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Sample records for acetylacetone

  1. Cyclopentadienyluranium(IV) acetylacetonates

    International Nuclear Information System (INIS)

    Bagnall, K.W.; Edwards, J.; Rickard, C.E.F.; Tempest, A.C.

    1979-01-01

    Cyclopentadienyluranium(IV) acetylacetonate complexes, (eta 5 C 5 H 5 )UClsub(3-x)(acac)sub(x), where x = 1 or 2, and the corresponding bis triphenylphosphine oxide (tppo) complexes have been prepared. The bis cyclopentadienyl complexes, (eta 5 C 5 H 5 ) 2 U(acac) 2 and (eta 5 C 5 H 5 ) 2 UCl(acac)(tppo) 2 have also been prepared and are stable with respect to disproportionation, whereas (eta 5 C 5 H 5 ) 2 UCl(acac) is not. The IR and UV/visible spectra of the complexes are reported, together with some additional information on the UCl 2 (acac) 2 thf and -tppo systems. (author)

  2. Enhancement of thermal stability of silver(I) acetylacetonate by platinum(II) acetylacetonate

    Czech Academy of Sciences Publication Activity Database

    Křenek, T.; Kovářík, T.; Pola, M.; Jakubec, Ivo; Bezdička, Petr; Bastl, Zdeněk; Pokorná, Dana; Urbanová, Markéta; Galíková, Anna; Pola, Josef

    2013-01-01

    Roč. 554, FEB (2013), s. 1-7 ISSN 0040-6031 Institutional support: RVO:61388980 ; RVO:61388955 ; RVO:67985858 Keywords : thermal gravimetric analysis * differential scanning calorimetry * silver(I) acetylacetonate * platinum(II) acetylacetonate * enhancement of thermal stability Subject RIV: CA - Inorganic Chemistry; CF - Physical ; Theoretical Chemistry (UFCH-W) Impact factor: 2.105, year: 2013

  3. Adducts of rare earth tris-acetylacetonates with dimethyl sulfoxide

    International Nuclear Information System (INIS)

    Dzyubenko, N.G.; Kalenichenko, Yu.V.; Martynenko, L.I.

    1988-01-01

    Adducts of rare earth and yttrium (r.e.e., M) acetylacetonates with dimethyl sulfoxide (DMSO), MA 3 xnDMSO are synthesized. The acetylacetonates of light r.e.e. (M=La-Tb) are shown by different physico-chemical methods to form diadducts of the MA 3 x2DMSOxH 2 O composition, where A - -acetylacetonate-ion, and the acetyl-acetonates of heavy r.e.e. (M=Dy-Lu, Y)-monoadducts MA 3 xDMSO. The estimation of adduct thermal stability is carried out using the values of seeming activation energy of their thermal degradation. Monoadducts are shown to give volatile forms of rare earth acetylacetonates during heating in vacuum, and diadducts do not form volatile forms of acetylacetonates

  4. New Mechanism for the Reduction of Vanadyl Acetylacetonate to Vanadium Acetylacetonate for Room Temperature Flow Batteries

    Energy Technology Data Exchange (ETDEWEB)

    Shamie, Jack S. [Department of Mechanical, Materials and Aerospace Engineering, Illinois Institute of Technology, Chicago Illinois 60616 USA; Liu, Caihong [Department of Mechanical, Materials and Aerospace Engineering, Illinois Institute of Technology, Chicago Illinois 60616 USA; Shaw, Leon L. [Department of Mechanical, Materials and Aerospace Engineering, Illinois Institute of Technology, Chicago Illinois 60616 USA; Sprenkle, Vincent L. [Energy Storage and Conversion Energy Materials, Pacific Northwest National Laboratory, Richland WA 99352 USA

    2016-12-29

    In this study, a new mechanism for the reduction of vanadyl acetylacetonate, VO(acac)2, to vanadium acetylacetonate, V(acac)3, is introduced. V(acac)3 has been studied for use in redox flow batteries (RFBs) for some time; however, contamination by moisture leads to the formation of VO(acac)2. In previous work, once this transformation occurs, it is no longer reversible because there is a requirement for extreme low potentials for the reduction to occur. Here, we propose that, in the presence of excess acetylacetone (Hacac) and free protons (H+), the reduction can take place between 2.25 and 1.5 V versus Na/Na+ via a one-electron-transfer reduction. This reduction can take place in situ during discharge in a novel hybrid Na-based flow battery (HNFB) with a molten Na–Cs alloy as the anode. The in situ recovery of V(acac)3 during discharge is shown to allow the Coulombic efficiency of the HNFB to be ≈100 % with little or no capacity decay over cycles. In addition, utilizing two-electron-transfer redox reactions (i.e., V3+/V4+ and V2+/V3+ redox couples) per V ion to increase the energy density of RFBs becomes possible owing to the in situ recovery of V(acac)3 during discharge. The concept of in situ recovery of material can lead to more advances in maintaining the cycle life of RFBs in the future.

  5. Pressure of saturated vapor of yttrium and zirconium acetylacetonates

    Energy Technology Data Exchange (ETDEWEB)

    Trembovetskij, G.V.; Berdonosov, S.S.; Murav' eva, I.A.; Martynenko, L.I. (Moskovskij Gosudarstvennyj Univ. (USSR))

    1984-08-01

    The static method and the flow method using /sup 91/Y and /sup 95/Zr radioactive indicators have been applied to determine pressure of saturated vapour of yttrium and zirconium acetylacetonates. Values of thermodynamic functions ..delta..Hsub(subl)=(98+-16)kJ/mol and ..delta..Ssub(subl.)=(155+-30)J/mol x K are calculated for sublimation of yttrium acetylacetonate. For sublimation of zirconium acetylacetonates ..delta..Hsub(subl) equals (116+-38) kJ/mol and ..delta..Ssub(subl) is equal to (198+-65) J/molxK.

  6. COORDINATION COMPOUNDS OF 3D-METALS ACETYLACETONATES WITH THIOSEMICARBAZIDE

    Directory of Open Access Journals (Sweden)

    T. V. Koksharova

    2015-03-01

    Full Text Available Coordination Compounds of 3d-Metals acetylacetonates with Thiosemicarbazide were synthesized. Their physical and chemical properties and structure were studied by conductometry, IR spectroscopy, electronic spectroscopy, magnetochemistry and thermo-gravimetricstudies. The complexes compositions correspond to the formulas Co(L2(Acac and M(L(Acac, where M = Cu, Ni, Zn, HL is thiosemicarbazide, HAcac is acetylacetone. All of them are nonelectrolytes. Thiosemicarbazide is deprotonated and coordinated through the nitrogen and sulphur atoms with the formation of four-membered ring in all cases. Acetylacetonate co-ordination mode does not change at acetylacetonates with Thiosemicarbazide interaction. Copper(II and nickel(II complexes have square-planar structure, and cobalt(III complex is octahedral.

  7. Clinical applications of indium-111-acetylacetone-labelled blood cells

    International Nuclear Information System (INIS)

    Georgi, P.; Sinn, H.; Wellman, H.; Clorius, J.H.; Becker, W.

    1981-01-01

    A method permitting red-cell labelling with 111 In-acetylacetone was reported in 1974 for evaluating intestinal blood loss, the liver-spleen ratio and the red-cell volume. White blood cells can be tagged similarly. In white-cell labelling, simultaneous red-cell or platelet tagging is avoided. Several procedures (dextran separation and gradient centrifugations) have been combined, to develop a highly selective cell separation. In osteomyelitis it may not be as advantageous to use 67 Ga-citrate, as in inflammatory soft tissue processes. The detection of inflammatory processes with labelled leukocytes could be of great importance for the scintigraphic diagnosis of osteomyelitidies. A group of 97 patients with suspected osteomyelitis have been examined using 111 In-acetylacetone-labelled leukocytes ( 111 In-AAL) immediately following positive routine skeletal scintigraphy. Images obtained 24 h post injection usually were the most satisfactory. In the followup group of 70 patients 21 true positives, 43 true negatives, 21 false negatives and 3 false positives were observed. These findings result in a specificity of 92%, sensitivity of 50% and accuracy of 70% with 111 In-AAL for osteomyelitis. Preliminary investigations using 111 In-acetylacetone-labelled thrombocytes ( 111 In-AAT) were carried out to detect rejection of transplanted kidneys. The platelets were separated by means of additional special density gradient centrifugations but no dextran from 15-20 ml of autologous whole blood. Scans have been obtained 15 min, 2.5 h and 24 h post injection in an initial group of 10 patients. In acute rejection, a high transplant uptake has been detected, whereas patients without acute rejection showed no or only a minimum activity accumulation. Patients with chronic rejection have intermediate uptakes

  8. Saturated vapor pressure of lutetium tris-acetylacetonate

    Energy Technology Data Exchange (ETDEWEB)

    Trembovetskij, G.V.; Berdonosov, S.S.; Murav' eva, I.A.; Martynenko, L.I. (Moskovskij Gosudarstvennyj Univ. (USSR))

    1983-12-01

    By the statical method using /sup 177/Lu radioactive isotope the saturated vapor pressure of anhydrous lutetium acetylacetonate at 130 to 160 deg is determined. The calculations are carried out assuming the vapor to be monomolecular. The equation of lgP versus 1/T takes the form: lg Psub((mmHg))=(8.7+-1.6)-(4110+-690)/T. The thermodynamical characteristics of LuA/sub 3/ sublimation are calculated to be ..delta..Hsub(subl.)=79+-13 kJ/mol; ..delta..Ssub(subl.)=111+-20 J/kxmol.

  9. Anodic dissolution of samarium in acetonitrile solution of acetylacetone

    International Nuclear Information System (INIS)

    Kostyuk, N.N.; Dik, T.A.; Trebnikov, A.G.; Shirokij, V.L.

    2003-01-01

    Electrochemical dissolution of metal samarium in acetonitrile medium in the presence of 0.1 M tetraethylammoniumbromide and 0.9 M acetylacetone (HAA) in argon atmosphere under a voltage of 3 V was considered for studying feasibility of electrochemical synthesis of samarium β-diketonates. Using IR and mass spectrometry, thermal and elementary analyses it was ascertained that, depending on cathode and anode areas ratio, anodic dissolution of samarium can give rise to formation of complexes of bi- and trivalent samarium featuring the composition Sm 4 (AA) 8 · 3HAA, Sm(AA) 3 · HAA and Sm(AA) 3 · 4HAA [ru

  10. Electronic structure of binuclear acetylacetonates of boron difluoride

    Science.gov (United States)

    Tikhonov, Sergey A.; Svistunova, Irina V.; Samoilov, Ilya S.; Osmushko, Ivan S.; Borisenko, Aleksandr V.; Vovna, Vitaliy I.

    2018-05-01

    The electronic structure of boron difluoride acetylacetonate and its three derivatives was studied using photoelectron and absorption spectroscopy, as well as the density functional theory. In a series of binuclear acetylacetonate complexes containing bridge-moieties of sulfur and selenium atoms, it was found an appreciable mixing of the π3-orbital of the chelate cycle with atomic orbitals S 3p and Se 4p resulting in destabilization of the HOMO levels by 0.4-0.6 eV, in comparison with the monomer. The positively charged fragment C(CH3)-CX-C(CH3) causes the field effect, which leads to stabilization of the LUMO levels by 0.3-0.4 eV and C 1s-levels by 0.5-1.2 eV. An analysis of the research results on the electronic structure made it possible to determine the effect of substituents in the γ position on the absorption spectra, which is mainly determined by the electron density transfer from the chalcogen atoms to the chelate cycles. It is shown that the calculated energy intervals between electron levels correlate well with the structure of the photoelectron spectra of valence and core electrons.

  11. Zone-refining of beryllium(II) acetylacetonate

    International Nuclear Information System (INIS)

    Yoshida, Isao; Kobayashi, Hiroshi; Ueno, Keihei

    1975-01-01

    Zone melting was applied to bis (acetylacetonato) beryllium(II), Be(AA) 2 , to remove trace metal constiutents. The effective distribution coefficient, k, of a minor component measured in a binary mixture with the majority of Be(AA) 2 , fell in the range of 0.4 to 0.8, while the value obtained in a multiple component mixture fell in the range of 0.8 to 0.9 except Zn(II)- and Ni(II) chelates. Cr(AA) 3 was concentrated upward in the direction of the zone travelling, and similar results were obtained with Cu(II)-, Co(III)- Fe(III)- and Al(III) acetylacetonates, while Zn(II)-, Ni(II)- and Mn(III) chelates were fractionated in the both ends of the column. On the other hand, when the zone was moved downward, the minor components were concentrated in the lower end of a column. Efficiency in zone refining was compared to each other between the upward- and downward zone travelling modes on the crude beryllium acetylacetonates obtained from a commercial reagent of beryllium nitrate, and the latter mode was found more effective in the concentration of trace components. Discussion was given on possible mechanisms resulting in the difference in the refining efficiency. (author)

  12. An application of the coincidence Doppler spectroscopy for substances of chemical interest: phthalocyanine and acetylacetonate complexes

    International Nuclear Information System (INIS)

    Ito, Y.; Suzuki, T.

    2000-01-01

    Coincidence Doppler spectroscopy, which is particularly powerful when one is concerned with high momentum components of positron annihilation gamma-rays, has been applied to two different kinds of organo-metallic ligands: metal phthalocyanines and metal acetylacetonates. The energy (momentum) profiles of the annihilation gamma-rays were the same for metal phthalocyanines indicating that positron and/or positronium are not interacting with the metal ions. However, the profiles for the metal acetylacetonates evidently showed a dependence on the kind of metal ions. Discussion is made on the features of positron interaction which are different for phthalocyanines and acetylacetonates.

  13. On the role of the ground state Tb(3)/acetylacetone complex in sensitized emission of Tb(3) in ethanol solution

    International Nuclear Information System (INIS)

    Lis, S.; Elbanowski, M.; Marciniak, B.

    1989-01-01

    The Tb(3)-acetylacetone system in ethanol solution has been studied by spectroscopic methods. The formation of a Tb(3)/acetylacetone (1:1) complex in the ground state has been proved and its stability constant determined, K = (0,97 ± 0,06).10 4 dm 3 mol -1 . The role of this complex in the spectrofluorimetric determination of Ln(3) ions in the presence of acetylacetone has been discussed. (Authors)

  14. Properties and adduct structure of rare earth tris-acetylacetonates with o-phenanthroline

    International Nuclear Information System (INIS)

    Dzyubenko, N.G.; Martynenko, L.I.

    1986-01-01

    Adducts of acetylacetonates of rare earths (M, REE) with O-phenanthroline (Phen) of the composition MA 3 xPhen (M=La-Lu, Y) are synthesized by different methods and studied. Phen coordination by M 3+ ion is proved using infrared spectroscopy, individual character of obtained preparations and their isostructure in a series of REE derivatives is confirmed by X-ray radiography. MA 3 xPhen thermal stability is much higher than that of corresponding hydrates of rare-earth acetylacetonates MA 3 xnH 2 O. In high vacuum under conditions of mass-spectrometric measurements MA 3 xPhen adducts degradate forming volatile rare earth acetylacetonates of MA 3 composition. When heating in vacuum (∼ 10 2 mm Hg) MA 3 xPhen are qualitatively sublimated not changing the composition. MA 3 xPhen volatility determined for the whole REE series may be of interest in practical problem solving

  15. Zinc acetylacetonate hydrate adducted with nitrogen donor ligands: Synthesis, spectroscopic characterization, and thermal analysis

    Science.gov (United States)

    Brahma, Sanjaya; Shivashankar, S. A.

    2015-12-01

    We report synthesis, spectroscopic characterization, and thermal analysis of zinc acetylacetonate complex adducted by nitrogen donor ligands, such as pyridine, bipyridine, and phenanthroline. The pyridine adducted complex crystallizes to monoclinic crystal structure, whereas other two adducted complexes have orthorhombic structure. Addition of nitrogen donor ligands enhances the thermal property of these complexes as that with parent metal-organic complex. Zinc acetylacetonate adducted with pyridine shows much higher volatility (106 °C), decomposition temperature (202 °C) as that with zinc acetylacetonate (136 °C, 220 °C), and other adducted complexes. All the adducted complexes are thermally stable, highly volatile and are considered to be suitable precursors for metal organic chemical vapor deposition. The formation of these complexes is confirmed by powder X-ray diffraction, Fourier transform infrared spectroscopy, mass spectroscopy, and elemental analysis. The complexes are widely used as starting precursor materials for the synthesis of ZnO nanostructures by microwave irradiation assisted coating process.

  16. Synthesis and physicochemical analysis of Sm (II, III) acetylacetone chelate complexes

    International Nuclear Information System (INIS)

    Kostyuk, N.N.; Dik, T.A.; Trebnikov, A.G.

    2004-01-01

    Sm (II, III) acetylacetone chelate complexes were synthesized by electrochemical method. It was shown that anode dissolution of the metal samarium over acetylacetone leads to formation of the Sm (II, III) chelate complexes: xSm(acac)2 · ySm(acac)3 · zH(acac). Factors x, y and z depend on quantity of the electricity, which flew through the electrolysis cell. The compositions of the obtained substances were confirmed by the physicochemical analysis (ultimate analysis, IR-, mass spectroscopy and thermal analysis (thermogravimetric, isothermal warming-up and differential scanning colorimetry). (Authors)

  17. Synthesis and investigation of rare earth tris-acetylacetonates addUcts with acetylaceoneimine

    International Nuclear Information System (INIS)

    Trembovetskij, G.V.; Smirnov, E.V.; Murav'eva, I.A.; Martynenko, L.I.

    1983-01-01

    Adducts of tris-acetylacetonates of pare earths With acetylacetonimine of the composition MA 3 x2L (M=La, Pr, Nd, Eu, Gd, Tb) and MA 3 XL (M=Dy, Ho, Er, Tm, Yb, LU) have been synthesized. The compounds prepared are studied using the methods of elemental analysis, IR spectroscopy, PMR spectroscopy, X-ray phase analysis. Volatile tris-acetylacetonates of the yttrium subgroUp rare earths have been prepared by thermal decomposition of MA 3 xL in vacuum

  18. Investigations of the conditions of obtaining and of purifying zirconium acetylacetonate

    International Nuclear Information System (INIS)

    Dobrowolski, J.; Kozera, F.; Hubicki, Z.

    1980-01-01

    The method of obtaining zirconium acetylacetonate with a yield of 90% has been elaborated and there has been presented the way of removing the impurities of Fe, Ti, Cl, N and Hf. The conditions of transforming the hydrated compound into an anhydrous one without using large quantities of anhydrous solvents have been determined. (author)

  19. Preparation of ferric acetylacetonate, bonzonate and caprate labelled with Fe-55 and tests of application to liquid scintillation measurements

    International Nuclear Information System (INIS)

    Los Arcos, J.M.; Rodriguez Barquero, L.; Grau Malonda, A.

    1990-01-01

    The methods of preparation of ferric acetylacetonate, benzoate and caprate labelled with 55 Fe are described. The quenching effect, the spectral baehaviour and the count rate stability are studied by liquid scintillation measurements in toluene, INSTAGEL and HISAFE II, for two different values of the sample concentration. The ferric acetylaceton-ate is stable for all the three scintillators but shows a strong quench, while the ferric benzoate and caprate are stable only for INSTAGEL and HISAFE II showing no significant quench at the concentrat-ions of interest in habitual measurements. (Author)

  20. Mass-spectrometric investigation of rare earth acetylacetonates dipivaloylmethanates and their adducts

    International Nuclear Information System (INIS)

    Gavrishzhuk, E.M.; Dzyubenko, N.G.; Martynenko, L.I.

    1985-01-01

    Peculiarities of fragmentation of molecular ions of rare earth acetylacetonates and dipivaloylmethanates under mass-spectrometric investigation of these compounds as well as their adducts with o-phenanthroline, α,α'-dipyridyl, triphenylphosphine oxide are considered in the given review. Similar data for identical derivants of some transitions metals are presented. Data on potentials of appearance and dissociation energy of basic ions in mass-spectra of the studied β-diketonates are analyzed

  1. 1,3-Dioxolane, tetrahydrofuran, acetylacetone and dimethyl sulfoxide as solvents for non-aqueous vanadium acetylacetonate redox-flow-batteries

    International Nuclear Information System (INIS)

    Herr, T.; Noack, J.; Fischer, P.; Tübke, J.

    2013-01-01

    Highlights: • Four solvents were employed in a non-aqueous redox flow battery system. • Coulombic efficiencies of 85.9–98.5% and energy efficiencies of 26.6–43.6% were achieved. • Discharge power density was enhanced up to 0.080 mW cm −2 . • Solubility of V(acac) 3 was increased to 0.8 M compared to the acetonitrile system. -- Abstract: A non-aqueous vanadium acetylacetonate redox flow battery with different organic solvents and tetrabutylammonium hexafluorophosphate has been investigated. Cyclic voltammograms show three redox couples in 1,3-dioxolane, tetrahydrofuran, acetylacetone and two redox couples in dimethyl sulfoxide. Cell potentials between 2.21 and 2.61 V are measured, depending on the solvent used. Impedance Spectroscopy has been used to determine rate limiting step in the non-aqueous redox flow battery. Experiments in a charge–discharge test cell yielded coulombic and energy efficiencies of 85.9–98.5% and 26.6–43.6%, respectively

  2. Investigation of zirconium oxychloride interaction with acetylacetone by the method of pH-metric titration

    International Nuclear Information System (INIS)

    Zharkova, N.Ya.; Martynenko, L.I.; Dzyubenko, N.G.

    1989-01-01

    Interaction of zirconium oxychloride with acetylacetone (NA) was studied by the method of pH-metric titration using KOH and NH 4 OH as neutralizing agents. It is shown that processes of hydrolysis and complexation complete in the system. It was established that decrease of hydrolysis of Zr-containing complex forms and ZrA 4 · 10H 2 O isolation takes place in relatively concentrated solutions of ZrOCl 2 and NA mixture, taken with 1:4 molar ratio when using NH 4 OH as neutralizing agent

  3. Mass spectrometry study of sublimation of rare earth acetylacetonate adducts with hexamethylphosphorustriamide

    International Nuclear Information System (INIS)

    Kuz'mina, N.P.; Semyannikov, P.P.; Martynenko, L.I.; Ch'eu Tkhi Nguet; AN SSSR, Novosibirsk

    1991-01-01

    Process of vacuum sublimation of MA 3 ·Q adducts (M=Nd,Ho,Er; A - -acetylacetonate-ion; Q-hexamethylphosphorustriamide) was studied by mass-spectrometry method. Composinion of gaseous phase, formed in 20-140 deg C range at 10 -5 mm Hg, was determined. Scheme of MA 3 ·Q sublimation, including Q splitting and transition of MA 3 ·Q adducts and MA 3 and Q products of their thermodestruction to gaseous phase, was suggested. ΔH values of MA 3 ·Q thermodestruction and MA 3 sublimation were calculated

  4. Extraction of acetylacetonates of some metals from melts of trihydrate lithium nitrate

    International Nuclear Information System (INIS)

    Sevast'yanov, A.I.; Rudenko, N.P.; Kuznetsov, A.F.; Lanskaya, N.G.

    1987-01-01

    Extraction of beryllium cobalt and lithium from melts of trihydrate lithium nitrate at 37 deg C using 0.5 mol solutions of acetylacetone in chloroform, tetrachlorethylene and carbon tetrachloride is studied. Beryllium is quantitatively extracted at pH 3.8-5.5, the phase volume ratio being V org :V melt from 1:1 to 1:10. The degree of the beryllium complex unitary extraction from melt depends on the nature of organic solvent and is 100% for CCl 4 , CHCl 3 and 85% for C 2 Cl 4 . Solvents on Be extraction ability are placed in the following series CCl 4 > CHCl 3 >C 2 Cl 4

  5. Influence of acetylacetonates of 3d-metals on the γ radiolysis of benzene

    International Nuclear Information System (INIS)

    Zatonskii, S.V.; Makhlyarchuk, V.V.; Morozova, L.N.

    1986-01-01

    This paper investigates the formation of diphenyl and phenylcyclohexadiene in the radiolysis of benzene in the presence of the following acetylacetonates: Cr (AA) 3 , Mn (AA) 2 .2H 2 O, Mn (AA) 3 , Fe (AA) 2 .2H 2 O, Fe (AA) 3 , Co (AA) 3 . It was found that bisacetylacetonatocobalt (II) lowers the radiation chemical yields of the dimers to a substantial degree. It was suggested that the effect is caused by a reaction of addition of free radicals, arising under the action of radiation, to the central ion of the chelate

  6. Cobalt(2) and nickel(2) tris-acetylacetonates with alkali metal cations in outer sphere

    International Nuclear Information System (INIS)

    Steblyanko, A.Yu.; Grigor'ev, A.N.; Martynenko, L.I.

    1996-01-01

    Anhydrous tris-acetylacetonates of Co(2) and Ni(2) with alkali metal cations in outer sphere were synthesized and investigated by different physicochemical methods. Chemical analysis and IR-spectroscopy show, that complex composition corresponds to the formula Eh[MA 3 ] (where Eh + - Li + , Na + , K + , Rb + , Cs + ; M - Co(2), Ni(2); A - - acetyacetonate-ion). Eh[MA 3 ] heating in vacuum leads to transition of volatile Co(2) and Ni(2) acetylacetonates to gaseous phase. The data of photoelectron spectroscopy and vacuum sublimation show, that Li[MA 3 ] is transformed to gaseous phase congruently and only partially dissociates to EhA and MA 2 . Li[MA 3 ] and Cs[MA 3 ] are characterized by the lowest thermal stability at atmospheric pressure. Low stability of Li[MA 3 ] is related with detachment of one of A - radical from [MA 3 ] complex anion by Li + cation under conditions, when LiA and Li[MA 3 ] are volatile. 11 refs.; 2 figs.; 3 tabs

  7. A New Homogeneous Catalyst for the Dehydrogenation of Dimethylamine Borane Starting with Ruthenium(III Acetylacetonate

    Directory of Open Access Journals (Sweden)

    Ebru Ünel Barın

    2015-06-01

    Full Text Available The catalytic activity of ruthenium(III acetylacetonate was investigated for the first time in the dehydrogenation of dimethylamine borane. During catalytic reaction, a new ruthenium(II species is formed in situ from the reduction of ruthenium(III and characterized using UV-Visible, Fourier transform infrared (FTIR, 1H NMR, and mass spectroscopy. The most likely structure suggested for the ruthenium(II species is mer-[Ru(N2Me43(acacH]. Mercury poisoning experiment indicates that the catalytic dehydrogenation of dimethylamine-borane is homogeneous catalysis. The kinetics of the catalytic dehydrogenation of dimethylamine borane starting with Ru(acac3 were studied depending on the catalyst concentration, substrate concentration and temperature. The hydrogen generation was found to be first-order with respect to catalyst concentration and zero-order regarding the substrate concentration. Evaluation of the kinetic data provides the activation parameters for the dehydrogenation reaction: the activation energy Ea = 85 ± 2 kJ·mol−1, the enthalpy of activation ∆H# = 82 ± 2 kJ·mol−1 and the entropy of activation; ∆S# = −85 ± 5 J·mol−1·K−1. The ruthenium(II catalyst formed from the reduction of ruthenium(III acetylacetonate provides 1700 turnovers over 100 hours in hydrogen generation from the dehydrogenation of dimethylamine borane before deactivation at 60 °C.

  8. Comparison of indium-111-oxine and indium-111-acetylacetone labelled leucocytes in the diagnosis of inflammatory disease

    Energy Technology Data Exchange (ETDEWEB)

    Peters, A.M.; Karimjee, S.; Saverymuttu, S.H.; Lavender, J.P. (Hammersmith Hospital, London (UK))

    1982-11-01

    /sup 111/In leucocyte scanning in a series of 132 patients has shown this technique to be a reliable and accurate means of diagnosing sepsis. Labelling with /sup 111/In oxine and with /sup 111/In acetylacetone gave similar values of sensitivity and specificity, and higher than those of ultrasound.

  9. Volatile mixed-ligand lanthanum (3) complex with acetylacetone and 1,10-phenanthroline

    International Nuclear Information System (INIS)

    Kuz'mina, N.P.; Chuparov, N.V.; Pisarevskij, A.P.; Martynenko, L.I.

    1997-01-01

    La(Acac) 3 Phen complex is synthetized, its X-tray structure analysis is carried out. Crystals are monoclinic ones, sp.gr. P2 1 /n, a=17.11 (12), b=18.16 (3), c=17.86 (2) A, β=91.32 (2) deg, V=5548 (13) A 3 , Z=8. Structure contains two crystallographically non-equivalent types of molecules differing in interatomic distances and valent angles, as well as, in angles between ligand planes. Behaviour of La(Acac) 3 Phen at heating in vacuum (0.1-0.01 mm Hg) is studied. It is shown that under those conditions processes of Phen splitting, of sublimation and polymerization of La(Acac) 3 lanthanum acetylacetonate formed following Phen splitting and that under 220 deg C during 30 min quantitative transition of La(Acac) 3 Phen into gas phase is reached. 10 refs., 2 figs., 3 tabs

  10. Films deposited from reactive sputtering of aluminum acetylacetonate under low energy ion bombardment

    Energy Technology Data Exchange (ETDEWEB)

    Battaglin, Felipe Augusto Darriba; Prado, Eduardo Silva; Cruz, Nilson Cristino da; Rangel, Elidiane Cipriano, E-mail: elidiane@sorocaba.unesp.br [Universidade Estadual Paulista Julio de Mesquita Filho (UNESP), Sorocaba, SP (Brazil). Lab. de Plasmas Tecnologicos; Caseli, Luciano [Universidade Federal de Sao Paulo (UNIFESP), Diadema, SP (Brazil). Instituto de Ciencias Ambientais, Quimicas e Farmaceuticas; Silva, Tiago Fiorini da; Tabacniks, Manfredo Harri [Universidade de Sao Paulo (USP), SP (Brazil). Instituto de Fisica

    2017-07-15

    Films were deposited from aluminum acetylacetonate (Al(acac)3 ) using a methodology involving reactive sputtering and low energy ion bombardment. The plasma was generated by the application of radiofrequency power to the powder containing electrode and simultaneously, negative pulses were supplied to the electrode where the substrates were attached. It was investigated the effect of the duty cycle of the pulses (Δ) on the properties of the coatings. Association of ion bombardment to the deposition process increased film thickness, structure reticulation and organic content. Ions from the deposition environment were implanted at the film-air interface or underneath it. Morphology and topography were altered depending on Δ. Considering the enhancement of Δ, it affected the flux of ions reaching the depositing interface and then the deposition rate, H content, crosslinking degree and surface microstructure. Alumina groups were detected in the infrared spectra, whereas the precipitation of amorphous alumina was confirmed by X-ray diffraction. (author)

  11. The molecular interactions in the extraction system: acetylacetone-InCl3-water

    International Nuclear Information System (INIS)

    Kulawik, I.; Bogon, E.

    1978-01-01

    The extraction process in the chelate system: acetylacetone-InCl 3 -Water and possibility of the investigations of some physico-chemical properties of this system were discussed. The preliminary measurements for determination the adsorption kinetics and the equilibrium in the system were presented. Also extraction coefficient of indium salt was determined. The results of the principal measurements of the surface and interfacial tension as a function of concentration and temperature in the phases were presented. The measurements were done in different conditions when the both phases were in contact during the same time but in the various temperature. The experimental data served also for the calculation of the work of cohesion and adhesion in the system. The entropy and surface energy of the particular phases of the system were also determined. (author)

  12. Physico-chemical characterization of mixed-ligand complexes of Mn(III based on the acetylacetonate and maleic acid and its hydroxylamine derivative

    Directory of Open Access Journals (Sweden)

    Cakić Suzana M.

    2005-01-01

    Full Text Available Two new Mn(III mixed-ligand complexes with two acetylacetonate (acac ligands and one maleate ligand and its hydroxylamine derivative of the general formula [Mn(C5H7O22L] were prepared. Their structure was established by using elemental analysis, FTIR and UV/VIS spectroscopic methods, as well as magnetic measurement. Replacement of the acetylacetonate ligand by the corresponding acid ligand has been confirmed in Mn(III acetylacetonate. Based on the obtained experimental data and literature indications, structural formulae to these compounds were assigned.

  13. Dinuclear Cu(II) complexes of isomeric bis-(3-acetylacetonate)benzene ligands: synthesis, structure, and magnetic properties.

    Science.gov (United States)

    Rancan, Marzio; Dolmella, Alessandro; Seraglia, Roberta; Orlandi, Simonetta; Quici, Silvio; Sorace, Lorenzo; Gatteschi, Dante; Armelao, Lidia

    2012-05-07

    Highly versatile coordinating ligands are designed and synthesized with two β-diketonate groups linked at the carbon 3 through a phenyl ring. The rigid aromatic spacer is introduced in the molecules to orient the two acetylacetone units along different angles and coordination vectors. The resulting para, meta, and ortho bis-(3-acetylacetonate)benzene ligands show efficient chelating properties toward Cu(II) ions. In the presence of 2,2'-bipyridine, they promptly react and yield three dimers, 1, 2, and 3, with the bis-acetylacetonate unit in bridging position between two metal centers. X-ray single crystal diffraction shows that the compounds form supramolecular chains in the solid state because of intermolecular interactions. Each of the dinuclear complexes shows a magnetic behavior which is determined by the combination of structural parameters and spin polarization effects. Notably, the para derivative (1) displays a moderate antiferromagnetic coupling (J = -3.3 cm(-1)) along a remarkably long Cu···Cu distance (12.30 Å).

  14. Vanadium oxide thin films and fibers obtained by acetylacetonate sol–gel method

    Energy Technology Data Exchange (ETDEWEB)

    Berezina, O.; Kirienko, D. [Department of Physical Engineering, Petrozavodsk State University, 185910 Petrozavodsk (Russian Federation); Pergament, A., E-mail: aperg@psu.karelia.ru [Department of Physical Engineering, Petrozavodsk State University, 185910 Petrozavodsk (Russian Federation); Stefanovich, G.; Velichko, A. [Department of Physical Engineering, Petrozavodsk State University, 185910 Petrozavodsk (Russian Federation); Zlomanov, V. [Department of Chemistry, Moscow State University, 119991 Moscow (Russian Federation)

    2015-01-01

    Vanadium oxide films and fibers have been fabricated by the acetylacetonate sol–gel method followed by annealing in wet nitrogen. The samples are characterized by X-ray diffraction and electrical conductivity measurements. The effects of a sol aging, the precursor decomposition and the gas atmosphere composition on the annealing process, structure and properties of the films are discussed. The two-stage temperature regime of annealing of amorphous films in wet nitrogen for formation of the well crystallized VO{sub 2} phase is chosen: 1) 25–550 °C and 2) 550–600 °C. The obtained films demonstrate the metal–insulator transition and electrical switching. Also, the effect of the polyvinylpyrrolidone additive concentration and electrospinning parameters on qualitative (absence of defects and gel drops) and quantitative (length and diameter) characteristics of vanadium oxide fibers is studied. - Highlights: • Vanadium oxide thin films and fibers are synthesized by sol–gel method. • The effect of annealing, atmosphere, time and electrospinning parameters is studied. • Produced VO{sub 2} structures exhibit metal–insulator transition and electrical switching.

  15. Surface defect modification of ZnO quantum dots based on rare earth acetylacetonate and their impacts on optical performance

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Lixi, E-mail: wanglixi_njut@163.com [School of Materials Science and Engineering, Nanjing Tech University, Nanjing, 210009, Jiangsu (China); Jiangsu Collaboration Innovation Center for Advanced Inorganic Function Composites, Nanjing, 210009, Jiangsu (China); Yang, Xiaojuan; Yang, Weimin [School of Materials Science and Engineering, Nanjing Tech University, Nanjing, 210009, Jiangsu (China); Jiangsu Collaboration Innovation Center for Advanced Inorganic Function Composites, Nanjing, 210009, Jiangsu (China); Zhang, Jing [China Geol Survey, Nanjing Ctr, Nanjing, 210016, Jiangsu (China); Zhang, Qitu [School of Materials Science and Engineering, Nanjing Tech University, Nanjing, 210009, Jiangsu (China); Jiangsu Collaboration Innovation Center for Advanced Inorganic Function Composites, Nanjing, 210009, Jiangsu (China); Song, Bo; Wong, Chingping [School of Materials Science and Engineering, Georgia Institute of Technology, Atlanta, 30332, GA (United States)

    2017-03-15

    Graphical abstract: RE(AcAc){sub 3} (RE = Ce, Dy and Tb) can realize the defects modification of ZnO QDs based on the linkage occurs between the protons of the hydroxyl groups on the surface of ZnO QDs and the π–system of acetylacetone. The color coordinate could be shifted among yellow-green, blue-green, and green region by changing the RE (AcAc){sub 3} ratios. The stable Ce(AcAc){sub 3}/ZnO QDs with average sizes of about 3.0 nm can be obtained. The calculated band gap data also proved the efficient modification of Ce(AcAc){sub 3} for ZnO QDs with the largest variation of band gap energy of 0.039 eV (from 3.583 eV to 3.544 eV). - Highlights: • Defects modification of ZnO QDs based on rare earth acetylacetonate. • Stable Ce(AcAc){sub 3}/ZnO QDs with an average sizes of about 3.0 nm. • The color coordinate could be shifted among yellow-green, blue-green, and green region by changing the RE (AcAc){sub 3} ratios. - Abstract: The surface defect modification has an important effect on the application of ZnO quantum dots, and it has gained much progress in recently years, propelled by the development of additives. Our research efforts are directed toward developing a new surface modification additive RE(AcAc){sub 3} (RE = Ce, Dy, Tb) to achieve fine ZnO QDs and adjust their surface properties. RE(AcAc){sub 3}/ZnO QDs nanostructured materials have been designed and prepared, and particular emphasis has been given to the relation between the surface modification and optical properties. The effects of RE(III) acetylacetonate modification on the FT-IR, TEM images and photoluminescence (PL) spectra were investigated, and the surface defect modification principle and effect were discussed in details. The band gap (E{sub g}) was also calculated to prove the surface modification effect. For the RE(AcAc){sub 3}/ZnO QDs complex materials, stable linkage occurs because of the affinity of −COOH from acetylacetonate anionic ligand to zinc oxide surfaces, with attachment

  16. Spectral studies on the interaction of acetylacetone with aluminum-containing MCM-41 mesoporous materials

    International Nuclear Information System (INIS)

    Zanjanchi, M.A.; Vaziri, M.

    2008-01-01

    Diffuse reflectance spectroscopy (DRS) was used to study the interaction of acetylacetone (acac) with the mesoporous aluminum-containing MCM-41 materials. A room temperature synthesis method was used for preparation of purely siliceous MCM-41 and for aluminum-containing MCM-41 materials. Samples with Si/Al ratios of 50, 20, 10 and 5 were synthesized. The synthesized mesoporous materials possess highly ordered structure and high surface area as evidenced from X-ray diffraction and nitrogen physisorption measurements, respectively. The treatment of the as-synthesized aluminum-containing MCM-41 samples with acac shows a distinct band at ∼290 nm. This band is assigned to six coordinated aluminum atoms in the structure which is produced by diffusion of acac molecules through surfactant micelles and their interaction with aluminum atoms. The 290-nm band disappears upon several successive washing of the sample with ethanol. The treatment of the calcined aluminum-containing MCM-41 sample with acac produces the same 290-nm band where its intensity increases with the aluminum content of the sample. The intensity of this band is reduced upon successive ethanol washing, but remains nearly constant after three times washing. This irremovable aluminum species can be assigned to framework aluminum. The measured acidity for our aluminum-containing MCM-41 samples correlates linearly with the intensity of 290-nm band for the ethanol treated samples. This supports the idea that the Bronsted acidity in aluminum-modified MCM-41 samples is a function of the amount of tetrahedral framework aluminum in the structure

  17. Comparison of 111In-oxine and 111In-acetylacetone for the labeling of cells: in vivo and in vitro biological testing

    International Nuclear Information System (INIS)

    Mathias, C.J.; Heaton, W.A.; Welch, M.J.

    1981-01-01

    Several complexes of indium were compared as cell labels: indium-111-acetylacetone, indium-111-oxine, and indium-111-chloride complexed with 8-hydroxyquinoline (oxine) immediately prior to use. In labeling with acetylacetone, it was shown that the labeling efficiency is directly proportional to the amount of acetylacetone present, but the cell viability (as measured by in vitro aggregation studies), is inversely proportional to the amount of acetylacetone present. Biological studies were carried out in dogs using indium-111-labeled platelets; survival times and recovery values obtained with platelets labeled using all three techniques were similar. The same solutions were also used to label white blood cells; labeling efficiencies of greater than 80% were obtained in all cases, and the viability (as measured by trypan blue exclusion) was high in all cases. Chemotactic ability of the white cells labeled with indium-111-oxine is higher than that of unlabeled control cells; however, cells labeled with indium-111-acetylacetone were the same as the unlabeled control cells. (author)

  18. Influence of post-deposition annealing on structural, morphological and optical properties of copper (II) acetylacetonate thin films.

    Science.gov (United States)

    Abdel-Khalek, H; El-Samahi, M I; El-Mahalawy, Ahmed M

    2018-05-21

    In this study, the effect of thermal annealing under vacuum conditions on structural, morphological and optical properties of thermally evaporated copper (II) acetylacetonate, cu(acac) 2 , thin films were investigated. The copper (II) acetylacetonate thin films were deposited using thermal evaporation technique at vacuum pressure ~1 × 10 -5  mbar. The deposited films were thermally annealed at 323, 373, 423, and 473 K for 2 h in vacuum. The thermogravimetric analysis of cu(acac) 2 powder indicated a thermal stability of cu(acac) 2 up to 423 K. The effects of thermal annealing on the structural properties of cu(acac) 2 were evaluated employing X-ray diffraction method and the analysis showed a polycrystalline nature of the as-deposited and annealed films with a preferred orientation in [1¯01] direction. Fourier transformation infrared (FTIR) technique was used to negate the decomposition of copper (II) acetylacetonate during preparation or/and annealing up to 423 K. The surface morphology of the prepared films was characterized by means of field emission scanning electron microscopy (FESEM). A significant enhancement of the morphological properties of cu(acac) 2 thin films was obtained till the annealing temperature reaches 423 K. The variation of optical constants that estimated from spectrophotometric measurements of the prepared thin films was investigated as a function of annealing temperature. The annealing process presented significantly impacted the nonlinear optical properties such as third-order optical susceptibility χ (3) and nonlinear refractive index n 2 of cu(acac) 2 thin films. Copyright © 2018 Elsevier B.V. All rights reserved.

  19. Facile synthesis of soluble functional graphene by reduction of graphene oxide via acetylacetone and its adsorption of heavy metal ions

    International Nuclear Information System (INIS)

    Xu, Minghan; Chai, Jing; Hu, Nantao; Huang, Da; Wang, Yuxi; Huang, Xiaolu; Wei, Hao; Yang, Zhi; Zhang, Yafei

    2014-01-01

    The synthesis of graphene (GR) from graphene oxide (GO) typically involves harmful chemical reducing agents that are undesirable for most practical applications. Here we report a green and facile synthesis method for the synthesis of GR that is soluble in water and organic solvents and that includes the additional benefit of adsorption of heavy metal ions. Acetylacetone, as both a reducing agent and a stabilizer, was used to prepare soluble GR from GO. Transmission electron microscopy and atomic force microscopy provide clear evidence for the formation of few-layer GR. The results from Fourier transform infrared spectroscopy and ultraviolet-visible spectroscopy show that reduction of GO to GR has occurred. Raman spectroscopy and X-ray photoelectron spectroscopy also indicate the removal of oxygen-containing functional groups from GO, resulting in the formation of GR. The results of dispersion experiments show that GR can be highly dispersed in water and N,N-Dimethylformamide. The reaction mechanism for acetylacetone reduction of exfoliated GO was also proposed. This method is a facile and environmentally friendly approach to the synthesis of GR and opens up new possibilities for preparing GR and GR-based nanomaterials for large-scale applications. Of even greater interest is that inductively coupled plasma atomic emission spectroscopy suggests that synthesized GR may be applied in the absorption of Cd 2+ and Co 2+ due to the strong coordination capacity of acetylacetone on the surfaces and edges of GR and the large surface area of GR in aqueous solutions. The maximum adsorptions are 49.28 mg g −1 for Cd 2+ , which is 4.5 times higher than that of carbon nanotubes, and 27.78 mg g −1 for Co 2+ , which is 3.6 times higher than that of titania beans. (paper)

  20. Surface-initiated addition polymerization of norbornene by a Pd(II) catalyst bearing acetylacetone ligand on the glass slide

    Science.gov (United States)

    He, Xiaohui; Wang, Kaiti; Chen, Yiwang; Yuan, Bin

    2012-02-01

    A Pd catalyst bearing acetylacetone ligand [(CH3CO)2CHPdCl2] was covalently attracted onto the surface of glass slides, and then these Pd-terminated glass slides were immersed into a toluene solution of norbornene (NB) to produce a vinyl-type addition polynorbornene (PNB) layer on the surface of glass slides. It was found that the contract angles of the PNB-terminated glass slides surface increased with the increasing of polymerization time, and the thickness of the PNB layers were approximately 0-44.0 μm when the polymerization time was 0.5-24 h. The researching on etching also has been operated.

  1. Silica functionalized Cu(II) acetylacetonate Schiff base complex: An efficient catalyst for the oxidative condensation reaction of benzyl alcohol with amines

    Science.gov (United States)

    Anbarasu, G.; Malathy, M.; Karthikeyan, P.; Rajavel, R.

    2017-09-01

    Silica functionalized Cu(II) acetylacetonate Schiff base complex via the one pot reaction of silica functionalized 3-aminopropyltriethoxysilane with acetyl acetone and copper acetate has been reported. The synthesized material was well characterized by analytical techniques such as FT-IR, UV-DRS, XRD, SEM-EDX, HR-TEM, EPR, ICP-AES and BET analysis. The characterization results confirmed the grafting of Cu(II) Schiff base complex on the silica surface. The catalytic activity of synthesized silica functionalized Cu(II) acetylacetonate Schiff base complex was evaluated through the oxidative condensation reaction of benzyl alcohol to imine.

  2. Quantum Effects for a Proton in a Low-Barrier, Double-Well Potential: Core Level Photoemission Spectroscopy of Acetylacetone.

    Science.gov (United States)

    Feyer, Vitaliy; Prince, Kevin C; Coreno, Marcello; Melandri, Sonia; Maris, Assimo; Evangelisti, Luca; Caminati, Walther; Giuliano, Barbara M; Kjaergaard, Henrik G; Carravetta, Vincenzo

    2018-02-01

    We have performed core level photoemission spectroscopy of gaseous acetylacetone, its fully deuterated form, and two derivatives, benzoylacetone and dibenzoylmethane. These molecules show intramolecular hydrogen bonds, with a proton located in a double-well potential, whose barrier height is different for the three compounds. This has allowed us to examine the effect of the double-well potential on photoemission spectra. Two distinct O 1s core hole peaks are observed, previously assigned to two chemical states of oxygen. We provide an alternative assignment of the double-peak structure of O 1s spectra by taking full account of the extended nature of the wave function associated with the nuclear motion of the proton, the shape of the ground and final state potentials in which the proton is located, and the nonzero temperature of the samples. The peaks are explained in terms of an unusual Franck-Condon factor distribution.

  3. Economically attractive route for the preparation of high quality magnetic nanoparticles by the thermal decomposition of iron(III) acetylacetonate.

    Science.gov (United States)

    Effenberger, Fernando B; Couto, Ricardo A; Kiyohara, Pedro K; Machado, Giovanna; Masunaga, Sueli H; Jardim, Renato F; Rossi, Liane M

    2017-03-17

    The thermal decomposition (TD) methods are among the most successful in obtaining magnetic nanoparticles with a high degree of control of size and narrow particle size distribution. Here we investigated the TD of iron(III) acetylacetonate in the presence of oleic acid, oleylamine, and a series of alcohols in order to disclose their role and also investigate economically attractive alternatives for the synthesis of iron oxide nanoparticles without compromising their size and shape control. We have found that some affordable and reasonably less priced alcohols, such as 1,2-octanediol and cyclohexanol, may replace the commonly used and expensive 1,2-hexadecanediol, providing an economically attractive route for the synthesis of high quality magnetic nanoparticles. The relative cost for the preparation of Fe 3 O 4 NPs is reduced to only 21% and 9% of the original cost when using 1,2-octanediol and cyclohexanol, respectively.

  4. On synergism in inhibition of liquidphase oxidation of styrene and tetralin by organic phosphites and transition eleement acetylacetonates

    International Nuclear Information System (INIS)

    Pobedimskij, D.G.; Nasobullin, Sh.A.; Kadyrova, V.Kh.; Kirpichnikov, P.A.

    1976-01-01

    Synergism has been observed during inhibiting initiated oxidation of styrene or tetralin by organic phosphites in the presence of complex compounds of some transition metals. The results are given of non-additive intensification of antioxidative activity of triphenylphosphite (TPP) and tri-(4-methyl-6-tert.-- butyl)-phenyl-phosphite (TMBP) in the process of initiated oxidation of styrene or tetralin with addition of acetylacetonates of cobalt and vanadyl. During styrene oxidation, inhibition of the reaction with chelate complex of vanadyl is weakened considerably when phosphite is added into the reaction system. During tetralin oxidation, postcatalytic (or branched) oxidation is observed only for large concentration of vanadyl complex. Addition of TPP to above complex sharply increases the induction period. When the induction period is completed, oxidation of tetralin follows the mechanism of usual, i.e. initiated, reaction

  5. Detection limits in the chromatographic element trace analysis - quantitative TLC, HPLC and GC with the example of beryllium acetylacetonate

    International Nuclear Information System (INIS)

    Schwedt, G.

    1981-01-01

    Chromatographic analyses of beryllium acetylacetonate are carried out in synthetic solutions within the nano- and picogram range of beryllium. For thin-layer chromatography (TLC) normal and silanized silica gel is used, for high-performance liquid chromatography (HPLC) silica gel of 7 μm particles, for gas chromatography (GC) silicone SE-30 as stationary phase. Visual evaluation and remission measurements in TLC, UV-254 nm absorption measurements in HPLC and measurements with a FID in GC are employed for the determination of the calibration curves. A calibration curve through the origin and a detection limit of 150 pg Be determinable form are received by HPLC only. For trace analyses by GC a new definition of a detection limit for the evaluation of substance peaks on a solvent tailing is suggested. (orig.) [de

  6. Surfactant controlled low-temperature thermal decomposition route to zinc oxide nanorods from zinc(II) acetylacetonate monohydrate

    Energy Technology Data Exchange (ETDEWEB)

    Purkayastha, Debraj Dhar; Sarma, Bedabrat; Bhattacharjee, Chira R., E-mail: crbhattacharjee@rediffmail.com

    2014-10-15

    Zinc oxide (ZnO) nanorods were synthesized via a low-temperature thermal decomposition of zinc(II) acetylacetonate monohydrate, [Zn(C{sub 5}H{sub 7}O{sub 2}){sub 2}].H{sub 2}O. A relatively inexpensive surfactant, octadecylamine (C{sub 18}H{sub 37}NH{sub 2}) served both as a reaction solvent and a capping agent during the synthesis of ZnO nanorods. The synthesized nanorods were characterized by powder X-ray diffraction (XRD), transmission electron microscopy (TEM), FT-IR, UV–visible, and photoluminescence (PL) studies. The XRD spectrum furnished evidence for the hexagonal wurtzite structure of ZnO. TEM images revealed the material to be rod shaped having diameter 30 nm and length 200 nm. The HRTEM image showed that the lattice fringes between the two adjacent planes are 0.244 nm apart, which corresponds to the interplanar separation of the (1 0 1) plane of hexagonal ZnO. The electron diffraction (ED) pattern confirmed the single crystalline nature of the nanorods. The PL spectrum showed two UV emissions at 356 nm (∼3.48 eV) and 382 nm (∼3.25 eV). ZnO nanorods also showed very weak blue bands at 445, 453 and 470 nm. - Highlights: Low temperature thermal decomposition of zinc(II) acetylacetonate monohydrate gave zinc oxide nanorods. Powder XRD showed hexagonal wurtzite structure of ZnO having average diameter about 24 nm. TEM images revealed the material to be of rod shape having diameter 30 nm and length 200 nm. ZnO showed band gap luminescence at 356 nm, excitonic emission at 382 nm and defect related blue bands. The synthesis is simple and can act as a paradigm for obtaining various metal oxide nanomaterials.

  7. Yb3+ can be much better than Dy3+: SMM properties and controllable self-assembly of novel lanthanide 3,5-dinitrobenzoate-acetylacetonate complexes.

    Science.gov (United States)

    Gavrikov, Andrey V; Efimov, Nikolay N; Ilyukhin, Andrey B; Dobrokhotova, Zhanna V; Novotortsev, Vladimir M

    2018-05-01

    The first representatives of the binuclear lanthanide 3,5-dinitrobenzoate-acetylacetonate complexes, namely isostructural compounds [Ln(dnbz)(acac)2(H2O)(EtOH)]2 (Ln = Eu (1), Gd (2), Tb (3), Dy (4), Ho (5), Er (6), Tm (7), and Yb (8); dnbz - 3,5-dinitrobenzoate anion; acac - acetylacetonate (pentane-2,4-dionate) anion) were prepared and characterized. The SMM behavior of the Yb compound 8 was shown to be surprisingly less sensitive to the composition of the Yb3+ coordination environment in comparison with that of the Dy derivative. For Yb compound 8, the anisotropy barrier is Δeff/kB = 26 K under the dc field of 2000 Oe. This value is the highest one currently known for binuclear Yb complexes.

  8. Assignment of solid-state 13C and 1H NMR spectra of paramagnetic Ni(II) acetylacetonate complexes aided by first-principles computations

    DEFF Research Database (Denmark)

    Rouf, Syed Awais; Jakobsen, Vibe Boel; Mareš, Jiří

    2017-01-01

    Recent advances in computational methodology allowed for first-principles calculations of the nuclear shielding tensor for a series of paramagnetic nickel(II) acetylacetonate complexes, [Ni(acac)2L2] with L = H2O, D2O, NH3, ND3, and PMe2Ph have provided detailed insight into the origin of the par......Recent advances in computational methodology allowed for first-principles calculations of the nuclear shielding tensor for a series of paramagnetic nickel(II) acetylacetonate complexes, [Ni(acac)2L2] with L = H2O, D2O, NH3, ND3, and PMe2Ph have provided detailed insight into the origin...

  9. Formation of TiO/Al2O3/C Composite in Thermal Co-decomposition of Aluminium(III) Acetylacetonate and Titanium(IV) Oxyacetylacetonate.

    Czech Academy of Sciences Publication Activity Database

    Kovářík, T.; Pokorná, Dana; Urbanová, Markéta; Bezdička, Petr; Bastl, Zdeněk; Kupčík, Jaroslav; Křenek, T.; Pola, M.; Kullová, L.; Pola, Josef

    2016-01-01

    Roč. 117, JAN 2016 (2016), s. 182-190 ISSN 0165-2370 R&D Projects: GA TA ČR TA04020860 Institutional support: RVO:67985858 ; RVO:61388980 ; RVO:61388955 Keywords : thermal co-decomposition * aluminium(III) acetylacetonate * titanium(IV) oxyacetylacetonate * titanium monoxide * alumina * Carbona Subject RIV: CF - Physical ; Theoretical Chemistry; CA - Inorganic Chemistry (UACH-T) Impact factor: 3.471, year: 2016

  10. Indium Doped Zinc Oxide Thin Films Deposited by Ultrasonic Chemical Spray Technique, Starting from Zinc Acetylacetonate and Indium Chloride

    Directory of Open Access Journals (Sweden)

    Rajesh Biswal

    2014-07-01

    Full Text Available The physical characteristics of ultrasonically sprayed indium-doped zinc oxide (ZnO:In thin films, with electrical resistivity as low as 3.42 × 10−3 Ω·cm and high optical transmittance, in the visible range, of 50%–70% is presented. Zinc acetylacetonate and indium chloride were used as the organometallic zinc precursor and the doping source, respectively, achieving ZnO:In thin films with growth rate in the order of 100 nm/min. The effects of both indium concentration and the substrate temperature on the structural, morphological, optical, and electrical characteristics were measured. All the films were polycrystalline, fitting well with hexagonal wurtzite type ZnO. A switching in preferential growth, from (002 to (101 planes for indium doped samples were observed. The surface morphology of the films showed a change from hexagonal slices to triangle shaped grains as the indium concentration increases. Potential applications as transparent conductive electrodes based on the resulting low electrical resistance and high optical transparency of the studied samples are considered.

  11. Phosphorescence quantum yield determination with time-gated fluorimeter and Tb(III)-acetylacetonate as luminescence reference

    Energy Technology Data Exchange (ETDEWEB)

    Penzkofer, A., E-mail: alfons.penzkofer@physik.uni-regensburg.de [Fakultät für Physik, Universität Regensburg, Universitätsstrasse 31, D-93053 Regensburg (Germany)

    2013-03-29

    Highlights: ► Procedure for absolute phosphorescence quantum yield measurement is described. ► Experimental setup for absolute luminescence quantum yield standard calibration. ► Tb(acac){sub 3} proposed as phosphorescence quantum yield reference standard. ► Luminescence quantum yield of Tb(acac){sub 3} in cyclohexane measured. ► Luminescence lifetime of Tb(acac){sub 3} in cyclohexane measured. - Abstract: Phosphorescence quantum yield measurements of fluorescent and phosphorescent samples require the use of time-gated fluorimeters in order to discriminate against the fluorescence contribution. As reference standard a non-fluorescent luminescent compound is needed for absolute phosphorescence quantum yield determination. For this purpose the luminescence behavior of the rare earth chelate terbium(III)-acetylacetonate (Tb(acac){sub 3}) was studied (determination of luminescence quantum yield and luminescence lifetime). The luminescence quantum yield of Tb(acac){sub 3} was determined by using an external light source and operating the fluorimeter in chemo/bioluminescence mode with a fluorescent dye (rhodamine 6G in methanol) as reference standard. A procedure is developed for absolute luminescence (phosphorescence) quantum yield determination of samples under investigation with a time-gated fluorimeter using a non-fluorescent luminescent compound of known luminescence quantum yield and luminescence lifetime.

  12. Acetylacetone as an efficient electron shuttle for concerted redox conversion of arsenite and nitrate in the opposite direction.

    Science.gov (United States)

    Chen, Zhihao; Song, Xiaojie; Zhang, Shujuan; Wu, Bingdang; Zhang, Guoyang; Pan, Bingcai

    2017-11-01

    The redox conversion of arsenite and nitrate has direct effects on their potential environment risks. Due to the similar reduction potentials, there are few technologies that can simultaneously oxidize arsenite and reduce nitrate in one process. Here, we demonstrate that a diketone-mediated photochemical process could efficiently do this. A combined experimental and theoretical investigation was conducted to elucidate the mechanisms behind the redox conversion in the UV/acetylacetone (AA) process. Our key finding is that UV irradiation significantly changed the redox potential of AA. The excited AA, 3 (AA)*, acted as a semiquinone radical-like electron shuttle. For arsenite oxidation, the efficiency of 3 (AA)* was 1-2 orders of magnitude higher than those of quinone-type electron shuttles, whereas the consumption of AA was 2-4 orders of magnitude less than those of benzonquinones. The oxidation of arsenite and reduction of nitrate could be both accelerated when they existed together in UV/AA process. The results indicate that small diketones are some neglected but potent electron shuttles of great application potential in regulating aquatic redox reactions with the combination of UV irradiation. Copyright © 2017 Elsevier Ltd. All rights reserved.

  13. Synthesis, structure, theoretical studies and luminescent properties of a ternary erbium(III) complex with acetylacetone and bathophenanthroline ligands

    Energy Technology Data Exchange (ETDEWEB)

    Martín-Ramos, Pablo [CEMDRX, Department of Physics, Universidade de Coimbra, Rua Larga, P-3004-516 Coimbra (Portugal); Advanced Materials Laboratory, ETSIIAA, Universidad de Valladolid, Avenida de Madrid 44, 34004 Palencia (Spain); Silva, Pedro S. Pereira, E-mail: psidonio@pollux.fis.uc.pt [CEMDRX, Department of Physics, Universidade de Coimbra, Rua Larga, P-3004-516 Coimbra (Portugal); Chamorro-Posada, Pedro [Higher Technical School of Telecommunications Engineering, Universidad de Valladolid, Campus Miguel Delibes, Paseo Belén 15, 47011 Valladolid (Spain); Silva, Manuela Ramos [CEMDRX, Department of Physics, Universidade de Coimbra, Rua Larga, P-3004-516 Coimbra (Portugal); Milne, Bruce F. [Centre for Computational Physics, Department of Physics, Universidade de Coimbra, P-3004-516 Coimbra (Portugal); Donostia International Physics Centre, Paseo Manuel de Lardizabal 4, 20018 Donostia-San Sebastián (Spain); Nogueira, Fernando [Centre for Computational Physics, Department of Physics, Universidade de Coimbra, P-3004-516 Coimbra (Portugal); Martín-Gil, Jesús [Advanced Materials Laboratory, ETSIIAA, Universidad de Valladolid, Avenida de Madrid 44, 34004 Palencia (Spain)

    2015-06-15

    A novel erbium(III) complex with acetylacetone (Hacac) and bathophenanthroline (4,7-diphenyl-1,10-phenanthroline, bath) ligands, formulated as [Er(acac){sub 3}(bath)], has been characterized by elemental analysis, X-ray diffraction, thermogravimetric analysis, Fourier transform infrared spectroscopy, Raman spectroscopy, absorption and emission spectroscopies. In the theoretical part of this study, semi-empirical quantum chemistry methods using AM1, PM3, PM6 and PM7 models have been employed to predict the structure of the complex, calculate the geometric and crystallographic parameters, and make comparisons with spectroscopic data using INDO/S-CI calculations. Real-time time-dependent density-functional theory (TDDFT) has also been used to calculate the optical absorption spectrum of the complex in the gas phase. - Highlights: • Synthesis and structure of a new erbium(III) β-diketonate complex. • TDDFT used for the first time to calculate the optical absorption spectrum. • Complex show strong near-infrared luminescence at 1.53 µm due to antenna effect.

  14. Synthesis, structure, theoretical studies and luminescent properties of a ternary erbium(III) complex with acetylacetone and bathophenanthroline ligands

    International Nuclear Information System (INIS)

    Martín-Ramos, Pablo; Silva, Pedro S. Pereira; Chamorro-Posada, Pedro; Silva, Manuela Ramos; Milne, Bruce F.; Nogueira, Fernando; Martín-Gil, Jesús

    2015-01-01

    A novel erbium(III) complex with acetylacetone (Hacac) and bathophenanthroline (4,7-diphenyl-1,10-phenanthroline, bath) ligands, formulated as [Er(acac) 3 (bath)], has been characterized by elemental analysis, X-ray diffraction, thermogravimetric analysis, Fourier transform infrared spectroscopy, Raman spectroscopy, absorption and emission spectroscopies. In the theoretical part of this study, semi-empirical quantum chemistry methods using AM1, PM3, PM6 and PM7 models have been employed to predict the structure of the complex, calculate the geometric and crystallographic parameters, and make comparisons with spectroscopic data using INDO/S-CI calculations. Real-time time-dependent density-functional theory (TDDFT) has also been used to calculate the optical absorption spectrum of the complex in the gas phase. - Highlights: • Synthesis and structure of a new erbium(III) β-diketonate complex. • TDDFT used for the first time to calculate the optical absorption spectrum. • Complex show strong near-infrared luminescence at 1.53 µm due to antenna effect

  15. Atomic absorption spectrophotometric determination of microamounts of beryllium in aluminum and copper using solvent extraction with acetylacetone

    International Nuclear Information System (INIS)

    Matsusaki, Koji

    1975-01-01

    A sensitive method for the determination of microamounts of beryllium in aluminum and copper by atomic absorption spectrophotometry using the methylisobutylketone (MIBK) extraction with acetylacetone (AA) was investigated. An aqueous sample solution containing (0.5--5)μg of beryllium and less than 100 mg of aluminum or less than 500 mg of copper was taken into a 100-ml separation funnel, and 2 ml of 5% AA, 20 mg of EDTA for 1 mg of aluminum or 8.8 mg of EDTA for 1 mg of copper, and 10 ml of saturated NaCl solution were added. The pH was adjusted to 5--7 with 10 ml of 2 M NaCH 3 COO-CH 3 COOH buffer, and the solution was diluted to 50 ml. After 10 minutes, the solution was shaken for 2 minutes with 10 ml of MIBK. The organic phase was introduced into a nitrous oxide-acetylene flame and the absorption measured at 234.9 nm against a reagent blank. None of metal elements interfered with the determination of beryllium, and beryllium above 0.001% in aluminum, and above 0.0002% in copper was determined. This method was successfully applied to the determination of beryllium in aluminum and copper alloys. (auth.)

  16. The energy of hydration and solvation of indium salts in the acetylacetone-InCl3-water system

    International Nuclear Information System (INIS)

    Kulawik, I.; Baumgartner, T.

    1978-01-01

    On the base of the previous papers concerning the investigations in the extraction systems the experiments were performed for the determination of thermodynamical distribution coefficient of indium salts between two phases in the system: acetylacetone-InCl 3 -water and the energy of hydration and solvation of that system. The results of the surface and interfacial potentials measurements of the system were presented as a function of the InCl 3 concentration in the system before the extraction. The extraction coefficients of indium as a function of concentration of InCl 3 in this system were determined. The method of the visible absorption spectra was used to the determination of concentration of indium in both phases after the extraction. The relation between the percentage of the extraction and the extraction coefficient was determined. The investigations were performed in the system containing 0.1 M HCl and 0.001 M HCl in the aqueous phase. The results of experiments are tabulated and graphically presented in figures. (author)

  17. Iron-Mediated Homogeneous ICAR ATRP of Methyl Methacrylate under ppm Level Organometallic Catalyst Iron(III Acetylacetonate

    Directory of Open Access Journals (Sweden)

    Jian Wu

    2016-01-01

    Full Text Available Atom Transfer Radical Polymerization (ATRP is an important polymerization process in polymer synthesis. However, a typical ATRP system has some drawbacks. For example, it needs a large amount of transition metal catalyst, and it is difficult or expensive to remove the metal catalyst residue in products. In order to reduce the amount of catalyst and considering good biocompatibility and low toxicity of the iron catalyst, in this work, we developed a homogeneous polymerization system of initiators for continuous activator regeneration ATRP (ICAR ATRP with just a ppm level of iron catalyst. Herein, we used oil-soluble iron (III acetylacetonate (Fe(acac3 as the organometallic catalyst, 1,1′-azobis (cyclohexanecarbonitrile (ACHN with longer half-life period as the thermal initiator, ethyl 2-bromophenylacetate (EBPA as the initiator, triphenylphosphine (PPh3 as the ligand, toluene as the solvent and methyl methacrylate (MMA as the model monomer. The factors related with the polymerization system, such as concentration of Fe(acac3 and ACHN and polymerization kinetics, were investigated in detail at 90 °C. It was found that a polymer with an acceptable molecular weight distribution (Mw/Mn = 1.43 at 45.9% of monomer conversion could be obtained even with 1 ppm of Fe(acac3, making it needless to remove the residual metal in the resultant polymers, which makes such an ICAR ATRP process much more industrially attractive. The “living” features of this polymerization system were further confirmed by chain-extension experiment.

  18. Applicability of light sources and the inner filter effect in UV/acetylacetone and UV/H{sub 2}O{sub 2} processes

    Energy Technology Data Exchange (ETDEWEB)

    Wu, Bingdang; Yang, Minghui [State Key Laboratory of Pollution Control and Resource Reuse, School of the Environment, Nanjing University, Nanjing, 210023 (China); Yin, Ran [Department of Civil and Environmental Engineering, The Hong Kong University of Science and Technology, Clear Water Bay, Kowloon (Hong Kong); Zhang, Shujuan, E-mail: sjzhang@nju.edu.cn [State Key Laboratory of Pollution Control and Resource Reuse, School of the Environment, Nanjing University, Nanjing, 210023 (China)

    2017-08-05

    Highlights: • Acetylacetone (AA) could directly use solar irradiation to decolorize dyes. • AA had a wider applicability than H{sub 2}O{sub 2} to a variety of light sources. • The photonic efficiency in the UV/AA process was target-dependent. • An accurate calculation approach for the inner filter effect was developed. - Abstract: Light source is a crucial factor in the application of a photochemical process, which determines the energy efficiency. The performances of acetylacetone (AA) in conversion of aqueous contaminants under irradiation with a low-pressure mercury lamp, a medium-pressure mercury lamp, a xenon lamp, and natural sunlight were investigated and compared with those of H{sub 2}O{sub 2} as reference. In all cases, AA was superior to H{sub 2}O{sub 2} in the degradation of Acid Orange 7. Using combinations of the different light sources with various cut-off and band-pass filters, the spectra responses of the absorbed photons in the UV/AA and UV/H{sub 2}O{sub 2} processes were determined for two colored and two colorless compounds. The photonic efficiency (φ) of the two photochemical processes was found to be target-dependent. A calculation approach for the inner filter effect was developed by taking the obtained φ into account, which provides a more accurate indication of the reaction mechanisms.

  19. Synthesis, Structure and Electrochemistry of Tetranuclear Oxygen-Centered Copper(II) Clusters with Acetylacetone and Benz-pyrazole Hydrolyzed Derivatives as Ligand.

    Science.gov (United States)

    Vafazadeh, Rasoul; Willis, Anthony C

    2016-01-01

    Two copper(II) clusters Cu(4)OCl(6)(pyrazole)4, 1, and Cu(4)OBr(6)(Br-pyrazole)4, 2, have been synthesized by reacting acetylacetone and benzohydrazide (1:1 ratio) with CuX(2) (X = Cl for 1 and X= Br for 2) in methanol solutions. The structures of both clusters have been established by X-ray crystallography. The clusters contain four Cu, one O, six μ(2)-X atoms, and four pyrazole ligands. The pyrazoles was prepared in situ by the reaction of acetylacetone with benzohydrazide in methanol under reflux. In 2, the methine hydrogens of the pyrazole ligands have been replaced by bromine atoms. The four copper atoms encapsulate the central O atom in a tetrahedral arrangement. All copper atoms are five-coordinate and have similar coordination environments with slightly distorted trigonal bipyramidal geometry. The cyclic voltammogram of the clusters 1 and 2 show a one-electron quasi-reversible reduction wave in the region 0.485 to 0.731 V, and a one-electron quasi-reversible oxidation wave in the region 0.767 to 0.898 V. In 1, one irreversible oxidative response is observed on the positive of side of the voltammogram at 1.512 V and this can be assigned to Cu(II) to Cu(III) oxidation.

  20. Determination of Chromium(III), Chromium(VI), and Chromium(III) acetylacetonate in water by ion-exchange disk extraction/metal furnace atomic absorption spectrometry

    International Nuclear Information System (INIS)

    Kamakura, Nao; Inui, Tetsuo; Kitano, Masaru; Nakamura, Toshihiro

    2014-01-01

    A new method for the separate determination of Chromium(III) (Cr(III)), Chromium(VI) (Cr(VI)), and Cr(III) acetylacetonate (Cr(acac) 3 ) in water was developed using a cation-exchange extraction disk (CED) and an anion-exchange extraction disk (AED) combined with metal furnace atomic absorption spectrometry (MFAAS). A 100-mL water sample was adjusted to pH 5.6 and passed through the CED placed on the AED. Cr(acac) 3 and Cr(III) were adsorbed on the CED, and Cr(VI) was adsorbed on the AED. The adsorbed Cr(acac) 3 was eluted with 50 mL of carbon tetrachloride, followed by the elution of Cr(III) with 50 mL of 3 mol L −1 nitric acid. Cr(VI) was eluted with 50 mL of 3 mol L −1 nitric acid. The chemical species of Cr eluted from the CED with carbon tetrachloride was identified as Cr(acac) 3 using infrared spectroscopy. The eluate of Cr(acac) 3 was diluted to 100 mL with carbon tetrachloride, and those of Cr(III) and Cr(VI) were diluted to 100 mL with deionized water. All of the solutions were subsequently analyzed by MFAAS. The calibration curve for the Cr(acac) 3 aqueous solutions exhibited good linearity in the range of 0.1 to 1 ng. The detection limit of Cr, which corresponded to three times the standard deviation (n = 10) of the blank values, was 20 pg. The recovery test for Cr(III), Cr(VI), and Cr(acac) 3 exhibited desirable results (96.0%–107%) when 5 μg of each species (50 μg L −1 ) was added to 100 mL water samples (i.e., tap water, rainwater, and bottled drinking water). In a humic acid solution, Cr(acac) 3 was quantitatively recovered (103%), but Cr(III) and Cr(VI) exhibited poor recoveries (i.e., 84.8% and 78.4%, respectively). - Highlights: • A determination method of Cr(III), Cr(VI), and Cr(III) acetylacetonate in water was developed. • The combination of ion-exchange resin disks with metal furnace AAS was used. • No effect of humic acid on the recovery of Cr(III) acetylacetonate was observed. • The proposed method enabled the determination

  1. Effect of the substituents on the photophysical, electrochemical and electroluminescence properties of OLED dopant Iridium bis(2-phenylbenzothiozolato- N,C2')(acetylacetonate)

    Science.gov (United States)

    Ivanov, P.; Tomova, R.; Petrova, P.

    2014-12-01

    The effect of two substituents: clorine and 1,3-diphenylpropane-1,3-dionate, placed on different position in the molecule of Iridium (III) bis(2-phenylbenzothiozolato-N,C2')- (acetylacetonate) (bt)2Ir(acac), on its electrochemical behaviour, photophysical and electroluminescence properties were investigated. Three complexes (bt)2Ir(acac), Iridium (III) bis[2-(4-chlorophenyl)benzothiazolato-N,C2']-acetylacetonate (Clbt)2Ir(acac), in which the Cl atom was introduced on the 4-position in the benzothiazole ring, and the new Iridium (Ill) bis[2 -phenylbenzothiazolato -N,C2'] -(1,3 -diphenylpropane-1,3 -dionate) (bt)2Ir(dbm), where ancillary acetylacetonate ligand was replaced by 1,3-diphenylpropane-1,3-dionate, were synthesized and characterised by 1H-NMR and elemental analysis. The HOMO/LUMO energy levels of the complexes were determined by cyclic voltammetry (CV) and their properties were established by UV-Visible and fluorescence spectroscopy. The application of (Clbt)2Ir(acac), (bt)2Ir(bsm) and (bt)2Ir(acac) as dopants in hole transporting layer (HTL) of Organic light- emitting diodes(OLEDs). It was found that with respect to the reference (bt)2Ir(acac): both LUMO and HOMO of the substituted complexes were shifted to more positive values accordingly with 0.23 and 0.19 eV for (Clbt)2Ir(acac) and 0.14 and 0.12 eV for (bt)2Ir(dbm). OLEDs doped with 1 w% of the complexes irradiated the warm white light with Commission internationale de l'eclairage (CIE) coordinates: 0.24;0.38 for (Clbt)2Ir(acac), 0.30;0.44 for (bt)2Ir(acac) and 0.28;0.46 for (bt)2Ir(dbm). Devices doped with 10 w% of all complexes irradiated in the yellow orange region of the spectrum.

  2. A comparative study of roles played by aluminum tribromide and aluminum acetylacetonate on the thermal degradation of PMMA by simultaneous thermoanalytical techniques

    International Nuclear Information System (INIS)

    Arshad, M.; Arif, M.

    2008-01-01

    Blends of poly(methyl methacrylate) (PMMA) were prepared with aluminum tribromide (AlBr/sub 3/) and aluminum acetylacetonate (Al(acac)/sub 3/) in definite ratios. Thermal studies (TG-DTG-DTA) of polymer and blends with both additives were carried out in inert atmosphere to investigate the mode of degradation and the effects of stability/destability on either component. The addition of compounds in polymer resulted early decompositions. The intermediates formed during decomposition were also identified. The possible explanation of the thermal degradation reactions is advanced on the basis of results gathered. The apparent activation energy (E/sub o/) and order of reaction (n) of the pyrolytic reactions were determined by Horowitz and Metzger method from the corresponding TG curves. (author)

  3. Multi-wall carbon nanotubes supported molybdenyl acetylacetonate: Efficient and highly reusable catalysts for epoxidation of alkenes with tert-butyl hydroperoxide

    Energy Technology Data Exchange (ETDEWEB)

    Esnaashari, Fariba [Department of Chemistry, Catalysis Division, University of Isfahan, Isfahan 81746-73441 (Iran, Islamic Republic of); Moghadam, Majid, E-mail: moghadamm@sci.ui.ac.ir [Department of Chemistry, Catalysis Division, University of Isfahan, Isfahan 81746-73441 (Iran, Islamic Republic of); Mirkhani, Valiollah, E-mail: mirkhani@sci.ui.ac.ir [Department of Chemistry, Catalysis Division, University of Isfahan, Isfahan 81746-73441 (Iran, Islamic Republic of); Tangestaninejad, Shahram; Mohammadpoor-Baltork, Iraj; Khosropour, Ahmad Reza; Zakeri, Maryam [Department of Chemistry, Catalysis Division, University of Isfahan, Isfahan 81746-73441 (Iran, Islamic Republic of)

    2012-11-15

    Efficient epoxidation of olefins catalyzed by MoO{sub 2}(acac){sub 2} supported on amines functionalized MWCNTs is reported. The MWCNTs bearing carboxylic acid groups were modified with 2-aminophenol and 2-aminothiophenol. These amine-MWCNTs act as bidentate ligand for attachment of Mo catalyst. These catalysts were characterized by elemental analysis, scanning electron microscopy, FT-IR and diffuse reflectance UV-Vis spectroscopic methods. The prepared catalysts were used for efficient epoxidation of different alkenes such as cyclic and linear ones with tert-butyl hydroperoxide in refluxing 1,2-dichloroethane. These heterogeneous catalysts can be reused several times without significant loss of their catalytic activity. Highlights: Black-Right-Pointing-Pointer Supporting of molybdenyl acetylacetonate on amine-modified MWCNTs. Black-Right-Pointing-Pointer Heterogeneous catalysts were prepared. Black-Right-Pointing-Pointer These catalysts were highly efficient in the epoxidation of alkenes with TBHP. Black-Right-Pointing-Pointer Makes the catalysts reusable.

  4. Multi-wall carbon nanotubes supported molybdenyl acetylacetonate: Efficient and highly reusable catalysts for epoxidation of alkenes with tert-butyl hydroperoxide

    International Nuclear Information System (INIS)

    Esnaashari, Fariba; Moghadam, Majid; Mirkhani, Valiollah; Tangestaninejad, Shahram; Mohammadpoor-Baltork, Iraj; Khosropour, Ahmad Reza; Zakeri, Maryam

    2012-01-01

    Efficient epoxidation of olefins catalyzed by MoO 2 (acac) 2 supported on amines functionalized MWCNTs is reported. The MWCNTs bearing carboxylic acid groups were modified with 2-aminophenol and 2-aminothiophenol. These amine–MWCNTs act as bidentate ligand for attachment of Mo catalyst. These catalysts were characterized by elemental analysis, scanning electron microscopy, FT-IR and diffuse reflectance UV–Vis spectroscopic methods. The prepared catalysts were used for efficient epoxidation of different alkenes such as cyclic and linear ones with tert-butyl hydroperoxide in refluxing 1,2-dichloroethane. These heterogeneous catalysts can be reused several times without significant loss of their catalytic activity. Highlights: ► Supporting of molybdenyl acetylacetonate on amine-modified MWCNTs. ► Heterogeneous catalysts were prepared. ► These catalysts were highly efficient in the epoxidation of alkenes with TBHP. ► Makes the catalysts reusable.

  5. Contribution to the study of the chemical consequences of the (n, {gamma}) reaction in solid Co(3) tris-acetylacetone; Contribution a l'etude des consequences chimiques de la reaction (n, {gamma}) dans le tris-acetylacetonate de cobalt (3)

    Energy Technology Data Exchange (ETDEWEB)

    Magnane Machado, R [Commissariat a l' Energie Atomique, Grenoble (France). Centre d' Etudes Nucleaires

    1969-07-01

    The fragmentation and annealing of thermal neutron irradiated Co(III) tris-acetylacetone was investigated using the thin layer chromatographic technique (silica-gel 1 mm thickness). Low temperature irradiations (0 C - -72 C and -180 C) lead to {sup 60}Co retentions as low as (1,1 {+-} 0,2) per cent. Annealing by linear temperature programming at different heating rates has shown the existence of eight reactions. The influences of pile dose and of gases (air and helium) as well as of thermal decomposition on the annealing processes were confirmed. A temperature and dose dependent effect was found out for the retentions of the {sup 60m}Co - {sup 60}Co isomers. (author) [French] On a etudie par chromatographie en couches minces (silicagel 1 mm), les phenomenes de fragmentation et de recuit sur l'acetylacetonate de Co(III) irradie aux neutrons thermiques. La valeur minimale de la retention observee pour des irradiations a basse temperature (0 C, -72 C, -180 C) se situe a (1,1 {+-} 0,2) pour cent. Le recuit thermique, par montee lineaire de la temperature a differentes vitesses de chauffage, montre l'existence de huit reactions. On confirme, de plus, l'influence sur les processus de recuit de la dose recue en pile, de l'atmosphere dans laquelle l'echantillon se trouve (air et helium) ainsi que de la decomposition thermique. Cette dependance de la temperature et de la dose est prouvee par les valeurs des retentions mesurees sur les isomeres {sup 60m}Co - {sup 60}Co. (auteur)

  6. ESI-MS studies of the reactions of novel platinum(II) complexes containing O,O'-chelated acetylacetonate and sulfur ligands with selected model proteins.

    Science.gov (United States)

    Marzo, Tiziano; De Pascali, Sandra A; Gabbiani, Chiara; Fanizzi, Francesco P; Messori, Luigi; Pratesi, Alessandro

    2017-08-01

    A group of mixed-ligand Pt(II) complexes bearing acetylacetonate and sulphur ligands were recently developed in the University of Lecce as a new class of prospective anticancer agents that manifested promising pharma-cological properties in preliminary in vitro and in vivo tests. Though modelled on the basis of cisplatin, these Pt(II) complexes turned out to exhibit a profoundly distinct mode of action as they were found to act mainly on non-genomic targets rather than on DNA. Accordingly, we have explored here their reactions with two representative model proteins through an established ESI-MS procedure with the aim to describe their general interaction mechanism with protein targets. A pronounced reactivity with the tested proteins was indeed documented; the nature of the resulting metallodrug-protein interactions could be characterised in depth in the various cases. Preferential binding to protein targets compared to DNA is supported by independent ICP-OES measurements. The implications of these findings are discussed.

