two phases are Pauli paramagnets, thus confirming the theoretical DOS prediction of metallic character. Also hints of superconductivity are found in the two phases, however lack of single phase samples has prevented confirmation. Furthermore, the thermodynamic stability of the two modifications of AMB (A=Nb, Ta; M =Ru, Os) are studied using DFT, as new possible phases containing either B 4 - or B 2 -units are predicted, the former being the most thermodynamically stable modification. - Graphical abstract: The two new ternary tantalum borides, Ta 2 OsB 2 and TaRuB, have been discovered. Their crystal structures contain boron dumbbells, which are the strongest bonds. Peirls distortion is found responsible for Os 2 -dumbbells formation in Ta 2 OsB 2 . Ta 2 OsB 2 and TaRuB are Pauli paramagnet and potential superconductors. - Highlights:

  9. 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.

  10. 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'

  11. 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.

  12. 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.

  13. 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.

  14. 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.

  15. 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.

  16. 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.

  17. 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.

  18. 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

  19. 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.

  20. 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

  1. 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)

  2. 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).

  3. 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

  4. 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.

  5. 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)

  6. 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.

  7. 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.

  8. 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.

  9. 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.

  10. 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.

  11. The coloring problem in the solid-state metal boride carbide ScB{sub 2}C{sub 2}. A theoretical analysis

    Energy Technology Data Exchange (ETDEWEB)

    Lassoued, Souheila [Universite de Rennes, Ecole Nationale Superieure de Chimie, UMR 6226 CNRS (France). Inst. des Sciences Chimiques; Universite Kasdi Merbah-Ouargla (Algeria). Faculte des Mathematiques et des Sciences de la Matiere; Boucher, Benoit [Universite de Rennes, Ecole Nationale Superieure de Chimie, UMR 6226 CNRS (France). Inst. des Sciences Chimiques; Max-Planck-Institut fuer Chemische Physik Fester Stoffe, Dresden (Germany); Boutarfaia, Ahmed [Universite Kasdi Merbah-Ouargla (Algeria). Faculte des Mathematiques et des Sciences de la Matiere; Gautier, Regis; Halet, Jean-Francois [Universite de Rennes, Ecole Nationale Superieure de Chimie, UMR 6226 CNRS (France). Inst. des Sciences Chimiques

    2016-08-01

    The electronic properties of the layered ternary metal boride carbide ScB{sub 2}C{sub 2}, the structure of which consists of B/C layers made of fused five- and seven-membered rings alternating with scandium sheets, are analyzed. In particular, the respective positions of the B and C atoms (the so-called coloring problem) are tackled using density functional theory, quantum theory of atoms in molecules, and electron localizability indicator calculations. Results reveal that (i) the most stable coloring minimizes the number of B-B and C-C contacts and maximizes the number of boron atoms in the heptagons, (ii) the compound is metallic in character, and (iii) rather important covalent bonding occurs between the metallic sheets and the boron-carbon network.

  12. 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

  13. 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.

  14. 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

  15. 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.

  16. 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...

  17. 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

  18. 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.

  19. 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

  20. 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

  1. 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)

  2. 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

  3. 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)

  4. 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.

  5. 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.

  6. 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)

  7. 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.

  8. 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.

  9. 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.

  10. 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.

  11. 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.

  12. 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

  13. 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

  14. 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 ...

  15. 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.

  16. 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.

  17. 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.

  18. 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)

  19. 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.

  20. 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...

  1. 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)

  2. 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.

  3. 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.

  4. 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.

  5. 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.

  6. 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.

  7. 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

  8. 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

  9. 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.

  10. 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

  11. 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

  12. 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.

  13. 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'.

  14. 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

  15. 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.

  16. 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.

  17. 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.

  18. 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.

  19. 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...

  20. 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...

  1. 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.

  2. 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

  3. 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.

  4. 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...

  5. 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)

  6. A Study on the Effect of the Boron Potential on the Mechanical Properties of the Borided Layers Obtained by Boron Diffusion at the Surface of AISI 316L Steel

    Directory of Open Access Journals (Sweden)

    E. Hernández-Sánchez

    2014-01-01

    Full Text Available The effect of the boron potential on the thickness and the mechanical properties of borided layers was evaluated. The boron potential was established by means of the available atoms of boron contained in a control volume inside a cylinder. The cylinders were manufactured from AISI 316L steel, and the boriding treatment was performed using the powder pack technique at a temperature of 1273 K over an exposure time of 6 h. Four different internal diameters of the cylinders were evaluated (3.17, 4.76, 6.35, and 7.93 mm. The mechanical properties were evaluated using the Berkovich instrumented indentation technique. The results showed a clear influence of the boron potential on the mechanical properties of the layers. The hardness of the layers was stablished in the range of 16.22 to 21.16 GPa. Young’s modulus values were stablished in the range of 255.96 to 341.37 GPa. Also the fracture toughness and brittleness of the layers reflected the influence of the boron potential supplied during the boriding process. Finally, the influence of the boron potential on the constant of parabolic growth (K was also established as a function of the inner diameter of the cylinders.

  7. 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.

  8. New ternary tantalum borides containing boron dumbbells: Experimental and theoretical studies of Ta{sub 2}OsB{sub 2} and TaRuB

    Energy Technology Data Exchange (ETDEWEB)

    Mbarki, Mohammed; Touzani, Rachid St.; Rehorn, Christian W.G.; Gladisch, Fabian C. [Institute of Inorganic Chemistry, RWTH Aachen University, D-52056 Aachen (Germany); Fokwa, Boniface P.T., E-mail: bfokwa@ucr.edu [Institute of Inorganic Chemistry, RWTH Aachen University, D-52056 Aachen (Germany); Department of Chemistry, University of California Riverside (UCR), Riverside, CA 92521 (United States)

    2016-10-15

    The new ternary transition metal-rich borides Ta{sub 2}OsB{sub 2} and TaRuB have been successfully synthesized by arc-melting the elements in a water-cooled crucible under an argon atmosphere. The crystal structures of both compounds were solved by single-crystal X-ray diffraction and their metal compositions were confirmed by EDX analysis. It was found that Ta{sub 2}OsB{sub 2} and TaRuB crystallize in the tetragonal Nb{sub 2}OsB{sub 2} (space group P4/mnc, no. 128) and the orthorhombic NbRuB (space group Pmma, no. 51) structure types with lattice parameters a=5.878(2) Å, c=6.857(2) Å and a=10.806(2) Å, b=3.196(1) Å, c=6.312(2) Å, respectively. Furthermore, crystallographic, electronic and bonding characteristics have been studied by density functional theory (DFT). Electronic structure relaxation has confirmed the crystallographic parameters while COHP bonding analysis indicates that B{sub 2}-dummbells are the strongest bonds in both compounds. Moreover, the formation of osmium dumbbells in Ta{sub 2}OsB{sub 2} through a Peierls distortion along the c-axis, is found to be the origin of superstructure formation. Magnetic susceptibility measurements reveal that the two phases are Pauli paramagnets, thus confirming the theoretical DOS prediction of metallic character. Also hints of superconductivity are found in the two phases, however lack of single phase samples has prevented confirmation. Furthermore, the thermodynamic stability of the two modifications of AMB (A=Nb, Ta; M =Ru, Os) are studied using DFT, as new possible phases containing either B{sub 4}- or B{sub 2}-units are predicted, the former being the most thermodynamically stable modification. - Graphical abstract: The two new ternary tantalum borides, Ta{sub 2}OsB{sub 2} and TaRuB, have been discovered. Their crystal structures contain boron dumbbells, which are the strongest bonds. Peirls distortion is found responsible for Os{sub 2}-dumbbells formation in Ta{sub 2}OsB{sub 2}. Ta{sub 2}OsB{sub 2} and

  9. 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.

  10. 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.

  11. 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.

  12. Structure and magnetic properties of the 3d transition-metal mono-borides TM–B (TM=Mn, Fe, Co) under pressures

    International Nuclear Information System (INIS)

    Bourourou, Y.; Beldi, L.; Bentria, B.; Gueddouh, A.; Bouhafs, B.

    2014-01-01

    In this paper, spin-polarization and pressure effects on the structural and electronic properties of the 3d transition-metal mono-borides TM–B (TM=Mn, Fe, Co) have been studied by using both local spin-density approximation (LSDA) and generalized gradient approximation (GGA) within the framework of density-functional theory (DFT). At equilibrium, spin-polarization calculations show that MnB and FeB compounds carry magnetic moment. The non-spin-polarization results show that the non-magnetic state is unstable for MnB and FeB compounds, but a stable non-magnetic phase for CoB compound, which is discussed in the framework of the well-known Stoner criterion. The calculated lattice parameters, bulk moduli, their first-pressure derivatives and magnetic moments agree well with experimental and other theoretical results. Significant differences in volume and in bulk modulus were found between the magnetic and non-magnetic case reached 4%, 22%, respectively. The effect of pressure on the crystal structure reflects in a compression of the unit cell volume with a decreasing in the magnetic moment. The density of states of MnB and FeB ferromagnetic compounds are significantly modified under high pressures. The exchange energy decreases with increasing pressure, at approximately V/V 0 =0.6, the exchange energy becomes absent in ferromagnetic compounds causes mirror in upper and lowers half panels. Finally, we notice that spin-polarization and pressure play a crucially important role in determining the electronic and structural properties of 3d transition-metal mono-borides. - Highlights: • Spin polarization and pressure effects on TM–B (TM=Mn, Fe, Co) have been investigated. • The non-spin-polarization results show that the non-magnetic state is stable for CoB. • The magnetic states of MnB and FeB are found more stable than their nonmagnetic states. • We report significant differences between the magnetic and non-magnetic cases. • The density of states of MnB and

  13. Electronic, structural and magnetic studies of niobium borides of group 8 transition metals, Nb2MB2 (M=Fe, Ru, Os) from first principles calculations

    International Nuclear Information System (INIS)

    Touzani, Rachid St.; Fokwa, Boniface P.T.

    2014-01-01

    The Nb 2 FeB 2 phase (U 3 Si 2 -type, space group P4/mbm, no. 127) is known for almost 50 years, but until now its magnetic properties have not been investigated. While the synthesis of Nb 2 OsB 2 (space group P4/mnc, no. 128, a twofold superstructure of U 3 Si 2 -type) with distorted Nb-layers and Os 2 -dumbbells was recently achieved, “Nb 2 RuB 2 ” is still not synthesized and its crystal structure is yet to be revealed. Our first principles density functional theory (DFT) calculations have confirmed not only the experimental structures of Nb 2 FeB 2 and Nb 2 OsB 2 , but also predict “Nb 2 RuB 2 ” to crystalize with the Nb 2 OsB 2 structure type. According to chemical bonding analysis, the homoatomic B–B interactions are optimized and very strong, but relatively strong heteroatomic M–B, B–Nb and M–Nb bonds (M=Fe, Ru, Os) are also found. These interactions, which together build a three-dimensional network, are mainly responsible for the structural stability of these ternary borides. The density-of-states at the Fermi level predicts metallic behavior, as expected, from metal-rich borides. Analysis of possible magnetic structures concluded preferred antiferromagnetic ordering for Nb 2 FeB 2 , originating from ferromagnetic interactions within iron chains and antiferromagnetic exchange interactions between them. -- Graphical abstract: Nb 2 FeB 2 (U 3 Si 2 structure type, space group P4/mbm, no. 127) is predicted to order antiferromagnetically, due to the presence of iron chains which show ferromagnetic interactions in the chains and antiferromagnetic interactions between them. “Nb 2 RuB 2 ” is predicted to crystallize with the recently discovered Nb 2 OsB 2 twofold superstructure (space group P4/mnc, no. 128) of U 3 Si 2 structure type. The building of ruthenium dumbbells instead of chains along [001] is found to be responsible for the stabilization of this superstructure. Highlights: • Nb 2 FeB 2 is predicted to order antiferromagnetically.

  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. Study of Transport and Micro-structural properties of Magnesium Di-Boride Strand under react and bend mode and bend and react mode

    International Nuclear Information System (INIS)

    Kundu, Ananya; Kumar Das, Subrat; Bano, Anees; Pradhan, Subrata

    2017-01-01

    I-V characterization of commercial multi-filamentary Magnesium Di-Boride (MgB 2 ) wire of diameter 0.83 mm were studied in Cryocooler at self-field I-V characterization system under both react and bend mode and bend and react mode for a range of temperature 6 K - 25 K. This study is of practical technical relevance where the heat treatment of the superconducting wire makes the wire less flexible for winding in magnet and in other applications. In the present work the bending diameter was varied from 40 mm to 20 mm and for each case critical current (I c ) of the strand is measured for above range of temperature. A customized sample holder is fabricated and thermally anchored with the 2 nd cold stage of Cryocooler. It is observed from the measurement that the strand is more susceptible to degradation for react and bend cases. The transport measurement of the strand was accompanied by SEM analyses of bend samples. Also the tensile strength of the raw strands and the heat treated strands were carried out at room temperature in Universal Testing Machine (UTM) to have an estimate about the limiting winding tension value during magnet fabrication. (paper)

  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. 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

  19. 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.

  20. 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)

  1. 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.

  2. 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.

  3. 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.

  4. 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)

  5. 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.

  6. 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)

  7. 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

  8. 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.

  9. 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)

  10. 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.

  11. 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)

  12. 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.

  13. 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

  14. 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

  15. 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.)

  16. 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.

  17. 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.

  18. 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.

  19. 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.

  20. Novel Base Metal-Palladium Catalytic Diesel Filter Coating with NO2 Reducing Properties

    DEFF Research Database (Denmark)

    Johansen, K.; Dahl, S.; Mogensen, G.

    2007-01-01

    A novel alternative base metal/palladium coat has been developed that has limited NO2 formation and which even removes NO2 in a wide temperature range.Soot combustion, HC conversion and CO conversion properties are comparable to current platinum based solutions but the coating has a more attracti...... solutions. Furthermore, durability results from base metal/Pd coated DPFs installed on operating taxis and related tests cycle data is given....

  1. Separation of palladium from high-level waste using metal ferro cyanide loaded resins

    International Nuclear Information System (INIS)

    Valsala, T.P.; Joseph, Annie; Yeotikar, R.G.

    2005-01-01

    High-level waste (HLW) is generated during reprocessing of spent fuel. HLW contains corrosion products, unextracted actinides, process chemicals and fission products. A recent trend is there to consider waste as a source of wealth. Among the fission products separation and recovery of platinum group metals have gained great attention. HLW is a good source of palladium of the platinum group metal. The present study shows the feasibility of ion exchange separation of Pd from HLW. (author)

  2. Neutron powder diffraction studies of Hydrogen and Denterium in Palladium Phosphides

    International Nuclear Information System (INIS)

    Andersson, Y.

    1986-01-01

    The use of the Rietveld-type profile refinements on neutron powder diffraction intensity data for determining crystallographic positions of hydrogen and deuterium in metal hydrides is illustrated by results obtained on some hydrogenated and deuterated palladium phosphides. The structural features of the solid solutions of hydrogen and deuterium in Pd/sb15/P/sb2/ Pd/sb6/P and Pd/sb3/P/sb1-u/ (0< u<0.28) are briefly presented and discussed

  3. Novel Role of Carbon Dioxide as a Selective Agent in Palladium-Catalyzed Cyclotrimerization of Alkynes

    Institute of Scientific and Technical Information of China (English)

    李金恒; 谢叶香

    2004-01-01

    Carbon dioxide was found as a selective agent to promote the palladium-catalyzed cyclotrimerization of alkynes in water. Both aryl and alkylacetylenes afforded the corresponding cyclotrimerization products regioselectively in high yields using PdCl2, CuCl2, and CO2 as the catalytic system. However, tert-butylacetylene bearing a bulky group gave a dimerization product. Mechanism of this reaction was also discussed.

  4. Interaction of ethylene with palladium clusters supported on oxidized tungsten foil

    Czech Academy of Sciences Publication Activity Database

    Jirka, Ivan; Plšek, Jan; Vondráček, Martin; Šutara, F.; Matolin, V.; Cháb, Vladimír; Prince, K. C.

    2007-01-01

    Roč. 601, č. 14 (2007), s. 3114-3124 ISSN 0039-6028 R&D Projects: GA ČR(CZ) GA202/05/0244 Institutional research plan: CEZ:AV0Z40400503; CEZ:AV0Z10100521 Keywords : synchrotron radiation photoelectron spectroscopy * thermal desorption spectroscopy * chemisorption * palladium Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 1.855, year: 2007

  5. Palladium-Catalyzed Carbenylative Cross-Coupling and Carbenylative Amination Utilizing Vinylcarbenes

    OpenAIRE

    Agee, Christopher

    2017-01-01

    This work focuses on the use of N-tosylhydrazones derived from α,β-unsaturated aldehydes – precursors to vinylcarbene ligands – in palladium-catalyzed carbenylative cross-coupling and carbenylative amination reactions. These carbenylative reactions were used to form η3-allylpalladium intermediates that generate stereogenic centers at the carbene center. An initial acyclic model system was used to intercept a well-known prochiral 1,3-diphenylallyl intermediate to probe the feasibility of enant...