  7. Molecular structure, spectroscopic studies, and coppersbnd oxygen bond strength of α-methyl and α-ethyl derivatives of copper (II) acetylacetonate; Experimental and theoretical approach

    Science.gov (United States)

    Seyedkatouli, Seyedabdollah; Vakili, Mohammad; Tayyari, Sayyed Faramarz; Afzali, Raheleh

    2018-05-01

    This paper presents a combined experimental and theoretical study on the Cusbnd O bond strength of copper (II) α-methylacetylacetonate, Cu(3-Meacac)2, and copper (II) α-ethylacetylacetonate, Cu(3-Etacac)2, complexes in comparison to that in copper (II) acetylacetonate, Cu(acac)2. For this purpose, the molecular structure, UV spectra, and complete vibrational assignment of target molecules were investigated by DFT, Natural Bond Orbital (NBO) theory, and Atoms-in-Molecules (AIM) analysis at the B3LYP/6-311G* level of theory. The mentioned results are compared with those in Cu(acac)2. Fourier transform-Raman, IR, and UV spectra of these complexes have been also recorded. A complete assignment of the observed band frequencies has been done. All theoretical and experimental spectroscopic results are consisting with a stronger metal-oxygen bond in Cu(3-Meacac)2 and Cu(3-Etacac)2 complexes compared with Cu(acac)2. In addition, these results confirm that there is no significant difference between the Cusbnd O bond strength of the Cu(3-Meacac)2 and Cu(3-Etacac)2 complexes.

  8. Radiation induced synthesis of In{sub 2}O{sub 3} nanoparticles - Part II: Synthesis of In{sub 2}O{sub 3} nanoparticles by thermal decomposition of un-irradiated and γ-irradiated indium acetylacetonate

    Energy Technology Data Exchange (ETDEWEB)

    Al-Resheedi, Ajayb Saud; Alhokbany, Norah Saad [Department of Chemistry, College of Science, King Saud University, KSU, (Saudi Arabia); Mahfouz, Refaat Mohammed, E-mail: rmhfouz@science.au.edu.eg [Chemistry Department, Faculty of Science, Assiut University, AUN, (Egypt)

    2015-09-15

    Pure cubic phase, In{sub 2}O{sub 3} nanoparticles with porous structure were synthesized by solid state thermal oxidation of un-irradiated and γ-irradiated indium acetyl acetonate in presence and absence of sodium dodecyl sulphate as surfactant. The as- synthesized In{sub 2}O{sub 3} nanoparticles were characterized by X-ray diffraction (XRD), fourier transformation infrared spectroscopy (FT-IR), scanning electron microscopy (SEM), transition electron microscopy (TEM) and thermogravimetry (TG). The shapes and morphologies of as- synthesized In{sub 2}O{sub 3} nanoparticles were highly affected by γ-irradiation of indium acetyl acetonate precursor and by addition of sodium dodecyl sulphate as surfactant. Calcination of un-irradiated indium acetyl acetonate precursor to 4 hours of 600 °C leads to the formation of spherical- shaped accumulative and merged In{sub 2}O{sub 3} nanoparticles with porous structure, whereas irregular porous architectures composed of pure In{sub 2}O{sub 3} nanoparticles were obtained by using γ-irradiated indium acetylacetonate precursor. The as- prepared In{sub 2}O{sub 3} nano products exhibit photoluminescence emission (PL) property and display thermal stability in a wide range of temperature (25-800 °C) which suggest possible applications in nanoscale optoelectronic devices. (author)

  9. Synthesis and characterization of tetraphenylporphyrinate of dysprosium route dysprosium acetylacetonate

    International Nuclear Information System (INIS)

    Martinez M, V.

    1992-01-01

    Dysprosium bis (tetraphenylporphyrinate) and bis (dysprosium) Tris (tetraphenylporphyrinate) were synthesized from dysprosium tetraphenylporphyrinate prepared in situ, and characterized by IR, UV-vis, TGA, DTA, EPR and magnetic susceptibility measurements. The double decker compound was obtained by direct oxidation of the HDy(TPP) 2 intermediate. The existence of the radical anion, (TPP) - , in the double decker product was conformed by EPR spectrometry. Dysprosium monoporphyrinate was isolated and characterized by the same techniques. (Author)

  10. NiOx Nanoparticle Synthesis by Chemical Vapor Deposition from Nickel Acetylacetonate

    Czech Academy of Sciences Publication Activity Database

    Moravec, Pavel; Smolík, Jiří; Keskinen, H.; Mäkelä, J.M.; Bakardjieva, Snejana; Levdansky, V.V.

    2011-01-01

    Roč. 2, č. 4 (2011), s. 258-264 ISSN 2153-117X R&D Projects: GA ČR GA104/07/1093 Institutional research plan: CEZ:AV0Z40720504; CEZ:AV0Z40320502 Keywords : electron diffraction * nickel nanostructures * hot wall tube reactor Subject RIV: CF - Physical ; Theoretical Chemistry http://www.scirp.org/journal/msa/

  11. Uranyl(VI)-acetylacetonate coordination compounds with various N-heterocyclic ligands

    International Nuclear Information System (INIS)

    Kawasaki, Takeshi; Nishimura, Tatsuru; Kitazawa, Takafumi

    2010-01-01

    Seven uranyl(VI) complexes, [UO 2 (acac) 2 (L)] [L=4-methylpyridine (1), 4-ethylpyridine (2), 2,4-dimethylpyridine (3), (-)-nicotine (4), and imidazole (5)], [{UO 2 (acac) 2 } 2 -(4,4'-bipyridine)] (6), and [(2,2'-bipyridine) 2 H][UO 2 (acac)(NO 3 ) 2 ] (7) have been synthesized and characterized crystallographically. The coordination geometry of U has a UNO 6 pentagonal-bipyramidal coordination in 1-6, and a UO 8 hexagonal-bipyramidal coordination in 7. (author)

  12. Study on Dihydrated Praseodymium Acetylacetonate by Photoacoustic Spectra with Broad Wavelength Range

    Institute of Scientific and Technical Information of China (English)

    于锡娟; 伍荣护; 宋慧宇; 苏庆德

    2003-01-01

    The UV-Vis, NIR and MIR photoacoustic spectra of Pr(aa)3*2H2O were measured and most f-f transition peaks of Pr3+ are detected. The peak split and peak shift are studied also. The covalency parameter is calculated and it turns out that the covalent bonds between Pr(Ⅲ) ions and ligands exist. The results conclude that photoacoustic spectroscopy offers a unique and complementary method in analysis of solid rare earth complexes. Compared with conventional FT-IR transmission and absorption approaches, PAS has the advantages of fast, nondestructive analysis and high resolution.

  13. Studies in technetium chemistry, Project 1: Evaluation of technetium acetylacetonates as potential cerebral blood flow agents, Project 2

    International Nuclear Information System (INIS)

    Jones, A.G.; Packard, A.B.; Treves, S.; Davison, A.

    1990-01-01

    Although the emphasis in our original submission was on N 2 S 2 and N 3 S coordinating ligands in technetium(V), we have now broadened the chemistry studies into areas that encompass new systems that allow the generation of neutral complexes. This change was based upon developments that have taken place in our basic chemistry studies that could bear on one of the original aims of this work, i.e., the design of complexes designed to penetrate cellular membranes and to remain trapped in target tissues. Among these topics are oxotechnetium(V) complexes containing amine and alcoholate ligands, coordination compounds containing the alternative technetium(V) nitrido core and the synthesis at macroscopic levels of a tetradentate ''umbrella'' ligand that successfully binds the metal. Basic studies with the original bisamide-bisthiol ligand system have continued with the identification of the products formed when aqueous solutions of the complex [TcO(ema)] - are acidified. This material is isolatable as yellow/brown crystals when HCl is added to the tetraphenylarsonium salt of the complex synthesized according to published procedures. Elemental analysis, FAB(+) mass spectrometry and 1 H NMR results were consistent with the formulation TcO(ema)H. Infrared spectra showed a dramatic shift in the Tc = O stretch to 966 cm -1 , as distinct from 945 cm -1 in the original complex

  14. Intratumoral Administration of Holmium-166 Acetylacetonate Microspheres : Antitumor Efficacy and Feasibility of Multimodality Imaging in Renal Cancer

    NARCIS (Netherlands)

    Bult, Wouter; Kroeze, Stephanie G. C.; Elschot, Mattijs; Seevinck, Peter R.; Beekman, Freek J.; de Jong, Hugo W. A. M.; Uges, Donald R. A.; Kosterink, Jos G. W.; Luijten, Peter R.; Hennink, Wim E.; Schip, Alfred D. van Het; Bosch, J. L. H. Ruud; Nijsen, J. Frank W.; Jans, Judith J. M.

    2013-01-01

    Purpose: The increasing incidence of small renal tumors in an aging population with comorbidities has stimulated the development of minimally invasive treatments. This study aimed to assess the efficacy and demonstrate feasibility of multimodality imaging of intratumoral administration of

  15. A highly selective and sensitive Tb3+-acetylacetone photo probe for the assessment of acetazolamide in pharmaceutical and serum samples

    Science.gov (United States)

    Youssef, A. O.

    2018-04-01

    A novel, simple, sensitive and selective spectrofluorimetric method was developed for the determination of Acetazolamide in pharmaceutical tablets and serum samples using photo probe Tb3+-ACAC. The Acetazolamide can remarkably quench the luminescence intensity of Tb3+-ACAC complex in DMSO at pH 6.8 and λex = 350 nm. The quenching of luminescence intensity of Tb3+-ACAC complex especially the electrical band at λem = 545 nm is used for the assessment of Acetazolamide in the pharmaceutical tablet and serum samples. The dynamic range found for the determination of Acetazolamide concentration is 4.49 × 10-9-1.28 × 10-7 mol L-1, and the limit of detection (LOD) and limit of quantification (LOQ) are (4.0 × 10-9 and 1.21 × 10-8) mol L-1, respectively.

  16. Single-molecule magnetism in three related {Co(III)2Dy(III)2}-acetylacetonate complexes with multiple relaxation mechanisms.

    Science.gov (United States)

    Langley, Stuart K; Chilton, Nicholas F; Moubaraki, Boujemaa; Murray, Keith S

    2013-06-17

    Three new heterometallic complexes with formulas of [Dy(III)2Co(III)2(OMe)2(teaH)2(acac)4(NO3)2] (1), [Dy(III)2Co(III)2(OH)2(teaH)2(acac)4(NO3)2]·4H2O (2), and [Dy(III)2Co(III)2(OMe)2(mdea)2(acac)4(NO3)2] (3) were characterized by single-crystal X-ray diffraction and by dc and ac magnetic susceptibility measurements. All three complexes have an identical "butterfly"-type metallic core that consists of two Dy(III) ions occupying the "body" position and two diamagnetic low-spin Co(III) ions occupying the outer "wing-tips". Each complex displays single-molecule magnet (SMM) behavior in zero applied magnetic field, with thermally activated anisotropy barriers of 27, 28, and 38 K above 7.5 K for 1-3, respectively, as well as observing a temperature-independent mechanism of relaxation below 5 K for 1 and 2 and at 3 K for 3, indicating fast quantum tunneling of magnetization (QTM). A second, faster thermally activated relaxation mechanism may also be active under a zero applied dc field as derived from the Cole-Cole data. Interestingly, these complexes demonstrate further relaxation modes that are strongly dependent upon the application of a static dc magnetic field. Dilution experiments that were performed on 1, in the {Y(III)2Co(III)2} diamagnetic analog, show that the slow magnetic relaxation is of a single-ion origin, but it was found that the neighboring ion also plays an important role in the overall relaxation dynamics.

  17. Synthesis and characterization of tetraphenylporphyrinate of dysprosium route dysprosium acetylacetonate.; Sintesis y caracterizacion de un porfirinato de disprosio via acetilacetonato de disprosio.

    Energy Technology Data Exchange (ETDEWEB)

    Martinez M, V

    1993-12-31

    Dysprosium bis (tetraphenylporphyrinate) and bis (dysprosium) Tris (tetraphenylporphyrinate) were synthesized from dysprosium tetraphenylporphyrinate prepared in situ, and characterized by IR, UV-vis, TGA, DTA, EPR and magnetic susceptibility measurements. The double decker compound was obtained by direct oxidation of the HDy(TPP){sub 2} intermediate. The existence of the radical anion, (TPP){sup -} , in the double decker product was conformed by EPR spectrometry. Dysprosium monoporphyrinate was isolated and characterized by the same techniques. (Author).

  18. The Triruthenium Complex [{(acac)(2)Ru-II}(3)(L)] Containing a Conjugated Diquinoxaline[2,3-a : 2 '',3 ''-c]phenazine (L) Bridge and Acetylacetonate (acac) as Ancillary Ligands. Synthesis, Spectroelectrochemical and EPR Investigation

    Czech Academy of Sciences Publication Activity Database

    Patra, S.; Sarkar, B.; Ghumaan, S.; Fiedler, Jan; Kaim, W.; Lahiri, G. K.

    -, č. 5 (2004), s. 754-758 ISSN 1477-9226 R&D Projects: GA MŠk OC D14.20; GA MŠk OC D15.10 Institutional research plan: CEZ:AV0Z4040901 Keywords : nonlinear-optical properties * electrochemical properties * spectroelectrochemistry Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 2.926, year: 2004

  19. Thermal Co-Decomposition of Silver Acetylacetonate and Tin (II) Hexafluoroacetylacetonate: Formation of Carbonaceous Ag/AgxSn(x=4 and 6.7)/SnO2 Composites

    Czech Academy of Sciences Publication Activity Database

    Křenek, T.; Duchek, P.; Urbanová, Markéta; Pokorná, Dana; Bezdička, Petr; Jakubec, Ivo; Pola, M.; Čerstvý, R.; Kovářík, T.; Galíková, Anna; Pola, Josef

    2013-01-01

    Roč. 566, AUG 20 (2013), s. 92-99 ISSN 0040-6031 Grant - others:GA MŠK(CZ) CZ1.05/2.1.00/03.0088 Institutional support: RVO:67985858 ; RVO:61388980 Keywords : co-decomposition * thermal gravimetric analysis * Ag-Sn intermetallic compounds Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 2.105, year: 2013

  20. SYNTHESIS AND ANALYSIS OF La o.9 MnO 3 BY COMBUSTION ...

    African Journals Online (AJOL)

    The Lao.9MnO3 has been synthesized from lanthanum acetylacetonate, manganese acetylacetonate and urea by combustion method at 800oC. The analysis of the synthesized Lao.9MnO3 show it to be a semi-conducting nanopolycrystalline material having orthorhombic geometry with unit-cell parameters: a = 5.50335Ao; ...

  1. Controlling Metal/Ligand/Metal Oxidation State Combinations by Ancillary Ligand (L) Variation in the Redox Systems [L2Ru(.mu.boptz)RuL2]n, boptz=3, 6-bis(2-oxidophenyl)- 1,2,4,5 tetrazine and L=acetylacetonate, 2,2´-bipyridine, or 2-phenylazopyridine

    Czech Academy of Sciences Publication Activity Database

    Patra, S.; Sarkar, B.; Maji, S.; Fiedler, Jan; Urbanos, F. A.; Jimenez-Aparicio, R.; Kaim, W.; Lahiri, G. K.

    2006-01-01

    Roč. 12, č. 2 (2006), s. 489-498 ISSN 0947-6539 R&D Projects: GA AV ČR IAA400400505; GA MŠk LC510 Institutional research plan: CEZ:AV0Z40400503 Keywords : bridging ligands * EPR spectroscopy * magnetic properties * N,O ligands * ruthenium Subject RIV: CF - Physical ; The oretical Chemistry Impact factor: 5.015, year: 2006

  2. Isovalent and Mixed-Valent Diruthenium Complexes [(acac)(2)Ru-II (.mu.-bpytz)Ru-II(acac)(2)] and [(acac)(2)Ru-II(.mu.-bpytz)Ru-III(acac)(2)](ClO4) (acac= Acetylacetonate and bpytz=3,6-Bis(3,5-dimethylpyrazolyi)-1,2,4,5-tetrazine): Synthesis, Spectroelectrochemical, and EPR Investigation

    Czech Academy of Sciences Publication Activity Database

    Patra, S.; Sarkar, B.; Ghumaan, S.; Fiedler, Jan; Kaim, W.; Lahiri, G. K.

    2004-01-01

    Roč. 43, č. 19 (2004), s. 6108-6113 ISSN 0020-1669 R&D Projects: GA MŠk OC D15.10; GA MŠk OC D14.20 Institutional research plan: CEZ:AV0Z4040901 Keywords : electron-transfer * bridging ligand * ruthenium complexes Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 3.454, year: 2004

  3. One step synthesis of chlorine-free Pt/Nitrogen-doped graphene composite for oxygen reduction reaction

    KAUST Repository

    Varga, Tamá s; Varga, Á gnes Tí mea; Ballai, Gergő; Haspel, Henrik; Kukovecz, Á kos; Kó nya, Z.

    2018-01-01

    Chlorine-free Platinum/nitrogen-doped graphene oxygen reduction reaction catalysts were synthesized by a one step method of annealing a mixture of platinum acetylacetonate and graphene oxide under ammonia atmosphere. Nanoparticles with close

  4. SYNTHESIS, CHARACTERIZATION AND CRYSTAL STRUCTURES ...

    African Journals Online (AJOL)

    B. S. Chandravanshi

    ABSTRACT. Reaction of [VO(acac)2] (acac = acetylacetonate) with ... Single crystal X-ray structural studies indicate that the hydrazone ligands coordinate to ..... Molecular structure of complex (1) at 30% probability displacement. Figure 4.

  5. SYNTHESIS, CHARACTERIZATION AND CRYSTAL STRUCTURE ...

    African Journals Online (AJOL)

    Preferred Customer

    Reaction of [MoO2(acac)2] (where acac = acetylacetonate) with N'-(2-hydroxy-4- ... Single crystal X-ray structural studies indicate that the hydrazone ligand coordinates .... Molecular structure of the complex at 30% probability displacement.

  6. Association of coordination compounds of cobalt and molybdenum in solution

    Energy Technology Data Exchange (ETDEWEB)

    Kudryavtsev, A.B.; Sapunov, V.N. (Moskovskij Lesotekhnicheskij Inst. (USSR))

    1981-01-01

    Association of acetylacetonates Co(2) and MoO/sub 2/(6) in CHCl/sub 3/ is studied using the PMR method. In the absence of hydroxyl-containing substances the compounds form labile complex with the bond through molybdenyl oxygen. Equilibrium constant at 23 deg is equal to 2.2+-0.6 l/mol. Alcohol introduction results in partial dischelating of MoO/sub 2/(Acac)/sub 2/ and formation of mixed acetylacetonate-alcoholate complex of molybdenyl. Equilibrium constant of the reaction at 23 deg constitutes 0.14+-0.02 l/mol. Under the conditions Co(2) acetylacetonate is introduced into the first coordination sphere of MoO/sub 2/, the splitting off of the second acetylacetonate ligand and formation of strong associate which might condition the decrease of catalytic activity of mixed cobaltmolybdenum catalysts of epoxidation.

  7. Study of decomposition kinetics of volatile β-diketonates of yttrium, barium and copper in flow reactor

    International Nuclear Information System (INIS)

    Devyatykh, G.G.; Gavrishchuk, E.M.; Gibin, A.M.; Dadanov, A.Yu.; Dzyubenko, N.G.; Kaul', A.R.; Nichiporuk, R.V.; Snezhko, N.T.; Ul'yanov, A.A.

    1990-01-01

    Heterogeneous oxidative decomposition of adduct of yttrium acetylacetonate with o-phenanthroline, copper acetylacetonate and barium dipivaloylmethanate in a flow-type reactor was carried out. The basic kinetic characteristics of chemical precipitation processes of films of yttrium, copper and barium oxides, which are components of high-temperature superconductors, were obtained. The values of activation energy of precipitation process of yttrium, copper and barium oxides constituted 76±10, 108±15, 81±12 (t 600 deg C) respectively

  8. Selection and development of an easy to process electrolyte for decontamination by electropolishing

    International Nuclear Information System (INIS)

    Steringer, A.; Moser, T.

    1989-01-01

    Three different organic electrolytes: formic acid (E 1), oxalic acid (E 2) and acetylacetone (E 3) using potassium bromide (KBr) as the auxiliary electrolyte, were tested in the laboratory for electrochemically dissolving steel and stainless steel. The best results in the preliminary test series were attained with acetylacetone. It ranks among the first for current efficiency, with the produced acetylacetonates having the lowest solubility and thus they settle out of the solution in the form of coarse crystalline products. Tests were made on radioactive reactor components using acetylacetone in a 400 A test facility, to verify and optimize the decontamination factors, the electrolyte service life and the produced waste volume, as well as the respective process parameters. The surface activity of the components ranged from 2 to 10 Bq/cm 2 , and a decontamination factor of 30 was attained. The obtained specific waste volume is 1.1 litre/m 2 of decontaminated surface. A gamma-spectrometric evaluation revealed that the activity in the settled-out metallic acetylacetonate is five times higher than that in the electrolyte. It is only necessary to refill the spent acetylacetonate which makes it then possible to continue to use the electrolyte solution almost unrestrictedly

  9. Effect of Ni doping on the structural and magnetic properties of FePt nanoparticles

    International Nuclear Information System (INIS)

    Yang, H.-W.; Chung, C.-M.; Ding, Jack Y.

    2007-01-01

    A serial of FePtNi nanoparticles were investigated on their crystal structure and magnetic properties. The FePtNi nanoparticles were synthesized simultaneously by the reduction of iron (III) acetylacetonate, platinum (II) acetylacetonate and nickel (II) acetylacetonate with 1,2-hexadecanediol as the reducing agent. The X-ray diffraction patterns indicate that the addition of 8, 12, 17 at% Ni in FePt nanoparticles suppressed the transformation of the particles from disorder face-centered cubic to order face-centered tetragonal L1 0 -phase under annealing treatment. However, further increasing Ni contents to 21 at%, the nanoparticle transformed to L1 2 phase. Doping of Ni into the FePt compound system may decrease coercivity and crystal anisotropy energy. A maximum coercivity of 7 KOe at room temperature was obtained for (Fe 52 Pt 48 ) 92 Ni 8 nanoparticles after annealing at 600 deg. C for 30 min

  10. FEATURES OF INITIATION OF STYRENE POLYMERIZATION BY CUMENE HYDROPEROXIDE IN PRESENCE OF ACETULACETONATE OF COPPER(II

    Directory of Open Access Journals (Sweden)

    A. V. Grekova

    2016-04-01

    Full Text Available Kinetics of sectional styrene polymerization initiated by cumene hydroperoxide, acetylacetonate of copper(II and by the system of cumene hydroperoxide — acetylacetonate of copper(II in a temperature range 333-363 K is studied. Kinetic parameters of polymerization process are determined. It is shown, that system of cumene hydroperoxide — acetylacetonate of copper(II is in 5-6 times more effective on the initiating ability comparatively to application of its individual components. From findings ensues that decline of energy of activating of initiation from 110 kdzh/mol’ to 87 kdzh/mol’ for cumene hydroperoxide at the use of the studied system is caused with participating of monomer in preliminary complexation facilitating formation of free radicals.

  11. Surface defects on the Gd2Zr2O7 oxide films grown on textured NiW technical substrates by chemical solution method

    DEFF Research Database (Denmark)

    Zhao, Y.; Opata, Yuri Aparecido; Wu, W.

    2017-01-01

    by the reaction of zirconium acetylacetonate with propionic acid during the precursor synthesis. The regular-shaped regions were probably formed by large Gd[sbnd]Zr[sbnd]O frameworks with a metastable structure in the solution with limited aging time. This study demonstrates the importance of the precise control...

  12. Iodine sorption by microwave irradiated hydrotalcites

    Energy Technology Data Exchange (ETDEWEB)

    Paredes, S.P. [Universidad Autonoma de Puebla, Facultad de Ciencias Quimicas, C.P. 72570, Puebla, Pue (Mexico); Instituto Politecnico Nacional, ESIQIE, C.P. 07738, Mexico, D.F. (Mexico); Fetter, G. [Universidad Autonoma de Puebla, Facultad de Ciencias Quimicas, C.P. 72570, Puebla, Pue (Mexico)]. E-mail: geolarfetter@yahoo.com.mx; Bosch, P. [Universidad Nacional Autonoma de Mexico, Instituto de Investigaciones en Materiales, C.P. 04510, Mexico, D.F. (Mexico); Bulbulian, S. [Instituto Nacional de Investigaciones Nucleares, A.P. 18-1027, C.P. 11801, Mexico, D.F. (Mexico)

    2006-12-15

    Mg-Al hydrotalcite-like compounds (HT) were prepared by the microwave method on the one hand with ethoxide-acetylacetonate and on the other with acetylacetonate as precursors. They presented a maximum sorption capacity of 2.179 and 1.517 meq of {sup 131}I{sup -}/g of hydrotalcite respectively. When the hydrotalcites were calcined and rehydrated in a {sup 131}I{sup -} solution, iodine sorption decreased in both samples to 1.515 and 1.446, respectively. The corresponding value for nitrated hydrotalcite which was prepared by the conventional method for comparison purposes, was 0.570. The radionuclide content in hydrotalcites was determined by {gamma}-spectrometry. {sup 131}I{sup -} sorption is dependent on two main parameters: one is the type of the interlayer organic material and the second the surface area. It was found that hydrotalcites prepared with ethoxide-acetylacetonate were better sorbents for {sup 131}I{sup -} than those with acetylacetonate. Still, if the specific surface area increased, {sup 131}I{sup -}sorption increased as well; nitrated HT resulted in low specific surface area and a low sorption capacity. It is, therefore, concluded that organic residues present in the samples prepared by the microwave method favor the sorption of radioactive anions, in particular {sup 131}I{sup -} if compared with nitrated and/or carbonate interlayered hydrotalcites.

  13. The enantioselective total synthesis of (+)-clusianone.

    Science.gov (United States)

    Horeischi, Fiene; Guttroff, Claudia; Plietker, Bernd

    2015-02-11

    (+)-Clusianone, an exo-type B PPAP with reported anti-HIV and chemoprotective activities, was synthesized in eleven steps with 97% ee starting from acetylacetone. An enantioselective decarboxylative Tsuji-Trost-allylation and a Ru-catalyzed ring-closing metathesis-decarboxylative allylation were used to control both diastereo- and enantioselectivity.

  14. A K Tyagi

    Indian Academy of Sciences (India)

    Home; Journals; Bulletin of Materials Science. A K Tyagi. Articles written in Bulletin of Materials Science. Volume 25 Issue 2 April 2002 pp 163-168 Thin Films. Carbonaceous alumina films deposited by MOCVD from aluminium acetylacetonate: a spectroscopic ellipsometry study · M P Singh G Raghavan A K Tyagi S A ...

  15. Thermodynamic modeling to analyse composition of carbonaceous ...

    Indian Academy of Sciences (India)

    Equilibrium thermodynamic analysis has been applied to the low-pressure MOCVD process using manganese acetylacetonate as the precursor. ``CVD phase stability diagrams” have been constructed separately for the processes carried out in argon and oxygen ambient, depicting the compositions of the resulting films as ...

  16. A facile route to inverted polymer solar cells using a precursor based zinc oxide electron transport layer

    NARCIS (Netherlands)

    Bruyn, P. de; Moet, D.J.D.; Blom, P.W.M.

    2010-01-01

    Inverted polymer:fullerene solar cells with ZnO and MoO3 transport layers are demonstrated. ZnO films are prepared through spin casting of a zinc acetylacetonate hydrate solution, followed by low temperature annealing under ambient conditions. The performance of solar cells with an inverted

  17. Beckmann rearrangement of aldoximes catalyzed by transition metal salts: mechanical aspects

    NARCIS (Netherlands)

    Leusink, A.J.; Meerbeek, T.G.; Noltes, J.G.

    1977-01-01

    The Beckmann rearrangement of aldoximes catalyzed by transition metal salts like palladium and nickel acetylacetonates is shown to be a dehydration‐hydration reaction in which the anti‐oxime is converted into nitrile and the nitrile is converted into amide.

  18. Journal of Chemical Sciences | Indian Academy of Sciences

    Indian Academy of Sciences (India)

    Synthesis, characterisation and electrochemical behaviour of Cu(II), Co(II), Ni(II) and Zn(II) complexes derived from acetylacetone and p-anisidine and their antimicrobial activity · N Raman V Muthuraj S Ravichandran A Kulandaisamy · More Details Abstract Fulltext PDF. Neutral tetradentate N2O2 type complexes of Cu(II), ...

  19. Synthesis, characterisation and electrochemical behaviour of Cu(II)

    Indian Academy of Sciences (India)

    Neutral tetradentate N2O2 type complexes of Cu(II), Ni(II), Co(II) and Zn(II) have been synthesised using the Schiff base formed by the condensation of acetylacetone and p-anisidine. Microanalysis, molar conductance, magnetic susceptibility, IR, UV-Vis, 1H NMR, CV and EPR studies have been carried out to determine the ...

  20. Synthesis and characterization of alumina-supported vanadium oxide catalysts prepared by the molecular designed dispersion of VO(acac)2 complexes

    NARCIS (Netherlands)

    Weckhuysen, B.M.; Baltes, M.; Voort, P. van der; Ramachandra Rao, R.; Catana, Gabriela; Schoonheydt, R.A.; Vansant, E.F.

    2000-01-01

    Alumina-supported vanadium oxide catalysts have been prepared by the molecular designed dispersion method, using the vanadyl acetylacetonate complex (VO(acac)2). The complex has been adsorbed on the support from solution, followed by thermal conversion into the corresponding supported vanadium oxide

  1. Optimization of process conditions for the production of TiO2–xNy ...

    Indian Academy of Sciences (India)

    Home; Journals; Bulletin of Materials Science; Volume 37; Issue 6 ... Based on the results in preliminary experiments, we selected molar ratio of surfactant to Ti, molar ratio of acetylacetone to Ti, molar ratio of water to Ti and calcination temperature as the key process factors affecting the roughness of TiO2–N film.

  2. Journal of Chemical Sciences | Indian Academy of Sciences

    Indian Academy of Sciences (India)

    Thiophene-substituted chalcones were cyclised with guanidine in the presence of potassium hydroxide to get 4-substituted-6-thiophenopyrimidines 2a-e which were then refluxed with acetylacetone to obtain pyrimidopyrimidines 3a-e. Compounds 2a-e were also refluxed with ethylacetoacetate to afford ...

  3. S A Shivashankar

    Indian Academy of Sciences (India)

    Home; Journals; Bulletin of Materials Science. S A Shivashankar. Articles written in Bulletin of Materials Science. Volume 25 Issue 2 April 2002 pp 163-168 Thin Films. Carbonaceous alumina films deposited by MOCVD from aluminium acetylacetonate: a spectroscopic ellipsometry study · M P Singh G Raghavan A K Tyagi ...

  4. Luminescent thin films by the chemical aerosol deposition technology (CADT)

    NARCIS (Netherlands)

    Martin, F.J.; Martin, F.J.; Albers, H.; Lambeck, Paul; Popma, T.J.A.; van de Velde, G.M.H.

    1992-01-01

    Zinc sulphide thin films have been deposited with CART using zinc chlorideand zinc acetylacetonate as Zn compounds and thiourea and 1,1,3,3-tetramethylthiourea as S compounds soluted in methanol, ethanol, isopropanol and cellosolve. After optimalization of the deposition process homogeneous layers

  5. Untitled

    Indian Academy of Sciences (India)

    . (II) acetylacetonate does so not only through the co-ordinating carbonyl groups, but through the two co-ordinated polar water molecules also. The faster migration of cobalt (III) and diffusive and slower migration of cobalt (II) can be accounted ...

  6. Rare earth [beta]-diketonate and carboxylate metal complexes as precursors for MOCVD of oxide films

    Energy Technology Data Exchange (ETDEWEB)

    Kuzmina, N.P. (Dept. of Chemistry, Moscow State Univ. (Russian Federation)); Martynenko, L.I. (Dept. of Chemistry, Moscow State Univ. (Russian Federation)); Tu, Z.A. (Dept. of Chemistry, Moscow State Univ. (Russian Federation)); Kaul, A.R. (Dept. of Chemistry, Moscow State Univ. (Russian Federation)); Girichev, G.V. (Dept. of Chemistry, Moscow State Univ. (Russian Federation)); Giricheva, N.I. (Dept. of Chemistry, Moscow State Univ. (Russian Federation)); Rykov, A.N. (Dept. of Chemistry, Moscow State Univ. (Russian Federation)); Korenev, Y.M. (Dept. of Chemistry, Moscow State Univ. (Russian Federation))

    1993-08-01

    Volatile and thermostable complexes of lanthanide acetylacetonates and pivalates were obtained and investigated by different methods. These compounds were used for lanthanide oxide containing film producing and for fabrication of silica optical fibers doped by lanthanide oxide. The properties of these and already known volatile precursors are compared. (orig.).

  7. Rare earth β-diketonate and carboxylate metal complexes as precursors for MOCVD of oxide films

    International Nuclear Information System (INIS)

    Kuzmina, N.P.; Martynenko, L.I.; Tu, Z.A.; Kaul, A.R.; Girichev, G.V.; Giricheva, N.I.; Rykov, A.N.; Korenev, Y.M.

    1993-01-01

    Volatile and thermostable complexes of lanthanide acetylacetonates and pivalates were obtained and investigated by different methods. These compounds were used for lanthanide oxide containing film producing and for fabrication of silica optical fibers doped by lanthanide oxide. The properties of these and already known volatile precursors are compared. (orig.)

  8. A facile route to inverted polymer solar cells using a precursor based zinc oxide electron transport layer

    NARCIS (Netherlands)

    de Bruyn, P.; Moet, D. J. D.; Blom, P. W. M.

    Inverted polymer: fullerene solar cells with ZnO and MoO(3) transport layers are demonstrated. ZnO films are prepared through spin casting of a zinc acetylacetonate hydrate solution, followed by low temperature annealing under ambient conditions. The performance of solar cells with an inverted

  9. Kinetic stability of the dysprosium(3) complex with tetraazaporphine in acetic acid-water and acetic acid-methanol mixtures

    International Nuclear Information System (INIS)

    Khelevina, O.G.; Vojnov, A.A.

    1999-01-01

    Water-soluble dysprosium tetraazaporphine with acetylacetonate-ion as extraligand is synthesized for the first time. Its kinetic stability in acetic acid solutions is investigated. It is shown that the complex is dissociated with formation of free tetraazaporphine. Kinetic parameters of dissociation reaction are determined [ru

  10. Journal of Chemical Sciences | Indian Academy of Sciences

    Indian Academy of Sciences (India)

    A novel, magnetically recoverable nanocatalyst is fabricated through simple immobilization of copper(II) acetylacetonate on the surface of amine-terminated silica-coated Fe3O4 nanoparticles: Cu(acac)2/NH2-T/SiO2@Fe3O4NPs. Unambiguous bonding of Cu to the terminal amine is indicated by Xray photoelectron ...

  11. Three Component Synthesis of Substituted 4H-[1,3]Dioxin Derivatives Under Solvent-Free Conditions

    Directory of Open Access Journals (Sweden)

    Mohammad Reza Hosseini-Tabatabaei

    2012-01-01

    Full Text Available Reaction between aryl aldehydes, acetylacetone and alkyl isocyanides in solvent-free conditions provided a simple and efficient one-pot route for the synthesis of 1-(2-alkylamino-6-methyl-4-aryl-4H-[1,3]dioxin-5-ylethanone derivatives in excellent yields.

  12. Self-assembly of a constitutional dynamic library of Cu(II) coordination polygons and reversible sorting by crystallization.

    Science.gov (United States)

    Rancan, Marzio; Tessarolo, Jacopo; Zanonato, Pier Luigi; Seraglia, Roberta; Quici, Silvio; Armelao, Lidia

    2013-06-07

    A small coordination constitutional dynamic library (CDL) is self-assembled from Cu(2+) ions and the ortho bis-(3-acetylacetone)benzene ligand. Two coordination polygons, a rhomboid and a triangle, establish a dynamic equilibrium. Quantitative sorting of the rhomboidal polygon is reversibly obtained by crystallization. Thermodynamic and kinetic aspects ruling the CDL system have been elucidated.

  13. Studies on the promotion of nickel—alumina coprecipitated catalysts: I. Titanium oxide

    NARCIS (Netherlands)

    Lansink Rotgerink, H.G.J.; Mercera, P.D.L.; van Ommen, J.G.; Ross, J.R.H.

    1988-01-01

    A series of TiO2-promoted nickel—alumina catalysts has been prepared and characterized. The promoter was added in various proportions to a calcined coprecipitated nickel—alumina material by adsorption of the acetylacetonate complex of titanium, followed by further calcination and reduction. The

  14. Cytocompatibility of aliphatic polyesters - in vitro study on fibroblasts and macrophages

    NARCIS (Netherlands)

    Pamula, E.; Dobrzynski, P.; Szot, B.; Kretek, M.; Krawciow, M.; Plytycz, B.; Chadzinska, M.K.

    2008-01-01

    A resorbable copolymer of glycolide and L-lactide (PGLA), a terpolymer of glycolide, L-lactide, and epsilon-caprolactone (PGLCL), and a copolymer of glycolide and E-caprolactone (PGCL) were synthesized by ring opening polymerization Using Zirconium acetylacetonate (Zr(acac)(4)) as an initiator. The

  15. Hydration of metal β-diketonates and its influence on partition equilibria in solvent extraction

    International Nuclear Information System (INIS)

    Narbutt, J.

    1991-01-01

    Studies are reported on the thermodynamics of liquid-liquid partition of beryllium, zinc, chromium and cobalt(3) chelates with acetylacetone, its C 6 and C 7 homologues, and monothioacetylacetone in the system water/aliphatic hydrocarbon. 117 refs., 11 figs., 8 tabs. (author)

  16. Analysis of carrier-free radioisotopes by paper chromatography

    Energy Technology Data Exchange (ETDEWEB)

    Ishibashi, M; Shigemetsu, T; Ishida, T

    1954-01-01

    Rf values of Ru-Rh, Zr, Nb, Y, Ce-Pr, I, Ca, and Sr, are listed. Zr and Nb were separable only when they were developed with mandelic acid of pH 5.2 and 7.9. Elements of the Ce group seemed to be separated when developed with acetylacetone-BuOH.

  17. Synthesis, characterization and antimicrobial activities of a Schiff ...

    African Journals Online (AJOL)

    Complexes of Cu(II), Ni(II) and Mn(II) with a Schiff base derived from condensation reaction of phenylalanine and acetylacetone have been synthesized and characterized analytically and spectroscopically. Melting point of the Schiff base was 188oC and the complexes decompose within a temperature range of 210-242oC.

  18. Antibacterial and antioxidant properties of macrocyclic Schiff bases ...

    African Journals Online (AJOL)

    CLEMENT O BEWAJI

    Electronic spectra of the compounds were recorded on a digital spectrophotometer. ... Acetylacetone in ethanol with the solutions of Semicarbazide hydrochloride in hot water ... pre-incubated for 1 h at room temperature and incubated at 37°C for 24 h.8 Ofloxacin was used as standard. 2.4 Scavenging of nitric oxide. Sodium ...

  19. Structure of alumina supported vanadia catalysts for oxidative dehydrogenation of propane prepared by flame spray pyrolysis

    DEFF Research Database (Denmark)

    Høj, Martin; Jensen, Anker Degn; Grunwaldt, Jan-Dierk

    2013-01-01

    .%. The catalysts were subsequently characterized by BET surface area, X-ray diffraction (XRD), Raman, UV–vis diffuse reflectance and X-ray absorption spectroscopy (XAS) as well as measurement of the catalytic performance. The catalysts had specific surface areas from 143 to 169 m2/g corresponding to average......A series of five vanadia on alumina catalysts for oxidative dehydrogenation of propane to propene were synthesized by flame spray pyrolysis (FSP) using vanadium(III)acetylacetonate and aluminium(III)acetylacetonate dissolved in toluene as precursors. The vanadium loading was 2, 3, 5, 7.5 and 10wt...... X-ray absorption near edge structure (XANES) spectroscopy showed that the vanadia can be reduced when operating at low oxygen concentrations. The catalyst performance was determined in fixed bed reactors with an inlet gas composition of C3H8/O2/N2=5/25/70. The main products were propene, CO and CO2...

  20. Chemical modification of chitosan in the absence of solvent for diclofenac sodium removal: pH and kinetics studies

    Energy Technology Data Exchange (ETDEWEB)

    Pereira, Kerlaine Alexandre Araujo; Osorio, Luizangela Reis; Silva, Marcos Pereira; Silva Filho, Edson Cavalcanti da, E-mail: edsonfilho@ufpi.edu.br [Universidade Federal do Piaui (UFPI/CCN), Teresina, PI (Brazil). Centro de Ciencias da Natureza. Lab. Interdisciplinar de Materiais Avancados; Sousa, Kaline Soares [Universidade Federal da Paraiba (UFPB/CCEN), Joao Pessoa, PB (Brazil). Centro de Ciencias Exatas e da Natureza. Dept. de Quimica

    2014-08-15

    Chitosan was modified with acetylacetone and ethylenediamine in the absence of solvent. The new biopolymer obtained from the modification was characterized by elemental analysis and NMR 13C and applied in the removal of diclofenac sodium aqueous solution varying the pH and time. Through elemental analysis was possible to verify a decreasing in C/N relation after reaction with acetylacetone and an increasing after modification with ethylenediamine. From NMR analysis was verified the appearance of peaks around 160-210 ppm in both materials due to free carbonyl groups in the first step of the modification, besides the formation of imine bonds. The adsorption tests showed that the highest value occurred at pH 4 and from the results of the kinetic study was found that maximum adsorption occurred within 45 minutes and experimental data adjusted better to linear adjustment, following pseudo second-order model. The results show a material efficient in the removal of emerging pollutants. (author)

  1. Monodisperse gold-palladium alloy nanoparticles and their composition-controlled catalysis in formic acid dehydrogenation under mild conditions.

    Science.gov (United States)

    Metin, Önder; Sun, Xiaolian; Sun, Shouheng

    2013-02-07

    Monodisperse 4 nm AuPd alloy nanoparticles with controlled composition were synthesized by co-reduction of hydrogen tetrachloroaurate(III) hydrate and palladium(II) acetylacetonate with a borane-morpholine complex in oleylamine. These NPs showed high activity (TOF = 230 h(-1)) and stability in catalyzing formic acid dehydrogenation and hydrogen production in water at 50 °C without any additives.

  2. Laser-induced chemical liquid deposition of discontinuous and continuous copper films

    Czech Academy of Sciences Publication Activity Database

    Ouchi, A.; Bastl, Zdeněk; Boháček, Jaroslav; Šubrt, Jan; Pola, Josef

    2007-01-01

    Roč. 201, č. 8 (2007), s. 4728-4733 ISSN 0257-8972 R&D Projects: GA AV ČR 1ET400400413 Institutional research plan: CEZ:AV0Z40400503; CEZ:AV0Z40320502; CEZ:AV0Z40720504 Keywords : copper films * laser photolysis * Cu(II) acetylacetonate * chemical liquid deposition Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 1.678, year: 2007

  3. Ultraviolet curing of acrylated liquid natural rubber for surface coating application

    OpenAIRE

    Kannikar Kwanming; Pairote Klinpituksa; Wae-asae Waehamad

    2009-01-01

    Ultraviolet curable acrylated liquid natural rubber was prepared by grafting of photosensitive molecule onto liquid natural rubber for surface coating application. The liquid natural rubber (LNR) was firstly obtained by degradation of natural rubber latex with hydrogen peroxide and cobalt acetylacetonate at 65oC for 72 hrs. The preparation of acrylated natural rubber was carried out by the reaction of acrylic acid and epoxidized liquid natural rubber (ELNR) prior obtained from LNR with formic...

  4. UV Laser Photolytic Solution Deposition of α-Fe/Polyoxocarbosilane/Carbon Nanocomposite and Evolution to α-Fe2O3/Polyoxocarbosilane/Carbon Nanocomposite

    Czech Academy of Sciences Publication Activity Database

    Pola, Josef; Maryško, Miroslav; Vorlíček, Vladimír; Bakardjieva, Snejana; Šubrt, Jan; Bastl, Zdeněk; Ouchi, A.

    2008-01-01

    Roč. 199, 2-3 (2008), s. 156-164 ISSN 1010-6030 R&D Projects: GA AV ČR IAA400720619 Institutional research plan: CEZ:AV0Z40720504; CEZ:AV0Z10100521; CEZ:AV0Z40320502; CEZ:AV0Z40400503 Keywords : Fe(II) acetylacetonate * Fe composite * laser solution deposition Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 2.362, year: 2008

  5. Lanthanide complexes with pivaloylacetone

    International Nuclear Information System (INIS)

    Eliseeva, S.V.; Chugarov, N.V.; Kuz'mina, N.P.; Martynenko, L.I.; Nichiporuk, R.V.; Ivanov, S.A.

    2003-01-01

    Complexes Ln(pa) 3 ·2H 2 O (Ln=La, Gd, Lu, Hpa - pivaloylacetone) are synthesized and investigated by the methods of element, IR spectroscopic and thermal analyses. Behaviour of the complexes during heating in vacuum is compared with such one for acetylacetonates and dipivaloylmethanates. Structure of the complexes in solution is studied by 1 H NMR and MALDI-MS [ru

  6. Investigation of adducts of tris-(acetylacetonato)lanthanides with o-phenanthroline and α,α'-dipyridyl by mass spectroscopy

    International Nuclear Information System (INIS)

    Gavrishchuk, E.M.; Dzyubenko, N.G.; Martynenko, L.I.

    1984-01-01

    Mass spectra of adducts of tris-acetylacetonates of REE (REE, Ln, M) with O-phenanthroline (Phen) and α, α 1 -dipyridyl (Dipy) are obtained. A scheme of fragmentation is suggested. Peculiarities of dissociative ionization processes for samarium-, europium-thulium-, and ytterbium compounds are shown to be determined by a possibility of changing the oxidation state of a central ion. Energy characteristics of separation of the first and second ligands of compleXes in the entire REE series are compared

  7. Separation of beryllium and mercury from lithium chloride solution by gaseous extraction

    International Nuclear Information System (INIS)

    Sevast'yanov, A.I.; Chepovol, V.I.

    1989-01-01

    The possibility is shown of extracting beryllium and mercury by acetylacetone (HAA) from lithium chloride solution by passing argon through the solution and the optimum conditions have been determined. The dependence of the degree of extraction and the distribution coefficients on various parameters of the liquid phase are presented, viz. the initial pH value, the lithium chloride concentration, and the initial HAA content

  8. Catalytic Synthesis and Antifungal Activity of New Polychlorinated Natural Terpenes

    Directory of Open Access Journals (Sweden)

    Hana Ighachane

    2017-01-01

    Full Text Available Various unsaturated natural terpenes were selectively converted to the corresponding polychlorinated products in good yields using iron acetylacetonate in combination with nucleophilic cocatalyst. The synthesized compounds were evaluated for their in vitro antifungal activity. The antifungal bioassays showed that 2c and 2d possessed significant antifungal activity against Fusarium oxysporum f. sp. albedinis (Foa, Fusarium oxysporum f. sp. canariensis (Foc, and Verticillium dahliae (Vd.

  9. Relaxation effects in ferrous complexes

    International Nuclear Information System (INIS)

    Nicolini, C.; Mathieu, J.P.; Chappert, J.

    1976-01-01

    The slow relaxation mechanism of the Fe 2+ ion in the tri-fluorinated TF(acac) and hexafluorinated HF(acac) complexes of Fe(II) acetylacetonate was investigated. The 300K and 77K Moessbauer spectra for TF(acac) consist in a slightly asymmetric quadrupole doublet. On the contrary, at 4.2K the higher energy line is strongly widened; that is typical of a slowing down in the electron relaxation frequency [fr

  10. Synthesis of Polyfunctionalized 4H-Pyrans

    Directory of Open Access Journals (Sweden)

    Manisha Bihani

    2013-01-01

    Full Text Available Amberlyst A21 catalyzed one-pot three-component coupling of aldehyde and malononitrile with active methylene compounds such as acetylacetone and ethyl acetoacetate for the synthesis of pharmaceutically important polyfunctionalized 4H-pyrans has been reported. Simple experimental procedure, no chromatographic purification, no hazardous organic solvents, easy recovery and reusability of the catalyst, and room temperature reaction conditions are some of the highlights of this protocol for the synthesis of pharmaceutically relevant focused libraries.

  11. New data on the reaction of 1,4-bifunctional derivatives of hydrazine with 1,3-diketones

    International Nuclear Information System (INIS)

    Zelenin, K.N.; Solod, O.V.; Tomchin, A.B.

    1987-01-01

    As a function of the conditions of the reaction and the structure of the reagents, mono- and bis-adducts of different structure - 5-hydroxy- and 5-hydrazino-2-pyrazolines, mono- and bis(hydrazones), and the corresponding pyrazoles - are formed in the reaction of hydrazine derivatives - aminoguanidine nitrate, 4-phenylsemicarbazide, amidrazonium iodides, and some thiosemicarbazides - with acetylacetone and dibenzoylmethane. The conditions of the formation of these products and the features of their structure were examined

  12. Infrared spectroscopy of some organocobalt (III) compounds

    International Nuclear Information System (INIS)

    Benedetti, A.V.; Mauro, A.E.

    1982-01-01

    The compounds [MeCo(DH) 2 py], [MeCo(DH) 2 H 2 O] (M = methyl; DH = dimethyl-glyoxymate; py = pyridine) and others of general formulae [Co(L)(H 2 O) 2 ] ClO 4 , where L = SALOPHEN = bis (salicylaldehyde)-o-phenylenediimine; SALCN = 1,2-bis (salicylaldehyde) cyclohexylenediimine; SALEN = bis (salicylaldehyde) ethylenediimine; BAE = bis (acetylacetone)-ethylenediimine were synthesized and studied by infrared spectroscopy. The frequencies observed have been assigned to specific group vibrations. (Author) [pt

  13. Preparation of molybdenum oxide thin films by MOCVD

    International Nuclear Information System (INIS)

    Guerrero, R. Martinez; Garcia, J.R. Vargas; Santes, V.; Gomez, E.

    2007-01-01

    In this study, molybdenum oxide films were prepared in a horizontal hot-wall MOCVD apparatus using molybdenum dioxide acetylacetonate as precursor. The molybdenum precursor was synthesized from acetylacetone and molybdenum oxide powder. Thermal gravimetric (TG) and differential thermal analyses (DTA) of the precursor suggested the formation of molybdenum oxides around 430 o C (703 K). Thus, a range of deposition temperatures varying from 350 to 630 o C (623-903 K) was explored to investigate the effects on the nature of the molybdenum oxide films. X-ray diffraction (XRD) results showed that the films consisted of α-MoO 3 phase at deposition temperatures ranging from 400 to 560 o C (673-833 K). Crystalline α-MoO 3 films can be obtained from molybdenum dioxide acetylacetonate precursor, without need of a post-annealing treatment. The best crystalline quality was found in films having needle-like crystallites grown at deposition temperature of about 560 o C (833 K), which exhibit a strong (0 1 0) preferred orientation and a transparent visual appearance

  14. Preparation of molybdenum oxide thin films by MOCVD

    Energy Technology Data Exchange (ETDEWEB)

    Guerrero, R. Martinez [Depto. de Ingenieria Metalurgica, ESIQIE-IPN, Mexico 07300, D.F. (Mexico); Garcia, J.R. Vargas [Depto. de Ingenieria Metalurgica, ESIQIE-IPN, Mexico 07300, D.F. (Mexico)]. E-mail: rvargasga@ipn.mx; Santes, V. [CIIEMAD-IPN, Miguel Othon de Mendizabal 485, Mexico 07700, D.F. (Mexico); Gomez, E. [Instituto de Quimica-UNAM, Circuito Exterior-Ciudad Universitaria, Mexico 04510, D.F. (Mexico)

    2007-05-31

    In this study, molybdenum oxide films were prepared in a horizontal hot-wall MOCVD apparatus using molybdenum dioxide acetylacetonate as precursor. The molybdenum precursor was synthesized from acetylacetone and molybdenum oxide powder. Thermal gravimetric (TG) and differential thermal analyses (DTA) of the precursor suggested the formation of molybdenum oxides around 430 {sup o}C (703 K). Thus, a range of deposition temperatures varying from 350 to 630 {sup o}C (623-903 K) was explored to investigate the effects on the nature of the molybdenum oxide films. X-ray diffraction (XRD) results showed that the films consisted of {alpha}-MoO{sub 3} phase at deposition temperatures ranging from 400 to 560 {sup o}C (673-833 K). Crystalline {alpha}-MoO{sub 3} films can be obtained from molybdenum dioxide acetylacetonate precursor, without need of a post-annealing treatment. The best crystalline quality was found in films having needle-like crystallites grown at deposition temperature of about 560 {sup o}C (833 K), which exhibit a strong (0 1 0) preferred orientation and a transparent visual appearance.

  15. Preparation of transparent sol-gel films containing europium, terbium, and ytterbium cations from 4-(3'-triethoxysilylpropylimino)pent-2-en-2-ol

    International Nuclear Information System (INIS)

    Semenov, V.V.; Cherepennikova, N.F.; Kuznetsova, O.V.; Melenskova, N.V.; Bushuk, B.A.; Bushuk, S.B.; Kal'vinkovskaya, Yu.A.; Duglas, V.E.

    2007-01-01

    A reaction of 3-aminopropyl(triethoxy)silane with acetylacetone gave a mixture of two isomeric carbon-functionalized organosilicon compounds capable of complexation and sol-gel polymerization. These were 4-(3'-triethoxysilylpropylimino)pent-2-en-2-ol (EtO) 3 Si-CH 2 CH 2 CH 2 -N=C(Me)CH=C(Me)OH (Ia, 83%) and 4-(3'-triethoxysilylpropylamino)pent-3-en-2-one (EtO) 3 Si-CH 2 CH 2 CH 2 -NH-C(Me)=CH-C(O)Me (Ib, 17%). With acetylacetone trimethylsilyl ether instead of acetylacetone itself, compound Ia and silylated derivatives (Me 3 SiO) n (EtO) 3-n Si-CH 2 CH 2 CH 2 -N=C(Me)CH=C(Me)OH were obtained as admixture in 84 and 16% yields, respectively. Reactions of ligands Ia and Ib with europium and terbium propan-2-olates afforded the corresponding complexes. Formulations of lanthanide complexes, oligodimethylsiloxanediols, and 3-aminopropyl(triethoxy)silane were used to prepare transparent sol-gel films. The photoluminescence spectra of the films show narrow bands due to Eu 3+ or Tb 3+ emission. Emission from the organosilicon matrix appears as a broad band at 430 to 435 nm [ru

  16. Development of 99Tcm-Q3 as a new type myocardial perfusion imaging agent

    International Nuclear Information System (INIS)

    Li Yunchun; Tan Tianzhi; Fan Chengzhong; Zhao Keqing; Wei Xihe; Li Quan

    1999-01-01

    Objective: To develop 99 Tc m -N,N'-ethylene-bis (acetylacetone iminato) bis [tris (3-methoxy-1-propyl) phosphine] ( 99 Tc m -Q 3 ) as a new type of myocardial perfusion imaging agent. Methods: After N,N'-ethylene-bis (acetylacetone iminato) and tris (3-methoxy-1-propyl) phosphine were made, N,N'-ethylene-bis (acetylacetone iminato) was labelled using reduced 99 Tc m O 4 - by SnCl 2 ·2H 2 O under the presence of alkali, then tris (3-methoxy-1-propyl) phosphine was added and reacted for ten minutes, 99 Tc m -Q 3 was obtained at the end. Biodistribution in mice, in vitro stability and acute toxicity of 99 Tc m -Q 3 were examined. Results: 99 Tc m -Q 3 was taken up rapidly by the heart, and the uptake rate was very high, by 5 minutes post injection, 24.66% of the injected dose was taken up in per gram heart, and no significant washout was shown up by 4 hours. But 99 Tc m -Q 3 was cleaned out rapidly from blood, lung and liver. No poisonousness and adverse effects were observed, and its stability lasted more than 6 hours. Conclusions: 99 Tc m -Q 3 is a fairly good myocardial perfusion imaging agent for improving the quality of myocardial perfusion imaging

  17. Characterization of microstructure and catalytic of cerium oxide obtained by colloidal solution

    International Nuclear Information System (INIS)

    Senisse, C.A.L.; Bergmann, C.P.; Alves, A.K.

    2012-01-01

    This study investigated to obtain particles of cerium oxide, for use as catalysts for the combustion of methane using the technique of through polymeric colloidal solution. Obtaining the colloidal system is based on hydrolysis of salts such as cerium acetylacetonate, cerium nitrate in the presence of additives such as polyvinylbutyral (PVB), polyvinylpyrrolidone (PVP) and polyvinyl acetate (PVA), at concentrations of 5, 10 and 15% in aqueous or alcoholic medium. These solutions containing ions of interest were subjected to a heat treatment at 650° C for 30 minutes, with heating rate of 2 ° C/ min. After heat treatment, the fibers were characterized according to their morphology, surface area, crystallinity, weight loss and catalytic activity. Samples obtained from cerium acetylacetonate were more reactive than the cerium nitrate to the combustion of methane, as showed greater conversions and higher temperatures reached during the process, which is of utmost importance since the combustion catalytic methane is used for generating thermal energy. After the reaction with methane, the samples underwent significant change in surface area, probably due to the intensity of combustion reactions of the nitrate and the generation of heat involved in this reaction, which gave rise to coarse particles. During the combustion process using the obtained from particles of cerium acetylacetonate, there was the release of large quantities of nitrogen compared to the results of assays with the particles obtained with cerium nitrate. (author)

  18. High-Performance Solution-Processed Amorphous InGaZnO Thin Film Transistors with a Metal–Organic Decomposition Method

    Directory of Open Access Journals (Sweden)

    Yingtao Xie

    2018-01-01

    Full Text Available A facile solution process was introduced for the preparation of IGZO thin films via a metal–organic decomposition (MOD method. The IGZO ink was synthesized by mixing the solutions of gallium acetylacetonate [Ga(C5H7O23], zinc acetylacetonate hydrate [Zn(C5H7O22·xH2O] dissolved in ethanol, and indium acetylacetonate [In(C5H7O23] dissolved in tetrahydrofuran (THF. The deposited films by spin-coating were annealed at moderate process temperature (≤500°C. The relationship between device performance and postannealing temperature was studied. The result demonstrated that mobility of IGZO TFT increased as the annealing temperature increased. Based on the analysis of O 1s statement, the annealing temperature can influence the number of oxygen vacancy to further affect the carrier centration. In addition, the IGZO TFT devices with various Ga molar ratios were compared to demonstrate the influence of the Ga addition. The result demonstrated that the saturated mobilities (μe decreased and VTH shifted to positive voltage as the Ga molar ratio was increased. It is likely that Ga can offer stronger chemical bonds between metal and oxygen that reduced the concentration of free carriers and thus help reducing VTH. As a result, the optimized performance of IGZO TFT with the mobility of 3.4 cm2V−1s−1 showed the MOD process was a promising approach.

  19. Comparative evaluation of red cell-labelling parameters of three lipid-soluble 111-In-chelates: Effect of lipid solubility on membrane incorporation and stability constant on transchelation

    International Nuclear Information System (INIS)

    Rao, S.A.; Dewanjee, M.K.

    1982-01-01

    A rabbit red cell model was used to determined the cell labeling properties of three lipid-soluble 111 In-complexes: 111 In-oxine, 111 In-acetylacetone, and 111 In-tropolone. Partition coefficients (olive oil/buffer) were measured to determine the lipid solubility and were 3.54, 7.93, and 18.18 for 111 In-oxine, 111 In-acetylacetone, and 111 In-tropolone respectively. The effect of the concentration of these three chelating agents on labeling efficiencies was studied. The factors influencing the labeling efficiencies of these complexes such as cell density, time of incubation, influence of temperature, pH, effect of plasma proteins, and citrate ion concentration in the cell-labeling medium were studied. Labeling yields as high as 95.15 +- 4.15% were achieved with 111 In-tropolone after a 10-min incubation at 37 0 C. The optimum pH for cell labeling was 6.5 Excess critrate ion (> 3.02 mg/ml) and small amounts of plasma proteins (> 10 μl/ml) decreased the labeling efficiencies in all three cases. Distribution of these 111 In-complexes in membrane, membrane frgments, and hemoglobin was studied after hemolysis. In spite of the higher lipid solubility of 111 In-tropolone, the transchelation capacity appears to be similar to that of 111 In-oxine. 111 In-acetylacetone had the highest transchelation capacity. (orig.)

  20. Influence of synthesis experimental parameters on the formation of nanoparticles of magnetite prepared by thermal decomposition method

    International Nuclear Information System (INIS)

    Vega, Jaime; Picasso, Gino; Lopez, Alcides; Aviles Felix, Luis

    2013-01-01

    In this work, nanoparticles based on magnetite have been synthesized by thermal decomposition via solvent-controlled synthesis in polyols, using triethylene glycol (TREG). The starting precursor were solutions of nitrate and acetylacetonate of Fe. The samples have been characterized by X-ray diffraction technique (XRD), adsorption-desorption of N 2 (BET equation model), scanning electronic microscopy (SEM), thermogravimetric analysis (TGA), vibration sample magnetometry (VSM) and Moessbauer spectroscopy. XRD diffractogram revealed the majority presence of spinel-like structural phases of magnetite in all samples. SEM micrographs showed morphological differences; the samples prepared from acetylacetonate presented good dispersion of particles whereas the ones prepared from nitrate-small agglomerations. BET isotherms of samples depicted a mesoporous profile which corresponded to IV type. TGA thermogram showed two defined regions which corresponded to vaporization of polyol light fractions and TREG. Zero coercivity on the magnetization curve of acetylacetonate precursor samples have been observed by VSM, which indicates superparamagnetic behavior. Moessbauer spectra of samples detected the presence of 4 doublet-like subspectra due to the presence of 4 sites occupied by Fe in paramagnetic or superparamagnetic state. (author)

  1. Ruthenium based redox flow battery for solar energy storage

    International Nuclear Information System (INIS)

    Chakrabarti, Mohammed Harun; Roberts, Edward Pelham Lindfield; Bae, Chulheung; Saleem, Muhammad

    2011-01-01

    Research highlights: → Undivided redox flow battery employing porous graphite felt electrodes was used. → Ruthenium acetylacetonate dissolved in acetonitrile was the electrolyte. → Charge/discharge conditions were determined for both 0.02 M and 0.1 M electrolytes. → Optimum power output of 0.180 W was also determined for 0.1 M electrolyte. → 55% voltage efficiency was obtained when battery was full of electrolytes. -- Abstract: The technical performance for the operation of a stand alone redox flow battery system for solar energy storage is presented. An undivided reactor configuration has been employed along with porous graphite felt electrodes and ruthenium acetylacetonate as electrolyte in acetonitrile solvent. Limiting current densities are determined for concentrations of 0.02 M and 0.1 M ruthenium acetylacetonate. Based on these, operating conditions for 0.02 M ruthenium acetylacetonate are determined as charging current density of 7 mA/cm 2 , charge electrolyte superficial velocity of 0.0072 cm/s (through the porous electrodes), discharge current density of 2 mA/cm 2 and discharge electrolyte superficial velocity of 0.0045 cm/s. An optimum power output of 35 mW is also obtained upon discharge at 2.1 mA/cm 2 . With an increase in the concentration of ruthenium species from 0.02 M to 0.1 M, the current densities and power output are higher by a factor of five approximately (at same superficial velocities) due to higher mass transport phenomenon. Moreover at 0.02 M concentration the voltage efficiency is better for battery full of electrolytes prior to charging (52.1%) in comparison to an empty battery (40.5%) due to better mass transport phenomenon. Voltage efficiencies are higher as expected at concentrations of 0.1 M ruthenium acetylacetonate (55% when battery is full of electrolytes and 48% when empty) showing that the all-ruthenium redox flow battery has some promise for future applications in solar energy storage. Some improvements for the

  2. Microspheres with an ultra high holmium content for brachytherapy of malignancies

    International Nuclear Information System (INIS)

    Lira, Raphael A.; Myamoto, Douglas M.; Souza, Jaime R.; Nascimento, Nanci; Azevedo, Mariangela de Burgos M. de; Osso Junior, Joao A.; Martinelli, Jose R.

    2011-01-01

    The overall objective of this work is to develop biodegradable microspheres intended for internal radiation therapy which provides an improved treatment for hepatic carcinomas. The most studied brachytherapy system employing microspheres made of holmium-biopolymer system is composed by poly(L-lactic acid) (PLLA) and holmium acetylacetonate (HoAcAc). The importance of the holmium high content in the microspheres can be interpreted as follow from a therapeutic standpoint, to achieve an effective use of microspheres loaded with HoAcAc, a high content of holmium is required to yield enough radioactivity with a relatively low amount of microspheres.The usual amounts of holmium that are incorporated in the microspheres composed by poly(L-lactic acid) and HoAcAc are 17.0 ± 0.5% (w/w) of holmium, which corresponds to a loading of about 50% of HoAcAc. Different approaches have been investigated to increase that value. One updated approach towards this direction is the production of microspheres with ultrahigh holmium as matrix using HoAcAc crystals as the sole starting material without the use of biopolymer. Likewise, in the search of microspheres with increased holmium content , it has been demonstrated that by changing the HoAcAc crystal structure by its recrystallization from crystal phase to the amorphous there is lost of acetylacetonate and water molecules causing the increasing of the holmium content. Microspheres were prepared by solvent evaporation, using holmium acetylacetonate (HoAcAc) crystals as the sole ingredient. Microspheres were characterized by using light and scanning electron microscopy, infrared and Raman spectroscopy, differential scanning calorimetry, X-rays diffraction, and confocal laser scanning microscopy. (author)

  3. Microspheres with an ultra high holmium content for brachytherapy of malignancies

    Energy Technology Data Exchange (ETDEWEB)

    Lira, Raphael A.; Myamoto, Douglas M.; Souza, Jaime R.; Nascimento, Nanci; Azevedo, Mariangela de Burgos M. de [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil). Centro de Biotecnologia; Osso Junior, Joao A. [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil). Centro de Radiofarmacia; Martinelli, Jose R. [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil). Centro de Ciencias e Tecnologia de Materiais

    2011-07-01

    The overall objective of this work is to develop biodegradable microspheres intended for internal radiation therapy which provides an improved treatment for hepatic carcinomas. The most studied brachytherapy system employing microspheres made of holmium-biopolymer system is composed by poly(L-lactic acid) (PLLA) and holmium acetylacetonate (HoAcAc). The importance of the holmium high content in the microspheres can be interpreted as follow from a therapeutic standpoint, to achieve an effective use of microspheres loaded with HoAcAc, a high content of holmium is required to yield enough radioactivity with a relatively low amount of microspheres.The usual amounts of holmium that are incorporated in the microspheres composed by poly(L-lactic acid) and HoAcAc are 17.0 {+-} 0.5% (w/w) of holmium, which corresponds to a loading of about 50% of HoAcAc. Different approaches have been investigated to increase that value. One updated approach towards this direction is the production of microspheres with ultrahigh holmium as matrix using HoAcAc crystals as the sole starting material without the use of biopolymer. Likewise, in the search of microspheres with increased holmium content , it has been demonstrated that by changing the HoAcAc crystal structure by its recrystallization from crystal phase to the amorphous there is lost of acetylacetonate and water molecules causing the increasing of the holmium content. Microspheres were prepared by solvent evaporation, using holmium acetylacetonate (HoAcAc) crystals as the sole ingredient. Microspheres were characterized by using light and scanning electron microscopy, infrared and Raman spectroscopy, differential scanning calorimetry, X-rays diffraction, and confocal laser scanning microscopy. (author)

  4. Structural studies of 4-aminoantipyrine derivatives

    Science.gov (United States)

    Cunha, Silvio; Oliveira, Shana M.; Rodrigues, Manoel T.; Bastos, Rodrigo M.; Ferrari, Jailton; de Oliveira, Cecília M. A.; Kato, Lucília; Napolitano, Hamilton B.; Vencato, Ivo; Lariucci, Carlito

    2005-10-01

    Reaction of 4-aminoantipyrine with acetylacetone, ethyl acetoacetate, benzoyl isothiocyanate, phenyl isothiocyanate, maleic anhydride and methoxymethylene Meldrum's acid afforded a series of new antipyrine derivatives. The antibacterial activity of the synthesized compounds against Micrococcus luteus ATCC 9341, Staphilococcus aureus ATCC 29737, and Escherichia coli ATCC 8739 was evaluated and the minimal inhibitory concentration determined. Modest activity was found only to the maleamic acid obtained from the reaction of 4-aminoantipyrine and maleic anhydride. 1H NMR investigation of this maleamic acid showed that it is slowly converted to the corresponding toxic maleimide. The structures of three derivatives were determined by X-ray diffraction analysis.

  5. Bicarbonate catalysis of exchange synthesis of [51Cr]Cr(III)-EDTA and other chromium complexes

    International Nuclear Information System (INIS)

    Aronson, F.L.; Strashun, A.M.; Lopez, C.; Steigman, J.

    1993-01-01

    Exchange syntheses of trivalent chromium complexes often require heating, thus limiting tagging of heat-sensitive biological compounds with 51 Cr. Bicarbonate at pH 6, accelerates the formation of mM Cr-EDTA. Accordingly, room temperature catalysis with [ 51 Cr]Cr(III) at 10 -7 -10 -8 M was investigated. Complexes were successfully formed with EDTA and iminodiacetic acid (electrophoretic analysis) and acetylacetone and tropolone (analyzed by chloroform extraction). The formation of these complexes normally requires extensive heating. (author)

  6. Titanium dioxide antireflective coating for silicon solar cells by spinning technique

    Energy Technology Data Exchange (ETDEWEB)

    Murozono, M; Kitamura, S

    1982-01-01

    Antireflective (AR) TiO2 films for Si solar cells are presently obtained by coating a solution that is derived from organotitanium compounds (with an acetylacetone ligand and an ethanol solvent) on the Si surface using a spinning technique, and then firing at high temperature. AR film thickness can be controlled by up to 1200 A by changing solution concentration and spin speed. Si solar cells with these AR films exhibit as much as a 50 percent improvement in conversion efficiency over uncoated cells. 12 references.

  7. Dielectric aluminium phosphate thin films. Couches minces dielectriques de phosphate d'aluminium

    Energy Technology Data Exchange (ETDEWEB)

    Daviero, S. (Lab. Physicochimie des Materiaux Solides, 34 - Montpellier (France)); Avinens, C. (Lab. Physicochimie des Materiaux Solides, 34 - Montpellier (France)); Ibanez, A. (Lab. Physicochimie des Materiaux Solides, 34 - Montpellier (France)); Giuntini, J.C. (Lab. Physicochimie des Materiaux Solides, 34 -Montpellier (France)); Philippot, E. (Lab. Physicochimie des Materiaux Solides, 34 - Montpellier (France))

    1993-04-01

    Aluminium phosphate thin films on silicium substrate have been carried out from tributylphosphate and aluminium acetylacetonate precursors in solution through the ''pyrosol'' process. It can be observed a large range of chemical analysis in terms of experimental conditions. These thin films have been characterized by X-ray diffraction and infrared spectrometry. Their electrical characteristics, defined from direct current and alternative current measurements, are quite different to those of the crystallized phosphate and can be explained by P-O and Al-O ''dangling bond'' existence. (orig.).

  8. On the mechanism of ion exchange in zirconium phosphates

    International Nuclear Information System (INIS)

    Clearfield, A.; Kalnins, J.M.

    1978-01-01

    The exchange of transition metal (M 2+ ) ions from manganese through cobalt, nickel, copper to zinc with γ-zirconium phosphate was examined. By using acetate salts the hydrogen ion concentration is kept low enough to achieve high loadings. The fully loaded solids have the composition ZrM(PO 4 ) 2 .4H 2 O. Near quantitative uptakes are achieved at 100 0 C. The interlayer spacings change very little with loading indicating that γ-zirconium phosphate is able to accommodate cations and water molecules without appreciable increase in volume. The copper exchanged phase readily forms an acetylacetonate when shaken with 2,4-pentanedione. (author)

  9. One-step flame synthesis of an active Pt/TiO2 catalyst for SO2 oxidation

    DEFF Research Database (Denmark)

    Johannessen, Tue; Koutsopoulos, Sotiris

    2002-01-01

    Flame synthesis as a route for production of composite metal oxides has been employed for the one-step synthesis of a supported noble metal catalyst, i.e. a Pt/TiO2 catalyst, by simultaneous combustion of Ti-isopropoxide and platinum acetylacetonate in a quench-cooled flame reactor. The average...... size of the platinum particles supported on aggregated nano-particles of TiO2 is approximately 2 nm. The high SO2-oxidation activity of the catalyst proves that platinum is not hidden in the titania matrix. The flame-produced catalyst showed catalytic activity similar to samples prepared by wet...

  10. Cathode and ion-luminescence of Eu:ZnO thin films prepared by reactive magnetron sputtering and plasma decomposition of non-volatile precursors

    Energy Technology Data Exchange (ETDEWEB)

    Gil-Rostra, Jorge [Instituto de Ciencia de Materiales de Sevilla, CSIC, Univ. Sevilla, C/Américo Vespucio 49, E-41092 Sevilla (Spain); Ferrer, Francisco J. [Centro Nacional de Aceleradores, CSIC, Univ. Sevilla, Av. Thomas A. Edison 7, E-41092 Sevilla (Spain); Martín, Inocencio R. [Departamento de Física Fundamental y Experimental, Electrónica y Sistemas, U. La Laguna, C/Astrofísico Francisco Sánchez s/n, E-38206 La Laguna, Santa Cruz de Tenerife (Spain); González-Elipe, Agustín R.; Yubero, Francisco [Instituto de Ciencia de Materiales de Sevilla, CSIC, Univ. Sevilla, C/Américo Vespucio 49, E-41092 Sevilla (Spain)

    2016-10-15

    This paper reports the luminescent behavior of Eu:ZnO thin films prepared by an one-step procedure that combines reactive magnetron sputtering deposition of ZnO with the plasma activated decomposition of a non-volatile acetylacetonate precursor of Eu sublimated in an effusion cell. Chemical composition and microstructure of the Eu:ZnO thin films have been characterized by several methods and their photo-, cathode- and ion-luminescent properties studied as a function of Eu concentration. The high transparency and well controlled optical properties of the films have demonstrated to be ideal for the development of cathode- and ion- luminescence sensors.

  11. Labelling of bacteria with indium chelates

    International Nuclear Information System (INIS)

    Kleinert, P.; Pfister, W.; Endert, G.; Sproessig, M.

    1985-01-01

    The indium chelates were prepared by reaction of radioactive indiumchloride with 10 μg oxine, 15 μg tropolone and 3 mg acetylacetone, resp. The formed chelates have been incubated with 10 9 germs/ml for 5 minutes, with labelling outputs from 90 to 95%. Both gram-positive (Streptococcus, Staphylococcus) and gram-negative bacteria (Escherichia coli) can be labelled. The reproductive capacity of the bacteria was not impaired. The application of indium labelled bacteria allows to show the distribution of microorganisms within the living organism and to investigate problems of bacterial adherence. (author)

  12. First kinetic discrimination between carbon and oxygen reactivity of enols.

    Science.gov (United States)

    García-Río, Luis; Mejuto, Juan C; Parajó, Mercedes; Pérez-Lorenzo, Moisés

    2008-11-07

    Nitrosation of enols shows a well-differentiated behavior depending on whether the reaction proceeds through the carbon (nucleophilic catalysis is observed) or the oxygen atom (general acid-base catalysis is observed). This is due to the different operating mechanisms for C- and O-nitrosation. Nitrosation of acetylacetone (AcAc) shows a simultaneous nucleophilic and acid-base catalysis. This simultaneous catalysis constitutes the first kinetic evidence of two independent reactions on the carbon and oxygen atom of an enol. The following kinetic study allows us to determine the rate constants for both reaction pathways. A similar reactivity of the nucleophilic centers with the nitrosonium ion is observed.

  13. Bis(acetylacetonato-κ2O,O′(2-amino-1-methyl-1H-benzimidazole-κN3oxidovanadium(IV

    Directory of Open Access Journals (Sweden)

    Zukhra Ch. Kadirova

    2009-07-01

    Full Text Available The title mixed-ligand oxidovanadium(IV compound, [VO(C5H7O22(C8H9N3], contains a VIV atom in a distorted octahedral coordination, which is typical for such complexes. The vanadyl group and the N-heterocyclic ligand are cis to each other. The coordination bond is located at the endocyclic N atom of the benzimidazole ligand. Intramolecular hydrogen bonds between the exo-NH2 group H atoms and acetylacetonate O atoms stabilize the crystal structure.

  14. Effect of adduct formation on valent state of cerium in its. beta. -diketonates

    Energy Technology Data Exchange (ETDEWEB)

    Spitsyn, V.I.; Martynenko, L.I.; Pechurova, N.I.; Snezhko, N.I.; Murav' eva, I.A.; Anufrieva, S.I. (Moskovskij Gosudarstvennyj Univ. (USSR))

    1982-04-01

    Physicochemical investigation of the system cerium (III, IV)-..beta..-diketone-additional ligand shows that ..beta..-diketonate ability to adduct formation decreases in the series tenoyltrifluoro-acetonate > acetylacetonate > dibenzoylmethanate > benzoylmethanate. Adduct formation of the cerium (III, IV) ..beta..-diketonates stabilizes cerium in trivalent condition, while oxidation degree 4+ is stable in tetrakis-..beta..-diketonates. The additional ligands are arranged in the series: tributhylphosphate < trioctyl-phosphineoxide < triphenylphosphineoxide < ..cap alpha.., ..cap alpha..'-dipyridyl < o-phenanthroline by the effect on cerium (III) stabilization in its ..beta..-diketonates.

  15. Investigation into kinetics of redox interaction in the system Ce(4) β-diketonate-additional ligand

    International Nuclear Information System (INIS)

    Anufrieva, S.I.; Snezhko, N.I.; Pechurova, N.I.; Martynenko, L.N.; Spitsyn, V.I.

    1981-01-01

    The rate of reduction of β-diketonate complexes of Ce(4) to Ce(3) β-diketonates in benzene solution in the presence and in the absence of additional ligands is studied using spectrophotometry. The rate of reduction of Ce(4) β-diketonates increases in the series Ce(TTFA) 4 4 4 4 4 (TTFA - thenoyltrifluoroacetone, DPM- --dipivaloylmethane, DBM - dibenzoylemethane, BA benzoylacetone, AA - acetylaceton). The studied phosphorus-containing additional ligands as to their effect on the rate of Ce (4) reduction can be arranged in the following order: trioctylphosphine oxide>triphenylphosphine oxide>tributyl phosphate [ru

  16. Effect of adduct formation on valent state of cerium in its ν-diketonates

    International Nuclear Information System (INIS)

    Spitsyn, V.I.; Martynenko, L.I.; Pechurova, N.I.; Snezhko, N.I.; Murav'eva, I.A.; Anufrieva, S.I.

    1982-01-01

    Physicochemical investigation of the system cerium (III, IV)-ν-diketone-additional ligand shows that ν-diketonate ability to adduct formation decreases in the series tenoyltrifluoro-acetonate > acetylacetonate > dibenzoylmethanate > benzoylmethanate. Adduct formation of the cerium (III, IV) ν-diketonates stabilizes cerium in trivalent condition, while oxidation degree 4+ is stable in tetrakis-ν-diketonates. The additional ligands are arranged in the series: tributhylphosphate < trioctyl-phosphineoxide < triphenylphosphineoxide < α, α'-dipyridyl < o-phenanthroline by the effect on cerium (III) stabilization in its ν-diketonates

  17. Theoretical study of the process of chelate ring scission in β-diketonates of metals. Basic state of lithium β-diketonates

    International Nuclear Information System (INIS)

    Sirenko, N.S.; L'vov, I.B.; Vovna, V.I.

    2000-01-01

    By the methods of Mndo and ab initio with configuration interaction (CI) accounting among them two variants of torsion scission of chelate ring in lithium malonodialdeginate and acetylacetonate are investigated. Effect of used approximation and optimization on calculated barriers of rotation and scission energies of metallocycle is estimated. It is shown that value of rotation barrier in ab initio approximation (2.0-2.5 eV) is for 30-100 % more then in MNDO approximation. Accounting of CI leads to insignificant changes of chelate ring scission energies and energy barriers as in direction of increase so in decrease one [ru

  18. Reverse saturable absorption (RSA) in fluorinated iridium derivatives

    Science.gov (United States)

    Ferry, Michael J.; O'Donnell, Ryan M.; Bambha, Neal; Ensley, Trenton R.; Shensky, William M.; Shi, Jianmin

    2017-08-01

    The photophysical properties of cyclometallated iridium compounds are beneficial for nonlinear optical (NLO) applications, such as the design of reverse saturable absorption (RSA) materials. We report on the NLO characterization of a family of compounds of the form [Ir(pbt)2(LX)], where pbt is 2-phenylbenzothiazole and LX is a beta-diketonate ligand. In particular, we investigate the effects of trifluoromethylation on compound solubility and photophysics compared to the parent acetylacetonate (acac) version. The NLO properties, such as the singlet and triplet excited-state cross sections, of these compounds were measured using the Z-scan technique. The excited-state lifetimes were determined from visible transient absorption spectroscopy.

  19. Orientation control of chemical solution deposited LaNiO3 thin films

    International Nuclear Information System (INIS)

    Ueno, Kengo; Yamaguchi, Toshiaki; Sakamoto, Wataru; Yogo, Toshinobu; Kikuta, Koichi; Hirano, Shin-ichi

    2005-01-01

    High quality LaNiO 3 (LNO) thin films with preferred orientation could be synthesized on Pt/Ti/SiO 2 /Si substrates at 700 deg. C using the chemical solution deposition method. The homogeneous and stable LNO precursor solutions were prepared using lanthanum isopropoxide and nickel (II) acetylacetonate in a mixed solvent of absolute ethanol and 2-methoxyethanol. The oriented LNO thin films exhibit metallic electro-conduction, and their resistivity at room temperature is sufficiently low for making them an alternative electrode material for functional ceramic thin films

  20. Synthesis and Characterization of V2O5/SiO2 Nanoparticles as Efficient Catalyst for Aromatization 1,4 Dihydropyridines

    International Nuclear Information System (INIS)

    Farzaneh, F.; Zamanifar, E.; Jafari Foruzin, L.; Ghandi, M.