  6. Palladium catalyzed selective distal C-H olefination of biaryl systems.

    Science.gov (United States)

    Maity, Soham; Hoque, Ehtasimul; Dhawa, Uttam; Maiti, Debabrata

    2016-11-29

    Palladium catalyzed selective distal C-H activation with nitrile based templates has been of significant research interest in recent times. In this report, we disclose the distal C-H olefination of biphenyl systems with high regio- and stereo-selectivity and useful synthetic yields. The utility of this method has been demonstrated through its wide olefin scope, its operation at the gram scale and the easy removal/recovery of the directing group.

  7. Site preference of rare earth doping in palladium-iron-arsenide superconductors

    Energy Technology Data Exchange (ETDEWEB)

    Stuerzer, Christine; Schulz, Anne; Johrendt, Dirk [Department Chemie, Ludwig-Maximilians-Universitaet Muenchen (Germany)

    2014-12-15

    The solid solutions (Ca{sub 1-y}RE{sub y}Fe{sub 1-x}Pd{sub x}As){sub 10}Pd{sub z}As{sub 8} with RE = La, Ce, and Pr were synthesized by solid state methods and characterized by X-ray powder diffraction with subsequent Rietveld refinements [(CaFeAs){sub 10}Pt{sub 3}As{sub 8}-type structure (''1038 type''), P anti 1, Z = 1]. Substitution levels (Ca/RE, Fe/Pd, and Pd/□) obtained from Rietveld refinements coincide well with the nominal values according to EDS and the linear courses of the lattice parameters as expected from the ionic radii. The RE atoms favor the one out of five calcium sites, which is eightfold coordinated by arsenic. This leads to significant stabilization of the structure, and especially prevents palladium over-doping in the iron-arsenide layers as observed in the pristine compound (CaFe{sub 1-x}Pd{sub x}As){sub 10}Pd{sub z}As{sub 8}. While the stabilization energy is estimated to about 40 kJ.mol{sup -1} by electronic structure calculations, the reason for the diminished Fe/Pd substitution through RE doping is still not yet understood. We suggest that the electrons transferred from RE{sup 3+} to the (Fe{sub 1-x}Pd{sub x})As layer makes higher palladium concentrations unfavorable. Anyway the reduced palladium doping enables superconductivity with critical temperatures up to 20 K (onset) in the RE doped Pd1038 samples, which could not be obtained earlier due to palladium over-doping in the active iron-arsenide layers. (Copyright copyright 2014 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  8. Electrochemical catalytic activities of nanoporous palladium rods for methanol electro-oxidation

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Xiaoguang; Wang, Weimin; Qi, Zhen; Zhao, Changchun; Ji, Hong; Zhang, Zhonghua [Key Laboratory for Liquid-Solid Structural Evolution and Processing of Materials (MOE), School of Materials Science and Engineering, Shandong University, Jingshi Road 73, Jinan 250061 (China)

    2010-10-01

    A novel electrocatalyst, nanoporous palladium (npPd) rods can be facilely fabricated by dealloying a binary Al{sub 80}Pd{sub 20} alloy in a 5 wt.% HCl aqueous solution under free corrosion conditions. The microstructure of these nanoporous palladium rods has been characterized using scanning electron microscopy and transmission electron microscopy. The results show that each Pd rod is several microns in length and several hundred nanometers in diameter. Moreover, all the rods exhibit a typical three-dimensional bicontinuous interpenetrating ligament-channel structure with length scale of 15-20 nm. The electrochemical experiments demonstrate that these peculiar nanoporous palladium rods (mixed with Vulcan XC-72 carbon powders to form a npPd/C catalyst) reveal a superior electrocatalytic performance toward methanol oxidation in the alkaline media. In addition, the electrocatalytic activity obviously depends on the metal loading on the electrode and will reach to the highest level (223.52 mA mg{sup -1}) when applying 0.4 mg cm{sup -2} metal loading on the electrode. Moreover, a competing adsorption mechanism should exist when performing methanol oxidation on the surface of npPd rods, and the electro-oxidation reaction is a diffusion-controlled electrochemical process. Due to the advantages of simplicity and high efficiency in the mass production, the npPd rods can act as a promising candidate for the anode catalyst for direct methanol fuel cells (DMFCs). (author)

  9. Practical, economical, and eco-friendly starch-supported palladium catalyst for Suzuki coupling reactions.

    Science.gov (United States)

    Baran, Talat

    2017-06-15

    In catalytic systems, the support materials need to be both eco friendly and low cost as well as having high thermal and chemical stability. In this paper, a novel starch supported palladium catalyst, which had these outstanding properties, was designed and its catalytic activity was evaluated in a Suzuki coupling reaction under microwave heating with solvent-free and mild reaction conditions. The starch supported catalyst gave remarkable reaction yields after only 5min as a result of the coupling reaction of the phenyl boronic acid with 23 different substrates, which are bearing aril bromide, iodide, and chloride. The longevity of the catalyst was also investigated, and the catalyst could be reused for 10 runs. The starch supported Pd(II) catalyst yielded remarkable TON (up to 25,000) and TOF (up to 312,500) values by using a simple, fast and eco-friendly method. In addition, the catalytic performance of the catalyst was tested against different commercial palladium catalysts, and the green starch supported catalyst had excellent selectivity. The catalytic tests showed that the novel starch based palladium catalyst proved to be an economical and practical catalyst for the synthesis of biaryl compounds. Copyright © 2017 Elsevier Inc. All rights reserved.

  10. Palladium extraction by a malonamide: behavior and particularities compared to rare earths

    International Nuclear Information System (INIS)

    Poirot, Remi

    2014-01-01

    Recycling of valuable metals appears as a solution of growing interest for a sustainable supply strategy nowadays. Palladium (Pd), along with other platinum group metals (PGM) and rare earth elements (REEs), represents one of the crucial issues in recovery processes. Malonamides are neutral amphiphilic molecules which have proved their potency for the extraction of lanthanides. These extractants in nitric media were thoroughly studied in frame of nuclear fuel treatment towards lanthanide-actinide separation. Within this framework, our purpose was to study liquid/liquid (L/L) extraction towards Pd recovery from nitric media by a malonamide: the DMDOHEMA. Various parameters such as as equilibration time, pH, extractant and nitrate concentrations were investigated in detail. In some experimental conditions, a Pd-rich solid third phase appears at the interface. These third phases were deeply analyzed with NMR, IR and XPS. Mechanistic studies involved complete analysis of the organic phases, including chemical speciation at the molecular level (coordination chemistry with NMR, IR, XRD), and supramolecular ordering characterization (with SAXS and NMR). Palladium complexes were identified and characterized. Similarities and differences between palladium and lanthanides behavior during extraction were evidenced and both can be efficiently co-extracted or separated according to different experimental conditions. (author) [fr

  11. Enantioconvergent synthesis by sequential asymmetric Horner-Wadsworth-Emmons and palladium-catalyzed allylic substitution reactions

    DEFF Research Database (Denmark)

    Pedersen, Torben Møller; Hansen, E. Louise; Kane, John

    2001-01-01

    A new method for enantioconvergent synthesis has been developed. The strategy relies on the combination of an asymmetric Horner-Wadsworth-Emmons (HWE) reaction and a palladium-catalyzed allylic substitution. Different $alpha@-oxygen-substituted, racemic aldehydes were initially transformed by asy...... the allylic stereocenter and the alkene geometry. Thus, a single $gamma@-substituted ester was obtained as the overall product, in high isomeric purity. The method was applied to a synthesis of a subunit of the iejimalides, a group of cytotoxic macrolides.......A new method for enantioconvergent synthesis has been developed. The strategy relies on the combination of an asymmetric Horner-Wadsworth-Emmons (HWE) reaction and a palladium-catalyzed allylic substitution. Different $alpha@-oxygen-substituted, racemic aldehydes were initially transformed...... by asymmetric HWE reactions into mixtures of two major $alpha@,$beta@-unsaturated esters, possessing opposite configurations at their allylic stereocenters as well as opposite alkene geometry. Subsequently, these isomeric mixtures of alkenes could be subjected to palladium-catalyzed allylic substitution...

  12. Spatial and temporal distribution of platinum, palladium and rhodium in Zagreb air.

    Science.gov (United States)

    Rinkovec, Jasmina; Pehnec, Gordana; Godec, Ranka; Davila, Silvije; Bešlić, Ivan

    2018-09-15

    Platinum (Pt), palladium (Pd) and rhodium (Rh) are most widely used in the production of automotive catalytic converters that serve to reduce toxic emissions from motor vehicles. The aim of this study was to quantitatively determine the levels of platinum, palladium and rhodium in the PM 10 and PM 2.5 fraction of airborne particle matter and find their spatial and temporal distribution at different polluted areas of the city of Zagreb, Croatia. The method used in this paper included weekly sampling of airborne particle matter on quartz filters, microwave digestion in acid under high pressure and temperature, and analysis by inductively coupled plasma mass spectrometry (ICP MS). The results have shown that the highest mean values at all three sampling stations (North, Center, South) were obtained for palladium (3.856 pg m -3 , 5.396 pg m -3 , 5.600 pg m -3 ) and the lowest for rhodium (0.444 pg m -3 , 0.643 pg m -3 , 0.750 pg m -3 ). The average mass concentrations of platinum group elements (PGE) in PM 10 increased for all three elements in the direction North Zagreb are the first results of their kind for this area and will provide insights into the contribution of catalytic converters to the presence of these elements in the environment. Copyright © 2018 Elsevier B.V. All rights reserved.

  13. Nonenzymatic glucose sensing based on deposited palladium nanoparticles on epoxy-silver electrodes

    International Nuclear Information System (INIS)

    Gutes, Albert; Carraro, Carlo; Maboudian, Roya

    2011-01-01

    Highlights: → New nonenzymatic glucose sensor material. → Modified epoxy-silver electrodes with palladium nanoparticles. → Simple electroless surface modification. → Wide linear response range. → Easy implementation. - Abstract: A new approach for nonenzymatic glucose sensing, based on a simple modification of epoxy-silver surfaces deposited on the tip of commercial copper electric wires, is presented. Palladium was galvanically displaced on the surface of the epoxy-silver surface in order to obtain metal nanoparticles that act as catalyst for the direct oxidation of glucose. Scanning electron microscopy revealed the formation of the metal nanoparticles. X-ray photoelectron spectroscopy confirmed the metallic nature of the formed nanostructures on the surface. Electrochemical characterization and calibration of the palladium-modified epoxy-silver electrode is reported, obtaining a linear range of 1-20 mM for the detection of glucose with low interference of ascorbic acid and uric acid. A simple 3-step coulometry was used as the detection technique. The developed sensing material is believed to be a great candidate for integration in small devices for clinical essays, due to the simplicity and cost effectiveness of the presented approach, compared to the state-of-the-art devices reported recently in the literature. Simplicity in the coulometry determinations makes these Pd-modified epoxy-silver sensors a good candidate for easy glucose determinations.

  14. Palladium-based on-wafer electroluminescence studies of GaN-based LED structures

    Energy Technology Data Exchange (ETDEWEB)

    Salcianu, C.O.; Thrush, E.J.; Humphreys, C.J. [Department of Materials Science and Metallurgy, University of Cambridge, Pembroke Street, Cambridge CB2 3QZ (United Kingdom); Plumb, R.G. [Centre for Photonic Systems, Department of Engineering, University of Cambridge, Cambridge CB3 0FD (United Kingdom); Boyd, A.R.; Rockenfeller, O.; Schmitz, D.; Heuken, M. [AIXTRON AG, Kackertstr. 15-17, 52072 Aachen (Germany)

    2008-07-01

    Electroluminescence (EL) testing of Light Emitting Diode (LED) structures is usually done at the chip level. Assessing the optical and electrical properties of LED structures at the wafer scale prior to their processing would improve the cost effectiveness of producing LED-lamps. A non-destructive method for studying the luminescence properties of the structure at the wafer-scale is photoluminescence (PL). However, the relationship between the on-wafer PL data and the final device EL can be less than straightforward (Y. H Aliyu et al., Meas. Sci. Technol. 8, 437 (1997)) as the two techniques employ different carrier injection mechanisms. This paper provides an overview of some different techniques in which palladium is used as a contact in order to obtain on-wafer electroluminescence information which could be used to screen wafers prior to processing into final devices. Quick mapping of the electrical and optical characteristics was performed using either palladium needle electrodes directly, or using the latter in conjunction with evaporated palladium contacts to inject both electrons and holes into the active region via the p-type capping layer of the structure. For comparison, indium was also used to make contact to the n-layer so that electrons could be directly injected into that layer. (copyright 2008 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  15. Effect of pH on the spontaneous synthesis of palladium nanoparticles on reduced graphene oxide

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Xiaorui [Faculty of Pure and Applied Sciences, University of Tsukuba, 1-1-1 Tennodai, Tsukuba, Ibaraki 305-8573 (Japan); Ooki, Wataru; Kosaka, Yoshinori R.; Okonogi, Akinori [Graduate School of Pure and Applied Sciences, University of Tsukuba, 1-1-1 Tennodai, Tsukuba, Ibaraki 305-8573 (Japan); Marzun, Galina; Wagener, Philipp; Barcikowski, Stephan [Technical Chemistry I and Center for Nanointegration Duisburg-Essen (CENIDE), University of Duisburg-Essen, Universitaetsstrasse 7, D-45141 Essen (Germany); NanoEnergieTechnikZentrum (NETZ), University of Duisburg-Essen, Carl-Benz-Strasse 199, D-47057 Duisburg (Germany); Kondo, Takahiro [Faculty of Pure and Applied Sciences, University of Tsukuba, 1-1-1 Tennodai, Tsukuba, Ibaraki 305-8573 (Japan); Tsukuba Research Center for Interdisciplinary Materials Science (TIMS) & Center for Integrated Research in Fundamental Science and Engineering (CiRfSE), University of Tsukuba, 1-1-1 Tennodai, 305-8573 (Japan); Nakamura, Junji, E-mail: nakamura@ims.tsukuba.ac.jp [Faculty of Pure and Applied Sciences, University of Tsukuba, 1-1-1 Tennodai, Tsukuba, Ibaraki 305-8573 (Japan); Tsukuba Research Center for Interdisciplinary Materials Science (TIMS) & Center for Integrated Research in Fundamental Science and Engineering (CiRfSE), University of Tsukuba, 1-1-1 Tennodai, 305-8573 (Japan)

    2016-12-15

    Highlights: • Palladium metal nanoparticles were spontaneously formed on reduced graphene oxide (rGO) via a redox reaction in H{sub 2}O. • The amount of Pd deposited on rGO was affected by pH. • The amount of oxygen-containing functional groups in rGO was increased with the deposition of palladium. • The importance of redox potential in spontaneous deposition was demonstrated by an experiment with Zn, Ni, Pt, Pd, etc.. • The spontaneous redox deposition method is facile, environmentally friendly, and needs no external reducing agents. - Abstract: Palladium (Pd) nanoparticles were spontaneously deposited on reduced graphene oxide (rGO) without any external reducing agents. The prepared Pd/rGO composites were then characterized by X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS). Spontaneous deposition occurred because of a redox reaction between the Pd precursor and rGO, which involved reduction of bivalent Pd to metallic Pd{sup 0} and oxidation of the sp{sup 2} carbon of rGO to oxygen-containing functional groups. The amount of Pd deposited on rGO varied with pH, and this was attributed to electrostatic interactions between the Pd precursor and rGO based on the results of zeta potential measurements. The importance of the redox reaction in the spontaneous deposition was demonstrated in the experiment with Zn, Ni, Cu, Ag, Pt, Pd, and Au.

  16. Palladium nanoparticles anchored on graphene nanosheets: Methanol, ethanol oxidation reactions and their kinetic studies

    International Nuclear Information System (INIS)

    Nagaraju, D.H.; Devaraj, S.; Balaya, P.

    2014-01-01

    Highlights: • Palladium nanoparticles decorated graphene is synthesized in a single step. • Electro-catalytic activity of Gra/Pd toward alcohol oxidation is evaluated. • 1:1 Gra/Pd exhibits good electro-catalytic activity and efficient electron transfer. - Abstract: Palladium nanoparticles decorated graphene (Gra/Pd nanocomposite) was synthesized by simultaneous chemical reduction of graphene oxide and palladium salt in a single step. The negatively charged graphene oxide (GO) facilitates uniform distribution of Pd 2+ ions onto its surface. The subsequent reduction by hydrazine hydrate provides well dispersed Pd nanoparticles decorated graphene. Different amount of Pd nanoparticles on graphene was synthesized by changing the volume to weight ratio of GO to PdCl 2 . X-ray diffraction studies showed FCC lattice of Pd with predominant (1 1 1) plane. SEM and TEM studies revealed that thin graphene nanosheets are decorated by Pd nanoparticles. Raman spectroscopic studies revealed the presence of graphene nanosheets. The electro-catalytic activity of Gra/Pd nanocomposites toward methanol and ethanol oxidation in alkaline medium was evaluated by cyclic voltammetric studies. 1:1 Gra/Pd nanocomposite exhibited good electro-catalytic activity and efficient electron transfer. The kinetics of electron transfer was studied using chronoamperometry. Improved electro-catalytic activity of 1:1 Gra/Pd nanocomposite toward alcohol oxidation makes it as a potential anode for the alcohol fuel cells

  17. High stability of palladium/kieselguhr composites during absorption/desorption cycling for hydrogen isotope separation

    Energy Technology Data Exchange (ETDEWEB)

    Lei, Yang, E-mail: lei.y@outlook.com; Liu, Xiaopeng; Li, Shuo; Jiang, Lijun; Zhang, Chao; Li, Shuai; He, Di; Wang, Shumao

    2016-12-15

    Highlights: • Pd/K composites with as high as 57 wt.% of Pd have been successfully prepared. • Palladium particles can be effectively packed into the pores of kieselguhr substrates. • Variation of heat-treatment temperatures hardly affect hydrogen absorption capacity and hydrogen saturation time of the Pd/K. • Anti-pulverization property of Pd/K can be improved by packing palladium into the kieselguhr internal pores and heating at 1300 °C. - Abstract: Palladium/kieselguhr (Pd/K) composites with 57 wt.% of Pd were prepared by an improved dipping and thermal decomposition method and heated at elevated temperature to reduce breakdown during hydrogenation-dehydrogenation cycles. The hydrogen absorption kinetic properties of the samples heated at different temperatures were tested under the condition of 20 °C with 100 kPa hydrogen pressure. The 1300 °C heated Pd/K composites were repeated up to 4010 absorption and desorption cycles at temperature ranges between −40 °C and 200 °C. The results show that the phase structure, hydrogen absorption capacity and hydrogen saturation time of the Pd/K were not affected by the change of heat-treated temperatures. And after heat treatment at 1300 °C, the Pd/K particles were strengthened and fraction of larger than 80 mesh were as high as 93.4%.

  18. Palladium nanoparticles anchored on graphene nanosheets: Methanol, ethanol oxidation reactions and their kinetic studies

    Energy Technology Data Exchange (ETDEWEB)

    Nagaraju, D.H., E-mail: dhnagu@gmail.com [Department of Mechanical Engineering, 117 576 (Singapore); Materials Science and Engineering, King Abdullah University of Science and Technology (KAUST), Thuwal, 23955-6900 (Saudi Arabia); Devaraj, S. [Department of Mechanical Engineering, 117 576 (Singapore); School of Chemical and Biotechnology, SASTRA University, Thanjavur, 613 401 (India); Balaya, P., E-mail: mpepb@nus.edu.sg [Department of Mechanical Engineering, 117 576 (Singapore); Engineering Science Program, National University of Singapore, 117 576 (Singapore)

    2014-12-15

    Highlights: • Palladium nanoparticles decorated graphene is synthesized in a single step. • Electro-catalytic activity of Gra/Pd toward alcohol oxidation is evaluated. • 1:1 Gra/Pd exhibits good electro-catalytic activity and efficient electron transfer. - Abstract: Palladium nanoparticles decorated graphene (Gra/Pd nanocomposite) was synthesized by simultaneous chemical reduction of graphene oxide and palladium salt in a single step. The negatively charged graphene oxide (GO) facilitates uniform distribution of Pd{sup 2+} ions onto its surface. The subsequent reduction by hydrazine hydrate provides well dispersed Pd nanoparticles decorated graphene. Different amount of Pd nanoparticles on graphene was synthesized by changing the volume to weight ratio of GO to PdCl{sub 2}. X-ray diffraction studies showed FCC lattice of Pd with predominant (1 1 1) plane. SEM and TEM studies revealed that thin graphene nanosheets are decorated by Pd nanoparticles. Raman spectroscopic studies revealed the presence of graphene nanosheets. The electro-catalytic activity of Gra/Pd nanocomposites toward methanol and ethanol oxidation in alkaline medium was evaluated by cyclic voltammetric studies. 1:1 Gra/Pd nanocomposite exhibited good electro-catalytic activity and efficient electron transfer. The kinetics of electron transfer was studied using chronoamperometry. Improved electro-catalytic activity of 1:1 Gra/Pd nanocomposite toward alcohol oxidation makes it as a potential anode for the alcohol fuel cells.

  19. Adhesion enhancement between electroless nickel and polyester fabric by a palladium-free process

    Energy Technology Data Exchange (ETDEWEB)

    Lu Yinxiang, E-mail: yxlu@fudan.edu.cn [Department of Materials Science, Fudan University, 220 Handan Road, Shanghai 200433 (China); Xue Longlong; Li Feng [Department of Materials Science, Fudan University, 220 Handan Road, Shanghai 200433 (China)

    2011-01-15

    A new, efficient, palladium- and etchant-free process for the electroless nickel plating of poly(ethylene terephthalate) (PET) fabric has been developed. PET electroless plating can be prepared in three steps, namely: (i) the grafting of thiol group onto PET, (ii) the silver Ag{sup 0} seeding of the PET surface, and (iii) the nickel metallization using electroless plating bath. Scanning electron microscopy (SEM), energy dispersive X-ray (EDX) analysis, X-ray photoelectron spectroscopy (XPS), Raman spectrometer, X-ray diffraction (XRD), and thermogravimetric analysis (TG) were used to characterize the samples in the process, and the nickel loading was quantified by weighing. This process successfully compares with the traditional one based on KMnO{sub 4}/H{sub 2}SO{sub 4} etching and palladium-based seed layer. The nickel coating obtained in this palladium-free process can pass through ultrasonic washing challenge, and shows excellent adhesion with the PET substrate. However, the sample with Pd catalyst via traditional process was damaged during the testing experiment.

  20. Electrooxidation of aliphatic alcohols on palladium oxide catalyst prepared by pulsed electrodeposition technique

    International Nuclear Information System (INIS)

    Casella, Innocenzo G.

    2009-01-01

    Palladium film can be deposited on gold polycrystalline electrodes, from a deoxygenated alkaline solution containing 50 mM NaOH plus 0.5 mM K 2 Pd(CN) 4 . A multipulse sequence of potentials of equal amplitude and duration was used for the palladium deposition process. In particular, an optimized waveform of potentials of E 1 = 1.0 V vs. SCE and E 2 = -1.0 V vs. SCE for the relevant pulse duration of t 1 = 0.05 s and t 2 = 0.05 s, for 30 s, was used. Cyclic voltammetry and scanning electron microscopy (SEM) were employed to characterize the gold-palladium modified electrode (Au-Pd) towards the electrooxidation of aliphatic alcohols in alkaline solutions. The voltammetric study suggests that the kinetics involved in the alcohol electrooxidation at the Pd-Au electrode are sensibly higher than those observed on the bare Pd and Au electrodes. In addition, the most interesting aspect of the electrooxidation of aliphatic alcohols at the Au-Pd electrode was that as the number of methylene groups on the homologous series of aliphatic alcohols increased, the molar response also increased. Under pulsed chronoamerometric conditions (PCC), using an optimized triple pulse waveform of potentials the modified electrode exhibits interesting catalytic currents without any apparent poisoning effects during the oxidation of aliphatic alcohols.

  1. Effect of pH on the spontaneous synthesis of palladium nanoparticles on reduced graphene oxide

    International Nuclear Information System (INIS)

    Zhang, Xiaorui; Ooki, Wataru; Kosaka, Yoshinori R.; Okonogi, Akinori; Marzun, Galina; Wagener, Philipp; Barcikowski, Stephan; Kondo, Takahiro; Nakamura, Junji

    2016-01-01

    Highlights: • Palladium metal nanoparticles were spontaneously formed on reduced graphene oxide (rGO) via a redox reaction in H_2O. • The amount of Pd deposited on rGO was affected by pH. • The amount of oxygen-containing functional groups in rGO was increased with the deposition of palladium. • The importance of redox potential in spontaneous deposition was demonstrated by an experiment with Zn, Ni, Pt, Pd, etc.. • The spontaneous redox deposition method is facile, environmentally friendly, and needs no external reducing agents. - Abstract: Palladium (Pd) nanoparticles were spontaneously deposited on reduced graphene oxide (rGO) without any external reducing agents. The prepared Pd/rGO composites were then characterized by X-ray diffraction (XRD) and X-ray photoelectron spectroscopy (XPS). Spontaneous deposition occurred because of a redox reaction between the Pd precursor and rGO, which involved reduction of bivalent Pd to metallic Pd"0 and oxidation of the sp"2 carbon of rGO to oxygen-containing functional groups. The amount of Pd deposited on rGO varied with pH, and this was attributed to electrostatic interactions between the Pd precursor and rGO based on the results of zeta potential measurements. The importance of the redox reaction in the spontaneous deposition was demonstrated in the experiment with Zn, Ni, Cu, Ag, Pt, Pd, and Au.

  2. Oxygen kinetics and mechanism at electrocatalysts on the base of palladium-iron system

    International Nuclear Information System (INIS)

    Tarasevich, M.R.; Zhutaeva, G.V.; Bogdanovskaya, V.A.; Radina, M.V.; Ehrenburg, M.R.; Chalykh, A.E.

    2007-01-01

    Binary nanodispersed carbon XC72 supported PdFe catalysts with different atomic palladium-to-iron ratios are synthesized and studied in oxygen reduction reaction in acid solution at 60 o C. The Pd:Fe ratio was well controlled by the initial concentrations of Pd and Fe in the precursor solutions. The nanoparticles were characterized by transmission electron microscopy, X-ray diffractometry and X-ray photoelectron spectroscopy. The optimum Pd:Fe ratio for this reaction was determined to be 3:1. The comparison of activities of the catalysts with component ratios equaled 3:1 and 10:1 is shown that the activities are differed from each other by 10-15 times in advantage of catalyst with lesser content of palladium. This phenomenon can be related to the different particle size of both catalysts and different distribution of particles by size discovered by TEM method. The achievement of maximum activity near the ratio of Pd:Fe = 3:1 is due to as effect of alloy-forming and the influence of binary system component ratio and synthesis conditions on dispersity degree of metallic phase nanoparticles. Under optimal conditions of precursor mixture high-temperature pyrolysis, iron produces the stabilizing effect palladium. It gives rise to obtaining the uniform and finely divided (7-8 nm) metallic particles

  3. Dechlorination of Environmental Contaminants Using a Hybrid Nanocatalyst: Palladium Nanoparticles Supported on Hierarchical Carbon Nanostructures

    Directory of Open Access Journals (Sweden)

    Hema Vijwani

    2012-01-01

    Full Text Available This paper demonstrates the effectiveness of a new type of hybrid nanocatalyst material that combines the high surface area of nanoparticles and nanotubes with the structural robustness and ease of handling larger supports. The hybrid material is made by fabricating palladium nanoparticles on two types of carbon supports: as-received microcellular foam (Foam and foam with carbon nanotubes anchored on the pore walls (CNT/Foam. Catalytic reductive dechlorination of carbon tetrachloride with these materials has been investigated using gas chromatography. It is seen that while both palladium-functionalized carbon supports are highly effective in the degradation of carbon tetrachloride, the rate of degradation is significantly increased with palladium on CNT/Foam. However, there is scope to increase this rate further if the wettability of these structures can be enhanced in the future. Microstructural and spectroscopic analyses of the fresh and used catalysts have been compared which indicates that there is no change in density or surface chemical states of the catalyst after prolonged use in dechlorination test. This implies that these materials can be used repeatedly and hence provide a simple, powerful, and cost-effective approach for dechlorination of water.

  4. Comportamiento parabólico del crecimiento de capas boradas en los aceros Y8A y X12M // Parabolic behavior of boriding layers growth in Y8A and X12M steels

    Directory of Open Access Journals (Sweden)

    C. Figueroa Hernández

    1999-01-01

    Full Text Available Se determina la influencia que tienen los principales parámetros tecnológicos del borado en el crecimiento de las capas y secorrobora el cumplimiento de la ley parabólica para predecir este comportamiento en los aceros Y8A y X12M.El proceso de borado se aplica en una mezcla de carburo de silicio y bórax (70 y 30 % a la temperatura de 850, 900 y 950 oCdurante un tiempo de 2, 4 y 6 horas. Como variable dependiente se seleccionó la profundidad del recubrimiento, a partir de lacual se obtuvieron los coeficientes del crecimiento parabólico y la energía de activación en función de la temperatura, el tiempodel proceso y el tipo de acero.La caracterización metalográfica reveló la presencia de la fase Fe2BPalabras claves: Borado, recubrimiento superf icial , t ecnología de recubrimiento.__________________________________________________________________________AbstractIt was determined the influence of the main technological parameters of the boriding process, and a mathematical model thatallows to predict this conduct on the steels Y8A and X12M steels was obtained.The boriding process is applied in a mixture of silicon carbide and borax (70 and 30% at 850, 900 and 950 oC temperatureduring a period of time 2, 4 and 6 hours. As an independent variable the depth of the coat was selected.It was obtained the parabolic growth coefficients, and the activation energy according to temperature, time and the chemicalcomposition of steel.Metallografic analysis reveals the presence of Fe2B phase.Key words: Boriding process, superf icial coat , coat technology.

  5. Synthesis and characterization of new metal-rich borides with boron fragments; Synthese und Charakterisierung von neuartigen metallreichen Boriden mit Borfragmenten

    Energy Technology Data Exchange (ETDEWEB)

    Mbarki, Mohammed

    2016-03-30

    The present dissertation deals with the synthesis and characterization of new metal-rich borides of the Ce{sub 7}Ni{sub 5±x}Ge{sub 3±x}In{sub 6{sup -}}, Nb{sub 2}OsB{sub 2{sup -}} and NbRuB-type.The samples are synthesized by a solid state reaction route from elements using an electric arc furnace. The structural characterization of the compounds was carried out by using X-ray diffraction methods on powder samples and single crystals. The chemical composition of single-crystals was verified by EDX analyses. Moreover, the magnetic properties of suitable samples were investigated by SQUID magnetometry.The crystal structure of compounds with the nominal composition NbFe{sub 1-x}Ir{sub 6+x}B{sub 8} is successfully solved from single crystal X-ray data. The most prominent feature in this structure are one-dimensional chains along the c-axis formed by the magnetically active element iron on a site of mixed occupation with Iridium (Fe: Ir = 0.77 (2) 0.23 (2)). Thermomagnetic investigations reveal, that ferromagnetic ordering is observed below the Curie temperature (TC) of 350 K. Theoretical investigations suggest that the iron-chains are mainly responsible for the ferromagnetic ordering. In addition, the magnetocaloric effect (MCE) is calculated using isothermal magnetization measurements at several temperatures. The maximal magnetic entropy change ΔS = 0.032 J kg{sup -1} K{sup -1} is observed in the vicinity of T{sub C}. For the phases Nb{sub 6}Mn{sub 0,75(2)}Ir{sub 6,25(2)}B{sub 8} and Nb{sub 6}Co{sub 1,09(2)}Ir{sub 5,91(2)}B{sub 8} a relationship between the measured ferrimagnetic ordering and the crystal structure is found. Tiny superstructure reflections measured by Selected Area Electron Diffraction (SEAD) indicate a different crystal system for those compounds, which allows a ferrimagnetic spin arrangement within this crystal structure.In the second part of the thesis new results about the Nb{sub 2}OsB{sub 2-} and NbRuB-type borides are presented, which both

  6. Synthesis, characterization and thermoelectric properties of metal borides, boron carbides and carbaborides; Synthese, Charakterisierung und thermoelektrische Eigenschaften ausgewaehlter Metallboride, Borcarbide und Carbaboride

    Energy Technology Data Exchange (ETDEWEB)

    Guersoy, Murat

    2015-07-06

    This work reports on the solid state synthesis and structural and thermoelectrical characterization of hexaborides (CaB{sub 6}, SrB{sub 6}, BaB{sub 6}, EuB{sub 6}), diboride dicarbides (CeB{sub 2}C{sub 2}, LaB{sub 2}C{sub 2}), a carbaboride (NaB{sub 5}C) and composites of boron carbide. The characterization was performed by X-ray diffraction methods and Rietveld refinements based on structure models from literature. Most of the compounds were densified by spark plasma sintering at 100 MPa. As high-temperature thermoelectric properties the Seebeck coefficients, electrical conductivities, thermal diffusivities and heat capacities were measured between room temperature and 1073 K. ZT values as high as 0.5 at 1273 K were obtained for n-type conducting EuB{sub 6}. High-temperature X-ray diffraction also confirmed its thermal stability. The solid solutions Ca{sub x}Sr{sub 1-x}B{sub 6}, Ca{sub x}Ba{sub 1-x}B{sub 6} and Sr{sub x}Ba{sub 1-x}B{sub 6} (x = 0, 0.25, 0.5, 0.75, 1) are also n-type but did not show better ZT values for the ternary compounds compared to the binaries, but for CaB{sub 6} the values of the figure of merit (ca. 0.3 at 1073 K) were significantly increased (ca. 50 %) compared to earlier investigations which is attributed to the densification process. Sodium carbaboride, NaB{sub 5}C, was found to be the first p-type thermoelectric material that crystallizes with the hexaboride-structure type. Seebeck coefficients of ca. 80 μV . K{sup -1} were obtained. Cerium diboride dicarbide, CeB{sub 2}C{sub 2}, and lanthanum diboride dicarbide, LaB{sub 2}C{sub 2}, are metallic. Both compounds were used as model compounds to develop compacting strategies for such layered borides. Densities obtained at 50 MPa were determined to be higher than 90 %. A new synthesis route using single source precursors that contain boron and carbon was developed to open the access to new metal-doped boron carbides. It was possible to obtain boron carbide, but metal-doping could not be

  7. Mechanical, electrical, and thermal expansion properties of carbon nanotube-based silver and silver-palladium alloy composites

    Science.gov (United States)

    Pal, Hemant; Sharma, Vimal

    2014-11-01

    The mechanical, electrical, and thermal expansion properties of carbon nanotube (CNT)-based silver and silver-palladium (10:1, w/w) alloy nanocomposites are reported. To tailor the properties of silver, CNTs were incorporated into a silver matrix by a modified molecular level-mixing process. CNTs interact weakly with silver because of their non-reactive nature and lack of mutual solubility. Therefore, palladium was utilized as an alloying element to improve interfacial adhesion. Comparative microstructural characterizations and property evaluations of the nanocomposites were performed. The structural characterizations revealed that decorated type-CNTs were dispersed, embedded, and anchored into the silver matrix. The experimental results indicated that the modification of the silver and silver-palladium nanocomposite with CNT resulted in increases in the hardness and Young's modulus along with concomitant decreases in the electrical conductivity and the coefficient of thermal expansion (CTE). The hardness and Young's modulus of the nanocomposites were increased by 30%-40% whereas the CTE was decreased to 50%-60% of the CTE of silver. The significantly improved CTE and the mechanical properties of the CNT-reinforced silver and silver-palladium nanocomposites are correlated with the intriguing properties of CNTs and with good interfacial adhesion between the CNTs and silver as a result of the fabrication process and the contact action of palladium as an alloying element.