    2012-01-01

    V 2 O 5 /SiO 2 nanoparticles was prepared via an one-pot sol gel method from vanadyl- acetylacetonate and tetraethyl orthosilicate in refluxing MeOH, followed by calcination at 700 °C for 2 hours. The resultant nanoparticles was characterized by means of scanning electron microscopy, transmission electron microscopy, X-ray diffraction, TGA and FTIR techniques. Rapid and efficient aromatization of 1,4-dihydropyridines catalyzed by V 2 O 5 /SiO 2 nanoparticles is described in this presentation.

  1. Synthesis of the first dimetallacarborane ruthenium-iridium cluster

    International Nuclear Information System (INIS)

    Lobanova, I.A.; Chizhevskij, I.T.; Petrovskij, P.V.; Bregadze, V.I.

    1996-01-01

    New electron-deficient dimetallic cluster (η 4 -C 8 H 12 )IrRu(μ-H)(PPh 3 ) 2 (η 5 -C 2 B 9 H 11 ) (1), has been prepared by the reaction of exo-nido-5,6,10-[Cl(PPh 3 ) 2 Ru]-5,6.10-(μ-H) 3 -10-H-7,8-C 2 B 9 H 8 with dimeric or acetylacetonate complexes of Ir in the presence of KOH in ethanol at 22 deg C. 1 H, 13 C, 31 P, 11 B NMR and IR spectral data for 1 are presented. 8 refs., 1 scheme

  2. Binary heterocyclic systems containing the ethylideneamino linkage: synthesis of some new heterocyclic compounds bearing the naphtho-[2,1-b]furan moiety

    Directory of Open Access Journals (Sweden)

    A. H. BEDAIR

    2006-05-01

    Full Text Available Ethylidene hydrazine (4a,b and thiazolidin-4-one (5 derivatives were synthesized by the reaction of ethylidenethiosemicarbazide derivative (3a with a-haloketone/ethyl bromoacetate, respectively. Hetrocyclization of ethylideneacetohydrazide derivative (7 with o-phenolic aldehydes gave the corresponding coumarin derivatives (8,9. The interaction of 7 with acetylacetone afforded the corresponding pyridine derivative (10. Treatment of the arylidene derivative 11b with malononitrile afforded the corresponding pyran derivative (12. The new products 3-12 were subjected to IR, 1H NMR and mass spectra studies.

  3. NOVEL SYNTHESIS OF POLYARYLENESULFONIUM CATIONS THROUGH A MULTI-ELECTRON TRANSFER PROCESS

    Institute of Scientific and Technical Information of China (English)

    1998-01-01

    The oxidative polymerization of aryl sulfoxides provides a novel polysulfonium compound, poly(methylsulfonio-1,4-phenylenethio-1,4-phenylene cation) in quantitative yield. The polymerization proceeds efficiently in an acidic solution under atmospheric conditions. Oxygen, chemical and electrochemical oxidations are available. Vanadyl acetylacetonate and cerium ammonium nitrate act as an effective catalyst for the oxygen oxidative polymerization. The polymerization mechanism involves multielectron oxidation of the sulfides followed by successive electrophilic substitution. The resulting polyarylenesulfonium cations are useful as a soluble precursor for the synthesis of high molecular weight (Mw>105) poly(thio arylne)s.

  4. Fluorine doped vanadium dioxide thin films for smart windows

    International Nuclear Information System (INIS)

    Kiri, Pragna; Warwick, Michael E.A.; Ridley, Ian; Binions, Russell

    2011-01-01

    Thermochromic fluorine doped thin films of vanadium dioxide were deposited from the aerosol assisted chemical vapour deposition reaction of vanadyl acetylacetonate, ethanol and trifluoroacetic acid on glass substrates. The films were characterised with scanning electron microscopy, variable temperature Raman spectroscopy and variable temperature UV/Vis spectroscopy. The incorporation of fluorine in the films led to an increase in the visible transmittance of the films whilst retaining the thermochromic properties. This approach shows promise for improving the aesthetic properties of vanadium dioxide thin films.

  5. The isolation of beryllium and mercury from lithium chloride solution by means of gas extraction

    International Nuclear Information System (INIS)

    Sevast'yanov, A.I.; Chepovoj, V.I.

    1988-01-01

    The possibility and optimal conditions of beryllium and mercury extraction using acetylacetone (HAA) from lithium chloride solution by argon blowing through the solution are determined. Dependences of extraction degrees and distribution coefficients on different parameters of liquid phase: initial pH value, lithium chloride concentration and initial content of HAA, are presented. The degree of beryllium extraction reaches the maximum at liquid phase pH of 4.4-5.25 and concentration of lithium chloride of 8.5 mol/l. Distribution coefficient changes in inverse proportion to the extraction degree

  6. 1. Mono([8]annulene)Uranium(4) half-sandwich complexes, 2. Novel syntheses of symmetrically substituted cyclooctatetetraenes

    International Nuclear Information System (INIS)

    Boussie, T.R.

    1991-10-01

    A reproducible, high-yield synthesis of mono([8]annulene)uranium(4)dichloride (1) is reported, along with the X-ray crystal structural of the bis(pyridine) adduct. Metathesis reactions of the half-sandwich complex 1 with a variety of simple alkyl and alkoxy reagents failed to generate any isolable mono-ring complexes. Reactions of 1 with polydentate, delocalized anions did produce stable derivatives, including mono([8]annulene)uranium(4)bis(acetylacetonate) (4). An X-ray crystal structure of 4 is reported

  7. Study of processes of interligand exchange between Cu(AA)2 and Y(DPM)3 in geseous phase

    International Nuclear Information System (INIS)

    Girichev, G.V.; Giricheva, N.I.; Belova, N.V.; Kuz'mina, N.P.; Kaul', A.R.; Gorbenko, O.Yu.

    1993-01-01

    Mass-spectrometric method was used to study the process, proceeding between gaseous copper acetylacetonate and yttrium dipivaloylmethanate in 150-630 deg C range. It was established that intensive ligand exchange with formation of Cu(DPM) (AA), Y(DPM) 2 (AA), Cu(DPM) 2 compounds in gaseous mixture took place between components. Thermal decomposition of copper and yttrium β-diketonates was observed with temperature growth, along with reactions of interligand exchange. Molecular forms of Y(DPM) 2 , Y(DPM)(AA), Cu(DPM) 2 and Cu(DPM)(AA) were the most thermally stable at that

  8. Quantification of chemical sulphur species in bulk soil and organic sulphur fractions by S K-edge Xanes spectroscopy

    DEFF Research Database (Denmark)

    Boye, K; Almkvist, G; Nilsson, S I

    2011-01-01

    residue (CR) incorporation and farmyard manure (FYM) application, with equal applications of mineral nutrients were included in the study. In the new data treatment method, internally calibrated spectra of dilute solutions (30 mm) of model compounds were used to fit the sample spectra. This greatly...... the opposite trend was observed. Sulphur XANES spectroscopy of acetylacetone extracts of physically protected and unprotected organic S in two of the soils revealed that physical protection was not related to S speciation; however, intermediate forms of oxidized S species appeared to accumulate in the residual...

  9. (Acetylacetonato-κ2O,O′bis[5-methoxy-2-(naphth[1,2-d][1,3]oxazol-2-ylphenyl-κ2C1,N]iridium(III

    Directory of Open Access Journals (Sweden)

    Yuan-Yuan Zhou

    2011-10-01

    Full Text Available In the title compound, [Ir(C18H12NO22(C5H7O2], the Ir atom is O,O′-chelated by the acetylacetonate group and C,N-chelated by the 2-arylnaphth[1,2-d]oxazole groups. The six-coordinate metal atom displays a distorted octahedral geometry. Intramolecular C—H...O hydrogen bonds occur. In the crystal, intermolecular C—H...O hydrogen bonds link the molecules into columns parallel to the b axis.

  10. Composition tunable cobalt–nickel and cobalt–iron alloy nanoparticles below 10 nm synthesized using acetonated cobalt carbonyl

    International Nuclear Information System (INIS)

    Schooneveld, Matti M. van; Campos-Cuerva, Carlos; Pet, Jeroen; Meeldijk, Johannes D.; Rijssel, Jos van; Meijerink, Andries; Erné, Ben H.; Groot, Frank M. F. de

    2012-01-01

    A general organometallic route has been developed to synthesize Co x Ni 1−x and Co x Fe 1−x alloy nanoparticles with a fully tunable composition and a size of 4–10 nm with high yield. In contrast to previously reported synthesis methods using dicobalt octacarbonyl (Co 2 (CO) 8 ), here the cobalt–cobalt bond in the carbonyl complex is first broken with anhydrous acetone. The acetonated compound, in the presence of iron carbonyl or nickel acetylacetonate, is necessary to obtain small composition tunable alloys. This new route and insights will provide guidelines for the wet-chemical synthesis of yet unmade bimetallic alloy nanoparticles.

  11. Synthesis and crystal structure of a new homoleptic tetraarylruthenium(IV) complex Ru(2,4,5-Me{sub 3}C{sub 6}H{sub 2}){sub 4}

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Chang-Jiu; Wu, Xiu-Li; Ma, Xiu-Fang; Jia, Ai-Quan; Zhang, Qian-Feng [Anhui Univ. of Technology, Anhui (China). Inst. of Molecular Engineering and Applied Chemistry and Anhui Province Key Lab. of Metallurgy Engineering and Resources Recycling

    2017-08-01

    Treatment of [Ru(acac){sub 3}] (acac-=acetylacetonate) with (2,4,5-Me{sub 3}C{sub 6}H{sub 2})MgBr, followed by column chromatography in air, afforded the homoleptic tetraaryl-ruthenium(IV) complex [Ru(2,4,5-Me{sub 3}C{sub 6}H{sub 2}){sub 4}] (1) in moderate yield. The product was characterized by proton NMR spectroscopy and microanalyses. Its crystal structure has also been established by X-ray crystallography.

  12. Radioisotope methods for leucocyte labelling

    International Nuclear Information System (INIS)

    Kostadinova, I.; Kovacheva, S.

    1988-01-01

    A review is made of the labelling methods with the following tracers: 3 H-thymidine, 32 P-DP, 111 In (oxine, tropolon, acetylacetone, MERC), 99m Tc (reduced 99m Tc, lypophyl 99m Tc-complexes and 99m Tc-colloids). The main diagnosis areas are mentioned: abdominal abscesses and inflammations, inflammation foci of skeleton or of implanted prosthesis; acute myocardial infarction, bacterial endocarditis, rejection of kydney transplantations or vascular grafts. It is concluded that labelled leucocytes are very reliable for noninvasive diagnosis of inflammation foci with unclear localization

  13. Radioisotope methods for leucocyte labelling

    Energy Technology Data Exchange (ETDEWEB)

    Kostadinova, I; Kovacheva, S [Meditsinska Akademiya, Sofia (Bulgaria). Katedra po Rentgenologiya i Radiologiya

    1988-01-01

    A review is made of the labelling methods with the following tracers: {sup 3}H-thymidine, {sup 32}P-DP, {sup 111}In (oxine, tropolon, acetylacetone, MERC), {sup 99m}Tc (reduced {sup 99m}Tc, lypophyl {sup 99m}Tc-complexes and {sup 99m}Tc-colloids). The main diagnosis areas are mentioned: abdominal abscesses and inflammations, inflammation foci of skeleton or of implanted prosthesis; acute myocardial infarction, bacterial endocarditis, rejection of kydney transplantations or vascular grafts. It is concluded that labelled leucocytes are very reliable for noninvasive diagnosis of inflammation foci with unclear localization.

  14. A study of Cu/ZnO/Al2O3 methanol catalysts prepared by flame combustion synthesis

    DEFF Research Database (Denmark)

    Jensen, Joakim Reimer; Johannessen, Tue; Wedel, Stig

    2003-01-01

    The flame combustion synthesis of Cu/ZnO/Al2O3 catalysts for the synthesis of methanol from CO, CO2 and H2 is investigated. The oxides are generated in a premixed flame from the acetyl-acetonate vapours of Cu, Zn and Al mixed with the fuel and air prior to combustion. The flame-generated powder...... temperature and quench-cooling of the flame tend to increase the dispersion of the phases and the specific surface area of the particles. Properties of both the ternary composition, the three binary compositions and the pure oxides are discussed. The calculation of simultaneous phase and chemical equilibrium...

  15. 1. Mono([8]annulene)Uranium(4) half-sandwich complexes, 2. Novel syntheses of symmetrically substituted cyclooctatetetraenes

    Energy Technology Data Exchange (ETDEWEB)

    Boussie, Thomas Richard [Univ. of California, Berkeley, CA (United States)

    1991-10-01

    A reproducible, high-yield synthesis of mono([8]annulene)uranium(4)dichloride (1) is reported, along with the X-ray crystal structural of the bis(pyridine) adduct. Metathesis reactions of the half-sandwich complex 1 with a variety of simple alkyl and alkoxy reagents failed to generate any isolable mono-ring complexes. Reactions of 1 with polydentate, delocalized anions did produce stable derivatives, including mono([8]annulene)uranium(4)bis(acetylacetonate) (4). An X-ray crystal structure of 4 is reported.

  16. 1. Mono((8)annulene)Uranium(4) half-sandwich complexes, 2. Novel syntheses of symmetrically substituted cyclooctatetetraenes

    Energy Technology Data Exchange (ETDEWEB)

    Boussie, T.R.

    1991-10-01

    A reproducible, high-yield synthesis of mono((8)annulene)uranium(4)dichloride (1) is reported, along with the X-ray crystal structural of the bis(pyridine) adduct. Metathesis reactions of the half-sandwich complex 1 with a variety of simple alkyl and alkoxy reagents failed to generate any isolable mono-ring complexes. Reactions of 1 with polydentate, delocalized anions did produce stable derivatives, including mono((8)annulene)uranium(4)bis(acetylacetonate) (4). An X-ray crystal structure of 4 is reported.

  17. Hydrophilic Pt nanoflowers: synthesis, crystallographic analysis and catalytic performance.

    Science.gov (United States)

    Mourdikoudis, Stefanos; Altantzis, Thomas; Liz-Marzán, Luis M; Bals, Sara; Pastoriza-Santos, Isabel; Pérez-Juste, Jorge

    2016-05-21

    Water-soluble Pt nanoflowers (NFs) were prepared by diethylene glycol-mediated reduction of Pt acetylacetonate (Pt(acac) 2 ) in the presence of polyethylenimine. Advanced electron microscopy analysis showed that the NFs consist of multiple branches with a truncated cubic morphology and different crystallographic orientations. We demonstrate that the nature of the solvent strongly influences the resulting morphology. The catalytic performance of the Pt NFs in 4-nitrophenol reduction was found to be superior to that of other nanoparticle-based catalysts. Additionally, the Pt NFs display good catalytic reusability with no loss of activity after five consecutive cycles.

  18. Complete removal of uranyl nitrate from tissue matrix using supercritical fluid extraction

    International Nuclear Information System (INIS)

    Kumar, R.; Sivaraman, N.; Senthil Vadivu, E.; Srinivasan, T.G.; Vasudeva Rao, P.R.

    2003-01-01

    The removal of uranyl nitrate from tissue matrix has been studied with supercritical carbon dioxide modified with methanol alone as well as complexing reagents dissolved in methanol. A systematic study of various complexing agents led to the development of an extraction procedure for the quantitative recovery of uranium from tissue matrix with supercritical carbon dioxide modified with methanol containing small quantities of acetylacetone. The drying time and temperature employed in loading of uranyl nitrate onto tissue paper were found to influence the extraction efficiency significantly

  19. Electrophoretic Deposition of SnO2 Nanoparticles and Its LPG Sensing Characteristics

    Directory of Open Access Journals (Sweden)

    Göktuğ Günkaya

    2015-01-01

    Full Text Available Homogenized SnO2 nanoparticles (60 nm in acetylacetone mediums, both with and without iodine, were deposited onto platinum coated alumina substrate and interdigital electrodes using the electrophoretic deposition (EPD method for gas sensor applications. Homogeneous and porous film layers were processed and analyzed at various coating times and voltages. The structure of the deposited films was characterized by a scanning electron microscopy (SEM. The gas sensing properties of the SnO2 films were investigated using liquid petroleum gas (LPG for various lower explosive limits (LEL. The results showed that porous, crack-free, and homogeneous SnO2 films were achieved for 5 and 15 sec at 100 and 150 V EPD parameters using an iodine-free acetylacetone based SnO2 suspension. The optimum sintering for the deposited SnO2 nanoparticles was observed at 500°C for 5 min. The results showed that the sensitivity of the films was increased with the operating temperature. The coated films with EPD demonstrated a better sensitivity for the 20 LEL LPG concentrations at a 450°C operating temperature. The maximum sensitivity of the SnO2 sensors at 450°C to 20 LEL LPG was 30.

  20. TiO2 thin-films on polymer substrates and their photocatalytic activity

    International Nuclear Information System (INIS)

    Yang, Jae-Hun; Han, Yang-Su; Choy, Jin-Ho

    2006-01-01

    We have developed dip-coating process for TiO 2 -thin film on polymer substrates (acrylonitrile-butadiene-styrene polymer: ABS, polystyrene: PS). At first, a monodispersed and transparent TiO 2 nano-sol solution was prepared by the controlled hydrolysis of titanium iso-propoxide in the presence of acetylacetone and nitric acid catalyst at 80 deg. C. Powder X-ray diffraction patterns of the dried particles are indicative of crystalline TiO 2 with anatase-type structure. According to the XRD and transmission electron microscopy (TEM) studies, the mean particle size was estimated to be ca. 5 nm. The transparent thin films on ABS and PS substrates were fabricated by dip-coating process by changing the processing variables, such as the number of dip-coating and TiO 2 concentration in nano-sol solution. Scanning electron microscopic (SEM) analysis for the thin film samples reveals that the acetylacetone-modified TiO 2 nano-sol particles are effective for enhancing the interfacial adherence between films and polymeric substrates compared to the unmodified one. Photocatalytic degradation of methylene blue (MB) on the TiO 2 thin-films has also been systematically investigated

  1. Lung transit of /sup 111/Indium-labelled granulocytes. Relationship to labelling techniques

    Energy Technology Data Exchange (ETDEWEB)

    Saverymuttu, S.H.; Peters, A.M.; Danpure, H.J.; Reavy, H.J.; Osman, S.; Lavender, J.P. (Hammersmith Hospital, London, England)

    1983-01-01

    The early in vivo distribution of /sup 111/Indium-labelled granulocytes, recorded by dynamic imaging using a gamma camera and computer, varied according to the separation and labelling technique. Following i.v. bolus injection, 4 kinetic patterns could be identified: (A) rapid transit through the pulmonary vasculature, (B) delayed transit through the lung with clearance by about 30 min, (C) complete retention by the lung, for up to 10 min, followed by slow release over a period of 1 to 2 h, (D) delayed transit through the lung with a similar time course to (B) but with subsequent heavy liver uptake. Granulocytes labelled with /sup 111/In-tropolonate and maintained in plasma throughout the labelling procedure, whether injected as a 'pure' (separated by plasma-enriched density gradient centrifugation) or 'crude' (seprated by differential centrifugation) preparation, displayed type A kinetics, thought to most closely represent the normal behaviour of granulocytes. 'Crude' cells labelled in saline with /sup 111/In-acetylacetonate displayed type B kinetics. 'Pure' cells isolated on Percoll-saline and labelled in saline with /sup 111/In-acetylacetonate displayed type C kinetics, thought to represent granulocyte 'stimulation' and/or damage, or type D kientics, thought to represent severe damage. The importance is stressed of labelling granulocytes for kinetic studies with a technique that results in minimal alteration of cell behaviour.

  2. 1T1R Nonvolatile Memory with Al/TiO2/Au and Sol-Gel-Processed Insulator for Barium Zirconate Nickelate Gate in Pentacene Thin Film Transistor

    Directory of Open Access Journals (Sweden)

    Ke-Jing Lee

    2017-12-01

    Full Text Available A one-transistor and one-resistor (1T1R architecture with a resistive random access memory (RRAM cell connected to an organic thin-film transistor (OTFT device is successfully demonstrated to avoid the cross-talk issues of only one RRAM cell. The OTFT device, which uses barium zirconate nickelate (BZN as a dielectric layer, exhibits favorable electrical properties, such as a high field-effect mobility of 2.5 cm2/Vs, low threshold voltage of −2.8 V, and low leakage current of 10−12 A, for a driver in the 1T1R operation scheme. The 1T1R architecture with a TiO2-based RRAM cell connected with a BZN OTFT device indicates a low operation current (10 μA and reliable data retention (over ten years. This favorable performance of the 1T1R device can be attributed to the additional barrier heights introduced by using Ni (II acetylacetone as a substitute for acetylacetone, and the relatively low leakage current of a BZN dielectric layer. The proposed 1T1R device with low leakage current OTFT and excellent uniform resistance distribution of RRAM exhibits a good potential for use in practical low-power electronic applications.

  3. New experiments in organic, fast-atom-bomdardment, and secondary-ion mass spectrometry

    International Nuclear Information System (INIS)

    DiDonato, G.C.

    1987-01-01

    The goal of research presented in this dissertation is the creative use of new ionization and instrumental techniques in mass spectrometry. This goal manifests itself in three areas of mass spectrometry. In the first portion, modern, state-of-the-art instrumentation and new experiments were used to re-examine the mass spectra of transition-metal acetates and acetylacetonates. High resolution, chemical ionization, negative chemical ionization, and extended-mass-range mass spectrometry uncovered a wealth of new gas-phase ionic species. Energy-resolved mass spectrometry/mass spectrometry was applied to the characterization of molecular and fragment ion first-row transition-metal acetylacetonates, and comprises the second portion of the thesis. Studies in fast-atom-bombardment mass spectrometry are the subject of the third portion of the dissertation. Since fast-atom bombardment samples a liquid matrix, absolute and relative abundances of sputtered secondary ions are influenced by solution chemistry. The design and construction of an imaging secondary-ion mass spectrometer is the subject of the final portion of the thesis. This instrument provides for direct mass-spectrometric analysis of thin-layer and paper chromatograms and electrophoretograms

  4. Long-chain amine-templated synthesis of gallium sulfide and gallium selenide nanotubes

    Science.gov (United States)

    Seral-Ascaso, A.; Metel, S.; Pokle, A.; Backes, C.; Zhang, C. J.; Nerl, H. C.; Rode, K.; Berner, N. C.; Downing, C.; McEvoy, N.; Muñoz, E.; Harvey, A.; Gholamvand, Z.; Duesberg, G. S.; Coleman, J. N.; Nicolosi, V.

    2016-06-01

    We describe the soft chemistry synthesis of amine-templated gallium chalcogenide nanotubes through the reaction of gallium(iii) acetylacetonate and the chalcogen (sulfur, selenium) using a mixture of long-chain amines (hexadecylamine and dodecylamine) as a solvent. Beyond their role as solvent, the amines also act as a template, directing the growth of discrete units with a one-dimensional multilayer tubular nanostructure. These new materials, which broaden the family of amine-stabilized gallium chalcogenides, can be tentatively classified as direct large band gap semiconductors. Their preliminary performance as active material for electrodes in lithium ion batteries has also been tested, demonstrating great potential in energy storage field even without optimization.We describe the soft chemistry synthesis of amine-templated gallium chalcogenide nanotubes through the reaction of gallium(iii) acetylacetonate and the chalcogen (sulfur, selenium) using a mixture of long-chain amines (hexadecylamine and dodecylamine) as a solvent. Beyond their role as solvent, the amines also act as a template, directing the growth of discrete units with a one-dimensional multilayer tubular nanostructure. These new materials, which broaden the family of amine-stabilized gallium chalcogenides, can be tentatively classified as direct large band gap semiconductors. Their preliminary performance as active material for electrodes in lithium ion batteries has also been tested, demonstrating great potential in energy storage field even without optimization. Electronic supplementary information (ESI) available. See DOI: 10.1039/c6nr01663d

  5. Facile synthesis and excellent microwave absorption properties of FeCo-C core-shell nanoparticles

    Science.gov (United States)

    Liang, Bingbing; Wang, Shiliang; Kuang, Daitao; Hou, Lizhen; Yu, Bowen; Lin, Liangwu; Deng, Lianwen; Huang, Han; He, Jun

    2018-02-01

    FeCo-C core-shell nanoparticles (NPs) with diameters of 10-50 nm have been fabricated on a large scale by one-step metal-organic chemical vapor deposition using the mixture of cobalt acetylacetonate and iron acetylacetonate as the precursor. The Fe/Co molar ratio of the alloy nanocores and graphitization degree of C shells, and thus the magnetic and electric properties of the core-shell NPs, can be tuned by the deposition temperature ranging from 700 °C to 900 °C. Comparative tests reveal that a relatively high Fe/Co molar ratio and low graphitization degree benefit the microwave absorption (MA) performance of the core-shell NPs. The composite with 20 wt% core-shell NP obtained at 800 °C and 80 wt% paraffin exhibits an optimal reflection loss ({{R}}{{L}}) of -60.4 dB at 7.5 GHz with a thickness of 3.3 mm, and an effective absorption bandwidth (frequency range for RL ≤10 dB) of 9.2 GHz (8.8-18.0 GHz) under an absorber thickness of 2.5 mm. Our study provides a facile route for the fabrication of alloy-C core-shell nanostructures with high MA performance.

  6. Characterisation of thin films of organic phosphorescent materials using synchrotron radiation

    International Nuclear Information System (INIS)

    Thompson, J.; Arima, V.; Matino, F.; Cingolani, R.; Blyth, R.I.R.

    2005-01-01

    Synchrotron radiation photoemission and X-ray absorption spectroscopy (NEXAFS) have been used to investigate the electronic structure of evaporated films of the phosphorescent organic iridium complexes iridium tris-(2-(4-totyl)pyridinato-N,C 2 ), iridium bis(2-(4,6-difluorophenyl)pyridinato-N,C 2 )picolinate, and iridium bis(2-(2'-benzothienyl)pyridinato-N,C 3 )-(acetylacetonate) and spin coated films of these materials in a polymer host. Resonant photoemission at the Ir N 6,7 edge indicates that the Ir 5d states are hybridised with the π orbitals of the organic ligands, in agreement with recent calculations. The nitrogen K-edge NEXAFS shows the difference in the unoccupied orbitals induced by the acetylacetonate group compared to those of the pyridinate ligands. Although the valence bands of the ex situ prepared films are not accessible to photoemission, the Ir 4f core levels remain visible, and demonstrate that the polymer host serves to lower the electron injection barrier in the iridium complexes in comparison to the pure films

  7. PtPb nanoparticle electrocatalysts: control of activity through synthetic methods

    International Nuclear Information System (INIS)

    Ghosh, Tanushree; Matsumoto, Futoshi; McInnis, Jennifer; Weiss, Marilyn; Abruna, Hector D.; DiSalvo, Francis J.

    2009-01-01

    Solution phase synthesis of intermetallic nanoparticles without using surfactants (for catalytic applications) and subsequent control of size distribution remains a challenge: of growing interest, but not widely explored yet. To understand the questions in the syntheses of Pt containing intermetallic nanoparticles (as electrocatalysts for direct fuel cells) by using sodium naphthalide as the reducing agent, the effects of the Pt precursors' organic ligands were investigated. PtPb syntheses were studied as the model case. In particular, methods that lead to nanoparticles that are independent single crystals are desirable. Platinum acetylacetonate, which is soluble in many organic solvents, has ligands that may interfere less with nanoparticle growth and ordering. Interesting trends, contrary to expectations, were observed when precursors were injected into a reducing agent solution at high temperatures. The presence of acetylacetonate, from the precursor, on the nanoparticles was confirmed by ATR, while SEM imaging showed evidence of morphological changes in the nanoparticles with increasing reaction temperature. A definite relationship between domain size and extent of observed residue (organic material and sodium) present on the particles could be established. By varying post-reaction solvent removal techniques, room temperature crystallization of PtPb nanoparticles was also achieved. Electrochemical activity of the nanoparticles was also much higher than that of nanoparticles synthesized by previous reaction schemes using sodium naphthalide as the reducing agent. Along with the above mentioned techniques, BET, TEM, CBED, SAED, and XRD were used as characterization tools for the prepared nanoparticles.

  8. Effect of Ag doping on the structural, electrical and optical properties of ZnO grown by MOCVD at different substrate temperatures

    Science.gov (United States)

    Ievtushenko, A.; Karpyna, V.; Eriksson, J.; Tsiaoussis, I.; Shtepliuk, I.; Lashkarev, G.; Yakimova, R.; Khranovskyy, V.

    2018-05-01

    ZnO films and nanostructures were deposited on Si substrates by MOCVD using single source solid state zinc acetylacetonate (Zn(AA)) precursor. Doping by silver was realized in-situ via adding 1 and 10 wt. % of Ag acetylacetonate (Ag(AA)) to zinc precursor. Influence of Ag on the microstructure, electrical and optical properties of ZnO at temperature range 220-550 °C was studied by scanning, transmission electron and Kelvin probe force microscopy, photoluminescence and four-point probe electrical measurements. Ag doping affects the ZnO microstructure via changing the nucleation mode into heterogeneous and thus transforming the polycrystalline films into a matrix of highly c-axis textured hexagonally faceted nanorods. Increase of the work function value from 4.45 to 4.75 eV was observed with Ag content increase, which is attributed to Ag behaviour as a donor impurity. It was observed, that near-band edge emission of ZnO NS was enhanced with Ag doping as a result of quenching deep-level emission. Upon high doping of ZnO by Ag it tends to promote the formation of basal plane stacking faults defect, as it was observed by HR TEM and PL study in the case of 10 wt.% of Ag. Based on the results obtained, it is suggested that NS deposition at lower temperatures (220-300 °C) is more favorable for p-type doping of ZnO.

  9. Characterisation of thin films of organic phosphorescent materials using synchrotron radiation

    Energy Technology Data Exchange (ETDEWEB)

    Thompson, J. [Float-Lux srl., via Ravenna 14, 73100 Lecce (Italy); Arima, V. [National Nanotechnology Laboratory of INFM, Distretto Tecnologico ISUFI, Universita di Lecce, via per Arnesano, 73100 Lecce (Italy); Matino, F. [National Nanotechnology Laboratory of INFM, Distretto Tecnologico ISUFI, Universita di Lecce, via per Arnesano, 73100 Lecce (Italy); Cingolani, R. [National Nanotechnology Laboratory of INFM, Distretto Tecnologico ISUFI, Universita di Lecce, via per Arnesano, 73100 Lecce (Italy); Blyth, R.I.R. [National Nanotechnology Laboratory of INFM, Distretto Tecnologico ISUFI, Universita di Lecce, via per Arnesano, 73100 Lecce (Italy)]. E-mail: rob.blyth@unile.it

    2005-07-30

    Synchrotron radiation photoemission and X-ray absorption spectroscopy (NEXAFS) have been used to investigate the electronic structure of evaporated films of the phosphorescent organic iridium complexes iridium tris-(2-(4-totyl)pyridinato-N,C{sup 2}), iridium bis(2-(4,6-difluorophenyl)pyridinato-N,C{sup 2})picolinate, and iridium bis(2-(2'-benzothienyl)pyridinato-N,C{sup 3})-(acetylacetonate) and spin coated films of these materials in a polymer host. Resonant photoemission at the Ir N{sub 6,7} edge indicates that the Ir 5d states are hybridised with the {pi} orbitals of the organic ligands, in agreement with recent calculations. The nitrogen K-edge NEXAFS shows the difference in the unoccupied orbitals induced by the acetylacetonate group compared to those of the pyridinate ligands. Although the valence bands of the ex situ prepared films are not accessible to photoemission, the Ir 4f core levels remain visible, and demonstrate that the polymer host serves to lower the electron injection barrier in the iridium complexes in comparison to the pure films.

  10. Molecular-mediated crystal growth of PbTiO3 nanostructure on silicon substrate

    International Nuclear Information System (INIS)

    Chao Chunying; Ren Zhaohui; Liu Zhenya; Xiao Zhen; Xu Gang; Li Xiang; Wei Xiao; Shen Ge; Han Gaorong

    2011-01-01

    A simple approach based on an organically modified sol-gel process has been developed to fabricate PbTiO 3 (PT) nanocrystals on Si (1 0 0) substrate, where the amorphous powder modified by acetylacetone (acac) was used as precursor. After dropping the amorphous powder precursor prepared by freeze-drying process, PT nanocrystals on Si (1 0 0) substrate were obtained after heat treatment at 720 deg. C for 30 min in air. PT nanocrystals have been detected by XRD to be tetragonal perovskite structure. With the increase of acac/Pb molar ratio, the relative (1 0 0)/(0 0 1) diffraction peak intensity gradually increases, which probably suggested an oriented growth of PT nanocrystal along [1 0 0] on Si (1 0 0) substrates. In addition, Atomic force microscopy (AFM) results indicated that the height and the average lateral size of PT nanocrystal increased and then decreased as the acac/Pb molar ratio increased. Piezoelectric force microscopy (PFM) results demonstrated that all the samples show obvious piezoelectric activity. These results implied that the acetylacetone molecular mediated the growth of PT nanocrystals on Si (1 0 0) substrates possibly by the acac/Pb molar ratio. This simple method has been suggested to be attractive for tailoring an oriented growth of the nanostructures of perovskite oxide systems on Si substrates.

  11. Simple one-pot synthesis of platinum-palladium nanoflowers with enhanced catalytic activity and methanol-tolerance for oxygen reduction in acid media

    International Nuclear Information System (INIS)

    Zheng, Jie-Ning; He, Li-Li; Chen, Fang-Yi; Wang, Ai-Jun; Xue, Meng-Wei; Feng, Jiu-Ju

    2014-01-01

    Graphical abstract: PtPd nanoflowers were fabricated by one-pot solvothermal co-reduction method in oleylamine system, which exhibited the improved electrocatalytic activity and higher methanol tolerance for oxygen reduction, compared with commercial Pt and Pd black catalysts. - Highlights: • Bimetallic alloyed PtPd nanoflowers are prepared by a simple one-pot solvothermal co-reduction method. • PtPd nanoflowers display high catalytic performance for ORR dominated by a four-electron pathway. • PtPd nanoflowers show good methanol tolerance for ORR. - Abstract: In this work, bimetallic alloyed platinum-palladium (PtPd) nanoflowers are fabricated by one-pot solvothermal co-reduction of Pt (II) acetylacetonate and Pd (II) acetylacetonate in oleylamine system. The as-prepared nanostructures show the enhanced electrocatalytic activity for oxygen reduction reaction (ORR), dominated by a four-electron pathway based on the Koutecky-Levich plots, mainly owing to the inhibition of the formation of Pt–OH ad via the downshift of d-band center for Pt. Meanwhile, PtPd nanoflowers display good methanol tolerance and improved stability for ORR. The chronoamperometry test reveals that the current of PtPd nanoflowers remains 45.9% of its original value within 6000 s, much higher than those of commercial Pt (36.7%) and Pd (32.2%) black catalysts. Therefore, PtPd nanoflowers with unique interconnected structures can be used as a promising cathode catalyst in direct methanol fuel cells

  12. Synthesis and spectroscopic characterization of some lanthanide(III nitrate complexes of ethyl 2-[2-(1-acetyl-2-oxopropylazo]-4,5-dimethyl-3-thiophenecarboxyate

    Directory of Open Access Journals (Sweden)

    CHEMPAKAM JANARDHANAN ATHIRA

    2011-02-01

    Full Text Available Ethyl 2-[2-(1-acetyl-2-oxopropylazo]-4,5-dimethyl-3-thiophenecarboxyate was synthesized by coupling diazotized ethyl 2-amino-4,5-dimethylthiophene-3-carboxylate with acetylacetone. Based on various spectral studies and elemental analysis, an intramolecularly hydrogen-bonded azo-enol structural form was assigned for the ligand. This ligand is versatile in forming a series of lanthanide(III complexes, viz., lanthanum(III, cerium(III, praseodymium(III, neodymium(III, samarium(III and gadolinium(III, which were characterized through various spectral studies, elemental analysis, magnetic susceptibility measurements, molar conductance and thermal analysis. The spectral data revealed that the ligand acted as a neutral tridentate, coordinating to the metal ion through one of the azo nitrogen atoms, the ester carbonyl and the enolic oxygen of the acetylacetone moiety, without deprotonation. Molar conductance values adequately supported their non-electrolytic nature. The ligand and lanthanum(III complex were subjected to X-ray diffraction studies. In addition, the lanthanum(III complex underwent a facile transesterification reaction on refluxing with methanol for a long period. The thermal behaviour of the lanthanum(III complex was also examined

  13. Synthesis of zirconia sol stabilized by trivalent cations (yttrium and neodymium or americium): a precursor for Am-bearing cubic stabilized zirconia.

    Science.gov (United States)

    Lemonnier, Stephane; Grandjean, Stephane; Robisson, Anne-Charlotte; Jolivet, Jean-Pierre

    2010-03-07

    Recent concepts for nuclear fuel and targets for transmuting long-lived radionuclides (minor actinides) and for the development of innovative Gen-IV nuclear fuel cycles imply fabricating host phases for actinide or mixed actinide compounds. Cubic stabilized zirconia (Zr, Y, Am)O(2-x) is one of the mixed phases tested in transmutation experiments. Wet chemical routes as an alternative to the powder metallurgy are being investigated to obtain the required phases while minimizing the handling of contaminating radioactive powder. Hydrolysis of zirconium, neodymium (a typical surrogate for americium) and yttrium in aqueous media in the presence of acetylacetone was firstly investigated. Progressive hydrolysis of zirconium acetylacetonate and sorption of trivalent cations and acacH on the zirconia particles led to a stable dispersion of nanoparticles (5-7 nm) in the 6-7 pH range. This sol gels with time or with temperature. The application to americium-containing solutions was then successfully tested: a stable sol was synthesized, characterized and used to prepare cubic stabilized zirconia (Zr, Y, Am)O(2-x).

  14. Effect of solution composition on anatase to rutile transformation of sprayed TiO{sub 2} thin films

    Energy Technology Data Exchange (ETDEWEB)

    Juma, Albert Owino, E-mail: albert.juma@ttu.ee [Laboratory of Thin Film Chemical Technologies, Department of Materials Science, Tallinn University of Technology, Ehitajate tee 5, EE-19086 Tallinn (Estonia); Acik, Ilona Oja [Laboratory of Thin Film Chemical Technologies, Department of Materials Science, Tallinn University of Technology, Ehitajate tee 5, EE-19086 Tallinn (Estonia); Mikli, Valdek [Chair of Semiconductor Materials Technology, Department of Materials Science, Tallinn University of Technology, Ehitajate tee 5, EE-19086 Tallinn (Estonia); Mere, Arvo; Krunks, Malle [Laboratory of Thin Film Chemical Technologies, Department of Materials Science, Tallinn University of Technology, Ehitajate tee 5, EE-19086 Tallinn (Estonia)

    2015-11-02

    Acetylacetone is used as a chelating agent for titanium(IV) isopropoxide to inhibit hydrolysis and stabilize the precursor solution. The effect of the molar ratio between titanium(IV) isopropoxide and acetylacetone of 1:1, 1:2, 1:3 and 1:4 in the precursor solution on the morphological, structural and optical properties of TiO{sub 2} thin film was investigated. These properties were studied using Fourier transformed infrared spectroscopy, scanning electron microscopy, Raman spectroscopy, X-ray diffraction and UV–vis spectroscopy as a function of the molar ratios for the as-deposited thin films and films annealed at temperatures of 700, 800 and 950 °C. Mixed anatase and rutile phases were detected after annealing at 800 °C for 1:1 and 1:2 molar ratios and at 700 °C for 1:3 and 1:4 molar ratios. The optical band gap decreased from 3.45 to 3.02 eV with an increase in the annealing temperature in agreement with corresponding structural changes. - Highlights: • The grain sizes of TiO{sub 2} thin films could be varied over the range of 20 to 210 nm. • TTIP and AcacH ratio affects the transformation process from anatase to rutile. • TiO{sub 2} bandgap decreased from 3.45 to 3.02 eV with an increase in annealing temperature.

  15. Semi-automatic spray pyrolysis deposition of thin, transparent, titania films as blocking layers for dye-sensitized and perovskite solar cells.

    Science.gov (United States)

    Krýsová, Hana; Krýsa, Josef; Kavan, Ladislav

    2018-01-01

    For proper function of the negative electrode of dye-sensitized and perovskite solar cells, the deposition of a nonporous blocking film is required on the surface of F-doped SnO 2 (FTO) glass substrates. Such a blocking film can minimise undesirable parasitic processes, for example, the back reaction of photoinjected electrons with the oxidized form of the redox mediator or with the hole-transporting medium can be avoided. In the present work, thin, transparent, blocking TiO 2 films are prepared by semi-automatic spray pyrolysis of precursors consisting of titanium diisopropoxide bis(acetylacetonate) as the main component. The variation in the layer thickness of the sprayed films is achieved by varying the number of spray cycles. The parameters investigated in this work were deposition temperature (150, 300 and 450 °C), number of spray cycles (20-200), precursor composition (with/without deliberately added acetylacetone), concentration (0.05 and 0.2 M) and subsequent post-calcination at 500 °C. The photo-electrochemical properties were evaluated in aqueous electrolyte solution under UV irradiation. The blocking properties were tested by cyclic voltammetry with a model redox probe with a simple one-electron-transfer reaction. Semi-automatic spraying resulted in the formation of transparent, homogeneous, TiO 2 films, and the technique allows for easy upscaling to large electrode areas. The deposition temperature of 450 °C was necessary for the fabrication of highly photoactive TiO 2 films. The blocking properties of the as-deposited TiO 2 films (at 450 °C) were impaired by post-calcination at 500 °C, but this problem could be addressed by increasing the number of spray cycles. The modification of the precursor by adding acetylacetone resulted in the fabrication of TiO 2 films exhibiting perfect blocking properties that were not influenced by post-calcination. These results will surely find use in the fabrication of large-scale dye-sensitized and perovskite solar

  16. Co3O4 protective coatings prepared by Pulsed Injection Metal Organic Chemical Vapour Deposition

    DEFF Research Database (Denmark)

    Burriel, M.; Garcia, G.; Santiso, J.

    2005-01-01

    of deposition temperature. Pure Co3O4 spinel structure was found for deposition temperatures ranging from 360 to 540 degreesC. The optimum experimental parameters to prepare dense layers with a high growth rate were determined and used to prepare corrosion protective coatings for Fe-22Cr metallic interconnects......Cobalt oxide films were grown by Pulsed Injection Metal Organic Chemical Vapour Deposition (PI-MOCVD) using Co(acac)(3) (acac=acetylacetonate) precursor dissolved in toluene. The structure, morphology and growth rate of the layers deposited on silicon substrates were studied as a function......, to be used in Intermediate Temperature Solid Oxide Fuel Cells. (C) 2004 Elsevier B.V. All rights reserved....

  17. Controlled synthesis and characterization of covellite (CuS) nanoflakes

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, H.T. [Hefei National Laboratory for Physical Sciences at Microscale and Department of Physics, University of Science and Technology of China, Hefei, Anhui 230026 (China); Wu, G. [Hefei National Laboratory for Physical Sciences at Microscale and Department of Physics, University of Science and Technology of China, Hefei, Anhui 230026 (China); Chen, X.H. [Hefei National Laboratory for Physical Sciences at Microscale and Department of Physics, University of Science and Technology of China, Hefei, Anhui 230026 (China)]. E-mail: chenxh@ustc.edu.cn

    2006-08-01

    Trigonal and hexagonal CuS (covellite) nanoflakes with controlled size (10-200 nm, and thickness of 3.6-5 nm) were synthesized through the reaction between copper acetylacetonate and sulfur in oleylamine. Size and shape of the products could be tuned by reaction parameters and reactant concentration. The as-prepared flakes have smooth surfaces and self-assemble face-to-face each other. High-resolution transmission electron microscopy and electron diffraction show that the nanoscale flakes were single-crystal hexagonal covellite. Formation mechanism of the nanoflakes is discussed. UV-vis spectra reveal that the samples have blue-shift absorbance onsets owning to the quantum size effects.

  18. Controlled synthesis and characterization of covellite (CuS) nanoflakes

    International Nuclear Information System (INIS)

    Zhang, H.T.; Wu, G.; Chen, X.H.

    2006-01-01

    Trigonal and hexagonal CuS (covellite) nanoflakes with controlled size (10-200 nm, and thickness of 3.6-5 nm) were synthesized through the reaction between copper acetylacetonate and sulfur in oleylamine. Size and shape of the products could be tuned by reaction parameters and reactant concentration. The as-prepared flakes have smooth surfaces and self-assemble face-to-face each other. High-resolution transmission electron microscopy and electron diffraction show that the nanoscale flakes were single-crystal hexagonal covellite. Formation mechanism of the nanoflakes is discussed. UV-vis spectra reveal that the samples have blue-shift absorbance onsets owning to the quantum size effects

  19. Induced assembly and photoluminescence of lanthanum (Tb, Eu, Dy) complexes/ZnO/polyethylene glycol hybrid phosphors

    Energy Technology Data Exchange (ETDEWEB)

    Yan Bing [Department of Chemistry, Tongji University, Siping Road 1239, Shanghai 200092 (China)]. E-mail: byan@tongji.edu.cn; Chen Xi [Department of Chemistry, Tongji University, Siping Road 1239, Shanghai 200092 (China); Wu Jianhua [Department of Chemistry, Tongji University, Siping Road 1239, Shanghai 200092 (China)

    2007-08-31

    Some novel kinds of hybrid phosphors were assembled with lanthanum (Tb, Eu, Dy) complexes (with four kinds of terbium complexes is 2,4-dihydroxybenzonic acid (DHBA), 1,10-phenanthroline (phen), acetylacetone (AA) and nicotinic acid (Nic), respectively) doped ZnO/PEG particles by co-precipitation approach derived from Zn(CH{sub 3}COO){sub 2} (Zn(AC){sub 2}), NaOH, PEG as precursors at room temperature. The characteristic luminescence spectra for f-f transitions of Tb{sup 3+}, Eu{sup 3+}, Dy{sup 3+} were observed. It is worthy to point out that ZnO is the excellent host for lanthanum ions by the assembly of PEG matrices.

  20. Synthesis of Novel 3H-Quinazolin-4-ones Containing Pyrazolinone, Pyrazole and Pyrimidinone Moieties

    Directory of Open Access Journals (Sweden)

    Abdel-Basset M. Shokr

    2003-04-01

    Full Text Available The diazonium salt of 3-(4-aminophenyl-2-methyl-3H-quinazolin-4-one (2a and its 6-bromo derivative 2b reacted with some active methylene compounds, namely ethyl acetoacetate (3, ethyl cyanoacetate (4 and acetylacetone (5, to afford the corresponding hydrazono quinazolinone derivatives 6-8. Treatment of 6a,b with hydrazine hydrate or phenyl hydrazine in refluxing ethanol afforded the corresponding pyrazolin-5-one derivatives of 3H-quinazolin-4-one 9a-d. Cyclization of 7a,b with hydrazine hydrate yielded the corresponding products 10a,b. Reaction of 8a,b with phenyl hydrazine or with urea afforded the corresponding derivatives 11a,b and 12a,b, respectively. Compounds 6-12 were identified by C,H,N analysis, IR, 1H-NMR, 13C-NMR and mass spectroscopy.

  1. Thermodynamic study of CVD-ZrO2 phase diagrams

    International Nuclear Information System (INIS)

    Torres-Huerta, A.M.; Vargas-Garcia, J.R.; Dominguez-Crespo, M.A.; Romero-Serrano, J.A.

    2009-01-01

    Chemical vapor deposition (CVD) of zirconium oxide (ZrO 2 ) from zirconium acetylacetonate Zr(acac) 4 has been thermodynamically investigated using the Gibbs' free energy minimization method and the FACTSAGE program. Thermodynamic data Cp o , ΔH o and S o for Zr(acac) 4 have been estimated using the Meghreblian-Crawford-Parr and Benson methods because they are not available in the literature. The effect of deposition parameters, such as temperature and pressure, on the extension of the region where pure ZrO 2 can be deposited was analyzed. The results are presented as calculated CVD stability diagrams. The phase diagrams showed two zones, one of them corresponds to pure monoclinic phase of ZrO 2 and the other one corresponds to a mix of monoclinic phase of ZrO 2 and graphite carbon.

  2. Thermodynamic study of CVD-ZrO{sub 2} phase diagrams

    Energy Technology Data Exchange (ETDEWEB)

    Torres-Huerta, A.M., E-mail: atorresh@ipn.m [Research Center for Applied Science and Advanced Technology, Altamira-IPN, Altamira C.P.89600 Tamaulipas (Mexico); Vargas-Garcia, J.R. [Dept of Metallurgical Eng., ESIQIE-IPN, Mexico 07300 D.F. (Mexico); Dominguez-Crespo, M.A. [Research Center for Applied Science and Advanced Technology, Altamira-IPN, Altamira C.P.89600 Tamaulipas (Mexico); Romero-Serrano, J.A. [Dept of Metallurgical Eng., ESIQIE-IPN, Mexico 07300 D.F. (Mexico)

    2009-08-26

    Chemical vapor deposition (CVD) of zirconium oxide (ZrO{sub 2}) from zirconium acetylacetonate Zr(acac){sub 4} has been thermodynamically investigated using the Gibbs' free energy minimization method and the FACTSAGE program. Thermodynamic data Cp{sup o}, DELTAH{sup o} and S{sup o} for Zr(acac){sub 4} have been estimated using the Meghreblian-Crawford-Parr and Benson methods because they are not available in the literature. The effect of deposition parameters, such as temperature and pressure, on the extension of the region where pure ZrO{sub 2} can be deposited was analyzed. The results are presented as calculated CVD stability diagrams. The phase diagrams showed two zones, one of them corresponds to pure monoclinic phase of ZrO{sub 2} and the other one corresponds to a mix of monoclinic phase of ZrO{sub 2} and graphite carbon.

  3. Epoxidation of soybean oil with [MoO{sub 2}(acac){sub 2}]/TBHP Catalytic system in [bmim][PF{sub 6}]; Epoxidacao do oleo de soja com o sistema catalitico [MoO{sub 2}(acac){sub 2}]/TBHP em [bmim][PF{sub 6}

    Energy Technology Data Exchange (ETDEWEB)

    Farias, Maritana [Instituto Federal de Educacao, Ciencia e Tecnologia Sul-rio-grandense, Pelotas, RS (Brazil); Martinelli, Marcia, E-mail: maritana@pelotas.ifsul.edu.br [Universidade Federal do Rio Grande do Sul, Porto Alegre, RS (Brazil). Inst. de Quimica. Dept. de Quimica Inorganica

    2012-07-01

    Epoxidation of soybean oil was investigated using 1-n-butyl-3-methylimidazolium hexafluorophosphate [bmim][PF{sub 6}] ionic liquid as biphasic medium with molybdenum(VI) acetylacetonate complex and tert-butyl hydroperoxide TBHP as oxidizing agent. Reaction conditions were molar ratio TBHP:number of double bonds of oil:catalyst of 100:100:1, reaction temperature of 60 deg C and reaction time between 2 and 24 h. The proposed system showed catalytic activity for epoxidation reactions under tested conditions. Reuse of ionic liquid/catalyst system for epoxidation reactions was also investigated. Evaluation of epoxidation observed in this catalytic system was done by quantitative {sup 1}H NMR data. (author)

  4. Efficient solution route to transparent ZnO semiconductor films using colloidal nanocrystals

    Directory of Open Access Journals (Sweden)

    Satoshi Suehiro

    2016-09-01

    Full Text Available ZnO nanocrystals (NCs were synthesized by heating Zn (II acetylacetonate in oleic acid/oleylamine in the presence of 1,2-hexadecanediol at 220 °C. Transmission electron microscopy (TEM and dynamic light scattering (DLS measurements revealed the formation of monodispersed ZnO NCs of ca. 7 nm. ZnO NC assembled films were fabricated on a glass substrate by deposition with the colloidal ZnO NCs dispersed in toluene. The film composed of the NCs showed good optical transparency in the visible to near-infrared region. A device coupling the ZnO NC film with a p-type Cu2ZnSnS4 (CZTS NC film exhibited an obvious diode-like current–voltage behavior. The results suggest that the transparent ZnO film has a potentiality to be used for an n-type window layer in some optoelectronic applications.

  5. Preparation of ZnO-Al2O3 Particles in a Premixed Flame

    DEFF Research Database (Denmark)

    Jensen, Joakim Reimer; Johannessen, Tue; Wedel, Stig

    2000-01-01

    Zinc oxide (ZnO) and alumina (Al2O3) particles are synthesized by the combustion of their volatilized acetylacetonate precursors in a premixed air-methane flame reactor. The particles are characterized by XRD, transmission electron microscopy, scanning mobility particle sizing and by measurement...... temperature and a decreasing precursor vapour pressure. The combustion of precursor mixtures leads to composite particles consisting of zinc aluminate ZnAl2O4 intermixed with either ZnO or Al2O3 phases. The zinc aluminate particles are dendritic aggregates, resembling the alumina particles, and are evidently...... synthesized to the full extent allowed by the overall precursor composition. The addition of even small amounts of alumina to ZnO increases the specific surface area of the composites significantly, for e.g. zinc aluminate particles to approximately 150 m2/g. The gas-to-particle conversion is initiated...

  6. Lifetime enhanced phosphorescent organic light emitting diode using an electron scavenger layer

    Energy Technology Data Exchange (ETDEWEB)

    Hong, Seokhwan; Kim, Ji Whan; Lee, Sangyeob, E-mail: sy96.lee@samsung.com [Samsung Advanced Institute of Technology, Samsung Electronics Co., Ltd., 130 Samsung-ro, Suwon, Gyeonggi 443-803 (Korea, Republic of)

    2015-07-27

    We demonstrate a method to improve lifetime of a phosphorescent organic light emitting diode (OLED) using an electron scavenger layer (ESL) in a hole transporting layer (HTL) of the device. We use a bis(1-(phenyl)isoquinoline)iridium(III)acetylacetonate [Ir(piq){sub 2}(acac)] doped HTL to stimulate radiative decay, preventing thermal degradation in HTL. The ESL effectively prevented non-radiative decay of leakage electron in HTL by converting non-radiative decay to radiative decay via a phosphorescent red emitter, Ir(piq){sub 2}(acac). The lifetime of device (t{sub 95}: time after 5% decrease of luminance) has been increased from 75 h to 120 h by using the ESL in a phosphorescent green-emitting OLED.

  7. Facile synthesis of deuterated and [14C]labeled analogues of vanillin and curcumin for use as mechanistic and analytical tools

    Science.gov (United States)

    Gordon, Odaine N.; Graham, Leigh A.; Schneider, Claus

    2014-01-01

    Curcumin is a dietary diphenol with antioxidant, antinflammatory and antitumor activity. We describe facile procedures for the synthesis of [14C2]curcumin (4 mCi/mmol), [d6]curcumin, [d3]curcumin, [13C5]curcumin, and [d6]bicyclopentadione, the major oxidative metabolite of curcumin. We also describe synthesis of the labeled building blocks [14C]vanillin, [d3]vanillin, and [13C5]acetylacetone. The overall molar yields of the labeled products were 52% ([14C]) and 47% ([d3]) for vanillin and 25% ([14C2]) and 27% ([d6]) for curcumin. The compounds can be used as radiotracers in biotransformation studies and as isotopic standards for mass spectrometry-based quantification in pharmacokinetic analyses. PMID:24339007

  8. Thermodynamics of alternating spin chains with competing nearest- and next-nearest-neighbor interactions: Ising model

    Science.gov (United States)

    Pini, Maria Gloria; Rettori, Angelo

    1993-08-01

    The thermodynamical properties of an alternating spin (S,s) one-dimensional (1D) Ising model with competing nearest- and next-nearest-neighbor interactions are exactly calculated using a transfer-matrix technique. In contrast to the case S=s=1/2, previously investigated by Harada, the alternation of different spins (S≠s) along the chain is found to give rise to two-peaked static structure factors, signaling the coexistence of different short-range-order configurations. The relevance of our calculations with regard to recent experimental data by Gatteschi et al. in quasi-1D molecular magnetic materials, R (hfac)3 NITEt (R=Gd, Tb, Dy, Ho, Er, . . .), is discussed; hfac is hexafluoro-acetylacetonate and NlTEt is 2-Ethyl-4,4,5,5-tetramethyl-4,5-dihydro-1H-imidazolyl-1-oxyl-3-oxide.

  9. Study by magnetic resonance and relaxation of carbon 13 of some paramagnetic coordination complexes

    International Nuclear Information System (INIS)

    Ronfard-Haret, Jean-Claude

    1977-01-01

    This research thesis reports the study of coordination complexes by using NMR. After a brief recall of the theoretical background required for the processing of experimental data (hyper-fine coupling and magnetic resonance, spin density distribution, chemical displacement, dipolar, scalar and electronic relaxation), the author describes the conditions in which experiments have been performed and presents measurement methods (pulsed nuclear magnetic resonance, relaxation time measurement, determination of hyper-fine coupling constants, spectrometers and reactants). The next chapters address the study of different coordination complexes: [(pyridine-N-oxide) 2 Ni(acetylacetonate) 2 ], carbon 13 in alkyl-anilines-Ni II, complexation of 1- and 2-aminonaphthalene by transition ions, complexation of pyridine-N-oxide by the nickel Ni ++ ion in presence of water

  10. (3,5-Dimethylpyrazol-1-yl-[4-(1-phenyl-1H-pyrazolo[3,4-d]pyrimidin-4-ylaminophenyl]methanone

    Directory of Open Access Journals (Sweden)

    Rania B. Bakr

    2016-11-01

    Full Text Available In an attempt to enhance cytotoxic activity of pyrazolo[3,4-d]pyrimidine core, we synthesized (3,5-dimethylpyrazol-1-yl-[4-(1-phenyl-1H-pyrazolo[3,4-d]pyrimidin-4-ylaminophenyl]methanone (4 by reacting 4-(1-phenyl-1H-pyrazolo[3,4-d]pyrimidin-4-ylaminobenzohydrazide (3 with acetylacetone. Antiproliferative activity of this compound was screened against breast (MCF-7, colon (HCT-116, and liver (HEPG-2 cancer cell lines. The tested compound exhibited cytotoxic activity with IC50 = 5.00–32.52 μM. Moreover, inhibitory activity of this compound was evaluated against the epidermal growth factor receptor (EGFR, the fibroblast growth factor receptor (FGFR, the insulin receptor (IR, and the vascular endothelial growth factor receptor (VEGFR. This target compound showed potent inhibitory activity, especially against FGFR with IC50 = 5.18 μM.

  11. Triphenylsilane-substituted arenes as host materials for use in green phosphorescent organic light emitting diodes

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Jwajin; Lee, Kum Hee; Kim, Young Seok; Lee, Hyun Woo [Department of Chemistry, Sungkyunkwan University, Suwon 440-746 (Korea, Republic of); Lee, Ho Won [Department of Information Display, Hongik University, Seoul 121-791 (Korea, Republic of); Kim, Young Kwan, E-mail: kimyk@hongik.ac.kr [Department of Information Display, Hongik University, Seoul 121-791 (Korea, Republic of); Yoon, Seung Soo, E-mail: ssyoon@skku.edu [Department of Chemistry, Sungkyunkwan University, Suwon 440-746 (Korea, Republic of)

    2016-03-15

    We demonstrated triphenylsilane-substituted arenes (1–4) as host materials for green phosphorescent organic light-emitting diodes. Particularly, a device using 9,9-dimethyl-2-(triphenylsilyl)-7-[4-(triphenylsilyl)phenyl]-9H-fluorene (compound 4) as the host material with the green phosphorescence dopant bis[2-(1,1′,2′,1′′-terphen-3-yl)pyridinato-C,N]iridium(III) (acetylacetonate) showed the efficient green emission with an external quantum efficiency of 4.64%, a power efficiency of 7.2 lm/W and luminous efficiency of 16.6 cd/A at 20 mA/cm{sup 2}, respectively, with the Commission International de L’Eclairage chromaticity coordinates of (0.33, 0.59) at 8.0 V.

  12. Thin films of In2O3 by atomic layer deposition using In(acac)3

    International Nuclear Information System (INIS)

    Nilsen, O.; Balasundaraprabhu, R.; Monakhov, E.V.; Muthukumarasamy, N.; Fjellvag, H.; Svensson, B.G.

    2009-01-01

    Thin films of indium oxide have been deposited using the atomic layer deposition (ALD) technique using In(acac) 3 (acac = acetylacetonate, pentane-2,4-dione) and either H 2 O or O 3 as precursors. Successful growth using In(acac) 3 is contradictory to what has been reported previously in the literature [J.W. Elam, A.B.F. Martinson, M.J. Pellin, J.T. Hupp, Chem. Mater. 18 (2006) 3571.]. Investigation of the dependence of temperature on the deposition shows windows where the growth rates are relatively unaffected by temperature in the ranges 165-200 o C for In(acac) 3 and H 2 O, 165-225 o C for In(acac) 3 and O 3 . The growth rates obtained are of the order 20 pm/cycle for In(acac) 3 and H 2 O, 12 pm/cycle for In(acac) 3 .

  13. 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.

  14. High mass-resolution electron-ion-ion coincidence measurements on core-excited organic molecules

    CERN Document Server

    Tokushima, T; Senba, Y; Yoshida, H; Hiraya, A

    2001-01-01

    Total electron-ion-ion coincidence measurements on core excited organic molecules have been carried out with high mass resolution by using multimode (reflectron/linear) time-of-flight mass analyzer. From the ion correlation spectra of core excited CH sub 3 OH and CD sub 3 OH, the reaction pathway to form H sub 3 sup + (D sub 3 sup +) is identified as the elimination of three H (D) atoms from the methyl group, not as the inter-group (-CH sub 3 and -OH) interactions. In a PEPIPICO spectrum of acetylacetone (CH sub 3 COCH sub 2 COCH sub 3) measured by using a reflectron TOF, correlations between ions up to mass number 70 with one-mass resolution was recorded.

  15. Electrochemical synthesis and investigation of uranium β-diketonates

    International Nuclear Information System (INIS)

    Kostyuk, N.N.; Kolevich, T.A.; Shirokij, V.L.; Umrejko, D.S.; AN Belorusskoj SSR, Minsk

    1989-01-01

    Using the method of anode solution of uranium in a cell without a diaphragm in the presence of acetylacetone (NAA) and benzoylacetone (NBA), complexes U(AA) 4 , U(BA) 4 , UO 2 (AA) 2 · NAA and UO 2 (BA) 2 (NBA) 0.5 are prepared. The U(4) complexes are formed in an inert medium, and U(6) complexes - in an oxidizing medium. The current efficiencies are 45-70%. The compounds are identified and studied by methods of chemical analysis and IR spectroscopy. It is shown that in the composition UO 2 (BA) 2 (NBA) 0.5 BA ligands form quasiaromatic metallocycles, and a NBA ligand is of a bridge type

  16. Application of the zone-melting technique to metal chelate systems-VI A new apparatus for zone-melting chromatography.

    Science.gov (United States)

    Maeda, S; Kobayashi, H; Ueno, K

    1973-07-01

    An improved apparatus has been constructed for zone-melting chromatography. An essential feature of the apparatus is that the length of the molten zone can be kept constant during a zone-melting operation, by employing heating and cooling compartments which are separated from each other by double partition plates. Each compartment is heated or cooled with jets of hot or cold air. The apparatus is suitable for organic materials melting in the range between 40 degrees and 180 degrees . The distribution of metal ion along the column after zone melting of copper acetylacetonate in 2-methoxynaphthalene was a smooth curve. The plot of the position of maximum concentration, x(max), against the number of zone passes, n, gave a relationship in accordance with theoretical prediction.

  17. Convenient preparation of ITO nanoparticles inks for transparent conductive thin films

    International Nuclear Information System (INIS)

    Ito, Daisuke; Masuko, Keiichiro; Weintraub, Benjamin A.; McKenzie, Lallie C.; Hutchison, James E.

    2012-01-01

    Tin-doped indium oxide (ITO) nanoparticles are useful precursors to transparent electrodes in a variety of technologically important applications. We synthesized ITO nanoparticles from indium and tin acetylacetonates in oleyl alcohol using a novel temperature ramp profile. The monodispersed ITO nanoparticles have an average diameter of 8.6 nm and form dense, flat films by simple spin coating. The thickness of the film can be controlled by varying the number of additional depositions. The resulting ITO film is transparent and has a resistivity of 7 × 10 −3 Ω cm after sintering at 300 °C. Using a suitable solvent, it is possible to coat high-aspect-ratio structures with ITO nanoparticles. This approach to ITO coatings is greener and offers a number of advantages for transparent electrodes because it is highly versatile, easily scalable, and supports low-cost manufacturing.

  18. SPECTROGRAPHIC DETERMINATION OF BERYLLIUM IN OILFIELD WATERS USING A PLASMA ARC

    Energy Technology Data Exchange (ETDEWEB)

    Collins, A. G.; Pearson, C. A.

    1963-10-15

    Geochemical studies of the distribution of the trace, minor, and major constituents of oilfield waters aid in the exploration for petroleum and other minerals, determination of the origin and distribution of oilfield waters and petroleum, and location of casing leaks and of water pollution sources. The determination of the beryllium and related data should be useful in these studies. An emission spectrographic method utilizing a plasma arc assembly for determining beryllium in oilfield waters, with a sensitivity permitting detection of less than 1 ppb, was developed. Beryllium was extracted from synthetic and natural oilfield waters with chloroform and acetylacetone. The extracts were aspirated directly into the plasma arc, and the beryllium emission intensity was recorded on photographic plates. (auth)

  19. Titration of thorium and rare earths with ethylenediaminetetraacetic acid using semimethylthymol blue by visual end-point indication

    International Nuclear Information System (INIS)

    Hafez, M.A.H.; Kenawy, I.M.M.; Ramadan, M.A.M.

    1994-01-01

    The precision and accuracy attainable in direct complexometric titrations of Thsup(4+) consecutively with either lighter (La 3+ , Nd 3+ , Sm 3+ , Eu 3+ or Gd 3+ ) or heavier lanthanides (Dy 3+ ) in different proportions using Semimethylthymol Blue (SMTB) as a metallochromic indicator and disodium dihydrogen ethylenediaminetetraacetate were studied. Thorium (IV) was titrated at pH 2, the Ph was adjusted to 5.5-6.0 by adding hexamethylenetetramine (hexamine) buffer and acetylacetone-acetone solution and La 3+ (or Nd 3+ , Sm 3+ , Eu 3+ , Gd 3+ or Dy 3+ ) was then titrated. A comparison of the indicators SMTB and Methylthymol Blue (MTB) for successive titrations of Th 4+ and any of the rare earth ions was carried out. The proposed titration method was applied successfully to some naturally occurring ores and minerals containing thorium and some lanthanides and the results were satisfactory. (Author)

  20. Preparation of Pt Nanocatalyst on Carbon Materials via a Reduction Reaction of a Pt Precursor in a Drying Process.

    Science.gov (United States)

    Lee, Jae-Young; Lee, Woo-Kum; Rim, Hyung-Ryul; Joung, Gyu-Bum; Weidner, John W; Lee, Hong-Ki

    2016-06-01

    Platinum (Pt) nanocatalyst for a proton-exchange membrane fuel cell (PEMFC) was prepared on a carbon black particle or a graphite particle coated with a nafion polymer via a reduction of platinum(II) bis(acetylacetonate) denoted as Pt(acac)2 as a Pt precursor in a drying process. Sublimed Pt(acac)2 adsorbed on the nafion-coated carbon materials was reduced to Pt nanoparticles in a glass reactor at 180 degrees C of N2 atmosphere. The morphology of Pt nanoparticles on carbon materials was observed by scanning electron microscopy (SEM) and the distribution of Pt nanoparticles was done by transmission electron microscopy (TEM). The particle size was estimated by analyzing the TEM image using an image analyzer. It was found that nano-sized Pt particles were deposited on the surface of carbon materials, and the number density and the average particle size increased with increasing reduction time.

  1. Some regularities of Ce(3) and Ce(4) stabilization in their compounds with β-diketones

    International Nuclear Information System (INIS)

    Pechurova, N.I.; Martynenko, L.I.; Snezhko, N.I.; Anufrieva, S.I.

    1985-01-01

    Adduct formation of cerium (3) and cerium (4) β-diketonates (acetylacetonate, benzoylacetonate, dibenzoylmethanate and thenoyltrifluoroacetonate) with oxygen- and nitrogen-donor ligands (Q-α, α'-dipyridyl, o-phenanthroline, trioctylphosphine oxide and triphenylphosphine oxide) is studied. The compounds obtained as a results of the reactions are studied by means of IR-spectroscopic, derivatographic and X-ray phase methods. It is concluded that composition and thermodynamic stability of adducts of Ce(3) tris-β-diketonates are determined by correlation of donor properties of the basis and additional ligand and stability of adducts to oxidation - as well as by their solubility. Introduction of the additional ligand to the system Ce(4)-β-diketones even in the presence of air oxygen stabilizes Ce(3) and destabilizes Ce(4)

  2. Investigation into kinetics of redox interaction in the system Ce(4). beta. -diketonate-additional ligand

    Energy Technology Data Exchange (ETDEWEB)

    Anufrieva, S.I.; Snezhko, N.I.; Pechurova, N.I.; Martynenko, L.N.; Spitsyn, V.I. (Moskovskij Gosudarstvennyj Univ. (USSR))

    1981-07-01

    The rate of reduction of ..beta..-diketonate complexes of Ce(4) to Ce(3) ..beta..-diketonates in benzene solution in the presence and in the absence of additional ligands is studied using spectrophotometry. The rate of reduction of Ce(4) ..beta..-diketonates increases in the series Ce(TTFA)/sub 4/acetylacetone). The studied phosphorus-containing additional ligands as to their effect on the rate of Ce (4) reduction can be arranged in the following order: trioctylphosphine oxide>triphenylphosphine oxide>tributyl phosphate.

  3. Shape control of the magnetic iron oxide nanoparticles under different chain length of reducing agents

    International Nuclear Information System (INIS)

    Ngoi, Kuan Hoon; Chia, Chin-Hua; Zakaria, Sarani; Chiu, Wee Siong

    2015-01-01

    We report on the effect of using reducing agents with different chain-length on the synthesis of iron oxide nanoparticles by thermal decomposition of iron (III) acetylacetonate in 1-octadecene. This modification allows us to control the shape of nanoparticles into spherical and cubic iron oxide nanoparticles. The highly monodisperse 14 nm spherical nanoparticles are obtained under 1,2-dodecanediol and average 14 nm edge-length cubic iron oxide nanoparticles are obtained under 1,2-tetradecanediol. The structural characterization such as transmission electron microscope (TEM) and X-ray diffraction (XRD) shows similar properties between two particles with different shapes. The vibrating sample magnetometer (VSM) shows no significant difference between spherical and cubic nanoparticles, which are 36 emu/g and 37 emu/g respectively and superparamagnetic in nature

  4. Shape control of the magnetic iron oxide nanoparticles under different chain length of reducing agents

    Energy Technology Data Exchange (ETDEWEB)

    Ngoi, Kuan Hoon; Chia, Chin-Hua, E-mail: chia@ukm.edu.my; Zakaria, Sarani [School of Applied Physics, Faculty Science and Technology, University Kebangsaan Malaysia 43600 UKM Bangi, Selangor (Malaysia); Chiu, Wee Siong [Low Dimensional Materials Research Centre, Department of Physics, Faculty of Science, University of Malaya, 50603 Lembah Pantai, Kuala Lumpur (Malaysia)

    2015-09-25

    We report on the effect of using reducing agents with different chain-length on the synthesis of iron oxide nanoparticles by thermal decomposition of iron (III) acetylacetonate in 1-octadecene. This modification allows us to control the shape of nanoparticles into spherical and cubic iron oxide nanoparticles. The highly monodisperse 14 nm spherical nanoparticles are obtained under 1,2-dodecanediol and average 14 nm edge-length cubic iron oxide nanoparticles are obtained under 1,2-tetradecanediol. The structural characterization such as transmission electron microscope (TEM) and X-ray diffraction (XRD) shows similar properties between two particles with different shapes. The vibrating sample magnetometer (VSM) shows no significant difference between spherical and cubic nanoparticles, which are 36 emu/g and 37 emu/g respectively and superparamagnetic in nature.

  5. Fabrication of highly luminescent InP/Cd and InP/CdS quantum dots

    International Nuclear Information System (INIS)

    Park, Jaehyun; Kim, Sunghoon; Kim, Sungwoo; Yu, Seung Tack; Lee, Bunyeoul; Kim, Sang-Wook

    2010-01-01

    Highly luminescent InP/Cd and InP/CdS core-shell QDs were fabricated by sequential addition of cadmium acetylacetonate and dodecanethiol to InP core solutions, which showed a red-shift in absorption and emission. ICP measurement revealed the existence of cadmium and TEM images showed the increased size of InP/CdS QDs. PXRD data identified zinc blend structures of InP and InP/CdS QDs, which indexed to the (1 1 1), (2 2 0) and (3 1 1) planes. The slight shift of peaks between InP and InP/CdS QDs can demonstrate the existence of CdS shell structures.

  6. Characterization of Cr2O3 thin films obtained by chemical vapor deposition

    International Nuclear Information System (INIS)

    Pillis, M.F.; Galego, E.; Serna, M.M.; Correa, O.V.; Ramanathan, L.V.; Franco, A.C.

    2010-01-01

    The goal of this work was the synthesis and characterization of Cr 2 O 3 thin films, obtained by chemical vapor deposition, using chromium acetylacetonate as chromium precursor. The growth of the films was carried out in a conventional horizontal MOCVD equipment, under pressures varying from 2 to 10 mbar, and temperature of 600 deg C. It was observed that the growth of the films only occurs when oxygen is present in the atmosphere. Under growth pressures of 2 and 5 mbar the growth takes place but under 10 mbar of pressure the precursor is dragged and the growth does not occur. The characterization of the films was performed by using scanning electron microscopy and X-ray diffraction. The films presented a columnar structure, and thickness varying from 40 to 250 nm. The influence of some process parameters is discussed. (author)

  7. Low-temperature metal-oxide thin-film transistors formed by directly photopatternable and combustible solution synthesis.

    Science.gov (United States)

    Rim, You Seung; Lim, Hyun Soo; Kim, Hyun Jae

    2013-05-01

    We investigated the formation of ultraviolet (UV)-assisted directly patternable solution-processed oxide semiconductor films and successfully fabricated thin-film transistors (TFTs) based on these films. An InGaZnO (IGZO) solution that was modified chemically with benzoylacetone (BzAc), whose chelate rings decomposed via a π-π* transition as result of UV irradiation, was used for the direct patterning. A TFT was fabricated using the directly patterned IGZO film, and it had better electrical characteristics than those of conventional photoresist (PR)-patterned TFTs. In addition, the nitric acid (HNO3) and acetylacetone (AcAc) modified In2O3 (NAc-In2O3) solution exhibited both strong UV absorption and high exothermic reaction. This method not only resulted in the formation of a low-energy path because of the combustion of the chemically modified metal-oxide solution but also allowed for photoreaction-induced direct patterning at low temperatures.

  8. Effects of the addition of H2O and NH4OH in the optical and structural properties of the thin films of Y2O3 deposited by pyrolytic spray

    International Nuclear Information System (INIS)

    Alarcon F, G.; Carvajal V, R.; Aguilar F, M.; Falcony, C.

    2005-01-01

    In this work we studied the optical and structural properties of yttrium oxide thin films deposited by spray pyrolysis. Yttrium acetylacetonate was used as raw material and N, N-DMF was used as solvent. The films were deposited on Si (100) and Si (111) substrates at temperatures of 400, 450, 500 and 550 C. The optical and structural characteristics of the films were dramatically improved when a mist of H 2 O and/or NH 4 0H was simultaneously added during deposition of the films. A refraction index up to 1.88, and deposition rates lower than 10 A/sec were obtained in the films. Infrared spectroscopy measurements indicate that the films resulted free from -OH bonds. X-ray diffraction patterns reveal that the films were polycrystalline. In addition, the relative chemical composition of the films was determined by Energy Dispersive Spectroscopy and the surface morphology was analyzed in the Atomic Force Microscope. (Author)

  9. Synthesis of Pyrroloquinones via a CAN Mediated Oxidative Free Radical Reaction of 1,3-Dicarbonyl Compounds with Aminoquinones

    Directory of Open Access Journals (Sweden)

    Thao Nguyen

    2013-01-01

    Full Text Available Pyrroloquinone ring systems are important structural units present in many biologically active molecules including a number of marine alkaloids. For example, they are found in a series of marine metabolites, such as tsitsikammamines, zyzzyanones, wakayin, and terreusinone. Several of these alkaloids have exhibited antimicrobial, antimalarial, antifungal, antitumor, and photoprotecting activities. Synthesis of pyrroloquinone unit is the key step in the synthesis of many of these important organic molecules. Here, we present a ceric (IV ammonium nitrate (CAN mediated oxidative free radical cyclization reaction of 1,3-dicarbonyl compounds with aminoquinones as a facile methodology for making various substituted pyrroloquinones. 1,3-dicarbonyl compounds used in this study are ethyl acetoacetate, acetylacetone, benzoyl acetone, and N,N-dimethyl acetoacetamide. The aminoquinones used in this study are 2-(benzylaminonaphthalene-1,4-dione and 6-(benzylamino-1-tosyl-1H-indole-4,7-dione. The yields of the synthesized pyrroloquinones ranged from 23–91%.

  10. Controllable synthesis of helical, straight, hollow and nitrogen-doped carbon nanofibers and their magnetic properties

    Energy Technology Data Exchange (ETDEWEB)

    Li, Xun [State Key Laboratory of Coordination Chemistry, Nanjing National Laboratory of Microstructure, School of Chemistry and Chemical Engineering, Nanjing University, Nanjing 210093 (China); State Key Laboratory of Soil and Sustainable Agriculture, Institute of Soil Science, Chinese Academy of Sciences, Nanjing 210008 (China); Xu, Zheng, E-mail: zhengxu@nju.edu.cn [State Key Laboratory of Coordination Chemistry, Nanjing National Laboratory of Microstructure, School of Chemistry and Chemical Engineering, Nanjing University, Nanjing 210093 (China)

    2012-12-15

    Graphical abstract: The helical, straight and hollow carbon nanofibers can be selectively synthesized by adjusting either the reaction temperature or feed gas composition. Display Omitted Highlights: ► CNFs were synthesized via pyrolysis of acetylene on copper NPs. ► The helical, straight, hollow and N-doped CNFs can be selectively synthesized. ► The growth mechanism of different types of CNFs was proposed. -- Abstract: Carbon nanofibers (CNFs) with various morphologies were synthesized by catalytic pyrolysis of acetylene on copper nanoparticles which were generated from the in situ decomposition of copper acetylacetonate. The morphology of the pristine and acid-washed CNFs was investigated by field emission scanning electron microscope and high-resolution transmission electron microscope. Helical, straight and hollow CNFs can be selectively synthesized by adjusting either the reaction temperature or feed gas composition. The growth mechanism for these three types of CNFs was proposed.

  11. N-[3-(2,6-Dimethylanilino-1-methylbut-2-enylidene]-2,6-dimethylanilinium chlorideThis paper is dedicated to Professor Dr Dr mult. h.c. Herbert W. Roesky.

    Directory of Open Access Journals (Sweden)

    Víctor M. Jiménez-Pérez

    2009-07-01

    Full Text Available The title salt, C21H27N2+·Cl− resulted from the condensation between 2,6-dimethylaniline and acetylacetone in acidified ethanol. The bulky cation is stabilized in a β-iminoenamine tautomeric form, and presents a W-shaped conformation. The benzene rings are arranged almost parallel, with a dihedral angle of 6.58 (4° between the mean planes. Both N—H groups in the cation form strong hydrogen bonds with two symmetry-related chloride anions. The resulting supramolecular structure is a one dimensional polymer running along [001], alternating cations and anions. The π–π interaction observed in the molecule, characterized by a centroid–centroid separation of 4.298 (4 Å, is thus extended to the chains, with separations of 5.222 (4 Å between benzene rings of neighbouring cations in the crystal.

  12. Reversible-Deactivation Radical Polymerization of Methyl Methacrylate Induced by Photochemical Reduction of Various Copper Catalysts

    Directory of Open Access Journals (Sweden)

    Jaroslav Mosnáček

    2014-11-01

    Full Text Available Photochemically mediated reversible-deactivation radical polymerization of methyl methacrylate was successfully performed using 50–400 ppm of various copper compounds such as CuSO4·5H2O, copper acetate, copper triflate and copper acetylacetonate as catalysts. The copper catalysts were reduced in situ by irradiation at wavelengths of 366–546 nm, without using any additional reducing agent. Bromopropionitrile was used as an initiator. The effects of various solvents and the concentration and structure of ligands were investigated. Well-defined polymers were obtained when at least 100 or 200 ppm of any catalyst complexed with excess tris(2-pyridylmethylamine as a ligand was used in dimethyl sulfoxide as a solvent.

  13. Cyanoacetanilides intermediates in heterocyclic synthesis. Part 6: Preparation of some hitherto unknown 2-oxopyridine, bipyridine, isoquinoline and chromeno[3,4-c]pyridine containing sulfonamide moiety

    Directory of Open Access Journals (Sweden)

    Yousry A. Ammar

    2014-11-01

    Full Text Available Treatment of cyanoacetanilide derivative 1 with tetracyanoethylene (2 in dioxane/triethylamine furnished 2-pyridone derivative 6. Aminopyridine 9 was obtained by cyclization of compound 1 with ketene dithioacetal 7/EtONa. Cyclocondensation of 1 with malononitrile and/or acetylacetone (1:1 M ratio gave pyridine derivatives 11 and 13. Ternary condensation of compound 1, aliphatic aldehydes and malononitrile (1:1:1 M ratio yielded the 2-pyridones 20a and b. Bipyridines 22a–c were prepared by refluxing of compound 21 with active methylene reagents. Cyclization of chromene derivatives 24 and 28 with malononitrile produced the novel chromeno[3,4-c]pyridine 26 and pyrano[3′,2′:6,7]chromeno[3,4-c]pyridine 29.