  8. Recovery of palladium, cesium, and selenium from heavy metal alkali borosilicate glass by combination of heat treatment and leaching processes

    Energy Technology Data Exchange (ETDEWEB)

    Xu, Zhanglian; Okada, Takashi, E-mail: t-okada@u-fukui.ac.jp; Nishimura, Fumihiro; Yonezawa, Susumu

    2017-06-05

    Highlights: • A separation technique of both noble and less noble metal from glass is studied. • Via reductive heat treatment, 80% of palladium is extracted in liquid bismuth. • Sodium–potassium-rich materials with cesium and selenium are phase separated. • From the materials, over 80% of cesium and selenium are extracted in water. - Abstract: Reductive heat-treatment and leaching process were applied to a simulated lead or bismuth soda-potash-borosilicate glass with palladium, cesium, and selenium to separate these elements. In the reductive heat treatment, palladium is extracted in liquid heavy metal phase generated by the reduction of the heavy metal oxides, whereas cesium and selenium are concentrated in phase separated Na–K-rich materials on the glass surface. From the materials, cesium and selenium can be extracted in water, and the selenium extraction was higher in the treatment of the bismuth containing glass. The chemical forms of palladium in the glass affected the extraction efficiencies of cesium and selenium. Among the examined conditions, in the bismuth glass treatment, the cesium and selenium extraction efficiencies in water were over 80%, and that of palladium in liquid bismuth was over 80%.

  9. Flexible palladium-based H2 sensor with fast response and low leakage detection by nanoimprint lithography.

    Science.gov (United States)

    Lim, Su Hui; Radha, Boya; Chan, Jie Yong; Saifullah, Mohammad S M; Kulkarni, Giridhar U; Ho, Ghim Wei

    2013-08-14

    Flexible palladium-based H2 sensors have a great potential in advanced sensing applications, as they offer advantages such as light weight, space conservation, and mechanical durability. Despite these advantages, the paucity of such sensors is due to the fact that they are difficult to fabricate while maintaining excellent sensing performance. Here, we demonstrate, using direct nanoimprint lithography of palladium, the fabrication of a flexible, durable, and fast responsive H2 sensor that is capable of detecting H2 gas concentration as low as 50 ppm. High resolution and high throughput patterning of palladium gratings over a 2 cm × 1 cm area on a rigid substrate was achieved by heat-treating nanoimprinted palladium benzyl mercaptide at 250 °C for 1 h. The flexible and robust H2 sensing device was fabricated by subsequent transfer nanoimprinting of these gratings into a polycarbonate film at its glass transition temperature. This technique produces flexible H2 sensors with improved durability, sensitivity, and response time in comparison to palladium thin films. At ambient pressure and temperature, the device showed a fast response time of 18 s at a H2 concentration of 3500 ppm. At 50 ppm concentration, the response time was found to be 57 s. The flexibility of the sensor does not appear to compromise its performance.

  10. New ternary tantalum borides containing boron dumbbells: Experimental and theoretical studies of Ta2OsB2 and TaRuB

    Science.gov (United States)

    Mbarki, Mohammed; Touzani, Rachid St.; Rehorn, Christian W. G.; Gladisch, Fabian C.; Fokwa, Boniface P. T.

    2016-10-01

    The new ternary transition metal-rich borides Ta2OsB2 and TaRuB have been successfully synthesized by arc-melting the elements in a water-cooled crucible under an argon atmosphere. The crystal structures of both compounds were solved by single-crystal X-ray diffraction and their metal compositions were confirmed by EDX analysis. It was found that Ta2OsB2 and TaRuB crystallize in the tetragonal Nb2OsB2 (space group P4/mnc, no. 128) and the orthorhombic NbRuB (space group Pmma, no. 51) structure types with lattice parameters a=5.878(2) Å, c=6.857(2) Å and a=10.806(2) Å, b=3.196(1) Å, c=6.312(2) Å, respectively. Furthermore, crystallographic, electronic and bonding characteristics have been studied by density functional theory (DFT). Electronic structure relaxation has confirmed the crystallographic parameters while COHP bonding analysis indicates that B2-dummbells are the strongest bonds in both compounds. Moreover, the formation of osmium dumbbells in Ta2OsB2 through a Peierls distortion along the c-axis, is found to be the origin of superstructure formation. Magnetic susceptibility measurements reveal that the two phases are Pauli paramagnets, thus confirming the theoretical DOS prediction of metallic character. Also hints of superconductivity are found in the two phases, however lack of single phase samples has prevented confirmation. Furthermore, the thermodynamic stability of the two modifications of AMB (A=Nb, Ta; M =Ru, Os) are studied using DFT, as new possible phases containing either B4- or B2-units are predicted, the former being the most thermodynamically stable modification.

  11. Tetradentate N2O2 Chelated Palladium(II Complexes: Synthesis, Characterization, and Catalytic Activity towards Mizoroki-Heck Reaction of Aryl Bromides

    Directory of Open Access Journals (Sweden)

    Siti Kamilah Che Soh

    2013-01-01

    Full Text Available Four air and moisture-stable palladium(II-Schiff base complexes, N,N′-bis(α-methylsalicylidenepropane-1,3-diamine palladium(II (2a, N,N′-bis(4-methyl-α-methylsalicylidenepropane-1,3-diamine palladium(II (2b, N,N′-bis(3,5-di-tert-butylsalicylidenepropane-1,3-diamine palladium(II (2c, and N,N′-bis(4-methoxy-salicylidenepropane-1,3-diamine palladium(II (2d, have been successfully synthesised and characterised by CHN elemental analyses and conventional spectroscopic methods. These complexes were investigated as catalysts in the phosphine-free Mizoroki-Heck cross-coupling reactions of aryl bromides with methyl acrylate.

  12. Activation and deactivation of neutral palladium(II) phosphinesulfonato polymerization catalysts

    KAUST Repository

    Rünzi, Thomas

    2012-12-10

    13C-Labeled ethylene polymerization (pre)catalysts [κ2-(anisyl)2P,O]Pd(13CH3)(L) (1-13CH3-L) (L = pyridine, dmso) based on di(2-anisyl)phosphine benzenesulfonate were used to assess the degree of incorporation of 13CH3 groups into the formed polyethylenes. Polymerizations of variable reaction time reveal that ca. 60-85% of the 13C-label is found in the polymer after already 1 min polymerization time, which provides evidence that the pre-equilibration between the catalyst precursor 1-13CH3-L and the active species 1-13CH3-(ethylene) is fast with respect to chain growth. The fraction of 1-13CH3-L that initiates chain growth is likely higher than the 60-85% determined from the 13C-labeled polymer chain ends since (a) chain walking results in in-chain incorporation of the 13C-label, (b) irreversible catalyst deactivation by formation of saturated (and partially volatile) alkanes diminishes the amount of 13CH3 groups incorporated into the polymer, and (c) palladium-bound 13CH3 groups, and more general palladium-bound alkyl(polymeryl) chains, partially transfer to phosphorus by reductive elimination. NMR and ESI-MS analyses of thermolysis reactions of 1-13CH3-L provide evidence that a mixture of phosphonium salts (13CH3)xP+(aryl)4-x (2-7) is formed in the absence of ethylene. In addition, isolation and characterization of the mixed bis(chelate) palladium complex [κ2-(anisyl)2P,O]Pd[κ2-(anisyl) (13CH3)P,O] (11) by NMR and X-ray diffraction analyses from these mixtures indicate that oxidative addition of phosphonium salts to palladium(0) species is also operative. The scrambling of palladium-bound carbyls and phosphorus-bound aryls is also relevant under NMR, as well as preparative reactor polymerization conditions exemplified by the X-ray diffraction analysis of [κ2-(anisyl)2P,O] Pd[κ2-(anisyl)(CH2CH3)P,O] (12) and [κ2-(anisyl)2P,O]Pd[κ2-(anisyl) ((CH2)3CH3)P,O] (13) isolated from pressure reactor polymerization experiments. In addition, ESI-MS analyses of reactor

  13. A new metal electrocatalysts supported matrix: Palladium nanoparticles supported silicon carbide nanoparticles and its application for alcohol electrooxidation

    International Nuclear Information System (INIS)

    Dai Hong; Chen Yanling; Lin Yanyu; Xu Guifang; Yang Caiping; Tong Yuejin; Guo Longhua; Chen Guonan

    2012-01-01

    In this paper, we propose a facile approach for palladium nanoparticles load using silicon carbide nanoparticles as the new supported matrix and a familiar NaBH 4 as reducer. Detailed X-ray photoelectron spectrum (XPS) and transmission electron microscopy (TEM) analysis of the resultant products indicated that palladium nanoparticles are successfully immobilized onto the surface of the silicon carbide nanoparticles with uniform size distribution between 5 and 7 nm. The relative electrochemical characterization clearly demonstrated excellent electrocatalytic activity of this material toward alcohol in alkaline electrolytes. Investigation on the characteristics of the electrocatalytic activity of this material further indicated that the palladium nanoparticles supporting on SiC are very promising for direct alcohol fuel cells (DMFCs), biosensor and electronic devices. Moreover, it was proved that silicon carbide nanoparticles with outstanding properties as support for catalysis are of strong practical interest. And the silicon carbide could perform attractive role in adsorbents, electrodes, biomedical applications, etc.

  14. QuadraPure-Supported Palladium Nanocatalysts for Microwave-Promoted Suzuki Cross-Coupling Reaction under Aerobic Condition

    Directory of Open Access Journals (Sweden)

    Kin Hong Liew

    2014-01-01

    Full Text Available Cross-linked resin-captured palladium (XL-QPPd was readily prepared by simple physical adsorption onto the high loading QuadraPure macroporous resin and a subsequent reduction process. To enhance the mechanical stability, entrapped palladium nanocatalysts were cross-linked with succinyl chloride. Both transmission electron microscopy images and X-ray diffraction analysis revealed that the palladium nanoparticles were well dispersed with diameters ranging in 4–10 nm. The catalyst performed good catalytic activity in microwave-promoted Suzuki cross-coupling reactions in water under aerobic condition with mild condition by using various aryl halides and phenylboronic acid. In addition, the catalyst showed an excellent recyclability without significant loss of catalytic activity.

  15. Palladium(II)-catalyzed desulfitative synthesis of aryl ketones from sodium arylsulfinates and nitriles: scope, limitations, and mechanistic studies.

    Science.gov (United States)

    Skillinghaug, Bobo; Sköld, Christian; Rydfjord, Jonas; Svensson, Fredrik; Behrends, Malte; Sävmarker, Jonas; Sjöberg, Per J R; Larhed, Mats

    2014-12-19

    A fast and efficient protocol for the palladium(II)-catalyzed production of aryl ketones from sodium arylsulfinates and various organic nitriles under controlled microwave irradiation has been developed. The wide scope of the reaction has been demonstrated by combining 14 sodium arylsulfinates and 21 nitriles to give 55 examples of aryl ketones. One additional example illustrated that, through the choice of the nitrile reactant, benzofurans are also accessible. The reaction mechanism was investigated by electrospray ionization mass spectrometry and DFT calculations. The desulfitative synthesis of aryl ketones from nitriles was also compared to the corresponding transformation starting from benzoic acids. Comparison of the energy profiles indicates that the free energy requirement for decarboxylation of 2,6-dimethoxybenzoic acid and especially benzoic acid is higher than the corresponding desulfitative process for generating the key aryl palladium intermediate. The palladium(II) intermediates detected by ESI-MS and the DFT calculations provide a detailed understanding of the catalytic cycle.

  16. A tandem Mannich addition–palladium catalyzed ring-closing route toward 4-substituted-3(2H-furanones

    Directory of Open Access Journals (Sweden)

    Jubi John

    2014-06-01

    Full Text Available A facile route towards highly functionalized 3(2H-furanones via a sequential Mannich addition–palladium catalyzed ring closing has been elaborated. The reaction of 4-chloroacetoacetate esters with imines derived from aliphatic and aromatic aldehydes under palladium catalysis afforded 4-substituted furanones in good to excellent yields. 4-Hydrazino-3(2H-furanones could also be synthesized from diazo esters in excellent yields by utilising the developed strategy. We could also efficiently transform the substituted furanones to aza-prostaglandin analogues.

  17. Natural phosphate-supported palladium: A highly efficient and recyclable catalyst for the suzuki-miyaura coupling under microwave irradiation

    KAUST Repository

    Hassine, Ayoub; Bouhrara, Mohamed; Sebti, Said; Solhy, Abderrahim; Mahfouz, Remi; Luart, Denis; Lene, Christophe; Fihri, Aziz

    2015-01-01

    This report explores Suzuki-Miyaura coupling under microwave irradiation, using a new generation of catalyst that is based on natural phosphate (NP) impregnated by palladium. This catalyst was prepared by the treatment of natural phosphate with bis(benzonitrile)palladium(II) chloride in acetone at room temperature. The catalyst displayed high catalytic activity for the Suzuki-Miyaura coupling of aryl bromides and chlorides with aryl boronic acids in pure water and with the use of microwave irradiation. The low-cost and availability of the solid support, mild reaction conditions, high yields of desired products, recyclability of the catalyst and short reaction times are the notable features of these methods.

  18. Test of the palladium diffuser in the JAERI Fuel Cleanup System in the Tritium Systems Test Assembly

    International Nuclear Information System (INIS)

    Konishi, Satoshi; Hayashi, Takumi; O-hira, Shigeru

    1993-03-01

    The JAERI Fuel Cleanup System (JFCU) is a major subsystem of the TSTA simulated fusion fuel loop. The palladium diffuser, that accepts simulated plasma exhaust and purifies the hydrogen isotopes mixture for the feed to the Isotope Separation System, was tested with deuterium to investigate the characteristics of the components. Permeation flow rate is a linear function of the difference of the square root of the pressure across the palladium alloy membrane. However at the low pressure region, an impediment on the permeation was observed. It was suspected to be caused by the impurity adsorbed on the surface of the permeated side of the membrane and was reduced by oxidation treatment. (author)

  19. Palladium on Nitrogen-Doped Mesoporous Carbon: A Bifunctional Catalyst for Formate-Based, Carbon-Neutral Hydrogen Storage.

    Science.gov (United States)

    Wang, Fanan; Xu, Jinming; Shao, Xianzhao; Su, Xiong; Huang, Yanqiang; Zhang, Tao

    2016-02-08

    The lack of safe, efficient, and economical hydrogen storage technologies is a hindrance to the realization of the hydrogen economy. Reported herein is a reversible formate-based carbon-neutral hydrogen storage system that is established over a novel catalyst comprising palladium nanoparticles supported on nitrogen-doped mesoporous carbon. The support was fabricated by a hard template method and nitridated under a flow of ammonia. Detailed analyses demonstrate that this bicarbonate/formate redox equilibrium is promoted by the cooperative role of the doped nitrogen functionalities and the well-dispersed, electron-enriched palladium nanoparticles. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  20. Antibiofilm effect enhanced by modification of 1,2,3-triazole and palladium nanoparticles on polysulfone membranes

    KAUST Repository

    Cheng, Hong

    2015-01-01

    Biofouling impedes the performance of membrane bioreactors. In this study, we investigated the antifouling effects of polysulfone membranes that were modified by 1,2,3-triazole and palladium nanoparticles. The membranes to be tested were embedded within a drip flow biofilm reactor, and Pseudomonas aeruginosa PAO1 was inoculated and allowed to establish biofilm on the tested membranes. It was found that 1,2,3-triazole and palladium nanoparticles can inhibit the bacterial growth in aerobic and anaerobic conditions. The decrease in bacterial growth was observed along with a decrease in the amount of total polysaccharide and Pel polysaccharide within the biofilm matrix but not the protein content.