  14. Method of reducing radioactivity in nuclear reactors

    International Nuclear Information System (INIS)

    Koshino, Yasuo

    1987-01-01

    Purpose: To prevent increase of radiation dose ratio in primary coolant circuit pipeways of nuclear reactor and reduce operators' exposure dose upon periodical inspection, etc. Method: β-diketone such as acetylacetone is added in a predetermined amount to reactor cooling water. β-diketone dissolves to catch metal ions and iron oxides as the main ingredient of cruds. The resultant β-diketone complex of metals is slightly water soluble neutron molecule, and the total metal amount in the reactor coolant is at a concentration of less than 10 ppb and completely dissolved in water. Accordingly, deposition of clads in the coolant to pipeways can be prevented thereby enabling to prevent the increase in the radiation dose ratio in the pipeways and thus reduce the operators' exposure dose. (Takahashi, M.)

  15. Well-Defined Macromolecules Using Horseradish Peroxidase as a RAFT Initiase.

    Science.gov (United States)

    Danielson, Alex P; Bailey-Van Kuren, Dylan; Lucius, Melissa E; Makaroff, Katherine; Williams, Cameron; Page, Richard C; Berberich, Jason A; Konkolewicz, Dominik

    2016-02-01

    Enzymatic catalysis and control over macromolecular architectures from reversible addition-fragmentation chain transfer polymerization (RAFT) are combined to give a new method of making polymers. Horseradish peroxidase (HRP) is used to catalytically generate radicals using hydrogen peroxide and acetylacetone as a mediator. RAFT is used to control the polymer structure. HRP catalyzed RAFT polymerization gives acrylate and acrylamide polymers with relatively narrow molecular weight distributions. The polymerization is rapid, typically exceeding 90% monomer conversion in 30 min. Complex macromolecular architectures including a block copolymer and a protein-polymer conjugate are synthesized using HRP to catalytically initiate RAFT polymerization. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  16. Synthesis and functionalization of biocompatible Tb:CePO{sub 4} nanophosphors with spindle-like shape

    Energy Technology Data Exchange (ETDEWEB)

    Rodriguez-Liviano, Sonia; Aparicio, Francisco J.; Becerro, Ana I. [Instituto de Ciencia de Materiales de Sevilla (CSIC-US) (Spain); Garcia-Sevillano, Jorge; Cantelar, Eugenio [C-04. Universidad Autonoma de Madrid, Dpto. Fisica de Materiales (Spain); Rivera, Sara; Hernandez, Yulan; Fuente, Jesus M. de la [Universidad de Zaragoza, Instituto de Nanociencia de Aragon (Spain); Ocana, Manuel, E-mail: mjurado@icmse.csic.es [Instituto de Ciencia de Materiales de Sevilla (CSIC-US) (Spain)

    2013-02-15

    Monoclinic Tb:CePO{sub 4} nanophosphors with a spindle-like morphology and tailored size (in the nanometer and micrometer range) have been prepared through a very simple procedure, which consists of aging, at low temperature (120 Degree-Sign C), ethylene glycol solutions containing only cerium and terbium acetylacetonates and phosphoric acid, not requiring the addition of surfactants or capping agents. The influence of the heating mode (conventional convection oven or microwave oven) and the Tb doping level on the luminescent, structural and morphological features of the precipitated nanoparticles have also been analyzed. This study showed that microwave-assisted heating resulted in an important beneficial effect on the luminescent properties of these nanophosphors. Finally, a procedure for the functionalization of the Tb:CePO{sub 4} nanoparticles with aspartic-dextran is also reported. The functionalized nanospindles presented negligible toxicity for Verocells, which along with theirs excellent luminescent properties, make them suitable for biomedical applications.

  17. MnO-carbon hybrid nanofiber composites as superior anode materials for lithium-ion batteries

    International Nuclear Information System (INIS)

    Wang, Jian-Gan; Yang, Ying; Huang, Zheng-Hong; Kang, Feiyu

    2015-01-01

    MnO-carbon hybrid nanofiber composites are fabricated by electrospinning polyimide/manganese acetylacetonate precursor and a subsequent carbonization process. The composition, phase structure and morphology of the composites are characterized by scanning and transmission electron microscopy, X-ray diffraction and thermogravimetric analysis. The results indicate that the composites exhibit good nanofibrous morphology with MnO nanoparticles uniformly encapsulated by carbon nanofibers. The hybrid nanofiber composites are used directly as freestanding anodes for lithium-ion batteries to evaluate their electrochemical properties. It is found that the optimized MnO-carbon nanofiber composite can deliver a high reversible capacity of 663 mAh g −1 , along with excellent cycling stability and good rate capability. The superior performance enables the composites to be promising candidates as an anode alternative for high-performance lithium-ion batteries

  18. Filmes de titânio-silício preparados por "spin" e "dip-coating"

    Directory of Open Access Journals (Sweden)

    Nassar Eduardo J.

    2003-01-01

    Full Text Available The conditions for the preparation of luminescent materials, consisting of Eu3+ ions entrapped in a titanium matrix, in the forma of a thin film, using the sol-gel process, are described. The films were obtained from sols prepared with TEOS and TEOT, in the presence of acetylacetone as the hidrolysis-retarding agent, using the dip-coating and spin-coating techniques. The influence of these techniques on the films based on titanium and silicon are presented. The Eu3+ was used as a luminescent probe. The films have been characterized by luminescence, reflection and transmittance. The thickness of the films could be related to the preparation procedure. Transparent thin films have been prepared by dip-coating technique.

  19. Synthesis and characterization of some new molybdenum(V) complexes

    International Nuclear Information System (INIS)

    Kamenar, Boris; Korpar-Choling, Branka; Cindrich, Marina; Matkovich-Chalogovich, Dubravka; Penavich, Maja

    1997-01-01

    The molybdenium(V) complexes of the types Mo 2 O 3 L 4 (L = acetylacetone or dibenzolymethane), Mo 2 O 4 L 2 L' 2 solvated with L' (L = dibenzolymethane, L' = morpholine or thiomorpholine), and NR-morphH)[Mo 8 O 2 0LL' 3 ] (R = methyl or ethyl, L = dibenzolymethane, L' = NR-morpholine) have been synthesized for the first time. All were characterized by chemical analyses, IR spectra and magnethochemical measurements. Crystal structure of [Mo 2 O 4 (dbm) 2 (morph) 2 ].(morph) has been determined by X-ray diffraction technique. Complex is dinuclear containing the molybdenium atoms in a distorted octahedral geometry. Each molybdenium atom is surrounded by two bridging oxo-oxygen atoms, two oxygen atoms from one bidentately coordinated dibenzolymethane ligand, one nitrogen atom from morpholine molecule and one terminal oxo-oxygen atom. The solvated morpholine molecule is disordered around the diad axis. (author)

  20. Size-controlled synthesis of nickel nanoparticles

    International Nuclear Information System (INIS)

    Hou, Y.; Kondoh, H.; Ohta, T.; Gao, S.

    2005-01-01

    A facile reduction approach with nickel acetylacetonate, Ni(acac) 2 , and sodium borohydride or superhydride leads to monodisperse nickel nanoparticles in the presence of hexadecylamine (HDA) and trioctylphosphine oxide (TOPO). The combination of HDA and TOPO used in the conventional synthesis of semiconductor nanocrystals also provides better control over particle growth in the metal nanoparticle synthesis. The size of Ni nanoparticles can be readily tuned from 3 to 11 nm, depending on the ratio of HDA to TOPO in the reaction system. As-synthesized Ni nanoparticles have a cubic structure as characterized by power X-ray diffraction (XRD), selected-area electron diffraction (SAED). Transmission electron microscopy (TEM) images show that Ni nanoparticles have narrow size distribution. SQUID magnetometry was also used in the characterization of Ni nanoparticles. The synthetic procedure can be extended to the preparation of high quality metal or alloy nanoparticles

  1. Phosphorescent Molecularly Doped Light-Emitting Diodes with Blended Polymer Host and Wide Emission Spectra

    Directory of Open Access Journals (Sweden)

    Jun Wang

    2013-01-01

    Full Text Available Stable green light emission and high efficiency organic devices with three polymer layers were fabricated using bis[2-(4′-tert-butylphenyl-1-phenyl-1H-benzoimidazole-N,C2′] iridium(III (acetylacetonate doped in blended host materials. The 1 wt% doping concentration showed maximum luminance of 7841 cd/cm2 at 25.6 V and maximum current efficiency of 9.95 cd/A at 17.2 V. The electroluminescence spectra of devices indicated two main peaks at 522 nm and 554 nm coming from phosphor dye and a full width at half maximum (FWHM of 116 nm. The characteristics of using blended host, doping iridium complex, emission spectrum, and power efficiency of organic devices were investigated.

  2. CVD synthesis of HTSC films using volatile coordination compounds

    International Nuclear Information System (INIS)

    Volkov, S.V.; Zub, V.Y.; Balakshina, O.N.; Mazurenko, E.A.

    1995-01-01

    Thin HTSC films of YBa 2 Cu 3 O 7-x with high c-axis orientation have been grown using PE MOCVD technique and adducts of copper, yttrium and barium acetylacetonate with α,α'- dipyridyl as precursors. In-situ films were deposited in N 2 and O 2 gas reactant mixture at reduced substrate temperatures. HTSC films prepared on SrTiO 3 , ZrO 2 (Y) and MgO substrates have rather high electric characteristics (e.g. j c ∼10 4 - 10 5 A/cm 2 ). The problem of β-diketonate adducts using as precursors for plasma enhanced chemical vapor deposition of superconductive films was discussed. (orig.)

  3. Organic Light-Emitting Diodes Based on Phthalimide Derivatives: Improvement of the Electroluminescence Properties

    Directory of Open Access Journals (Sweden)

    Frédéric Dumur

    2018-03-01

    Full Text Available In this study, a phthalimide-based fluorescent material has been examined as a green emitter for multilayered organic light-emitting diodes (OLEDs. By optimizing the device stacking, a maximum brightness of 28,450 cd/m2 at 11.0 V and a maximum external quantum efficiency of 3.11% could be obtained. Interestingly, OLEDs fabricated with Fluo-2 presented a 20-fold current efficiency improvement compared to the previous results reported in the literature, evidencing the crucial role of the device stacking in the electroluminescence (EL performance of a selected emitter. Device lifetime was also examined and an operational stability comparable to that reported for a standard triplet emitter i.e., bis(4-methyl-2,5-diphenyl-pyridineiridium(III acetylacetonate [(mdppy2Iracac] was evidenced.

  4. Preparation and characterization of electroluminescent devices based on complexes of {beta}-diketonates of Tb{sup 3+}, Eu{sup 3+}, Gd{sup 3+} ions with macrocyclic ligands and UO{sub 2}{sup 2+} films; Preparacao e caracterizacao de dispositivos eletroluminescentes de complexos de {beta}-dicetonados de ions Tb{sup 3+}, Eu{sup 3+}, Gd{sup 3+} com ligantes macrociclicos e filmes de UO{sub 2}{sup 2+}

    Energy Technology Data Exchange (ETDEWEB)

    Gibelli, Edison Bessa

    2010-07-01

    Complexes containing Rare Earth ions are of great interest in the manufacture of electro luminescent devices as organic light emitting devices (OLED). These devices, using rare earth trivalent ions (TR{sup 3+}) as emitting centers, show high luminescence with extremely fine spectral bands due to the structure of their energy levels, long life time and high quantum efficiency. This work reports the preparation of Rare Earth {beta}-diketonate complexes (Tb{sup 3+}, Eu{sup 3+} and Gd{sup 3+}) and (tta - thenoyltrifluoroacetonate and acac - acetylacetonate) containing a ligand macrocyclic crown ether (DB18C6 - dibenzo18coroa6) and polymer films of UO{sub 2}{sup 2+}. The materials were characterized by complexometric titration with EDTA, CH elemental analysis, near infrared absorption spectroscopy, thermal analysis, X-ray diffraction (powder method) and luminescence spectroscopy. For manufacturing the OLED it was used the technique of deposition of thin films by physical vapor (PVD, Physical Vapor Deposition). (author)

  5. Preparation and characterization of electroluminescent devices based on complexes of β-diketonates of Tb3+, Eu3+, Gd3+ ions with macrocyclic ligands and UO22+ films

    International Nuclear Information System (INIS)

    Gibelli, Edison Bessa

    2010-01-01

    Complexes containing Rare Earth ions are of great interest in the manufacture of electro luminescent devices as organic light emitting devices (OLED). These devices, using rare earth trivalent ions (TR 3+ ) as emitting centers, show high luminescence with extremely fine spectral bands due to the structure of their energy levels, long life time and high quantum efficiency. This work reports the preparation of Rare Earth β-diketonate complexes (Tb 3+ , Eu 3+ and Gd 3+ ) and (tta - thenoyltrifluoroacetonate and acac - acetylacetonate) containing a ligand macrocyclic crown ether (DB18C6 - dibenzo18coroa6) and polymer films of UO 2 2+ . The materials were characterized by complexometric titration with EDTA, CH elemental analysis, near infrared absorption spectroscopy, thermal analysis, X-ray diffraction (powder method) and luminescence spectroscopy. For manufacturing the OLED it was used the technique of deposition of thin films by physical vapor (PVD, Physical Vapor Deposition). (author)

  6. Aloe vera plant-extracted solution hydrothermal synthesis and magnetic properties of magnetite (Fe3O4) nanoparticles

    Science.gov (United States)

    Phumying, Santi; Labuayai, Sarawuth; Thomas, Chunpen; Amornkitbamrung, Vittaya; Swatsitang, Ekaphan; Maensiri, Santi

    2013-06-01

    Magnetite (Fe3O4) nanoparticles have been successfully synthesized by a novel hydrothermal method using ferric acetylacetonate (Fe(C5H8O2)3) and aloe vera plant-extracted solution. The influences of different reaction temperatures and times on the structure and magnetic properties of the synthesized Fe3O4 nanoparticles were investigated. The synthesized nanoparticles are crystalline and have particle sizes of ˜6-30 nm, as revealed by transmission electron microscopy (TEM). The results of X-ray diffraction (XRD), High resolution TEM (HRTEM) and selected area electron diffraction (SAED) indicate that the synthesized Fe3O4 nanoparticles have the inverse cubic spinel structure without the presence of any other phase impurities. The hysteresis loops of the Fe3O4 nanoparticles at room temperature show superparamagnetic behavior and the saturation magnetization of the Fe3O4 samples increases with increasing reaction temperature and time.

  7. Characterization of cubic yttria-stabilized zirconia obtained by spray pyrolysis

    International Nuclear Information System (INIS)

    Halmenschlager, Cibele M.; Nunes, Marilia; Vieira, Ramaugusto; Bergmann, Carlos Perez; Falcade, Tiago; Malfatti, Celia de Fraga

    2009-01-01

    Yttria-stabilized-zirconia (YSZ) has been the object of many studies as a SOFC electrolyte. The aim of this work is to produce, by spray pyrolysis process, thin and dense films of YSZ. A disk of steel 316L, previously heated, was used as substrate. The film was obtained with zirconium acetylacetonate (Zr(C 6 H 7 O 2 ) 4 ) and yttrium chloride (YCl 3.6 H 2 O), dissolved in a mixture of ethanol + butyl carbitol with volume ratio (1:1). ZrO 2 amorphous films were deposited in the substrate heated at many temperatures. After thermal treatment at 700 deg C the films were changed into cubic yttria-stabilized-zirconia structure. The thin films obtained were characterized by thermal analysis, scanning electron microscopy, transmission electron microscopy, X-ray diffraction and micro-Raman spectroscopy. (author)

  8. Optical and electrical characteristics of zirconium oxide thin films deposited on silicon substrates by spray pyrolysis

    International Nuclear Information System (INIS)

    Aguilar-Frutis, M.; Araiza, J.J.; Falcony, C.; Garcia, M.

    2002-01-01

    The optical and electrical characteristics of zirconium oxide thin films deposited by spray pyrolysis on silicon substrates are reported. The films were deposited from a spraying solution of zirconium acetylacetonate in N,N-dimethylformamide using an ultrasonic mist generator on (100) Si substrates. The substrate temperature during deposition was in the range of 400 to 600 grad C. Deposition rates up to 16 A/sec were obtained depending on the spraying solution concentration and on the substrate temperature. A refraction index of the order of 2.0 was measured on these films by ellipsometry. The electrical characteristics of the films were determined from the capacitance and current versus voltage measurements. The addition of water mist during the spraying deposition process was also studied in the characteristics of the films. (Authors)

  9. Mixed-ligand Al complex—a new approach for more high efficient OLEDs

    International Nuclear Information System (INIS)

    Petrova, Petia K.; Tomova, Reni L.; Stoycheva-Topalova, Rumiana T.; Kaloyanova, Stefka S.; Deligeorgiev, Todor G.

    2012-01-01

    The mixed-ligand Aluminum bis(8-hydroxyquinoline) acetylacetonate (Alq 2 Acac) complex was presented and its performance as electroluminescent and electron transporting layer for OLED was studied. The photophysical properties of the novel complex were investigated and compared with the properties of the parent Alq 3 . Highly efficient OLED based on the mixed-ligand Al complex was developed with two times higher luminescence and efficiency compared to the identical OLED based on the conventional Alq 3 The better performance of the devices make the novel Al complex a very promising material for OLEDs. - Highlights: ► A novel electroluminescent Alq 2 Acac complex is presented as material for OLED. ► Electroluminescent emission of Alq 2 Acac is very similar to that of commercial Alq 3 . ► Devices with Alq 2 Acac show better characteristics compared to those with Alq 3 .

  10. Ligand isotopic exchange of tris(acetylacetonato)germanium(IV) perchlorate in organic solvents

    International Nuclear Information System (INIS)

    Nagasawa, Akira; Saito, Kazuo

    1978-01-01

    The ligand isotopic exchange between tris(acetylacetonato)germanium(IV) perchlorate and acetylacetone[ 14 C] has been studied in 1,1,2,2-tetrachloroethane (TCE), nitromethane (NM), and acetonitrile (AN), at 100 - 120 0 C. In these solvents, the rate formula was R = k[H 2 O][complex]; the concentrations of the complex, free ligand, and water in solution were in the ranges from 0.01 to 0.1 mol dm -3 . The activation enthalpies and entropies for the k's are 105, 98, and 90 kJ mol -1 ; and -25, -53, and -69 JK -1 mol -1 , in TCE, NM, and AN, respectively. Influence of acid and base concentrations, and deuterium isotope effect on the rate in AN suggest that the rate controlling step of the exchange is governed by the ease of the proton transfer between the leaving and the incoming acac - in an intermediate. (auth.)

  11. Rapid radiochemical separation of short-lived radionuclides in neutron-activated samples

    International Nuclear Information System (INIS)

    Fardy, J.

    1985-11-01

    Radiochemical separation procedures based on the removal of metal ions by columns of C 18 -bonded silica gel after selective complexation are examined and the simplicity of the method demonstrated by its application to determination of Mn, Cu and Zn in neutron-activated biological material from the following solutions (pH 0-10, sulphate concentration 0,18M and 1,44M SO 4 ): 8-hydroxyquinoline (oxine), ammonium pyrrolidinedithiocarbamate (APDC), cupferron (CUP), 1-(2-pyridylazo)-2-naphthol (PAN), 1-(2'-thiazolylazo)-2-naphthol (TAN), 4-(2-pyridylazo) resorcinol (PAR), diethylammonium diethyldithiocarbamate (DDC), potassium ethyl xanthate (PEX), acetylacetone (AcAc) or thenoyltrifluoracetone (TTA). The method is rapid and reliable and readily adaptable in all radiochemical laboratories

  12. Emission characteristics in solution-processed asymmetric white alternating current field-induced polymer electroluminescent devices

    Science.gov (United States)

    Chen, Yonghua; Xia, Yingdong; Smith, Gregory M.; Gu, Yu; Yang, Chuluo; Carroll, David L.

    2013-01-01

    In this work, the emission characteristics of a blue fluorophor poly(9, 9-dioctylfluorene) (PFO) combined with a red emitting dye: Bis(2-methyl-dibenzo[f,h]quinoxaline)(acetylacetonate)iridium (III) [Ir(MDQ)2(acac)], are examined in two different asymmetric white alternating current field-induced polymer electroluminescent (FIPEL) device structures. The first is a top-contact device in which the triplet transfer is observed resulting in the concentration-dependence of the emission similar to the standard organic light-emitting diode (OLED) structure. The second is a bottom-contact device which, however, exhibits concentration-independence of emission. Specifically, both dye emission and polymer emission are found for the concentrations as high as 10% by weight of the dye in the emitter. We attribute this to the significant different carrier injection characteristics of the two FIPEL devices. Our results suggest a simple and easy way to realize high-quality white emission.

  13. Efficient white organic light-emitting devices using a thin 4,4'-bis(2,2'-diphenylvinyl)-1,1'-diphenyl layer

    International Nuclear Information System (INIS)

    Wang Jun; Yu Junsheng; Li Lu; Tang Xiaoqing; Jiang Yadong

    2008-01-01

    White organic light-emitting devices (OLEDs) were fabricated using phosphorescent material bis[2-(4-tert-butylphenyl)benzothiazolato-N,C 2' ]iridium (acetylacetonate) [(t-bt) 2 Ir(acac)] doped in 4,4'-bis(carbazol-9-yl) biphenyl (CBP) matrix as a yellow light-emitting layer and a thin layer 4,4'-bis(2,2'-diphenylvinyl)-1,1'-diphenyl (DPVBi) as the blue light-emitting layer. The light colour of the OLEDs can be adjusted by changing doped concentration and the thickness of the DPVBi thin layer. The maximum luminance and power efficiency of 5% doped device reached 15 460 cd m -2 and 8.1 lm W -1 , respectively. The 3% doped device showed the CIE coordinates of (0.344, 0.322) at 8 V and a maximum power efficiency of 5.7 lm W -1 at 4.5 V

  14. Phosphorescence white organic light-emitting diodes with single emitting layer based on isoquinolinefluorene-carbazole containing host.

    Science.gov (United States)

    Koo, Ja Ryong; Lee, Seok Jae; Hyung, Gun Woo; Kim, Bo Young; Shin, Hyun Su; Lee, Kum Hee; Yoon, Seung Soo; Kim, Woo Young; Kim, Young Kwan

    2013-03-01

    We have demonstrated a stable phosphorescent white organic light-emitting diodes (WOLEDs) using an orange emitter, Bis(5-benzoyl-2-(4-fluorophenyl)pyridinato-C,N) iridium(III)acetylacetonate [(Bz4Fppy)2Ir(III)acac] doped into a newly synthesized blue host material, 2-(carbazol-9-yl)-7-(isoquinolin-1-yl)-9,9-diethylfluorene (CzFliq). When 1 wt.% (Bz4Fppy)2Ir(III)acac was doped into emitting layer, it was realized an improved EL performance and a pure white color in the OLED. The optimum WOLED showed maximum values as a luminous efficiency of 10.14 cd/A, a power efficiency of 10.24 Im/W, a peak external quantum efficiency 4.07%, and Commission Internationale de L'Eclairage coordinates of (0.34, 0.39) at 8 V.

  15. Silica sulfuric acid: a reusable solid catalyst for one pot synthesis of densely substituted pyrrole-fused isocoumarins under solvent-free conditions

    Directory of Open Access Journals (Sweden)

    Sudipta Pathak

    2013-11-01

    Full Text Available A convenient and efficient methodology for the synthesis of densely substituted pyrrole-fused isocoumarins, which employs solid-supported silica sulfuric acid (SSA as catalyst, has been developed. When the mixture of ninhydrin adducts of acetylacetone/ethyl acetoacetate and primary amines was heated on the solid surface of SSA under solvent-free conditions, the pyrrole-fused isocoumarins were formed in good yields. This synthetic method has several advantages such as the employment of solvent-free reaction conditions without the use of any toxic reagents and metal catalysts, the ease of product isolation, the use of a recyclable catalyst, the low cost, the easy availability of the starting materials, and the excellent yields of products.

  16. Electrochemical investigation of tetravalent uranium β-diketones for active materials of all-uranium redox flow battery

    International Nuclear Information System (INIS)

    Yamamura, Tomoo; Shiokawa, Yoshinobu; Ikeda, Yasuhisa

    2002-01-01

    For active materials of the all-uranium redox flow battery for the power storage, tetravalent uranium β-diketones were investigated. The electrode reactions of U(ba) 4 and U(btfa) 4 were examined in comparison with that of U(acac) 4 , where ba denotes benzoylacetone, btfa benzoyltrifluoroacetone and acac acetylacetone. The cyclic voltammograms of U(ba) 4 and U(btfa) 4 solutions indicate that there are two series of redox reactions corresponding to the complexes with different coordination numbers of four and three. The electrode kinetics of the U(IV)/U(III) redox reactions for btfa complexes is examined. The obtained result supports that the uranium β-diketone complexes examined in the present study will serve as excellent active materials for negative electrolyte in the redox flow battery. (author)

  17. Ferrocene and cobaltocene derivatives for non-aqueous redox flow batteries.

    Science.gov (United States)

    Hwang, Byunghyun; Park, Min-Sik; Kim, Ketack

    2015-01-01

    Ferrocene and cobaltocene and their derivatives are studied as new redox materials for redox flow cells. Their high reaction rates and moderate solubility are attractive properties for their use as active materials. The cyclability experiments are carried out in a static cell; the results showed that these materials exhibit stable capacity retention and predictable discharge potentials, which agree with the potential values from the cyclic voltammograms. The diffusion coefficients of these materials are 2 to 7 times higher than those of other non-aqueous materials such as vanadium acetylacetonate, iron tris(2,2'-bipyridine) complexes, and an organic benzene derivative. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. Titanium-silicon films prepared by spin and dip-coating

    International Nuclear Information System (INIS)

    Nassar, Eduardo J.; Ciuffi, Katia J.; Goncalves, Rogeria R.; Messaddeq, Younes; Ribeiro, Sidney J.L.

    2003-01-01

    The conditions for the preparation of luminescent materials, consisting of Eu 3+ ions entrapped in a titanium matrix, in the form of a thin film, using the sol-gel process, are described. The films were obtained from sols prepared with TEOS and TEOT, in the presence of acetylacetone as the hydrolysis-retarding agent, using the dip-coating and spin-coating techniques. The influence of these techniques on the films based on titanium and silicon are presented. The Eu 3+ was used as a luminescent probe. The films have been characterized by luminescence, reflection and transmittance. The thickness of the films could be related to the preparation procedure. Transparent thin films have been prepared by dip-coating technique. (author)

  19. Highly efficient red electrophosphorescent devices at high current densities

    International Nuclear Information System (INIS)

    Wu Youzhi; Zhu Wenqing; Zheng Xinyou; Sun, Runguang; Jiang Xueyin; Zhang Zhilin; Xu Shaohong

    2007-01-01

    Efficiency decrease at high current densities in red electrophosphorescent devices is drastically restrained compared with that from conventional electrophosphorescent devices by using bis(2-methyl-8-quinolinato)4-phenylphenolate aluminum (BAlq) as a hole and exciton blocker. Ir complex, bis(2-(2'-benzo[4,5-α]thienyl) pyridinato-N,C 3' ) iridium (acetyl-acetonate) is used as an emitter, maximum external quantum efficiency (QE) of 7.0% and luminance of 10000cd/m 2 are obtained. The QE is still as high as 4.1% at higher current density J=100mA/cm 2 . CIE-1931 co-ordinates are 0.672, 0.321. A carrier trapping mechanism is revealed to dominate in the process of electroluminescence

  20. Solvent - solute interaction

    International Nuclear Information System (INIS)

    Urbanczyk, A.; Kalinowski, M.K.

    1983-01-01

    The electronic absorption spectrum of vanadyl acetylacetonate has been studied in 15 organic solvents. It has been found that wavenumbers and molar absorptivities of the long-wavelength bands (d-d transitions) can be well described by a complementary Lewis acid-base model including Gutmann's donor number [Gutmann V., Wychera E., Inorg. Nucl. Chem. Letters 2, 257 (1966)] and acceptor number [Mayer U., Gutmann V., Gerger W., Monatsh. Chem. 106, 1235 (1975)] of a solvent. This model describes also the solvent effect of the hyperfine splitting constant, Asub(iso)( 51 V), from e.s.r. spectra of VOacac 2 . These observations are discussed in terms of the donor-acceptor concept for solvent-solute interactions. (Author)

  1. Study of substitution reactions of ligands in VO2+ complexes in toluene solutions by ESR method

    International Nuclear Information System (INIS)

    Lundkvist, R.; Panfilov, A.T.; Kalinichenko, N.B.; Marov, I.N.; AN SSSR, Moscow. Inst. Geokhimii i Analiticheskoj Khimii)

    1976-01-01

    Kinetics and equilibrium of stepwise substitution of ligands have been investigated at different temperatures for the complexes of oxovanadium (4) with salicylaldoxime, 8-oxyquinoline, acetylacetone, benzoylacetone, and tenoyltrifluoroacetone. The relative complexability of these ligands in toluene has been studied. The parameters of spin-Hamiltonian of EPR spectra of the VO 2+ complexes have been determined. The equilibrium constants, the rate constants, and activation energy have been found for the substitution reactions of ligands in the complexes VOA 2 : VOA 2 +HB=VOAB+HA; VOAB+HB=VOB 2 +HA, where HA and HB are the ligands with different donor atoms. The mixed complexes have been detected of the general formula VOAB, where HA is salicylaldoxime or 8-oxyquinoline and HB is β-diketone

  2. Abordagem teórico-experimental da teoria do campo cristalino na disciplina de síntese inorgânica

    Directory of Open Access Journals (Sweden)

    Bárbara C Leal

    2011-01-01

    Full Text Available We describe herein the synthesis and characterization of the complexes KNiF3, [Ni(en3]I2, [Ni(en3]Cl2, [Ni(acac2(H2O2], [Ni(en2(H2O2]Cl2 and [Ni(NH36](BF42 (en = ethylenediamine, acac- = acetylacetonate performed in the inorganic synthesis major course at the Chemistry Institute of UFRGS (Universidade Federal do Rio Grande do Sul. The compounds were characterized by infrared and electronic spectroscopy and the electrolytic conductivity was measured. The parameters 10Dq and B were obtained from the electronic spectra and the nefelauxetic and spectrochemical series were determined. The obtained spectrochemical series was F- < acac- < NH3 < en and the nefeulaxetic series was en < NH3 < acac- < F-.

  3. Ion-molecule interactions of biological importance. A vibrational spectroscopic study of magnesium complexes with hydroxylated quinones; Interactions ions-molecules d'interet biologique. Etude par spectrometrie de vibrations de la complexation du magnesium avec des molecules quinoniques hydroxylees

    Energy Technology Data Exchange (ETDEWEB)

    Kirszenbaum, Marek

    1976-06-14

    Luteoskyrin and rugulosin are two naturally occurring yellow pigments with hydroxylated bis-anthraquinonic structures. They cause serious liver disorders in man due to the formation of complexes of the type pigment-Mg{sup 2+}-DNA. In order to elucidate the structure of these complexes we have studied the vibrational spectra of some model systems, namely 1-hydroxy- and 1,4-dihydroxyanthraquinone, their magnesium chelate complexes, and a series of simpler complexes as the acetylacetonates of some divalent metals. Complete vibrational assignment are proposed for anthraquinone-9,10, the two hydroxylated and deureroxylated derivatives and their magnesium complexes. The substitution of {sup 26}Mg in place of {sup 24}Mg in these complexes enabled us to assign the Mg-O vibrations; their number corresponds to a hexa-coordinated metal in the acetylacetonate case and to a tetra-coordinated structure in the anthraquinone-olates complexes. The position of the ν C=0 and ν C-0 vibrations bands in the complexes shows that the bonds in the chelated ring of Mg(1-O-AQ){sub 2} retains their single and double bond characteristic whereas in the CMg(1,4-O{sub 2},-AQ){sub n} a resonating structure appears in the ring. The study of the IR and R spectra of the complexes enabled a tetrahedral structure to be proposed for the oxygens around the magnesium. Finally it was noted that the Mg-O bonds possessed a high degree of covalent character. (author) [French] La luteoskyrine et la rugulosine, deux pigments jaunes de structure de bis-anthraquinones hydroxylees, provoquent des troubles hepatiques graves par la formation des complexes pigment-Mg{sup 2+}-ADN. Dans le but d'eclaircir la structure de ces complexes nous avons etudie, par spectrometrie de vibrations, les systemes-modeles suivants: la 1-hydroxy- et la 1,4-dihydroxyanthraquinones, leurs complexes magnesies et une serie des complexes plus simples, tels que les acetylacetonates. de metaux divalents. Nous avons propose une attribution

  4. Azo coupling of 4-nitrophenyldiazonium chloride with aliphatic nucleophiles: an integrated organic synthesis and X-ray crystallography experiment; Acoplamento de cloreto de 4-nitrofenildiazonio com nucleofilos alifaticos: experimento integrado de sintese organica e cristalografia de raios X

    Energy Technology Data Exchange (ETDEWEB)

    Cunha, Silvio; Marques, Monique F.; Rocha, Valeria, E-mail: silviodc@ufba.br [Universidade Federal da Bahia (UFBA), Salvador, BA (Brazil). Instituto de Quimica; Lariucci, Carlito; Vencato, Ivo [Universidade Federal de Goiania (UFG), GO (Brazil). Instituto de Fisica

    2013-11-01

    This article describes an undergraduate experiment for the synthesis of p-nitrophenyldiazonium chloride and its coupling with acetylacetone and two enaminones, 4-phenylamino-pent-3-en-2-one and 4-amino-pent-3-en-2-one, in an adaptation of a previously reported synthetic protocol. The azo dyes 4-(E)-phenylamino-3-[(E)-2-(4-nitrophenylazo)]-3-penten-2-one and 4-(E)-amino-3-[(E)-2-(4-nitrophenylazo)]-3-penten-2-one were obtained, and the solid state structure of this latter azo compound was characterized by single crystal X-ray diffraction studies. This two-week integrated laboratory approach involves simple synthetic experiments and microwave chemistry in the organic laboratory plus crystallography analysis, suitable for novice students on undergraduate experimental chemistry courses. (author)

  5. A general chelate-assisted co-assembly to metallic nanoparticles-incorporated ordered mesoporous carbon catalysts for Fischer-Tropsch synthesis.

    Science.gov (United States)

    Sun, Zhenkun; Sun, Bo; Qiao, Minghua; Wei, Jing; Yue, Qin; Wang, Chun; Deng, Yonghui; Kaliaguine, Serge; Zhao, Dongyuan

    2012-10-24

    The organization of different nano objects with tunable sizes, morphologies, and functions into integrated nanostructures is critical to the development of novel nanosystems that display high performances in sensing, catalysis, and so on. Herein, using acetylacetone as a chelating agent, phenolic resol as a carbon source, metal nitrates as metal sources, and amphiphilic copolymers as a template, we demonstrate a chelate-assisted multicomponent coassembly method to synthesize ordered mesoporous carbon with uniform metal-containing nanoparticles. The obtained nanocomposites have a 2-D hexagonally arranged pore structure, uniform pore size (~4.0 nm), high surface area (~500 m(2)/g), moderate pore volume (~0.30 cm(3)/g), uniform and highly dispersed Fe(2)O(3) nanoparticles, and constant Fe(2)O(3) contents around 10 wt %. By adjusting acetylacetone amount, the size of Fe(2)O(3) nanoparticles is readily tunable from 8.3 to 22.1 nm. More importantly, it is found that the metal-containing nanoparticles are partially embedded in the carbon framework with the remaining part exposed in the mesopore channels. This unique semiexposure structure not only provides an excellent confinement effect and exposed surface for catalysis but also helps to tightly trap the nanoparticles and prevent aggregating during catalysis. Fischer-Tropsch synthesis results show that as the size of iron nanoparticles decreases, the mesoporous Fe-carbon nanocomposites exhibit significantly improved catalytic performances with C(5+) selectivity up to 68%, much better than any reported promoter-free Fe-based catalysts due to the unique semiexposure morphology of metal-containing nanoparticles confined in the mesoporous carbon matrix.

  6. Photocatalytic deposition of Ag nanoparticles on TiO2: Metal precursor effect on the structural and photoactivity properties

    Directory of Open Access Journals (Sweden)

    E. Albiter

    2015-09-01

    Full Text Available A series of 1 wt.% Ag–TiO2 photocatalysts were obtained by photodeposition using different organic (acetylacetonate, Ag-A and inorganic (nitrate, Ag-N, and perchlorate, Ag-C silver precursors in order to determinate the influence of the silver precursor on final properties of the photocatalysts. The resulting photocatalytic materials were characterized by different techniques (UV–Vis DRS, TEM/HRTEM and XPS and their photocatalytic activity was evaluated in the degradation of rhodamine B (used as model pollutant in aqueous solution under simulated solar light. The photocatalytic reduction of Ag species to Ag0 on TiO2 was higher with silver nitrate as precursor compared to acetylacetonate or perchlorate. All the Ag-modified TiO2 photocatalysts exhibited a surface plasmon resonance effect in the visible region (400–530 nm indicating different metal particle sizes depending on the Ag precursor used in their synthesis. A higher photocatalytic activity was obtained with all the Ag/TiO2 samples compared with non-modified TiO2. The descending order of photocatalytic activity was as follows: Ag-A/TiO2 ≈ Ag-N/TiO2 > Ag-C/TiO2 > TiO2-P25. The enhanced photoactivity was attributed to the presence of different amounts Ag0 nanoparticles homogeneously distributed on Ag2O and TiO2, trapping the photogenerated electrons and avoiding charge recombination.

  7. Increasing the energy density of the non-aqueous vanadium redox flow battery with new electrolytes; Neue Elektrolyte zur Steigerung der Energiedichte einer nicht-waessrigen Vanadium-Acetylacetonat-Redox-Flow-Batterie

    Energy Technology Data Exchange (ETDEWEB)

    Herr, Tatjana

    2015-07-01

    Redox flow battery (RFB) is a promising energy storage technology which is similar to a polymer electrolyte membrane fuel cell. Currently, this electrochemical energy conversion device is used as a storage system for renewable energies or as uninterruptable power source. All-Vanadium-RFB (VRFB) and Zinc-Bromine-RFB are most well-known types of the aqueous RFB for these applications. But also the non-aqueous RFB is becoming more and more famous, because non-aqueous electrolytes offer wider operating temperature ranges, wider stable potential windows and a potentially higher energy density. However, current research studies show that the solubility of the most used redox active species is not sufficient. Therefore, present study aims to show concepts in order to solve this problem. Vanadium(III)acetylacetonate (V(acac){sub 3}) is used as active species, supported by tetrabutylammonium hexafluorophosphate. In acetonitrile it shows two quasi-reversible redox couples and a cell potential ∝2.2 V. The maximum solubility is ∝0.6 M. In this work other solvents and solvent mixtures were examined with the objective of increasing the solubility of V(acac){sub 3}. In 1,3-dioxolane the solubility was e.g. 0.8 M, dimethyl sulfoxide showed good battery performance with the highest energy efficiency ∝44 %. Acetylacetone is able to regenerate V(acac){sub 3} from the side product that is formed by reaction with water. The new electrolyte solution consisting of acetonitrile, 1,3-dioxolane and dimethyl sulfoxide nearly doubled the solubility of V(acac){sub 3}. In galvanostatic charge-discharge tests, single cell V(acac){sub 3} RFB exhibited energy efficiency between 25-50 % depending an test conditions. Also, the influence of water and oxygen addition an electrolyte was investigated. Finally, experiments with different ambient temperatures show that V(acac){sub 3} RFB is able to operate at temperatures such as 0 C and -25 C.

  8. Studies on the porphine labeled with 99mTc-pertechnetate

    International Nuclear Information System (INIS)

    Ai-Yih Wang; Jiunn-Liang Lin; Wen-Chieh Lin

    2010-01-01

    The aim of this research is to use acetylacetonate as a 99m Tc chelating agent label with porphyrin and evaluate its radiochemical and biological characteristics. Stannous chloride was used as a reductant to determine the chemical and biological characterization of 99m Tc-complexes from labeling porphine (4',4'',4'''-(2lH,23H-Porphine-5,10,15,20-terayl)tetrakis-(benzoic acid), TPPB) with 99m Tc-pertechnetate. Instant thin layer chromatography (ITLC), size exclusion chromatography (SEC), paper electrophoresis, and UV/Vis spectrophotometry were used to evaluate chemical characterization. Finally, biodistribution and liver function tests were applied to evaluate biological characteristics. The results of this study show that the labeling efficiency of 99m Tc(acac)-TPPB was nearly 100% when using acetylacetone (acac) as a conjugator. Three major 99m Tc(acac)-TPPB complexes were separated by SEC, and all of them were hydrophilic. The UV-Vis spectra of 99m Tc(acac)-TPPB complexes closely resembled those of the TPPB, but the wave lengths of their peaks changed 430, 521, 556, 591 and 647 nm after complexation. The biodistribution study selected the liver as the target organ. The 99m Tc(acac)-TPPB complex may cause short-term liver injury. However, this injury can be repaired, and the reagent is quickly metabolized. Hence, the toxicity of the 99m Tc(acac)-TPPB complex is within an acceptable range, and making it a promising liver imaging agent. (author)

  9. Sol-gel chemistry applied to the synthesis of polymetallic oxides including actinides reactivity and structure from solution to solid state

    International Nuclear Information System (INIS)

    Lemonnier, St.

    2006-02-01

    Minor actinides transmutation is studied at present in order to reduce the radiotoxicity of nuclear waste and the assessment of its technical feasibility requires specific designed materials. When considering americium, yttria stabilized zirconia (Am III YII Zriv)Or x is among the ceramic phases that one which presents the required physico-chemical properties. An innovative synthesis of this mixed oxide by sol-gel process is reported in this manuscript. The main aim of this work is to adjust the reactivity of the different metallic cations in aqueous media using complexing agent, in order to initiate a favourable interaction for a homogeneous elements repartition in the forming solid phase. The originality of the settled synthesis lies on an in-situ formation of a stable and monodisperse nano-particles dispersion in the presence of acetylacetone. The main reaction mechanisms have been identified: the sol stabilisation results from an original interaction between the three compounds (Zrly, trivalent cations and acetylacetone). The sol corresponds to a structured system at the nanometer scale for which zirconium and trivalent cations are homogeneously dispersed, preliminary to the sol-gel transition. Furthermore, preliminary studies were carried out with a view to developing materials. They have demonstrated that numerous innovative and potential applications can be developed by taking advantage of the direct and controlled formation of the sol and by adapting the sol-gel transition. The most illustrating result is the preparation of a sintered pellet with the composition Am0,13Zro,73Yo,0901,89 using this approach. (author)

  10. Sol-gel chemistry applied to the synthesis of polymetallic oxides including actinides reactivity and structure from solution to solid state; Synthese par voie douce d'oxydes polymetalliques incluant des actinides: reactivite et structure de la solution au solide

    Energy Technology Data Exchange (ETDEWEB)

    Lemonnier, St

    2006-02-15

    Minor actinides transmutation is studied at present in order to reduce the radiotoxicity of nuclear waste and the assessment of its technical feasibility requires specific designed materials. When considering americium, yttria stabilized zirconia (Am{sup III} YII Zriv)Or{sub x} is among the ceramic phases that one which presents the required physico-chemical properties. An innovative synthesis of this mixed oxide by sol-gel process is reported in this manuscript. The main aim of this work is to adjust the reactivity of the different metallic cations in aqueous media using complexing agent, in order to initiate a favourable interaction for a homogeneous elements repartition in the forming solid phase. The originality of the settled synthesis lies on an in-situ formation of a stable and monodisperse nano-particles dispersion in the presence of acetylacetone. The main reaction mechanisms have been identified: the sol stabilisation results from an original interaction between the three compounds (Zrly, trivalent cations and acetylacetone). The sol corresponds to a structured system at the nanometer scale for which zirconium and trivalent cations are homogeneously dispersed, preliminary to the sol-gel transition. Furthermore, preliminary studies were carried out with a view to developing materials. They have demonstrated that numerous innovative and potential applications can be developed by taking advantage of the direct and controlled formation of the sol and by adapting the sol-gel transition. The most illustrating result is the preparation of a sintered pellet with the composition Am0,13Zro,73Yo,0901,89 using this approach. (author)

  11. Synthesis and characterization of water-soluble SiO{sub 1.5}/TiO{sub 2} hybrid nanoparticles by hydrolytic co-condensation of triethoxysilane containing hydroxyl groups

    Energy Technology Data Exchange (ETDEWEB)

    Mori, Hideharu [Department of Polymer Science and Engineering, Graduate School of Science and Engineering, Yamagata University, 4-3-16 Jonan, Yonezawa 992-8510 (Japan)], E-mail: h.mori@yz.yamagata-u.ac.jp; Miyamura, Yasushi [Department of Polymer Science and Engineering, Graduate School of Science and Engineering, Yamagata University, 4-3-16 Jonan, Yonezawa 992-8510 (Japan); Endo, Takeshi [Molecular Engineering Institute, Kinki University, Iizuka, Fukuoka 820-8555 (Japan)

    2009-05-15

    Novel R-SiO{sub 1.5}/TiO{sub 2} hybrid nanoparticles were synthesized by hydrolytic co-condensation of titanium alkoxides (Ti(OR'){sub 4}, R' = ethyl, isopropyl, and butyl) with a triethoxysilane precursor, R-Si(OCH{sub 2}CH{sub 3}){sub 3}, R = -CH{sub 2}CH{sub 2}CH{sub 2}N(CH{sub 2}CH{sub 2}COOCH{sub 2}CH{sub 2}OH){sub 2}, derived from 2-hydroxyethyl acrylate. Co-condensation of a titanium alkoxide with the triethoxysilane precursor was investigated at different feed ratios, suggesting that water-soluble nanoparticles were obtained only at less than 30% of Ti(OEt){sub 4} molar ratio in the feed. In contrast, the co-condensation of titanium tetraisopropoxide, Ti(O{sup i}Pr){sub 4}, with the triethoxysilane precursor in the presence of acetylacetone proceeded as a homogeneous system until 70% of Ti(O{sup i}Pr){sub 4} molar ratio to afford water-soluble organic-inorganic hybrid nanoparticles containing titania-silica mixed oxides, as confirmed by NMR, FT-IR, elemental and ICP analyses. Scanning force microscopy (SFM) measurements of the product prepared at Ti(O{sup i}Pr){sub 4}/triethoxysilane = 50/50 mol% with acetylacetone indicated the formation of the nanoparticles having relatively narrow size distribution with average particle diameter less than 2.0 nm without aggregation. The refractive index of the hybrid nanoparticle was 1.571. The isolated nanoparticles distributed homogeneously were visualized by transmission electron microscopy (TEM), and the size of the hybrid nanoparticle (1.9 nm) was determined by X-ray diffraction (XRD)

  12. Transparent conductive zinc-oxide-based films grown at low temperature by mist chemical vapor deposition

    Energy Technology Data Exchange (ETDEWEB)

    Shirahata, Takahiro [New Energy and Environmental Business Division, Toshiba Mitsubishi-Electric Industrial Systems Corporation, Kobe International Business Center (KIBC) 509, 5-5-2 Minatojima-Minami, Chuo-Ku, Kobe 650-0047 (Japan); Kawaharamura, Toshiyuki [Research Institute, Kochi University of Technology, Kami, Kochi 780-8502 (Japan); School of Systems Engineering, Kochi University of Technology, Kami, Kochi 780-8502 (Japan); Fujita, Shizuo, E-mail: fujitasz@kuee.kyoto-u.ac.jp [Photonics and Electronics Science and Engineering Center, Kyoto University, Katsura, Nishikyo-ku, Kyoto 615-8520 (Japan); Orita, Hiroyuki [New Energy and Environmental Business Division, Toshiba Mitsubishi-Electric Industrial Systems Corporation, Kobe International Business Center (KIBC) 509, 5-5-2 Minatojima-Minami, Chuo-Ku, Kobe 650-0047 (Japan)

    2015-12-31

    Atmospheric pressure mist chemical vapor deposition (Mist–CVD) systems have been developed to grow zinc-oxide-based (ZnO-based) transparent conductive oxide (TCO) films. Low-resistive aluminum-doped ZnO (AZO) TCOs, showing resistivity of the order on 10{sup −4} Ωcm, previously were grown using a safe source material zinc acetate [Zn(ac){sub 2}], at a growth temperature as high as 500 °C. To grow superior TCOs at lower temperatures, we proposed the addition of NH{sub 3} to accelerate the reaction of acetylacetonate compounds. As the result, we could grow gallium-doped ZnO (GZO) TCOs with a resistivity of 2.7 × 10{sup −3} Ω cm and transmittance higher than 90% at 300 °C by using zinc acetylacetonate [Zn(acac){sub 2}] as the Zn source. To grow boron-doped ZnO (BZO) TCOs at a lower growth temperature of 200 °C, we used boron doping along with a toluene solution of diethylzinc (DEZ), that maintained high reactivity without being flammable. These BZO TCOs showed a resistivity of 1.5 × 10{sup −3} Ω cm and transmittance higher than 90%, despite the use of a non-vacuum-based open-air technology. - Highlights: • Introduction of Mist–CVD as a non-vacuum-based, safe, and cost-effective growth technology • Process evolution of the growth technology to lower the growth temperature. • Achievement of low resistive ZnO films at 200oC.

  13. Transparent conductive zinc-oxide-based films grown at low temperature by mist chemical vapor deposition

    International Nuclear Information System (INIS)

    Shirahata, Takahiro; Kawaharamura, Toshiyuki; Fujita, Shizuo; Orita, Hiroyuki

    2015-01-01

    Atmospheric pressure mist chemical vapor deposition (Mist–CVD) systems have been developed to grow zinc-oxide-based (ZnO-based) transparent conductive oxide (TCO) films. Low-resistive aluminum-doped ZnO (AZO) TCOs, showing resistivity of the order on 10"−"4 Ωcm, previously were grown using a safe source material zinc acetate [Zn(ac)_2], at a growth temperature as high as 500 °C. To grow superior TCOs at lower temperatures, we proposed the addition of NH_3 to accelerate the reaction of acetylacetonate compounds. As the result, we could grow gallium-doped ZnO (GZO) TCOs with a resistivity of 2.7 × 10"−"3 Ω cm and transmittance higher than 90% at 300 °C by using zinc acetylacetonate [Zn(acac)_2] as the Zn source. To grow boron-doped ZnO (BZO) TCOs at a lower growth temperature of 200 °C, we used boron doping along with a toluene solution of diethylzinc (DEZ), that maintained high reactivity without being flammable. These BZO TCOs showed a resistivity of 1.5 × 10"−"3 Ω cm and transmittance higher than 90%, despite the use of a non-vacuum-based open-air technology. - Highlights: • Introduction of Mist–CVD as a non-vacuum-based, safe, and cost-effective growth technology • Process evolution of the growth technology to lower the growth temperature. • Achievement of low resistive ZnO films at 200oC.

  14. Influences of alcoholic solvents on spray pyrolysis deposition of TiO{sub 2} blocking layer films for solid-state dye-sensitized solar cells

    Energy Technology Data Exchange (ETDEWEB)

    Jiang, Changyun, E-mail: jiangc@imre.a-star.edu.sg [Institute of Materials Research and Engineering, A-STAR, 3 Research Link, 117602 Singapore (Singapore); Koh, Wei Lin; Leung, Man Yin [Institute of Materials Research and Engineering, A-STAR, 3 Research Link, 117602 Singapore (Singapore); Hong, Wei [Department of Chemical Engineering and Waterloo Institute for Nanotechnology (WIN), University of Waterloo, 200 University Ave West ON, Waterloo, Canada N2L 3G1 (Canada); Li, Yuning, E-mail: yuning.li@uwaterloo.ca [Institute of Materials Research and Engineering, A-STAR, 3 Research Link, 117602 Singapore (Singapore); Department of Chemical Engineering and Waterloo Institute for Nanotechnology (WIN), University of Waterloo, 200 University Ave West ON, Waterloo, Canada N2L 3G1 (Canada); Zhang, Jie [Institute of Materials Research and Engineering, A-STAR, 3 Research Link, 117602 Singapore (Singapore)

    2013-02-15

    Influences of alcoholic solvents for titanium diisopropoxide bis(acetylacetonate) (TPA) precursor solutions on the spray pyrolysis deposited TiO{sub 2} films and the photovoltaic performance of the solid-state dye-sensitized solar cells (SDSCs) using these TiO{sub 2} films as the blocking layers were investigated. Smooth TiO{sub 2} films were obtained by spray pyrolysis deposition of a TPA solution in isopropanol (IPA) at a relatively low temperature of 260 Degree-Sign C. On the other hand, when ethanol was used as solvent, the TiO{sub 2} films fabricated at the same temperature showed much rougher surfaces with many pinholes. Our results showed that ethanol reacts with TPA to form titanium diethoxide bis(acetylacetonate) (TEA), which requires a higher thermal decomposition temperature than that of TPA. SDSCs with TiO{sub 2} blocking layer films fabricated using a TPA solution in IPA showed higher power conversion efficiencies with smaller variations. - Graphical abstract: Alcoholic solvents used for the TiO{sub 2} precursor play a critical role in determining the surface morphology of blocking layers and thus the photovoltaic performance of the SDSCs. Highlights: Black-Right-Pointing-Pointer Solvent influences morphology of spray pyrolysis deposited TiO{sub 2} blocking layer. Black-Right-Pointing-Pointer Ethanol reacts with TPA, resulting poor quality of blocking layer. Black-Right-Pointing-Pointer Isopropanol is better than ethanol for obtaining smooth blocking layer. Black-Right-Pointing-Pointer SDSC with blocking layer made with isopropanol showed better performance.

  15. Sol-gel chemistry applied to the synthesis of polymetallic oxides including actinides reactivity and structure from solution to solid state; Synthese par voie douce d'oxydes polymetalliques incluant des actinides: reactivite et structure de la solution au solide

    Energy Technology Data Exchange (ETDEWEB)

    Lemonnier, St

    2006-02-15

    Minor actinides transmutation is studied at present in order to reduce the radiotoxicity of nuclear waste and the assessment of its technical feasibility requires specific designed materials. When considering americium, yttria stabilized zirconia (Am{sup III} YII Zriv)Or{sub x} is among the ceramic phases that one which presents the required physico-chemical properties. An innovative synthesis of this mixed oxide by sol-gel process is reported in this manuscript. The main aim of this work is to adjust the reactivity of the different metallic cations in aqueous media using complexing agent, in order to initiate a favourable interaction for a homogeneous elements repartition in the forming solid phase. The originality of the settled synthesis lies on an in-situ formation of a stable and monodisperse nano-particles dispersion in the presence of acetylacetone. The main reaction mechanisms have been identified: the sol stabilisation results from an original interaction between the three compounds (Zrly, trivalent cations and acetylacetone). The sol corresponds to a structured system at the nanometer scale for which zirconium and trivalent cations are homogeneously dispersed, preliminary to the sol-gel transition. Furthermore, preliminary studies were carried out with a view to developing materials. They have demonstrated that numerous innovative and potential applications can be developed by taking advantage of the direct and controlled formation of the sol and by adapting the sol-gel transition. The most illustrating result is the preparation of a sintered pellet with the composition Am0,13Zro,73Yo,0901,89 using this approach. (author)

  16. Complexing properties of α-iso-saccharinate: thorium

    International Nuclear Information System (INIS)

    Allard, S.; Ekberg, C.

    2005-01-01

    Full text of publication follows: In the alkaline conditions of the intended Swedish repository for long-lived, low to intermediate level waste, SFL3-5, cellulose based items will degrade with iso-saccharinate being the dominant end-product. Iso-saccharinate is a strong complexing agent for tetravalent actinides, as well as for trivalent lanthanides, and its complexation properties are of interest for the long-term repository assessment. In the presented study, the complexation of 234 Th-α-iso-saccharinate is examined using liquid-liquid- extraction and radioanalytical techniques. An organic phase consisting of 0.1 M acetylacetone in toluene was used with a 1.0 M NaClO 4 aqueous phase kept at pH 8 in a thermostated AKUFVE unit. Since the α-iso-saccharinic system consists of three species - the carboxylic α-iso-saccharinic acid, α-iso-saccharinate and α-D-iso-saccharino-1,4-lactone - care must be taken when choosing the operational pH. Keeping the aqueous phase at pH 8 results in negligible concentrations of all but the α-iso-saccharinate form while at the same time being an excellent pH for the 234 Th-acetylacetone complexation with very limited hydrolysis effect. The α- iso-saccharinate concentration was incrementally increased, and samples of equal volumes were taken from the two phases and analyzed in a liquid scintillation detector once the radioactive equilibrium between 234 Th and 234 Pa had been reached. Two complexation constants were used to fit a distribution equation to the experimental data. (authors)

  17. Zirconium doped TiO{sub 2} thin films deposited by chemical spray pyrolysis

    Energy Technology Data Exchange (ETDEWEB)

    Juma, A. [Laboratory of Thin Film Chemical Technologies, Department of Materials Science, Tallinn University of Technology, Ehitajate tee 5, 19086 Tallinn (Estonia); Department of Physics and Astronomy, Botswana International University of Science and Technology, Private bag 16, Palapye (Botswana); Oja Acik, I., E-mail: ilona.oja@ttu.ee [Laboratory of Thin Film Chemical Technologies, Department of Materials Science, Tallinn University of Technology, Ehitajate tee 5, 19086 Tallinn (Estonia); Oluwabi, A.T.; Mere, A. [Laboratory of Thin Film Chemical Technologies, Department of Materials Science, Tallinn University of Technology, Ehitajate tee 5, 19086 Tallinn (Estonia); Mikli, V.; Danilson, M. [Chair of Semiconductor Materials Technology, Department of Materials Science, Tallinn University of Technology, Ehitajate tee 5, 19086 Tallinn (Estonia); Krunks, M. [Laboratory of Thin Film Chemical Technologies, Department of Materials Science, Tallinn University of Technology, Ehitajate tee 5, 19086 Tallinn (Estonia)

    2016-11-30

    Highlights: • Mean crystallite size of TiO{sub 2}:Zr film decreases with increasing [Zr] in the solution. • Zr doping supresses the anatase to rutile transformation process in TiO{sub 2} films. • Band gap of TiO{sub 2}:Zr film is 3.4 eV irrespective of the annealing temperature. - Abstract: Chemical spray pyrolysis (CSP) is a flexible deposition technique that allows for mixing of the precursor solutions in different proportions suitable for doping thin films. The CSP method was used to dope TiO{sub 2} thin films with Zr by adding zirconium(IV) acetylacetonate into a solution of titanium(IV) isopropoxide in ethanol stabilized by acetylacetone at [Zr]/[Ti] of 0, 5, 10 and 20 at%. The Zr-doped TiO{sub 2} thin films were uniform and homogeneous showing much smaller grains than the undoped TiO{sub 2} films. Zr stabilized the anatase phase to temperatures above 800 °C depending on Zr concentration in the spray solution. The concentration of Zr determined by XPS was 6.4 at% for the thin film deposited from the 20 at% solution. According to AFM studies, Zr doping decreased the root mean square roughness of TiO{sub 2} film from 5.9 to 1.1 nm. An XRD study of samples with the highest Zr amount showed the ZrTiO{sub 4} phase started forming after annealing at 800 °C. The optical band gap for TiO{sub 2} decreased from 3.3 eV to 3.0 eV after annealing at 800 °C but for the TiO{sub 2}:Zr(20) film it remained at 3.4 eV. The dielectric constant increased by more than four times with Zr-doping and this was associated with the change in the bond formations caused by substitution of Ti by Zr in the lattice.

  18. Pt-doped In{sub 2}O{sub 3} nanoparticles prepared by flame spray pyrolysis for NO{sub 2} sensing

    Energy Technology Data Exchange (ETDEWEB)

    Inyawilert, K. [Chiang Mai University, Department of Physics and Materials Science, Faculty of Science (Thailand); Channei, D. [Naresuan University, Department of Chemistry, Faculty of Science (Thailand); Tamaekong, N. [Maejo University, Program in Materials Science, Faculty of Science (Thailand); Liewhiran, C. [Chiang Mai University, Department of Physics and Materials Science, Faculty of Science (Thailand); Wisitsoraat, A.; Tuantranont, A. [National Electronics and Computer Technology Center (NECTEC), Nanoelectronics and MEMS Laboratory (Thailand); Phanichphant, S., E-mail: sphanichphant@gmail.com [Chiang Mai University, Faculty of Science, Materials Science Research Center (Thailand)

    2016-02-15

    Undoped In{sub 2}O{sub 3} and 0.25–1.00 wt% M (M=Pt, Nb, and Ru)-doped/loaded In{sub 2}O{sub 3} nanoparticles were successfully synthesized in a single-step flame spray pyrolysis technique using indium nitrate, platinum (II) acetylacetonate, niobium ethoxide, and ruthenium (III) acetylacetonate precursors. The undoped In{sub 2}O{sub 3} and M-doped In{sub 2}O{sub 3} nanoparticles were characterized by Brunauer–Emmett–Teller (BET) analysis, X-ray diffraction (XRD), and scanning and transmission electron microscopy (SEM & TEM). The BET average diameter of spherical nanoparticles was found to be in the range of 10.2–15.2 nm under 5/5 (precursor/oxygen) flame conditions. All XRD peaks were confirmed to correspond to the cubic structure of In{sub 2}O{sub 3}. TEM images showed that there is no Pt nanoparticle loaded on In{sub 2}O{sub 3} surface, suggesting that Pt should form solid solution with the In{sub 2}O{sub 3} lattice. Gas sensing studies showed that 0.5 wt% Pt doping in In{sub 2}O{sub 3} nanoparticles gave a significant enhancement of NO{sub 2} sensing performances in terms of sensor response and selectivity. 0.5 wt% Pt/In{sub 2}O{sub 3} exhibited a high NO{sub 2} response of ∼1904 to 5 ppm NO{sub 2} at 250 °C and good NO{sub 2} selectivity against NO, H{sub 2}S, H{sub 2}, and C{sub 2}H{sub 5}OH. In contrast, Nb and Ru loading resulted in deteriorated NO{sub 2} response. Therefore, Pt is demonstrated to be an effective additive to enhance NO{sub 2} sensing performances of In{sub 2}O{sub 3}-based sensors.

  19. Long-Range Intramolecular Electronic Communication in a Trinuclear Ruthenium Tropolonate Complex.

    Science.gov (United States)

    Yoshida, Jun; Kuwahara, Kyohei; Suzuki, Kota; Yuge, Hidetaka

    2017-02-20

    Dinuclear and trinuclear ruthenium complexes, [Ru(trop) 2 (C 2 trop)Ru(dppe)Cp] [2b; trop = tropolonato, C 2 trop = ethynyltropolonato, dppe = 1,2-bis(diphenylphosphino)ethane] and [Ru(trop){(C 2 trop)Ru(dppe)Cp} 2 ] (3), were synthesized, and their electronic and electrochemical properties were investigated in comparison with our previously reported complex [Ru(acac) 2 (C 2 trop)Ru(dppe)Cp] (2a). The electron-donating Ru II (dppe)Cp unit and electron-accepting Ru III O 6 unit are connected by C 2 trop in these complexes. 2a incorporates acetylacetonate as an ancillary ligand, while 2b and 3 incorporate tropolonate as an ancillary ligand. Every complex, 2a, 2b, and 3, exhibits similar UV-vis-near-IR (NIR) absorption spectra, demonstrating the lack of explicit intramolecular electronic communication between the units at least in the neutral state. The weak NIR absorption in 2a further diminished upon electrochemical oxidation, indicating almost no electronic communication between the units. In contrast, 2b and 3 exhibit broad NIR absorptions upon oxidation. Additionally, 3 exhibits four stepwise redox couples in the electrochemical study, which are formally attributed to [Ru II (trop) 3 ] - /[Ru III (trop) 3 ], two [Ru II (dppe)Cp]/[Ru III (dppe)Cp] + , and [Ru III (trop) 3 ]/[Ru IV (trop) 3 ] + couples. Clear separation of the redox couples attributed to the two terminal [Ru(dppe)Cp] units demonstrates the thermodynamic stability of the intermediate oxidation states with respect to disproportionation. Further electrochemical studies using an electrolyte including perfluorinated weakly coordinating anions and density functional theory/time-dependent density functional theory calculations confirmed the effect of ancillary ligands, acetylacetonate and tropolonate. In the case of 2a, electronic delocalization over the whole complex, especially over the [Ru(acac) 2 (trop)] unit, appears to be small. In contrast, the electronic communication between [Ru(dppe)Cp] and [Ru

  20. Synthesis, characterization, single crystal X-ray determination, fluorescence and electrochemical studies of new dinuclear nickel(II) and oxovanadium(IV) complexes containing double Schiff base ligands

    Science.gov (United States)

    Shafaatian, Bita; Ozbakzaei, Zahra; Notash, Behrouz; Rezvani, S. Ahmad

    2015-04-01

    A series of new bimetallic complexes of nickel(II) and vanadium(IV) have been synthesized by the reaction of the new double bidentate Schiff base ligands with nickel acetate and vanadyl acetylacetonate in 1:1 M ratio. In nickel and also vanadyl complexes the ligands were coordinated to the metals via the imine N and enolic O atoms. The complexes have been found to possess 1:1 metals to ligands stoichiometry and the molar conductance data revealed that the metal complexes were non-electrolytes. The nickel and vanadyl complexes exhibited distorted square planar and square pyramidal coordination geometries, respectively. The emission spectra of the ligands and their complexes were studied in methanol. Electrochemical properties of the ligands and their metal complexes were also investigated in DMSO solvent at 150 mV s-1 scan rate. The ligands and metal complexes showed both quasi-reversible and irreversible processes at this scan rate. The Schiff bases and their complexes have been characterized by FT-IR, 1H NMR, UV/Vis spectroscopies, elemental analysis and conductometry. The crystal structure of the nickel complex has been determined by single crystal X-ray diffraction.

  1. Surface modification of magnetite nanoparticle with azobenzene-containing water dispersible polymer

    International Nuclear Information System (INIS)

    Theamdee, Pawinee; Traiphol, Rakchart; Rutnakornpituk, Boonjira; Wichai, Uthai; Rutnakornpituk, Metha

    2011-01-01

    We here report the synthesis of magnetite nanoparticle (MNP) grafted with poly (ethylene glycol) methyl ether methacrylate (PEGMA)-azobenzene acrylate (ABA) statistical copolymer via atom transfer radical polymerization (ATRP) for drug entrapment and photocontrolled release. MNP was synthesized via thermal decomposition of iron (III) acetylacetonate in benzyl alcohol and surface functionalized to obtain ATRP initiating sites. Molar compositions of the copolymer on MNP surface were systematically varied (100:0, 90:10, 70:30, and 50:50 of PEGMA:ABA, respectively) to obtain water dispersible particles with various amounts of azobenzene. The presence of polymeric shell on MNP core was evidenced by transmission electron microscopy (TEM). Drug loading and entrapment efficiencies as well as drug release behavior of the copolymer–MNP complexes were investigated. It was found that when percent of ABA in the copolymers was increased, entrapment and loading efficiencies of prednisolone model drug were enhanced. Releasing rate and percent of the released prednisolone of the complex exposed in UV light were slightly enhanced as compared to the system without UV irradiation. This copolymer–MNP complex with photocontrollable drug release and magnetic field-directed properties is warranted for further studies for potential uses as a novel drug delivery vehicle.

  2. Effect of the substrate on the properties of ZnO-MgO thin films grown by atmospheric pressure metal-organic chemical vapor deposition

    Energy Technology Data Exchange (ETDEWEB)

    Torres-Huerta, A.M., E-mail: atohuer@hotmail.com [Instituto Politecnico Nacional, Grupo de Ingenieria en Procesamiento de Materiales CICATA-IPN, Unidad Altamira, km 14.5, Carretera Tampico-Puerto Industrial Altamira. C. P. 89600, Altamira, Tamps (Mexico); Dominguez-Crespo, M.A. [Instituto Politecnico Nacional, Grupo de Ingenieria en Procesamiento de Materiales CICATA-IPN, Unidad Altamira, km 14.5, Carretera Tampico-Puerto Industrial Altamira. C. P. 89600, Altamira, Tamps (Mexico); Brachetti-Sibaja, S.B. [Alumna del postgrado en Tecnologia Avanzada del CICATA-IPN, Unidad Altamira IPN, km 14.5, Carretera Tampico-Puerto Industrial Altamira. C. P. 89600, Altamira, Tamps (Mexico); Arenas-Alatorre, J. [Instituto de Fisica, UNAM, Apartado Postal 20-364, 01000, D.F. (Mexico); Rodriguez-Pulido, A. [Unidad Profesional Adolfo Lopez Mateos, Luis Enrique Erro s/n, 07738, D. F. (Mexico)

    2011-07-01

    The ZnO-MgO alloys possess attractive properties for possible applications in optoelectronic and display devices; however, the optical properties are strongly dependent on the deposition parameters. In this work, the effect of the glassy and metallic substrates on the structural, morphological and optical properties of ZnO-MgO thin films using atmospheric pressure metal-organic chemical vapor deposition was investigated at relatively low deposition temperature, 500 deg. C. Magnesium and zinc acetylacetonates were used as the metal-organic source. X-ray diffraction experiments provided evidence that the kind of substrates cause a deviation of c-axis lattice constant due to the constitution of a oxide mixture (ZnO and MgO) in combination with different intermetallic compounds(Mg{sub 2}Zn{sub 11} and Mg{sub 4}Zn{sub 7}) in the growth films. The substitutional and interstitial sites of Mg{sup 2+} instead of Zn{sup 2+} ions in the lattice are the most probable mechanism to form intermetallic compounds. The optical parameters as well as thickness of the films were calculated by Spectroscopic Ellipsometry using the classical dispersion model based on the sum of the single and double Lorentz and Drude oscillators in combination with Kato-Adachi equations, as well as X-ray reflectivity.

  3. Combustion synthesized indium-tin-oxide (ITO) thin film for source/drain electrodes in all solution-processed oxide thin-film transistors

    International Nuclear Information System (INIS)

    Tue, Phan Trong; Inoue, Satoshi; Takamura, Yuzuru; Shimoda, Tatsuya

    2016-01-01

    We report combustion solution synthesized (SCS) indium-tin-oxide (ITO) thin film, which is a well-known transparent conductive oxide, for source/drain (S/D) electrodes in solution-processed amorphous zirconium-indium-zinc-oxide TFT. A redox-based combustion synthetic approach is applied to ITO thin film using acetylacetone as a fuel and metal nitrate as oxidizer. The structural and electrical properties of SCS-ITO precursor solution and thin films were systematically investigated with changes in tin concentration, indium metal precursors, and annealing conditions such as temperature, time, and ambient. It was found that at optimal conditions the SCS-ITO thin film exhibited high crystalline quality, atomically smooth surface (RMS ∝ 4.1 Aa), and low electrical resistivity (4.2 x 10 -4 Ω cm). The TFT using SCS-ITO film as the S/D electrodes showed excellent electrical properties with negligible hysteresis. The obtained ''on/off'' current ratio, subthreshold swing factor, subthreshold voltage, and field-effect mobility were 5 x 10 7 , 0.43 V/decade, 0.7 V, and 2.1 cm 2 /V s, respectively. The performance and stability of the SCS-ITO TFT are comparable to those of the sputtered-ITO TFT, emphasizing that the SCS-ITO film is a promising candidate for totally solution-processed oxide TFTs. (orig.)

  4. The solvent extraction of alkali metal ions with β-diketones

    International Nuclear Information System (INIS)

    Munakata, Megumu; Niina, Syozo; Shimoji, Noboru

    1974-01-01

    This work was undertaken to investigate effects of solvent and chelating-agent on the solvent extraction of alkali metal ions by seven β-diketones, acetylacetone (Acac), benzoylacetone (BzA), dipivaloylmethane (DPM), dibenzoylmethane (DBM), thenoyltrifluoloacetone (TTA), benzoyltrifluoroacetone (BFA) and hexafluoroacetylacetone (HFA), and to separate lithium from alkali metals. The extraction of alkali metals increase with increasing donor power of the solvent: i.e., benzene Na>K>Rb>Cs, which is also the order in which the adduct formation of these β-diketone chelates with donor solvents increase. The adduct formations between β-diketone chelates of alkali metals and donor solvents markedly enhance the solubilities of the chelates in solvents and, consequently, the extractabilities of alkali metals with β-diketones. Lithium was extracted with TTA in ether at such a low base concentration that sodium, potassium, rubidium and cesium were hardly extracted, and this enabled to separate lithium from other metals by the use of rubidium hydroxide (0.02 M). An attempt has been made to isolate alkali metal β-diketone chelates and some chelates have been obtained as crystals. The infrared absorption bands arising from C=O and C.=C of TTA shift to lower frequencies in the alkali metal chelates with TTA, and consequently, β-diketones is suggested to coordinate to alkali metal as a bidentate ligand. (JPN)

  5. Infrared heating mediated synthesis and characterization of FeCo/C nanocomposites

    Energy Technology Data Exchange (ETDEWEB)

    Karpenkov, Dmitriy Yu., E-mail: Karpenkov_dmitriy@yahoo.com [National University of Science and Technology “MISiS”, 119991 Moscow (Russian Federation); Technical University of Darmstadt, 64289 Darmstadt (Germany); Muratov, Dmitriy G. [National University of Science and Technology “MISiS”, 119991 Moscow (Russian Federation); A.V.Topchiev Institute of Petrochemical Synthesis, RAS, 119991 Moscow (Russian Federation); Kozitov, Lev V. [National University of Science and Technology “MISiS”, 119991 Moscow (Russian Federation); Skokov, Konstantin P. [Technical University of Darmstadt, 64289 Darmstadt (Germany); Karpenkov, Alexey Yu. [Chelyabinsk State University, 454001 Chelyabinsk (Russian Federation); Tver State University, 170100 Tver (Russian Federation); Popkova, Alena V. [Tver State University, 170100 Tver (Russian Federation); Gutfleisch, Oliver [Technical University of Darmstadt, 64289 Darmstadt (Germany)

    2017-05-01

    Metal-filled carbon nanocomposites containing 20 wt% of metallic FeCo nanoparticles were synthesized by means of infrared heating of precursors (polyacrylonitrile – iron acetylacetonate - cobalt acetate). This fabrication approach shows promise for making radiation-absorbent materials in short one-step process with ability to control the size of nanoparticles and attune the composition of the metallic components. In this work the magnetic behavior of reaction products obtained at different stages of the synthesis have been investigated in detail. We report on the influence of the annealing temperature on evolution of the structure, chemical composition, size, surface morphology, spontaneous magnetization and coercivity of the FeCo nanoparticles. - Highlights: • A method of preparation of FeCo metal-filled carbon nanocomposites was proposed. • Proposed method is based on infrared heating of the precursors. • This technique excels at up scaling and the ability to control the particle size. • Usage of IR radiation leads to significant reduction of process time and temperature. • The influence of the synthesis parameters on physical properties was studied.

  6. One step synthesis of chlorine-free Pt/Nitrogen-doped graphene composite for oxygen reduction reaction

    KAUST Repository

    Varga, Tamás

    2018-03-14

    Chlorine-free Platinum/nitrogen-doped graphene oxygen reduction reaction catalysts were synthesized by a one step method of annealing a mixture of platinum acetylacetonate and graphene oxide under ammonia atmosphere. Nanoparticles with close to the ideal particle size for oxygen reduction reaction (ORR) were formed, i.e., with diameter of 3–4 nm (500 and 600 °C) and 6 nm (700 °C). X-ray photoelectron spectroscopy confirmed the successful introduction of both pyridinic and pyrrolic type nitrogen moieties into the graphene layers, which indicates a strong interaction between the nanoparticles and the graphene layers. The electrocatalytic activity of glassy carbon electrodes (GCE) modified with the synthesized Pt/NG samples for oxygen reduction was compared to that of a platinum/carbon black catalyst modified electrode in acidic and alkaline media. Based on the measured limiting current densities and calculated electron transfer number, the highest activity was measured in acidic and alkaline media on the samples annealed at 600 and 700 °C, respectively.

  7. Spectral and cyclic voltammetric studies on some intramolecularly hydrogen bonded arylhydrazones: Crystal and molecular structure of 2-(2-(3-nitrophenyl)hydrazono)-5,5-dimethylcyclohexane-1,3-dione

    Science.gov (United States)

    Sethukumar, A.; Arul Prakasam, B.

    2010-01-01

    A series of arylhydrazone derivatives ( 1- 7) were prepared by the coupling of acetylacetone/dimedone with respective aromatic diazonium salts and characterized by IR, 1H and 13C NMR spectra. The IR and NMR spectral data clearly manifests the effective intramolecular hydrogen bonding in all the cases. Cyclic voltammetric studies certainly indicate that in all the cases the reduced center is C dbnd N bond of hydrazonic moiety. The single crystal X-ray structural analysis of 2-(2-(3-nitrophenyl)hydrazono)-5,5-dimethylcyclohexane-1,3-dione ( 6) is also reported. Single crystal X-ray analysis of 6 evidences the intramolecular hydrogen bonding with the N(2)⋯O(4) distance of 2.642(15) Å, which can be designated as S(6) according to Etter's graph nomenclature. The cyclohexane ring conformation in the molecule ( 6) can be described as an envelope. RAHB studies suggest that the resonance assistance for hydrogen bonding is significantly reduced for the compound ( 6) due to the non-planarity of the six atoms which are involved in resonant cycle S(6) of Etter's graph. The planarity of the resonant cycle S(6) is very much disturbed by the conformational requirement of the cyclohexane ring and hence RAHB concept is less operative in this case.

  8. Synthesis and Antimicrobial Evaluation of Some Novel Thiazole, Pyridone, Pyrazole, Chromene, Hydrazone Derivatives Bearing a Biologically Active Sulfonamide Moiety

    Science.gov (United States)

    Darwish, Elham S.; Abdel Fattah, Azza M.; Attaby, Fawzy A.; Al-Shayea, Oqba N.

    2014-01-01

    This study aimed for the synthesis of new heterocyclic compounds incorporating sulfamoyl moiety suitable for use as antimicrobial agents via a versatile, readily accessible N-[4-(aminosulfonyl)phenyl]-2-cyanoacetamide (3). The 2-pyridone derivatives were obtained via reaction of cyanoacetamide with acetylacetone or arylidenes malononitrile. Cycloaddition reaction of cyanoacetamide with salicyaldehyde furnished chromene derivatives. Diazotization of 3 with the desired diazonium chloride gave the hydrazone derivatives 13a–e. Also, the reactivity of the hydrazone towards hydrazine hydrate to give Pyrazole derivatives was studied. In addition, treatment of 3 with elemental sulfur and phenyl isothiocyanate or malononitrile furnished thiazole and thiophene derivatives respectively. Reaction of 3 with phenyl isothiocyanate and KOH in DMF afforded the intermediate salt 17 which reacted in situ with 3-(2-bromoacetyl)-2H-chromen-2-one and methyl iodide afforded the thiazole and ketene N,S-acetal derivatives respectively. Finally, reaction of 3 with carbon disulfide and 1,3-dibromopropane afforded the N-[4-(aminosulfonyl) phenyl]-2-cyano-2-(1,3-dithian-2-ylidene)acetamide product 22. All newly synthesized compounds were elucidated by considering the data of both elemental and spectral analysis. The compounds were evaluated for both their in vitro antibacterial and antifungal activities and showed promising results. PMID:24445259

  9. Synthesis and antimicrobial activities of 9H-carbazole derivatives

    Directory of Open Access Journals (Sweden)

    Nadia Salih

    2016-09-01

    Full Text Available In this work 9H-carbazole was utilized as a precursor to prepare new heterocyclic derivatives. Treatment of carbazole 1 with ethyl acetoacetate gave ethyl 9H-carbazol-9-ylacetate 2. The acetate ester derivative 2 was transformed into the 2-(9H-carbazol-9-ylacetohydrazide 3 through treatment with hydrazine hydrate. Reaction of compound 3 with sodium nitrite/HCl afforded [(9H-carbazol-9-ylacetylamino]diazonium chloride 4. Compounds 3-[3-(9H-carbazol-9-ylacetyltriazanylidene]pentane-2,4-dione 5 and ethyl 2-[3-(9H-carbazol-9-ylacetyltriazanylidene]-3-oxobutnoate 6 were obtained by reaction of compound 4 with acetylacetone and ethyl acetoacetate, respectively. Treatment of compounds 5 and 6 with urea and phenylhydrazine afforded 5-[3-(9H-carbazol-9-ylacetyltriazanylidene]-4,6-dimethyl pyrimidin-2(5H-one 7 and 4-[3-(9H-carbazol-9-yl acetyltriazanylidene]-5-methyl-2-phenyl-2,4-dihydro-3H-pyrazol-3-one 8, respectively. The structures of the synthesized compounds were characterized by IR, 1H NMR, 13C NMR and elemental analysis. All synthesized products were tested and evaluated as antimicrobial agents.

  10. Synthesis and Antimicrobial Evaluation of Some Novel Thiazole, Pyridone, Pyrazole, Chromene, Hydrazone Derivatives Bearing a Biologically Active Sulfonamide Moiety

    Directory of Open Access Journals (Sweden)

    Elham S. Darwish

    2014-01-01

    Full Text Available This study aimed for the synthesis of new heterocyclic compounds incorporating sulfamoyl moiety suitable for use as antimicrobial agents via a versatile, readily accessible N-[4-(aminosulfonylphenyl]-2-cyanoacetamide (3. The 2-pyridone derivatives were obtained via reaction of cyanoacetamide with acetylacetone or arylidenes malononitrile. Cycloaddition reaction of cyanoacetamide with salicyaldehyde furnished chromene derivatives. Diazotization of 3 with the desired diazonium chloride gave the hydrazone derivatives 13a–e. Also, the reactivity of the hydrazone towards hydrazine hydrate to give Pyrazole derivatives was studied. In addition, treatment of 3 with elemental sulfur and phenyl isothiocyanate or malononitrile furnished thiazole and thiophene derivatives respectively. Reaction of 3 with phenyl isothiocyanate and KOH in DMF afforded the intermediate salt 17 which reacted in situ with 3-(2-bromoacetyl-2H-chromen-2-one and methyl iodide afforded the thiazole and ketene N,S-acetal derivatives respectively. Finally, reaction of 3 with carbon disulfide and 1,3-dibromopropane afforded the N-[4-(aminosulfonyl phenyl]-2-cyano-2-(1,3-dithian-2-ylideneacetamide product 22. All newly synthesized compounds were elucidated by considering the data of both elemental and spectral analysis. The compounds were evaluated for both their in vitro antibacterial and antifungal activities and showed promising results.

  11. Ultraviolet curing of acrylated liquid natural rubber for surface coating application

    Directory of Open Access Journals (Sweden)

    Kannikar Kwanming

    2009-01-01

    Full Text Available Ultraviolet curable acrylated liquid natural rubber was prepared by grafting of photosensitive molecule onto liquid natural rubber for surface coating application. The liquid natural rubber (LNR was firstly obtained by degradation of natural rubber latex with hydrogen peroxide and cobalt acetylacetonate at 65oC for 72 hrs. The preparation of acrylated natural rubber was carried out by the reaction of acrylic acid and epoxidized liquid natural rubber (ELNR prior obtained from LNR with formic acid and hydrogen peroxide in the ratio of 2:1 by weight in toluene at 80oC for 6, 9, 12, 18, and 24 hrs. It was found that the percentage of acrylate grafted onto liquid natural rubber depended on the reaction time. Surface coating was performed by using acrylated liquid natural rubber and 1,6-hexanediol diacrylate (HDDA or tripropylene glycol diacrylate (TPGDA as a crosslinker and Irgarcure 184 or Irgarcure 651 as a photoinitiator under UV exposure for 30, 60, and 90 seconds. The hardness test of cured products was investigated using the Pencil hardness test at pencil level of 2B to 6H. It was found that the highest hardness of surface coating was at pencil level of 4H for the product using TPGDA and Irgacure 651 in the ratio of 80:10 parts per hundred of rubber (phr. The cured products were able to resist to 2% H2SO4 and distilled water for more than 24 hrs.

  12. The Influence of Chain Microstructure of Biodegradable Copolyesters Obtained with Low-Toxic Zirconium Initiator to In Vitro Biocompatibility

    Science.gov (United States)

    Orchel, Arkadiusz; Kasperczyk, Janusz; Marcinkowski, Andrzej; Pamula, Elzbieta; Orchel, Joanna; Bielecki, Ireneusz

    2013-01-01

    Because of the wide use of biodegradable materials in tissue engineering, it is necessary to obtain biocompatible polymers with different mechanical and physical properties as well as degradation ratio. Novel co- and terpolymers of various composition and chain microstructure have been developed and applied for cell culture. The aim of this study was to evaluate the adhesion and proliferation of human chondrocytes to four biodegradable copolymers: lactide-coglycolide, lactide-co-ε-caprolactone, lactide-co-trimethylene carbonate, glycolide-co-ε-caprolactone, and one terpolymer glycolide-colactide-co-ε-caprolactone synthesized with the use of zirconium acetylacetonate as a nontoxic initiator. Chain microstructure of the copolymers was analyzed by means of 1H and 13C NMR spectroscopy and surface properties by AFM technique. Cell adhesion and proliferation were determined by CyQUANT Cell Proliferation Assay Kit. After 4 h the chondrocyte adhesion on the surface of studied materials was comparable to standard TCPS. Cell proliferation occurred on all the substrates; however, among the studied polymers poly(L-lactide-coglycolide) 85 : 15 that characterized the most blocky structure best supported cell growth. Chondrocytes retained the cell membrane integrity evaluated by the LDH release assay. As can be summarized from the results of the study, all the studied polymers are well tolerated by the cells that make them appropriate for human chondrocytes growth. PMID:24062998

  13. /sup 111/In autologous leucocytes in the diagnosis and assessment of inflammatory bowel disease. [Tropolone

    Energy Technology Data Exchange (ETDEWEB)

    Saverymuttu, S.H.; Peters, A.M.; Chadwick, V.S.; Hodgson, H.J.; Lavender, J.P. (Hammersmith Hospital, London (UK))

    1982-01-01

    Indium-111 autologous leukocyte scanning is now established as an effective method of localising sepsis (Ascher and others, 1980). In view of the extensive leucocyte infiltration of the intestinal wall in inflammatory bowel disease, the authors have prospectively studied the use of indium-111 labelled white cells in a variety of inflammatory bowel disorders. Leukocytes were labelled in 68 patients using /sup 111/In acetylacetonate and in 18 patients /sup 111/In tropolone. Crude mixed leukocytes preparations were used in 74 patients and pure neutrophil preparation used in 12 patients. Gamma scans over the abdomen were performed from 40 min later after re-injection of the labelled cells and assessed. /sup 111/In-tropolone labelling appeared to offer the advantage over /sup 111/In-acac labelling in localising inflamed bowel earlier. The technique of /sup 111/In-leukocyte scanning offers several advantages over the alternative technique of imaging diseased bowel using gallium-67 citrate. Indium-111 leukocyte scanning provides a novel approach to the problem of diagnosis and assessment of inflammatory bowel disease. It is non-invasive, requires no bowel preparation and this is safe in the acutely sick patient where conventional radiological imaging methods may be hazardous. /sup 111/In faecal excretion provides an objective assessment of disease activity which should prove useful in evaluating treatment regimes.

  14. MOCVD of zirconium oxide thin films: Synthesis and characterization

    International Nuclear Information System (INIS)

    Torres-Huerta, A.M.; Dominguez-Crespo, M.A.; Ramirez-Meneses, E.; Vargas-Garcia, J.R.

    2009-01-01

    The synthesis of thin films of zirconia often produces tetragonal or cubic phases, which are stable at high temperatures, but that can be transformed into the monoclinic form by cooling. In the present study, we report the deposition of thin zirconium dioxide films by metalorganic chemical vapor deposition using zirconium (IV)-acetylacetonate as precursor. Colorless, porous, homogeneous and well adherent ZrO 2 thin films in the cubic phase were obtained within the temperature range going from 873 to 973 K. The deposits presented a preferential orientation towards the (1 1 1) and (2 2 0) planes as the substrate temperature was increased, and a crystal size ranging between 20 and 25 nm. The kinetics is believed to result from film growth involving the deposition and aggregation of nanosized primary particles produced during the CVD process. A mismatch between the experimental results obtained here and the thermodynamic prediction was found, which can be associated with the intrinsic nature of the nanostructured materials, which present a high density of interfaces.

  15. MOCVD of zirconium oxide thin films: Synthesis and characterization

    Energy Technology Data Exchange (ETDEWEB)

    Torres-Huerta, A.M., E-mail: atohuer@hotmail.com [Centro de Investigacion en Ciencia Aplicada y Tecnologia Avanzada, Unidad Altamira, Instituto Politecnico Nacional, Km. 14.5 Carr. Tampico-Puerto Industrial, C.P. 89600, Altamira, Tamaulipas (Mexico); Dominguez-Crespo, M.A.; Ramirez-Meneses, E. [Centro de Investigacion en Ciencia Aplicada y Tecnologia Avanzada, Unidad Altamira, Instituto Politecnico Nacional, Km. 14.5 Carr. Tampico-Puerto Industrial, C.P. 89600, Altamira, Tamaulipas (Mexico); Vargas-Garcia, J.R. [ESIQIE, Departamento de Metalurgia y Materiales, Instituto Politecnico Nacional. A.P. 75-876, 07300 Mexico, D.F. (Mexico)

    2009-02-15

    The synthesis of thin films of zirconia often produces tetragonal or cubic phases, which are stable at high temperatures, but that can be transformed into the monoclinic form by cooling. In the present study, we report the deposition of thin zirconium dioxide films by metalorganic chemical vapor deposition using zirconium (IV)-acetylacetonate as precursor. Colorless, porous, homogeneous and well adherent ZrO{sub 2} thin films in the cubic phase were obtained within the temperature range going from 873 to 973 K. The deposits presented a preferential orientation towards the (1 1 1) and (2 2 0) planes as the substrate temperature was increased, and a crystal size ranging between 20 and 25 nm. The kinetics is believed to result from film growth involving the deposition and aggregation of nanosized primary particles produced during the CVD process. A mismatch between the experimental results obtained here and the thermodynamic prediction was found, which can be associated with the intrinsic nature of the nanostructured materials, which present a high density of interfaces.

  16. A comparative study of alumina-supported Ni catalysts prepared by photodeposition and impregnation methods on the catalytic ozonation of 2,4-dichlorophenoxyacetic acid

    International Nuclear Information System (INIS)

    Rodríguez, Julia L.; Valenzuela, Miguel A.; Tiznado, Hugo; Poznyak, Tatiana; Chairez, Isaac; Magallanes, Diana

    2017-01-01

    The heterogeneous catalytic ozonation on unsupported and supported oxides has been successfully tested for the removal of several refractory compounds in aqueous solution. In this work, alumina-supported nickel catalysts prepared by photodeposition and impregnation methods were compared in the catalytic ozonation of 2,4-dichlorophenoxyacetic acid (2,4-D). The catalysts were characterized by high-resolution electron microscopy and X-ray photoelectron spectroscopy. The photochemical decomposition of Ni acetylacetonate to produce Ni(OH) 2 , NiO, and traces of Ni° deposited on alumina was achieved in the presence of benzophenone as a sensitizer. A similar surface composition was found with the impregnated catalyst after its reduction with hydrogen at 500 °C and exposed to ambient air. Results indicated a higher initial activity and maleic acid (byproduct) concentration with the photodeposited catalyst (1 wt% Ni) compared to the impregnated catalyst (3 wt% Ni). These findings suggest the use of the photodeposition method as a simple and reliable procedure for the preparation of supported metal oxide/metal catalysts under mild operating conditions.

  17. The Preparation of TiO₂ Film by the Sol-Gel Method and Evaluation of Its Self-Cleaning Property.

    Science.gov (United States)

    Liang, Yu; Sun, Sijia; Deng, Tongrong; Ding, Hao; Chen, Wanting; Chen, Ying

    2018-03-19

    TiO₂ sol was produced by the sol-gel method through the hydrolysis and the aging of tetrabutyl titanate and the TiO₂ film was obtained by dipping and uniform lifting of the acid-treated and ultrasound-treated clean glass slides into the TiO₂ sol followed by aging, drying, and calcination. The effect of the hydrolysis control agents to the formed sol was researched and the crystalline state, the morphology, and the photocatalytic properties of the products after calcination were characterized. The structural morphology, the contact angles before and after illumination, and the self-cleaning properties of the TiO₂ film were characterized as well. The results showed that by using acetylacetone as the hydrolysis control agent, the formed TiO₂ sol had relatively high stability. The product after the calcination of the TiO₂ sol was of single anatase type with crystalline size of 18-20 nm and it could degrade nearly 100% of methylene blue after 90 min illumination. The formed TiO₂ film is compact, continuous, smooth, and had the properties of super-hydrophilicity (after 30 min illumination due to its contact angle decreasing from 21° to nearly 0°) and anti-fogging capability, which indicated its excellent self-cleaning property.

  18. Effect of Particle Size on the Magnetic Properties of Ni Nanoparticles Synthesized with Trioctylphosphine as the Capping Agent

    Directory of Open Access Journals (Sweden)

    Toshitaka Ishizaki

    2016-09-01

    Full Text Available Magnetic cores of passive components are required to have low hysteresis loss, which is dependent on the coercive force. Since it is well known that the coercive force becomes zero at the superparamagnetic regime below a certain critical size, we attempted to synthesize Ni nanoparticles in a size-controlled fashion and investigated the effect of particle size on the magnetic properties. Ni nanoparticles were synthesized by the reduction of Ni acetylacetonate in oleylamine at 220 °C with trioctylphosphine (TOP as the capping agent. An increase in the TOP/Ni ratio resulted in the size decrease. We succeeded in synthesizing superparamagnetic Ni nanoparticles with almost zero coercive force at particle size below 20 nm by the TOP/Ni ratio of 0.8. However, the saturation magnetization values became smaller with decrease in the size. The saturation magnetizations of the Ni nanoparticles without capping layers were calculated based on the assumption that the interior atoms of the nanoparticles were magnetic, whereas the surface-oxidized atoms were non-magnetic. The measured and calculated saturation magnetization values decreased in approximately the same fashion as the TOP/Ni ratio increased, indicating that the decrease could be mainly attributed to increases in the amounts of capping layer and oxidized surface atoms.

  19. Effects of solvent and chelating agent on synthesis of solid oxide fuel cell perovskite, La0.8Sr0.2CrO3-δ

    International Nuclear Information System (INIS)

    Lee, Byoung I.; Gupta, Ravindra K.; Whang, Chin M.

    2008-01-01

    Effects of solvent and chelating agent on synthesis of La 0.8 Sr 0.2 CrO 3-δ perovskite are reported. Samples are synthesized using a solvent (ethylene glycol or 2-methoxyethanol) and a chelating agent (acetylacetone, citric acid or ethylene diamine tetraacetic acid) by polymeric-gel method, and characterized by X-ray diffractometry and Fourier-transform infrared spectroscopy. Citric acid to metal cations molar ratio (Rc) is varied for ethylene glycol-citric acid system. Samples are mainly orthorhombic perovskite. SrCrO 4 is appeared as a secondary phase and found to be the lowest for ethylene glycol-citric acid combination with Rc equal to 7. Crystallographic parameters of perovskite phase are determined and compared with those of LaCrO 3 . A mechanism employing a partial-charge model, chelating effect and solvent-cage effect is proposed to explain the results. Effect of sintering temperature on phase, relative density and morphology of samples prepared using ethylene glycol and citric acid (Rc = 7) is also reported

  20. Mesoporous activated carbons with metal-oxide particles prepared from Morwell coal; Morwell tan wo genryo to shita kinzoku sankabutsu tanji kasseitan no saiko kozo

    Energy Technology Data Exchange (ETDEWEB)

    Yoshizawa, N.; Yamada, Y.; Shiraishi, M. [National Institute for Resources and Environment, Tsukuba (Japan); Kojima, S.; Tamai, H.; Yasuda, H. [Hiroshima University, Hiroshima (Japan). Faculty of Engineering

    1996-10-28

    The metal dependence of mesoporous activated carbons with various metal acetylacetonate (acac) particles prepared from Morwell coal was studied. In experiment, the mixture of Morwell coal and acac metal complexes were dissipated into tetrahydrofuran, and after agitation in Ar atmosphere, the solvent was removed by vacuum distillation. Coal specimens with Fe(acac)3, Ni(acac)2 and Co(acac)2 as acac complexes were activated by exchanging flow gas with water vapor after heat treatment in N2 gas flow at 900{degree}C. The pore sizes of the specimens were obtained from N2 adsorption isotherms by BET method and BJH method. Conditions of pores and metals in the specimens were examined by XRD measurement and TEM observation. The relation between the above conditions and pore characteristics obtained from adsorption experiment was also examined. As a result, the difference in mesopore ratio between the specimens and blank specimens was larger in the order of Fe, Co and Ni, and the effect of added metal complexes was also larger in this order. 3 refs., 3 figs., 3 tabs.

  1. Tetragonal zirconia quantum dots in silica matrix prepared by a modified sol-gel protocol

    Science.gov (United States)

    Verma, Surbhi; Rani, Saruchi; Kumar, Sushil

    2018-05-01

    Tetragonal zirconia quantum dots (t-ZrO2 QDs) in silica matrix with different compositions ( x)ZrO2-(100 - x)SiO2 were fabricated by a modified sol-gel protocol. Acetylacetone was added as a chelating agent to zirconium propoxide to avoid precipitation. The powders as well as thin films were given thermal treatment at 650, 875 and 1100 °C for 4 h. The silica matrix remained amorphous after thermal treatment and acted as an inert support for zirconia quantum dots. The tetragonal zirconia embedded in silica matrix transformed into monoclinic form due to thermal treatment ≥ 1100 °C. The stability of tetragonal phase of zirconia is found to enhance with increase in silica content. A homogenous dispersion of t-ZrO2 QDs in silica matrix was indicated by the mapping of Zr, Si and O elements obtained from scanning electron microscope with energy dispersive X-ray analyser. The transmission electron images confirmed the formation of tetragonal zirconia quantum dots embedded in silica. The optical band gap of zirconia QDs (3.65-5.58 eV) was found to increase with increase in zirconia content in silica. The red shift of PL emission has been exhibited with increase in zirconia content in silica.

  2. Structural and Luminescence Properties of Lu2O3:Eu3+ F127 Tri-Block Copolymer Modified Thin Films Prepared by Sol-Gel Method

    Science.gov (United States)

    de Jesus Morales Ramírez, Angel; Hernández, Margarita García; Murillo, Antonieta García; de Jesús Carrillo Romo, Felipe; Palmerin, Joel Moreno; Velazquez, Dulce Yolotzin Medina; Jota, María Luz Carrera

    2013-01-01

    Lu2O3:Eu3+ transparent, high density, and optical quality thin films were prepared using the sol-gel dip-coating technique, starting with lutetium and europium nitrates as precursors and followed by hydrolysis in an ethanol-ethylene glycol solution. Acetic acid and acetylacetonate were incorporated in order to adjust pH and as a sol stabilizer. In order to increment the thickness of the films and orient the structure, F127 Pluronic acid was incorporated during the sol formation. Structural, morphological, and optical properties of the films were investigated for different F127/Lu molar ratios (0–5) in order to obtain high optical quality films with enhanced thickness compared with the traditional method. X-ray diffraction (XRD) shows that the films present a highly oriented cubic structure beyond 1073 K for a 3-layer film, on silica glass substrates. The thickness, density, porosity, and refractive index evolution of the films were investigated by means of m-lines microscopy along with the morphology by scanning electron microscope (SEM) and luminescent properties. PMID:28809336

  3. Highly conductive electrospun carbon nanofiber/MnO2 coaxial nano-cables for high energy and power density supercapacitors

    Science.gov (United States)

    Zhi, Mingjia; Manivannan, Ayyakkannu; Meng, Fanke; Wu, Nianqiang

    2012-06-01

    This paper presents highly conductive carbon nanofiber/MnO2 coaxial cables in which individual electrospun carbon nanofibers are coated with an ultrathin hierarchical MnO2 layer. In the hierarchical MnO2 structure, an around 4 nm thick sheath surrounds the carbon nanofiber (CNF) in a diameter of 200 nm, and nano-whiskers grow radically outward from the sheath in view of the cross-section of the coaxial cables, giving a high specific surface area of MnO2. The CNFs are synthesized by electrospinning a precursor containing iron acetylacetonate (AAI). The addition of AAI not only enlarges the specific surface area of the CNF but also greatly enhances their electronic conductivity, which leads to a dramatic improvement in the specific capacitance and the rate capability of the CNF/MnO2 electrode. The AAI-CNF/MnO2 electrode shows a specific capacitance of 311 F g-1 for the whole electrode and 900 F g-1 for the MnO2 shell at a scan rate of 2 mV s-1. Good cycling stability, high energy density (80.2 Wh kg-1) and high power density (57.7 kW kg-1) are achieved. This work indicates that high electronic conductivity of the electrode material is crucial to achieving high power and energy density for pseudo-supercapacitors.

  4. Simulated reaction of formaldehyde and ambient atmospheric particulate matter using a chamber

    Institute of Scientific and Technical Information of China (English)

    Yueyue Chen; Jia Liu; Jing Shang; Tong Zhu

    2017-01-01

    The reaction of HCHO with Beijing winter's real ambient particulate matter (PM) inside a 3.3 m3 Teflon Chamber was conducted in this study.NO2,O3 and H2O gases were removed from the ambient aerosol before entering into the chamber.The decays of HCHO were monitored (acetylacetone spectrophotometry method) during the reactions at different PM number concentrations (Na) and relative humidities (RHs),and the formed particulate formate was detected by IC and XPS techniques.The results showed that when RH was 10%-15%,the decay rate of HCHO in the chamber was higher with the existence of PM from relatively clean days (with number concentration (Na) < 200,000 particle/L,0.35-22.5 μm) compared to dirty days (Na > 200,000 particle/L,0.35-22.5 μm).When RH increased to 30%-45%,PM can hardly have significant influences on the decay of HCHO.The formations of formate on the reacted PM were consistent with the HCHO decay rates at different ambient PM Na and RH conditions.This is a first study related to the "real" ambient PM reacted with HCHO and suggested that in the clean and low RH days,PM could be an effective medium for the conversion of HCHO to formate.

  5. Remedial action of matrices contaminated by cobalt with supercritical CO_2: contribution to the understanding of the complex formation mechanisms and to the diphasic transfers

    International Nuclear Information System (INIS)

    Gervais, Florence

    2001-01-01

    Soils rehabilitation using supercritical CO_2 seems an interesting alternative way to existing techniques. No effluents are generated during the supercritical fluid extraction, which is the main advantage of this process. In order to be extracted by this techniques, metals or radionuclides have to be complexed by suitable chelating agents. Beta-diketones and dithiocarbamates (fluorinated or not) have been chosen. The first part of this work deals with chemical equilibria mechanisms study in an aqueous phase. Experiments show a very weak cobalt complexation kinetics with acetylacetone. Moreover, this complex exhibit a hydrophilic behaviour. On the other hand, cobalt and dithiocarbamate instantaneously from a chelate which is very hydrophobic. Mass transfer between extracting and aqueous phases (hexane and SC CO_2) are also investigated. Supercritical CO_2 seems to have a greater affinity towards fluorinated beta-diketones than hexane. This tendency is confirmed by in situ commercial chelates (fluorinates or not) solubility measurements using X-ray absorption spectroscopy. However, cobalt-beta-diketonates are hydrophilic because of their partial hydration. This kind of chelating agents is not suitable to cobalt supercritical fluid extraction from an aqueous phase. Inversely, distribution coefficients of hydrophobic dithiocarbamates are higher than beta-diketonates, whatever the extracting solvent is. Metals extraction from an aqueous matrix seems possible with these chelating agents. (author) [fr

  6. Poly(L-lactic acid) microspheres containing neutron-activatable holmium-165: a study of the physical characteristics of microspheres before and after irradiation in a nuclear reactor.

    Science.gov (United States)

    Mumper, R J; Jay, M

    1992-01-01

    The solvent evaporation technique was employed to prepare poly(L-lactic acid) (PLA) microspheres with 165Ho acetylacetonate (Ho-AcAc). Particle size, percentage Ho-165, percent residual solvent, and retentive ability of the spheres were found to be strongly affected by preparatory conditions. Differential scanning calorimetry (DSC) thermograms suggested that the Ho-AcAc existed in the PLA matrix as a molecular dispersion. High neutron flux irradiations of the PLA spheres in a nuclear reactor produced Ho-166, a therapeutic radionuclide that emits high-energy negatrons (Emax = 1.84 MeV; half-life = 26.9 hr). The gamma radiation dose (53-75 Mrad) from the core of the reactor provided an overkill of all bioburdens in the PLA spheres. Gel permeation chromatography (GPC) analysis showed that these irradiations caused a reduction in PLA molecular weight. Infrared spectra, 13C NMR spectra, 1H NMR spectra, and DSC thermograms further confirmed the presence of lower molecular weight PLA but proved the overall maintenance of PLA structure.

  7. Synthesis and characterization of thin films of Pd/TiO2 with possible applications in photo catalysis

    International Nuclear Information System (INIS)

    Tirado G, S.; Valenzuela Z, M. A.

    2015-10-01

    In this paper the synthesis and study of thin films of titanium oxide is reported, as well as those that were surface modified with palladium nanoparticles Pd/TiO 2 . First, the TiO 2 films are grown on substrates of soda-lime glass using chemical sol-gel route and the repeated immersion procedure. The salt precursor titanium oxy-acetylacetonate to 0.2 M, in the solvent 2-methoxyethanol and monoethanolamine was used as stabilizer. The number of used immersions gave an average thickness estimate for these films of 172.8 nm. Second, the series of Pd/TiO 2 films surface modified were obtained from a solution of palladium nitrate dehydrate at low concentration, with the same procedure. The films grown TiO 2 and those surface-modified films were characterized in its structure by X-ray diffraction, morphology by scanning electron microscopy, the topography with atomic force microscopy, optical properties by UV-Vis, among others. Photoluminescence properties and/or possible applications in photo catalysis are reported in this paper. (Author)

  8. A versatile single molecular precursor for the synthesis of layered oxide cathode materials for Li-ion batteries.

    Science.gov (United States)

    Li, Maofan; Liu, Jiajie; Liu, Tongchao; Zhang, Mingjian; Pan, Feng

    2018-02-01

    A carbonyl-bridged single molecular precursor LiTM(acac) 3 [transition metal (TM) = cobalt/manganese/nickel (Co/Mn/Ni), acac = acetylacetone], featuring a one-dimensional chain structure, was designed and applied to achieve the layered oxide cathode materials: LiTMO 2 (TM = Ni/Mn/Co, NMC). As examples, layered oxides, primary LiCoO 2 , binary LiNi 0.8 Co 0.2 O 2 and ternary LiNi 0.5 Mn 0.3 Co 0.2 O 2 were successfully prepared to be used as cathode materials. When they are applied to lithium-ion batteries (LIBs), all exhibit good electrochemical performance because of their unique morphology and great uniformity of element distribution. This versatile precursor is predicted to accommodate many other metal cations, such as aluminum (Al 3+ ), iron (Fe 2+ ), and sodium (Na + ), because of the flexibility of organic ligand, which not only facilitates the doping-modification of the NMC system, but also enables synthesis of Na-ion layered oxides. This opens a new direction of research for the synthesis of high-performance layered oxide cathode materials for LIBs.

  9. Electrical conductivity in Fe_2O_3 and CoFe_2O_4 nanoparticle arrays and their application in gas sensing

    International Nuclear Information System (INIS)

    Luby, S.; Benkovicova, M.; Jergel, M.; Siffalovic, P.; Majkova, E.; Rella, R.; Capone, S.; Manera, M. G.

    2013-01-01

    In this paper we summarize the results obtained as a by product of γ-Fe_2O_3 and CoFe_2O_4 sensors testing. Monodisperse γ-Fe_2O_3 and CoFe_2O_4 NPs with the size of 6.4 ± 0.6 and 7.6 ± 0.6 nm, respectively, were synthesized by high-temperature solution phase reaction from methyl acetylacetonates. The thickness of surfactant is 1 nm and 0.8 nm for two types of NPs, respectively. Surfactant stops the growth of NPs at a certain size. The self-assembled NP monolayers were prepared by Langmuir-Blodgett technique from the colloid solutions spread on the water sub-phase in a standard LB trough. M = 1, 2, 4 or 10 NP monolayers (L) were deposited onto auxiliary oxidized Si substrates or onto 2 mm x 2 mm Al_2O_3 sensor substrates equipped with 20 nm Ti/500 nm Pt comb electrodes to read the measuring current and with 20 nm Ti/500 nm Pt meander on the back side for the heating of the structure to a working temperature. Material properties of NPs and arrays were studied by SEM/EDS, GI XRD, GISAXS, XANES and ellipsometry. (authors)

  10. Spectroscopic Characteristics of Highly Selective Manganese Catalysis in Acqueous Polyurethane Systems

    Directory of Open Access Journals (Sweden)

    Miroljub Barac

    2006-11-01

    Full Text Available The latest investigations on producing more efficient catalytic aqueouspolyurethane systems are in the domain of metal complexes with mixed ligands. In ourprevious research works, the high selectivity for the isocyanate-hydroxyl reaction inaqueous polyurethane systems has been shown by the manganese(III mixed-ligandcomplexes. The two new complexes have been prepared with two acetylacetonate (acacligands and one maleate ligand and its hydroxylamine derivative of the general formula[Mn(C5H7O22L]. Their structures have been established by using the fundamental analyses,the FTIR and UV/VIS spectroscopic methods, as well as the magnetic measurements. Inorder to explain the different selectivity of the manganese(III mixed-ligand complexes, theUV and ESR spectroscopy have been employed to determine the kinetics of the complexes’decomposition. The thermal stability of the complexes has been determined by way of thedynamic TG method at the heating rate of 5°C⋅min-1 and at the temperature ranged 20-550°C. It suggests the decomposition of the complexes by loss of acid ligand. The main factor in the selective catalysis control in theaqueous polyurethane systems is the nature of the acid ligands and their impact on themanganese(II/manganese(III equilibrium.

  11. Synthesis of Some Novel Heterocyclic and Schiff Base Derivatives as Antimicrobial Agents

    Directory of Open Access Journals (Sweden)

    Mohamed E. Azab

    2015-10-01

    Full Text Available Treatment of 2,3-diaryloxirane-2,3-dicarbonitriles 1a–c with different nitrogen nucleophiles, e.g., hydrazine, methyl hydrazine, phenyl hydrazine, hydroxylamine, thiosemicarbazide, and/or 2-amino-5-phenyl-1,3,4-thiadiazole, afforded pyrazole, isoxazole, pyrrolotriazine, imidazolothiadiazole derivatives 2–5, respectively. Reacting pyrazoles 2a–c with aromatic aldehydes and/or methyl glycinate produced Schiff’s bases 7a–d and pyrazolo[3,4-b]-pyrazinone derivative 8, respectively. Treating 7 with ammonium acetate and/or hydrazine hydrate, furnished the imidazolopyrazole and pyrazolotriazine derivatives 9 and 10, respectively. Reaction of 8 with chloroacetic acid and/or diethyl malonate gave tricyclic compound 11 and triketone 12, respectively. On the other hand, compound 1 was reacted with active methylene precursors, e.g., acetylacetone and/or cyclopentanone producing adducts 14a,b which upon fusion with ammonium acetate furnished the 3-pyridone derivatives 15a,b, respectively. Some of newly synthesized compounds were screened for activity against bacterial and fungal strains and most of the newly synthesized compounds showed high antimicrobial activities. The structures of the new compounds were elucidated using IR, 1H-NMR, 13C-NMR and mass spectroscopy.

  12. Charge separation in photoinitiated electron transfer reactions induced by a polyelectrolyte

    International Nuclear Information System (INIS)

    Meyerstein, D.; Rabani, J.; Matheson, M.S.; Meisel, D.

    1978-01-01

    When uncharged molecules quench the luminescence of Ru(bpy) 3 /sup 2+*/ by electron transfer to the quencher, the addition of poly(vinyl sulfate) (PVS) may, through its potential field, affect the rate of quenching, enhance the net separated charge yield, and slow the back reaction of the separated photoredox products. In all such cases that we have studied the quenching rate in the presence of PVS was reduced to about 60% of the rate measured in the absence of PVS. For two neutral species, iron(III) nitrilotriacetate (FeNTA) and cobalt(III) acetylacetonate (Co(acac) 3 ), photoreduction of the quencher was observed, and the redox yield escaping geminate recombination was substantially increased by added PVS. In the case of FeNTA the rate of the bulk back reaction was not changed appreciably by the presence of PVS owing to the rapid neutralization of Fe(NTA) - by protonation. For Co(acac) 3 the rate of the bulk back reaction was decreased by several orders of magnitude and the back reaction was shown to occur via the enolate form of the ligand which is released to the bulk solution. 4 figures, 4 tables

  13. Highly efficient and simplified phosphorescence white organic light-emitting diodes based on synthesized deep-blue host and orange emitter

    Energy Technology Data Exchange (ETDEWEB)

    Koo, Ja Ryong; Lee, Seok Jae; Hyung, Gun Woo; Kim, Bo Young; Lee, Dong Hyung [Department of Information Display, Hongik University, Seoul 121-791 (Korea, Republic of); Kim, Woo Young [Department of Green Energy and Semiconductor Engineering, Hoseo University, Asan 336-795 (Korea, Republic of); Lee, Kum Hee [Department of Chemistry, Sungkyunkwan University, Suwon 440-746 (Korea, Republic of); Yoon, Seung Soo, E-mail: ssyoon@skku.edu [Department of Chemistry, Sungkyunkwan University, Suwon 440-746 (Korea, Republic of); Kim, Young Kwan, E-mail: kimyk@hongik.ac.kr [Department of Information Display, Hongik University, Seoul 121-791 (Korea, Republic of)

    2013-10-01

    The authors have demonstrated a highly efficient and stable phosphorescent white organic light-emitting diode (WOLED), which has been achieved by doping only one orange phosphorescent emitter, Bis(5-benzoyl-2-(4-fluorophenyl)pyridinato-C,N)iridium(III) acetylacetonate into an appropriate deep blue phosphorescent host, 4,4'-bis(4-(triphenylsilyl)phenyl)-1,1'-binaphthyl as an emitting layer (EML). The WOLED has been achieved by effective confinement of triplet excitons to emit a warm white color. The optimized WOLED, with a simple structure as a hole transporting layer-EML-electron transporting layer, showed a maximum luminous efficiency of 22.38 cd/A, a maximum power efficiency of 12.01 lm/W, a maximum external quantum efficiency of 7.32%, and CIEx,y coordinates of (0.38,0.42) at 500 cd/m{sup 2}, respectively. - Highlights: • Highly efficient phosphorescent white organic light-emitting diode (WOLED) • Single emitting layer consists of synthesized deep blue host and orange emitter • The WOLED with high EL efficiencies due to efficient triplet exciton confinement.

  14. Highly efficient and heavily-doped organic light-emitting devices based on an orange phosphorescent iridium complex

    Energy Technology Data Exchange (ETDEWEB)

    Zhou, Shunliang; Wang, Qi [State Key Laboratory of Electronic Thin Films and Integrated Devices, School of Optoelectronic Information, University of Electronic Science and Technology of China (UESTC), Chengdu 610054 (China); Li, Ming [College of Chemistry, Sichuan University, Chengdu, 610064 (China); Lu, Zhiyun, E-mail: luzhiyun@scu.edu.cn [College of Chemistry, Sichuan University, Chengdu, 610064 (China); Yu, Junsheng, E-mail: jsyu@uestc.edu.cn [State Key Laboratory of Electronic Thin Films and Integrated Devices, School of Optoelectronic Information, University of Electronic Science and Technology of China (UESTC), Chengdu 610054 (China)

    2014-10-15

    Heavily doped and highly efficient phosphorescent organic light-emitting devices (PhOLEDs) had been fabricated by utilizing an orange iridium complex, bis[2-(3′,5′-di-tert-butylbiphenyl-4-yl)benzothiazolato-N,C{sup 2'}]iridium(III) (acetylacetonate) [(tbpbt){sub 2}Ir(acac)], as a phosphor. When the doping concentration of [(tbpbt){sub 2}Ir(acac)] reached as high as 15 wt%, the PhOLEDs exhibited a power efficiency, current efficiency, and external quantum efficiency of 24.5 lm/W, 32.1 cd/A, 15.7%, respectively, implying a promising quenching-resistant characteristics of this novel phosphor. Furthermore, the efficient white PhOLEDs had been obtained by employing (tbpbt){sub 2}Ir(acac) as a self-host orange emitter, indicating that (tbpbt){sub 2}Ir(acac) could serve as a promising phosphor to fabricate white organic light-emitting devices with simplified manufacturing process. - Highlights: • Efficient phosphorescent devices were fabricated. • Optimized phosphor doping ratio reached as high as 15 wt%. • The results proved a promising quench-resistant property of the phosphor. • Efficient white devices based on this phosphor as self-host layer had been realized.

  15. Highly efficient and concentration-insensitive organic light-emitting devices based on self-quenching-resistant orange–red iridium complex

    Energy Technology Data Exchange (ETDEWEB)

    Qi, Yige; Wang, Xu [State Key Laboratory of Electronic Thin Films and Integrated Devices, School of Optoelectronic Information, University of Electronic Science and Technology of China (UESTC), Chengdu 610054 (China); Li, Ming [College of Chemistry, Sichuan University, Chengdu 610064 (China); Lu, Zhiyun, E-mail: luzhiyun@scu.edu.cn [College of Chemistry, Sichuan University, Chengdu 610064 (China); Yu, Junsheng, E-mail: jsyu@uestc.edu.cn [State Key Laboratory of Electronic Thin Films and Integrated Devices, School of Optoelectronic Information, University of Electronic Science and Technology of China (UESTC), Chengdu 610054 (China)

    2014-11-15

    Orange–red phosphorescent organic light-emitting devices (PHOLEDs) with high efficiency and concentration insensitivity based on a novel iridium complex, bis[2-(biphenyl-4-yl)benzothiazole-N,C{sup 2}′]iridium(III) (acetylacetonate) [(4Phbt){sub 2}Ir(acac)], were fabricated. With the heavily doped emissive layer (EML) of 4,4′-N,N′-dicarbazolylbiphenyl (CBP): (4Phbt){sub 2}Ir(acac) in a wide and easily controlled dopant concentration range from 12 wt% to 24 wt%, a maximum power efficiency of 29 lm/W and an external quantum efficiency of >16% of the PHOLEDs were obtained, implying the insensitivity of electroluminescence (EL) properties to doping concentration. Meanwhile, a maximum power efficiency of 5.0 lm/W was achieved from a non-doped device with neat (4Phbt){sub 2}Ir(acac) as the EML, indicating a superior property of self-quenching resistance. The mechanism of direct exciton formation, in which exciton-formation regions are distributed throughout the EML, is responsible for the significant alleviation of triplet–triplet annihilation and superior EL performance. - Highlights: • Highly efficient and concentration-insensitive PHOLEDs were obtained. • The high efficiency of non-doped PHOLEDs indicated a quenching-resistant property. • The independence of EL spectra on doping concentration was observed. • The heavily doped devices were dominated by mechanism of direct exciton formation.

  16. High-efficiency and heavily doped organic light-emitting devices based on quench-resistant red iridium complex

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Qi [State Key Laboratory of Electronic Thin Films and Integrated Devices, School of Optoelectronic Information, University of Electronic Science and Technology of China, Chengdu 610054 (China); Yu, Junsheng, E-mail: jsyu@uestc.edu.cn [State Key Laboratory of Electronic Thin Films and Integrated Devices, School of Optoelectronic Information, University of Electronic Science and Technology of China, Chengdu 610054 (China); Zhao, Juan; Wang, Jun [State Key Laboratory of Electronic Thin Films and Integrated Devices, School of Optoelectronic Information, University of Electronic Science and Technology of China, Chengdu 610054 (China); Li, Ming [College of Chemistry, Sichuan University, Chengdu 610064 (China); Lu, Zhiyun, E-mail: luzhiyun@scu.edu.cn [College of Chemistry, Sichuan University, Chengdu 610064 (China)

    2013-02-15

    Highly efficient red phosphorescent organic light-emitting devices had been fabricated using a new iridium complex, bis[2-(9,9-dimethyl-9H-fluoren-2-yl) benzothiazolato-N,C{sup 2'}]iridium(III) (acetylacetonate) [(fbt){sub 2}Ir(acac)] as phosphor. With a high doping concentration of 15 wt%, the device exhibited a maximum luminance efficiency, power efficiency and external quantum efficiency (EQE) of 35.2 cd/A, 21.3 lm/W, 18.2%, respectively, indicating an excellent quench-resistant property of (fbt){sub 2}Ir(acac). The results are appealing towards the development of 'easy-to-make' OLEDs. It has been demonstrated that the high efficiency arises from more balanced charge carriers in the emissive layer. - Highlight: Black-Right-Pointing-Pointer We obtained efficient OLEDs based on newly synthesized quench-resistant phosphor. Black-Right-Pointing-Pointer Peak performance was obtained with 15 wt% (fbt){sub 2}Ir(acac) doped device. Black-Right-Pointing-Pointer Our devices gave one of the best performance among heavily-doped red devices. Black-Right-Pointing-Pointer Balanced carrier transport is crucial for the high performance of our devices.

  17. Red phosphorescent organic light-emitting diodes (PhOLEDs) based on a heteroleptic cyclometalated Iridium (III) complex

    Energy Technology Data Exchange (ETDEWEB)

    Lepeltier, Marc [Institut Lavoisier de Versailles, UMR 8180 CNRS, Université de Versailles Saint-Quentin en Yvelines, 45 avenue des Etats-Unis, 78035 Versailles Cedex (France); Dumur, Frédéric, E-mail: frederic.dumur@univ-amu.fr [Aix-Marseille Université, CNRS, ICR, UMR 7273, F-13397 Marseille (France); Wantz, Guillaume, E-mail: guillaume.wantz@ims-bordeaux.fr [University of Bordeaux, IMS, UMR 5218, F-33400 Talence (France); CNRS, IMS, UMR 5218, F-33400 Talence (France); Vila, Neus; Mbomekallé, Israel [Institut Lavoisier de Versailles, UMR 8180 CNRS, Université de Versailles Saint-Quentin en Yvelines, 45 avenue des Etats-Unis, 78035 Versailles Cedex (France); Bertin, Denis; Gigmes, Didier [Aix-Marseille Université, CNRS, ICR, UMR 7273, F-13397 Marseille (France); Mayer, Cédric R., E-mail: cmayer@lisv.uvsq.fr [Laboratoire d’Ingénierie des Systèmes de Versailles LISV – EA 4048, Université de Versailles Saint Quentin en Yvelines, 10/12 avenue de l’Europe, 78140 Vélizy (France)

    2013-11-15

    Highly efficient red-emitting Phosphorescent Organic Light-Emitting Diodes (PhOLEDs) based on a neutral vacuum-sublimatable heteroleptic iridium (III) complex have been designed and studied. Heteroleptic complex Ir(piq){sub 2}(acac) was prepared in one step with acetylacetone (acac) as the ancillary ligand. Electronic and spectroscopic properties of Ir(piq){sub 2}(acac) were investigated by UV–visible absorption, fluorescence spectroscopy and cyclic voltammetry. Electrophosphorescent devices comprising Ir(piq){sub 2}(acac) as dopant of TCTA exhibited outstanding electroluminescence performance with a current efficiency of 10.0 cd A{sup −1}, a maximum power efficiency of 7.2 lm W{sup −1} and a maximal brightness of 3540 cd m{sup −2} was reached at 8.0 V. CIE coordinates close to the standard red of the national television system committee were obtained (0.67, 0.33). -- Highlights: • A saturated red OLED has been prepared. • High power efficiency and brightness were obtained. • Thickness of the device was determined as a parameter determining the overall performance. • CIE coordinates close to the standard red of the national television system committee were obtained.

  18. Multi-Directional Growth of Aligned Carbon Nanotubes Over Catalyst Film Prepared by Atomic Layer Deposition

    Directory of Open Access Journals (Sweden)

    Zhou Kai

    2010-01-01

    Full Text Available Abstract The structure of vertically aligned carbon nanotubes (CNTs severely depends on the properties of pre-prepared catalyst films. Aiming for the preparation of precisely controlled catalyst film, atomic layer deposition (ALD was employed to deposit uniform Fe2O3 film for the growth of CNT arrays on planar substrate surfaces as well as the curved ones. Iron acetylacetonate and ozone were introduced into the reactor alternately as precursors to realize the formation of catalyst films. By varying the deposition cycles, uniform and smooth Fe2O3 catalyst films with different thicknesses were obtained on Si/SiO2 substrate, which supported the growth of highly oriented few-walled CNT arrays. Utilizing the advantage of ALD process in coating non-planar surfaces, uniform catalyst films can also be successfully deposited onto quartz fibers. Aligned few-walled CNTs can be grafted on the quartz fibers, and they self-organized into a leaf-shaped structure due to the curved surface morphology. The growth of aligned CNTs on non-planar surfaces holds promise in constructing hierarchical CNT architectures in future.

  19. Separations Science Data Base: an abstractor's manual

    International Nuclear Information System (INIS)

    Roddy, J.W.; McDowell, W.J.; Michelson, D.C.

    1981-07-01

    The Separations Science Data Base, designed specifically for the retrieval of information needed in chemical separations problems (i.e., how to perform a given separation under given conditions), is described. The procedure for entering records into the data base is given. The initial entries are concerned primarily with liquid-liquid extraction and liquid-solid ion exchange methods for metal ions and salts; however, the data base is constructed so that almost any separations process can be accommodated. Each record is indexed with information provided under the following fields: author; title; publication source; date of publication; organization performing and/or sponsoring the work; brief abstract of the work; abstract number if the work has been so referenced, and/or abstractor's initials; type of separation system used (e.g., flotation); specific or generic name of the separation agent used (e.g., acetylacetone); list of substances separated (e.g., gold, copper); qualitative description of the supporting medium or matrix containing the substances before separation (e.g., nitrate); type of literature where the article was printed (e.g., book); and type of information that the article contains. Each of these fields may be searched independently of the others (or in combination), and the last six fields contain specific key words that are listed on the input form. Definitions are provided for the 39 information terms

  20. Efficient white organic light-emitting devices based on blue, orange, red phosphorescent dyes

    International Nuclear Information System (INIS)

    Chen Ping; Duan Yu; Xie Wenfa; Zhao Yi; Hou Jingying; Liu Shiyong; Zhang Liying; Li Bin

    2009-01-01

    We demonstrate efficient white organic light-emitting devices (WOLEDs) based on an orange phosphorescent iridium complex bis(2-(2-fluorphenyl)-1,3-benzothiozolato-N, C 2' )iridium(acetylacetonate) in combination with blue phosphorescent dye bis[(4, 6-difluorophenyl)-pyridinato-N,C 2 )](picolinato) Ir(III) and red phosphorescent dye bis[1-(phenyl)isoquinoline] iridium (III) acetylanetonate. By introducing a thin layer of 4, 7-diphenyl-1,10-phenanthroline between blue and red emission layers, the diffusion of excitons is confined and white light can be obtained. WOLEDs with the interlayer all have a higher colour rendering index (>82) than the device without it (76). One device has the maximum current efficiency of 17.6 cd A -1 and a maximum luminance of 39 050 cd m -2 . The power efficiency is 8.7 lm W -1 at 100 cd m -2 . Furthermore, the device has good colour stability and the CIE coordinates just change from (0.394, 0.425) to (0.390, 0.426) with the luminance increasing from 630 to 4200 cd m -2 .

  1. Preparation and Characterization of a Molybdenum(VI Schiff Base Complex as Magnetic Nanocatalyst for Synthesis of 2-Amino-4H-benzo[h]chromenes

    Directory of Open Access Journals (Sweden)

    Naghmeh Divsalar

    2016-10-01

    Full Text Available A new recoverable molybdenum nanocatalyst was prepared by immobilization  of a Schiff base ligand on the surface of silica coated magnetite nanoparticles (Fe3O4@SiO2 through condensation reaction between 3-aminopropyl triethoxysilane and 2-hydroxy1-naphthaldehyde and succeeding reaction with dioxomolybdenum(VI acetylacetonate (MoO2(acac2. The synthesized catalyst was characterized by inductively coupled plasma, thermogravimetric analysis, scanning electron microscopy, vibrating sample magnetometry, Energy-dispersive X-ray, Fourier transform infrared and X-raydiffraction spectroscopy. Catalytic performance of the synthesized nanocatalyst was investigated for the preparation of 2-amino-4H-benzo[h]chromenes. The compounds were prepared high yield through one-pot, three-component reaction of 1-naphthol, various of aldehydes and malonitrile in the presence of nanocatalyst, Fe3O4@SiO2@Mo-Schiff base, under solvent-free conditions. The benefits of this protocol are short reaction time, simple work-up procedure, high yields and use of the concept of green chemistry. The magnetic nanocatalyst could be separated easily from the reaction media using an external magnetic field and reused in subsequent catalytic runs without significant deterioration of its activity.

  2. Synthesis and studies on Cu(II), Co(II), Ni(II) complexes of Knoevenagel β-diketone ligands

    Science.gov (United States)

    Sumathi, S.; Tharmaraj, P.; Sheela, C. D.; Anitha, C.

    2012-11-01

    Transition metal complexes of various acetylacetone based ligands of the type ML [where M = Cu(II), Ni(II), Co(II); L = 3-(aryl)-pentane-2,4-dione] have been synthesized. The structural features have been derived from their elemental analysis, magnetic susceptibility, molar conductance, IR, UV-Vis, 1H NMR, Mass and ESR spectral studies. Conductivity measurements reveal that all the complexes are non-electrolytic in nature. Spectroscopic and other analytical data of the complexes suggest octahedral geometry for other metal(II) complexes. The redox behavior of the copper(II) complexes have been studied by cyclic voltammetry. The free ligands and their metal complexes have been screened for their in vitro biological activities against the bacteria Pseudomonas aeruginosa, Escherichia coli and Staphylococcus aureus as well as the fungus Candida albicans by well diffusion method. The zone of inhibition value indicates that the most of the metal(II) complexes are found to possess increased activities compared to those of the free ligands. All synthesized compounds may serve as potential photoactive materials as indicated from their characteristic fluorescence properties. The second harmonic generation (SHG) efficiency of the ligands (L1-L3) was found to be considerable effect than that of urea and KDP (potassium dihydrogen phosphate).

  3. Synthesis and preservation of graphene-supported uranium dioxide nanocrystals

    Energy Technology Data Exchange (ETDEWEB)

    Ma, Hanyu [Department of Civil and Environmental Engineering and Earth Sciences, University of Notre Dame, 156 Fitzpatrick Hall, Notre Dame, IN 46556 (United States); Wang, Haitao [Department of Civil and Environmental Engineering and Earth Sciences, University of Notre Dame, 156 Fitzpatrick Hall, Notre Dame, IN 46556 (United States); Department of Civil, Environmental, and Construction Engineering, Texas Tech University, 911 Boston Ave., Lubbock, TX 79409 (United States); Burns, Peter C. [Department of Civil and Environmental Engineering and Earth Sciences, University of Notre Dame, 156 Fitzpatrick Hall, Notre Dame, IN 46556 (United States); Department of Chemistry and Biochemistry, University of Notre Dame, 251 Nieuwland Science Hall, Notre Dame, IN 46556 (United States); McNamara, Bruce K.; Buck, Edgar C. [Nuclear Chemistry & Engineering Group, Pacific Northwest National Laboratory, 902 Battelle Boulevard, Richland, WA 99352 (United States); Na, Chongzheng, E-mail: chongzheng.na@gmail.com [Department of Civil and Environmental Engineering and Earth Sciences, University of Notre Dame, 156 Fitzpatrick Hall, Notre Dame, IN 46556 (United States); Department of Civil, Environmental, and Construction Engineering, Texas Tech University, 911 Boston Ave., Lubbock, TX 79409 (United States)

    2016-07-15

    Graphene-supported uranium dioxide (UO{sub 2}) nanocrystals are potentially important fuel materials. Here, we investigate the possibility of synthesizing graphene-supported UO{sub 2} nanocrystals in polar ethylene glycol compounds by the polyol reduction of uranyl acetylacetone under boiling reflux, thereby enabling the use of an inexpensive graphene precursor graphene oxide into a one-pot process. We show that triethylene glycol is the most suitable solvent with an appropriate reduction potential for producing nanometer-sized UO{sub 2} crystals compared to monoethylene glycol, diethylene glycol, and polyethylene glycol. Graphene-supported UO{sub 2} nanocrystals synthesized with triethylene glycol show evidence of heteroepitaxy, which can be beneficial for facilitating heat transfer in nuclear fuel particles. Furthermore, we show that graphene-supported UO{sub 2} nanocrystals synthesized by polyol reduction can be readily stored in alcohols, impeding oxidation from the prevalent oxygen in air. Together, these methods provide a facile approach for preparing and storing graphene-supported UO{sub 2} nanocrystals for further investigation and development under ambient conditions. - Highlights: • UO{sub 2} nanocrystals are synthesized using polyol reduction method. • Triethylene glycol is the best reducing agent for nano-sized UO{sub 2} crystals. • UO{sub 2} nanocrystals grow on graphene through heteroepitaxy. • Graphene-supported UO{sub 2} nanocrystals can be stored in alcohols to prevent oxidation.

  4. Combined sol–gel and carbothermal synthesis of ZrC–TiC powders for composites

    Energy Technology Data Exchange (ETDEWEB)

    Umalas, Madis [Institute of Physics, University of Tartu, Riia 142, 51014, Tartu (Estonia); Estonian Nanotechnology Competence Centre, Riia 142, 51014, Tartu (Estonia); Hussainova, Irina, E-mail: irina.hussainova@ttu.ee [Department of Materials Engineering, Tallinn University of Technology, Ehitajate 5, 19086, Tallinn (Estonia); ITMO University, Kronverksky 49, St. Petersburg, 197101 (Russian Federation); Reedo, Valter [Institute of Physics, University of Tartu, Riia 142, 51014, Tartu (Estonia); Young, Der-Liang [Department of Materials Engineering, Tallinn University of Technology, Ehitajate 5, 19086, Tallinn (Estonia); Cura, Erkin; Hannula, Simo-Pekka [Department of Materials Science and Engineering, Aalto University, School of Chemical Technology, POB 16200, Aalto, 00076 (Finland); Lõhmus, Rünno [Institute of Physics, University of Tartu, Riia 142, 51014, Tartu (Estonia); Estonian Nanotechnology Competence Centre, Riia 142, 51014, Tartu (Estonia); Lõhmus, Ants [Institute of Physics, University of Tartu, Riia 142, 51014, Tartu (Estonia)

    2015-03-01

    The TiC–ZrC binary compound of nanostructured powders was synthesised by combination of sol–gel and carbothermal reduction. The polymeric precursor of the blend was produced by sol–gel process from titanium tetrabutoxide, zirconium tetrabutoxide and benzene-1.4-diol; then carbothermally reduced to the TiC–ZrC blend at 1600 °C in an inert environment. The chemical reactions occurring in the system were monitored by infrared spectrometry. Stable alkoxide solution was obtained by adding acetylacetone to avoid premature gelation of the metal alkoxide mixture. A solid solution of ZrTiC{sub 2} was produced by spark plasma sintering at temperature of 2000 °C. - Highlights: • A polymeric precursor of TiC–ZrC blend was synthesised by sol–gel process. • The polymeric precursor synthesis was studied by infrared spectroscopy. • TiC–ZrC powder blend was carbothermally reduced from polymeric precursor. • TiC–ZrC powder blend was sintered to ZrTiC{sub 2} solid solution by spark plasma sintering. • Sintered ZrTiC{sub 2} have good mechanical properties.

  5. Low temperature superparamagnetic nanocomposites obtained by Fe(acac3-SiO2-PVA hybrid xerogel thermolysis

    Directory of Open Access Journals (Sweden)

    Catalin Ianasi

    2016-12-01

    Full Text Available Fe(acac3/silica/PVA hybrid xerogel nanocomposite was obtained by one pot acid catalysed sol-gel synthesis using the homogeneous mixture of iron(III acetylacetonate (Fe(acac3, tetraethylorthosilicate (TEOS, and polyvinyl alcohol (PVA. Nominal composition ratio of iron oxide/silica was 15/85 (weight percent. Nitric acid was used as catalyst. Another sample of Fe(acac3/silica xerogel without PVA addition was prepared in the similar processing conditions. Based on thermal analysis studies, the thermal behaviour of both xerogel samples was unveiled and it allowed choosing the optimal calcination temperatures in order to obtain iron oxide silica magnetic nanocomposite samples. The two xerogel (with and without PVA samples were thermally treated, in air, at 220, 260 and 300 °C and characterized by different techniques. XRD investigations revealed phase composition evolution with calcination temperature, from cubic spinel phase (maghemite to hexagonal stable hematite containing nanocomposite of 10–20 nm average crystallite size. These findings were confirmed by Mössbauer spectroscopy. Up to 300 °C, the surface area and total pores volume increased with temperature for all samples. By calcination at the same temperature, the hybrid xerogel containing PVA resulted in significantly higher magnetization and free volume values in comparison with the sample without PVA.

  6. Blood cells radiolabelling achievements, challanges, and prospects

    International Nuclear Information System (INIS)

    Weininger, Jolie; Trumper, Jacob

    1987-01-01

    A study in performed about the different ways of blood cells radiolabelling. The labelling of red blood cells (RBCs), compared with that of other blood cells, is facilitated by several factors such as a) RBCs are the most abundant of all cellular blood elements, b) they are relatively easy to separate and manipulate in vitro, c) in vitro they are less dependent on energy and nutricional requirements, d) they are easy to label due to the presence of a variety of cellular transport mechanism. 99m Tc was reconized and became as the ideal radioisotope for nuclear medicine imaging. After considerations about RBCs radiolabelling, it is presented a new in vitro technique based on the BNL kit, developed by Srivastava and co-workers. The Sorep optimized one-vial labelling method for 2 ml whole blood. In vivo and in vivo/in vitro labelling are presented too, the last method seems to combine the superior binding efficiency of in vitro labelling with the convenience of in vitro labelling. Lipophilic chelates of 111 In with oxine, acetylacetone, tropolone and mercaptopyridine N-oxide have been used successfully for labelling platelets and leukocytes. A very promising aproach is the labelling of cells with monoclonal antibodies and the developing optimized methods for in vitro labelling with various radionuclides such as 123 I, 125 I, 131 I, 111 I and 99m Tc. The advantages of the antibody technique over conventional cell labelling are shown. (M.E.L.) [es

  7. Electrospun N-doped Hierarchical Porous Carbon Nanofiber with Improved Graphitization Degree for High Performance Lithium Ion Capacitor.

    Science.gov (United States)

    Li, Baohua; Shi, Ruiying; Han, Cuiping; Xu, Xiaofu; Qing, Xianying; Xu, Lei; Li, Hongfei; Li, Junqin; Wong, Ching-Ping

    2018-05-14

    Lithium ion capacitor (LIC) has been regarded as a promising device to combine the merits of lithium ion batteries and supercapacitors, which can meet the requirements for both high energy and power density. The development of advanced electrode is the key. Herein, we demonstrate the bottom-up synthesis of activated carbon nanofiber (a-PANF) with hierarchical porous structure and high graphitization degree. Electrospinning is employed to prepare interconnected fiber network with macropores and ferric acetylacetonate is introduced as both mesopore creating agent and graphitic catalyst to increase the graphitization degree. Furthermore, chemical activation enlarges the specific surface area by producing rich micropores. Half cell evaluation of the as-prepared a-PANF displays a discharge capacity of 80 mAh g-1 at 0.1 A g-1 within 2~4.5 V and no capacity fading after 1000 cycles at 2 A g-1, which is significantly higher than conventional activated carbon. Furthermore, the as-assembled LIC with a-PANF cathode and Fe3O4 anode achieves a superior energy density of 124.6 Wh kg-1 at a specific power of 93.8 W kg-1, and remains 103.7 Wh kg-1 at 4687.5 W kg-1, demonstrating the promising application of a-PANF as potential electrode candidates for efficient energy storage systems. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  8. Vanadia-silica and vanadia-cesium-silica catalysts for oxidation of SO2

    DEFF Research Database (Denmark)

    Pârvulescu, Vasile I.; Paun, Christina; Pârvulescu, Viorica

    2004-01-01

    %. The samples were impregnated with Cs2SO4 resulting in a Cs:V ratio of 3:1 and then dried and calcined under the same conditions. The catalysts were characterized using several methods: sorption isotherms of N-2 at 77 K, XRD, and XPS. The results of the characterization indicated that during calcination...... catalysts were also performed. The activation of the catalysts and the catalytic behavior were monitored by in situ Raman and EPR spectroscopy. These characterization techniques indicated that the active molten phase contains vanadium oxosulfato complexes similar to the V2O5-M2S2O7 (M = alkali metal......Mesoporous vanadia-silica catalysts have been prepared by three different sol-gel procedures using tetraethylorthosilicate (TEOS), vanadyl acetylacetonate (VAA), or VOCl3 and in some cases quaternary ammonium salts ((CH3)(3)C14H29N+Br- or (C10H21)(4)N+Br-) as surfactants. According to procedure A...

  9. Sol-gel based sensor for selective formaldehyde determination

    Energy Technology Data Exchange (ETDEWEB)

    Bunkoed, Opas [Trace Analysis and Biosensor Research Center, Prince of Songkla University, Hat Yai, Songkhla 90112 (Thailand); Department of Chemistry and Center for Innovation in Chemistry, Faculty of Science, Prince of Songkla University, Hat Yai, Songkhla 90112 (Thailand); Davis, Frank [Cranfield Health, Cranfield University, Bedford MK43 0AL (United Kingdom); Kanatharana, Proespichaya, E-mail: proespichaya.K@psu.ac.th [Trace Analysis and Biosensor Research Center, Prince of Songkla University, Hat Yai, Songkhla 90112 (Thailand); Department of Chemistry and Center for Innovation in Chemistry, Faculty of Science, Prince of Songkla University, Hat Yai, Songkhla 90112 (Thailand); Thavarungkul, Panote [Trace Analysis and Biosensor Research Center, Prince of Songkla University, Hat Yai, Songkhla 90112 (Thailand); Department of Physics, Faculty of Science, Prince of Songkla University, Hat Yai, Songkhla 90112 (Thailand); Higson, Seamus P.J., E-mail: s.p.j.higson@cranfield.ac.uk [Cranfield Health, Cranfield University, Bedford MK43 0AL (United Kingdom)

    2010-02-05

    We report the development of transparent sol-gels with entrapped sensitive and selective reagents for the detection of formaldehyde. The sampling method is based on the adsorption of formaldehyde from the air and reaction with {beta}-diketones (for example acetylacetone) in a sol-gel matrix to produce a yellow product, lutidine, which was detected directly. The proposed method does not require preparation of samples prior to analysis and allows both screening by visual detection and quantitative measurement by simple spectrophotometry. The detection limit of 0.03 ppmv formaldehyde is reported which is lower than the maximum exposure concentrations recommended by both the World Health Organisation (WHO) and the Occupational Safety and Health Administration (OSHA). This sampling method was found to give good reproducibility, the relative standard deviation at 0.2 and 1 ppmv being 6.3% and 4.6%, respectively. Other carbonyl compounds i.e. acetaldehyde, benzaldehyde, acetone and butanone do not interfere with this analytical approach. Results are provided for the determination of formaldehyde in indoor air.

  10. Sol-gel based sensor for selective formaldehyde determination

    International Nuclear Information System (INIS)

    Bunkoed, Opas; Davis, Frank; Kanatharana, Proespichaya; Thavarungkul, Panote; Higson, Seamus P.J.

    2010-01-01

    We report the development of transparent sol-gels with entrapped sensitive and selective reagents for the detection of formaldehyde. The sampling method is based on the adsorption of formaldehyde from the air and reaction with β-diketones (for example acetylacetone) in a sol-gel matrix to produce a yellow product, lutidine, which was detected directly. The proposed method does not require preparation of samples prior to analysis and allows both screening by visual detection and quantitative measurement by simple spectrophotometry. The detection limit of 0.03 ppmv formaldehyde is reported which is lower than the maximum exposure concentrations recommended by both the World Health Organisation (WHO) and the Occupational Safety and Health Administration (OSHA). This sampling method was found to give good reproducibility, the relative standard deviation at 0.2 and 1 ppmv being 6.3% and 4.6%, respectively. Other carbonyl compounds i.e. acetaldehyde, benzaldehyde, acetone and butanone do not interfere with this analytical approach. Results are provided for the determination of formaldehyde in indoor air.

  11. Chemical speciation and equilibria of some nucleic acid compounds and their iron(III) complexes

    Science.gov (United States)

    Masoud, Mamdouh S.; Abd El-Kaway, Marwa Y.; Hindawy, Ahmed M.; Soayed, Amina A.

    The pH effect on electronic absorption spectra of some biologically active nucleic acid constituents have been studied at room temperature and the mechanism of ionization was explained. These compounds are of two categories (pyrimidines: [barbital; 5,5'-diethyl-barbituric acid], [SBA; 4,6-dihydroxy-2-mercapto-pyrimidin], [NBA; 5-nitro-2,4,6(1H,3H,5H)-pyrimidine trione] and [TU; 2,3-dihydro-2-thioxo-pyrimidin-4(1H)-one]) and (purines: [adenine; 6-amino purine], its [Schiff bases derived from adenine-acetylacetone; (Z)-4-(7H-purin-6-ylimino)pentan-2-one) and adenine-salicylaldehyde; 2-((7H-purin-6-ylimino) methyl) phenol] and its [Azo derived from adenine-resorcinol; 4-((7H-purin-6-yl)-diazenyl) benzene-1,3-diol]. The phenomena of tautomerization assigned different tautomers. Different spectrophotometric methods are applied to evaluate the pK's values that explained with their molecular structures. The interaction of Fe3+ with some selected pyrimidines (barbital, NBA and SBA) was explained using familiar six spectrophotometric methods. The data typified the existence of different absorbing species with the different stoichiometries 1:1, 1:2, 1:3 and 2:3. The stability constant of the complexes was computed. More approach was deduced to assign the existence of different species applying the distribution diagrams.

  12. Synthesis and characterization of thin films of Pd/TiO{sub 2} with possible applications in photo catalysis; Sintesis y caracterizacion de peliculas delgadas de Pd/TiO{sub 2} con posibles aplicaciones en fotocatalisis

    Energy Technology Data Exchange (ETDEWEB)

    Tirado G, S. [IPN, Escuela Superior de Fisica y Matematicas, U. P. Adolfo Lopez Mateos Edif. 9, San Pedro Zacatenco, 07738 Mexico D. F. (Mexico); Valenzuela Z, M. A., E-mail: tirado@esfm.ipn.mx [IPN, Escuela Superior de Ingenieria Quimica e Industrias Extractivas, Laboratorio de Catalisis y Materiales, U. P. Adolfo Lopez Mateos Edif. 8, San Pedro Zacatenco, 07738 Mexico D. F. (Mexico)

    2015-10-15

    In this paper the synthesis and study of thin films of titanium oxide is reported, as well as those that were surface modified with palladium nanoparticles Pd/TiO{sub 2}. First, the TiO{sub 2} films are grown on substrates of soda-lime glass using chemical sol-gel route and the repeated immersion procedure. The salt precursor titanium oxy-acetylacetonate to 0.2 M, in the solvent 2-methoxyethanol and monoethanolamine was used as stabilizer. The number of used immersions gave an average thickness estimate for these films of 172.8 nm. Second, the series of Pd/TiO{sub 2} films surface modified were obtained from a solution of palladium nitrate dehydrate at low concentration, with the same procedure. The films grown TiO{sub 2} and those surface-modified films were characterized in its structure by X-ray diffraction, morphology by scanning electron microscopy, the topography with atomic force microscopy, optical properties by UV-Vis, among others. Photoluminescence properties and/or possible applications in photo catalysis are reported in this paper. (Author)

  13. H/D exchange in the reaction of D2 with Bis(triphenyl phosphite)(acetylacetonato)rhodium(I), Rh(P(OPh)3)2(acac)

    International Nuclear Information System (INIS)

    Whitmore, B.C.; Eisenberg, R.

    1984-01-01

    The reaction of Rh(P)OPh) 3 ) 2 (acac) (1) with D 2 benzene has been studied by 1 H NMR spectroscopy, and complex 1 has been found to undergo H/D exchange at the ortho positions of the coordinated phosphite ligands and at the central methine position of the acetylacetonate ligand. At 75 0 C, the exchange reaction proceeds with the extent of deuterium incorporation into P(OPh) 3 being the same as that into acac at all stages of the H/D exchange process. At 60 0 C, deuterium incorporation into P(OPh) 3 is initially more rapid than that into the acac ligand. The initial rate of deuterium incorporation into P(OPh) 3 by 1 in benzene-d 6 under D 2 at 60 0 C proceeds with a first-order rate constant of 9.6 x 10 -5 s -1 . A mechanism for this exchange process is proposed. 13 references, 3 figures, 2 tables

  14. Zinc oxide films impurified with Ti and prepared by the Sol-gel method; Peliculas de oxido de zinc impurificadas con Ti y preparadas por el metodo Sol-gel

    Energy Technology Data Exchange (ETDEWEB)

    Tirado G, S. [ESFM-IPN, 07738 Mexico D.F. (Mexico); Cazares R, J.M.; Maldonado, A. [CINVESTAV-IPN, A.P. 14-740, 07000 Mexico D.F. (Mexico)

    2006-07-01

    Titanium-doped zinc oxide thin films have been prepared on silicon substrate using the Sol-Gel technique. The structural, morphology, electrical and optical properties of such thin films were studied as a function of titanium concentration (0.5, 1 and 1.5 %) and the thin films thickness. Zinc acetate dihydrate and titanium (VI)-oxy acetylacetonate were used as precursor materials, using 2-methoxyethanol and monoethanolamine as via. The X-ray diffraction spectra show polycrystalline films in all the cases. It can see for all the thin films a preferential growth along the (002) planes where the titanium concentration and also the thin films thickness play an important rule. No structural changes are observed at all. The surface morphology studied shows as the grain size decreases when thin thickness is increases. For titanium concentration of 0.5, 1 and 1.5 % values the grains size increase also. The thin films thickness for titanium concentration of 1.5 % was 500 nm (4v), 400 nm (3v), 180 nm (2v) and 130 nm (1v), values obtained from cross-section micrographs. Highly resistive samples are obtained for substrate soda-lime even showing high transmittance. Better physical properties are required for gas sensors or semitransparent electrodes and other possible applications. (Author)

  15. Okadaic Acid, a Bioactive Fatty Acid from Halichondria okadai, Stimulates Lipolysis in Rat Adipocytes: The Pivotal Role of Perilipin Translocation

    Directory of Open Access Journals (Sweden)

    Nen-Chung Chang

    2013-01-01

    Full Text Available Lipid metabolism in visceral fat cells is correlated with metabolic syndrome and cardiovascular diseases. Okadaic-acid, a 38-carbon fatty acid isolated from the black sponge Halichondria okadai, can stimulate lipolysis by promoting the phosphorylation of several proteins in adipocytes. However, the mechanism of okadaic acid-induced lipolysis and the effects of okadaic acid on lipid-droplet-associated proteins (perilipins and beta-actin remain unclear. We isolated adipocytes from rat epididymal fat pads and treated them with isoproterenol and/or okadaic acid to estimate lipolysis by measuring glycerol release. Incubating adipocytes with okadaic acid stimulated time-dependent lipolysis. Lipid-droplet-associated perilipins and beta-actin were analyzed by immunoblotting and immunofluorescence, and the association of perilipin A and B was found to be decreased in response to isoproterenol or okadaic acid treatment. Moreover, okadaic-acid treatment could enhance isoproterenol-mediated lipolysis, whereas treatment of several inhibitors such as KT-5720 (PKA inhibitor, calphostin C (PKC inhibitor, or KT-5823 (PKG inhibitor did not attenuate okadaic-acid-induced lipolysis. By contrast, vanadyl acetylacetonate (tyrosine phosphatase inhibitor blocked okadaic-acid-dependent lipolysis. These results suggest that okadaic acid induces the phosphorylation and detachment of lipid-droplet-associated perilipin A and B from the lipid droplet surface and thereby leads to accelerated lipolysis.

  16. Preparation of epitaxial YBa2Cu3O7-y films on CeO2-buffered yttria-stabilized zirconia substrates by fluorine-free metalorganic deposition

    International Nuclear Information System (INIS)

    Tsukada, Kenichi; Yamaguchi, Iwao; Sohma, Mitsugu; Kondo, Wakichi; Kamiya, Kunio; Kumagai, Toshiya; Manabe, Takaaki

    2007-01-01

    Epitaxial YBa 2 Cu 3 O 7-y (YBCO) films of 120-550 nm thickness have been prepared by fluorine-free metalorganic deposition using a metal acetylacetonate-based coating solution on yttria-stabilized zirconia (YSZ) substrates with an evaporated CeO 2 buffer layer. The YBCO films were highly (0 0 1)-oriented by X-ray diffraction θ-2θ scanning and φ scanning. The YBCO films 120-400 nm in thickness demonstrated high critical current densities (J c ) with an average in excess of 3 MA/cm 2 at 77 K using an inductive method. In particular, a 210-nm-thick film showed a J c of 4.5 MA/cm 2 . These excellent properties are attributed to the high crystallinity, small in-plane fluctuation due to high epitaxy and to the microstructure free from grain boundaries in the YBCO films. Further increase of film thickness increased the fraction of irregularities, i.e., precipitates and micropores, in the film surfaces, resulting in lower J c values

  17. Hybrid white organic light-emitting devices consisting of a non-doped thermally activated delayed fluorescent emitter and an ultrathin phosphorescent emitter

    International Nuclear Information System (INIS)

    Zhao, Juan; Wang, Zijun; Wang, Run; Chi, Zhenguo; Yu, Junsheng

    2017-01-01

    Hybrid white organic light-emitting devices (OLEDs) are fabricated by employing non-doped emitting layers (EMLs), which are consisted of a blue thermally activated delayed fluorescent (TADF) emitter 9,9-dimethyl-9,10-dihydroacridine-diphenylsulfone (DMAC-DPS) and an ultrathin yellow iridium complex bis[2-(4-tertbutylphenyl)benzothiazolato-N,C 2′ ] iridium (acetylacetonate) [(tbt) 2 Ir(acac)]. With thickness optimization of DMAC-DPS, a white OLED achieves maximum current efficiency, power efficiency and external quantum efficiency of 34.9 cd/A, 29.2 lm/W and 11.4%, respectively, as well as warm white emission with relatively stable electroluminescence spectra. The results suggest that, bipolar charge carrier transport property and concentration independent property of DMAC-DPS, charge carrier trapping effect of the ultrathin (tbt) 2 Ir(acac), and balanced self-emission process and energy transfer process between DMAC-DPS and (tbt) 2 Ir(acac), contribute to high device performance.

  18. Hybrid white organic light-emitting devices consisting of a non-doped thermally activated delayed fluorescent emitter and an ultrathin phosphorescent emitter

    Energy Technology Data Exchange (ETDEWEB)

    Zhao, Juan [State Key Laboratory of Electronic Thin Film and Integrated Devices, School of Optoelectronic Information, University of Electronic Science and Technology of China, Chengdu 610054 (China); School of Chemistry, Sun Yat-sen University, Guangzhou 510275 (China); Wang, Zijun; Wang, Run [State Key Laboratory of Electronic Thin Film and Integrated Devices, School of Optoelectronic Information, University of Electronic Science and Technology of China, Chengdu 610054 (China); Chi, Zhenguo, E-mail: chizhg@mail.sysu.edu.cn [School of Chemistry, Sun Yat-sen University, Guangzhou 510275 (China); Yu, Junsheng, E-mail: jsyu@uestc.edu.cn [State Key Laboratory of Electronic Thin Film and Integrated Devices, School of Optoelectronic Information, University of Electronic Science and Technology of China, Chengdu 610054 (China)

    2017-04-15

    Hybrid white organic light-emitting devices (OLEDs) are fabricated by employing non-doped emitting layers (EMLs), which are consisted of a blue thermally activated delayed fluorescent (TADF) emitter 9,9-dimethyl-9,10-dihydroacridine-diphenylsulfone (DMAC-DPS) and an ultrathin yellow iridium complex bis[2-(4-tertbutylphenyl)benzothiazolato-N,C{sup 2′}] iridium (acetylacetonate) [(tbt){sub 2}Ir(acac)]. With thickness optimization of DMAC-DPS, a white OLED achieves maximum current efficiency, power efficiency and external quantum efficiency of 34.9 cd/A, 29.2 lm/W and 11.4%, respectively, as well as warm white emission with relatively stable electroluminescence spectra. The results suggest that, bipolar charge carrier transport property and concentration independent property of DMAC-DPS, charge carrier trapping effect of the ultrathin (tbt){sub 2}Ir(acac), and balanced self-emission process and energy transfer process between DMAC-DPS and (tbt){sub 2}Ir(acac), contribute to high device performance.

  19. Composition and hydrophilicity control of Mn-doped ferrite (MnxFe3-xO4) nanoparticles induced by polyol differentiation.

    Science.gov (United States)

    Vamvakidis, Kosmas; Katsikini, Maria; Vourlias, George; Angelakeris, Mavroeidis; Paloura, Eleni C; Dendrinou-Samara, Catherine

    2015-03-28

    Manganese doped ferrite (MnxFe3-xO4) nanoparticles with x = 0.29-0.77 were prepared under solvothermal conditions in the presence solely of a polyol using the trivalent manganese and iron acetylacetonates as precursors. In this facile approach, a variety of polyols such as polyethylene glycol (PEG 8000), tetraethylene glycol (TEG), propylene glycol (PG) and a mixture of TEG and PG (1 : 1) were utilized in a triple role as a solvent, a reducing agent and a surface-functionalizing agent. The composition of the fine cubic-spinel structures was found to be related to the reductive ability of each polyol, while determination of structural characteristics plus the inversion parameter (i = 0.18-0.38) were provided by X-ray absorption near edge structure (XANES) and extended X-ray absorption fine structure (EXAFS) spectroscopy at both the Fe and Mn K-edges. The saturation magnetization increased up to 80 emu g(-1) when x = 0.35 and i = 0.22. In addition, the as-prepared nanocrystals coated with PEG, PG and PG&TEG showed excellent colloidal stability in water, while the TEG-coated particles were not water dispersible and converted to hydrophilic when were extra PEGylated. Measurements of the (1)H NMR relaxation in water were carried out and the nanoprobes were evaluated as potential contrast agents.

  20. APCVD Transition Metal Oxides – Functional Layers in ''Smart windows''

    International Nuclear Information System (INIS)

    Gesheva, K A; Ivanova, T M; Bodurov, G K

    2014-01-01

    Transition metal oxides (TMO) exhibit electrochromic effect. Under a small voltage they change their optical transmittance from transparent to collored (absorbing) state. The individual material can manifest its electrochromic properties only when it is part of electrochromic (EC) multilayer system. Smart window is controlling the energy of solar flux entering the building or car and makes the interiors comfortable and energy utilization more effective. Recently the efforts of material researchers in this field are directed to price decreasing. APCVD technology is considered as promissing as this process permits flowthrough large-scale production process. The paper presents results on device optimization based on WO 3 -MoO 3 working electrode. Extensive research reveals that WO 3 -MoO 3 structure combines positive features of single oxides: excellent electrochromic performance of WO 3 and better kinetic properties of MoO 3 deposition. The achieved color efficiency of APCVD WO 3 -MoO 3 films is 200cm 2 /C and optical modulation of 65-70% are practically favorable electrochromic characteristics. To respond to low cost requirement, the expensive hexacarbonyl can be replaced with acetylacetonate. We have started with this precursor to fabricate mixed W x V 1-x O 3 films. The films possess excellent surface coverage and high growth-rate. CVD deposition of VO 2 , a promissing thermochromic thin film material is also presented

  1. Suspension chemistry and electrophoretic deposition of zirconia electrolyte on conducting and non-conducting substrates

    International Nuclear Information System (INIS)

    Das, Debasish; Basu, Rajendra N.

    2013-01-01

    Graphical abstract: - Highlights: • Stable suspension of yttria stabilized zirconia (YSZ) obtained in isopropanol medium. • Suspension chemistry and process parameters for electrophoretic deposition optimized. • Deposited film quality changed with iodine and water (dispersants) concentration. • Dense YSZ film (∼5 μm) fabricated onto non-conducting porous NiO-YSZ anode substrate. - Abstract: Suspensions of 8 mol% yttria stabilized zirconia (YSZ) particulates in isopropanol medium are prepared using acetylacetone, iodine and water as dispersants. The effect of dispersants concentration on suspension stability, particle size distribution, electrical conductivity and pH of the suspensions are studied in detail to optimize the suspension chemistry. Electrophoretic deposition (EPD) has been conducted to produce thin and dense YSZ electrolyte films. Deposition kinetics have been studied in depth and good quality films on conducting substrate are obtained at an applied voltage of 15 V for 3 min. YSZ films are also fabricated on non-conducting NiO-YSZ anode substrate using a steel plate on the reverse side of the substrate. Upon co-firing at 1400 °C for 6 h a dense YSZ film of thickness ∼5 μm is obtained. Such a half cell (anode + electrolyte) can be used to fabricate a solid oxide fuel cell on applying a suitable cathode layer

  2. ZnO THIN FILMS PREPARED BY SPRAY-PYROLYSIS TECHNIQUE FROM ORGANO-METALLIC PRECURSOR

    Directory of Open Access Journals (Sweden)

    Martin Mikulics

    2012-07-01

    Full Text Available Presented experiments utilize methanolic solution of zinc acetyl-acetonate as a precursor and sapphire (001 as a substrate for deposition of thin films of ZnO. The X-ray diffraction analysis revealed polycrystalline character of prepared films with preferential growth orientation along c-axis. The roughness of prepared films was assessed by AFM microscopy and represented by roughness root mean square (RMS value in range of 1.8 - 433 nm. The surface morphology was mapped by scanning electron microscopy showing periodical structure with several local defects. The optical transmittance spectrum of ZnO films was measured in wavelength range of 200-1000 nm. Prepared films are transparent in visible range with sharp ultra-violet cut-off at approximately 370 nm. Raman spectroscopy confirmed wurtzite structure and the presence of compressive stress within its structure as well as the occurrence of oxygen vacancies. The four-point Van der Pauw method was used to study the transport prosperities. The resistivity of presented ZnO films was found 8 × 10–2 Ω cm with carrier density of 1.3 × 1018 cm–3 and electron mobility of 40 cm2 V–1 s–1.

  3. A novel thermal decomposition approach for the synthesis of silica-iron oxide core–shell nanoparticles

    International Nuclear Information System (INIS)

    Kishore, P.N.R.; Jeevanandam, P.

    2012-01-01

    Highlights: ► Silica-iron oxide core–shell nanoparticles have been synthesized by a novel thermal decomposition approach. ► The silica-iron oxide core–shell nanoparticles are superparamagnetic at room temperature. ► The silica-iron oxide core–shell nanoparticles serve as good photocatalyst for the degradation of Rhodamine B. - Abstract: A simple thermal decomposition approach for the synthesis of magnetic nanoparticles consisting of silica as core and iron oxide nanoparticles as shell has been reported. The iron oxide nanoparticles were deposited on the silica spheres (mean diameter = 244 ± 13 nm) by the thermal decomposition of iron (III) acetylacetonate, in diphenyl ether, in the presence of SiO 2 . The core–shell nanoparticles were characterized by X-ray diffraction, infrared spectroscopy, field emission-scanning electron microscopy coupled with energy dispersive X-ray analysis, transmission electron microscopy, diffuse reflectance spectroscopy, and magnetic measurements. The results confirm the presence of iron oxide nanoparticles on the silica core. The core–shell nanoparticles are superparamagnetic at room temperature indicating the presence of iron oxide nanoparticles on silica. The core–shell nanoparticles have been demonstrated as good photocatalyst for the degradation of Rhodamine B.