  1. Antibiofilm effect enhanced by modification of 1,2,3-triazole and palladium nanoparticles on polysulfone membranes

    KAUST Repository

    Cheng, Hong

    2015-08-01

    Biofouling impedes the performance of membrane bioreactors. In this study, we investigated the antifouling effects of polysulfone membranes that were modified by 1,2,3-triazole and palladium nanoparticles. The membranes to be tested were embedded within a drip flow biofilm reactor, and Pseudomonas aeruginosa PAO1 was inoculated and allowed to establish biofilm on the tested membranes. It was found that 1,2,3-triazole and palladium nanoparticles can inhibit the bacterial growth in aerobic and anaerobic conditions. The decrease in bacterial growth was observed along with a decrease in the amount of total polysaccharide and Pel polysaccharide within the biofilm matrix but not the protein content.

  2. Determination of trace level of palladium and platinum content in anticancer drug Imatinib base by ICP-MS

    International Nuclear Information System (INIS)

    Yadav, Ravi; Salunke-Gawali, Sunita

    2013-01-01

    Metal impurities in Pharmaceutical drug substance is of great concern not only because of the intrinsic toxicity of certain contaminants but also due to the opposite effect that the contaminants which may have on drug stability and shelf life. Therefore it is necessary to monitor the organic as well as inorganic impurities throughout the process of manufacturing process at every stage from raw material, intermediate and finished products. An Inductively Coupled Plasma - Mass Spectrometry (ICP-MS) method has been developed for Palladium and Platinum content in the anticancer drug, Imatinib mesylate. Rhodium (Rh) was used as internal standard for determination of Palladium and Platinum content on in Imatinib mesylate. (author)

  3. Density functional theory metadynamics of silver, caesium and palladium diffusion at β-SiC grain boundaries

    Energy Technology Data Exchange (ETDEWEB)

    Rabone, Jeremy, E-mail: jeremy.rabone@ec.europa.eu [European Commission, Joint Research Centre, Institute for Transuranium Elements, D-76125 Karlsruhe (Germany); López-Honorato, Eddie [Centro de Investigación y de Estudios Avanzados del IPN (CINVESTAV), Unidad Saltillo, Industria Metalúrgica 1062, Parque Industrial, Ramos Arizpe 25900, Coahuila (Mexico)

    2015-03-15

    Highlights: • DFT metadynamics of diffusion of Pd, Ag and Cs on grain boundaries in β-SiC. • The calculated diffusion rates for Pd and Ag tally with experimental release rates. • A mechanism of release other than grain boundary diffusion seems likely for Cs. - Abstract: The use of silicon carbide in coated nuclear fuel particles relies on this materials impermeability towards fission products under normal operating conditions. Determining the underlying factors that control the rate at which radionuclides such as Silver-110m and Caesium-137 can cross the silicon carbide barrier layers, and at which fission products such as palladium could compromise or otherwise alter the nature of this layer, are of paramount importance for the safety of this fuel. To this end, DFT-based metadynamics simulations are applied to the atomic diffusion of silver, caesium and palladium along a Σ5 grain boundary and to palladium along a carbon-rich Σ3 grain boundary in cubic silicon carbide at 1500 K. For silver, the calculated diffusion coefficients lie in a similar range (7.04 × 10{sup −19}–3.69 × 10{sup −17} m{sup 2} s{sup −1}) as determined experimentally. For caesium, the calculated diffusion rates are very much slower (3.91 × 10{sup −23}–2.15 × 10{sup −21} m{sup 2} s{sup −1}) than found experimentally, suggesting a different mechanism to the simulation. Conversely, the calculated atomic diffusion of palladium is very much faster (7.96 × 10{sup −11}–7.26 × 10{sup −9} m{sup 2} s{sup −1}) than the observed penetration rate of palladium nodules. This points to the slow dissolution and rapid regrowth of palladium nodules as a possible ingress mechanism in addition to the previously suggested migration of entire nodules along grain boundaries. The diffusion rate of palladium along the Σ3 grain boundary was calculated to be slightly slower (2.38 × 10{sup −11}–8.24 × 10{sup −10} m{sup 2} s{sup −1}) than along the Σ5 grain boundary. Rather

  4. Natural phosphate-supported palladium: A highly efficient and recyclable catalyst for the suzuki-miyaura coupling under microwave irradiation

    KAUST Repository

    Hassine, Ayoub

    2015-01-19

    This report explores Suzuki-Miyaura coupling under microwave irradiation, using a new generation of catalyst that is based on natural phosphate (NP) impregnated by palladium. This catalyst was prepared by the treatment of natural phosphate with bis(benzonitrile)palladium(II) chloride in acetone at room temperature. The catalyst displayed high catalytic activity for the Suzuki-Miyaura coupling of aryl bromides and chlorides with aryl boronic acids in pure water and with the use of microwave irradiation. The low-cost and availability of the solid support, mild reaction conditions, high yields of desired products, recyclability of the catalyst and short reaction times are the notable features of these methods.

  5. Catalytic Enantioselective Alkylation of β-Keto Esters with Xanthydrol in the Presence of Chiral Palladium Complex

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Kyu Yeon; Kim, Dae Young [Soonchunhyang Univ., Asan (Korea, Republic of)

    2016-01-15

    Our research interest has been directed toward the development of synthetic methods for the enantioselective construction of stereogenic carbon centers. Recently, we explored the catalytic enantioselective functionalization of active methines in the presence of chiral palladium(II) complexes. In conclusion, we have accomplished the efficient catalytic enantioselective alkylation of β-keto esters 1 with xanthydrol 2 with high yields and excellent enantioselectivity (up to 98% ee). It should be noted that this alkyaltion reaction proceeds well using air- and moisture-stable chiral palladium com- plexes with low loading (1 mol%)

  6. Synthesis, characterization, DFT calculations and antibacterial activity of palladium(II) cyanide complexes with thioamides

    Science.gov (United States)

    Ahmad, Saeed; Nadeem, Shafqat; Anwar, Aneela; Hameed, Abdul; Tirmizi, Syed Ahmed; Zierkiewicz, Wiktor; Abbas, Azhar; Isab, Anvarhusein A.; Alotaibi, Mshari A.

    2017-08-01

    Palladium(II) cyanide complexes of thioamides (or thiones) having the general formula PdL2(CN)2, where L = Thiourea (Tu), Methylthiourea (Metu), N,N‧-Dimethylthiourea (Dmtu), Tetramethylthiourea (Tmtu), 2-Mercaptopyridine (Mpy) and 2-Mercaptopyrimidine (Mpm) were prepared by reacting K2[PdCl4] with potassium cyanide and thioamides in the molar ratio of 1:2:2. The complexes were characterized by elemental analysis, thermal and spectroscopic methods (IR, 1H and 13C NMR). The structures of three of the complexes were predicted by DFT calculations. The appearance of a band around 2100 cm-1 in IR and resonances around 120-130 ppm in the 13C NMR spectra indicated the coordination of cyanide to palladium(II). More than one resonances were observed for CN- carbon atoms in 13C NMR indicating the existence of equilibrium between different species in solution. DFT calculations revealed that in the case of the palladium(II) complex of Tmtu, the ionic dinuclear [Pd(Tmtu)4][Pd(CN)4] form was more stable than the dimer of mononuclear complex [Pd(Tmtu)2(CN)2] by 0.91 kcal mol-1, while for the complexes of Tu or Mpy ligands, the nonionic [Pd(L)2(CN)2] forms were more stable than the corresponding [Pd(L)4][Pd(CN)4] complexes by 1.26 and 6.49 kcal mol-1 for L = Tu and Mpy, respectively. The complexes were screened for antibacterial effects and some of them showed significant activities against both gram positive as well as gram negative bacteria.

  7. A Facile Synthesis of a Palladium-Doped Polyaniline-Modified Carbon Nanotube Composites for Supercapacitors

    Science.gov (United States)

    Giri, Soumen; Ghosh, Debasis; Malas, Asish; Das, Chapal Kumar

    2013-08-01

    Supercapacitors have evolved as the premier choice of the era for storing huge amounts of charge in the field of energy storage devices, but it is still necessary to enhance their performance to meet the increasing requirements of future systems. This could be achieved either through advancing the interfaces of the material at the nanoscale or by using novel material compositions. We report a high-performance material composition prepared by combining a transition metal (palladium)-doped conductive polymer with multiwalled carbon nanotubes (MWCNTs). MWCNTs/palladium-doped polyaniline (MWCNTs/Pd/PANI) composites and multiwalled carbon nanotube/polyaniline (MWCNTs/PANI) composites (for comparison) were prepared via in situ oxidative polymerization of aniline monomer. The reported composites were characterized by Fourier-transform infrared (FTIR), x-ray diffraction (XRD), field-emission scanning electron microscopy (FESEM), and transmission electron microscopy (TEM) studies. FESEM and TEM studies indicated the narrow size distribution of the π-conjugated polymer-protected palladium nanoparticles on the surface of the carbon nanotubes. All the electrochemical characterizations were executed using a three-electrode system in 1 M H2SO4 electrolyte. Cyclic voltammetry (CV) analysis was performed to observe the capacitive performance and redox behavior of the composites. The ion transfer behavior and cyclic stability of the composites were investigated by electrochemical impedance spectroscopy (EIS) analysis and cyclic charge-discharge (CCD) testing, respectively. The MWCNTs/Pd/PANI composite was found to exhibit an especially high specific capacitance value of 920 F/g at scan rate of 2 mV/s.

  8. Effects of palladium coatings on oxygen sensors of titanium dioxide thin films

    International Nuclear Information System (INIS)

    Castaneda, L.

    2007-01-01

    Titanium dioxide (TiO 2 -anatase phase) thin films were deposited by the ultrasonic spray pyrolysis technique employing titanium (IV) oxide acetylacetonate (TiO(acac) 2 ) dissolved in pure methanol as a source material. In order to prepare oxygen sensors, TiO 2 thin films were deposited on interdigitated gold electrodes with contacted alumina substrates. Palladium (Pd) coatings were carried out by vacuum thermal evaporation through a metallic mask. The effect of the surface additive (Pd) on the response of the thin film TiO 2 oxygen sensors was monitored in a mixture with zero-grade air. The electrical characterization (monitoring of the electrical surface resistance with the operation temperature) of the sensors in an atmosphere of oxygen (diluted in zero-grade air) was performed in a vacuum chamber (10 -6 Torr), where the gas pressure can be controlled. The films sensitivity was estimated by the following relation: s=R gas -R 0 /R 0 . The response time of the sensor is defined to be the time needed to reach a 0.9R 0 value when the oxygen excess is removed. The gas-sensing properties of TiO 2 sensors in an atmosphere of 10 4 ppm of oxygen were measured between 100 and 450 deg. C. Experimental results obtained using palladium as a surface additive show that the sensitivity reaches a stationary value of 1.18 for O 2 concentration of 100ppm in zero-grade air at 300 deg. C, which is as high as those reported for oxygen sensors prepared with more expensive and complex techniques. The role and activity of palladium coatings incorporated on solid-state oxygen sensors are determined by their chemical state, aggregation form and interaction with the metal-oxide semiconductor

  9. Facile synthesis of palladium nanoparticle doped polyaniline nanowires in soft templates for catalytic applications

    Science.gov (United States)

    Kshirasagar, Krushna J.; Markad, Uddhav S.; Saha, Abhijit; Sharma, Kiran Kumar K.; Sharma, Geeta K.

    2017-02-01

    Palladium nanoparticles doped polyaniline (Pd-PANI) nanocomposite (NCs) is synthesized in surfactant based liquid crystalline mesophase by chemical oxidation followed by radiolysis. The confinement of the liquid crystalline mesophase facilitates polymerization of aniline monomers and their 1D growth into polyaniline (PANI) nanowires by using ammonium persulfate. The PANI nanowires have an average diameter of 30-40 nm. The in situ radiolytic reduction of palladium ions ensures uniform size distribution of the palladium (Pd) nanoparticles on the surface of the PANI nanowires. The synthesized Pd-PANI nanocomposites show wire like structures of PANI (diameter ~30-40 nm) on which Pd nanoparticles of the size 10 nm are decorated. The identical average diameter of the PANI nanowires before and post gamma irradiation suggest high stability of the PANI nanowires in liquid crystalline mesophase. Surface characterization of the NCs were carried out using BET and XPS. The catalytic activity of Pd-PANI NCs are investigated in the reduction of methylene blue (MB) and 4-nitro phenol (4-NP) by sodium borohydride (NaBH4). The kinetics of the Pd-PANI NCs catalysed reactions are analysed using the Langmuir-Hinshelwood model. The apparent rate constant (k app) for the MB and 4-NP reduction reactions is 29  ×  10-3 s-1 and 20  ×  10-3 s-1 respectively with an actual Pd catalyst loading of 2.665  ×  10-4 ppm. Further, the recyclability of the Pd-PANI NCs catalyst in both the reduction reactions shows the stability of the catalyst up to four reaction cycles tested in this investigation and the multifunctional nature of the catalyst. The study provides a new approach for the directional synthesis of conducting polymer-metal nanocomposites and their possible application as a nanocatalyst in environmental remediation.

  10. Effects of soldering methods on tensile strength of a gold-palladium metal ceramic alloy.

    Science.gov (United States)

    Ghadhanfari, Husain A; Khajah, Hasan M; Monaco, Edward A; Kim, Hyeongil

    2014-10-01

    The tensile strength obtained by conventional postceramic application soldering and laser postceramic welding may require more energy than microwave postceramic soldering, which could provide similar tensile strength values. The purpose of the study was to compare the tensile strength obtained by microwave postceramic soldering, conventional postceramic soldering, and laser postceramic welding. A gold-palladium metal ceramic alloy and gold-based solder were used in this study. Twenty-seven wax specimens were cast in gold-palladium noble metal and divided into 4 groups: laser welding with a specific postfiller noble metal, microwave soldering with a postceramic solder, conventional soldering with the same postceramic solder used in the microwave soldering group, and a nonsectioned control group. All the specimens were heat treated to simulate a normal porcelain sintering sequence. An Instron Universal Testing Machine was used to measure the tensile strength for the 4 groups. The means were analyzed statistically with 1-way ANOVA. The surface and fracture sites of the specimens were subjectively evaluated for fracture type and porosities by using a scanning electron microscope. The mean (standard deviation) ultimate tensile strength values were as follows: nonsectioned control 818 ±30 MPa, microwave 516 ±34 MPa, conventional 454 ±37 MPa, and laser weld 191 ±39 MPa. A 1-way ANOVA showed a significant difference in ultimate tensile strength among the groups (F3,23=334.5; Ptensile strength for gold and palladium noble metals than either conventional soldering or laser welding. Conventional soldering resulted in a higher tensile strength than laser welding. Under the experimental conditions described, either microwave or conventional postceramic soldering would appear to satisfy clinical requirements related to tensile strength. Copyright © 2014 Editorial Council for the Journal of Prosthetic Dentistry. Published by Elsevier Inc. All rights reserved.

  11. Catalytic Palladium Film Deposited by Scalable Low-Temperature Aqueous Combustion.

    Science.gov (United States)

    Voskanyan, Albert A; Li, Chi-Ying Vanessa; Chan, Kwong-Yu

    2017-09-27

    This article describes a novel method for depositing a dense, high quality palladium thin film via a one-step aqueous combustion process which can be easily scaled up. Film deposition of Pd from aqueous solutions by conventional chemical or electrochemical methods is inhibited by hydrogen embrittlement, thus resulting in a brittle palladium film. The method outlined in this work allows a direct aqueous solution deposition of a mirror-bright, durable Pd film on substrates including glass and glassy carbon. This simple procedure has many advantages including a very high deposition rate (>10 cm 2 min -1 ) and a relatively low deposition temperature (250 °C), which makes it suitable for large-scale industrial applications. Although preparation of various high-quality oxide films has been successfully accomplished via solution combustion synthesis (SCS) before, this article presents the first report on direct SCS production of a metallic film. The mechanism of Pd film formation is discussed with the identification of a complex formed between palladium nitrate and glycine at low temperature. The catalytic properties and stability of films are successfully tested in alcohol electrooxidation and electrochemical oxygen reduction reaction. It was observed that combustion deposited Pd film on a glassy carbon electrode showed excellent catalytic activity in ethanol oxidation without using any binder or additive. We also report for the first time the concept of a reusable "catalytic flask" as illustrated by the Suzuki-Miyaura cross-coupling reaction. The Pd film uniformly covers the inner walls of the flask and eliminates the catalyst separation step. We believe the innovative concept of a reusable catalytic flask is very promising and has the required features to become a commercial product in the future.

  12. Palladium nanoparticles exposure: Evaluation of permeation through damaged and intact human skin.

    Science.gov (United States)

    Larese Filon, Francesca; Crosera, Matteo; Mauro, Marcella; Baracchini, Elena; Bovenzi, Massimo; Montini, Tiziano; Fornasiero, Paolo; Adami, Gianpiero

    2016-07-01

    The intensified use of palladium nanoparticles (PdNPs) in many chemical reactions, jewellery, electronic devices, in car catalytic converters and in biomedical applications lead to a significant increase in palladium exposure. Pd can cause allergic contact dermatitis when in contact with the skin. However, there is still a lack of toxicological data related to nano-structured palladium and information on human cutaneous absorption. In fact, PdNPs, can be absorbed through the skin in higher amounts than bulk Pd because NPs can release more ions. In our study, we evaluated the absorption of PdNPs, with a size of 10.7 ± 2.8 nm, using intact and damaged human skin in Franz cells. 0.60 mg cm(-2) of PdNPs were applied on skin surface for 24 h. Pd concentrations in the receiving solutions at the end of experiments were 0.098 ± 0.067 μg cm(-2) and 1.06 ± 0.44 μg cm(-2) in intact skin and damaged skin, respectively. Pd flux permeation after 24 h was 0.005 ± 0.003 μg cm(-2) h(-1) and 0.057 ± 0.030 μg cm(-2) h(-1) and lag time 4.8 ± 1.7 and 4.2 ± 3.6 h, for intact and damaged skin respectively. This study indicates that Pd can penetrate human skin. Copyright © 2016 Elsevier Ltd. All rights reserved.