  4. Synthesis and characterization of TiC nanopowders via sol-gel and subsequent carbothermal reduction process

    Science.gov (United States)

    Chen, Xu; Fan, Jinglian; Lu, Qiong

    2018-06-01

    TiC nanocrystalline powders were synthesized by in-situ carbothermic reduction of Ti-O-C precursor under vacuum atmosphere. And the Ti-O-C precursor was formed by sol-gel method from titanium butyrate (TBOT) and sucrose. To obtain stable sol, TBOT was directly added into mixed solution which contains water, sucrose, acetic acid (AcOH) and acetylacetone (ACAC). This procedure is more convenient and economical because it avoids the use of alcohol which is used as solvent in most reports of alkoxide hydrolysis sol-gel method. TG-DSC, XRD, FTIR and SEM/TEM were employed to analyze and characterize the product during the entire process. The phase composition and crystalline structure parameters of powders with different C/Ti molar ratio were investigated by Rietveld refinement method, and elemental quantitative analysis of the samples were performed. Furthermore, the optimal parameters of carbothermal reduction were obtained and the grain growth mechanism was demonstrated. The results show that TiC nanocrystalline powders (C/Ti molar ratio is 3.5 in the precursor) were synthesized at 1300 °C for 2 h, which have near standard lattice parameter, well crystallinity and fine average grain size ( 37.4 nm).

  5. Preparation of a novel fluorescence probe of terbium-europium co-luminescence composite nanoparticles and its application in the determination of proteins

    Energy Technology Data Exchange (ETDEWEB)

    Gao Feng [College of Chemistry and Materials Science, Anhui Key Laboratory of Chemo/Biosensing, Anhui Normal University, Wuhu 241000 (China)], E-mail: summit8848cn@hotmail.com; Luo Fabao; Tang Lijuan; Dai Lu [College of Chemistry and Materials Science, Anhui Key Laboratory of Chemo/Biosensing, Anhui Normal University, Wuhu 241000 (China); Wang Lun [College of Chemistry and Materials Science, Anhui Key Laboratory of Chemo/Biosensing, Anhui Normal University, Wuhu 241000 (China)], E-mail: wanglun@mail.ahnu.edu.cn

    2008-03-15

    Terbium-europium Tb-Eu/acetylacetone(acac)/poly(acrylamide) (PAM) co-luminescence composite nanoparticles were successfully prepared using the ultrasonic approach. The as-prepared composite nanoparticles show the characteristic emission spectra of Tb{sup 3+}, located at 496 and 549 nm. Furthermore, the nanoparticles are water soluble, stable and have extremely narrow emission bands and high internal fluorescence quantum yield due to the co-luminescence effect. Further studies indicate that proteins can interact with the nanoparticles and induce the fluorescence quenching of the nanoparticles. Based on the fluorescence quenching of nanopaticles in the presence of proteins, a novel method for the sensitive determination of trace amounts of proteins was proposed. Under the optimal experimental conditions, the linear ranges of calibration curves are 0-3.5 {mu}g mL{sup -1} for human serum albumin (HSA) and 0-4.0 {mu}g mL{sup -1} for {gamma}-globulin ({gamma}-IgG), respectively. The limits of detection are 7.1 for HSA and 6.7ng mL{sup -1} for {gamma}-IgG, respectively. The method was applied to the quantification of proteins in synthetic samples and actual human serum samples with satisfactory results. This proposed method is sensitive, simple and has potential application in the clinical assay of proteins.

  6. Enhancement of visible-light photoactivity by polypropylene coated plasmonic Au/TiO2 for dye degradation in water solution

    Science.gov (United States)

    D'Amato, C. A.; Giovannetti, R.; Zannotti, M.; Rommozzi, E.; Ferraro, S.; Seghetti, C.; Minicucci, M.; Gunnella, R.; Di Cicco, A.

    2018-05-01

    A new approach to obtain a heterogeneous photocatalytic material with gold nanoparticles and TiO2 semiconductor was performed exploiting the reducing ability of acetylacetone, a chemical present in the TiO2 paste formulation. Gold/TiO2 heterogeneous catalyst supported on polypropylene [PP@Au-TiO2]A was prepared; composition, structure and morphology of this new material were defined by using UV-Vis spectroscopy, Scanning Electron Microscopy (SEM), Atomic Force Microscopy (AFM), X-ray diffraction (XRD), X-ray Fluorescence (XRF), Raman Spectroscopy, Photoluminescence and Diffuse Reflectance Spectroscopy. The new material was tested in the photocatalytic degradation of Alizarin Red S in water solution, as target pollutant, under visible light and correlated with structural and spectroscopic characterizations. [PP@Au-TiO2]A showed higher photocatalytic activity respect to pure [PP@TiO2]A with an improvement of photodegradation kinetic. The best performance was obtained using [PP@Au-TiO2]A sample with 0.006 wt.% of Au and the photocatalytic improvement was correlated with the band gap energy decrease of photocatalyst.

  7. Combined sol–gel and carbothermal synthesis of ZrC–TiC powders for composites

    International Nuclear Information System (INIS)

    Umalas, Madis; Hussainova, Irina; Reedo, Valter; Young, Der-Liang; Cura, Erkin; Hannula, Simo-Pekka; Lõhmus, Rünno; Lõhmus, Ants

    2015-01-01

    The TiC–ZrC binary compound of nanostructured powders was synthesised by combination of sol–gel and carbothermal reduction. The polymeric precursor of the blend was produced by sol–gel process from titanium tetrabutoxide, zirconium tetrabutoxide and benzene-1.4-diol; then carbothermally reduced to the TiC–ZrC blend at 1600 °C in an inert environment. The chemical reactions occurring in the system were monitored by infrared spectrometry. Stable alkoxide solution was obtained by adding acetylacetone to avoid premature gelation of the metal alkoxide mixture. A solid solution of ZrTiC 2 was produced by spark plasma sintering at temperature of 2000 °C. - Highlights: • A polymeric precursor of TiC–ZrC blend was synthesised by sol–gel process. • The polymeric precursor synthesis was studied by infrared spectroscopy. • TiC–ZrC powder blend was carbothermally reduced from polymeric precursor. • TiC–ZrC powder blend was sintered to ZrTiC 2 solid solution by spark plasma sintering. • Sintered ZrTiC 2 have good mechanical properties

  8. Atomic layer deposition of cobalt carbide films and their magnetic properties using propanol as a reducing agent

    Energy Technology Data Exchange (ETDEWEB)

    Sarr, Mouhamadou, E-mail: sarrtapha44@yahoo.fr [Luxembourg Instituteof Science and Technology, 41, rue du Brill, L-4422 Belvaux (Luxembourg); Bahlawane, Naoufal; Arl, Didier [Luxembourg Instituteof Science and Technology, 41, rue du Brill, L-4422 Belvaux (Luxembourg); Dossot, Manuel [Laboratory of Physical Chemistry and Microbiology for the Environment, UMR 7564 CNRS-Université de Lorraine, 405 rue de Vandoeuvre, 54601 Villers-lès-Nancy (France); McRae, Edward [Institut Jean Lamour, UMR 7198CNRS-Université de Lorraine, FST, BP 70239, 54506 Vandoeuvre-lès-Nancy (France); Lenoble, Damien, E-mail: damien.lenoble@list.lu [Luxembourg Instituteof Science and Technology, 41, rue du Brill, L-4422 Belvaux (Luxembourg)

    2016-08-30

    Highlights: • Conformal carbon-Co-carbide thin films. • Chemically growth carbone-Co-carbide composite. • Tuneable magnetic properties. - Abstract: The investigation of highly conformal thin films using Atomic Layer Deposition (ALD) is driven by a variety of applications in modern technologies. In particular, the emergence of 3D memory device architectures requires conformal materials with tuneable magnetic properties. Here, nanocomposites of carbon, cobalt and cobalt carbide are deposited by ALD using cobalt acetylacetonate with propanol as a reducing agent. Films were grown by varying the ALD deposition parameters including deposition temperature and propanol exposure time. The morphology, the chemical composition and the crystalline structure of the cobalt carbide film were investigated. Vibrating Sample Magnetometer (VSM) measurements revealed magnetic hysteresis loops with a coercivity reaching 500 Oe and a maximal saturation magnetization of 0.9 T with a grain size less than 15 nm. Magnetic properties are shown to be tuneable by adjusting the deposition parameters that significantly affect the microstructure and the composition of the deposited films.

  9. Photoisomerization Mechanism of Ruthenium Sulfoxide Complexes: Role of the Metal-Centered Excited State in the Bond Rupture and Bond Construction Processes.

    Science.gov (United States)

    Li, Huifang; Zhang, Lisheng; Zheng, Lvyin; Li, Xun; Fan, Xiaolin; Zhao, Yi

    2016-09-26

    Phototriggered intramolecular isomerization in a series of ruthenium sulfoxide complexes, [Ru(L)(tpy)(DMSO)](n+) (where tpy=2,2':6',2''-terpyridine; DMSO=dimethyl sulfoxide; L=2,2'-bipyridine (bpy), n=2; N,N,N',N'-tetramethylethylenediamine (tmen) n=2; picolinate (pic), n=1; acetylacetonate (acac), n=1; oxalate (ox), n=0; malonate (mal), n=0), was investigated theoretically. It is observed that the metal-centered ligand field ((3) MC) state plays an important role in the excited state S→O isomerization of the coordinated DMSO ligand. If the population of (3) MCS state is thermally accessible and no (3) MCO can be populated from this state, photoisomerization will be turned off because the (3) MCS excited state is expected to lead to fast radiationless decay back to the original (1) GSS ground state or photodecomposition along the Ru(2+) -S stretching coordinate. On the contrary, if the population of (3) MCS (or (3) MCO ) state is inaccessible, photoinduced S→O isomerization can proceed adiabatically on the potential energy surface of the metal-to-ligand charge transfer excited states ((3) MLCTS →(3) MLCTO ). It is hoped that these results can provide valuable information for the excited state isomerization in photochromic d(6) transition-metal complexes, which is both experimentally and intellectually challenging as a field of study. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  10. Application of exciplex in the fabrication of white organic light emitting devices with mixed fluorescent and phosphorescent layers

    Energy Technology Data Exchange (ETDEWEB)

    Yang, Dan; Duan, Yahui; Yang, Yongqiang [State Key Laboratory on Integrated Optoelectronics, College of Electronic Science & Engineering, Jilin University, Changchun 130012 (China); Hu, Nan [State Key Laboratory on Integrated Optoelectronics, College of Electronic Science & Engineering, Jilin University, Changchun 130012 (China); Changchun University of Science and Technology, Changchun 130012 (China); Wang, Xiao [State Key Laboratory on Integrated Optoelectronics, College of Electronic Science & Engineering, Jilin University, Changchun 130012 (China); Sun, Fengbo [State Key Laboratory on Integrated Optoelectronics, College of Electronic Science & Engineering, Jilin University, Changchun 130012 (China); Changchun University of Science and Technology, Changchun 130012 (China); Duan, Yu, E-mail: duanyu@jlu.edu.cn [State Key Laboratory on Integrated Optoelectronics, College of Electronic Science & Engineering, Jilin University, Changchun 130012 (China)

    2015-10-15

    In this study, a highly efficient fluorescent/phosphorescent white organic light-emitting device (WOLED) was fabricated using exciplex light emission. The hole-transport material 4,4',4''-tris(N-carbazolyl)triphenylamine (TCTA), and electron-transport material, 4,7-diphenyl-1,10-phenanthroline (Bphen), were mixed to afford a blue-emitting exciplex. The WOLED was fabricated with a yellow phosphorescent dye, Ir(III) bis(4-phenylthieno [3,2-c] pyridinato-N,C{sup 2'}) acetylacetonate (PO-01), combined with the exciplex. In this structure, the energy can be efficiently transferred from the blend layer to the yellow phosphorescent dye, thus improving the efficiency of the utilization of the triplet exciton. The maximum power efficiency of the WOLED reached a value 9.03 lm/W with an external quantum efficiency of 4.3%. The Commission Internationale de I'Eclairage (CIE) color coordinates (x,y) of the device were from (0.39, 0.45) to (0.27, 0.31), with a voltage range of 4–9 V. - Highlights: • An exciplex/phosphorescence hybrid white OLED was fabricated for the first time with blue/orange complementary emitters. • By using exciplex as the blue emitter, non-radiative triplet-states on the exciplex can be harvested for light-emission by transferring them to low triplet-state phosphors.

  11. Preparation and photoluminescence enhancement in terbium(III ternary complexes with β-diketone and monodentate auxiliary ligands

    Directory of Open Access Journals (Sweden)

    Devender Singh

    2016-12-01

    Full Text Available A series of new solid ternary complexes of terbium(III ion based on β-diketone ligand acetylacetone (acac and monodentate auxiliary ligands (aqua/urea/triphenylphosphineoxide/pyridine-N-oxide had been prepared. The structural characterizations of synthesized ternary compounds were studied by means of elemental analysis, infrared (IR, and proton nuclear magnetic resonance (NMR spectral techniques. The optical characteristics were investigated with absorption as well as photoluminescence spectroscopy. Thermal behavior of compounds was examined by TGA/DTA analysis and all metal complexes were found to have good thermal stability. The luminescence decay time of complexes were also calculated by monitoring at emission wavelength corresponding to 5D4 → 7F5 transition. A comparative inspection of the luminescent behavior of prepared ternary compounds was performed in order to determine the function of auxiliary ligands in the enhancement of luminescence intensity produced by central terbium(III ion. The color coordinates values suggested that compounds showed bright green emission in visible region in electromagnetic spectrum. Complexes producing green light could play a significant role in the fabrication of efficient light conversion molecular devices for display purposes and lightning systems.

  12. Effects of the addition of H{sub 2}O and NH{sub 4}OH in the optical and structural properties of the thin films of Y{sub 2}O{sub 3} deposited by pyrolytic spray; Efectos de la adicion de H{sub 2}O y NH{sub 4}OH en las propiedades opticas y estructurales de las peliculas delgadas de Y{sub 2}O{sub 3} depositadas por rocio pirolitico

    Energy Technology Data Exchange (ETDEWEB)

    Alarcon F, G.; Carvajal V, R.; Aguilar F, M. [CICATA-IPN, Legaria 694, Col. Irrigacion, 11500 Mexico D.F. (Mexico); Falcony, C. [CINVESTAV, A.P. 14-740, 07000 Mexico D.F. (Mexico)] [and others

    2005-07-01

    In this work we studied the optical and structural properties of yttrium oxide thin films deposited by spray pyrolysis. Yttrium acetylacetonate was used as raw material and N, N-DMF was used as solvent. The films were deposited on Si (100) and Si (111) substrates at temperatures of 400, 450, 500 and 550 C. The optical and structural characteristics of the films were dramatically improved when a mist of H{sub 2}O and/or NH{sub 4}0H was simultaneously added during deposition of the films. A refraction index up to 1.88, and deposition rates lower than 10 A/sec were obtained in the films. Infrared spectroscopy measurements indicate that the films resulted free from -OH bonds. X-ray diffraction patterns reveal that the films were polycrystalline. In addition, the relative chemical composition of the films was determined by Energy Dispersive Spectroscopy and the surface morphology was analyzed in the Atomic Force Microscope. (Author)

  13. Highly efficient and heavily-doped organic light-emitting devices based on an orange phosphorescent iridium complex

    International Nuclear Information System (INIS)

    Zhou, Shunliang; Wang, Qi; Li, Ming; Lu, Zhiyun; Yu, Junsheng

    2014-01-01

    Heavily doped and highly efficient phosphorescent organic light-emitting devices (PhOLEDs) had been fabricated by utilizing an orange iridium complex, bis[2-(3′,5′-di-tert-butylbiphenyl-4-yl)benzothiazolato-N,C 2' ]iridium(III) (acetylacetonate) [(tbpbt) 2 Ir(acac)], as a phosphor. When the doping concentration of [(tbpbt) 2 Ir(acac)] reached as high as 15 wt%, the PhOLEDs exhibited a power efficiency, current efficiency, and external quantum efficiency of 24.5 lm/W, 32.1 cd/A, 15.7%, respectively, implying a promising quenching-resistant characteristics of this novel phosphor. Furthermore, the efficient white PhOLEDs had been obtained by employing (tbpbt) 2 Ir(acac) as a self-host orange emitter, indicating that (tbpbt) 2 Ir(acac) could serve as a promising phosphor to fabricate white organic light-emitting devices with simplified manufacturing process. - Highlights: • Efficient phosphorescent devices were fabricated. • Optimized phosphor doping ratio reached as high as 15 wt%. • The results proved a promising quench-resistant property of the phosphor. • Efficient white devices based on this phosphor as self-host layer had been realized

  14. New cyclometalated Iridium(III) beta-dicetone complex as phosphorescent dopant in Organic light emitting devices

    Science.gov (United States)

    Ivanov, P.; Petrova, P.; Stanimirov, S.; Tomova, R.

    2017-01-01

    A new Bis[4-(benzothiazolato-N,C2‧-2-yl)-N,N-dimethylaniline]Iridium(III) acetylacetonate (Me2N-bt) 2Ir(acac) was synthesized and identified by 1H NMR and elemental analysis. The application of the new compound as a dopant in the hole transporting layer (HTL) of Organic light emitting diode (OLED) structure: HTL/EL/ETL, where HTL was N,N’-bis(3-methylphenyl)-N,N’-diphenylbenzidine (TPD), incorporated in Poly(N-vinylcarbazole) (PVK) matrix, EL - electroluminescent layer of Bis(8-hydroxy-2-methylquinoline)-(4-phenylpheno-xy)aluminum (BAlq) and ETL - electron-transporting layer of Tris-(8-hydroxyquinoline) aluminum (Alq3) or Bis[2-(2-benzothiazoly) phenolato]zinc (Zn(btz)2). We established that the electroluminescent spectra of OLEDs at different concentrations of the dopant were basically the sum of the greenish-blue emission of BAlq and yellowish-green emission of Ir complex. It was found that with increasing of the dopant concentration the relative electroluminescent intensity of Iridium complex emission increased and this of BAlq decreased and as a result the fine tuning of OLED color was observed.

  15. Growth and electrical properties of AlOx grown by mist chemical vapor deposition

    Directory of Open Access Journals (Sweden)

    Toshiyuki Kawaharamura

    2013-03-01

    Full Text Available Aluminum oxide (AlOx thin films were grown using aluminum acetylacetonate (Al(acac3 as a source solute by mist chemical vapor deposition (mist CVD. The AlOx thin films grown at temperatures above 400°C exhibited a breakdown field (EBD over 6 MV/cm and a dielectric constant (κ over 6. It is suggested that residual OH bonding in the AlOx thin films grown at temperatures below 375°C caused degradation of the breakdown field (EBD. With FC type mist CVD, the reaction proceeded efficiently (Ea = 22–24 kJ/mol because the solvent, especially H2O, worked as a stronger oxygen source. The AlOx film could be grown at 450°C with a high deposition rate (23 nm/min and smooth surface (RMS = 1.5 nm. Moreover, the AlOx thin films grown by mist CVD had excellent practicality as insulators because the gate leakage current (IG of the oxide thin film transistor (TFT with an IGZO/AlOx stack was suppressed below 1 pA at a gate voltage (VG of 20 V.

  16. Sequential spectrofluorimetric determination of free and total glycerol in biodiesel in a multicommuted flow system

    Energy Technology Data Exchange (ETDEWEB)

    Silva, Sidnei G. [Universidade de Sao Paulo, Instituto de Quimica, Sao Paulo (Brazil); Morales-Rubio, Angel; Guardia, Miguel de la [Universidad de Valencia, Department of Analytical Chemistry, Burjassot, Valencia (Spain); Rocha, Fabio R.P. [Universidade de Sao Paulo, Centro de Energia Nuclear na Agricultura, Piracicaba (Brazil)

    2011-07-15

    A new procedure for spectrofluorimetric determination of free and total glycerol in biodiesel samples is presented. It is based on the oxidation of glycerol by periodate, forming formaldehyde, which reacts with acetylacetone, producing the luminescent 3,5-diacetyl-1,4-dihydrolutidine. A flow system with solenoid micro-pumps is proposed for solution handling. Free glycerol was extracted off-line from biodiesel samples with water, and total glycerol was converted to free glycerol by saponification with sodium ethylate under sonication. For free glycerol, a linear response was observed from 5 to 70 mg L{sup -1} with a detection limit of 0.5 mg L{sup -1}, which corresponds to 2 mg kg{sup -1} in biodiesel. The coefficient of variation was 0.9% (20 mg L{sup -1}, n = 10). For total glycerol, samples were diluted on-line, and the linear response range was 25 to 300 mg L{sup -1}. The detection limit was 1.4 mg L{sup -1} (2.8 mg kg{sup -1} in biodiesel) with a coefficient of variation of 1.4% (200 mg L{sup -1}, n = 10). The sampling rate was ca. 35 samples h{sup -1} and the procedure was applied to determination of free and total glycerol in biodiesel samples from soybean, cottonseed, and castor beans. (orig.)

  17. Flexible all-fiber electrospun supercapacitor

    Science.gov (United States)

    Liu, Xinhua; Naylor Marlow, Max; Cooper, Samuel J.; Song, Bowen; Chen, Xiaolong; Brandon, Nigel P.; Wu, Billy

    2018-04-01

    We present an all-fiber flexible supercapacitor with composite nanofiber electrodes made via electrospinning and an electrospun separator. With the addition of manganese acetylacetonate (MnACAC) to polyacrylonitrile (PAN) as a precursor for the electrospinning process and subsequent heat treatment, the performance of pure PAN supercapacitors was improved from 90 F g-1 to 200 F g-1 (2.5 mV s-1) with possible mass loadings of MnACAC demonstrated as high as 40 wt%. X-ray diffraction measurements showed that after thermal treatment, the MnACAC was converted to MnO, meanwile, the thermal decomposition of MnACAC increased the graphitic degree of the carbonised PAN. Scanning electron microscopy and image processing showed that static electrospinning of pure PAN and PAN-Mn resulted in fiber diameters of 460 nm and 480 nm respectively after carbonisation. Further analysis showed that the fiber orientation exhibited a slight bias which was amplified with the addition of MnACAC. Use of focused ion beam scanning electron microscopy tomography also showed that MnO particles were evenly distributed through the fiber at low MnACAC concentrations, while at a 40 wt% loading the MnO particles were also visible on the surface. Comparison of the electrospun separators showed improved performance relative to a commercial Celgard separator (200 F g-1 vs 141 F g-1).

  18. Electrospun N-Doped Porous Carbon Nanofibers Incorporated with NiO Nanoparticles as Free-Standing Film Electrodes for High-Performance Supercapacitors and CO2 Capture.

    Science.gov (United States)

    Li, Qi; Guo, Jiangna; Xu, Dan; Guo, Jianqiang; Ou, Xu; Hu, Yin; Qi, Haojun; Yan, Feng

    2018-04-01

    Carbon nanofibers (CNF) with a 1D porous structure offer promising support to encapsulate transition-metal oxides in energy storage/conversion relying on their high specific surface area and pore volume. Here, the preparation of NiO nanoparticle-dispersed electrospun N-doped porous CNF (NiO/PCNF) and as free-standing film electrode for high-performance electrochemical supercapacitors is reported. Polyacrylonitrile and nickel acetylacetone are selected as precursors of CNF and Ni sources, respectively. Dicyandiamide not only improves the specific surface area and pore volume, but also increases the N-doping level of PCNF. Benefiting from the synergistic effect between NiO nanoparticles (NPs) and PCNF, the prepared free-standing NiO/PCNF electrodes show a high specific capacitance of 850 F g -1 at a current density of 1 A g -1 in 6 m KOH aqueous solution, good rate capability, as well as excellent long-term cycling stability. Moreover, NiO NPs dispersed in PCNF and large specific surface area provide many electroactive sites, leading to high CO 2 uptake, and high-efficiency CO 2 electroreduction. The synthesis strategy in this study provides a new insight into the design and fabrication of promising multifunctional materials for high-performance supercapacitors and CO 2 electroreduction. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  19. Single-Site VO x Moieties Generated on Silica by Surface Organometallic Chemistry: A Way To Enhance the Catalytic Activity in the Oxidative Dehydrogenation of Propane

    KAUST Repository

    Barman, Samir

    2016-07-26

    We report here an accurate surface organometallic chemistry (SOMC) approach to propane oxidative dehydrogenation (ODH) using a μ2-oxo-bridged, bimetallic [V2O4(acac)2] (1) (acac = acetylacetonate anion) complex as a precursor. The identity and the nuclearity of the product of grafting and of the subsequent oxidative treatment have been systematically studied by means of FT-IR, Raman, solid-state (SS) NMR, UV-vis DRS, EPR and EXAFS spectroscopies. We show that the grafting of 1 on the silica surface under a rigorous SOMC protocol and the subsequent oxidative thermal treatment lead exclusively to well-defined and isolated monovanadate species. The resulting material has been tested for the oxidative dehydrogenation of propane in a moderate temperature range (400-525 °C) and compared with that of silica-supported vanadium catalysts prepared by the standard impregnation technique. The experimental results show that the catalytic activity in propane ODH is strongly upgraded by the degree of isolation of the VOx species that can be achieved by employing the SOMC protocol. © 2016 American Chemical Society.

  20. Synthesis of the Gleditschia Horrida-like Silver Nanoparticles via Soft Template Method%软模板法制备皂荚形貌银纳米粒子

    Institute of Scientific and Technical Information of China (English)

    何鑫; 张梅; 王忆; 阳素玉; 尹荔松

    2009-01-01

    Novel gleditschia horrida-like silver nanoparticles with average size of 60-70nm are prepared by a soft template method. The network strucutre chelate by tetrabutyl titanate and acetylacetone can guide the formation of one-dimensional silver nanoparticles with gleditschia horrida morphology. The results show that the process temperature and time are crucial factors to shape gleditschia horrida-like silver nanoparticles.%利用软模板法制备了具有新颖皂荚形貌的Ag纳米粒子,其平均尺寸为60~70nm.钛酸丁酯和乙酰丙酮螯舍而成的网络结构可指导一维Ag纳米粒子的生长.实验结果表明,反应温度和反应时间会影响皂英形貌Ag纳米粒子的生长动力学过程.

  1. Upgrading of heavy crude oil with supported and unsupported transition metals

    Energy Technology Data Exchange (ETDEWEB)

    Nares, H.R.; Schacht-Hernandez, P.; Cabrera-Reyes, M.C.; Ramirez-Garnica, M.; Cazarez-Candia, O. [Instituto Mexicano del Petroleo, Atepehuacan (Mexico)

    2006-07-01

    Heavy crude oil presents many problems such as difficulty in transportation, low processing capacity in refineries, and low mobility through the reservoir due to high viscosity which affects the index of productivity of the wells. Because of these challenges, it is necessary to enhance heavy crude oil, both aboveground and underground. The effects of several metallic oxides used to upgrade heavy crude oil properties were examined in order to increase the mobility of reservoir oil by reducing viscosity and improving the quality of the oil. This can be accomplished by reducing the asphaltene and sulfur contents and increasing the American Petroleum Institute (API) gravity using transition metal supported in alumina and unsupported from transition metals derived from either acetylacetonate or alkylhexanoate in liquid phase homogeneously mixed with heavy crude oil as well as metal transition supported in alumina. KU-H heavy crude oil from the Golf of Mexico was studied. The results were obtained by Simulated Distillation and True Boiling Point (TBP). It was concluded that the use of crude oil thermal hydrocracking allowed the API gravity to increase and considerably reduce the viscosity. As a result, the productivity index in wells was increased. However there is a high formation of coke that could damage the conductivity of the rock and then reduce the potential of oil recovery. 27 refs., 3 tabs., 5 figs.

  2. Ultrasonic Spray-Coating of Large-Scale TiO2 Compact Layer for Efficient Flexible Perovskite Solar Cells

    Directory of Open Access Journals (Sweden)

    Peng Zhou

    2017-02-01

    Full Text Available Flexible electronics have attracted great interest in applications for the wearable devices. Flexible solar cells can be integrated into the flexible electronics as the power source for the wearable devices. In this work, an ultrasonic spray-coating method was employed to deposit TiO2 nanoparticles on polymer substrates for the fabrication of flexible perovskite solar cells (PSCs. Pre-synthesized TiO2 nanoparticles were first dispersed in ethanol to prepare the precursor solutions with different concentrations (0.5 mg/mL, 1.0 mg/mL, 2.0 mg/mL and then sprayed onto the conductive substrates to produce compact TiO2 films with different thicknesses (from 30 nm to 150 nm. The effect of the different drying processes on the quality of the compact TiO2 film was studied. In order to further improve the film quality, titanium diisopropoxide bis(acetylacetonate (TAA was added into the TiO2-ethanol solution at a mole ratio of 1.0 mol % with respect to the TiO2 content. The final prepared PSC devices showed a power conversion efficiency (PCE of 14.32% based on the indium doped tin oxide coated glass (ITO-glass substrate and 10.87% on the indium doped tin oxide coated polyethylene naphthalate (ITO-PEN flexible substrate.

  3. Feasibility of the UV/AA process as a pretreatment approach for bioremediation of dye-laden wastewater.

    Science.gov (United States)

    Yang, Minghui; Wu, Bingdang; Li, Qiuhao; Xiong, Xiaofeng; Zhang, Haoran; Tian, Yu; Xie, Jiawen; Huang, Ping; Tan, Suo; Wang, Guodong; Zhang, Li; Zhang, Shujuan

    2018-03-01

    Biodegradability and toxicity are two important indexes in considering the feasibility of a chemical process for environmental remediation. The acetylacetone (AA) mediated photochemical process has been proven as an efficient approach for dye decolorization. Both AA and its photochemical degradation products had a high bioavailability. However, the biocompatibility and ecotoxicology of the UV/AA treated solutions are unclear yet. In the present work, we evaluated the biocompatibility and toxicity of the UV/AA treated solutions at both biochemical and organismal levels. The biodegradability of the treated solution was evaluated with the ratio of 5-d biological oxygen demand (BOD 5 ) to chemical oxygen demand (COD) and a 28-d activated sludge assay (Zahn-Wellens tests). The UV/AA process significantly improved the biodegradability of the tested dye solutions. Toxicity was assessed with responses of microorganisms (microbes in activated sludge and Daphnia magna) and plants (bok choy, rice seed, and Arabidopsis thaliana) to the treated solutions, which showed that the toxicity of the UV/AA treated solutions was lower or comparable to that of the UV/H 2 O 2 counterparts. The results are helpful for us to determine whether the UV/AA process is applicable to certain wastewaters and how the UV/AA process could be effectively combined into a sequential chemical-biological water treatment. Copyright © 2017 Elsevier Ltd. All rights reserved.

  4. Zinc oxide films impurified with Ti and prepared by the Sol-gel method

    International Nuclear Information System (INIS)

    Tirado G, S.; Cazares R, J.M.; Maldonado, A.

    2006-01-01

    Titanium-doped zinc oxide thin films have been prepared on silicon substrate using the Sol-Gel technique. The structural, morphology, electrical and optical properties of such thin films were studied as a function of titanium concentration (0.5, 1 and 1.5 %) and the thin films thickness. Zinc acetate dihydrate and titanium (VI)-oxy acetylacetonate were used as precursor materials, using 2-methoxyethanol and monoethanolamine as via. The X-ray diffraction spectra show polycrystalline films in all the cases. It can see for all the thin films a preferential growth along the (002) planes where the titanium concentration and also the thin films thickness play an important rule. No structural changes are observed at all. The surface morphology studied shows as the grain size decreases when thin thickness is increases. For titanium concentration of 0.5, 1 and 1.5 % values the grains size increase also. The thin films thickness for titanium concentration of 1.5 % was 500 nm (4v), 400 nm (3v), 180 nm (2v) and 130 nm (1v), values obtained from cross-section micrographs. Highly resistive samples are obtained for substrate soda-lime even showing high transmittance. Better physical properties are required for gas sensors or semitransparent electrodes and other possible applications. (Author)

  5. Facile synthesis of palladium nanoparticles supported on multi-walled carbon nanotube for efficient hydrogenation of biomass-derived levulinic acid

    Energy Technology Data Exchange (ETDEWEB)

    Yan, Kai, E-mail: kyan@lakeheadu.ca; Lafleur, Todd [Lakehead University, Department of Chemistry (Canada); Liao, Jiayou [Tianjin University, School of Chemical Engineering and Technology (China)

    2013-09-15

    Different loading of palladium (Pd) nanoparticles were successfully fabricated on multi-walled carbon nanotubes using Pd acetylacetonate as the precursor via a simple liquid impregnation method. The crystal phase, morphology, textural structure and the chemical state of the resulting Pd nanoparticles (Pd/CNT) catalysts were studied and the characterization results indicated that the uniform dispersion of small Pd nanoparticles with the size range of 1.0-4.5 nm was achieved. The synthesized Pd/CNT catalysts exhibited efficient performance for the catalytic hydrogenation of biomass-derived levulinic acid into biofuel {gamma}-valerolactone. In comparison with the commercial 5 wt% Pd/C and the 5 wt% Pd/CNT catalyst prepared by Pd nitrate precursor, much higher activities were achieved, whereas the biofuel {gamma}-valerolactone was highly produced with 56.3 % yield at 57.6 % conversion of levulinic acid on the 5 wt% Pd/CNT catalyst under mild conditions. The catalyst developed in this work may be a good candidate for the wide applications in the hydrogenation.

  6. Thermal treatment to enhance saturation magnetization of superparamagnetic Ni nanoparticles while maintaining low coercive force

    Science.gov (United States)

    Ishizaki, Toshitaka; Yatsugi, Kenichi; Akedo, Kunio

    2018-05-01

    Superparamagnetic nanoparticles capped by insulators have the potential to decrease eddy current and hysteresis losses. However, the saturation magnetization ( M s) decreases significantly with decreasing the particle size. In this study, superparamagnetic Ni nanoparticles having the mean size of 11.6 ± 1.8 nm were synthesized from the reduction of Ni(II) acetylacetonate in oleylamine with the addition of trioctylphosphine, indicating the coercive force ( H c) less than 1 Oe. Thermal treatments of the Ni nanoparticles were investigated as a method to enhance the M s. The results indicated that the M s was enhanced by an increase of the Ni mass ratio with increasing thermal treatment temperature. However, the decomposition behavior of the capping layers indicated that their alkyl chains actively decomposed at temperatures above 523 K to form Ni3P via reaction between Ni and P, resulting in particle growth with a significant increase in the H c. Therefore, the optimal temperature was determined to be 473 K, which increased the Ni ratio without formation of Ni3P while maintaining particle sizes with superparamagnetic properties. Further, the M s could be improved by 22% (relative to the as-synthesized Ni nanoparticles) after thermal treatment at 473 K while maintaining the H c to be less than 1 Oe.

  7. Synthesis and Cytotoxic Effect of Some Novel 1,2-Dihydropyridin-3-carbonitrile and Nicotinonitrile Derivatives

    Directory of Open Access Journals (Sweden)

    Eman M. Flefel

    2015-12-01

    Full Text Available 1-(2,4-Dichlorophenyl-3-(4-fluorophenylpropen-1-one (1 was prepared and reacted with an active methylene compound (ethyl cyanoacetate in the presence of ammonium acetate to give the corresponding cyanopyridone 2. Compound 2 reacted with hydrazine hydrate, malononitrile, ethyl bromoacetate and phosphorous oxychloride to afford compounds 4 and 7–11, respectively. The 2-chloropyridine derivative 11 reacted with different primary amines, namely benzyl amine, piperonyl amine, 1-phenylethyl amine, and/or the secondary amines 2-methyl-pipridine and morpholine to give the corresponding derivatives 12–15. Hydrazinolysis of chloropyridine derivative 11 with hydrazine hydrate afforded the corresponding hydrazino derivative 17. Condensation of compound 17 with ethyl acetoacetate, acetylacetone, isatin and different aldehydes gave the corresponding derivatives 18–21. Some of newly synthesized compounds were screened for cytotoxic activity against three tumor cell lines. The results indicated that compounds 8 and 16 showed the best results, exhibiting the highest inhibitory effects towards the three tumor cell lines, which were higher than that of the reference doxorubicin and these compounds were non-cytotoxic towards normal cells (IC50 values > 100 μg/mL.

  8. Methane dry reforming over Ni catalysts supported on Ce–Zr oxides prepared by a route involving supercritical fluids

    Directory of Open Access Journals (Sweden)

    Smirnova Marina Yu.

    2017-12-01

    Full Text Available Ce0.5Zr0.5O2 mixed oxides were prepared in a flow reactor in supercritical isopropanol with acetylacetone as a complexing agent. Variation of the nature of the Zr salt and the temperature of synthesis affected the phase composition, morphology and specific surface area of oxides. X-ray diffraction and Raman spectroscopy studies revealed formation of metastable t” and t’ phases. Oxides are comprised of agglomerates with sizes depending on the synthesis parameters. Loading NiO decreases the specific surface area without affecting X-ray particle sizes of supports. Such sintering was the most pronounced for a support with the highest specific surface area, which resulted in the lowest surface content of Ni as estimated by X-ray photoelectron spectroscopy and in the formation of flattened NiO particles partially embedded into the support. The catalytic activity and stability of these samples in the dry reforming of methane were determined by the surface concentration of Ni and the morphology of its particle controlled by the metal-support interaction, which also depends on the type of catalyst pretreatment. Samples based on ceria-zirconia oxides prepared under these conditions provide a higher specific catalytic activity as compared with the traditional Pechini route, which makes them promising for the practical application.

  9. Model Research On Deposition Of Pure Aluminium Oxide Layers By MOCVD Method

    Directory of Open Access Journals (Sweden)

    Sawka A.

    2015-06-01

    Full Text Available The purpose of this research is to develop an optimal method for synthesizing of nanocrystalline Al2O3 monolayers at high growth rates on cemented carbides coated with an intermediate layer of pre-Al2O3-C (composite layers Al2O3-C/Al2O3. The use of quartz glass substrate allows for obtaining information about the quality of the layers such the thickness and density, because of its high transparency. The Al2O3 layers that do not containing carbon were synthesized on quartz glass by MOCVD using aluminum acetylacetonate and air as the reactants at temperatures of 700-1000°C. Argon was also a carrier gas. The resulting layers were transparent, as homogeneous nucleation did not occur during the synthesis process. The layers synthesized at lower temperatures were subjected to a crystallization process at temperatures above 900°C. The crystallization process was studied as a function of time and temperature. The obtained layers were characterized by their nanocrystalline microstructure.

  10. New cyclometalated iridium(III) complex as a phosphorescent dopant in organic light emitting devices

    Science.gov (United States)

    Ivanov, P.; Tomova, R.; Petrova, P.; Stanimirov, S.; Petkov, I.

    2014-05-01

    A new cyclometalated iridium (III) bis[2-(4-chlorophenyl)benzothiazolato-N,C2]-acetylacetonate, (Cl-bt)2Ir(acac), was synthesized and identified by 1H NMR and elemental analysis. The application was studied of the new compound as a dopant in the hole transporting layer (HTL) of the following organic light emitting diode (OLED) structure: HTL/EL/ETL, where HTL was 4,4'-bis(9H-carbazol-9-yl)biphenyl (CBP) or N,N'-bis(3-methylphenyl)-N,N'-diphenylbenzidine (TPD), incorporated in a poly(N-vinylcarbazole) (PVK) matrix; EL was an electroluminescent layer of bis(8-hydroxy-2-methylquinoline)-(4-phenylpheno-xy) aluminum (BAlq); and ETL was an electron-transporting layer of bis[2-(2-benzothiazoly) phenolato]zinc(II) (Zn(btz)2). We established that the electroluminescence spectra of the OLEDs at different dopant concentrations were basically the sum of the greenish-blue emission of BAlq and the yellowish-green emission of the Ir complex. It was also found that increasing the dopant concentration resulted in an increase in the relative electroluminescent intensity of the Ir complex emission, while that of BAlq decreased, thus a fine tuning of the OLED color was observed.

  11. Separation through liquid-liquid extraction and spectrophotometric determination of U(VI) with the ortho-aminophenol reagent

    International Nuclear Information System (INIS)

    Marian Raileanu

    2012-01-01

    The extractive properties of the ortho-aminophenol reagent upon U(VI) were investigated in two solvents: 4-chlor-acetophenone and acetylacetone, in a water-organic solvent system. The method here proposed is based on the complexation reaction of the uranyl ion, UO 2 2+ , with ortho-aminophenol dissolved in 4-chlor-acetophenone, at room temperature, over a pH interval 4-6, followed by spectro-photometry of the organic phase, involving measuring of absorbancy at 569.6 nm. The Beer law is valid over the 1-12, μg U(VI)/mL concentration interval, with molar absorptivity ε max 4.3 x 10 5 mol -1 cm 2 and Sandell sensitivity = 0.0526 μg cm -2 . The structure, stability and solubility of the formed complex was studied by UV-VIS and IR spectrometry, diffractometry and scanning electron microscopy. The mixed complex formed between the uranyl ion and the ortho-aminophenol dissolved in 4-chlor-acetophenone, [UO 2 .(L) 2 .(S) 4 ], is characterized by the following parameters: metal/ligand combination ratio: M/L = 1/2, stability constant β = 2.06 x 10 6 , distribution coefficient D = 66.56 (V org = V aq ), percentage extraction E% = 98.52, and recovery factor, R%, ranging between 99.48 and 99.85%. (author)

  12. Electron microscopy and EXAFS studies on oxide-supported gold-silver nanoparticles prepared by flame spray pyrolysis

    Energy Technology Data Exchange (ETDEWEB)

    Hannemann, Stefan [Institute of Chemical and Bioengineering, Swiss Federal Institute of Technology, ETH Hoenggerberg, CH-8093 Zurich (Switzerland); Grunwaldt, Jan-Dierk [Institute of Chemical and Bioengineering, Swiss Federal Institute of Technology, ETH Hoenggerberg, CH-8093 Zurich (Switzerland)]. E-mail: grunwaldt@chem.ethz.ch; Krumeich, Frank [Laboratory of Inorganic Chemistry, Swiss Federal Institute of Technology, ETH Hoenggerberg, CH-8093 Zurich (Switzerland); Kappen, Peter [Department of Physics, La Trobe University, Victoria 3086 (Australia); Baiker, Alfons [Institute of Chemical and Bioengineering, Swiss Federal Institute of Technology, ETH Hoenggerberg, CH-8093 Zurich (Switzerland)

    2006-09-15

    Gold and gold-silver nanoparticles prepared by flame spray pyrolysis (FSP) were characterized by electron microscopy, in situ X-ray absorption spectroscopy (XANES and EXAFS), X-ray diffraction (XRD) and their catalytic activity in CO oxidation. Within this one-step flame-synthesis procedure, precursor solutions of dimethyl gold(III) acetylacetonate and silver(I) benzoate together with the corresponding precursor of the silica, iron oxide or titania support, were sprayed and combusted. In order to prepare small metal particles, a low noble metal loading was required. A loading of 0.1-1 wt.% of Au and Ag resulted in 1-6 nm particles. The size of the noble metal particles increased with higher loadings of gold and particularly silver. Both scanning transmission electron microscopy (STEM) combined with energy dispersive X-ray spectroscopy (EDXS) and X-ray absorption spectroscopy (XAS) studies proved the formation of mixed Au-Ag particles. In case of 1% Au-1% Ag/SiO{sub 2}, TEM combined with electron spectroscopic imaging (ESI) using an imaging filter could be used in addition to prove the presence of silver and gold in the same noble metal particle. CO oxidation in the presence of hydrogen was chosen as a test reaction sensitive to small gold particles. Both the influence of the particle size and the alloying of gold and silver were reflected in the CO oxidation activity.

  13. Electron microscopy and EXAFS studies on oxide-supported gold-silver nanoparticles prepared by flame spray pyrolysis

    International Nuclear Information System (INIS)

    Hannemann, Stefan; Grunwaldt, Jan-Dierk; Krumeich, Frank; Kappen, Peter; Baiker, Alfons

    2006-01-01

    Gold and gold-silver nanoparticles prepared by flame spray pyrolysis (FSP) were characterized by electron microscopy, in situ X-ray absorption spectroscopy (XANES and EXAFS), X-ray diffraction (XRD) and their catalytic activity in CO oxidation. Within this one-step flame-synthesis procedure, precursor solutions of dimethyl gold(III) acetylacetonate and silver(I) benzoate together with the corresponding precursor of the silica, iron oxide or titania support, were sprayed and combusted. In order to prepare small metal particles, a low noble metal loading was required. A loading of 0.1-1 wt.% of Au and Ag resulted in 1-6 nm particles. The size of the noble metal particles increased with higher loadings of gold and particularly silver. Both scanning transmission electron microscopy (STEM) combined with energy dispersive X-ray spectroscopy (EDXS) and X-ray absorption spectroscopy (XAS) studies proved the formation of mixed Au-Ag particles. In case of 1% Au-1% Ag/SiO 2 , TEM combined with electron spectroscopic imaging (ESI) using an imaging filter could be used in addition to prove the presence of silver and gold in the same noble metal particle. CO oxidation in the presence of hydrogen was chosen as a test reaction sensitive to small gold particles. Both the influence of the particle size and the alloying of gold and silver were reflected in the CO oxidation activity

  14. Ruthenium nanoparticles decorated curl-like porous carbons for high performance supercapacitors

    Science.gov (United States)

    Lou, Bih-Show; Veerakumar, Pitchaimani; Chen, Shen-Ming; Veeramani, Vediyappan; Madhu, Rajesh; Liu, Shang-Bin

    2016-01-01

    The synthesis of highly dispersed and stable ruthenium nanoparticles (RuNPs; ca. 2-3 nm) on porous activated carbons derived from Moringa Oleifera fruit shells (MOC) is reported and were exploited for supercapacitor applications. The Ru/MOC composites so fabricated using the biowaste carbon source and ruthenium acetylacetonate as the co-feeding metal precursors were activated at elevated temperatures (600-900 oC) in the presence of ZnCl2 as the pore generating and chemical activating agent. The as-prepared MOC carbonized at 900 oC was found to possess a high specific surface area (2522 m2 g-1) and co-existing micro- and mesoporosities. Upon incorporating RuNPs, the Ru/MOC nanocomposites loaded with modest amount of metallic Ru (1.0-1.5 wt%) exhibit remarkable electrochemical and capacitive properties, achiving a maximum capacitance of 291 F g-1 at a current density of 1 A g-1 in 1.0 M H2SO4 electrolyte. These highly stable and durable Ru/MOC electrodes, which can be facily fabricated by the eco-friendly and cost-effective route, should have great potentials for practical applications in energy storage, biosensing, and catalysis.

  15. Nanowires and nanotubes of BN, GaN and Si3N4

    International Nuclear Information System (INIS)

    Deepak, F.L.; Gundiah, G.; Govindaraj, A.; Rao, C.N.

    2002-01-01

    Simple methods of synthesizing nanotubes and nanowires of boron nitride, gallium nitride and silicon nitride have been investigated. The nanotubes and nanowires have been examined by electron microscopy and other techniques. In the case of BN, activated carbon or multi-walled carbon nanotubes (MWNTs) was heated with boric acid in the presence of NH 3 . With activated carbon, BN nanowires constitute the primary products, but good yields of BN nanotubes are obtained with MWNTs. Aligned BN nanotubes are obtained when aligned MWNTs are employed as the starting material suggesting templating role of carbon nanotubes. Single crystal gallium nitride nanowires have been obtained by heating carbon nanotubes coated with gallium acetylacetonate in NH 3 vapor at 910 o C. Single walled carbon nanotubes were used as templated to reduce the diameter of the GaN nanowires. The growth direction of the GaN nanowires is nearly perpendicular to the [100] planes and the nanowires exhibit satisfactory photoluminescence spectra. Si 3 N 4 nanowires have been synthesized by heating multi-walled carbon nanotubes with silica gel at 1360 o C in an atmosphere of NH 3 . Si 3 N 4 nanotubes are found occasionally when aligned multi-walled nanotubes are employed as templates. (author)

  16. Band gap tuning of ZnO nanoparticles via Mg doping by femtosecond laser ablation in liquid environment

    International Nuclear Information System (INIS)

    Chelnokov, E.; Rivoal, M.; Colignon, Y.; Gachet, D.; Bekere, L.; Thibaudau, F.; Giorgio, S.; Khodorkovsky, V.; Marine, W.

    2012-01-01

    Highlights: ► Femtosecond laser ablation synthesis of Mg doped ZnO nanoparticles. ► Electronic properties of ZnO are modified by Mg. ► Band gap and exciton energy shifts to the blue. ► The exciton energy shift is saturated at Mg content of about 20%. ► Phase separation at Mg content is at more than 25%. ► Mechanism of exciton pinning – recombination via new surface states. - Abstract: We use multiphoton IR femtosecond laser ablation to induce non-thermal non-equilibrium conditions of the nanoparticle growth in liquids. Modifications of the electronic properties of ZnO NP were achieved by Mg ion doping of targets prepared from mixtures of Zn and Mg acetylacetonates. The nanoparticle sizes were 3–20 nm depending on the ablation conditions. X-ray fluorescence indicates that stoichiometric ablation and incorporation of Mg in nanocrystalline ZnO occurs. HRTEM observations show that nanoparticles retain their wurtzite structure, while at high Mg concentrations we detect the MgO rich domains. Exciton emissions exhibit relatively narrow bands with progressive and controlled blue shifts up to 184 meV. The exciton energy correlates to band edge absorption indicating strong modification of the NP band gaps. Stabilisation of the exciton blue shift is observed at high Mg concentration. It is accompanied by the formation of structure defects and ZnO/MgO phase separation within the nanoparticles.

  17. Single step thermal decomposition approach to prepare supported γ-Fe2O3 nanoparticles

    International Nuclear Information System (INIS)

    Sharma, Geetu; Jeevanandam, P.

    2012-01-01

    γ-Fe 2 O 3 nanoparticles supported on MgO (macro-crystalline and nanocrystalline) were prepared by an easy single step thermal decomposition method. Thermal decomposition of iron acetylacetonate in diphenyl ether, in the presence of the supports followed by calcination, leads to iron oxide nanoparticles supported on MgO. The X-ray diffraction results indicate the stability of γ-Fe 2 O 3 phase on MgO (macro-crystalline and nanocrystalline) up to 1150 °C. The scanning electron microscopy images show that the supported iron oxide nanoparticles are agglomerated while the energy dispersive X-ray analysis indicates the presence of iron, magnesium and oxygen in the samples. Transmission electron microscopy images indicate the presence of smaller γ-Fe 2 O 3 nanoparticles on nanocrystalline MgO. The magnetic properties of the supported magnetic nanoparticles at various calcination temperatures (350-1150 °C) were studied using a superconducting quantum interference device which indicates superparamagnetic behavior.

  18. Microspheres of polyester loaded with Holmium-165: effect of gamma irradiation on the polymeric structure

    International Nuclear Information System (INIS)

    Azevedo, Mariangela de Burgos M. de; Pires, Geovanna; Lira, Rafael A. de; Geraldes, Adriana N.; Nascimento, Nanci; Melo, Vitor Hugo Soares de; Kodama, Yasko

    2011-01-01

    Biodegradable polymers containing radioactive isotopes have potential applications as delivery vehicles of beta radiation to the cancer tumors by brachytherapy. 166-Ho is an example of such radioisotope emitting high-energy beta particles, and also its gamma rays allow nuclear imaging in everywhere is applied. Among the biodegradable polymers, different types of poly(lactide) have been investigated in our laboratory, and poly(L-lactide) (PLLA) was used as substrate to prepare microparticles loaded with holmium acetylacetonate HoAcAc (PLLA-HoAcAc-MP). The aim of this study was to evaluate the stability of these microparticles to gamma radiation. The PLLA-HoAcAc-MP were irradiated in a nuclear reactor IEA-R1 at IPEN/CNEN-SP, and their stability studied out with gamma radiation of 25, 50 and 100 kGy doses. MP were characterized before and after irradiation by differential scanning calorimetry analysis (DSC), thermogravimetric analysis (TGA), scanning electron microscopy (SEM), X-ray diffraction (XRD) and con focal laser scanning microscopy (CLSM). Preliminary results showed that gamma radiation did not damage morphologically the prepared PLLA-HoAcAc-MP in the dose range studied, and this procedure may be an important tool for knowing the stabilities of the polymers studied as MP for possible application in brachytherapy. (author)

  19. The research of preparing methodology and pharmacokinetics for a novel myocardial perfusion imaging agent 99Tcm-Q3

    International Nuclear Information System (INIS)

    Li Yunchun; Tan Tianzhi; Fan Chengzhong; Kuang Anren; Liang Zhenglu

    1999-01-01

    The preparing methodology and pharmacokinetics of myocardial perfusion imaging agent 99 Tc m -Q 3 are studied. The optimum scheme of 99 Tc m labelling on the basis of exploring the effects of varied labelled condition on radiochemical purity is established by multivariate orthogonal experimental design. The pharmacokinetics is investigated in rabbits, and the plasma protein binding rate is also measured. '30 μL of 1 mol/L KOH in 50% ethanol, 20 μL of 2 g/L SnCl 2 ·2H 2 O in degassed ethanol, 20 mg of N,N'-ethylene-bis (acetylacetone imine) and 5 mg of tris (3-methoxy-1-propyl) phosphine' are chosen as the optimum scheme of this labelled complex. Each of the factors exists significant effect on the radiochemical purity and there is no one-class cross effect on the radiochemical purity between them. The pharmacokinetics of 99 Tc m -Q 3 conform to two-compartment model with 0.23 +- 0.09 mL/min of excellent blood clearance, an initial half-time of 1.6 +- 0.4 min and a late half-time of 203.0 +- 25.8 min. In vitro protein binding rate is lower

  20. NMR and luminescence spectroscopy study of formation of mixed β-diketonate europium complexes

    International Nuclear Information System (INIS)

    Kavun, V.Ya.; Kalinovskaya, I.V.; Karasev, V.E.; Chernyshov, B.N.; Steblevskaya, N.I.

    1987-01-01

    Methods of NMR ('H, 19 F) and luminescent spectroscopy were applied to study ligand substitution in Eu(β-dik) 3 phen-CDCl 3 -(β-dik)' systems, where β-dik-acetylacetone (AA) and hexafluoroacetyl-acetone (HFAA), phen-1.10-phenathroline at different mole ratio (m) of competing ligands (m=AA/HFAA). Formation of mixed Eu(AA) 2 (HFAA)phen and Eu(AA)(HFAA) 2 phen complexes is proved; calculation of the stark structure of 5 D 0 - 7 F j (j=0,1,2) transitions in low-temperature luminescence spectra is conducted for these complexes. It is stated that at minimum HFAA concentration in the solution the latter replaces AA from europium coordination sphere. It is shown that depending on the value in substitution of acidoligands proceeds successfully by the equations Eu(AA) 3 phen+(NHFAA) n → Eu(AA) 3-n → (HFAA) n phen+(NAA) n ; (n=1,2,3)

  1. Laboratory Evaluation of Synthetic Blends of l-(+)-Lactic Acid, Ammonia, and Ketones As Potential Attractants For Aedes aegypti.

    Science.gov (United States)

    Venkatesh, P M; Sen, A

    2017-12-01

    Attraction of Aedes aegypti to various binary, trinary, and quaternary blends of lactic acid and ketones with or without ammonia was studied using a dual choice olfactometer. A dose dependent attraction was observed in cases of single compounds where cyclopentanone attracted the highest percentage (36.9 ± 1.8%) of Ae. aegypti when tested alone. No significant difference was observed between the attraction levels of trinary and binary blends of lactic acid and acetone or butanone when tested against clear air. However, in competitive bioassays, the trinary blend of lactic acid, acetone, and butanone was significantly preferred over binary blends of individual compounds ( P lactic acid. However, acetylacetone acted as an attraction inhibitor when blended with other compounds. Cyclopentanone was attractive, but enhancement of attraction was not observed when blended with other components. Addition of ammonia to binary or trinary blends of lactic acid, acetone, and/or butanone did not increase the attraction significantly. In competitive bioassays, the blends containing ammonia were significantly preferred over the blends lacking ammonia ( P lactic acid, ammonia, acetone, and butanone was most attractive (65 ± 1.5%) and preferred blend of all other combinations.

  2. Preparation and Characterization of TiO2/CdS Layers as Potential Photoelectrocatalytic Materials

    Directory of Open Access Journals (Sweden)

    Teofil-Danut Silipas

    2011-01-01

    Full Text Available The TiO2/CdS semiconductor composites were prepared on
    indium tin oxide (ITO substrates in di®erent mass proportions via wet-chemical techniques using bi-distilled water, acetyl-acetone, poly-propylene-glycol and Triton X-100 as additives. The composite layers were annealed in normal conditions at the temperature of 450±C, 120 min. with a rate of temperature increasing of 5±C/min. The structural and optical properties of all the TiO2/CdS ayers were characterized by X-ray di®raction, UV-VIS spectroscopy, spectrofluorimetry and FT/IR microscopy. The microstructural properties of the deposited TiO2/CdS layers can be modi¯ed by varying the mass proportions of TiO2:CdS. The good crystallinity level and the high optical adsorption of
    the TiO2/CdS layers make them attractive for photoelectrochemical cell applications.

  3. Size effect on L10 ordering and magnetic properties of chemically synthesized FePt and FePtAu nanoparticles

    Science.gov (United States)

    Jia, Zhiyong; Kang, Shishou; Shi, Shifan; Nikles, David E.; Harrell, J. W.

    2005-05-01

    There is growing evidence that FePt nanoparticles become increasingly difficult to chemically order as the size approaches a few nanometers. We have studied the chemical ordering of FePt and FePtAu nanoparticle arrays as a function of particle size. Monodisperse Fe49Pt51 and Fe48Pt44Au8 nanoparticles with a size about 6nm were synthesized by the simultaneous decomposition of iron pentacarbonyl and reduction of platinum acetylacetonate and gold (III) acetate in a mixture of phenyl ether and hexadecylamine (HDA), with 1-adamantanecarboxylic acid and HDA as stabilizers. The nanoparticles were dispersed in toluene, films of the particles were cast onto silicon wafers from the dispersion, and the films were annealed in a tube furnace with flowing Ar +5%H2. The magnetic anisotropy and switching volumes were determined from time- and temperature-dependent coercivity measurements. By comparing with 3-nm FePt and FePtAu nanoparticles of comparable composition, the phase transformation is easier for the larger particles. Under the same annealing conditions, the larger particles have higher anisotropy and order parameter. Additive Au is very effective in enhancing the chemical ordering in both small and large particles, with x-ray diffraction superlattice peaks appearing after annealing at 350°C. Dynamic remnant coercivity measurements and magnetic switching volumes suggest particle aggregation at the higher annealing temperatures in both small and large particles.

  4. Fabrication of barium titanate nanoparticles/poly (methylmethacrylate composite films by a combination of deposition process and spin-coating technique

    Directory of Open Access Journals (Sweden)

    Yoshio Kobayashi

    2014-10-01

    Full Text Available The present work proposes a method for fabricating poly(methylmethacrylate (PMMA film containing barium titanate (BT nanoparticles (BT/PMMA film. BT particles with an average size of 77.6 ± 30.5 nm and a crystal size of 28.1 nm were synthesized by adding sodium hydroxide aqueous solution to titanium tetraisopropoxide/acetylacetone/i-propanol solution suspending barium hydroxide. A sodium glass plate, of which surface was modified with polyvinylpyrrolidone, was immersed into water suspending the BT particles, which resulted in deposition of the BT particles on the plate. A BT/PMMA film was fabricated by twice performance of a process composed of spin-coating of N-methyl-2-pyrrolidone (NMP dissolving PMMA on the plate, and then drying the coated plate in the atmosphere at room temperature. Spin-coating of a PMMA/NMP solution with a PMMA concentration of 150 g/L at a rotating speed of 5000 rpm provided fabrication of a BT/PMMA film with a BT volume fraction of 35.5%, a thickness of ca. 300 nm, and a transmittance of ca. 90% in the visible light region.

  5. Electronic structure and spectroscopic properties of mononuclear manganese(III) Schiff base complexes: a systematic study on [Mn(acen)X] complexes by EPR, UV/vis, and MCD spectroscopy (X = Hal, NCS).

    Science.gov (United States)

    Westphal, Anne; Klinkebiel, Arne; Berends, Hans-Martin; Broda, Henning; Kurz, Philipp; Tuczek, Felix

    2013-03-04

    The manganese(III) Schiff base complexes [Mn(acen)X] (H2acen: N,N'-ethylenebis(acetylacetone)imine, X: I(-), Br(-), Cl(-), NCS(-)) are considered as model systems for a combined study of the electronic structure using vibrational, UV/vis absorption, parallel-mode electron paramagnetic resonance (EPR) and low-temperature magnetic circular dichroism (MCD) spectroscopy. By variation of the co-ligand X, the influence of the axial ligand field within a given square-pyramidal coordination geometry on the UV/vis, EPR, and MCD spectra of the title compounds is investigated. Between 25000 and 35000 cm(-1), the low-temperature MCD spectra are dominated by two very intense, oppositely signed pseudo-A terms, referred to as "double pseudo-A terms", which change their signs within the [Mn(acen)X] series dependent on the axial ligand X. Based on molecular orbital (MO) and symmetry considerations, these features are assigned to π(n.b.)(s, a) → yz, z(2) ligand-to-metal charge transfer transitions. The individual MCD signs are directly determined from the calculated MOs of the [Mn(acen)X] complexes. The observed sign change is explained by an inversion of symmetry among the π(n.b.)(s, a) donor orbitals which leads to an interchange of the positive and negative pseudo-A terms constituting the "double pseudo-A term".

  6. Knigth's Move in the Periodic Table, From Copper to Platinum, Novel Antitumor Mixed Chelate Copper Compounds, Casiopeinas, Evaluated by an in Vitro Human and Murine Cancer Cell Line Panel.

    Science.gov (United States)

    Gracia-Mora, I; Ruiz-Ramírez, L; Gómez-Ruiz, C; Tinoco-Méndez, M; Márquez-Quiñones, A; Lira, L R; Marín-Hernández, A; Macías-Rosales, L; Bravo-Gómez, M E

    2001-01-01

    We synthesized a novel anticancer agents based on mixed chelate copper (II) complexes, named Casiopeínas((R)) has of general formula [Cu(N-N)(N-O)H(2)O]NO(3) (where, N-N = diimines as 1,10- phenanthroline, 2,2-bipyridine, or substituted and N-O=aminoeidate or [Cu(N-N)(O-O)H(2)O]NO(3) (where NN= diimines as 10-phenanthroline, 2,2-bipyridine or substituted Casiopeínas I, II, IV, V, VI, VII VIII and O-O=acetylacetonate, salicylaldehidate Casiopínas III). We evaluated the in vitro antitumor activity using a human cancer cell panel and some nurine cancer cells. Eleven Casiopeinas are evaluated in order to acquire some structure-activity correlations and some monodentated Casiopeinäs analogues; cisplatinum was used as control drug. The 50% growth inhibition observed is, in all cases reach with concentrations of Casiopeina's 10 or 100 times lower than cisplatinum. In a previous work we reported the induction of apoptosis by Casiopeina II. The results indicate that Casiopeinass are a promising new anticancer drug candidates to be developed further toward clinical trials.

  7. Direct arylation of benzene with aryl bromides using high-temperature/high-pressure process windows: expanding the scope of C-H activation chemistry.

    Science.gov (United States)

    Pieber, Bartholomäus; Cantillo, David; Kappe, C Oliver

    2012-04-16

    A detailed investigation on the direct arylation of benzene with aryl bromides by using first-row transition metals under high-temperature/high-pressure (high-T/p) conditions is described. By employing a parallel reactor platform for rapid reaction screening and discovery at elevated temperatures, various metal/ligand/base combinations were evaluated for their ability to enable biaryl formation through C-H activation. The combination of cobalt(III) acetylacetonate and lithium bis(trimethylsilyl)amide was subjected to further process intensification at 200 °C (15 bar), allowing a significant reduction of the catalyst/base loading and a dramatic increase in catalytic efficiency (turnover frequency) by a factor of 1000 compared to traditional protocols. The high-throughput screening additionally identified novel nickel- and copper-based metal/ligand combinations that favored an amination pathway competing with C-H activation, with the addition of ligands, such as 1,10-phenanthroline, having a profound influence on the selectivity. In addition to metal-based catalysts, high-T/p process windows were also successfully applied to transition-metal-free systems, utilizing 1,10-phenanthroline as organocatalyst. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  8. Adjusting White OLEDs with Yellow Light Emission Phosphor Dye and Ultrathin NPB Layer Structure

    Directory of Open Access Journals (Sweden)

    Jun Wang

    2013-01-01

    Full Text Available High efficiency white organic light emission devices were demonstrated with phosphor material dye bis[2-(4-tertbutylphenylbenzothiazolato-N,C2′]iridium (acetylacetonate and ultrathin layer structure. The ultra thin layer be composed of 4,4′-bis[N-1-naphthyl-N-phenyl-amino]biphenyl (NPB or 4,4′-N,N′-dicarbazole-biphenyl : NPB mixed layer with blue light emission. The emission spectra of devices could be adjusted by different phosphor doping concentrations and ultra thin layer structure. Warm white light emitting device could be obtained with 5 wt% doping concentration and power efficiency of 9.93 lm/W at 5 V. Pure white light with Commission Internationale de l'Eclairage (CIE coordinates of (0.33, 0.30 and external quantum efficiency of 4.49% could be achieved with ultra thin layer device structure and 3 wt% phosphor doped device.

  9. Copper-assisted shape control in colloidal synthesis of indium oxide nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Selishcheva, Elena; Parisi, Juergen; Kolny-Olesiak, Joanna, E-mail: joanna.kolny@uni-oldenburg.de [University of Oldenburg, Energy and Semiconductor Research Laboratory, Institute of Physics (Germany)

    2012-02-15

    Indium oxide is an important n-type transparent semiconductor, finding application in solar cells, sensors, and optoelectronic devices. We present here a novel non-injection synthesis route for the preparation of colloidal indium oxide nanocrystals by using oleylamine (OLA) as ligand and as solvent. Indium oxide with cubic crystallographic structure is formed in a reaction between indium acetate and OLA, the latter is converted to oleylamide during the synthesis. The shape of the nanocrystals can be influenced by the addition of copper ions. When only indium (III) acetate is used as precursor flower-shaped indium oxide nanoparticles are obtained. Addition of copper salts such as copper (I) acetate, copper (II) acetate, copper (II) acetylacetonate, or copper (I) chloride, under otherwise identical reaction conditions changes the shape of nanoparticles to quasi-spherical or elongated. The anions, except for chloride, do not influence the shape of the resulting nanocrystals. This finding suggests that adsorption of copper ions on the In{sub 2}O{sub 3} surface during the nanoparticles growth is responsible for shape control, whereas changes in the reactivity of the In cations caused by the presence of different anions play a secondary role. X-ray diffraction, transmission electron microscopy, nuclear magnetic resonance, energy dispersive X-ray analysis, and UV-Vis-absorption spectroscopy are used to characterize the samples.

  10. Copper-assisted shape control in colloidal synthesis of indium oxide nanoparticles

    International Nuclear Information System (INIS)

    Selishcheva, Elena; Parisi, Jürgen; Kolny-Olesiak, Joanna

    2012-01-01

    Indium oxide is an important n-type transparent semiconductor, finding application in solar cells, sensors, and optoelectronic devices. We present here a novel non-injection synthesis route for the preparation of colloidal indium oxide nanocrystals by using oleylamine (OLA) as ligand and as solvent. Indium oxide with cubic crystallographic structure is formed in a reaction between indium acetate and OLA, the latter is converted to oleylamide during the synthesis. The shape of the nanocrystals can be influenced by the addition of copper ions. When only indium (III) acetate is used as precursor flower-shaped indium oxide nanoparticles are obtained. Addition of copper salts such as copper (I) acetate, copper (II) acetate, copper (II) acetylacetonate, or copper (I) chloride, under otherwise identical reaction conditions changes the shape of nanoparticles to quasi-spherical or elongated. The anions, except for chloride, do not influence the shape of the resulting nanocrystals. This finding suggests that adsorption of copper ions on the In 2 O 3 surface during the nanoparticles growth is responsible for shape control, whereas changes in the reactivity of the In cations caused by the presence of different anions play a secondary role. X-ray diffraction, transmission electron microscopy, nuclear magnetic resonance, energy dispersive X-ray analysis, and UV–Vis-absorption spectroscopy are used to characterize the samples.

  11. Preparation and in vitro evaluation of folate-receptor-targeted SPION–polymer micelle hybrids for MRI contrast enhancement in cancer imaging

    International Nuclear Information System (INIS)

    Mahajan, Shveta; Choudhary, Veena; Koul, Veena; Shishodia, Gauri; Bharti, Alok C

    2013-01-01

    Polymer–SPION hybrids were investigated for receptor-mediated localization in tumour tissue. Superparamagnetic iron oxide nanoparticles (SPIONs) prepared by high-temperature decomposition of iron acetylacetonate were monodisperse (9.27 ± 3.37 nm), with high saturation magnetization of 76.8 emu g −1 . Amphiphilic copolymers prepared from methyl methacrylate and PEG methacrylate by atom transfer radical polymerization were conjugated with folic acid (for folate-receptor specificity). The folate-conjugated polymer had a low critical micellar concentration (0.4 mg l −1 ), indicating stability of the micellar formulation. SPION–polymeric micelle clusters were prepared by desolvation of the SPION dispersion/polymer solution in water. Magnetic resonance imaging of the formulation revealed very good contrast enhancement, with transverse (T 2 ) relaxivity of 260.4 mM −1 s −1 . The biological evaluation of the SPION micelles included cellular viability assay (MTT) and uptake in HeLa cells. These studies demonstrated the potential use of these nanoplatforms for imaging and targeting. (paper)

  12. Preparation and in vitro evaluation of folate-receptor-targeted SPION-polymer micelle hybrids for MRI contrast enhancement in cancer imaging

    Science.gov (United States)

    Mahajan, Shveta; Koul, Veena; Choudhary, Veena; Shishodia, Gauri; Bharti, Alok C.

    2013-01-01

    Polymer-SPION hybrids were investigated for receptor-mediated localization in tumour tissue. Superparamagnetic iron oxide nanoparticles (SPIONs) prepared by high-temperature decomposition of iron acetylacetonate were monodisperse (9.27 ± 3.37 nm), with high saturation magnetization of 76.8 emu g-1. Amphiphilic copolymers prepared from methyl methacrylate and PEG methacrylate by atom transfer radical polymerization were conjugated with folic acid (for folate-receptor specificity). The folate-conjugated polymer had a low critical micellar concentration (0.4 mg l-1), indicating stability of the micellar formulation. SPION-polymeric micelle clusters were prepared by desolvation of the SPION dispersion/polymer solution in water. Magnetic resonance imaging of the formulation revealed very good contrast enhancement, with transverse (T2) relaxivity of 260.4 mM-1 s-1. The biological evaluation of the SPION micelles included cellular viability assay (MTT) and uptake in HeLa cells. These studies demonstrated the potential use of these nanoplatforms for imaging and targeting.

  13. Preparation and characterization of Fe{sub 3}O{sub 4}-Pt nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Andrade, Ângela Leão, E-mail: angelala01@hotmail.com [Federal University of Ouro Preto (UFOP), Department of Chemistry, ICEB (Brazil); Cavalcante, Luis Carlos Duarte [Federal University of Piauí (UFPI), Center of Natural Sciences (Brazil); Fabris, José Domingos [Federal University of Minas Gerais (UFMG), Department of Chemistry, ICEx (Brazil); Pereira, Márcio César [Federal University of the Jequitinhonha and Mucuri Valleys (UFVJM), Institute of Science, Engineering and Technology (Brazil); Ardisson, José Domingos [Center for the Development of the Nuclear Technology (CDTN), Laboratory of Applied Physics (Brazil); Domingues, Rosana Zacarias [Federal University of Minas Gerais (UFMG), Department of Chemistry, ICEx (Brazil)

    2017-11-15

    Pt and Pt-based nanomaterials are active anticancer drugs for their ability to inhibit the division of living cells. Nanoparticles of magnetite containing variable proportions of platinum were prepared in the laboratory. The magnetite nanoparticles with platinum (Pt-Fe{sub 3}O{sub 4}) were obtained by reducing the Fe{sup 3+} of the maghemite (γ Fe{sub 2}O{sub 3}) mixed with platinum (II) acetylacetonate and sucrose in two inversely coupled ceramic crucibles and heated in a furnace at 400 °C for 20 min. The formed carbon during this preparation acts to chemically reduce the ferric iron in maghemite. Moreover, its residual layer on the particle surface prevents the forming magnetite from oxidizing in air and helps retain the platinum in the solid mixture. The produced Pt-magnetite samples were characterized by {sup 57}Fe-Mössbauer spectroscopy, powder X-ray diffraction, scanning electron microscopy, and magnetization measurements. Measurements of AC magnetic-field-induced heating properties of the obtained nanocomposites, in aqueous solution, showed that they are suitable as a hyperthermia agent for biological applications.

  14. Photoluminescence studies of organic phosphor coated diffusing surface using blue inorganic light-emitting diode as excitation source

    International Nuclear Information System (INIS)

    Singh, Gyanendra; Mehta, Dalip Singh

    2013-01-01

    We report the studies on photoluminescence (PL) of organic phosphor coated on a diffusing surface using a blue inorganic light-emitting diode (LED) array as an excitation source. The organic phosphor composite coated diffuser was used to scatter the directional blue light from the LED array. Some of the blue light is absorbed by the organic phosphor composite and the phosphor molecules are excited and re-emit light at longer wavelengths due to the PL process. The output light consists of scattered blue light plus phosphor generated broadband yellow light, thus making white light. The diffuser was made up of a plastic substrate coated with an organic composite of small molecule fluorescent material zinc(II)bis(8-hydroxyquinoline) (Znq 2 ) doped with different percentages of electro-phosphorescent metal complex iridium(III)bis(2-methyldibenzo-[f, h] quinoxaline) (acetylacetonate) ([Ir(MDQ) 2 (acac)]). By means of changing the concentration and the thickness of the phosphor composite material the colour coordinates of white light were achieved. The CIE coordinates and correlated colour temperature were calculated for various thicknesses and phosphor composite concentrations and the results are reported. (paper)

  15. A comparative study of alumina-supported Ni catalysts prepared by photodeposition and impregnation methods on the catalytic ozonation of 2,4-dichlorophenoxyacetic acid

    Energy Technology Data Exchange (ETDEWEB)

    Rodríguez, Julia L., E-mail: ozliliana@yahoo.com.mx [Lab. Ing. Química Ambiental. ESIQIE–Instituto Politécnico Nacional (Mexico); Valenzuela, Miguel A. [Lab.Catálisis y Materiales. ESIQIE–Instituto Politécnico Nacional. Zacatenco (Mexico); Tiznado, Hugo [Centro de Nanociencias y Nanotecnología. CNyN Universidad Nacional Autónoma de México (Mexico); Poznyak, Tatiana [Lab. Ing. Química Ambiental. ESIQIE–Instituto Politécnico Nacional (Mexico); Chairez, Isaac [Departamento de Bioprocesos, UPIBI- Instituto Politécnico Nacional (Mexico); Magallanes, Diana [Lab. Ing. Química Ambiental. ESIQIE–Instituto Politécnico Nacional (Mexico)

    2017-02-15

    The heterogeneous catalytic ozonation on unsupported and supported oxides has been successfully tested for the removal of several refractory compounds in aqueous solution. In this work, alumina-supported nickel catalysts prepared by photodeposition and impregnation methods were compared in the catalytic ozonation of 2,4-dichlorophenoxyacetic acid (2,4-D). The catalysts were characterized by high-resolution electron microscopy and X-ray photoelectron spectroscopy. The photochemical decomposition of Ni acetylacetonate to produce Ni(OH){sub 2}, NiO, and traces of Ni° deposited on alumina was achieved in the presence of benzophenone as a sensitizer. A similar surface composition was found with the impregnated catalyst after its reduction with hydrogen at 500 °C and exposed to ambient air. Results indicated a higher initial activity and maleic acid (byproduct) concentration with the photodeposited catalyst (1 wt% Ni) compared to the impregnated catalyst (3 wt% Ni). These findings suggest the use of the photodeposition method as a simple and reliable procedure for the preparation of supported metal oxide/metal catalysts under mild operating conditions.

  16. Application of exciplex in the fabrication of white organic light emitting devices with mixed fluorescent and phosphorescent layers

    International Nuclear Information System (INIS)

    Yang, Dan; Duan, Yahui; Yang, Yongqiang; Hu, Nan; Wang, Xiao; Sun, Fengbo; Duan, Yu

    2015-01-01

    In this study, a highly efficient fluorescent/phosphorescent white organic light-emitting device (WOLED) was fabricated using exciplex light emission. The hole-transport material 4,4',4''-tris(N-carbazolyl)triphenylamine (TCTA), and electron-transport material, 4,7-diphenyl-1,10-phenanthroline (Bphen), were mixed to afford a blue-emitting exciplex. The WOLED was fabricated with a yellow phosphorescent dye, Ir(III) bis(4-phenylthieno [3,2-c] pyridinato-N,C 2' ) acetylacetonate (PO-01), combined with the exciplex. In this structure, the energy can be efficiently transferred from the blend layer to the yellow phosphorescent dye, thus improving the efficiency of the utilization of the triplet exciton. The maximum power efficiency of the WOLED reached a value 9.03 lm/W with an external quantum efficiency of 4.3%. The Commission Internationale de I'Eclairage (CIE) color coordinates (x,y) of the device were from (0.39, 0.45) to (0.27, 0.31), with a voltage range of 4–9 V. - Highlights: • An exciplex/phosphorescence hybrid white OLED was fabricated for the first time with blue/orange complementary emitters. • By using exciplex as the blue emitter, non-radiative triplet-states on the exciplex can be harvested for light-emission by transferring them to low triplet-state phosphors

  17. Highly Efficient Solution-Processed Deep-Red Organic Light-Emitting Diodes Based on an Exciplex Host Composed of a Hole Transporter and a Bipolar Host.

    Science.gov (United States)

    Huang, Manli; Jiang, Bei; Xie, Guohua; Yang, Chuluo

    2017-10-19

    With the aim to achieve highly efficient deep-red emission, we introduced an exciplex forming cohost, 4,4',4″-tris(3-methylphenylphenylamino)triphenylamine (m-MTDATA): 2,5-bis(2-(9H-carbazol-9-yl)phenyl)-1,3,4-oxadiazole (o-CzOXD) (1:1). Due to the efficient triplet up-conversion processes upon the exciplex forming cohost, excellent performances of the devices were achieved with deep-red emission. Using the heteroleptic iridium complexes as the guest dopants, the solution-processed deep-red phosphorescent organic light-emitting diodes (PhOLEDs) with the iridium(III) bis(6-(4-(tert-butyl)phenyl)phenanthridine)acetylacetonate [(TP-BQ) 2 Ir(acac)]-based phosphorescent emitter exhibited an electroluminescent peak at 656 nm and a maximum external quantum efficiency (EQE) of 11.9%, which is 6.6 times that of the device based on the guest emitter doped in the polymer-based cohost. The unique exciplex with a typical hole transporter and a bipolar material is ideal and universal for hosting the red PhOLEDs and tremendously improves the device performances.

  18. Highly efficient inverted top emitting organic light emitting diodes using a transparent top electrode with color stability on viewing angle

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Jung-Bum; Lee, Jeong-Hwan; Moon, Chang-Ki; Kim, Jang-Joo, E-mail: jjkim@snu.ac.kr [Department of Materials Science and Engineering, Seoul National University, Seoul 151-742 (Korea, Republic of)

    2014-02-17

    We report a highly efficient phosphorescent green inverted top emitting organic light emitting diode with excellent color stability by using the 1,4,5,8,9,11-hexaazatriphenylene-hexacarbonitrile/indium zinc oxide top electrode and bis(2-phenylpyridine)iridium(III) acetylacetonate as the emitter in an exciplex forming co-host system. The device shows a high external quantum efficiency of 23.4% at 1000 cd/m{sup 2} corresponding to a current efficiency of 110 cd/A, low efficiency roll-off with 21% at 10 000 cd/m{sup 2} and low turn on voltage of 2.4 V. Especially, the device showed very small color change with the variation of Δx = 0.02, Δy = 0.02 in the CIE 1931 coordinates as the viewing angle changes from 0° to 60°. The performance of the device is superior to that of the metal/metal cavity structured device.

  19. 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

  20. Self-organization of nickel nanoparticles dispersed in acetone: From separate nanoparticles to three-dimensional superstructures

    Directory of Open Access Journals (Sweden)

    I. Hernández-Pérez

    2017-02-01

    Full Text Available Sonochemical synthesis of monodisperse nickel nanoparticles (Ni-NPs by reduction of Ni acetylacetonate in the presence of polyvinylpyrrolidone stabilizer is reported. The Ni-NPs size is readily controlled to 5 nanometer diameter with a standard deviation of less than 5%. The as-prepared Ni-NPs sample was dispersed in acetone, for 4 weeks. For structural analysis was not applied to a magnetic field or heat treatment as key methods to direct the assembly. The transition from separate Ni-NPs into self-organization of three dimensions (3D superstructures was studied by electron microscopy. Experimental analysis suggests that the translation and rotation movement of the Ni-NPs are governed by magnetic frustration which promotes the formation of different geometric arrangements in two dimensions (2D. The formation of 3D superstructures is confirmed from scanning electron microscopy revealing a layered domain that consists of staking of several monolayers having multiple well-defined supercrystalline domains, enabling their use for optical, electronic and sensor applications.

  1. Vapor deposition of molybdenum oxide using bis(ethylbenzene) molybdenum and water

    International Nuclear Information System (INIS)

    Drake, Tasha L.; Stair, Peter C.

    2016-01-01

    Three molybdenum precursors—bis(acetylacetonate) dioxomolybdenum, molybdenum isopropoxide, and bis(ethylbenzene) molybdenum—were tested for molybdenum oxide vapor deposition. Quartz crystal microbalance studies were performed to monitor growth. Molybdenum isopropoxide and bis(ethylbenzene) molybdenum achieved linear growth rates 0.01 and 0.08 Å/cycle, respectively, using atomic layer deposition techniques. Negligible MoO_x growth was observed on alumina powder using molybdenum isopropoxide, as determined by inductively coupled plasma optical emission spectroscopy. Bis(ethylbenzene) molybdenum achieved loadings of 0.5, 1.1, and 1.9 Mo/nm"2 on alumina powder after one, two, and five cycles, respectively, using atomic layer deposition techniques. The growth window for bis(ethylbenzene) molybdenum is 135–150 °C. An alternative pulsing strategy was also developed for bis(ethylbenzene) molybdenum that results in higher growth rates in less time compared to atomic layer deposition techniques. The outlined process serves as a methodology for depositing molybdenum oxide for catalytic applications. All as-deposited materials undergo further calcination prior to characterization and testing.

  2. Single-Site VO x Moieties Generated on Silica by Surface Organometallic Chemistry: A Way To Enhance the Catalytic Activity in the Oxidative Dehydrogenation of Propane

    KAUST Repository

    Barman, Samir; Maity, Niladri; Bhatte, Kushal; Ould-Chikh, Samy; Dachwald, Oliver; Haeß ner, Carmen; Saih, Youssef; Abou-Hamad, Edy; Llorens, Isabelle; Hazemann, Jean-Louis; Kö hler, Klaus; D’ Elia, Valerio; Basset, Jean-Marie

    2016-01-01

    We report here an accurate surface organometallic chemistry (SOMC) approach to propane oxidative dehydrogenation (ODH) using a μ2-oxo-bridged, bimetallic [V2O4(acac)2] (1) (acac = acetylacetonate anion) complex as a precursor. The identity and the nuclearity of the product of grafting and of the subsequent oxidative treatment have been systematically studied by means of FT-IR, Raman, solid-state (SS) NMR, UV-vis DRS, EPR and EXAFS spectroscopies. We show that the grafting of 1 on the silica surface under a rigorous SOMC protocol and the subsequent oxidative thermal treatment lead exclusively to well-defined and isolated monovanadate species. The resulting material has been tested for the oxidative dehydrogenation of propane in a moderate temperature range (400-525 °C) and compared with that of silica-supported vanadium catalysts prepared by the standard impregnation technique. The experimental results show that the catalytic activity in propane ODH is strongly upgraded by the degree of isolation of the VOx species that can be achieved by employing the SOMC protocol. © 2016 American Chemical Society.

  3. Fabrication of a Combustion-Reacted High-Performance ZnO Electron Transport Layer with Silver Nanowire Electrodes for Organic Solar Cells.

    Science.gov (United States)

    Park, Minkyu; Lee, Sang-Hoon; Kim, Donghyuk; Kang, Juhoon; Lee, Jung-Yong; Han, Seung Min

    2018-02-28

    Herein, a new methodology for solution-processed ZnO fabrication on Ag nanowire network electrode via combustion reaction is reported, where the amount of heat emitted during combustion was minimized by controlling the reaction temperature to avoid damaging the underlying Ag nanowires. The degree of participation of acetylacetones, which are volatile fuels in the combustion reaction, was found to vary with the reaction temperature, as revealed by thermogravimetric and compositional analyses. An optimized processing temperature of 180 °C was chosen to successfully fabricate a combustion-reacted ZnO and Ag nanowire hybrid electrode with a sheet resistance of 30 Ω/sq and transmittance of 87%. A combustion-reacted ZnO on Ag nanowire hybrid structure was demonstrated as an efficient transparent electrode and electron transport layer for the PTB7-Th-based polymer solar cells. The superior electrical conductivity of combustion-reacted ZnO, compared to that of conventional sol-gel ZnO, increased the external quantum efficiency over the entire absorption range, whereas a unique light scattering effect due to the presence of nanopores in the combustion-derived ZnO further enhanced the external quantum efficiency in the 450-550 nm wavelength range. A power conversion efficiency of 8.48% was demonstrated for the PTB7-Th-based polymer solar cell with the use of a combustion-reacted ZnO/Ag NW hybrid transparent electrode.

  4. Mixed-ligand Al complex-a new approach for more high efficient OLEDs

    Energy Technology Data Exchange (ETDEWEB)

    Petrova, Petia K., E-mail: petia@clf.bas.bg [Institute of Optical Materials and Technologies ' Acad. J. Malinowski' , Bulgarian Academy of Sciences, Acad. G Bonchev st., bl. 109, 1113 Sofia (Bulgaria); Tomova, Reni L.; Stoycheva-Topalova, Rumiana T. [Institute of Optical Materials and Technologies ' Acad. J. Malinowski' , Bulgarian Academy of Sciences, Acad. G Bonchev st., bl. 109, 1113 Sofia (Bulgaria); Kaloyanova, Stefka S.; Deligeorgiev, Todor G. [Applied Organic Chemistry, Faculty of Chemistry, University of Sofia, Sofia 1164 (Bulgaria)

    2012-02-15

    The mixed-ligand Aluminum bis(8-hydroxyquinoline) acetylacetonate (Alq{sub 2}Acac) complex was presented and its performance as electroluminescent and electron transporting layer for OLED was studied. The photophysical properties of the novel complex were investigated and compared with the properties of the parent Alq{sub 3}. Highly efficient OLED based on the mixed-ligand Al complex was developed with two times higher luminescence and efficiency compared to the identical OLED based on the conventional Alq{sub 3} The better performance of the devices make the novel Al complex a very promising material for OLEDs. - Highlights: Black-Right-Pointing-Pointer A novel electroluminescent Alq{sub 2}Acac complex is presented as material for OLED. Black-Right-Pointing-Pointer Electroluminescent emission of Alq{sub 2}Acac is very similar to that of commercial Alq{sub 3}. Black-Right-Pointing-Pointer Devices with Alq{sub 2}Acac show better characteristics compared to those with Alq{sub 3}.

  5. Influence of the processing conditions on the structural properties of ZnO layers obtained by PECVD

    Energy Technology Data Exchange (ETDEWEB)

    Kitova, S; Danev, G, E-mail: skitova@clf.bas.b [Institute of Optical Materials and Technology ' Acad. J. Malinowski' , Bulgarian Academy of Sciences, Acad. G. Bonchev str., bl.109, 1113 Sofia (Bulgaria)

    2010-11-01

    The plasma enhanced chemical vapor deposition (PECVD) is a powerful and flexible instrument for depositing thin layers, nanocomposites or nanostructures. In this work ZnO layers have been grown by metal-organic PECVD (RF - 13.56 MHz) on Si wafers. Zn acetylacetonate has been used as a precursor and oxygen as oxidant. The influence of the oxygen content in gas mixture, the total pressure, substrate temperature and ZnO seed layer on the structural properties of the layers deposited on Si wafers has been studied. ZnO layer properties were investigated by X-ray diffraction (XRD) and scanning electron microscopy (SEM). XRD data have shown that all layers are crystalline with hexagonal wurtzite structure. The crystallites are preferentially oriented along c-axis direction perpendicular to the substrate surfaces. The results obtained indicate that by controlling the oxygen content in gas mixture, the total pressure and substrate temperature during the film growth one can control the formation of c-axis phase and the crystallite grain size. Nanorods with good alignment, vertically orientated to the substrate surface can be observed in the layers deposited at low content of O{sub 2} in plasma at substrate temperature of 400 {sup o}C. Due to their structural characteristics these layers are potential materials for preparing chemical- and biosensors where inherently large surface to volume ratio of structured materials are important prerequisite for enhanced sensitivity.

  6. Effect of the substrate surface topology and temperature on the structural properties of ZnO layers obtained by plasma enhanced chemical vapour deposition

    Energy Technology Data Exchange (ETDEWEB)

    Kitova, S; Danev, G, E-mail: skitova@clf.bas.b [Acad. J .Malinowski Central Laboratory of Photoprocesses, Bulgarian Academy of Sciences, Acad. G. Bonchev Str., Bl.109, 1113 Sofia (Bulgaria)

    2010-04-01

    In this work thin ZnO layers were grown by metal-organic PECVD (RF 13.56 MHz) on Si wafers. Zn acetylacetonate was used as a precursor and oxygen as oxidant. A system for dosed injection of the precursor and oxidant into the plasma reactor was developed. The influence of the substrate surface topology and temperature on the structural properties of the deposited layers was studied. ZnO and graphite powder dispersions were used to modify the silicon wafers before starting the deposition process of the layers. Some of the ZnO layers were deposited on the back, unpolished, side of Si wafers. Depositions at 400 {sup 0}C were performed to examine the effect of the substrate temperatures on the layer growth. The film structure was examined by XRD and SEM. The results show that all layers are crystalline with hexagonal wurtzite structure. The crystallites are preferentially oriented along the c-axis direction perpendicular to the substrate surfaces. ZnO layers deposited on thin ZnO seed films and clean Si surface exhibit well-developed grain structures and more c-axis preferred phase with better crystal quality than that of the layers deposited on graphite seed layer or rough, unpolished Si wafer.

  7. New approach towards the polyol route to fabricate MFe2O4 magnetic nanoparticles: The use of MCl2 and Fe(acac)3 as chemical precursors

    Science.gov (United States)

    Solano, Eduardo; Yáñez, Ramón; Ricart, Susagna; Ros, Josep

    2015-05-01

    A new more efficient approach of the polyol route to generate MFe2O4 (M=Mn, Fe, Co, Ni, Cu, Zn) nanoparticles in triethylene glycol (TREG) is presented. The selected thermal procedure is based on the Fe metalorganic precursor (iron(III) acetylacetonate) decomposition in presence of an inorganic transition metal chloride salt (MCl2, M=Mn, Fe, Co, Ni, Cu, Zn) to produce high quality polar dispersible nanoparticles with lower production cost. In addition, the nanoparticles are stabilized by ionic (from the Cl-) and steric (TREG as capping ligand) effects inducing into the nanoparticles an extraordinary stability in different polar solvents. As result of this optimized methodology, the colloidal polar dispersible nanoparticles present a size around 10 nm with an adequate size dispersion demonstrated by analyzing transmission electron microscopy (TEM) images. X-ray powder diffraction (XRPD) results corroborate the absence of secondary phases and the high crystalline degree obtained for the spinel structure, fact proved by using synchrotron X-ray diffraction. The high magnetic performance at low and room temperature of the nanoparticles studied by magnetometry proves the high internal crystal order of the spinel. Parallel to this, the influence of the heating ramp and annealing time in the thermal procedure were also investigated for the CuFe2O4 case, where a relationship between these two parameters and the final size and their associated diameter distribution was found, allowing a possible size control of the final ferrite magnetic nanoparticles synthesized.

  8. Hybrid chemical vapour and nanoceramic aerosol assisted deposition for multifunctional nanocomposite thin films

    Energy Technology Data Exchange (ETDEWEB)

    Warwick, Michael E.A.; Dunnill, Charles W.; Goodall, Josie; Darr, Jawwad A.; Binions, Russell, E-mail: uccarbi@ucl.ac.uk

    2011-07-01

    Hybrid atmospheric pressure chemical vapour and aerosol assisted deposition via the reaction of vanadium acetylacetonate and a suspension of preformed titanium dioxide or cerium dioxide nanoparticles, led to the production of vanadium dioxide nanocomposite thin films on glass substrates. The preformed nanoparticle oxides used for the aerosol were synthesised using a continuous hydrothermal flow synthesis route involving the rapid reaction of a metal salt solution with a flow of supercritical water in a flow reactor. Multifunctional nanocomposite thin films from the hybrid deposition process were characterised using scanning electron microscopy, X-ray diffraction and X-ray photoelectron spectroscopy. The functional properties of the films were evaluated using variable temperature optical measurements to assess thermochromic behaviour and methylene blue photodecolourisation experiments to assess photocatalytic activity. The tests show that the films are multifunctional in that they are thermochromic (having a large change in infra-red reflectivity upon exceeding the thermochromic transition temperature) and have significant photocatalytic activity under irradiation with 254 nm light.

  9. Gas-diffusion microextraction coupled with spectrophotometry for the determination of formaldehyde in cork agglomerates.

    Science.gov (United States)

    Brandão, Pedro F; Ramos, Rui M; Valente, Inês M; Almeida, Paulo J; Carro, Antonia M; Lorenzo, Rosa A; Rodrigues, José A

    2017-04-01

    In this work, a simple methodology was developed for the extraction and determination of free formaldehyde content in cork agglomerate samples. For the first time, gas-diffusion microextraction was used for the extraction of volatile formaldehyde directly from samples, with simultaneous derivatization with acetylacetone (Hantzsch reaction). The absorbance of the coloured solution was read in a spectrophotometer at 412 nm. Different extraction parameters were studied and optimized (extraction temperature, sample mass, volume of acceptor solution, extraction time and concentration of derivatization reagent) by means of an asymmetric screening. The developed methodology proved to be a reliable tool for the determination of formaldehyde in cork agglomerates with the following suitable method features: low LOD (0.14 mg kg -1 ) and LOQ (0.47 mg kg -1 ), r 2  = 0.9994, and intraday and interday precision of 3.5 and 4.9%, respectively. The developed methodology was applied to the determination of formaldehyde in different cork agglomerate samples, and contents between 1.9 and 9.4 mg kg -1 were found. Furthermore, formaldehyde was also determined by the standard method EN 717-3 for comparison purposes; no significant differences between the results of both methods were observed. Graphical abstract Representation of the GDME system and its main components.

  10. Novel composite Zr/PBI-O-PhT membranes for HT-PEFC applications.

    Science.gov (United States)

    Kondratenko, Mikhail S; Ponomarev, Igor I; Gallyamov, Marat O; Razorenov, Dmitry Yu; Volkova, Yulia A; Kharitonova, Elena P; Khokhlov, Alexei R

    2013-01-01

    Novel composite membranes for high temperature polymer-electrolyte fuel cells (HT-PEFC) based on a poly[oxy-3,3-bis(4'-benzimidazol-2″-ylphenyl)phtalide-5″(6″)-diyl] (PBI-O-PhT) polymer with small amounts of added Zr were prepared. It was shown in a model reaction between zirconium acetylacetonate (Zr(acac)4) and benzimidazole (BI) that Zr-atoms are capable to form chemical bonds with BI. Thus, Zr may be used as a crosslinking agent for PBI membranes. The obtained Zr/PBI-O-PhT composite membranes were examined by means of SAXS, thermomechanical analysis (TMA), and were tested in operating fuel cells by means of stationary voltammetry and impedance spectroscopy. The new membranes showed excellent stability in a 2000-hour fuel cell (FC) durability test. The modification of the PBI-O-PhT films with Zr facilitated an increase of the phosphoric acid (PA) uptake by the membranes, which resulted in an up to 2.5 times increased proton conductivity. The existence of an optimal amount of Zr content in the modified PBI-O-PhT film was shown. Larger amounts of Zr lead to a lower PA doping level and a reduced conductivity due to an excessively high degree of crosslinking.

  11. Experimental investigation of some coordination complexes using the sup(151)Eu Moessbauer resonance

    International Nuclear Information System (INIS)

    Lal, Asharfi; Rama Reddy, A.; Arvind; Ahmad, Naseer

    1979-01-01

    Several Schiff base complexes containing Eu 151 metal ions have been synthesized and their Moessbauer spectra are recorded using the constant acceleration velocity spectrometer. The least-square analysis method for the evaluation of the hyperfine field coupling constants is adopted using the computer dec system-10. From the systematic analysis of the quadrupole coupling constants (q.c.c.) and isomer shifts it has been established that the coordination number of the metal ion of Bis(acetylacetone) benzidine and thiourea complexes is five, that of bis-vanillin benzidine and bis-salicylaldehyde-o-dianisidine is six, and that of bis-vanillin-o-phenylene diamine is seven. It is also found that the q.c.c. being negative in all these complexes decreases monotonically as the coordination number increases. One unusual aspect of this experimental data is that most of the coordination complexes have very low f-factors whereas the Schiff base complexes studied here have a fairly high recoilless fractions. Attempts are in progress to synthesize and study the Fe Schiff base complexes in place of Eu. (auth.)

  12. Sol–gel preparation of well-adhered films and long range ordered inverse opal films of BaTiO{sub 3} and Bi{sub 2}Ti{sub 2}O{sub 7}

    Energy Technology Data Exchange (ETDEWEB)

    Al-Arjan, Wafa S. [Chemistry, University of Southampton, Highfield, Southampton SO17 1BJ (United Kingdom); King Faisal University, PO Box 380, Al Hofuf (Saudi Arabia); Algaradah, Mohammed M.F. [Chemistry, University of Southampton, Highfield, Southampton SO17 1BJ (United Kingdom); King Khalid College, Riyadh (Saudi Arabia); Brewer, Jack [Chemistry, University of Southampton, Highfield, Southampton SO17 1BJ (United Kingdom); Hector, Andrew L., E-mail: a.l.hector@soton.ac.uk [Chemistry, University of Southampton, Highfield, Southampton SO17 1BJ (United Kingdom)

    2016-02-15

    Highlights: • Highly adaptable sols are presented for processing of the electroceramic materials BaTiO{sub 3} and Bi{sub 2}Ti{sub 2}O{sub 7}. • High quality thin films are produced by dip coating with good phase control. • Infiltration of cross-linked polystyrene templates led to high quality inverse opals. - Abstract: Barium and bismuth titanate thin films and well-ordered inverse opal films are produced by dip coating from sols containing titanium alkoxides with acetic acid, acetylacetone, methoxyethanol and water. The inverse opal preparations used crosslinked polystyrene opal templates. Heat treatment in air produced tetragonal BaTiO{sub 3} or mixtures of the hexagonal and tetragonal phases, or phase pure Bi{sub 2}Ti{sub 2}O{sub 7}. Good quality films were obtained with a thickness of 5 μm from a single dipping, and the thickness could be increased by dipping multiple times. Inverse opals were well ordered and exhibited opalescence and photonic stop band effects.

  13. Storage of charge carriers on emitter molecules in organic light-emitting diodes

    Science.gov (United States)

    Weichsel, Caroline; Burtone, Lorenzo; Reineke, Sebastian; Hintschich, Susanne I.; Gather, Malte C.; Leo, Karl; Lüssem, Björn

    2012-08-01

    Organic light-emitting diodes (OLEDs) using the red phosphorescent emitter iridium(III)bis(2-methyldibenzo[f,h]quinoxaline) (acetylacetonate) [Ir(MDQ)2(acac)] are studied by time-resolved electroluminescence measurements. A transient overshoot after voltage turn-off is found, which is attributed to electron accumulation on Ir(MDQ)2(acac) molecules. The mechanism is verified via impedance spectroscopy and by application of positive and negative off-voltages. We calculate the density of accumulated electrons and find that it scales linearly with the doping concentration of the emitter. Using thin quenching layers, we locate the position of the emission zone during normal OLED operation and after voltage turn-off. In addition, the transient overshoot is also observed in three-color white-emitting OLEDs. By time- and spectrally resolved measurements using a streak camera, we directly attribute the overshoot to electron accumulation on Ir(MDQ)2(acac). We propose that similar processes are present in many state-of-the-art OLEDs and believe that the quantification of charge carrier storage will help to improve the efficiency of OLEDs.

  14. Optimization of white organic light emitting diodes based on emitting layer charge carrier conduction properties

    International Nuclear Information System (INIS)

    Baek, H I; Lee, C H

    2008-01-01

    We have fabricated white organic light emitting diodes (OLEDs) with multi-emitting layer (EML) structures in which 4,4'-N,N'-dicarbazole-biphenyl (CBP) layers doped with the phosphorescent dopants fac-tris(2-phenylpyridine) iridium (Ir(ppy) 3 ) and bis(2-(2'-benzo[4,5-a]thienyl)pyridinato-N,C3')iridium(acetylacetonate) (btp 2 Ir(acac)) and the fluorescent dopant 4,4'-bis[2-{4-(N,N-diphenylamino) phenyl}vinyl]biphenyl (DPAVBi) were used as green (G), red (R) and blue (B) EMLs, respectively. A higher efficiency was expected with the R/G/B EML sequence from the hole transport layer interface than with the G/R/B sequence because of the differences in the charge carrier conduction properties of the EMLs doped with phosphorescent dopants and the luminance balance between the phosphorescent and fluorescent emissions. A high efficiency of 18.3 cd A -1 (an external quantum efficiency of 8.5%) at 100 cd m -2 and good colour stability were achieved with the R/G/B EML sequence as expected, with an additional non-doped CBP interlayer used between the G and B EMLs. In addition, the OLED with this sequence was found to have the longest lifetime of the white devices we tested

  15. The effect of a charge control layer on the electroluminescent characteristic of blue and white organic light-emitting diodes.

    Science.gov (United States)

    Lee, Dong Hyung; Lee, Seok Jae; Koo, Ja-Ryong; Lee, Ho Won; Shin, Hyun Su; Lee, Song Eun; Kim, Woo Young; Lee, Kum Hee; Yoon, Seung Soo; Kim, Young Kwan

    2014-08-01

    We investigated blue fluorescent organic light-emitting diode (OLED) with a charge control layer (CCL) to produce high efficiency and improve the half-decay lifetime. Three types of devices (device A, B, and C) were fabricated following the number of CCLs within the emitting layer (EML), maintaining the thickness of whole EML. The CCL and host material, 2-methyl-9,10-di(2-naphthyl)anthracene, which has a bipolar property, was able to control the carrier movement with ease inside the EML. Device B demonstrated a maximum luminous efficiency (LE) and external quantum efficiency (EQE) of 9.19 cd/A and 5.78%, respectively. It also showed that the enhancement of the half-decay lifetime, measured at an initial luminance of 1,000 cd/m2, was 1.5 times longer than that of the conventional structure. A hybrid white OLED (WOLED) was also fabricated using a phosphorescent red emitter, bis(2-phenylquinoline)-acetylacetonate iridium III doped in 4,4'-N,N'-dicarbazolyl-biphenyl. The property of the hybrid WOLED with CCL showed a maximum LE and an EQE of 13.46 cd/A and 8.32%, respectively. It also showed white emission with Commission International de L'Éclairage coordinates of (x = 0.41, y = 0.33) at 10 V.

  16. Electroluminescence of organic light-emitting diodes consisting of an undoped (pbi)2Ir(acac) phosphorescent layer

    Science.gov (United States)

    Lei, Xia; Yu, Junsheng; Zhao, Juan; Jiang, Yadong

    2011-11-01

    The electroluminescence (EL) characteristics of phosphorescent organic light-emitting diodes (OLEDs) with an undoped bis(1,2-dipheny1-1H-benzoimidazole) iridium (acetylacetonate) [(pbi)2Ir(acac)] emissive layer (EML) of various film thicknesses were studied. The results showed that the intensity of green light emission decreased rapidly with the increasing thickness of (pbi)2Ir(acac), which was relevant to the triplet excimer emission. It suggested that the concentration quenching of monomer emission in the undoped (pbi)2Ir(acac) film was mainly due to the formation of triplet excimer and partly due to the triplet-triplet annihilation (TTA) and triplet-polaron annihilation (TPA). A green OLED with a maximum luminance of 26,531 cd/m2, a current efficiency of 36.2 cd/A, and a power efficiency of 32.4 lm/W was obtained, when the triplet excimer emission was eliminated. Moreover, the white OLED with low efficiency roll-off was realized due to the broadened recombination zone and reduced quenching effects in the EML when no electron blocking layer was employed.

  17. Enhanced efficiency in single-host white organic light-emitting diode by triplet exciton conversion

    International Nuclear Information System (INIS)

    Wu, Qingyang; Zhang, Shiming; Yue, Shouzhen; Zhang, Zhensong; Xie, Guohua; Zhao, Yi; Liu, Shiyong

    2013-01-01

    The authors observe that the external quantum efficiency (EQE) of the Iridium (III) bis(4-phenylthieno [3,2-c]pyridinato-N,C 2′ )acetylacetonate (PO-01) based yellow organic light-emitting diode (OLED) is significantly increased by uniformly co-doping Iridium (III)bis[(4,6-difluorophenyl)-pyridinato-N,C 2− ] (FIrpic) and PO-01 into the same wide band-gap host of N,N ′ -dicarbazolyl-3, 5-benzene (mCP). Detailed investigation indicates that the efficiency enhancement is ascribed to effective triplet exciton gathering by FIrpic, followed by energy transfer to PO-01. Compared to the control device, which has maximum EQE of 10.5%, an improved maximum EQE of 13.2% is obtained in the optimization white device based on FIrpic and PO-01 emission according to this principle. This work makes it easier for a single host white OLED to simultaneously harvest high efficiency in both blue and yellow units. Comprehensive experimental results show that this phenomenon can also be found and utilized in other popular hosts to realize more efficient white devices. -- Highlights: • This work makes easier for a single host white OLED to harvest high efficiency in both blue and yellow units. • Efficiency enhancement is ascribed to effective triplet exciton gathering by FIrpic, followed by energy transfer to PO-01. • This phenomenon can also be found and utilized in other popular hosts to realize more efficient white devices

  18. Optimization of white organic light emitting diodes based on emitting layer charge carrier conduction properties

    Energy Technology Data Exchange (ETDEWEB)

    Baek, H I; Lee, C H [School of Electrical Engineering and Computer Science and Inter-University Semiconductor Research Center, Seoul National University, Seoul 151-744 (Korea, Republic of)], E-mail: hibaek75@snu.ac.kr

    2008-05-21

    We have fabricated white organic light emitting diodes (OLEDs) with multi-emitting layer (EML) structures in which 4,4'-N,N'-dicarbazole-biphenyl (CBP) layers doped with the phosphorescent dopants fac-tris(2-phenylpyridine) iridium (Ir(ppy){sub 3}) and bis(2-(2'-benzo[4,5-a]thienyl)pyridinato-N,C3')iridium(acetylacetonate) (btp{sub 2}Ir(acac)) and the fluorescent dopant 4,4'-bis[2-{l_brace}4-(N,N-diphenylamino) phenyl{r_brace}vinyl]biphenyl (DPAVBi) were used as green (G), red (R) and blue (B) EMLs, respectively. A higher efficiency was expected with the R/G/B EML sequence from the hole transport layer interface than with the G/R/B sequence because of the differences in the charge carrier conduction properties of the EMLs doped with phosphorescent dopants and the luminance balance between the phosphorescent and fluorescent emissions. A high efficiency of 18.3 cd A{sup -1} (an external quantum efficiency of 8.5%) at 100 cd m{sup -2} and good colour stability were achieved with the R/G/B EML sequence as expected, with an additional non-doped CBP interlayer used between the G and B EMLs. In addition, the OLED with this sequence was found to have the longest lifetime of the white devices we tested.

  19. Enhanced efficiency in single-host white organic light-emitting diode by triplet exciton conversion

    Energy Technology Data Exchange (ETDEWEB)

    Wu, Qingyang, E-mail: wqy1527@163.com [State Key laboratory on Integrated Optoelectronics, College of Electronic Science and Engineering, Jilin University, Changchun 130012 (China); Zhang, Shiming [State Key laboratory on Integrated Optoelectronics, College of Electronic Science and Engineering, Jilin University, Changchun 130012 (China); Département of Chemical Engineering, École Polytechnique de Montréal, Montréal, Québec, Canada H3C3J7 (Canada); Yue, Shouzhen; Zhang, Zhensong [State Key laboratory on Integrated Optoelectronics, College of Electronic Science and Engineering, Jilin University, Changchun 130012 (China); Xie, Guohua [Institut für Angewandte Photophysik, Technische Universtität Dresden, Dresden 01062 (Germany); Zhao, Yi; Liu, Shiyong [State Key laboratory on Integrated Optoelectronics, College of Electronic Science and Engineering, Jilin University, Changchun 130012 (China)

    2013-11-15

    The authors observe that the external quantum efficiency (EQE) of the Iridium (III) bis(4-phenylthieno [3,2-c]pyridinato-N,C{sup 2′})acetylacetonate (PO-01) based yellow organic light-emitting diode (OLED) is significantly increased by uniformly co-doping Iridium (III)bis[(4,6-difluorophenyl)-pyridinato-N,C{sup 2−}] (FIrpic) and PO-01 into the same wide band-gap host of N,N{sup ′}-dicarbazolyl-3, 5-benzene (mCP). Detailed investigation indicates that the efficiency enhancement is ascribed to effective triplet exciton gathering by FIrpic, followed by energy transfer to PO-01. Compared to the control device, which has maximum EQE of 10.5%, an improved maximum EQE of 13.2% is obtained in the optimization white device based on FIrpic and PO-01 emission according to this principle. This work makes it easier for a single host white OLED to simultaneously harvest high efficiency in both blue and yellow units. Comprehensive experimental results show that this phenomenon can also be found and utilized in other popular hosts to realize more efficient white devices. -- Highlights: • This work makes easier for a single host white OLED to harvest high efficiency in both blue and yellow units. • Efficiency enhancement is ascribed to effective triplet exciton gathering by FIrpic, followed by energy transfer to PO-01. • This phenomenon can also be found and utilized in other popular hosts to realize more efficient white devices.

  20. Study of different roles phosphorescent material played in different positions of organic light emitting diodes

    Science.gov (United States)

    Keke, Gu; Jian, Zhong; Jiule, Chen; Yucheng, Chen; Ming, Deng

    2013-09-01

    Phosphorescent materials are crucial to improve the luminescence and efficiency of organic light emitting diodes (OLED), because its internal quantum efficiency can reach 100%. So the studying of optical and electrical properties of phosphorescent materials is propitious for the further development of phosphorescent OLED. Phosphorescent materials were generally doped into different host materials as emitting components, not only played an important role in emitting light but also had a profound influence on carrier transport properties. We studied the optical and electrical properties of the blue 4,4'-bis(2,2-diphenylvinyl)-1,1'-biphenyl (DPVBi)-based devices, adding a common yellow phosphorescent material bis[2-(4- tert-butylphenyl)benzothiazolato- N,C2'] iridium(acetylacetonate) [( t-bt)2Ir(acac)] in different positions. The results showed ( t-bt)2Ir(acac) has remarkable hole-trapping ability. Especially the ultrathin structure device, compared to the device without ( t-bt)2Ir(acac), had increased the luminance by about 60%, and the efficiency by about 97%. Then introduced thin 4,4'-bis(carbazol-9-yl)biphenyl (CBP) host layer between DPVBi and ( t-bt)2Ir(acac), and got devices with stable white color.

  1. Influence of solvents on species crossover and capacity decay in non-aqueous vanadium redox flow batteries: Characterization of acetonitrile and 1, 3 dioxolane solvent mixture

    Science.gov (United States)

    Bamgbopa, Musbaudeen O.; Almheiri, Saif

    2017-02-01

    The importance of the choice of solvent in a non-aqueous redox flow battery (NARFB) cannot be overemphasized. Several studies demonstrated the influence of the solvent on electrolyte performance in terms of reaction rates, energy/power densities, and efficiencies. In this work, we investigate capacity decay as a direct consequence of varying reactant crossover rates through membranes in different solvent environments. Specifically, we demonstrate the superiority of an 84/16 vol% acetonitrile/1,3 dioxolane solvent mixture over pure acetonitrile in terms of energy efficiency (up to 89%) and capacity retention for vanadium NARFBs - while incorporating a Nafion 115 membrane. The permeability of Nafion to the vanadium acetylacetonate active species is an order of magnitude lower when pure acetonitrile is replaced by the solvent mixture. A method to estimate relative membrane permeability is formulated from numerical analysis of self-discharge experimental data. Furthermore, tests on a modified Nafion/SiO2 membrane, which generally offered low species permeability, also show that different solvents alter membrane permeability. Elemental and morphological analyses of cycled Nafion and NafionSi membranes in different solvent environments indicate that different crossover rates induced by the choice of solvent during cycling are due to changes in the membrane microstructure, intrinsic permeability, swelling rates, and chemical stability.

  2. Synthesis and green electrophosphorescence of a novel cyclometalated iridium complex in polymer light-emitting diodes

    Energy Technology Data Exchange (ETDEWEB)

    Wu Lilan [Department of Chemistry, National Cheng Kung University, Tainan, Taiwan 70101 (China); Tsai Sunghao [Institute of Electro-Optical Science and Engineering, National Cheng Kung University, Tainan, Taiwan 70101 (China); Guo Tzungfang [Institute of Electro-Optical Science and Engineering, National Cheng Kung University, Tainan, Taiwan 70101 (China); Yang Chenghsien [Carbon Nanocapsules Research Department, Nano-Powder and Thin Film Technology Center, ITRI South, Tainan, Taiwan 709 (China)]. E-mail: jasonyang0606@yahoo.com.tw; Sun, I-W. [Department of Chemistry, National Cheng Kung University, Tainan, Taiwan 70101 (China)]. E-mail: iwsun@mail.ncku.edu.tw

    2007-10-15

    Abstact: In this paper, we synthesized a new complex bis(dibenzo[f,h]quinolinato-N,C {sup 2'}) iridium(III) acetylactonate ((DBQ){sub 2}Ir(acac)) having a longer conjugate system than bis(2-phenylpyridinato-N,C {sup 2'}) iridium(III) acetylacetonate ((PPY){sub 2}Ir(acac)). Interestingly (DBQ){sub 2}Ir(acac) emits at the same wavelength as (photoluminescence of 530 nm) (PPY){sub 2}Ir(acac). A high-efficiency electrophosphorescent polymer light-emitting diodes was constructed by using (DBQ){sub 2}Ir(acac) as the dopant, and a blend of poly(vinylcarbazole) (PVK) with 2-tert-butylphenyl-5-biphenyl-1,3,4-oxadiazol (PBD) as the host material. The electroluminescence efficiency of 9.5 cd/A is reported for the device doped with 3 wt% of (DBQ){sub 2}Ir(acac). In this device, the emission from the PVK or PBD host was effectively inhibited with the using (DBQ){sub 2}Ir(acac) . Emission from the dopant molecules in such devices involve localization of the injected electron and hole on the metal-organic center. This can occur by a variety of mechanisms, including Foerster and Dexter energy transfer from the host transport material to the dopant, and direct trapping of both electrons and holes on the metal-organic center.

  3. Study of the catalytic selectivity of an aqueous two-component polyurethane system by ftir spectroscopy

    Directory of Open Access Journals (Sweden)

    Stamenković Jakov V.

    2003-01-01

    Full Text Available The difficulty in formulating a two component waterborne polyurethane, is the isocyanate-water side reaction, which can lead to gassing/foaming, loss of isocyanate functionality, low gloss and a reduced pot life. To compensate for this side reaction, these formulations usually contain a large excess of isocyanate. Tin compounds, especially dibutyltin dilaurate, are widely used in coatings as catalysts for the isocyanate/hydroxyl reaction. Because of the high aquatic toxicity of some organotin compounds, there has been an attempt to ban organotin compounds from all coating applications. As a general rule, organotin catalysts are not selective, they catalyze the reaction of isocyanates with both hydroxyl groups and water and also catalyze the hydrolysis of ester groups. One novel approach to control the water side reaction is the use of catalysts which selectively catalyze the isocyanate-polyol reaction and not the isocyanate-water reaction. The selectivity of a variety of metal catalysts (metal octoates, metal acetylacetonates and mangan chelates with mixed ligands to catalyze the preferred reaction was measured using the FTIR method.

  4. Utility of Hantzsch reaction for development of highly sensitive spectrofluorimetric method for determination of alfuzosin and terazosin in bulk, dosage forms and human plasma.

    Science.gov (United States)

    Hammad, Mohamed A; Omar, Mahmoud A; Salman, Baher I

    2017-09-01

    A highly sensitive, cheap, simple and accurate spectrofluorimetric method has been developed and validated for the determination of alfuzosin hydrochloride and terazosin hydrochloride in their pharmaceutical dosage forms and in human plasma. The developed method is based on the reaction of the primary amine moiety in the studied drugs with acetylacetone and formaldehyde according to the Hantzsch reaction, producing yellow fluorescent products that can be measured spectrofluorimetrically at 480 nm after excitation at 415 nm. Different experimental parameters affecting the development and stability of the reaction products were carefully studied and optimized. The fluorescence-concentration plots of alfuzosin and terazosin were rectilinear over a concentration range of 70-900 ng ml -1 , with quantitation limits 27.1 and 32.2 ng ml -1 for alfuzosin and terazosin, respectively. The proposed method was validated according to ICH guidelines and successfully applied to the analysis of the investigated drugs in dosage forms, content uniformity test and spiked human plasma with high accuracy. Copyright © 2017 John Wiley & Sons, Ltd.

  5. Morphology evaluation of ZrO2 dip coating on mild steel and its corrosion performance in NaOH solution

    Science.gov (United States)

    Anwar, M. A.; Kurniawan, T.; Asmara, Y. P.; Harun, W. S. W.; Oumar, A. N.; Nandyanto, A. B. D.

    2017-10-01

    In this work, the morphology of ZrO2 thin film from dip coating process on mild steel has been investigated. Mild steel was dip-coated on solution made of zirconium butoxide as a precursor, ethanol as solvent, acetylacetone as chelating agent and water for hydrolysis. Number of dipping was adjusted at 3, 5 and 7 times. The dipped sample then annealed at 350°C for two hours by adjusting the heating rate at 1°C/min respectively. The optical microscope showed that micro-cracks were observed on the surface of the coating with its concentration reduced as dipping sequence increased. The XRD result showed that annealing process can produce polycrystalline tetragonal-ZrO2. Meanwhile, SEM image showed that the thicknesses of the ZrO2 coatings were in between 400-600 nm. The corrosion resistance of uncoated and coated substrates was studied by polarization test through potentio-dynamic polarization curve at 1mV/s immersed in with 3.5% NaCl. The coating efficiency was improved as the number of layer dip coated increased, which showed improvement in corrosion protection.

  6. Functional doped metal oxide films. Zinc oxide (ZnO) as transparent conducting oxide (TCO) titanium dioxide (TiO{sub 2}) as thermographic phosphor and protective coating

    Energy Technology Data Exchange (ETDEWEB)

    Nebatti Ech-Chergui, Abdelkader

    2011-07-29

    Metalorganic chemical vapor deposition (MOCVD) was used in the present work. Un-doped and Al-doped ZnO films were developed using two reactors: Halogen Lamp Reactor (HLR) (a type of Cold Wall Reactor) and Hot Wall Reactor (HWR), and a comparison was made between them in terms of the film properties. Zinc acetylacetonate was used as precursor for ZnO films while aluminum acetylacetonate was used for doping. The amount of Al doping can be controlled by varying the gas flow rate. Well ordered films with aluminum content between 0 and 8 % were grown on borosilicate glass and silicon. The films obtained are 0.3 to 0.5 {mu}m thick, highly transparent and reproducible. The growth rate of ZnO films deposited using HLR is less than HWR. In HLR, the ZnO films are well oriented along c-axis ((002) plane). ZnO films are commonly oriented along the c-axis due to its low surface free energy. On the other hand, the HWR films are polycrystalline and with Al doping these films aligned along the a-axis ((100) plane) which is less commonly observed. The best films were obtained with the HLR method showing a minimum electrical resistivity of 2.4 m{omega}cm and transmittance of about 80 % in the visible range. The results obtained for Al-doped films using HLR are promising to be used as TCOs. The second material investigated in this work was un-doped and doped titanium dioxide (TiO{sub 2}) films- its preparation and characterization. It is well known that thermographic phosphors can be used as an optical method for the surface temperature measurement. For this application, the temperature-dependent luminescence properties of europium (III)-doped TiO{sub 2} thin films were studied. It was observed that only europium doped anatase films show the phosphorescence. Rutile phase do not show phosphorescence. The films were prepared by the sol-gel method using the dip coating technique. The structures of the films were determined by X-ray diffraction (XRD). The excitation and the emission

  7. Amorphous V-O-C composite nanofibers electrospun from solution precursors as binder- and conductive additive-free electrodes for supercapacitors with outstanding performance

    Science.gov (United States)

    Chen, Xia; Zhao, Bote; Cai, Yong; Tadé, Moses O.; Shao, Zongping

    2013-11-01

    Flexible V-O-C composite nanofibers were fabricated from solution precursors via electrospinning and were investigated as free-standing and additive-free film electrodes for supercapacitors. Specifically, composite nanofibers (V0, V5, V10 and V20) with different vanadyl acetylacetonate (VO(acac)2) contents of 0, 5, 10 and 20 wt% with respect to polyacrylonitrile (PAN) were prepared. The composite nanofibers were comparatively studied using XRD, Raman spectroscopy, XPS, N2 adsorption-desorption, FE-SEM, TEM and S-TEM. The vanadium element was found to be well-dispersed in the carbon nanofibers, free from the formation of an aggregated crystalline phase, even in the case of V20. A specific surface area of 587.9 m2 g-1 was reached for V10 after calcination, which is approximately twice that of the vanadium-free carbon nanofibers (V0, 300.9 m2 g-1). To perform as an electrode for supercapacitors in an aqueous electrolyte, the V10 film delivered a specific capacitance of 463 F g-1 at 1 A g-1. V10 was also able to retain a specific capacitance of 380 F g-1, even at a current density of 10 A g-1. Additionally, very stable cycling stability was achieved, maintaining an outstanding specific capacitance of 400 F g-1 at 5 A g-1 after charge-discharge cycling 5000 times. Thus, V-O-C composite nanofibers are highly attractive electrode materials for flexible, high-power, thin film energy storage devices and applications.Flexible V-O-C composite nanofibers were fabricated from solution precursors via electrospinning and were investigated as free-standing and additive-free film electrodes for supercapacitors. Specifically, composite nanofibers (V0, V5, V10 and V20) with different vanadyl acetylacetonate (VO(acac)2) contents of 0, 5, 10 and 20 wt% with respect to polyacrylonitrile (PAN) were prepared. The composite nanofibers were comparatively studied using XRD, Raman spectroscopy, XPS, N2 adsorption-desorption, FE-SEM, TEM and S-TEM. The vanadium element was found to be well

  8. Sol-Gel Process for Making Pt-Ru Fuel-Cell Catalysts

    Science.gov (United States)

    Narayanan, Sekharipuram; Valdez, Thomas; Kumta, Prashant; Kim, Y.

    2005-01-01

    A sol-gel process has been developed as a superior alternative to a prior process for making platinum-ruthenium alloy catalysts for electro-oxidation of methanol in fuel cells. The starting materials in the prior process are chloride salts of platinum and ruthenium. The process involves multiple steps, is time-consuming, and yields a Pt-Ru product that has relatively low specific surface area and contains some chloride residue. Low specific surface area translates to incomplete utilization of the catalytic activity that might otherwise be available, while chloride residue further reduces catalytic activity ("poisons" the catalyst). In contrast, the sol-gel process involves fewer steps and less time, does not leave chloride residue, and yields a product of greater specific area and, hence, greater catalytic activity. In this sol-gel process (see figure), the starting materials are platinum(II) acetylacetonate [Pt(C5H7O2)2, also denoted Pt-acac] and ruthenium(III) acetylacetonate [Ru(C5H7O2)3, also denoted Ru-acac]. First, Pt-acac and Ru-acac are dissolved in acetone at the desired concentrations (typically, 0.00338 moles of each salt per 100 mL of acetone) at a temperature of 50 C. A solution of 25 percent tetramethylammonium hydroxide [(CH3)4NOH, also denoted TMAH] in methanol is added to the Pt-acac/Ruacac/ acetone solution to act as a high-molecular-weight hydrolyzing agent. The addition of the TMAH counteracts the undesired tendency of Pt-acac and Ru-acac to precipitate as separate phases during the subsequent evaporation of the solvent, thereby helping to yield a desired homogeneous amorphous gel. The solution is stirred for 10 minutes, then the solvent is evaporated until the solution becomes viscous, eventually transforming into a gel. The viscous gel is dried in air at a temperature of 170 C for about 10 hours. The dried gel is crushed to make a powder that is the immediate precursor of the final catalytic product. The precursor powder is converted to the

  9. Cathode materials produced by spray flame synthesis for lithium ion batteries

    Energy Technology Data Exchange (ETDEWEB)

    Hamid, NoorAshrina Binti A.

    2013-07-03

    Lithium ion batteries are one of the most enthralling rechargeable energy storage systems for portable application due to their high energy density. Nevertheless, with respect to electromobility innovation towards better electrochemical properties such as higher energy and power density is required. Altering the cathode material used in Li-ion batteries is favorable since the mass- and volume performance is closely related to the cathode electrode mass. Instead of using LiCoO{sub 2} as cathode electrode, LiFePO{sub 4} has gained serious attention as this material owns a high theoretical capacity of 170 mAh g{sup -1}. It is non-toxic, cheap and consists of abundant materials but suffers from low electronic and ionic conductivity. Utilization of nanotechnology methods in combination with composite formation is known to cure this problem effectively. In this work, a new combination of techniques using highly scalable gas-phase synthesis namely spray-flame synthesis and subsequent solid-state reaction has been used to synthesize nanocomposite LiFePO{sub 4}/C. At first this work deals with the formation and characterization of nanosize FePO{sub 4} from a solution of iron(III)acetylacetonate and tributyl phosphate in toluene using spray-flame synthesis. It was shown that a subsequent solid state reaction with Li{sub 2}CO{sub 3} and glucose yielded a LiFePO{sub 4}/C nanocomposite with very promising electrochemical properties. Based on these initial findings the influence of two synthesis parameter - carbon content and annealing temperature - was investigated towards the physicochemical properties of LiFePO{sub 4}/C. It was shown that an annealing temperature of 700 C leads to high purity composite materials consisting of crystalline LiFePO{sub 4} with crystallite sizes well below 100 nm and amorphous carbon consisting of disordered and graphite-like carbon. Variation of glucose amount between 10 and 30 wt% resulted in carbon contents between 2.1 and 7.3 wt%. In parallel

  10. Cathode materials produced by spray flame synthesis for lithium ion batteries

    Energy Technology Data Exchange (ETDEWEB)

    Hamid, NoorAshrina Binti A.

    2013-07-03

    Lithium ion batteries are one of the most enthralling rechargeable energy storage systems for portable application due to their high energy density. Nevertheless, with respect to electromobility innovation towards better electrochemical properties such as higher energy and power density is required. Altering the cathode material used in Li-ion batteries is favorable since the mass- and volume performance is closely related to the cathode electrode mass. Instead of using LiCoO{sub 2} as cathode electrode, LiFePO{sub 4} has gained serious attention as this material owns a high theoretical capacity of 170 mAh g{sup -1}. It is non-toxic, cheap and consists of abundant materials but suffers from low electronic and ionic conductivity. Utilization of nanotechnology methods in combination with composite formation is known to cure this problem effectively. In this work, a new combination of techniques using highly scalable gas-phase synthesis namely spray-flame synthesis and subsequent solid-state reaction has been used to synthesize nanocomposite LiFePO{sub 4}/C. At first this work deals with the formation and characterization of nanosize FePO{sub 4} from a solution of iron(III)acetylacetonate and tributyl phosphate in toluene using spray-flame synthesis. It was shown that a subsequent solid state reaction with Li{sub 2}CO{sub 3} and glucose yielded a LiFePO{sub 4}/C nanocomposite with very promising electrochemical properties. Based on these initial findings the influence of two synthesis parameter - carbon content and annealing temperature - was investigated towards the physicochemical properties of LiFePO{sub 4}/C. It was shown that an annealing temperature of 700 C leads to high purity composite materials consisting of crystalline LiFePO{sub 4} with crystallite sizes well below 100 nm and amorphous carbon consisting of disordered and graphite-like carbon. Variation of glucose amount between 10 and 30 wt% resulted in carbon contents between 2.1 and 7.3 wt%. In parallel

  11. Comparing particles for radiosynovectomy labeled with Ho-166

    International Nuclear Information System (INIS)

    Argueelles, M.G.; Luppi Berlanga, I.S.; Torres, E.A.; Pereyra Molina, V.

    2002-01-01

    Aim: Three types of microparticles containing Ho-166 were investigated as potential agents for radiation synovectomy. These are: hydroxyapatite (HA), ferric hydroxide macro-aggregates (FHMA) and polymeric micro-spheres (PM). Labeling was performed by three different methods: coprecipitation, two steps labeling using citrate and irradiation of Ho-165 complexed to acetylacetone (AcAc) incorporated into poly-L-lactic acid spheres (PLA) by the solvent evaporation technique. Material and methods: a coprecipitation technique of holmium hydroxide and ferric hydroxide was used in order to obtain 166 Ho-FHMA. Particle size was determined by optical microscopy and selective filtration (1.2 - 100 μm). Obtainment efficiency of FHMA was always higher than 90%. Radiochemical purity was checked by thin layer chromatography using ITLC/SG and EDTA solution as solvent. In vitro stability studies were performed by incubating labelled particles in either saline, or EDTA solution. Hydroxyapatite particles were prepared from the reaction of calcium nitrate and ammonia phosphate at high pH. By strong heating of the precipitate at 800 0 C, the product becomes largely anhydrous and hardened. The yield of the hydroxyapatite synthesis was always greater than 80%. Particle size range was studied using light microscopy. Labeling was done in two steps: 166Ho-citrate was prepared by adding sufficient citric acid to the 166 Ho-Cl 3 solution. The radioactive solution was added to the particulate suspension stirring continuously. Radiolabelled particles were rinsed and separated by centrifugation. Stable Ho-165, complexed to acetylacetone (AcAc), was incorporated into PLA spheres by the solvent evaporation technique. The particle size distribution of the micro-spheres was determined by electronic microscopy. A X-ray fluorescence technique was used to determine the percentage of 165 Ho-AcAc incorporated in the microspheres by studying standards and prepared PLA spheres. Stability studies were

  12. Free radical transfer in polymers

    International Nuclear Information System (INIS)

    Sonntag, C. von; Bothe, E.; Ulanski, P.

    1998-01-01

    For the present study of free-radical transfer in polymers pulse radiolysis and product studies have been carried out in aqueous solutions using thus far only the water-soluble polymers polyacrylic acid, polymethacrylic acid and polyvinyl alcohol. When OH radicals, generated in the radiolysis of N 2 O-saturated aqueous solutions, react with polymers the lifetime of the polymer radical thus created very much depends on the number of radicals per polymer chain. When there are a large number of radicals per chain their bimolecular decay may be faster than the corresponding (diffusion controlled) decay of monomeric radicals, but when the macromolecule contains only few or even just one radical their lifetime is considerably prolonged. Highly charged polymers such as polyacrylic acid at high pH attain a rod-like conformation which again favors a long lifetime of the radicals. Under such conditions, radical transfer reactions can occur. For example, in polyacrylic acid OH radicals generate two kinds of radicals side by side. The radical in β-position to the carboxylate group converts into the thermodynamically more stable α-radicals by an H-transfer reaction as can be followed by spectrophotometry. Besides radical transfer reactions β-fragmentation reactions occur causing chain scission. Such reactions can be followed in a pulse radiolysis experiment by conductometry, because counter ions are released upon chain scission. Such a process is especially effective in the case of polymethacrylic acid, where it results in a chain depolymerization. An intramolecular H-abstraction is also observed in the γ-radiolysis of polyacrylic acid with the corresponding peroxyl radicals. This causes a chain reaction to occur. The resulting hydroperoxides are unstable and decarboxylate given rise to acetylacetone-like products. In polyvinyl alcohol the peroxyl radicals in α-position to the alcohol function undergo HO 2 -elimination. This prevents a scission of the polymer chain in the

  13. Coordination Chemistry Inside Polymeric Nanoreactors: Interparticle Metal Exchange and Ionic Compound Vectorization in Phosphine-Functionalized Amphiphilic Polymer Latexes.

    Science.gov (United States)

    Chen, Si; Gayet, Florence; Manoury, Eric; Joumaa, Ahmad; Lansalot, Muriel; D'Agosto, Franck; Poli, Rinaldo

    2016-04-25

    Stable latexes of hierarchically organized core-cross-linked polymer micelles that are functionalized at the core with triphenylphosphine (TPP@CCM) have been investigated by NMR spectroscopic analysis at both natural (ca. pH 5) and strongly basic (pH 13.6) pH values after core swelling with toluene. The core-shell interface structuring forces part of the hydrophilic poly(ethylene oxide) (PEO) chains to reside inside the hydrophobic core at both pH values. Loading the particle cores with [Rh(acac)(CO)2 ] (acac=acetylacetonate) at various Rh/P ratios yielded polymer-supported [Rh(acac)(CO)(TPP)] (TPP=triphenylphosphine). The particle-to-particle rhodium migration is very fast at natural pH, but slows down dramatically at high pH, whereas the size distribution of the nanoreactors remains unchanged. The slow migration at pH 13.6 leads to the generation of polymer-anchored [Rh(OH)(CO)(TPP)2 ], which is also generated immediately upon the addition of NaOH to the particles with a [Rh(acac)(CO)] loading of 50 %. Similarly, treatment of the same particles with NaCl yielded polymer-anchored [RhCl(CO)(TPP)2 ]. Interparticle coupling occurs during these rapid processes. These experiments prove that the major contribution to metal migration is direct core-core contact. The slow migration at the high pH value, however, must result from a pathway that does not involve core-core contact. The facile penetration of the polymer cores by NaOH and NaCl results from the presence of shell-linked poly(ethylene oxide) methyl ether functions both outside and inside the polymer core-shell interface. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  14. Mixed (phthalocyaninato)(Schiff-base) di-dysprosium sandwich complexes. Effect of magnetic coupling on the SMM behavior.

    Science.gov (United States)

    Wang, Hailong; Liu, Chenxi; Liu, Tao; Zeng, Suyuan; Cao, Wei; Ma, Qi; Duan, Chunying; Dou, Jianmin; Jiang, Jianzhuang

    2013-11-21

    Reaction between Schiff-base ligand and half-sandwich complex M(Pc)(acac) led to the isolation of new sandwich-type mixed (phthalocyaninato)(Schiff-base) di-lanthanide compounds M2(Pc)2(L)H2O (M = Dy, Gd) (1, 2) [H2Pc = metal free phthalocyanine, Hacac = acetylacetone, H2L = N,N'-bis(3-methyloxysalicylidene)benzene-1,2-diamine] with the triple-decker molecular structure clearly revealed by single crystal X-ray diffraction analysis. For the comparative studies, sandwich triple-decker analogues with pure Schiff-base ligand M2(L)3H2O (M = Dy, Gd) (3, 4) were also prepared. Dynamic magnetic measurement result reveals the single-molecule magnet (SMM) nature of the di-dysprosium derivative 1, while the static magnetic investigation over both pure and the diamagnetic diluted samples of this compound discloses the interionic ferromagnetic coupling between the two dysprosium ions, which in turn effectively suppresses the QTM and enhances the energy barrier of this SMM. Nevertheless, comparative studies over the static magnetic properties of the di-dysprosium triple-decker complexes 1 and 3 indicate the stronger magnetic coupling between the two lanthanide ions in mixed (phthalocyaninato)(Schiff-base) species than in the pure Schiff-base triple-decker analogue, suggesting the special coordination sphere around the dysprosium ions in the former compound over the latter one on the more intense inter-ionic ferromagnetic coupling. As a very small step towards understanding the structure-property relationship, the present result will be surely helpful for the design and synthesis of the multinuclear lanthanide-based SMMs with good properties.

  15. Influence of different TiO2 blocking films on the photovoltaic performance of perovskite solar cells

    Science.gov (United States)

    Zhang, Chenxi; Luo, Yudan; Chen, Xiaohong; Ou-Yang, Wei; Chen, Yiwei; Sun, Zhuo; Huang, Sumei

    2016-12-01

    Organolead trihalide perovskite materials have been successfully used as light absorbers in efficient photovoltaic (PV) cells. Cell structures based on mesoscopic metal oxides and planar heterojunctions have already demonstrated very impressive and brisk advances, holding great potential to grow into a mature PV technology. High power conversion efficiency (PCE) values have been obtained from the mesoscopic configuration in which a few hundred nano-meter thick mesoporous scaffold (e.g. TiO2 or Al2O3) infiltrated by perovskite absorber was sandwiched between the electron and hole transport layers. A uniform and compact hole-blocking layer is necessary for high efficient perovskite-based thin film solar cells. In this study, we investigated the characteristics of TiO2 compact layer using various methods and its effects on the PV performance of perovskite solar cells. TiO2 compact layer was prepared by a sol-gel method based on titanium isopropoxide and HCl, spin-coating of titanium diisopropoxide bis (acetylacetonate), screen-printing of Dyesol's bocking layer titania paste, and a chemical bath deposition (CBD) technique via hydrolysis of TiCl4, respectively. The morphological and micro-structural properties of the formed compact TiO2 layers were characterized by scanning electronic microscopy and X-ray diffraction. The analyses of devices performance characteristics showed that surface morphologies of TiO2 compact films played a critical role in affecting the efficiencies. The nanocrystalline TiO2 film deposited via the CBD route acts as the most efficient hole-blocking layer and achieves the best performance in perovskite solar cells. The CBD-based TiO2 compact and dense layer offers a small series resistance and a large recombination resistance inside the device, and makes it possible to achieve a high power conversion efficiency of 12.80%.

  16. Cobalt(II Complexes with N,N,N-Scorpionates and Bidentate Ligands: Comparison of Hydrotris(3,5-dimethylpyrazol-1-ylborate Tp* vs. Phenyltris(4,4-dimethyloxazolin-2-ylborate ToM to Control the Structural Properties and Reactivities of Cobalt Centers

    Directory of Open Access Journals (Sweden)

    Toshiki Nishiura

    2018-06-01

    Full Text Available Scorpionate ligands Tp* (hydrotris(3,5-dimethylpyrazol-1-ylborate and ToM (tris(4,4-dimethyloxazolin-2-ylphenylborate complexes of cobalt(II with bidentate ligands were synthesized. Both Tp* and ToM coordinate to cobalt(II in a tridentate fashion when the bidentate ligand is the less hindered acetylacetonate. In crystal structures, the geometry of cobalt(II supported by the N3O2 donor set in the Tp* complex is a square-pyramid, whereas that in the ToM complex is close to a trigonal-bipyramid. Both Tp*- and ToM-acac complexes exhibit solvatochromic behavior, although the changing structural equilibria of these complexes in MeCN are quite different. In the bis(1-methylimidazol-2-ylmethylphenylborate (LPh complexes, Tp* retains the tridentate (к3 mode, whereas ToM functions as the bidentate (к2 ligand, giving the tetrahedral cobalt(II complex. The bowl-shaped cavity derived from the six methyl groups on ToM lead to susceptibility to the bulkiness of the opposite bidentate ligand. The entitled scorpionate compounds mediate hydrocarbon oxidation with organic peroxides. Allylic oxidation of cyclohexene occurs mainly on the reaction with tert-butyl hydroperoxide (TBHP, although the catalytic efficiency of the scorpionate ligand complexes is lower than that of Co(OAc2 and Co(acac2. On cyclohexane oxidation with meta-chloroperbenzoic acid (mCPBA, both ToM and Tp* complexes function as catalysts for hydroxylation. The higher electron-donating ToM complexes show faster initial reaction rates compared to the corresponding Tp* complexes.

  17. TiO2 nanoparticles for enhancing the refractive index of hydrogels for ophthalmological applications

    Science.gov (United States)

    Hampp, Norbert; Dams, Christian; Badur, Thorben; Reinhardt, Hendrik

    2017-02-01

    Intraocular lenses (IOL) are currently the only treatment for cataract dependent vision impairment and blindness [1]. A polymer suitable for IOL manufacture needs to meet a plurality of properties, biocompatibility, excellent transmission in the visible range, a high flexibility for micro invasive surgery, a high refractive index as well as a good ABBE-number, just to mention the most important ones [2]. We present the use of in situ generated TiO2-nanoparticles to enhance the refractive index of poly-HEMA hydrogels - with are suitable polymers for IOL manufacture[3] - from 1.44 to 1.527 at 589.3 nm combined with an excellent ABBE-number of 54. The nanoparticles were prepared using titaniumdiisopropoxide- bis(acetylacetonate) as a precursor. First the titanium salt was diffused into the poly-HEMA matrix and then it was transformed into TiO2 in boiling water. The resulting pHEMA [TiO2] hydrogel was dried for 10 days under ambient conditions. By lathing these polymers were machined into lens precursors, the so-called Saturn-rings. After reswelling in physiological saline solutions flexible polymer lenses with high surface quality, shape memory and superior optical properties were obtained. The crystal structure of the formed TiO2 nanoparticles was identified as anatase via Xray. No release of titanium ions or TiO2 nanoparticles was observe under physiological conditions. Such hybrid materials of TiO2 nanoparticles and poly-HEMA like hydrogels are promising materials for IOL.

  18. Formation of inorganic nanocomposites by filling TiO{sub 2} nanopores with indium and antimony sulfide precursor aerosols

    Energy Technology Data Exchange (ETDEWEB)

    Juma, Albert, E-mail: jumalberto@yahoo.com [Helmholtz-Zentrum Berlin für Materialien und Energie, Hahn-Meitner-Platz 1, 14109 Berlin (Germany); Azarpira, Anahita [Helmholtz-Zentrum Berlin für Materialien und Energie, Hahn-Meitner-Platz 1, 14109 Berlin (Germany); Fischer, Ch.-H. [Helmholtz-Zentrum Berlin für Materialien und Energie, Hahn-Meitner-Platz 1, 14109 Berlin (Germany); Free University Berlin, Institute of Chemistry and Biochemistry, Fabeckstr. 34-36, 14195 Berlin (Germany); Wendler, Elke [Friedrich-Schiller-Universität Jena, Institut für Festkörperphysik, Max-Wien-Platz 1, 07743 Jena (Germany); Dittrich, Thomas [Helmholtz-Zentrum Berlin für Materialien und Energie, Hahn-Meitner-Platz 1, 14109 Berlin (Germany)

    2014-09-01

    Nanocomposites of nanoporous-TiO{sub 2}/In{sub 2}S{sub 3} and np-TiO{sub 2}/Sb{sub 2}S{sub 3} were formed by deposition of In{sub 2}S{sub 3} or Sb{sub 2}S{sub 3} using spray ion layer gas reaction technique from their precursor solutions onto nanoporous TiO{sub 2} substrates at temperatures of 150, 175 and 200 °C. The least penetration of the precursor into np-TiO{sub 2} was achieved for np-TiO{sub 2}/In{sub 2}S{sub 3} nanocomposites from indium acetylacetonate salt. The deepest penetration was obtained for both np-TiO{sub 2}/In{sub 2}S{sub 3}(Cl) and np-TiO{sub 2}/Sb{sub 2}S{sub 3} nanocomposites with effective diffusion coefficients of 3.3 × 10{sup −3} cm{sup 2}/s and 3.2 × 10{sup −3} cm{sup 2}/s, respectively. The transport of the precursors in np-TiO{sub 2} and the formation of different nanocomposites were described the regime of the Knudsen diffusion model. - Highlights: • Deposition of metal sulfides by ion layer gas reaction technique • Penetration and diffusion depend on precursor characteristics. • Pore transport described by Knudsen diffusion model • InCl{sub 3} precursor penetrates more than In(acac){sub 3}.

  19. On the optical, structural, and morphological properties of ZrO2 and TiO2 dip-coated thin films supported on glass substrates

    International Nuclear Information System (INIS)

    Cueto, Luisa F.; Sanchez, Enrique; Torres-Martinez, Leticia M.; Hirata, Gustavo A.

    2005-01-01

    This article reports the optical and morphological properties of dip-coated TiO 2 and ZrO 2 thin films on soda-lime glass substrates by metal-organic decomposition (MOD) of titanium IV and zirconium IV acetylacetonates respectively. Thermogravimetric and differential thermal analysis (DTA-TG) were performed on the precursor powders, indicating pure TiO 2 anatase and tetragonal ZrO 2 phase formation. Phase crystallization processes took place in the range of 300-500 deg. C for anatase and of 410-500 deg. C for ZrO 2 . Fourier Transform Infrared Spectroscopy (FT-IR) was used to confirm precursor bidentate ligand formation with keno-enolic equilibrium character. Deposited films were heated at different temperatures, and their structural, optical and morphological properties were studied by grazing-incidence X-ray Diffraction (GIXRD) and X-Ray Photoelectron Spectroscopy (XPS), Ultraviolet Visible Spectroscopy (UV-Vis), and Atomic Force Microscopy (AFM) respectively. Film thinning and crystalline phase formation were enhanced with increasing temperature upon chelate decomposition. The optimum annealing temperature for both pure anatase TiO 2 and tetragonal ZrO 2 thin films was found to be 500 deg. C since solid volume fraction increased with temperature and film refractive index values approached those of pure anatase and tetragonal zirconia. Conditions for clean stoichiometric film formation with an average roughness value of 2 nm are discussed in terms of material binding energies indicated by XPS analyses, refractive index and solid volume fraction obtained indirectly by UV-Vis spectra, and crystalline peak identification provided by GIXRD

  20. High-capacity cathodes for lithium-ion batteries from nanostructured LiFePO4 synthesized by highly-flexible and scalable flame spray pyrolysis

    Science.gov (United States)

    Hamid, N. A.; Wennig, S.; Hardt, S.; Heinzel, A.; Schulz, C.; Wiggers, H.

    2012-10-01

    Olivine, LiFePO4 is a promising cathode material for lithium-ion batteries due to its low cost, environmental acceptability and high stability. Its low electric conductivity prevented it for a long time from being used in large-scale applications. Decreasing its particle size along with carbon coating significantly improves electronic conductivity and lithium diffusion. With respect to the controlled formation of very small particles with large specific surface, gas-phase synthesis opens an economic and flexible route towards high-quality battery materials. Amorphous FePO4 was synthesized as precursor material for LiFePO4 by flame spray pyrolysis of a solution of iron acetylacetonate and tributyl phosphate in toluene. The pristine FePO4 with a specific surface from 126-218 m2 g-1 was post-processed to LiFePO4/C composite material via a solid-state reaction using Li2CO3 and glucose. The final olivine LiFePO4/C particles still showed a large specific surface of 24 m2 g-1 and were characterized using X-ray diffraction (XRD), electron microscopy, X-ray photoelectron spectrocopy (XPS) and elemental analysis. Electrochemical investigations of the final LiFePO4/C composites show reversible capacities of more than 145 mAh g-1 (about 115 mAh g-1 with respect to the total coating mass). The material supports high drain rates at 16 C while delivering 40 mAh g-1 and causes excellent cycle stability.

  1. Solution-Processed Ultrathin TiO2 Compact Layer Hybridized with Mesoporous TiO2 for High-Performance Perovskite Solar Cells.

    Science.gov (United States)

    Jeong, Inyoung; Park, Yun Hee; Bae, Seunghwan; Park, Minwoo; Jeong, Hansol; Lee, Phillip; Ko, Min Jae

    2017-10-25

    The electron transport layer (ETL) is a key component of perovskite solar cells (PSCs) and must provide efficient electron extraction and collection while minimizing the charge recombination at interfaces in order to ensure high performance. Conventional bilayered TiO 2 ETLs fabricated by depositing compact TiO 2 (c-TiO 2 ) and mesoporous TiO 2 (mp-TiO 2 ) in sequence exhibit resistive losses due to the contact resistance at the c-TiO 2 /mp-TiO 2 interface and the series resistance arising from the intrinsically low conductivity of TiO 2 . Herein, to minimize such resistive losses, we developed a novel ETL consisting of an ultrathin c-TiO 2 layer hybridized with mp-TiO 2 , which is fabricated by performing one-step spin-coating of a mp-TiO 2 solution containing a small amount of titanium diisopropoxide bis(acetylacetonate) (TAA). By using electron microscopies and elemental mapping analysis, we establish that the optimal concentration of TAA produces an ultrathin blocking layer with a thickness of ∼3 nm and ensures that the mp-TiO 2 layer has a suitable porosity for efficient perovskite infiltration. We compare PSCs based on mesoscopic ETLs with and without compact layers to determine the role of the hole-blocking layer in their performances. The hybrid ETLs exhibit enhanced electron extraction and reduced charge recombination, resulting in better photovoltaic performances and reduced hysteresis of PSCs compared to those with conventional bilayered ETLs.

  2. Chemically fabricated LiFePO{sub 4} thin film electrode for transparent batteries and electrochromic devices

    Energy Technology Data Exchange (ETDEWEB)

    Béléké, Alexis B. [Institut de recherche d’Hydro-Québec, 1800 Boul. Lionel-Boulet, Varennes, QC J3X 1S3 (Canada); Department of Mining and Materials Engineering, McGill University, M.H. Wong Building, 3610 rue University, Montréal, QC H3A 2B2 (Canada); Faure, Cyril [Institut de recherche d’Hydro-Québec, 1800 Boul. Lionel-Boulet, Varennes, QC J3X 1S3 (Canada); Röder, Manuel [Center for Applied Electrochemistry, Fraunhofer Institute for Silicate Research, Neunerplatz 2, 97083 Würzburg (Germany); Hovington, Pierre [Institut de recherche d’Hydro-Québec, 1800 Boul. Lionel-Boulet, Varennes, QC J3X 1S3 (Canada); Posset, Uwe [Center for Applied Electrochemistry, Fraunhofer Institute for Silicate Research, Neunerplatz 2, 97083 Würzburg (Germany); Guerfi, Abdelbast [Institut de recherche d’Hydro-Québec, 1800 Boul. Lionel-Boulet, Varennes, QC J3X 1S3 (Canada); Zaghib, Karim, E-mail: zaghib.karim@ireq.ca [Institut de recherche d’Hydro-Québec, 1800 Boul. Lionel-Boulet, Varennes, QC J3X 1S3 (Canada)

    2016-12-15

    Graphical abstract: Simplified diagram of the novel sol-gel approach of preparation of colorless and transparent LiFePO{sub 4} thin film electrode. - Highlights: • Novel sol-gel synthesis of colorless LFP thin film electrode for transparent Li-ion battery. • High performance of the electrode at various current densities: 5, 10, 20, 50 and 100 μA/cm{sup 2}. • LFP nanoparticles exhibit an excellent electro-activity. • Colorless LFP thin film shows a transmittance above 80% versus FTO. • Higher transmittance of LFP electrode a potential candidate for electrochromic devices. - Abstract: We report a new sol-gel approach of synthesis of LiFePO{sub 4} (LFP) thin film and its application as cathode materials for transparent Li-ion battery in half-cell configuration. LFP thin films were obtained from an alcoholic colloidal suspension of iron acetylacetonate (Fe(AcAc){sub 3}) and aqueous lithium dihydrogen phosphate (LiH{sub 2}PO{sub 4}) deposited on fluorine tin oxide (FTO) glass substrate, followed by heating at 450 °C under nitrogen gas for 1 h. X-ray diffraction (XRD) confirmed that the LFP films have an orthorhombic crystal system with space group Pnma (62). Scanning electron microscopy (SEM) shows spherical LFP nanoparticles aggregates homogenously deposited all over the surface of FTO substrate containing 3-D open pores. The electrochemical behaviors of thin film vs Li/Li{sup +} cell were investigated by cyclic voltammetry and galvanostatic charge-discharge measurements. The cycle life was evaluated by running 1000 cycles of charge-discharge at a current density of 20 μA/cm{sup 2}. The transmission spectra reveal 85–90% of transparency versus FTO as reference, which makes it a potential candidate as a complementary electrode in electrochromic devices (ECDs).

  3. Synthesis and fabrication of Y{sub 2}O{sub 3}:Tb{sup 3+} and Y{sub 2}O{sub 3}:Eu{sup 3+} thin films for electroluminescent applications: Optical and structural characteristics

    Energy Technology Data Exchange (ETDEWEB)

    Alarcón-Flores, G., E-mail: alar_fbeto@yahoo.com [Centro de Investigación en Ciencia Aplicada y Tecnología Avanzada, IPN, Legaría 694, Irrigación, C.P. 11500, México D.F. (Mexico); García-Hipólito, M. [Instituto de Investigaciones en Materiales, UNAM, Apdo. Postal 70-360, Delegación Coyoacán, C.P. 04150, México D.F. (Mexico); Aguilar-Frutis, M. [Centro de Investigación en Ciencia Aplicada y Tecnología Avanzada, IPN, Legaría 694, Irrigación, C.P. 11500, México D.F. (Mexico); Carmona-Téllez, S. [Instituto de Física, UNAM, Coyoacán, C.P. 04150, México D.F. (Mexico); Martinez-Martinez, R. [Universidad Tecnológica de la Mixteca, Carretera Acatlima Km 2.5, Huajuapan de León Oaxaca, C.P. 69000, México (Mexico); Campos-Arias, M.P. [Centro de Investigación en Ciencia Aplicada y Tecnología Avanzada, IPN, Legaría 694, Irrigación, C.P. 11500, México D.F. (Mexico); Zaleta-Alejandre, E. [Universidad Autónoma del Estado de Hidalgo-Escuela Superior de Apan, Carretera Apan-Calpulalpan Km. 8, C.P. 43920, Apan, Hidalgo (Mexico); and others

    2015-01-15

    Terbium, europium and yttrium β diketonates have been synthesized from acetylacetone and inorganic metal salts and used as precursors for the deposition of Tb{sup 3+} or Eu{sup 3+} doped Y{sub 2}O{sub 3} polycrystalline films by the ultrasonic spray pyrolysis technique. The films were deposited on c-Si substrates at temperatures in the 400–550 °C range. The optical and structural characterization of these films as a function of substrate temperature and Tb{sup 3+} and Eu{sup 3+} concentration was carried out by means of photoluminescence (PL), cathodoluminescence (CL), infrared (IR), ellipsometry, and UV–visible spectroscopy and atomic force microscopy (AFM), energy dispersive spectroscopy (EDS) and X ray diffraction (XRD) measurements respectively. The PL intensity from these films was found to depend on deposition temperature. Films deposited above 450 °C exhibited the characteristic PL peaks associated with either Tb{sup 3+} or Eu{sup 3+} intra electronic energy levels transitions. The most intense PL emission was found for dopant concentration of 10 at% for Tb{sup 3+} and at 8 at% for Eu{sup 3+} ions into precursor solution. In both cases concentration quenching of the PL emission was observed for concentrations above these values. The films had a refractive index (1.81), low average surface roughness (∼62 Å) and a UV–Vis. transmission of the order of 90 %T. - Highlights: • Terbium, europium and yttrium β diketonates have been synthesized. • Luminescent thin films of Y{sub 2}O{sub 3}:Tb{sup 3+} and Y{sub 2}O{sub 3}:Eu{sup 3+} were obtained. • Optical and structural characteristics of these thin films are presented. • The films had a refractive index (1.81) and low average surface roughness (∼62 Å)

  4. Dysprosium complexes with the tetraphenylporphyrin macrocyclic ligand; Complejos de disprosio con el ligante macrociclico tetrafenilporfirina

    Energy Technology Data Exchange (ETDEWEB)

    Martinez M, V.; Padilla, J.; Ramirez, F.M

    1992-04-15

    In this report, the results obtained on the synthesis, characterization and study of the chemical behavior of dysprosium complex with the acetylacetone chelating agent (Hacac) and the tetraphenylporphyrin macrocyclic ligand (H{sub 2}TFP) are given. Based on the literature but according to our necessities and interest, the appropriate methodology settled down from the synthesis of prime matters until the obtaining and characterization of the products. The acetyl acetonate complex was obtained of mono hydrated dysprosium [Dy(acac){sub 3}. H{sub 2}0] and trihydrated [Dy(acac){sub 3} .3 H{sub 2}0], the mono tetra phenyl porphyrinate [Dy(TFP)(acac). 2 ac] the double sandwich of the dysprosium porphyrinate [Dy(TFP){sub 2}] and the triple sandwich of the dysprosium porphyrinate [Dy(TFP){sub 3}. 2 TCB] (TCB = trichlorobenzene). Its were characterized by their melting points, solubility, IR, UV, TGA and DTA both first and besides the techniques already mentioned for NMR'H, RPE and Magnetic susceptibility the three last complexes. From the spectroscopic point of view, IR and RPE its suggested the existence of a complex of inverse mixed valence [Dy(TFP){sup 2-} (TFP) {sup 1-}] for the Dy(TFP){sub 2} as a result of the existence of the free radical (TFP' {sup 1-} and that it was not in none of the other porphyrin compounds. In the NMR'H spectra of the compounds were not observed signals in the region from 0 to 10 ppm that which shows that the dysprosium complexes in special those of the porphyrin type are highly paramagnetic and its could be used as displacement reagents, creators of images and contrast agents of great utility in these days in studies of NMR, technique today by today used in medical diagnoses. (Author)

  5. 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

  6. Thorium/uranium mixed oxide nano-crystals: Synthesis, structural characterization and magnetic properties

    International Nuclear Information System (INIS)

    Hudry, Damien; Griveau, Jean-Christophe; Apostolidis, Christos; Colineau, Eric; Rasmussen, Gert; Walter, Olaf; Wang, Di; Venkata Sai Kiran Chakravadhaluna; Courtois, Eglantine; Kubel, Christian

    2014-01-01

    One of the primary aims of the actinide community within nano-science is to develop a good understanding similar to what is currently the case for stable elements. As a consequence, efficient, reliable and versatile synthesis techniques dedicated to the formation of new actinide-based nano-objects (e.g., nano-crystals) are necessary. Hence, a 'library' dedicated to the preparation of various actinide based nano-scale building blocks is currently being developed. Nano-scale building blocks with tunable sizes, shapes and compositions are of prime importance. So far, the non-aqueous synthesis method in highly coordinating organic media is the only approach which has demonstrated the capability to provide size and shape control of actinide-based nano-crystals (both for thorium and uranium, and recently extended to neptunium and plutonium). In this paper, we demonstrate that the non-aqueous approach is also well adapted to control the chemical composition of the nano-crystals obtained when mixing two different actinides. Indeed, the controlled hot co-injection of thorium acetylacetonate and uranyl acetate (together with additional capping agents) into benzyl ether can be used to synthesize thorium/uranium mixed oxide nano-crystals covering the full compositional spectrum. Additionally, we found that both size and shape are modified as a function of the thorium/uranium ratio. Finally, the magnetic properties of the different thorium/uranium mixed oxide nano-crystals were investigated. Contrary to several reports, we did not observe any ferromagnetic behavior. As a consequence, ferromagnetism cannot be described as a universal feature of nano-crystals of non-magnetic oxides as recently claimed in the literature. (authors)

  7. Epoxidación de aceite de soja refinado mediante oxígeno molecular. Influencia de las variables. Estudio cinético

    Directory of Open Access Journals (Sweden)

    Martínez de la Cuesta, P. J.

    1991-02-01

    Full Text Available The influences of temperature, concentration of catalyst and initial concentration of unsaturation on epoxide formation and esters from oleic and linoleic acids disappearance in liquid phase epoxidation reaction by molecular oxygen of soy-bean oil using molibdenyl-acetylacetonate as catalyst, has been studied. From experimental data obtained by a complex factorial design, an equation for epoxide formation reaction rate as a function of temperature, catalyst concentration and unsaturation initial concentration were deduced. A kinetic model is proposed too and using a calculation program based on 4th Order Runge-Kutta numerical procedure to simulate the reactions that took place, the kinetic coefficients and activation energies that best fitted the calculated data to the experimental data were determined.

    Se ha estudiado la influencia de la temperatura, concentración de catalizador y concentración inicial de insaturación sobre la formación de epóxido y desaparición de los esteres de los ácidos oleico y linoleico, en la reacción de epoxidación en fase líquida de aceite de soja con oxígeno molecular usando acetilacetonato de molibdenilo (AAMo como catalizador. A partir de los datos, obtenidos según un diseño factorial complejo, se ha deducido una ecuación para la velocidad de formación de epóxido en función de las tres variables estudiadas. Se propone también un modelo cinético a partir del cual, y siguiendo el método numérico de Runge-Kutta que simula la reacción que tiene lugar, se determinan los valores de las constantes cinéticas y respectivas energías de activación.

  8. The Effect of Precursor Ligands and Oxidation State in the Synthesis of Bimetallic Nano-Alloys

    KAUST Repository

    LaGrow, Alec P.

    2015-05-12

    The characteristics of bimetallic nanomaterials are dictated by their size, shape and elemental distribution. Solution synthesis is widely utilized to form nanomaterials, such as nanoparticles, with controlled size and shape. However, the effects of variables on the characteristics of bimetallic nanomaterials are not completely understood. In this study, we used a continuous-flow synthetic strategy to explore the effects of the ligands and the oxidation state of a metal precursor in a shape-controlled synthesis on the final shape of the nanomaterials and the elemental distribution within the alloy. We demonstrate that this strategy can tune the size of monodisperse PtM (M=Ni or Cu) alloy nanocrystals ranging from 3 to 16 nm with an octahedral shape using acetylacetonate or halide precursors of Pt(II), Pt(IV) and Ni or Cu (II). The nanoparticles formed from halide precursors showed an enrichment of platinum on their surfaces, and the bromides could oxidatively etch the nanoparticles during synthesis with the O2/Br- pair. The two nanocrystal precursors can be uti-lized independently and can control the size with a trend of Pt(acac)2

  9. Moessbauer studies of SnO2 powders doped with dilute 57Fe, prepared by a sol-gel method

    International Nuclear Information System (INIS)

    Nomur, K.; Sakuma, J.; Takeda, M.

    2006-01-01

    Diluted magnetic semiconductor (DMS) is prospected as new materials with both semiconductor and magnetic properties. In order to confirm these phenomena, we prepared the powders of SnO 2 doped with various amount of 57 Fe by a sol-gel method. Various compositions of Sn 1-x 57 Fe x O 2 were obtained by mixing some ratio of Fe 3+ nitrate solution and acetylacetonate Sn 4+ complex in the ethylene glycol and citric acid solution. The solutions were evaporated, ashed at around 200 grad C, and finally annealed at 500 grad C, 600 grad C, and 650 grad C, respectively. These Sn 1-x 57 Fe x O 2 (x=0.005, 0.01, 0.03 and 0.05) were measured by XRD, VSM, and Moessbauer spectrometry. The prepared powder samples were confirmed to be a rutile structure, but iron compounds were not detected by XRD. Moessbauer spectra of Sn 1-x 57 Fe x O 2 prepared at 500 grad C were shown in Fig. 1. A small amount of broad sextets were observed in MS spectra of Sn 1-x 57 Fe x O 2 in addition to paramagnetic components. The relative intensity seems to be strong with the decrease of the amount of doped Fe. Moessbauer spectrum at 10 K shows clearly the magnetic components. The magnetic sextet was observed in MS spectra of samples prepared at 650 grad C, but the magnetic behavior weakened because of antiferromagnetic α-Fe 2 O 3 , produced due to the phase separation at high temperatures. (authors)

  10. Chemical vapor deposition (CVD) of uranium for alpha spectrometry

    International Nuclear Information System (INIS)

    Ramirez V, M. L.; Rios M, C.; Ramirez O, J.; Davila R, J. I.; Mireles G, F.