  13. Size effects in electronic and catalytic properties of unsupported palladium nanoparticles in electrooxidation of formic acid.

    Science.gov (United States)

    Zhou, Wei Ping; Lewera, Adam; Larsen, Robert; Masel, Rich I; Bagus, Paul S; Wieckowski, Andrzej

    2006-07-13

    We report a combined X-ray photoelectron spectroscopy (XPS), cyclic voltammetry (CV), and chronoamperometry (CA) study of formic acid electrooxidation on unsupported palladium nanoparticle catalysts in the particle size range from 9 to 40 nm. The CV and CA measurements show that the most active catalyst is made of the smallest (9 and 11 nm) Pd nanoparticles. Besides the high reactivity, XPS data show that such nanoparticles display the highest core-level binding energy (BE) shift and the highest valence band (VB) center downshift with respect to the Fermi level. We believe therefore that we found a correlation between formic acid oxidation current and BE and VB center shifts, which, in turn, can directly be related to the electronic structure of palladium nanoparticles of different particle sizes. Clearly, such a trend using unsupported catalysts has never been reported. According to the density functional theory of heterogeneous catalysis, and mechanistic considerations, the observed shifts are caused by a weakening of the bond strength of the COOH intermediate adsorption on the catalyst surface. This, in turn, results in the increase in the formic acid oxidation rate to CO2 (and in the associated oxidation current). Overall, our measurements demonstrate the particle size effect on the electronic properties of palladium that yields different catalytic activity in the HCOOH oxidation reaction. Our work highlights the significance of the core-level binding energy and center of the d-band shifts in electrocatalysis and underlines the value of the theory that connects the center of the d-band shifts to catalytic reactivity.

  14. Manufacturing process and electrode properties of palladium-electroded ionic polymer–metal composite

    International Nuclear Information System (INIS)

    Chang, Longfei; Chen, Hualing; Zhu, Zicai; Li, Bo

    2012-01-01

    This paper primarily focuses on the manufacturing process of palladium-electroded ionic polymer–metal composite (IPMC). First, according to the special properties of Pd, many experiments were done to determine several specific procedures, including the addition of a reducing agent and the time consumed. Subsequently, the effects of the core manufacturing steps on the electrode morphology were revealed by scanning electron microscopy studies of 22 IPMC samples treated with different combinations of manufacturing steps. Finally, the effects of electrode characteristics on the electromechanical properties, including the sheet resistivity, the elastic modulus and the electro-active performance, of IPMCs were evaluated experimentally and analyzed according to the electrode morphology. (paper)

  15. Kinetics of oxygen reduction reaction at electrochemically fabricated tin-palladium bimetallic electrocatalyst in acidic media

    Energy Technology Data Exchange (ETDEWEB)

    Miah, Md. Rezwan, E-mail: mrmche@yahoo.co [Department of Electronic Chemistry, Interdisciplinary Graduate School of Science and Engineering, Tokyo Institute of Technology, Mail Box G1-5, 4259 Nagatsuta, Midori-ku, Yokohama 226-8502 (Japan); Masud, Jahangir [Department of Electronic Chemistry, Interdisciplinary Graduate School of Science and Engineering, Tokyo Institute of Technology, Mail Box G1-5, 4259 Nagatsuta, Midori-ku, Yokohama 226-8502 (Japan); Ohsaka, Takeo, E-mail: ohsaka@echem.titech.ac.j [Department of Electronic Chemistry, Interdisciplinary Graduate School of Science and Engineering, Tokyo Institute of Technology, Mail Box G1-5, 4259 Nagatsuta, Midori-ku, Yokohama 226-8502 (Japan)

    2010-12-15

    In the present article, oxygen reduction reaction (ORR) at electrochemically fabricated tin-palladium (Sn-Pd) bimetallic electrocatalyst-modified glassy carbon (GC) electrode (Sn-Pd/GC electrode) in acidic media is addressed. Hydrodynamic voltammetric measurements were employed with a view to evaluating various kinetic parameters of the ORR at the Sn-Pd/GC electrode. The obtained results obviously demonstrated that the Sn-Pd bimetallic electrocatalyt substantially promoted the activity of the GC electrode and drove the ORR through an exclusive one-step four-electron pathway forming H{sub 2}O as the final product.

  16. Kinetics of oxygen reduction reaction at electrochemically fabricated tin-palladium bimetallic electrocatalyst in acidic media

    International Nuclear Information System (INIS)

    Miah, Md. Rezwan; Masud, Jahangir; Ohsaka, Takeo

    2010-01-01

    In the present article, oxygen reduction reaction (ORR) at electrochemically fabricated tin-palladium (Sn-Pd) bimetallic electrocatalyst-modified glassy carbon (GC) electrode (Sn-Pd/GC electrode) in acidic media is addressed. Hydrodynamic voltammetric measurements were employed with a view to evaluating various kinetic parameters of the ORR at the Sn-Pd/GC electrode. The obtained results obviously demonstrated that the Sn-Pd bimetallic electrocatalyt substantially promoted the activity of the GC electrode and drove the ORR through an exclusive one-step four-electron pathway forming H 2 O as the final product.

  17. Palladium catalyst system comprising zwitterion and/or acid-​functionalized ionic liquid

    DEFF Research Database (Denmark)

    2011-01-01

    The present invention concerns a catalyst system in particular a catalyst system comprising Palladium (Pd), a zwitterion and/or an acid-functionalized ionic liquid, and one or more phosphine ligands, wherein the Pd catalyst can be provided by a complex precursor, such as Pd(CH3COO)2, PdCI2, Pd(CH3...... methyl methacrylate and/or methacrylic acid. Catalyst systems according to the invention are suitable for reactions forming separable product and catalyst phases and supported ionic liquid phase SILP applications....

  18. Copolymerization of carbon monoxide and styrene catalyzed by resin-supported palladium polymer

    Directory of Open Access Journals (Sweden)

    2007-02-01

    Full Text Available Polyketone was prepared by the copolymerization of carbon monoxide (CO and styrene (ST catalyzed by o-phenylenediamine resin-supported palladium acetate. Effects of each catalytic system component such as 2,2’-bipyridine, 1,4-quinone and p-toluene-sulphonate on the copolymerization were investigated. The resin-supported catalyst and the copolymerization product were characterized by infrared spectroscopy (IR, differential scanning calorimetry (DSC, thermogravimetry (TG, X-ray photoelectron spectroscopy (XPS, Scanning Electron Microscopy (SEM. Results indicated that the resin-supported catalyst has excellent catalytic property. Furthermore, partial catalytic activity was maintained after the catalyst was used for five times.

  19. Artificial crystals with 3d metal and palladium particles subjected to high-temperature heat treatment

    Science.gov (United States)

    Rinkevich, A. B.; Nemytova, O. V.; Perov, D. V.; Samoylovich, M. I.; Kuznetsov, E. A.

    2018-04-01

    High-temperature heat treatment has valuable impact on the structure and physical properties of artificial crystals with 3d metal and palladium particles. Artificial crystals are obtained by means of introduction of particles into the interspherical voids of opal matrices. The magnetic properties are studied at the temperatures ranging from 2 to 300 K and in fields up to 350 kOe. Microwave properties are investigated in the millimeter frequency range. The complex dielectric permittivity of several nanocomposites is measured. The influence of heat treatment up to 960 °C on the structure of artificial crystals is clarified.

  20. On problems of hydrogen load of sponge palladium and determination of hydrogen content in it

    International Nuclear Information System (INIS)

    Mittag, E.; Pleis, U.; Roemer, J.

    1977-01-01

    In the process of catalytic dehalogenation applied as a method for preparation of organic compounds labelled with tritium a special importance pertains to the determination of hydrogen (or tritium) bound on the catalyst. Hydrogen contained in palladium black may be determined quantitatively by oxidation with Pd ++ ions and successive potentiometric titration of the released H + ions. The method permits to obtain data on the quality of the catalyst and on the gas losses on the catalyst. Moreover, in connection with the radioactivity measurement, this method may be used for specific activity determination of the tritium gas

  1. Electrochemical permeation tests on the kinetics of the hydrogen absorption of palladium and iron

    International Nuclear Information System (INIS)

    Dafft, E.G.

    1977-01-01

    Electrochemical permeation tests were performed to investigate the kinetics of the hydrogen development and hydrogen absorption. The cathode side of the samples was galvanostatically cathodically polarized in different electrolyte solutions with and without additions. THe hydrogen atoms diffusing out of the opposite side for iron and α-palladium were oxidized with potentiostatic, sufficiently anodic polarization. The thus registered stationary current is proportional to the hydrogen activity on the cathode side. Test apparatus and conditions are described. The measurements on iron are discussed. (orig./HPOE) [de

  2. Heteroaryl ethers by oxidative palladium catalysis of pyridotriazol-1-yloxy pyrimidines with arylboronic acids.

    Science.gov (United States)

    Bardhan, Sujata; Wacharasindhu, Sumrit; Wan, Zhao-Kui; Mansour, Tarek S

    2009-06-18

    The oxidative palladium-catalyzed cross-coupling of pyrimidines containing pyridotriazol-1-yloxy (OPt) as either a urea or an amide functional group with arylboronic acids in the presence of Cs(2)CO(3) in DME containing 0.6-1.0% H(2)O is described for the preparation of heteroaryl ethers. The bromo substitution in the case of 3-(5-bromo-pyrimidin-2-yloxy)-3H-[1,2,3]triazolo[4,5-b]pyridine 1 could serve as a handle for further elaborations such as Suzuki coupling for attaching varied aryl groups.

  3. Reactivity of Aryl Halides for Reductive Dehalogenation in (Seawater Using Polymer-Supported Terpyridine Palladium Catalyst

    Directory of Open Access Journals (Sweden)

    Toshimasa Suzuka

    2015-05-01

    Full Text Available A polymer-supported terpyridine palladium complex was prepared. The complex was found to promote hydrodechlorination of aryl chlorides with potassium formate in seawater. Generally, reductive cleavage of aryl chlorides using transition metal catalysts is more difficult than that of aryl bromides and iodides (reactivity: I > Br > Cl; however, the results obtained did not follow the general trend. Therefore, we investigated the reaction inhibition agents and found a method to remove these inhibitors. The polymeric catalysts showed high catalytic activity and high reusability for transfer reduction in seawater.

  4. Mild Palladium Catalyzed ortho C-H Bond Functionalizations of Aniline Derivatives.

    Science.gov (United States)

    Tischler, Ms Orsolya; Tóth, Mr Balázs; Novák, Zoltán

    2017-02-01

    This account collects the developments and transformations which avoid the utilization of harsh reaction conditions in the field of palladium catalyzed, ortho-directed C-H activation of aniline derivatives from the first attempts to up-to-date results, including the results of our research laboratory. The discussed functionalizations performed under mild conditions include acylation, olefination, arylation, alkylation, alkoxylation reactions. Beside the optimization studies and the synthetic applications mechanistic investigations are also presented. © 2017 The Chemical Society of Japan & Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  5. Carbon monoxide migratory insertion - A comparison of cationic and neutral palladium(II) complexes

    International Nuclear Information System (INIS)

    Frankcombe, K.; Cavell, K.J.; Yates, B.F.; Knott, R.B.

    1998-01-01

    With the use of ANSTO's resources and expertise and with support from AINSE, we have carried out extensive computer modelling on the mechanism of the palladium catalysed carbonylation reaction, a process which is used industrially in the conversion of carbon monoxide into biodegradable polymers. In this project, experimental and theoretical work has focussed on using Pd(II) complexes containing pyridine carboxylate ligands (NC 5 H 4 COO ) to explore the fundamental mechanistic steps. The results for subsequent steps in the catalytic cycle are presented and their implication for the design of more efficient catalysts are discussed

  6. Thermal neutron measurements on electrolytic cells with deuterated palladium cathodes subjected to a pulsed current

    International Nuclear Information System (INIS)

    Granada, J.R.; Mayer, R.E.; Guido, G.; Florido, P.C.; Larreteguy, A.; Gillette, V.H.; Patino, N.E.; Converti, J.; Gomez, S.E.

    1990-01-01

    The present work describes the design of a high efficiency thermal neutron detection system and the measurements performed with it on electrolytic cells containing LiH dissolved in D 2 O with palladium cathodes. A procedure involving the use of a non-stationary (pulsed) current through the cell caused a correlated neutron production to be observed in a repeatable manner. These patterns are strongly dependent on the previous charging history of the cathodes. The technique employed seems to be very useful as a research tool for a systematic study of the different variables governing the phenomenon. (author)

  7. Synthesis of monodisperse palladium nanocubes and their catalytic activity for methanol electrooxidation

    International Nuclear Information System (INIS)

    Hao, Ding; Xue-Zhao, Shi; Cheng-Min, Shen; Chao, Hui; Zhi-Chuan, Xu; Chen, Li; Yuan, Tian; Deng-Ke, Wang; Hong-Jun, Gao

    2010-01-01

    The single crystalline palladium nanocubes with an average size of 7 nm were prepared in the presence of poly (vinyl pyrrolidone) (PVP) and KBr using the polyol method. The as-prepared Pd nanocubes were highly uniform in both size and shape. The ordered packing structures including monolayer and multilayer can be fabricated via the rate-controlled evaporation of solution solvent. The electrochemical catalytic activity of these Pd nanocubes towards methanol oxidation was found to be higher than that of spherical Pd nanoparticles of similar size. (condensed matter: structure, thermal and mechanical properties)

  8. Synthesis of monodisperse palladium nanocubes and their catalytic activity for methanol electrooxidation

    Science.gov (United States)

    Ding, Hao; Shi, Xue-Zhao; Shen, Cheng-Min; Hui, Chao; Xu, Zhi-Chuan; Li, Chen; Tian, Yuan; Wang, Deng-Ke; Gao, Hong-Jun

    2010-10-01

    The single crystalline palladium nanocubes with an average size of 7 nm were prepared in the presence of poly (vinyl pyrrolidone) (PVP) and KBr using the polyol method. The as-prepared Pd nanocubes were highly uniform in both size and shape. The ordered packing structures including monolayer and multilayer can be fabricated via the rate-controlled evaporation of solution solvent. The electrochemical catalytic activity of these Pd nanocubes towards methanol oxidation was found to be higher than that of spherical Pd nanoparticles of similar size.

  9. Palladium-catalyzed ring-opening reactions of cyclopropanated 7-oxabenzonorbornadiene with alcohols

    Directory of Open Access Journals (Sweden)

    Katrina Tait

    2016-10-01

    Full Text Available Palladium-catalyzed ring-opening reactions of cyclopropanated 7-oxabenzonorbornadiene derivatives using alcohol nucleophiles were investigated. The optimal conditions were found to be 10 mol % PdCl2(CH3CN2 in methanol, offering yields up to 92%. The reaction was successful using primary, secondary and tertiary alcohol nucleophiles and was compatible with a variety of substituents on cyclopropanated oxabenzonorbornadiene. With unsymmetrical C1-substituted cyclopropanated 7-oxabenzonorbornadienes, the regioselectivity of the reaction was excellent, forming only one regioisomer in all cases.

  10. Palladium-catalyzed arylation of enoates with iodobenzene: stereoselective synthesis of trisubstituted olefins

    Energy Technology Data Exchange (ETDEWEB)

    Fernandes, Talita de A. [Universidade Federal do Rio de Janeiro (UFRJ/LQB), RJ (Brazil). Nucleo de Pesquisas de Produtos Naturais. Laboratorio de Quimica Bioorganica; Universidade Federal do Rio de Janeiro (UFRJ), RJ (Brazil). Instituto de Quimica. Interlab; Silva, Alcides J.M. da; Costa, Paulo R.R., E-mail: prrcosta2011@gmail.com [Universidade Federal do Rio de Janeiro (UFRJ/LQB), RJ (Brazil). Nucleo de Pesquisas de Produtos Naturais. Laboratorio de Quimica Bioorganica; Esteves, Pierre M. [Universidade Federal do Rio de Janeiro (UFRJ), RJ (Brazil). Instituto de Quimica. Interlab; Eberlin, Marcos N., E-mail: eberlin@iqm.unicamp.br [Universidade Estadual de Campinas (UNICAMP), SP (Brazil). Instituto de Quimica. Laboratorio ThoMSon de Espectrometria de Massas; Vaz, Boniek G. [Universidade Estadual de Campinas (UNICAMP), SP (Brazil). Instituto de Quimica. Laboratorio ThoMSon de Espectrometria de Massas; Universidade Federal de Goias (UFGO), Goiania, GO (Brazil). Instituto de QuImica

    2013-03-15

    The Heck reaction between E- and Z-enoates and iodobenzene was studied in the presence of Pd(OAc){sub 2}. The stereochemistry in resulting adducts was dependent on the enoate geometry (stereospecific reaction). Best yields were obtained from Z-isomers in acetone using Ag{sub 2} CO{sub 3} as base. The main cationic palladium intermediates possibly involved in the catalytic cycle could be intercepted and characterized by electrospray ionization mass spectrometry (ESI-MS). The stereoselectivity observed was rationalized through the classic mechanism of the Heck reaction. (author)

  11. Mechanistic study of the isotopic-exchange reaction between gaseous hydrogen and palladium hydride powder

    International Nuclear Information System (INIS)

    Outka, D.A.; Foltz, G.W.

    1991-01-01

    A detailed mechanism for the isotopic-exchange reaction between gaseous hydrogen and solid palladium hydride is developed which extends previous model for this reaction by specifically including surface reactions. The modeling indicates that there are two surface-related processes that contribute to the overall rate of exchange: the desorption of hydrogen from the surface and the exchange between surface hydrogen and bulk hydrogen. This conclusion is based upon measurements examining the effect of small concentrations of carbon monoxide were helpful in elucidating the mechanism. Carbon monoxide reversibly inhibits certain steps in the exchange; this slows the overall rate of exchange and changes the distribution of products from the reactor

  12. Platinum, palladium, and rhodium in volcanic and plutonic rocks from the Gravina-Nutzotin belt, Alaska

    Science.gov (United States)

    Page, Norman J; Berg, Henry C.; Haffty, Joseph

    1977-01-01

    The Gravina-Nutzotin belt of Middle (?) Jurassic to middle Cretaceous sedimentary and volcanic rocks in south and southeastern Alaska includes concentrically zoned ultramafic complexes known to contain platinum-group metals. Previous isotopic, petrologic, and geologic studies suggested a close relation in time and space between the volcanic rocks and the ultramafic complexes. Interpretation of 40 analyses for platinum, palladium, and rhodium in volcanic and plutonic rocks of the belt indicates a strong geochemical correlation between the two groups of rocks and is in support of their being cogenetic either from directly connected magma chambers and flows or indirectly by selective concentration processes from similar mantle material.

  13. Platinum, palladium, and rhodium analyses of ultramafic and mafic rocks from the Stillwater Complex, Montana

    Science.gov (United States)

    Page, Norman J; Riley, Leonard Benjamin; Haffty, Joseph

    1969-01-01

    Analyses by a combination fire- assay-solution-optical-emission spectrographic method of 137 rocks from the Stillwater Complex, Mont., indicate that platinum, palladium, and rhodium are preferentially concentrated in chromitite zones. The A chromitite zone (21 samples) has an average of 988.9 ppb (pans per billion, 10-9) Pt, 2290.2 ppb Pd, and 245.9 ppb Rh and reaches a maximum (to date) of 8,000 ppb Pt, 11,000 ppb Pd, and 1,700 ppb Rh.

  14. Palladium-catalyzed arylation of enoates with iodobenzene: stereoselective synthesis of trisubstituted olefins

    International Nuclear Information System (INIS)

    Fernandes, Talita de A.; Universidade Federal do Rio de Janeiro; Silva, Alcides J.M. da; Costa, Paulo R.R.; Esteves, Pierre M.; Eberlin, Marcos N.; Vaz, Boniek G.; Universidade Federal de Goias

    2013-01-01

    The Heck reaction between E- and Z-enoates and iodobenzene was studied in the presence of Pd(OAc) 2 . The stereochemistry in resulting adducts was dependent on the enoate geometry (stereospecific reaction). Best yields were obtained from Z-isomers in acetone using Ag 2 CO 3 as base. The main cationic palladium intermediates possibly involved in the catalytic cycle could be intercepted and characterized by electrospray ionization mass spectrometry (ESI-MS). The stereoselectivity observed was rationalized through the classic mechanism of the Heck reaction. (author)

  15. Scope and mechanism in palladium-catalyzed isomerizations of highly substituted allylic, homoallylic, and alkenyl alcohols.

    Science.gov (United States)

    Larionov, Evgeny; Lin, Luqing; Guénée, Laure; Mazet, Clément

    2014-12-03

    Herein we report the palladium-catalyzed isomerization of highly substituted allylic alcohols and alkenyl alcohols by means of a single catalytic system. The operationally simple reaction protocol is applicable to a broad range of substrates and displays a wide functional group tolerance, and the products are usually isolated in high chemical yield. Experimental and computational mechanistic investigations provide complementary and converging evidence for a chain-walking process consisting of repeated migratory insertion/β-H elimination sequences. Interestingly, the catalyst does not dissociate from the substrate in the isomerization of allylic alcohols, whereas it disengages during the isomerization of alkenyl alcohols when additional substituents are present on the alkyl chain.

  16. Palladium-Catalyzed Tandem Oxidative Arylation/Olefination of Aromatic Tethered Alkenes/Alkynes.

    Science.gov (United States)

    Gao, Yang; Gao, Yinglan; Wu, Wanqing; Jiang, Huanfeng; Yang, Xiaobo; Liu, Wenbo; Li, Chao-Jun

    2017-01-18

    We describe herein a palladium-catalyzed tandem oxidative arylation/olefination reaction of aromatic tethered alkenes/alkynes for the synthesis of dihydrobenzofurans and 2 H-chromene derivatives. This reaction features a 1,2-difunctionalization of C-C π-bond with two C-H bonds using O 2 as terminal oxidant at room temperature. The products obtained are valuable synthons and important scaffolds in biological agents and natural products. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  17. Study of transport and micro-structural properties of magnesium di-boride strand under react and bend mode and bend and react mode

    International Nuclear Information System (INIS)

    Kundu, Ananya; Das, Subrat Kumar; Bano, Anees; Pradhan, Subrata

    2015-01-01

    I-V characterization of commercial multi-filamentary Magnesium Di-Boride (MgB 2 ) wire of diameter 0.83 mm were studied in cryocooler based self-field characterization system under both react and bent mode and bent and react mode for a range of temperature 6 K - 25 K. This study is of practical technical relevance where the heat treatment of the superconducting wire makes the sample less flexible for winding in magnet and in other applications. There are limited reported data, available on degradation of MgB 2 wire with bending induced strain in react and wind and wind and react method. In the present work the bending diameter were varied from 80 mm to 20 mm in the interval of 10 mm change of bending diameter and for each case critical current (Ic) of the strand is measured for the above range of temperature. An ETP copper made customized sample holder for mounting the MgB 2 strand was fabricated and is thermally anchored to the cooling stage of the cryocooler. It is seen from the experimental data that in react and bent mode the critical current degrades from 105 A to 87 A corresponding to bending diameter of 80 mm and 20 mm respectively. The corresponding bending strain was analytically estimated and compared with the simulation result. It is also observed that in react and bent mode, the degradation of the transport property of the strand is less as compared to react and bent mode. For bent and react mode in the same sample, the critical current (Ic) was measured to be ∼145 A at 15 K for bending diameter of 20 mm. Apart from studying the bending induced strain on MgB 2 strand, the tensile test of the strand at RT was carried out. The electrical characterizations of the samples were accompanied by the microstructure analyses of the bent strand to examine the bending induced degradation in the grain structure of the strand. All these experimental findings are expected to be used as input to fabricate prototype MgB 2 based magnet. (author)

  18. The production of carbon nanofibers and thin films on palladium catalysts from ethylene oxygen mixtures

    Energy Technology Data Exchange (ETDEWEB)

    Phillips, Jonathan [Los Alamos National Laboratory; Doorn, Stephen [Los Alamos National Laboratory; Atwater, Mark [UNM MECH.ENG.; Leseman, Zayd [UNM MECH.ENG.; Luhrs, Claudia C [UNM ENG.MECH; Diez, Yolanda F [SPAIN; Diaz, Angel M [SPAIN

    2009-01-01

    The characteristics of carbonaceous materials deposited in fuel rich ethylene-oxygen mixtures on three types of palladium: foil, sputtered film, and nanopowder, are reported. It was found that the form of palladium has a dramatic influence on the morphology of the deposited carbon. In particular, on sputtered film and powder, tight 'weaves' of sub-micron filaments formed quickly. In contrast, on foils under identical conditions, the dominant morphology is carbon thin films with basal planes oriented parallel to the substrate surface. Temperature, gas flow rate, reactant flow ratio (C2H4:02), and residence time (position) were found to influence both growth rate and type for all three forms of Pd. X-ray diffraction, high-resolution transmission electron microscopy, temperature-programmed oxidation, and Raman spectroscopy were used to assess the crystallinity of the as-deposited carbon, and it was determined that transmission electron microscopy and x-ray diffraction were the most reliable methods for determining crystallinity. The dependence of growth on reactor position, and the fact that no growth was observed in the absence of oxygen support the postulate that the carbon deposition proceeds by combustion generated radical species.

  19. Palladium Gate All Around - Hetero Dielectric -Tunnel FET based highly sensitive Hydrogen Gas Sensor

    Science.gov (United States)

    Madan, Jaya; Chaujar, Rishu

    2016-12-01

    The paper presents a novel highly sensitive Hetero-Dielectric-Gate All Around Tunneling FET (HD-GAA-TFET) based Hydrogen Gas Sensor, incorporating the advantages of band to band tunneling (BTBT) mechanism. Here, the Palladium supported silicon dioxide is used as a sensing media and sensing relies on the interaction of hydrogen with Palladium-SiO2-Si. The high surface to volume ratio in the case of cylindrical GAA structure enhances the fortuities for surface reactions between H2 gas and Pd, and thus improves the sensitivity and stability of the sensor. Behaviour of the sensor in presence of hydrogen and at elevated temperatures is discussed. The conduction path of the sensor which is dependent on sensors radius has also been varied for the optimized sensitivity and static performance analysis of the sensor where the proposed design exhibits a superior performance in terms of threshold voltage, subthreshold swing, and band to band tunneling rate. Stability of the sensor with respect to temperature affectability has also been studied, and it is found that the device is reasonably stable and highly sensitive over the bearable temperature range. The successful utilization of HD-GAA-TFET in gas sensors may open a new door for the development of novel nanostructure gas sensing devices.

  20. Sulphur poisoning of palladium catalysts used for methane combustion: Effect of the support

    International Nuclear Information System (INIS)

    Escandon, Lara S.; Ordonez, Salvador; Vega, Aurelio; Diez, Fernando V.

    2008-01-01

    Four different supported palladium catalysts (using alumina, silica, zirconia and titania as supports), prepared by incipient wetness impregnation, were tested as catalysts for methane oxidation in presence of sulphur dioxide. The catalyst supported on zirconia showed the best performance, whereas the silica-supported one showed the fastest deactivation. Temperature-programmed desorption experiments of the poisoned catalysts suggest that SO 2 adsorption capacity of the support plays a key role in the catalyst poisoning. In order to study the effect of promoters, expected to improve the thermal stability and thioresistance of the catalyst, commercial zirconia modified by yttrium and lantane was tested as supports. It was found that the presence of these promoters does not improve the performance of the zirconia-supported catalyst. A deactivation model - considering two different active sites (fresh and poisoning), pseudo-first order dependence on methane concentration and poisoning rate depending on sulphur concentration and fraction of non-poisoned palladium - was used for modelling the deactivation behaviour

  1. Palladium nanoparticles anchored on graphene nanosheets: Methanol, ethanol oxidation reactions and their kinetic studies

    KAUST Repository

    Nagaraju, Doddahalli H.

    2014-12-01

    Palladium nanoparticles decorated graphene (Gra/Pd nanocomposite) was synthesized by simultaneous chemical reduction of graphene oxide and palladium salt in a single step. The negatively charged graphene oxide (GO) facilitates uniform distribution of Pd2+ ions onto its surface. The subsequent reduction by hydrazine hydrate provides well dispersed Pd nanoparticles decorated graphene. Different amount of Pd nanoparticles on graphene was synthesized by changing the volume to weight ratio of GO to PdCl2. X-ray diffraction studies showed FCC lattice of Pd with predominant (1 1 1) plane. SEM and TEM studies revealed that thin graphene nanosheets are decorated by Pd nanoparticles. Raman spectroscopic studies revealed the presence of graphene nanosheets. The electro-catalytic activity of Gra/Pd nanocomposites toward methanol and ethanol oxidation in alkaline medium was evaluated by cyclic voltammetric studies. 1:1 Gra/Pd nanocomposite exhibited good electro-catalytic activity and efficient electron transfer. The kinetics of electron transfer was studied using chronoamperometry. Improved electro-catalytic activity of 1:1 Gra/Pd nanocomposite toward alcohol oxidation makes it as a potential anode for the alcohol fuel cells. © 2014 Elsevier Ltd.

  2. Recent palladium membrane reactor development at the tritium systems test assembly

    International Nuclear Information System (INIS)

    Willms, R.S.; Birdsell, S.A.; Wilhelm, R.C.

    1995-01-01

    The palladium membrane reactor (PMR) is proving to be a simple and effective means for recovering hydrogen isotopes from fusion fuel impurities such as methane and water. This device directly combines two techniques which have long been utilized for hydrogen processing, namely catalytic shift reactions and palladium/silver permeators. A proof-of-principle (PMR) has been constructed and tested at the Tritium Systems Test Assembly of Los Alamos National Laboratory. The first tests with this device showed that is was effective for the proposed purpose. Initial work concluded that a nickel catalyst was an appropriate choice for use in a PMR. More detailed testing of the PMR with such a catalyst was performed and reported in other works. It was shown that a nickel catalyst-packed PMR did, indeed, recover hydrogen from water and methane with efficiencies approaching 100% in a single processing pass. These experiments were conducted over an extended period of time and no failure or need for regeneration was encountered. These positive results have prompted further PMR development. Topics addressed include alternate PMR geometries and initial testing of the PMR with tritium. These are the subjects of this paper

  3. Palladium Loaded on Magnetic Nanoparticles as Efficient and Recyclable Catalyst for the Suzuki- Miyaura Reaction

    Directory of Open Access Journals (Sweden)

    H. Khojasteh

    2015-07-01

    Full Text Available Palladium is the best metal catalyst for Suzuki cross coupling reaction for synthesize of unsymmetrical biaryl compounds. But its high cost limits its application in wide scale. Using of nanoscale particles as active catalytic cites is a good approach for reducing needed noble metal. By loading precious nanoparticles on magnetic nanocores as a support, recycling and reusing of catalyst will be possible. Magnetic nanoparticles have super paramagnetic feature and applying an external magnetic field can collect the supported catalyst from reaction milieu simply. In this work new palladium catalyst immobilized on modified magnetic nanoparticles containing NNO donor atoms were synthesized. Then the catalyst characterized by FT-IR spectroscopy, thermogravimetric analysis, X-ray diffraction and ICP. Prepared catalyst showed high activity in the Suzuki– Miyaura cross-coupling reaction of phenylboronic acid with aryl halides. Activity, Pd loading, reusability and Pd leaching of catalyst were studied. Results showed that the supported catalyst has the advantage to be completely recoverable with the simple application of an external magnetic field.

  4. Production of 4He in D2-Loaded Palladium-Carbon Catalyst I

    International Nuclear Information System (INIS)

    Clarke, W. Brian

    2003-01-01

    A series of lead vials of internal volume 1.0 cm 3 were charged with ∼200 mg of carbon catalyst containing 0.5% Pd and 0.4% Pd. The vials were clamped to stainless steel manifolds on a vacuum line, then pumped out and filled with high-purity H 2 or D 2 at a pressure of 152 cm Hg and a temperature of 23 deg. C. Several vials contained ordinary activated carbon instead of palladium-carbon, and some vials contained only H 2 or D 2 . All the vials were stored in a sandbox heated to ∼ 200 deg. C for times up to 45 days before mass spectrometer measurements of 3 He and 4 He were made. No evidence was found for the high concentrations of 4 He claimed in similar experiments by several other researchers. The upper limit for the concentration excess of 4 He in D 2 in vials containing palladium-carbon is 11 ppt (parts per trillion) at the 95% confidence level. This limit for 4 He may be compared with previous claims in similar experiments of 100 ppm (parts per million) by Case and 11 ppm by George and McKubre et al

  5. Palladium nanoparticles in electrochemical sensing of trace terazosin in human serum and pharmaceutical preparations

    Energy Technology Data Exchange (ETDEWEB)

    Sefid-sefidehkhan, Yasaman [Department of Chemistry, University of Mohaghegh Ardabili, Ardabil (Iran, Islamic Republic of); Nekoueian, Khadijeh [Laboratory of Green Chemistry, Faculty of Technology, Lappeenranta University of Technology, Sammonkatu 12, FI-50130 Mikkeli (Finland); Amiri, Mandana, E-mail: mandanaamiri@uma.ac.ir [Department of Chemistry, University of Mohaghegh Ardabili, Ardabil (Iran, Islamic Republic of); Sillanpaa, Mika [Laboratory of Green Chemistry, Faculty of Technology, Lappeenranta University of Technology, Sammonkatu 12, FI-50130 Mikkeli (Finland); Eskandari, Habibollah [Department of Chemistry, University of Mohaghegh Ardabili, Ardabil (Iran, Islamic Republic of)

    2017-06-01

    In this approach, palladium nanoparticle film was simply fabricated on the surface of carbon paste electrode by electrochemical deposition method. The film was characterized using scanning electron microscopy, electrochemical impedance spectroscopy and cyclic voltammetry. The prepared electrode exhibited an excellent electrocatalytic activity toward detection of trace amounts of terazosin, which is an antihypertensive drug. Under the optimum experimental conditions, a linear range of 1.0 × 10{sup −8}–1.0 × 10{sup −3} mol L{sup −1} with a detection limit of 1.9 × 10{sup −9} mol L{sup −1} was obtained for determination of terazosin using differential pulse voltammetry as a sensitive method. The efficiency of palladium nanoparticle film on the surface of carbon paste electrode successfully proved for determination of terazosin in pharmaceutical sample and human serum sample with promising recovery results. The effect of some foreign species has been studied. - Highlights: • PdNPs were simply fabricated by electrochemical deposition. • PdNPs exhibited an excellent electrocatalytic activity toward oxidation of terazosin. • Terazosin has been determined in pharmaceutical sample and human serum sample.

  6. Ratio of dialytic coefficients of hydrogen and tritium in permeation through palladium alloy film

    International Nuclear Information System (INIS)

    Fujita, Haruyuki; Fujita, Kunio; Sakamoto, Hiroshi; Higashi, Kunio; Okada, Sakae.

    1982-01-01

    The dialytic coefficient for hydrogen is especially large in palladium and its alloys. Recently, with the research on fusion reactors, the dialytic coefficient of tritium permeating through solids and its isotopic effect have been the object of interest. The ratio of the dialytic coefficients of tritium and hydrogen has been usually assumed to be 3. The measurement of the dialytic coefficient in solids using pure tritium is practically difficult. Therefore, the authors carried out the experiment to determine the ratio of the dialytic coefficients of pure T 2 and pure H 2 by permeating the mixed gas of T and H through Pd-Au-Ag alloy. The mixed hydrogen gas was filled in a separation cell containing a palladium alloy tube, and the separation factor of tritium and hydrogen was measured by changing pressure, flow rate and temperature. The separation factor depends mainly on the relative dialytic coefficients of tritium and hydrogen, therefore, the ratio of dialytic coefficients can be determined by the simple analysis of the experimental results. This experimental method is suitable to determine the relative value of dialytic coefficients, and the obtained ratio was about 2.1. (Kako, I.)

  7. Ion flotation of rhodium(III) and palladium(II) with anionic surfactants.

    Science.gov (United States)

    He, X C

    1991-03-01

    The ion flotation of rhodium(III) and palladium(II) with some anionic surfactants has been investigated. Two flotation procedures are proposed for the separation of some platinum metals, based on differences in the kinetic properties of the chloro-complexes of rhodium(III), palladium(II) and platinum(IV). The first involves the selective flotation of Rh(H(2)O)(3+)(6) from PdCl(2-)(4) and PtCl(2-)(6) in dilute hydrochloric acid with sodium dodecylbenzenesulfonate (SDBS). After precipitation of the hydroxide and redissolution in dilute acid, the Rh(III) is converted into Rh(H(2)O)(3+)(6), Pd(II) and Pt(IV) remaining as PdCl(2-)(4) and PtCl(2-)(6) respectively, and separation is achieved by floating the Rh(H(2)O)(3+)(6) with SDBS. The second is for separation of Pd(II). Prior to flotation, the solution of PdCl(2-)(4) and PtCl(2-)(6) is heated with ammonium acetate to convert PdCl(2-)(4) into Pd(NH(3))(2+)(4). The chloro-complex of Pt(IV) is unaffected. The complex cation, Pd(NH(3))(2+)(4), is then selectively floated with SDBS. The procedures are fast, simple and do not require expensive reagents and apparatus.

  8. Chromatographic enrichment of isotopes in hydrogen and water samples on palladium

    International Nuclear Information System (INIS)

    Andreev, B.M.; Polevoi, A.S.; Perevezentsev, A.N.

    1987-01-01

    Data on the isotopic enrichment of hydrogen and water samples by chromatography on palladium have been analyzed. Experimental data on the effect of temperature, hydrogen flow, volume of the enriched fraction, and length of the chromatographic column on the degree of separation attainable in the column have been obtained. It has been shown that the maximum separation achievable (regardless of the type of the isotope mixture) at 273 K falls with increase of hydrogen flow and volume of the enriched gas fraction recoverable from the column. A separation degree of ∼ 1040 has been achieved for a mixture of protium and deuterium in a 10-mm wide and 0.6-m long chromatographic column packed with palladium black with a grain size of 0.2-0.5 mm at 273 K and a specific hydrogen flow of 1.22 mole/m 2 x sec. For a protium-tritium mixture a separation degree of ∼ 90 has been reached in a similar column at 273 K and a specific hydrogen flow of 0.4 mole/m 2 x sec

  9. Green synthesis, characterization and antibacterial efficacy of palladium nanoparticles synthesized using Filicium decipiens leaf extract

    Science.gov (United States)

    Sharmila, G.; Farzana Fathima, M.; Haries, S.; Geetha, S.; Manoj Kumar, N.; Muthukumaran, C.

    2017-06-01

    Synthesis of metal nanoparticles through green chemistry route is an emerging eco-friendly approach in the present days. An eco-friendly, biogenic synthesis of palladium nanoparticles (PdNPs) using Filicium decipiens leaf extract was reported in the present study. The synthesized PdNPs were characterized by UV-visible spectroscopy, Transmission electron microscopy (TEM), X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FTIR). The PdNPs formation was confirmed by UV-visible spectrophotometer and spherical shaped PdNPs with size range of 2-22 nm was observed in TEM analysis. Energy dispersive X-ray spectroscopy (EDS) analysis confirmed the presence of palladium in the synthesized nanoparticles. The crystalline nature of PdNPs was confirmed by XRD pattern and compared with the standard. The phytochemicals and proteins were identified by their functional groups in FT-IR spectrum and revealed the amide, amine groups present in F. decipiens may have involved in the bio-reduction reaction for PdNPs synthesis. Prepared PdNPs showed potential antibacterial activity against both Gram-positive and Gram-negative bacteria. F. decipiens leaf extract based PdNPs showed high bactericidal activity against Escherichia coli, Pseudomonas aeruginosa as compared to Staphylococcus aureus and Bacillus subtilis Results showed that phytochemicals rich F. decipiens leaf extract may be utilized as an effective non-toxic reducing agent for PdNPs synthesis and prepared PdNPs may useful in biomedical applications.

  10. Synthesis of palladium-doped silica nanofibers by sol-gel reaction and electrospinning process

    Energy Technology Data Exchange (ETDEWEB)

    San, Thiam Hui; Daud, Wan Ramli Wan; Kadhum, Abdul Amir Hassan; Mohamad, Abu Bakar; Kamarudin, Siti Kartom; Shyuan, Loh Kee; Majlan, Edy Herianto [Fuel Cell Institute, Universiti Kebangsaan Malaysia, 43600 UKM Bangi, Selangor (Malaysia); Fuel Cell Institute, Universiti Kebangsaan Malaysia, 43600 UKM Bangi, Selangor, Malaysia and Department of Chemical and Process Engineering, Universiti Kebangsaan Malaysia, 43600 UKM Bangi, Selangor (Malaysia); Fuel Cell Institute, Universiti Kebangsaan Malaysia, 43600 UKM Bangi, Selangor (Malaysia)

    2012-06-29

    Nanofiber is drawing great attention nowadays with their high surface area per volume and flexibility in surface functionalities that make them favorable as a proton exchange membrane in fuel cell application. In this study, incorporation of palladium nanoparticles in silica nanofibers was prepared by combination of a tetraorthosilane (TEOS) sol-gel reaction with electrospinning process. This method can prevent the nanoparticles from aggregation by direct mixing of palladium nanoparticles in silica sol. The as-produced electrospun fibers were thermally treated to remove poly(vinyl pyrrolidone) (PVP) and condensation of silanol in silica framework. PVP is chosen as fiber shaping agent because of its insulting and capping properties for various metal nanoparticles. Scanning electron microscopy (SEM), energy dispersive spectrometer (EDS) and Fourier transform infrared spectroscopy (FTIR) were used to characterize the silica fibers and Pd nanoparticles on the fibers. Spun fibers with average diameter ranged from 100nm to 400nm were obtained at optimum operating condition and distribution of Pd nanoparticles on silica fibers was investigated.

  11. Palladium(II-Catalyzed othro-C–H-Benzoxylation of 2-Arylpyridines by Oxidative Coupling with Aryl Acylperoxides

    Directory of Open Access Journals (Sweden)

    Wing-Yiu Yu

    2013-04-01

    Full Text Available A palladium(II-catalyzed ortho-benzoxylation of 2-arylpyridines with aryl acylperoxides was developed. With pyridyl as directing group, the benzoxylation reaction exhibits remarkable regioselectivity and excellent functional group tolerance, providing the products in up to 87% yield.

  12. Palladium-catalyzed three-component reaction of N-tosyl hydrazones, isonitriles and amines leading to amidines.

    Science.gov (United States)

    Dai, Qiang; Jiang, Yan; Yu, Jin-Tao; Cheng, Jiang

    2015-12-04

    A palladium-catalyzed three-component reaction between N-tosyl hydrazones, aryl isonitriles and amines was developed, leading to amidines in moderate to good yields. This procedure features the rapid construction of amidine frameworks with high diversity and complexity. Ketenimines serve as intermediates, which encounter nucleophilic attack by amines to produce amidines.

  13. Theoretical Evidence for Low-Ligated Palladium(0): [Pd-L] as the Active Species in Oxidative Addition Reactions

    DEFF Research Database (Denmark)

    Ahlquist, Mårten Sten Gösta; Fristrup, Peter; Tanner, David Ackland

    2006-01-01

    The oxidative addition of PhI to Pd0 has been studied by DFT with a continuum representation of the solvent. It is shown that the preferred number of ligands on palladium is lower than would be expected from “conventional wisdom” and the 18-electron rule. The most favored oxidative addition is ob...

  14. Palladium-catalyzed domino C,N-coupling/carbonylation/Suzuki coupling reaction: an efficient synthesis of 2-aroyl-/heteroaroylindoles.

    Science.gov (United States)

    Arthuis, Martin; Pontikis, Renée; Florent, Jean-Claude

    2009-10-15

    A convenient one-pot synthesis of 2-aroylindoles using a domino palladium-catalyzed C,N-coupling/carbonylation/C,C-coupling sequence is described. The reaction involved easily prepared 2-gem-dibromovinylanilines and boronic acids under carbon monoxide. Optimized reaction conditions allowed the construction of a wide variety of highly functionalized 2-aroyl-/heteroaroylindoles in satisfactory yields.

  15. Driving Unidirectional Molecular Rotary Motors with Visible Light by Intra- And Intermolecular Energy Transfer from Palladium Porphyrin

    NARCIS (Netherlands)

    Cnossen, Arjen; Hou, Lili; Pollard, Michael M.; Wesenhagen, Philana V.; Browne, Wesley R.; Feringa, Ben L.

    2012-01-01

    Driving molecular rotary motors using visible light (530-550 nm) instead of UV light was achieved using palladium tetraphenylporphyrin as a triplet sensitizer. Visible light driven rotation was confirmed by UV/vis absorption, circular dichroism and H-1 NMR spectroscopy and the rotation was confirmed

  16. Suzuki coupling reactions catalyzed by poly(N-ethyl-4-vinylpyridinium bromide stabilized palladium nanoparticles in aqueous solution

    Directory of Open Access Journals (Sweden)

    2008-04-01

    Full Text Available InIn this work, it was investigated to use of poly(N-ethyl-4-vinylpyridinium bromide stabilized palladium nanoparticles in the Suzuki reaction between phenylboronic acid and aryl halides in aqueous solution. The nanoparticles were isolated and re-used several times with low loss of activity.

  17. Electrochemical behavior of ruthenium (III), rhodium (III) and palladium (II) in 1-butyl-3-methylimidazolium chloride ionic liquid

    Energy Technology Data Exchange (ETDEWEB)

    Jayakumar, M.; Venkatesan, K.A. [Fuel Chemistry Division, Indira Gandhi Centre for Atomic Research, Kalpakkam 603102 (India); Srinivasan, T.G. [Fuel Chemistry Division, Indira Gandhi Centre for Atomic Research, Kalpakkam 603102 (India)], E-mail: tgs@igcar.gov.in; Vasudeva Rao, P.R. [Fuel Chemistry Division, Indira Gandhi Centre for Atomic Research, Kalpakkam 603102 (India)

    2009-11-01

    Electrochemical behavior of ruthenium (III), rhodium (III) and palladium (II) in 1-butyl-3-methylimidazolium chloride (bmimCl) and their ternary and binary solutions in bmimCl was studied at various working electrodes at 373 K by cyclic voltammetry and chronoamperometry. Ruthenium (III) chloride forms a stable solution with bmimCl and the cyclic voltammogram of ruthenium (III) in bmimCl recorded at glassy carbon electrode consisted of several redox waves due to the complex nature of ruthenium to exist in several oxidation states. Electrolysis of ruthenium (III) chloride in bmimCl at the cathodic limit of bmimCl (-1.8 V (vs. Pd)) did not result in ruthenium metal deposition. However, it was deposited from bmimPF{sub 6} and bmimNTf{sub 2} room temperature ionic liquids at -0.8 V (vs. Pd). The electrochemical behavior of ruthenium (III) in bmimCl in the presence of palladium (II) and rhodium (III) was studied by cyclic voltammetry. The presence of palladium (II) in bmimCl favors underpotential deposition of ruthenium metal. The nuclear loop at -0.5 V (vs. Pd) was observed in all solutions when palladium (II) co-existed with other two metal ions. Nucleation and growth of the metal on glassy carbon working electrode was investigated by chronoamperometry. The growth and decay of chronocurrents has been found to follow the instantaneous nucleation model with three-dimensional growth of nuclei.

  18. Prefunctionalized Porous Organic Polymers: Effective Supports of Surface Palladium Nanoparticles for the Enhancement of Catalytic Performances in Dehalogenation.

    Science.gov (United States)

    Zhong, Hong; Liu, Caiping; Zhou, Hanghui; Wang, Yangxin; Wang, Ruihu

    2016-08-22

    Three porous organic polymers (POPs) containing H, COOMe, and COO(-) groups at 2,6-bis(1,2,3-triazol-4-yl)pyridyl (BTP) units (i.e., POP-1, POP-2, and POP-3, respectively) were prepared for the immobilization of metal nanoparticles (NPs). The ultrafine palladium NPs are uniformly encapsulated in the interior pores of POP-1, whereas uniform- and dual-distributed palladium NPs are located on the external surface of POP-2 and POP-3, respectively. The presence of carboxylate groups not only endows POP-3 an outstanding dispersibility in H2 O/EtOH, but also enables the palladium NPs at the surface to show the highest catalytic activity, stability, and recyclability in dehalogenation reactions of chlorobenzene at 25 °C. The palladium NPs on the external surface are effectively stabilized by the functionalized POPs containing BTP units and carboxylate groups, which provides a new insight for highly efficient catalytic systems based on surface metal NPs of porous materials. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  19. Reductive dehalogenation of aryl halides over palladium catalysts deposited on SBA-15 type molecular sieve modified with amine donor groups

    Czech Academy of Sciences Publication Activity Database

    Štěpnička, P.; Semler, M.; Demel, J.; Zukal, Arnošt; Čejka, Jiří

    2011-01-01

    Roč. 341, č. 1-2 (2011), s. 97-102 ISSN 1381-1169 R&D Projects: GA ČR GA104/09/0561 Institutional research plan: CEZ:AV0Z40400503 Keywords : heterogeneous catalysts * supported catalysts * palladium Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 2.947, year: 2011

  20. Hydrogen storage studies on palladium-doped carbon materials (AC, CB, CNMs) @ metal-organic framework-5.

    Science.gov (United States)

    Viditha, V; Srilatha, K; Himabindu, V

    2016-05-01

    Metal organic frameworks (MOFs) are a rapidly growing class of porous materials and are considered as best adsorbents for their high surface area and extraordinary porosity. The MOFs are synthesized by using various chemicals like triethylamine, terepthalic acid, zinc acetate dihydrate, chloroform, and dimethylformamide (DMF). Synthesized MOFs are intercalated with palladium/activated carbon, carbon black, and carbon nanomaterials by chemical reduction method for the purpose of enhancing the hydrogen adsorption capacities. We have observed that the palladium doped activated carbon on MOF-5 showed high hydrogen storage capacity. This may be due to the affinity of the palladium toward hydrogen molecule. The samples are characterized by X-ray diffraction, scanning electron microscopy (SEM), and Brunauer-Emmett-Teller (BET) surface area analysis. We have observed a clear decrease in the BET surface area and pore volume. The obtained results show a better performance for the synthesized sample. To our best knowledge, no one has reported the work on palladium-doped carbon materials (activated carbon, carbon black, carbon nanomaterials) impregnated to the metal-organic framework-5. We have attempted to synthesize carbon nanomaterials using indigenously fabricated chemical vapor deposition (CVD) unit as a support. We have observed an increase in the hydrogen storage capacities.