    2015-09-01

    The uranium determination through radiometric techniques as alpha spectrometry requires for its proper analysis, preparation methods of the source to analyze and procedures for the deposit of this on a surface or substrate. Given the characteristics of alpha particles (small penetration distance and great loss of energy during their journey or its interaction with the matter), is important to ensure that the prepared sources are thin, to avoid problems of self-absorption. The routine methods used for this are the cathodic electro deposition and the direct evaporation, among others. In this paper the use of technique of chemical vapor deposition (CVD) for the preparation of uranium sources is investigated; because by this, is possible to obtain thin films (much thinner than those resulting from electro deposition or evaporation) on a substrate and comprises reacting a precursor with a gas, which in turn serves as a carrier of the reaction products to achieve deposition. Preliminary results of the chemical vapor deposition of uranium are presented, synthesizing and using as precursor molecule the uranyl acetylacetonate, using oxygen as carrier gas for the deposition reaction on a glass substrate. The uranium films obtained were found suitable for alpha spectrometry. The variables taken into account were the precursor sublimation temperatures and deposition temperature, the reaction time and the type and flow of carrier gas. Of the investigated conditions, two depositions with encouraging results that can serve as reference for further work to improve the technique presented here were selected. Alpha spectra obtained for these depositions and the characterization of the representative samples by scanning electron microscopy and X-ray diffraction are also presented. (Author)

  11. Dry Sintered Metal Coating of Halloysite Nanotubes

    Directory of Open Access Journals (Sweden)

    James C. Nicholson

    2016-09-01

    Full Text Available Halloysite nanotubes (HNTs are a naturally-occurring aluminosilicate whose dimensions measure microns in length and tens of nanometers in diameter. Bonding defects between the alumina and silica lead to net negative and positive charges on the exterior and interior lumen, respectively. HNTs have been shown to enhance the material properties of polymer matrices and enable the sustained release of loaded chemicals, drugs, and growth factors. Due to the net charges, these nanotubes can also be readily coated in layered-depositions using the HNT exterior lumen’s net negative charge as the basis for assembly. These coatings are primarily done through wet chemical processes, the majority of which are limited in their use of desired chemicals, due to the polarity of the halloysite. Furthermore, this restriction in the type of chemicals used often requires the use of more toxic chemicals in place of greener options, and typically necessitates the use of a significantly longer chemical process to achieve the desired coating. In this study, we show that HNTs can be coated with metal acetylacetonates—compounds primarily employed in the synthesis of nanoparticles, as metal catalysts, and as NMR shift reagents—through a dry sintering process. This method was capable of thermally decaying the metal acetylacetonate, resulting in a free positively-charged metal ion that readily bonded to the negatively-charged HNT exterior, resulting in metallic coatings forming on the HNT surface. Our coating method may enable greater deposition of coated material onto these nanotubes as required for a desired application. Furthermore, the use of chemical processes using toxic chemicals is not required, thus eliminating exposure to toxic chemicals and costs associated with the disposal of the resultant chemical waste.

  12. Hybrid white organic light-emitting devices based on phosphorescent iridium-benzotriazole orange-red and fluorescent blue emitters

    Energy Technology Data Exchange (ETDEWEB)

    Xia, Zhen-Yuan, E-mail: xiazhenyuan@hotmail.com [Key Laboratory for Advanced Materials and Institute of Fine Chemicals, East China University of Science and Technology, Shanghai 200237 (China); Su, Jian-Hua [Key Laboratory for Advanced Materials and Institute of Fine Chemicals, East China University of Science and Technology, Shanghai 200237 (China); Chang, Chi-Sheng; Chen, Chin H. [Display Institute, Microelectronics and Information Systems Research Center, National Chiao Tung University, Hsinchu, Taiwan 300 (China)

    2013-03-15

    We demonstrate that high color purity or efficiency hybrid white organic light-emitting devices (OLEDs) can be generated by integrating a phosphorescent orange-red emitter, bis[4-(2H-benzotriazol-2-yl)-N,N-diphenyl-aniline-N{sup 1},C{sup 3}] iridium acetylacetonate, Ir(TBT){sub 2}(acac) with fluorescent blue emitters in two different emissive layers. The device based on deep blue fluorescent material diphenyl-[4-(2-[1,1 Prime ;4 Prime ,1 Double-Prime ]terphenyl-4-yl-vinyl)-phenyl]-amine BpSAB and Ir(TBT){sub 2}(acac) shows pure white color with the Commission Internationale de L'Eclairage (CIE) coordinates of (0.33,0.30). When using sky-blue fluorescent dopant N,N Prime -(4,4 Prime -(1E,1 Prime E)-2,2 Prime -(1,4-phenylene)bis(ethene-2,1-diyl) bis(4,1-phenylene))bis(2-ethyl-6-methyl-N-phenylaniline) (BUBD-1) and orange-red phosphor with a color-tuning phosphorescent material fac-tris(2-phenylpyridine) iridium (Ir(ppy){sub 3} ), it exhibits peak luminance yield and power efficiency of 17.4 cd/A and 10.7 lm/W, respectively with yellow-white color and CIE color rendering index (CRI) value of 73. - Highlights: Black-Right-Pointing-Pointer An iridium-based orange-red phosphor Ir(TBT){sub 2}(acac) was applied in hybrid white OLEDs. Black-Right-Pointing-Pointer Duel- and tri-emitter WOLEDs were achieved with either high color purity or efficiency performance. Black-Right-Pointing-Pointer Peak luminance yield of tri-emitter WOLEDs was 17.4 cd/A with yellow-white color and color rendering index (CRI) value of 73.

  13. High-efficiency white organic light-emitting devices with a non-doped yellow phosphorescent emissive layer

    Energy Technology Data Exchange (ETDEWEB)

    Zhao Juan; Yu Junsheng, E-mail: jsyu@uestc.edu.cn; Hu Xiao; Hou Menghan; Jiang Yadong

    2012-03-30

    Highly efficient phosphorescent white organic light-emitting devices (PHWOLEDs) with a simple structure of ITO/TAPC (40 nm)/mCP:FIrpic (20 nm, x wt.%)/bis[2-(4-tertbutylphenyl)benzothiazolato-N,C{sup 2} Prime ] iridium (acetylacetonate) (tbt){sub 2}Ir(acac) (y nm)/Bphen (30 nm)/Mg:Ag (200 nm) have been developed, by inserting a thin layer of non-doped yellow phosphorescent (tbt){sub 2}Ir(acac) between doped blue emitting layer (EML) and electron transporting layer. By changing the doping concentration of the blue EML and the thickness of the non-doped yellow EML, a PHWOLED comprised of higher blue doping concentration and thinner yellow EML achieves a high current efficiency of 31.7 cd/A and Commission Internationale de l'Eclairage coordinates of (0.33, 0.41) at a luminance of 3000 cd/m{sup 2} could be observed. - Highlights: Black-Right-Pointing-Pointer We introduce a simplified architecture for phosphorescent white organic light-emitting device. Black-Right-Pointing-Pointer The key concept of device fabrication is combination of doped blue emissive layer (EML) with non-doped ultra-thin yellow EML. Black-Right-Pointing-Pointer Doping concentration of the blue EML and thickness of the yellow EML are sequentially adjusted. Black-Right-Pointing-Pointer High device performance is achieved due to improved charge carrier balance as well as two parallel emission mechanisms in the EMLs.

  14. Microspheres of poly(ε-caprolactone) loaded Holmium-165: morphology and thermal degradation behavior

    International Nuclear Information System (INIS)

    Geraldes, Adriana Napoleao; Miyamoto, Douglas Massao; Lira, Raphael Arivar de; Osso Junior, Joao Alberto; Nascimento, Nanci; Azevedo, Mariangela de Burgos M. de

    2011-01-01

    Polycaprolactone (PCL), being one of the most important biocompatible and biodegradable aliphatic polyester, provides many potential biomedical. The preparation of biodegradable materials, polymer-based microspheres, is being developed by our group and the goal is to prepare and label with Ho-165 different polymer-based microspheres. The use of radionuclide-loaded microspheres is a promising treatment of liver malignancies. PCL microspheres can be loaded with holmium acetylacetonate (HoAcAc). PCL and PCL/HoAcAc microspheres were prepared by an emulsion solvent extraction/evaporation technique. The PCL/ HoAcAc microspheres were irradiated in a nuclear reactor IEA-R1 at IPEN/CNEN-SP to radionuclide activation. Gamma irradiation was performed at 25 and 50 kGy doses. The microspheres were evaluated by differential scanning calorimetry analysis (DSC), thermogravimetric analysis (TG), Fourier transformed infrared spectroscopy (FTIR), scanning electron microscopy (SEM) and con focal laser scanning microscopy (CLSM). In the CLSM images were observed emission in 488 nm characteristic of holmium. The SEM surface image of PCL/HoAcAc microspheres showed more roughness than PCL microspheres. TG of PCL/HoAcAc microspheres showed a substantial weight loss above 200 degree C, indicating decomposition of HoAcAc. The residual weight indicates the presence of Ho 2 O 3 . Gamma irradiation at 25 and 50 kGy doses had no effect on the PCL/HoAcAc microspheres, which indicates that the chemical composition of the microspheres had not change. (author)

  15. Microspheres of poly({epsilon}-caprolactone) loaded Holmium-165: morphology and thermal degradation behavior

    Energy Technology Data Exchange (ETDEWEB)

    Geraldes, Adriana Napoleao; Miyamoto, Douglas Massao; Lira, Raphael Arivar de; Osso Junior, Joao Alberto; Nascimento, Nanci; Azevedo, Mariangela de Burgos M. de [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil)

    2011-07-01

    Polycaprolactone (PCL), being one of the most important biocompatible and biodegradable aliphatic polyester, provides many potential biomedical. The preparation of biodegradable materials, polymer-based microspheres, is being developed by our group and the goal is to prepare and label with Ho-165 different polymer-based microspheres. The use of radionuclide-loaded microspheres is a promising treatment of liver malignancies. PCL microspheres can be loaded with holmium acetylacetonate (HoAcAc). PCL and PCL/HoAcAc microspheres were prepared by an emulsion solvent extraction/evaporation technique. The PCL/ HoAcAc microspheres were irradiated in a nuclear reactor IEA-R1 at IPEN/CNEN-SP to radionuclide activation. Gamma irradiation was performed at 25 and 50 kGy doses. The microspheres were evaluated by differential scanning calorimetry analysis (DSC), thermogravimetric analysis (TG), Fourier transformed infrared spectroscopy (FTIR), scanning electron microscopy (SEM) and con focal laser scanning microscopy (CLSM). In the CLSM images were observed emission in 488 nm characteristic of holmium. The SEM surface image of PCL/HoAcAc microspheres showed more roughness than PCL microspheres. TG of PCL/HoAcAc microspheres showed a substantial weight loss above 200 degree C, indicating decomposition of HoAcAc. The residual weight indicates the presence of Ho{sub 2}O{sub 3}. Gamma irradiation at 25 and 50 kGy doses had no effect on the PCL/HoAcAc microspheres, which indicates that the chemical composition of the microspheres had not change. (author)

  16. In situ preparation of cobalt nanoparticles decorated in N-doped carbon nanofibers as excellent electromagnetic wave absorbers.

    Science.gov (United States)

    Liu, Huihui; Li, Yajing; Yuan, Mengwei; Sun, Genban; Li, Huifeng; Ma, Shulan; Liao, Qingliang; Zhang, Yue

    2018-06-11

    The electrospinning and annealing methods is applied to prepare cobalt nanoparticles decorated in N-doped carbon nanofibers (Co/N-C NFs) with solid and macroporous structures. In detail, the nanocomposites are synthesized by carbonization of as-electrospun polyacrylonitrile (PAN)/cobalt acetylacetonate nanofibers in an argon atmosphere. The solid Co/N-C NFs has lengths up to dozens of microns with the average diameter of ca. 500 nm and possess abundant cobalt nanoparticles on both the surface and within the fibers, and the cobalt nanoparticles size is about 20 nm. The macroporous Co/N-C NFs possess a hierarchical pore structure, and there are macropores (500 nm) and mesopores (2-50 nm) existed in this material. The saturation magnetization (Ms) and coercivity (Hc) of the solid Co/N-C NFs are 28.4 emu g-1 and 661 Oe, respectively. And those of the macroporous Co/N-C NFs are 23.3 emu g-1 and 580 Oe, respectively. The solid Co/N-C NFs exhibits excellent electromagnetic wave absorbability, a minimum reflection loss (RL) value of -25.7 dB is achieved with a matching thickness of 2 mm for solid Co/N-C NFs when the filler loading is 5 wt%, and the effective bandwidth (BW) (RL≤-10 dB) is 4.3 GHz. Moreover, the effective microwave absorption can be achieved in the whole range of 1-18 GHz by adjusting the thickness of the sample layer and content of the dopant sample.

  17. Ligand induced shape transformation of thorium dioxide nanocrystals.

    Science.gov (United States)

    Wang, Gaoxue; Batista, Enrique R; Yang, Ping

    2018-04-27

    Nanocrystals (NCs) with size and shape dependent properties are a thriving research field. Remarkable progress has been made in the controlled synthesis of NCs of stable elements in the past two decades; however, the knowledge of the NCs of actinide compounds has been considerably limited due the difficulties in handling them both experimentally and theoretically. Actinide compounds, especially actinide oxides, play a critical role in many stages of the nuclear fuel cycle. Recently, a non-aqueous surfactant assisted approach has been developed for the synthesis of actinide oxide NCs with different morphologies, but an understanding of its control factors is still missing to date. Herein we present a comprehensive study on the low index surfaces of thorium dioxide (ThO2) and their interactions with relevant surfactant ligands using density functional calculations. A systematic picture on the thermodynamic stability of ThO2 NCs of different sizes and shapes is obtained employing empirical models based on the calculated surface energies. It is found that bare ThO2 NCs prefer the octahedral shape terminated by (111) surfaces. Oleic acid displays selective adsorption on the (110) surface, leading to the shape transformation from octahedrons to nanorods. Other ligands such as acetylacetone, oleylamine, and trioctylphosphine oxide do not modify the equilibrium shape of ThO2 NCs. This work provides atomic level insights into the anisotropic growth of ThO2 NCs that was recently observed in experiments, and thus may contribute to the controlled synthesis of actinide oxide NCs with well-defined size and shape for future applications.

  18. Luminescent rare earth vanadate nanoparticles doped with Eu3+ and Bi3 for sensing and imaging applications

    Science.gov (United States)

    Escudero, Alberto; Carrillo-Carrión, Carolina; Zyuzin, Mikhail; Hartmann, Raimo; Ashraf, Sumaira; Parak, Wolfgang J.

    2016-03-01

    Nanoparticles (NPs) are attracting interest in nanomedicine due to their potential medical applications, ranging from optical biolabels and contrast agents for magnetic resonance imaging to carriers for drug and gene delivery for disease therapy.[1] Rare earth (RE) based nanophosphors exhibit important advantages compared with other available luminescent materials, such as quantum dots and nanostructures functionalized with organic dyes, due to their lower toxicities, photostabilities, high thermal and chemical stabilities, high luminescence quantum yields, and sharp emission bands.[2] Yttrium orthovanadate NPs doped with Eu3+ and Bi3+, functionalized with poly acryl acid (PAA), and excitable by near-ultraviolet light have been synthesized by homogeneous precipitation at 120 °C from solutions of rare earth precursors (yttrium acetylacetonate and europium nitrate), bismuth nitrate, sodium orthovanadate, and PAA, in an ethylene glycol/water mixture. Quasispheres with sizes from 93 to 51 nm were obtained. The as synthesized NPs were already functionalized with PAA. The NPs showed the typical red luminescence of Eu3+, which can be excited with near-UV light through an energy transfer from the vanadate anion. The presence of Bi3+ shifts the maximum of the broad excitation band from 280 nm to 342 nm. This excitation path is much more efficient than the direct excitation of the Eu3+ electronic levels, and results in a much higher luminescence. The NPs can be uptaken by HeLa cells, and are eventually located in the lysosomes after being internalized. Finally, the functionalization with PAA provides -COOH anchors for adding functional ligands of biomedical interest that can be used for sensing applications.

  19. In situ X-ray Rietveld analysis of Ni-YSZ solid oxide fuel cell anodes during NiO reduction in H2

    International Nuclear Information System (INIS)

    Reyes Rojas, A; Esparza-Ponce, H E; Fuentes, L; Lopez-Ortiz, A; Keer, A; Reyes-Gasga, J

    2005-01-01

    A synthesis and characterization of solid oxide fuel cell (SOFC) anodes of nickel with 8%mol yttrium stabilized zirconia (Ni-YSZ) is presented. Attention was focused on the kinetics and phase composition associated with the transformation of NiO-YSZ to Ni-YSZ. The anodes were prepared with an alternative synthesis method that includes the use of nickel acetylacetonate as an inorganic precursor to obtain a highly porous material after sintering at 1400 deg. C and oxide reduction (NiO-YSZ → Ni-YSZ) at 800 deg. C for 8 h in a tubular reactor furnace using 10% H 2 /N 2 . The obtained material was compressed by unidirectional axial pressing into 1 cm-diameter discs with 15-66 wt% Ni and calcinated from room temperature to 800 deg. C. A heating rate of 1 deg. C min -1 showed the best results to avoid any anode cracking. Their structural and chemical characterization during the isothermal reduction were carried out by in situ time-resolved X-ray diffraction, refined with the Rietveld method (which allowed knowing the kinetic process of the reduction), scanning electron microscopy and X-ray energy dispersive spectroscopy. The results showed the formation of tetragonal YSZ 8%mol in the presence of nickel, a decrement in the unit cell volume of Ni and an increment of Ni in the Ni-YSZ anodes during the temperature reduction. The analysis indicated that the Johnson-Mehl-Avrami equation is unable to provide a good fit to the kinetics of the phase transformation. Instead, an alternative equation is presented

  20. Quartz Crystal Microbalance Coated with Sol-gel-derived Thin Films as Gas Sensor for NO Detection

    Directory of Open Access Journals (Sweden)

    S. J. O’Shea

    2003-10-01

    Full Text Available This paper presents the possibilities and properties of Indium tin oxide (ITO-covered quartz crystal as a NOx toxic gas-sensor. The starting sol-gel solution was prepared by mixing indium chloride dissolved in acetylacetone and tin chloride dissolved in ethanol (0-20% by weight. The ITO thin films were deposited on the gold electrodes of quartz crystal by spin-coating technique and subsequently followed a standard photolithography to pattern the derived films to ensure all sensors with the same sensing areas. All heat treatment processes were controlled below 500°C in order to avoid the piezoelectric characteristics degradation of quartz crystal (Quartz will lose its piezoelectricity at ~573°C due to the phase change from α to β. The electrical and structural properties of ITO thin films were characterized with Hall analysis system, TG/DTA, XRD, XPS, SEM and etc. The gas sensor had featured with ITO thin films of ~100nm as the receptor to sense the toxic gas NO and quartz crystal with frequency of 10MHz as the transducer to transfer the surface reactions (mass loading, etc into the frequency shift. A homemade setup had been employed to measure the sensor response under the static mode. The experimental results had indicated that the ITO-coated QCM had a good sensitivity for NO gas, ~12Hz/100ppm within 5mins. These results prove that the ITO-covered quartz crystals are usable as a gas sensor and as an analytical device.

  1. Effect of iron salt counter ion in dose-response curves for inactivation of Fusarium solani in water through solar driven Fenton-like processes

    Science.gov (United States)

    Aurioles-López, Verónica; Polo-López, M. Inmaculada; Fernández-Ibáñez, Pilar; López-Malo, Aurelio; Bandala, Erick R.

    2016-02-01

    The inactivation of Fusarium solani in water was assessed by solar driven Fenton-like processes using three different iron salts: ferric acetylacetonate (Fe(acac)3), ferric chloride (FeCl3) and ferrous sulfate (FeSO4). The experimental conditions tested were [Fe] ≈ 5 mg L-1, [H2O2] ≈ 10 mg L-1 and [Fe] ≈ 10 mg L-1; [H2O2] ≈ 20 mg L-1 mild and high, respectively, and pH 3.0 and 5.0, under solar radiation. The highest inactivation rates were observed at high reaction conditions for the three iron salts tested at pH 5.0 with less than 3.0 kJ L-1 of accumulate energy (QUV) to achieve over 99.9% of F. solani inactivation. Fe(acac)3 was the best iron salt to accomplishing F. solani inactivation. The modified Fermi equation was used to fix the experimental inactivation, data showed it was helpful for modeling the process, adequately describing dose-response curves. Inactivation process using FeSO4 at pH 3.0 was modeled fairly with r2 = 0.98 and 0.99 (mild and high concentration, respectively). Fe(acac)3, FeCl3 and FeSO4 at high concentration (i.e. [Fe] ≈ 10 mg L-1; [H2O2] ≈ 20 mg L-1) and pH 5.0 showed the highest fitting values (r2 = 0.99). Iron salt type showed a remarkable influence on the Fenton-like inactivation process.

  2. Study of the Ni-NiAl{sub 2}O{sub 4}-YSZ cermet for its possible application as an anode in solid oxide fuel cells

    Energy Technology Data Exchange (ETDEWEB)

    Reyes-Rojas, A [Centro de Investigacion en Materiales Avanzados SC, Miguel de Cervantes 120, Complejo Industrial Chihuahua, Chihuahua (Mexico); Universidad Autonoma del Estado de Mexico, Facultad de Quimica, Toluca (Mexico); Esparza-Ponce, H E [Centro de Investigacion en Materiales Avanzados SC, Miguel de Cervantes 120, Complejo Industrial Chihuahua, Chihuahua (Mexico); Reyes-Gasga, J [Universidad Nacional Autonoma de Mexico, Instituto de Fisica, Mexico DF (Mexico)

    2006-05-17

    Nanocrystalline Ni-NiAl{sub 2}O{sub 4}-YSZ cermet with a possible application as anode in solid oxide fuel cells (SOFCs) has been developed. The powders were prepared by using an alternative solid-state method that includes the use of nickel acetylacetonate as an inorganic precursor to obtain a highly porous material after sintering at 1400 {sup o}C and oxide reduction (NiO -Al{sub 2}O{sub 3}-YSZ {yields} Ni-NiAl{sub 2}O{sub 4}-YSZ) at 800 {sup o}C for 8 h in a tubular reactor furnace using 10% H{sub 2}/N{sub 2}. Eight samples with 45% Ni and 55% Al{sub 2}O{sub 3}-YSZ in concentrations of Al{sub 2}O{sub 3} oxides from 10 to 80 wt% of were mixed to obtain the cermets. The obtained material was compressed using unidirectional axial pressing and calcinations from room temperature to 800 {sup o}C. Good results were registered using a heating rate of 1 {sup o}C min{sup -1} and a special ramp to avoid anode cracking. Thermal expansion, electrical conductivity, and structural characterization by thermo-mechanical analyser (TMA) techniques/methods, the four-point probe method for conductivity, scanning electron microscopy (SEM), x-ray energy dispersive spectroscopy (EDS), x-ray diffraction (XRD), and the Rietveld method were carried out. Cermets in the range 5.5 to 11% Al{sub 2}O{sub 3} present a crystal size around 200 nm. An inversion degree (I) in the NiAl{sub 2}O{sub 4} spinel structure of the cermets Ni-NiAl{sub 2}O{sub 4}-YSZ was found after the sintering and reduction processes. Good electrical conductivity and thermal expansion coefficient were obtained for the cermet with 12 wt% of spinel structure formation.

  3. Progammed synthesis of magnetic mesoporous silica coated carbon nanotubes for organic pollutant adsorption

    Energy Technology Data Exchange (ETDEWEB)

    Tong, Yue; Zhang, Min, E-mail: congmingyang123@163.com; Xia, Peixiong; Wang, Linlin; Zheng, Jing; Li, Weizhen; Xu, Jingli, E-mail: xujingli@sues.edu.cn

    2016-05-15

    Magnetic mesoporous silica coated carbon nanotubes were produced from hydrophilic monodisperse magnetic nanoparticles decorated carbon nanotubes using well controlled programmed synthesis method and were characterized by TEM, XRD, FTIR, TGA, N{sub 2} adsorption–desorption and VSM. The well-designed mesoporous magnetic nanotubes had a large specific area, a highly open mesoporous structure and high magnetization. Firstly, SiO{sub 2}-coated maghemite/CNTs nanoparticles (CNTs/Fe{sub 3}O{sub 4}@SiO{sub 2} composites) were synthesized by the combination of high temperature decomposition process and an sol–gel method, in which the iron acetylacetonate as well as TEOS acted as the precursor for maghemite and SiO{sub 2}, respectively. The CNTs/Fe{sub 3}O{sub 4}@SiO{sub 2} composites revealed a core–shell structure, Then, CNTs/Fe{sub 3}O{sub 4}@mSiO{sub 2} was obtained by extracting cetyltrimethylammonium bromide (CTAB) via an ion-exchange procedure. The resulting composites show not only a magnetic response to an externally applied magnetic field, but also can be a good adsorbent for the organic pollutant in the ambient temperature. - Graphical abstract: Magnetic mesoporous silica coated carbon nanotubes were produced from hydrophilic monodisperse magnetic nanoparticles decorated carbon nanotubes using well controlled programmed synthesis, which can be a good adsorbent for the organic pollutant in the ambient temperature. - Highlights: • The surface of CNTs/Fe{sub 3}O{sub 4} is hydrophilic, which facilitates the silica coating. • The CNTs/Fe{sub 3}O{sub 4}@mSiO{sub 2} was synthesized by a facile method. • The CNTs/Fe{sub 3}O{sub 4}@mSiO{sub 2} can be a good adsorbent for the organic pollutant.

  4. Controllable Synthesis of Lindqvist Alkoxopolyoxovanadate Clusters as Heterogeneous Catalysts for Sulfoxidation of Sulfides.

    Science.gov (United States)

    Li, Ji-Kun; Dong, Jing; Wei, Chuan-Ping; Yang, Song; Chi, Ying-Nan; Xu, Yan-Qing; Hu, Chang-Wen

    2017-05-15

    Six alkoxohexavanadate-based Cu- or Co-POVs [Cu(dpa)(acac)(H 2 O)] 2 [V 6 O 13 (OMe) 6 ] (1), [Cu(phen)(acac)(MeOH)] 2 [V 6 O 13 (OMe) 6 ] (2), [Co(dpa)(acac) 2 ] 2 [V 6 O 13 (OMe) 6 ]·2MeOH (3), [Co(phen)(acac) 2 ] 2 [V 6 O 13 (OMe) 6 ] (4), [Cu(dpa)(acac)] 2 [V IV 2 V V 4 O 12 (OMe) 7 ] (5), and [Cu(dpa)(acac)(MeOH)] 2 [V IV 2 V V 4 O 11 (OMe) 8 ] (6) (POV = polyoxovanadate; dpa = 2,2'-dipyridine amine; phen = 1,10-phenanthroline; acac = acetylacetone anion) have been synthesized by controlling the reaction conditions and characterized by single-crystal X-ray diffraction and powder X-ray diffraction analyses, FT-IR spectroscopy, element analyses, and X-ray photoelectron spectroscopy. In compounds 1-4 and 6, Cu or Co complexes and alkoxohexavanadate anions are assembled through electrostatic interactions. Differently, in compound 5, seven-methoxo-substituted Lindqvist-type [V 6 O 12 (OMe) 7 ] 2- are bridged to Cu complex via terminal O atoms by coordination bonds. All compounds 1-6 exhibit excellent heterogeneous catalytic performance in oxidative desulfurization and CEES ((2-chloroethyl) ethyl sulfide, a sulfur mustard simulant) abatement with H 2 O 2 as oxidant. Among them, the catalytic activity of 6 [conv. of DBT (dibenzothiophene) up to 100% in 6 h; conv. of CEES reached 100% and selectivity of CEESO ((2-chloroethyl) ethyl sulfoxide) up to 85% after 4 h] outperforms others and can be reused without losing its activity.

  5. Sandwich-type mixed tetrapyrrole rare-earth triple-decker compounds. Effect of the coordination geometry on the single-molecule-magnet nature.

    Science.gov (United States)

    Kan, Jinglan; Wang, Hailong; Sun, Wei; Cao, Wei; Tao, Jun; Jiang, Jianzhuang

    2013-08-05

    Employment of the raise-by-one step method starting from M(TClPP)(acac) (acac = monoanion of acetylacetone) and [Pc(OPh)8]M'[Pc(OPh)8] led to the isolation and free modulation of the two rare-earth ions in the series of four mixed tetrapyrrole dysprosium sandwich complexes {(TClPP)M[Pc(OPh)8]M'[Pc(OPh)8]} [1-4; TClPP = dianion of meso-tetrakis(4-chlorophenyl)porphyrin; Pc(OPh)8 = dianion of 2,3,9,10,16,17,23,24-octa(phenoxyl)phthalocyanine; M-M' = Dy-Dy, Y-Dy, Dy-Y, and Y-Y]. Single-crystal X-ray diffraction analysis reveals different octacoordination geometries for the two metal ions in terms of the twist angle (defined as the rotation angle of one coordination square away from the eclipsed conformation with the other) between the two neighboring tetrapyrrole rings for the three dysprosium-containing isostructural triple-decker compounds, with the metal ion locating between an inner phthalocyanine ligand and an outer porphyrin ligand with a twist angle of 9.64-9.90° and the one between two phthalocyanine ligands of 25.12-25.30°. Systematic and comparative studies over the magnetic properties reveal magnetic-field-induced single-molecule magnet (SMM), SMM, and non-SMM nature for 1-3, respectively, indicating the dominant effect of the coordination geometry of the spin carrier, instead of the f-f interaction, on the magnetic properties. The present result will be helpful for the future design and synthesis of tetrapyrrole lanthanide SMMs with sandwich molecular structures.

  6. Experimental setup and analytical methods for the non-invasive determination of volatile organic compounds, formaldehyde and NOx in exhaled human breath

    International Nuclear Information System (INIS)

    Riess, Ulrich; Tegtbur, Uwe; Fauck, Christian; Fuhrmann, Frank; Markewitz, Doreen; Salthammer, Tunga

    2010-01-01

    Different analytical devices were tested and evaluated for their suitability of breath gas analysis by examining the physiological parameters and chemical substances in the exhaled breath of ten healthy probands during light cycling in dependence of methanol-rich nutrition. The probands exercised under normal breathing conditions on a bicycle ergometer. Breath air was exhaled into a glass cylinder and collected under steady-state conditions. Non-invasively measured parameters were pulse rate, breath frequency, temperature, relative humidity, NO x , total volatile organic compounds (TVOC PAS ), carbon dioxide (CO 2 ), formaldehyde, methanol, acetaldehyde, acetone, isoprene and volatile organic compounds (VOCs). Methanol rich food and beverages strongly influenced the concentration of methanol and other organic substances in human breath. On the other hand, nutrition and smoking had no clear effect on the physical conditions of the probands. The proton transfer reaction mass spectrometry (PTR-MS) method was found to be very suitable for the analysis of breath gas but the m/z 31, if assigned to formaldehyde, is sensitive to interferences. The time vs. concentration curves of nitric oxide showed sudden peaks up to 120 ppb in most of the measurements. In one case a strong interference of the NO x signal was observed. The time resolved analysis of exhaled breath gas is of high capability and significance for different applications if reliable analytical techniques are used. Some compounds like nitric oxide (NO), methanol, different VOCs as well as sum parameters like TVOC PAS are especially suitable as markers. Formaldehyde, which is rapidly metabolized in the human body, could be measured reliably as a trace component by the acetylacetone (acac) method but not by PTR-MS.

  7. Experimental setup and analytical methods for the non-invasive determination of volatile organic compounds, formaldehyde and NO{sub x} in exhaled human breath

    Energy Technology Data Exchange (ETDEWEB)

    Riess, Ulrich; Tegtbur, Uwe [Hannover Medical School, Sports Physiology and Sports Medicine, Carl-Neuberg-Str. 1, 30625 Hannover (Germany); Fauck, Christian; Fuhrmann, Frank; Markewitz, Doreen [Fraunhofer WKI, Department of Material Analysis and Indoor Chemistry, Bienroder Weg 54 E, 38108 Braunschweig (Germany); Salthammer, Tunga, E-mail: tunga.salthammer@wki.fraunhofer.de [Fraunhofer WKI, Department of Material Analysis and Indoor Chemistry, Bienroder Weg 54 E, 38108 Braunschweig (Germany)

    2010-06-11

    Different analytical devices were tested and evaluated for their suitability of breath gas analysis by examining the physiological parameters and chemical substances in the exhaled breath of ten healthy probands during light cycling in dependence of methanol-rich nutrition. The probands exercised under normal breathing conditions on a bicycle ergometer. Breath air was exhaled into a glass cylinder and collected under steady-state conditions. Non-invasively measured parameters were pulse rate, breath frequency, temperature, relative humidity, NO{sub x}, total volatile organic compounds (TVOC{sub PAS}), carbon dioxide (CO{sub 2}), formaldehyde, methanol, acetaldehyde, acetone, isoprene and volatile organic compounds (VOCs). Methanol rich food and beverages strongly influenced the concentration of methanol and other organic substances in human breath. On the other hand, nutrition and smoking had no clear effect on the physical conditions of the probands. The proton transfer reaction mass spectrometry (PTR-MS) method was found to be very suitable for the analysis of breath gas but the m/z 31, if assigned to formaldehyde, is sensitive to interferences. The time vs. concentration curves of nitric oxide showed sudden peaks up to 120 ppb in most of the measurements. In one case a strong interference of the NO{sub x} signal was observed. The time resolved analysis of exhaled breath gas is of high capability and significance for different applications if reliable analytical techniques are used. Some compounds like nitric oxide (NO), methanol, different VOCs as well as sum parameters like TVOC{sub PAS} are especially suitable as markers. Formaldehyde, which is rapidly metabolized in the human body, could be measured reliably as a trace component by the acetylacetone (acac) method but not by PTR-MS.

  8. [Pt(O,O'-acac)(gamma-acac)(DMS)], a new Pt compound exerting fast cytotoxicity in MCF-7 breast cancer cells via the mitochondrial apoptotic pathway.

    Science.gov (United States)

    Muscella, A; Calabriso, N; Fanizzi, F P; De Pascali, S A; Urso, L; Ciccarese, A; Migoni, D; Marsigliante, S

    2008-01-01

    We showed previously that a new Pt complex containing an O,O'-chelated acetylacetonate ligand (acac) and a dimethylsulphide in the Pt coordination sphere, [Pt(O,O'-acac)(gamma-acac)(DMS)], induces apoptosis in HeLa cells. The objective of this study was to investigate the hypothesis that [Pt(O,O'-acac)(gamma-acac)(DMS)] is also cytotoxic in a MCF-7 breast cancer cell line relatively insensitive to cisplatin, and to gain a more detailed analysis of the cell death pathways. Cells were treated with Pt compounds and cytotoxicity tests were performed, together with Western blotting of various proteins involved in apoptosis. The mitochondrial membrane potential was assessed by fluorescence microscopy and spectrofluorometry and the Pt bound to cell fractions was measured by atomic absorption spectrometry. In contrast to cisplatin, the cytotoxicity of [Pt(O,O'-acac)(gamma-acac)(DMS)] correlated with cellular accumulation but not with DNA binding. Also, the Pt content in DNA bases was considerably higher for cisplatin than for [Pt(O,O'-acac)(gamma-acac)(DMS)], thus excluding DNA as a target of [Pt(O,O'-acac)(gamma-acac)(DMS)]. [Pt(O,O'-acac)(gamma-acac)(DMS)] exerted high and fast apoptotic processes in MCF-7 cells since it provoked: (a) mitochondria depolarization; (b) cytochrome c accumulation in the cytosol; (c) translocation of Bax and truncated-Bid from cytosol to mitochondria and decreased expression of Bcl-2; (d) cleavage of caspases -7 and -9, and PARP degradation; (e) chromatin condensation and DNA fragmentation. [Pt(O,O'-acac)(gamma-acac)(DMS)] is highly cytotoxic for MCF-7 cells, cells relatively resistant to many chemotherapeutic agents, as it activates the mitochondrial apoptotic pathway. Hence, [Pt(O,O'-acac)(gamma-acac)(DMS)] has the potential to provide us with new opportunities for therapeutic intervention.

  9. Separations systems data base: a users' manual. Revision I

    International Nuclear Information System (INIS)

    Roddy, J.W.; McDowell, W.J.

    1981-01-01

    A separations systems data base (SEPSYS), designed specifically for the retrieval of information needed in chemical separations problems (i.e., how to perform a given separation under given conditions), is described. Included are descriptions of the basic methods of searching and retrieving information from the data base, the procedure for entering records into the data base, a listing of additional references concerning the computer information process, and an example of a typical record. The initial entries are concerned primarily with liquid-liquid extraction and liquid-solid ion exchange methods for metal ions and salts; however, the data base is constructed so that almost any separation process can be accommodated. Each record is indexed with information provided under the following fields: author; title; publication source; data of publication; organization sponsoring the work; brief abstract of the work; abstract number if the work has been so referenced, and/or abstractors initials; type of separation system used (e.g., flotation); specific or generic name of the separation agent used (e.g., acetylacetone); list of substances separated (e.g., gold, copper); qualitative description of the supporting medium or matrix containing the substances before separation (e.g., nitrate); type of literature where the record was printed (e.g., book); and type of information that the article contains. Each of these fields may be searched independently of the others (or in combination), and the last six fields contain specific key words that are listed in the report. Definitions are provided for the 36 information terms

  10. Obtention of zirconia films stabilized with Yttria via pyrolysis spray: study of the solvent influence; Obtencao de filmes de zirconia estabilizada com itria via spray pirolise: estudo da influencia do solvente

    Energy Technology Data Exchange (ETDEWEB)

    Halmenschlager, Cibele Melo; Vieira, Ramaugusto da Porciuncula; Takimi, Antonio Shigueaki; Bergmann, Carlos Perez; Silva, Aline Lima da; Malfatti, Celia de Fraga [Universidade Federal do Rio Grande do Sul (UFRGS), Porto Alegre, RS (Brazil). Programa de Pos-Graduacao em Engenharia de Minas, Metalurgica e de Materiais (PPGEM). Lab. de Materiais Ceramicos (LACER)]. E-mail: cibelemh@yahoo.com.br

    2008-07-01

    Yttria-stabilized-zirconia (YSZ) has been object of many studies, due to its great chemical stability and excellent ionic conduction in high temperature. This material has been studies with an intention of to be used with electrolyte of oxide solid fuel cells, which work in high temperature. The aim of the present work was to evaluate the influence of the solvent on the elaboration of crystalline films of YSZ via spray pyrolysis. The film was prepared by spray pyrolysis with zirconium acetylacetonate (Zr(C{sub 6}H{sub 7}O{sub 2}){sub 4}) and yttrium chloride (YCl{sub 3}.6H{sub 2}O), dissolved in different solvents: ethanol (C{sub 2}H{sub 6}O), ethanol (C{sub 2}H{sub 6}O) + propyleneglycol (C{sub 3}H{sub 8}O{sub 2}) with volume ratio (1:1) and ethanol (C{sub 2}H{sub 6}O) + diethylene glycol butyl ether (C{sub 8}H{sub 18}O{sub 3}) with volume ratio of 1:1. A disk of steel 316L was used as substrate. The amorphous film was deposited in the substrate heated at 280 deg C {+-} 50 deg C. After deposition from thermal treatment at 700 deg C the amorphous film was changed into Yttria-stabilized-zirconia film. The thermal behavior of the films has been studied by both (DTA/TGA) thermogravimetric and mass spectroscopy analyses. The morphology and crystalline phase of the films was investigated by scanning electron microscopy (SEM) and X-ray diffraction (XRD), respectively. The YSZ film obtained after heat treatment was dense and crystalline, however, the analyses indicate a significant influence of the solvent and of the substrate temperature during the deposition process on the film morphology.(author)

  11. Dysprosium complexes with the tetraphenylporphyrin macrocyclic ligand; Complejos de disprosio con el ligante macrociclico tetrafenilporfirina

    Energy Technology Data Exchange (ETDEWEB)

    Martinez M, V; Padilla, J; Ramirez, F M

    1992-04-15

    In this report, the results obtained on the synthesis, characterization and study of the chemical behavior of dysprosium complex with the acetylacetone chelating agent (Hacac) and the tetraphenylporphyrin macrocyclic ligand (H{sub 2}TFP) are given. Based on the literature but according to our necessities and interest, the appropriate methodology settled down from the synthesis of prime matters until the obtaining and characterization of the products. The acetyl acetonate complex was obtained of mono hydrated dysprosium [Dy(acac){sub 3}. H{sub 2}0] and trihydrated [Dy(acac){sub 3} .3 H{sub 2}0], the mono tetra phenyl porphyrinate [Dy(TFP)(acac). 2 ac] the double sandwich of the dysprosium porphyrinate [Dy(TFP){sub 2}] and the triple sandwich of the dysprosium porphyrinate [Dy(TFP){sub 3}. 2 TCB] (TCB = trichlorobenzene). Its were characterized by their melting points, solubility, IR, UV, TGA and DTA both first and besides the techniques already mentioned for NMR'H, RPE and Magnetic susceptibility the three last complexes. From the spectroscopic point of view, IR and RPE its suggested the existence of a complex of inverse mixed valence [Dy(TFP){sup 2-} (TFP) {sup 1-}] for the Dy(TFP){sub 2} as a result of the existence of the free radical (TFP' {sup 1-} and that it was not in none of the other porphyrin compounds. In the NMR'H spectra of the compounds were not observed signals in the region from 0 to 10 ppm that which shows that the dysprosium complexes in special those of the porphyrin type are highly paramagnetic and its could be used as displacement reagents, creators of images and contrast agents of great utility in these days in studies of NMR, technique today by today used in medical diagnoses. (Author)

  12. Preparations and characterization of some carbonyl-(1-cyanoethyl)ruthenium(II) complexes

    Energy Technology Data Exchange (ETDEWEB)

    Hiraki, Katsuma; Ochi, Naoyuki; Kitamura, Tsuneyuki; Sasada, Yoko [Nagasaki Univ. (Japan); Shinoda, Sumio

    1982-08-01

    A hydridoruthenium(II) complex (RuClH(CO)(PPh/sub 3/)/sub 3/) reacted easily with acrylonitrile and fumaronitrile to give chloro-bridged binuclear (1-cyanoethyl)ruthenium(II) complexes, ((Ru(MeCHCN)Cl(CO)(PPh/sub 3/)/sub 2/)/sub 2/) (2) and ((Ru(NCCH/sub 2/CHCN)Cl(CO)(PPh/sub 3/)/sub 2/)/sub 2/), respectively. Complex 2 reacted with 4-picoline (pic), Na(BHPz/sub 3/) (Pz = 1-pyrazolyl), Na(BPz/sub 4/), and Na(Et/sub 2/NCS/sub 2/).3H/sub 2/O to afford the corresponding (1-cyanoethyl)ruthenium(II) complexes, ((Ru(MeCHCN)Cl(CO)(pic)(PPh/sub 3/))/sub 2/) (3), (Ru(MeCHCN)(BHPz/sub 3/)(CO)(PPh/sub 3/)) (accompanied by a small amount of (Ru/sub 2/(MeCHCN)/sub 2/Cl(BHPz/sub 3/)(CO)/sub 2/(PPh/sub 3/)/sub 4/)), (Ru/sub 2/(MeCHCN)/sub 2/Cl(BPz/sub 4/)(CO)/sub 2/(PPh/sub 3/)/sub 2/), and Na(Ru(MeCHCN)Cl(Et/sub 2/NCS/sub 2/)(CO)(PPh/sub 3/)), respectively. Complex 3 reacted with thallium (I) acetylacetonate (Tl(acac)), resulting in the formation of ((Ru(MeCHCN)(acac)(CO)(PPh/sub 3/))/sub 2/) and (Ru(MeCHCN)(acad)(CO)(pic)(PPh/sub 3/)). These new complexes were characterized by means of elemental analysis and spectroscopic data. The diastereoisomerism was also discussed as regards these (1-cyanoethyl)ruthenium(II) complexes.

  13. Recombination region improvement for reduced efficiency roll-off in phosphorescent OLEDs with dual emissive layers

    Energy Technology Data Exchange (ETDEWEB)

    Ma, Zhu; Zhou, Shunliang [State Key Laboratory of Electronic Thin Films and Integrated Devices, School of Optoelectronic Information, University of Electronic Science and Technology of China (UESTC), Chengdu 610054 (China); Hu, Song [Chengdu Institute of Optics and Electronics, Chinese Academy of Sciences, Chengdu 610209 (China); Yu, Junsheng, E-mail: jsyu@uestc.edu.cn [State Key Laboratory of Electronic Thin Films and Integrated Devices, School of Optoelectronic Information, University of Electronic Science and Technology of China (UESTC), Chengdu 610054 (China)

    2014-10-15

    High-performance phosphorescent organic light-emitting diodes (PhOLEDs) by using dual-emissive-layer (DEL) structure to reduce efficiency roll-off were fabricated. The DEL was comprised of a hole-transport-type host of N, N′-bis(naphthalen-1-yl)-N, N′-bis(phenyl)-benzidine (NPB) and a bipolar host of 4,4′-bis(carbazol-9-yl)biphenyl (CBP), which were both doped with an orange phosphorescent dopant of bis[2-(4-tert-butylphenyl)-benzothiazolato-N,C2′]iridium (acetylacetonate) [(t-bt){sub 2}Ir(acac)]. After the optimization of doping concentration of the first emissive layer (FEL), the device with DEL exhibited 11% lower roll-off power efficiency than single emissive layer devices (SED) when the luminance increased from 1000 cd/m{sup 2} to 10,000 cd/m{sup 2}. The hole–electron recombination zone in DEL was illuminated by inserting an ultrathin fluorescent probe of 4-(dicyanomethylene)-2-tert-butyl-6 (1,1,7,7-tetramethyljulolidin-4-yl-vinyl)-4H-pyran (DCJTB) in different emissive regions. The performance improvement was attributed to the optimization of energy barrier and the expansion of exciton formation zone within the DEL. - Highlights: • PhOLEDs by using a dual-emissive-layer structure to reduce efficiency roll-off were fabricated. • The DED exhibited 11% lower efficiency roll-off, 57% lower turn-on voltage, and 174% higher brightness than SED. • A DCJTB fluorescent probe was inserted at different positions of DED to investigate the expansion of exciton formation zone.

  14. New approach towards the polyol route to fabricate MFe{sub 2}O{sub 4} magnetic nanoparticles: The use of MCl{sub 2} and Fe(acac){sub 3} as chemical precursors

    Energy Technology Data Exchange (ETDEWEB)

    Solano, Eduardo, E-mail: eduardo.solano@ugent.be [Departament de Química, Universitat Autònoma de Barcelona, 08193 Bellaterra, Catalonia (Spain); Institut de Ciència de Materials de Barcelona, ICMAB-CSIC, Campus de la UAB, 08193 Bellaterra, Catalonia (Spain); Yáñez, Ramón [Departament de Química, Universitat Autònoma de Barcelona, 08193 Bellaterra, Catalonia (Spain); Ricart, Susagna [Institut de Ciència de Materials de Barcelona, ICMAB-CSIC, Campus de la UAB, 08193 Bellaterra, Catalonia (Spain); Ros, Josep [Departament de Química, Universitat Autònoma de Barcelona, 08193 Bellaterra, Catalonia (Spain)

    2015-05-15

    A new more efficient approach of the polyol route to generate MFe{sub 2}O{sub 4} (M=Mn, Fe, Co, Ni, Cu, Zn) nanoparticles in triethylene glycol (TREG) is presented. The selected thermal procedure is based on the Fe metalorganic precursor (iron(III) acetylacetonate) decomposition in presence of an inorganic transition metal chloride salt (MCl{sub 2}, M=Mn, Fe, Co, Ni, Cu, Zn) to produce high quality polar dispersible nanoparticles with lower production cost. In addition, the nanoparticles are stabilized by ionic (from the Cl{sup −}) and steric (TREG as capping ligand) effects inducing into the nanoparticles an extraordinary stability in different polar solvents. As result of this optimized methodology, the colloidal polar dispersible nanoparticles present a size around 10 nm with an adequate size dispersion demonstrated by analyzing transmission electron microscopy (TEM) images. X-ray powder diffraction (XRPD) results corroborate the absence of secondary phases and the high crystalline degree obtained for the spinel structure, fact proved by using synchrotron X-ray diffraction. The high magnetic performance at low and room temperature of the nanoparticles studied by magnetometry proves the high internal crystal order of the spinel. Parallel to this, the influence of the heating ramp and annealing time in the thermal procedure were also investigated for the CuFe{sub 2}O{sub 4} case, where a relationship between these two parameters and the final size and their associated diameter distribution was found, allowing a possible size control of the final ferrite magnetic nanoparticles synthesized. - Highlights: • An optimized one-pot methodology is presented to produce pure MFe{sub 2}O{sub 4} nanoparticles. • MCl{sub 2} and Fe(acac){sub 3} precursors in TREG are used for a more efficient process. • Polar dispersible nanoparticles are obtained with high physicochemical properties. • The influence of the temperature ramp and rate on the final size is studied.

  15. New approach towards the polyol route to fabricate MFe2O4 magnetic nanoparticles: The use of MCl2 and Fe(acac)3 as chemical precursors

    International Nuclear Information System (INIS)

    Solano, Eduardo; Yáñez, Ramón; Ricart, Susagna; Ros, Josep

    2015-01-01

    A new more efficient approach of the polyol route to generate MFe 2 O 4 (M=Mn, Fe, Co, Ni, Cu, Zn) nanoparticles in triethylene glycol (TREG) is presented. The selected thermal procedure is based on the Fe metalorganic precursor (iron(III) acetylacetonate) decomposition in presence of an inorganic transition metal chloride salt (MCl 2 , M=Mn, Fe, Co, Ni, Cu, Zn) to produce high quality polar dispersible nanoparticles with lower production cost. In addition, the nanoparticles are stabilized by ionic (from the Cl − ) and steric (TREG as capping ligand) effects inducing into the nanoparticles an extraordinary stability in different polar solvents. As result of this optimized methodology, the colloidal polar dispersible nanoparticles present a size around 10 nm with an adequate size dispersion demonstrated by analyzing transmission electron microscopy (TEM) images. X-ray powder diffraction (XRPD) results corroborate the absence of secondary phases and the high crystalline degree obtained for the spinel structure, fact proved by using synchrotron X-ray diffraction. The high magnetic performance at low and room temperature of the nanoparticles studied by magnetometry proves the high internal crystal order of the spinel. Parallel to this, the influence of the heating ramp and annealing time in the thermal procedure were also investigated for the CuFe 2 O 4 case, where a relationship between these two parameters and the final size and their associated diameter distribution was found, allowing a possible size control of the final ferrite magnetic nanoparticles synthesized. - Highlights: • An optimized one-pot methodology is presented to produce pure MFe 2 O 4 nanoparticles. • MCl 2 and Fe(acac) 3 precursors in TREG are used for a more efficient process. • Polar dispersible nanoparticles are obtained with high physicochemical properties. • The influence of the temperature ramp and rate on the final size is studied

  16. Highly Simplified Reddish Orange Phosphorescent Organic Light-Emitting Diodes Incorporating a Novel Carrier- and Exciton-Confining Spiro-Exciplex-Forming Host for Reduced Efficiency Roll-off.

    Science.gov (United States)

    Xu, Ting; Zhang, Ye-Xin; Wang, Bo; Huang, Chen-Chao; Murtaza, Imran; Meng, Hong; Liao, Liang-Sheng

    2017-01-25

    A novel exciplex-forming host is applied so as to design highly simplified reddish orange light-emitting diodes (OLEDs) with low driving voltage, high efficiency, and an extraordinarily low efficiency roll-off, by combining N,N-10-triphenyl-10H-spiro [acridine-9,9'-fluoren]-3'-amine (SAFDPA) with 4,7-diphenyl-1,10-phenanthroline (Bphen) doped with trivalent iridium complex bis(2-methyldibenzo[f,h]quinoxaline) (acetylacetonate)iridium(III) (Ir(MDQ) 2 (acac)). The reddish orange OLEDs achieve a strikingly high power efficiency (PE) of 31.80 lm/W with an ultralow threshold voltage of 2.24 V which is almost equal to the triplet energy level of the phosphorescent reddish orange emitting dopant. The power efficiency of the device with the exciplex-forming host is enhanced, achieving 36.2% mainly owing to the lower operating voltage by the novel exciplex forming cohost, compared with the reference device (23.54 lm/W). Moreover, the OLEDs show extraordinarily low current efficiency (CE) roll-off to 1.41% at the brightness from 500 to 5000 cd/m 2 with a maximal CE of 32.87 cd/A (EQE max = 11.01%). The devices display a good reddish orange color (CIE of (0.628, 0.372) at 500 cd/m 2 ) nearly without color shift with increasing brightness. Co-host architecture phosphorescent OLEDs show a simpler device structure, lower working voltage, and a better efficiency and stability than those of the reference devices without the cohost architecture, which helps to simplify the OLED structure, lower the cost, and popularize OLED technology.

  17. Chemical vapor deposition (CVD) of uranium for alpha spectrometry; Deposicion quimica de vapor (CVD) de uranio para espectrometria alfa

    Energy Technology Data Exchange (ETDEWEB)

    Ramirez V, M. L.; Rios M, C.; Ramirez O, J.; Davila R, J. I.; Mireles G, F., E-mail: luisalawliet@gmail.com [Universidad Autonoma de Zacatecas, Unidad Academica de Estudios Nucleares, Cipres No. 10, Fracc. La Penuela, 98068 Zacatecas (Mexico)

    2015-09-15

    The uranium determination through radiometric techniques as alpha spectrometry requires for its proper analysis, preparation methods of the source to analyze and procedures for the deposit of this on a surface or substrate. Given the characteristics of alpha particles (small penetration distance and great loss of energy during their journey or its interaction with the matter), is important to ensure that the prepared sources are thin, to avoid problems of self-absorption. The routine methods used for this are the cathodic electro deposition and the direct evaporation, among others. In this paper the use of technique of chemical vapor deposition (CVD) for the preparation of uranium sources is investigated; because by this, is possible to obtain thin films (much thinner than those resulting from electro deposition or evaporation) on a substrate and comprises reacting a precursor with a gas, which in turn serves as a carrier of the reaction products to achieve deposition. Preliminary results of the chemical vapor deposition of uranium are presented, synthesizing and using as precursor molecule the uranyl acetylacetonate, using oxygen as carrier gas for the deposition reaction on a glass substrate. The uranium films obtained were found suitable for alpha spectrometry. The variables taken into account were the precursor sublimation temperatures and deposition temperature, the reaction time and the type and flow of carrier gas. Of the investigated conditions, two depositions with encouraging results that can serve as reference for further work to improve the technique presented here were selected. Alpha spectra obtained for these depositions and the characterization of the representative samples by scanning electron microscopy and X-ray diffraction are also presented. (Author)

  18. Tunable fluorescence emission of ternary nonstoichiometric Ag-In-S alloyed nanocrystals

    Energy Technology Data Exchange (ETDEWEB)

    Feng Jian, E-mail: dhjfeng@ciac.jl.cn; Yang Xiurong, E-mail: xryang@ciac.jl.cn [Chinese Academy of Sciences, State Key Laboratory of Electroanalytical Chemistry, Changchun Institute of Applied Chemistry (China)

    2012-08-15

    Low toxic, nonstoichiometric colloidal Ag-In-S ternary quantum dots with different Ag content were synthesized by a one-pot hot-injection method based on the reaction of metal acetylacetonates with sulfur dissolved in octadecene. X-ray diffraction (XRD), transmission electron microscopy, and high-resolution transmission electron microscopy (HRTEM) were used to characterize the size, structure, and morphology of these samples. ICP-MS was employed to analyze the compositions of Ag-In-S nanocrystals. The optical properties were characterized by UV-Vis absorption, photoluminescence (PL) spectroscopy, and time-resolved photoluminescence. Varying the fraction of cationic and capping agents, the compositions of Ag-In-S nanocrystals were precisely controlled. XRD and HRTEM results indicate the compositional homogeneity of Ag-In-S. The emission spectra across the different compositions exhibiting a single bandgap feature further confirm the formation of Ag-In-S alloy NCs, rather than phase separated Ag{sub 2}S and In{sub 2}S{sub 3}. Composition-dependent tunable PL emissions have been observed. The relative PL quantum yield is up to 16 %, which exhibited substantially enhanced comparing with the stoichiometric AgInS{sub 2} semiconductor core QDs reported in previous literature. The PL decay curve of Ag-In-S has a biexponential characteristic, which indicates that the recombination of an electron and a hole is dominated by the surface defect and the recombination process associated with internal traps is reduced significantly. The large Stokes shift between the absorption peaks and their emissions should inhibit the reabsorption and Foerster energy transfer between Ag-In-S nanocrystals, which provides the alternative in the further applications where high-concentrations of nanocrystals are needed.

  19. Sensitive inexpensive spectrophotometric and spectrofluorimetric analysis of ezogabine, levetiracetam and topiramate in tablet formulations using Hantzsch condensation reaction

    Science.gov (United States)

    Ibrahim, F. A.; El-Yazbi, A. F.; Wagih, M. M.; Barary, M. A.

    2017-09-01

    Two highly sensitive, simple and selective spectrophotometric and spectrofluorimetric assays have been investigated for the analysis of ezogabine, levetiracetam and topiramate in their pure and in pharmaceutical dosage forms. The suggested methods depend on the condensation of the primary amino-groups in the three drugs with acetylacetone and formaldehyde according to Hantzsch reaction yielding highly fluorescent yellow colored dihydropyridine derivatives. The reaction products of ezogabine, levetiracetam and topiramate were measured spectrophotometrically at 418, 390 and 380 nm or spectrofluorimetrically at λem/ex of 495/425 nm, 490/415 nm and 488/410 nm, respectively. Various experimental conditions have been carefully studied to maximize the reaction yield. At the optimum reaction conditions, the calibration curves were rectilinear over the concentration ranges of 8-25, 60-180 and 80-200 μg/mL spectrophotometrically and 0.02-0.2, 0.2-1.2 and 0.2-1.5 μg/mL spectrofluorimetrically for ezogabine, levetiracetam and topiramate, respectively with good correlation coefficients. The suggested methods were applied successfully for the analysis of ezogabine, levetiracetam and topiramate in their commercial tablets with high percentage recoveries and negligible interference from various excipients in pharmaceutical dosage forms. The results were statistically analyzed and showed the absence of any significant difference between both developed and published methods. The procedures were validated and evaluated by the ICH guidelines revealing good reproducibility and accuracy. Therefore, the two proposed methods may be considered of high interest for practical and reliable analysis of ezogabine, levetiracetam and topiramate in pharmaceutical dosage forms.

  20. Hybrid white organic light-emitting devices based on phosphorescent iridium–benzotriazole orange–red and fluorescent blue emitters

    International Nuclear Information System (INIS)

    Xia, Zhen-Yuan; Su, Jian-Hua; Chang, Chi-Sheng; Chen, Chin H.

    2013-01-01

    We demonstrate that high color purity or efficiency hybrid white organic light-emitting devices (OLEDs) can be generated by integrating a phosphorescent orange–red emitter, bis[4-(2H-benzotriazol-2-yl)-N,N-diphenyl-aniline-N 1 ,C 3 ] iridium acetylacetonate, Ir(TBT) 2 (acac) with fluorescent blue emitters in two different emissive layers. The device based on deep blue fluorescent material diphenyl-[4-(2-[1,1′;4′,1″]terphenyl-4-yl-vinyl)-phenyl]-amine BpSAB and Ir(TBT) 2 (acac) shows pure white color with the Commission Internationale de L'Eclairage (CIE) coordinates of (0.33,0.30). When using sky-blue fluorescent dopant N,N′-(4,4′-(1E,1′E)-2,2′-(1,4-phenylene)bis(ethene-2,1-diyl) bis(4,1-phenylene))bis(2-ethyl-6-methyl-N-phenylaniline) (BUBD-1) and orange–red phosphor with a color-tuning phosphorescent material fac-tris(2-phenylpyridine) iridium (Ir(ppy) 3 ), it exhibits peak luminance yield and power efficiency of 17.4 cd/A and 10.7 lm/W, respectively with yellow-white color and CIE color rendering index (CRI) value of 73. - Highlights: ► An iridium-based orange–red phosphor Ir(TBT) 2 (acac) was applied in hybrid white OLEDs. ► Duel- and tri-emitter WOLEDs were achieved with either high color purity or efficiency performance. ► Peak luminance yield of tri-emitter WOLEDs was 17.4 cd/A with yellow-white color and color rendering index (CRI) value of 73.

  1. Structure and multiferroic properties of barium hexaferrite ceramics

    International Nuclear Information System (INIS)

    Tan, Guolong; Chen, Xiuna

    2013-01-01

    Simultaneous occurrence of large ferroelectricity and strong ferromagnetism have been observed in barium hexaferrite ceramics. Barium hexaferrite (BaFe 12 O 19 ) powders with hexagonal crystal structure were successfully synthesized in a polymer precursor method using barium acetate and ferric acetylacetonate as the precursors. The powders were pressed into pellets which were sintered into ceramics at 1200 °C and 1300 °C for 1 h. The structure and morphology of the ceramics were examined using X-ray diffraction and field emission scanning electron microscopy. Large spontaneous polarization was observed in the BaFe 12 O 19 ceramics at room temperature, revealing a clear ferroelectric hysteresis loop. The maximum remanent polarization of the BaFe 12 O 19 ceramic was estimated approximately 11.8 μC cm −2 . The FeO 6 octahedron in its perovskite-like hexagonal unit cell and the shift of Fe 3+ off the center of octahedron are suggested to be the origin of the polarization in BaFe 12 O 19 . The BaFe 12 O 19 ceramics also showed strong ferromagnetism at room temperature. - Graphical abstract: Ferroelectric hysteresis loops of BaFe 12 O 19 ceramics measured at a frequency of 120 Hz, which shows that the ceramics sintered at 1200 °C is ferroelectric with P r ∼11.8 μC/cm 2 . Highlights: ► Large ferroelectricity and strong ferromagnetism were observed in barium hexaferrite ceramics. ► The maximum remanent polarization of the BaFe 12 O 19 ceramic was estimated to be 11.8 μC cm −2 . ► The FeO 6 octahedron and off-center shift of Fe 3+ are suggested to be the origin of the polarization.

  2. Multiferroic properties of Pb2Fe2O5 ceramics

    International Nuclear Information System (INIS)

    Wang, Min; Tan, Guolong

    2011-01-01

    Research highlights: → Simultaneous occurrence of ferromagnetism and ferroelectricity in Pb 2 Fe 2 O 5 ceramics. → The off-centers of shifted Pb 2+ ions as well as the FeO 6 octahedra in the 'Pb 2 Fe 2 O 5 ' lead to a ferroelectric polarization. → Pb 2 Fe 2 O 5 ceramic demonstrates ferromagnetic order state due to the spin arrangement in the double chains of FeO 5 tetrahedral pyramids. -- Abstract: Pb 2 Fe 2 O 5 (PFO) powders in monoclinic structure have been synthesized using lead acetate in glycerin and ferric acetylacetonate as the precursor. The powders were pressed into pellets, which were sintered into ceramics at 800 o C for 1 h. The morphology and structure have been determined by X-ray diffraction (XRD) and field emission scanning electron microscopy (FESEM). Polarization was observed in Pb 2 Fe 2 O 5 ceramics at room temperature, exhibiting a clear ferroelectric hysteresis loop. The remanent polarization of Pb 2 Fe 2 O 5 ceramic is estimated to be Pr ∼ 0.22 μC/cm 2 . The origin of the polarization may be attributed to the off-centers of shifted Pb 2+ ions as well as the FeO 6 octahedra in the perovskite-based structure of Pb 2 Fe 2 O 5 . Magnetic hysteresis loop was also observed at room temperature. The Pb 2 Fe 2 O 5 ceramic shows coexistence of ferroelectricity and ferromagnetism. It provides a new field of research for complex oxides with multiferroic properties.

  3. Hydrogen/deuterium fractionation factors of the aqueous ligand of cobalt in Co(H2O)62+ and Co(II)-substituted carbonic anhydrase

    International Nuclear Information System (INIS)

    Kassebaum, J.W.

    1988-01-01

    The author has measured the hydrogen/deuterium fractionation factor for the rapidly exchanging aqueous ligands of cobalt in Co(H 2 O) 6 2+ and in three Co(II)-substituted isozymes of carbonic anhydrase. The fractionation factor was determined from NMR relaxation rates at 300 MHz of the protons of water in mixed solutions of H 2 O and D 2 O containing these complexes. In each case, the paramagnetic contribution to 1/T 2 was greater than to 1/T 1 , consistent with a chemical shift mechanism affecting 1/T 2 . The fractionation factors obtained from T 2 were 0.73 ± 0.02 for Co(H 2 O) 6 2+ , 0.72 ± 0.02 for Co(II)-substituted carbonic anhydrase I, 0.77 ± 0.01 for Co(II)-substituted carbonic anhydrase II, and 1.00 ± 0.07 for Co(Il)-substituted carbonic anhydrase III. He concluded that fractionation factors in these cases determined from T 1 and T 2 measured isotope preferences for different populations of ligand sites. Since T 2 has a large contribution from a chemical shift mechanism, the fractionation factor determined from T 2 has a large contribution of the fractionation of inner shell ligands. The fractionation factor of Co(H 2 O) 6 2+ was used to interpret the solvent hydrogen isotope effects on the formation of complexes of cobalt with the bidentate ligands glycine, N,N-dimethylglycine, and acetylacetone. The contribution of the fractionation factor of the inner water shell in Co(H 2 O) 6 2+ did not account completely for the measured isotope effect, and that the hydrogen/deuterium fractionation of outer shell water makes a large contribution to the isotope effect on the formation of these complexes

  4. Core-shell nanoreactors for efficient aqueous biphasic catalysis.

    Science.gov (United States)

    Zhang, Xuewei; Cardozo, Andrés F; Chen, Si; Zhang, Wenjing; Julcour, Carine; Lansalot, Muriel; Blanco, Jean-François; Gayet, Florence; Delmas, Henri; Charleux, Bernadette; Manoury, Eric; D'Agosto, Franck; Poli, Rinaldo

    2014-11-17

    Water-borne phosphine-functionalized core-cross-linked micelles (CCM) consisting of a hydrophobic core and a hydrophilic shell were obtained as stable latexes by reversible addition-fragmentation chain transfer (RAFT) in water in a one-pot, three-step process. Initial homogeneous aqueous-phase copolymerization of methacrylic acid (MAA) and poly(ethylene oxide) methyl ether methacrylate (PEOMA) is followed by copolymerization of styrene (S) and 4-diphenylphosphinostyrene (DPPS), yielding P(MAA-co-PEOMA)-b-P(S-co-DPPS) amphiphilic block copolymer micelles (M) by polymerization-induced self-assembly (PISA), and final micellar cross-linking with a mixture of S and diethylene glycol dimethacrylate. The CCM were characterized by dynamic light scattering and NMR spectroscopy to evaluate size, dispersity, stability, and the swelling ability of various organic substrates. Coordination of [Rh(acac)(CO)2 ] (acac=acetylacetonate) to the core-confined phosphine groups was rapid and quantitative. The CCM and M latexes were then used, in combination with [Rh(acac)(CO)2 ], to catalyze the aqueous biphasic hydroformylation of 1-octene, in which they showed high activity, recyclability, protection of the activated Rh center by the polymer scaffold, and low Rh leaching. The CCM latex gave slightly lower catalytic activity but significantly less Rh leaching than the M latex. A control experiment conducted in the presence of the sulfoxantphos ligand pointed to the action of the CCM as catalytic nanoreactors with substrate and product transport into and out of the polymer core, rather than as a surfactant in interfacial catalysis. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  5. Dysprosium complexes with the tetraphenylporphyrin macrocyclic ligand

    International Nuclear Information System (INIS)

    Martinez M, V.; Padilla, J.; Ramirez, F.M.

    1992-04-01

    In this report, the results obtained on the synthesis, characterization and study of the chemical behavior of dysprosium complex with the acetylacetone chelating agent (Hacac) and the tetraphenylporphyrin macrocyclic ligand (H 2 TFP) are given. Based on the literature but according to our necessities and interest, the appropriate methodology settled down from the synthesis of prime matters until the obtaining and characterization of the products. The acetyl acetonate complex was obtained of mono hydrated dysprosium [Dy(acac) 3 . H 2 0] and trihydrated [Dy(acac) 3 .3 H 2 0], the mono tetra phenyl porphyrinate [Dy(TFP)(acac). 2 ac] the double sandwich of the dysprosium porphyrinate [Dy(TFP) 2 ] and the triple sandwich of the dysprosium porphyrinate [Dy(TFP) 3 . 2 TCB] (TCB = trichlorobenzene). Its were characterized by their melting points, solubility, IR, UV, TGA and DTA both first and besides the techniques already mentioned for NMR'H, RPE and Magnetic susceptibility the three last complexes. From the spectroscopic point of view, IR and RPE its suggested the existence of a complex of inverse mixed valence [Dy(TFP) 2- (TFP) 1- ] for the Dy(TFP) 2 as a result of the existence of the free radical (TFP' 1- and that it was not in none of the other porphyrin compounds. In the NMR'H spectra of the compounds were not observed signals in the region from 0 to 10 ppm that which shows that the dysprosium complexes in special those of the porphyrin type are highly paramagnetic and its could be used as displacement reagents, creators of images and contrast agents of great utility in these days in studies of NMR, technique today by today used in medical diagnoses. (Author)

  6. Synthesis of monodisperse MFe{sub 2}O{sub 4} (M = Fe and Zn) nanoparticles for polydiethylsiloxane-based ferrofluid with a solvothermal method

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Wei [State Key Laboratory of Optoelectronic Materials and Technologies, Guangdong Provincial Key Laboratory of Photovoltaics Technologies, School of Physics and Engineering, Sun Yat-Sen University, Guangzhou 510275 (China); Laboratory of Nanophotonic Functional Materials and Devices, Institute of Optoelectronic Materials and Technology, South China Normal University, Guangzhou 510631 (China); Zhuang, Lin, E-mail: stszhl@mail.sysu.edu.cn [State Key Laboratory of Optoelectronic Materials and Technologies, Guangdong Provincial Key Laboratory of Photovoltaics Technologies, School of Physics and Engineering, Sun Yat-Sen University, Guangzhou 510275 (China); Zhang, Yong [Laboratory of Nanophotonic Functional Materials and Devices, Institute of Optoelectronic Materials and Technology, South China Normal University, Guangzhou 510631 (China); Shen, Hui [State Key Laboratory of Optoelectronic Materials and Technologies, Guangdong Provincial Key Laboratory of Photovoltaics Technologies, School of Physics and Engineering, Sun Yat-Sen University, Guangzhou 510275 (China)

    2015-09-15

    Highlights: • MFe{sub 2}O{sub 4} nanoparticles were synthesized through a facile solvothermal method. • The relationship between viscosity and temperature of the polydiethylsiloxane-based ferrofluid is discussed. • Fe{sub 3}O{sub 4} nanoparticles have a saturation magnetization of 73.06 emu/g at room temperature. - Abstract: Monodisperse MFe{sub 2}O{sub 4} (M = Fe, Zn) nanoparticles were successfully synthesized for the application of polydiethylsiloxane-based (PDES) ferrofluids (FFs) via a novel solvothermal method, with which 1-octanol and 1-octanamine act as binary solvent, oleic acid (OA) as the surfactant and metal acetylacetonate [M(acac){sub 3}](M = Fe and Zn) as the metal source. X-ray diffractometer confirms that the resultant nanoparticles are pure MFe{sub 2}O{sub 4} with a spinel structure. Infrared spectroscopy indicates that oleic acid is bound to the surface of MFe{sub 2}O{sub 4} through a covalent bond between carboxylate (COO{sup −}) and metal cations. The ratio of 1-octanol and 1-octanamine plays a key role in the formation of the sphere-shaped morphology. Transmission electron microscopy (TEM) images confirm that the Fe{sub 3}O{sub 4} particles are of 4–11 nm with good monodispersity and a narrow size distribution. The saturation magnetization of Fe{sub 3}O{sub 4} nanoparticles with sizes of 7 nm can reach up to 73.06 emu/g. Polydiethylsiloxane-based (PDES) FFs show relatively smaller changes of the viscosity with low temperatures (from −7 to 20 °C) than the polydimethylsiloxane-based (PDMS) FFs. For FFs applications, the relationship between viscosity and temperature is also discussed.

  7. Design, synthesis, characterization, and OFET properties of amphiphilic heteroleptic tris(phthalocyaninato) europium(III) complexes. The effect of crown ether hydrophilic substituents.

    Science.gov (United States)

    Gao, Yingning; Ma, Pan; Chen, Yanli; Zhang, Ying; Bian, Yongzhong; Li, Xiyou; Jiang, Jianzhuang; Ma, Changqin

    2009-01-05

    Two amphiphilic heteroleptic tris(phthalocyaninato) europium complexes with hydrophilic crown ether heads and hydrophobic octyloxy tails [Pc(mCn)(4)]Eu[Pc(mCn)(4)]Eu[Pc(OC(8)H(17))(8)] [m = 12, n = 4, H(2)Pc(12C4)(4) = 2,3,9,10,16,17,23,24-tetrakis(12-crown-4)phthalocyanine; m = 18, n = 6, H(2)Pc(18C6)(4) = 2,3,9,10,16,17,23,24-tetrakis(18-crown-6)phthalocyanine; H(2)Pc(OC(8)H(17))(8) = 2,3,9,10,16,17,23,24-octakis(octyloxy)phthalocyanine] (1, 2) were designed and prepared from the reaction between homoleptic bis(phthalocyaninato) europium compound [Pc(mCn)(4)]Eu[Pc(mCn)(4)] (m = 12, n = 4; m = 18, n = 6) and metal-free H(2)Pc(OC(8)H(17))(8) in the presence of Eu(acac)(3).H(2)O (Hacac = acetylacetone) in boiling 1,2,4-trichlorobenzene. These novel sandwich triple-decker complexes were characterized by a wide range of spectroscopic methods and electrochemically studied. With the help of the Langmuir-Blodgett technique, these typical amphiphilic triple-decker complexes were fabricated into organic field effect transistors (OFET) with top contact configuration on bare SiO(2)/Si substrate, hexamethyldisilazane-treated SiO(2)/Si substrate, and octadecyltrichlorosilane (OTS)-treated SiO(2)/Si substrate, respectively. The device performance is revealed to be dependent on the species of crown ether substituents and substrate surface treatment. OFETs fabricated from the triple decker with 12-crown-4 hydrophilic substituents, 1, allow the hole transfer in the direction parallel to the aromatic phthalocyanine rings. In contrast, the devices of a triple-decker compound containing 18-crown-6 as hydrophilic heads, 2, transfer holes in a direction along the long axis of the assembly composed of face-to-face aggregated triple-decker molecules, revealing the effect of molecular structure, specifically the crown ether substituents on the film structure and OFET functional properties. The carrier mobility for hole as high as 0.33 cm(2) V(-1) s(-1) and current modulation of 7.91 x 10

  8. Thin films of copper oxide and copper grown by atomic layer deposition for applications in metallization systems of microelectronic devices

    Energy Technology Data Exchange (ETDEWEB)

    Waechtler, Thomas

    2010-05-25

    Copper-based multi-level metallization systems in today's ultralarge-scale integrated electronic circuits require the fabrication of diffusion barriers and conductive seed layers for the electrochemical metal deposition. Such films of only several nanometers in thickness have to be deposited void-free and conformal in patterned dielectrics. The envisaged further reduction of the geometric dimensions of the interconnect system calls for coating techniques that circumvent the drawbacks of the well-established physical vapor deposition. The atomic layer deposition method (ALD) allows depositing films on the nanometer scale conformally both on three-dimensional objects as well as on large-area substrates. The present work therefore is concerned with the development of an ALD process to grow copper oxide films based on the metal-organic precursor bis(trin- butylphosphane)copper(I)acetylacetonate [({sup n}Bu{sub 3}P){sub 2}Cu(acac)]. This liquid, non-fluorinated {beta}-diketonate is brought to react with a mixture of water vapor and oxygen at temperatures from 100 to 160 C. Typical ALD-like growth behavior arises between 100 and 130 C, depending on the respective substrate used. On tantalum nitride and silicon dioxide substrates, smooth films and selfsaturating film growth, typical for ALD, are obtained. On ruthenium substrates, positive deposition results are obtained as well. However, a considerable intermixing of the ALD copper oxide with the underlying films takes place. Tantalum substrates lead to a fast self-decomposition of the copper precursor. As a consequence, isolated nuclei or larger particles are always obtained together with continuous films. The copper oxide films grown by ALD can be reduced to copper by vapor-phase processes. If formic acid is used as the reducing agent, these processes can already be carried out at similar temperatures as the ALD, so that agglomeration of the films is largely avoided. Also for an integration with subsequent

  9. Highly efficient white organic light-emitting devices consisting of undoped ultrathin yellow phosphorescent layer

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Shengqiang [State Key Laboratory of Electronic Thin Films and Integrated Devices, School of Optoelectronic Information, University of Electronic Science and Technology of China (UESTC), Chengdu 610054 (China); Yu, Junsheng, E-mail: jsyu@uestc.edu.cn [State Key Laboratory of Electronic Thin Films and Integrated Devices, School of Optoelectronic Information, University of Electronic Science and Technology of China (UESTC), Chengdu 610054 (China); Ma, Zhu; Zhao, Juan [State Key Laboratory of Electronic Thin Films and Integrated Devices, School of Optoelectronic Information, University of Electronic Science and Technology of China (UESTC), Chengdu 610054 (China)

    2013-02-15

    High-efficiency white organic light-emitting devices (WOLEDs) based on an undoped ultrathin yellow light-emitting layer and a doped blue light-emitting layer were demonstrated. While the thickness of blue light-emitting layer, formed by doping a charge-trapping phosphor, iridium(III) bis(4 Prime ,6 Prime -difluorophenylpyridinato)tetrakis(1-pyrazolyl)borate (FIr6) in a wide bandgap host, was kept constant, the thickness of neat yellow emissive layer of novel phosphorescent material, bis[2-(4-tertbutylphenyl)benzothiazolato-N,C{sup 2 Prime }]iridium (acetylacetonate) [(t-bt){sub 2}Ir(acac)] was varied to optimize the device performance. The optimized device exhibited maximum luminance, current efficiency and power efficiency of 24,000 cd/m{sup 2} (at 15.2 V), 79.0 cd/A (at 1550 cd/m{sup 2}) and 40.5 lm/W (at 1000 cd/m{sup 2}), respectively. Besides, the white-light emission covered a wide range of visible spectrum, and the Commission Internationale de l'Eclairage coordinates were (0.32, 0.38) with a color temperature of 5800 K at 8 V. Moreover, high external quantum efficiency was also obtained in the high-efficiency WOLEDs. The performance enhancement was attributed to the proper thickness of (t-bt){sub 2}Ir(acac) layer that enabled adequate current density and enough phosphorescent dye to trap electrons. - Highlights: Black-Right-Pointing-Pointer Highly efficient WOLEDs based on two complementary layers were fabricated. Black-Right-Pointing-Pointer The yellow emissive layer was formed by utilizing undoping system. Black-Right-Pointing-Pointer The blue emissive layer was made by host-guest doping system. Black-Right-Pointing-Pointer The thickness of the yellow emissive layer was varied to make device optimization. Black-Right-Pointing-Pointer The optimized device achieved high power efficiency of 40.5 lm/W.

  10. Nanocrystalline spinel ferrite (MFe{sub 2}O{sub 4}, M = Ni, Co, Mn, Mg, Zn) powders prepared by a simple aloe vera plant-extracted solution hydrothermal route

    Energy Technology Data Exchange (ETDEWEB)

    Phumying, Santi; Labuayai, Sarawuth; Swatsitang, Ekaphan; Amornkitbamrung, Vittaya [Department of Physics, Faculty of Science, Khon Kaen University, Khon Kaen 40002 (Thailand); Integrated Nanotechnology Research Center (INRC), Khon Kaen University, Khon Kaen 40002 (Thailand); Maensiri, Santi, E-mail: santimaensiri@gmail.com [School of Physics, Institute of Science, Suranaree University of Technology, Nakhon Ratchasima 30000 (Thailand)

    2013-06-01

    Graphical abstract: This figure shows the specific magnetization curves of the as-prepared MFe{sub 2}O{sub 4} (M = Ni, Co, Mn, Mg, Zn) powders obtained from room temperature VSM measurement. These curves are typical for a soft magnetic material and indicate hysteresis ferromagnetism in the field ranges of ±500 Oe, ±1000 Oe, and ±2000 Oe for the CoFe{sub 2}O{sub 4}, MgFe{sub 2}O{sub 4} and MnFe{sub 2}O{sub 4} respectively, whereas the samples of NiFe{sub 2}O{sub 4} and ZnFe{sub 2}O{sub 4} show a superparamagnetic behavior. Highlights: ► Nanocrystalline MFe{sub 2}O{sub 4} powders were synthesized by a novel hydrothermal method. ► Metal acetylacetonates and aloe vera plant-extracted solution are used. ► This biosynthetic route is very simple and provides high-yield oxide nanomaterials. ► XRD and TEM results indicate that the prepared samples have only spinel structure. ► The maximum M{sub s} of 68.9 emu/g at 10 kOe were observed for the samples of MnFe{sub 2}O{sub 4}. - Abstract: Nanocrystalline spinel ferrite MFe{sub 2}O{sub 4} (M = Ni, Co, Mn, Mg, Zn) powders were synthesized by a novel hydrothermal method using Fe(acac){sub 3}, M(acac){sub 3} (M = Ni, Co, Mn, Mg, Zn) and aloe vera plant extracted solution. The X-ray diffraction and selected-area electron diffraction results indicate that the synthesized nanocrystalline have only spinel structure without the presence of other phase impurities. The crystal structure and morphology of the spinel ferrite powders, as revealed by TEM, show that the NiFe{sub 2}O{sub 4} and CoFe{sub 2}O{sub 4} samples contain nanoparticles, whereas the MnFe{sub 2}O{sub 4} and MgFe{sub 2}O{sub 4} samples consist of many nanoplatelets and nanoparticles. Interestingly, the ZnFe{sub 2}O{sub 4} sample contains plate-like structure of networked nanocrystalline particles. Room temperature magnetization results show a ferromagnetic behavior of the CoFe{sub 2}O{sub 4}, MnFe{sub 2}O{sub 4} and MgFe{sub 2}O{sub 4} samples, whereas the

  11. Thin films of copper oxide and copper grown by atomic layer deposition for applications in metallization systems of microelectronic devices

    Energy Technology Data Exchange (ETDEWEB)

    Waechtler, Thomas

    2010-05-25

    Copper-based multi-level metallization systems in today's ultralarge-scale integrated electronic circuits require the fabrication of diffusion barriers and conductive seed layers for the electrochemical metal deposition. Such films of only several nanometers in thickness have to be deposited void-free and conformal in patterned dielectrics. The envisaged further reduction of the geometric dimensions of the interconnect system calls for coating techniques that circumvent the drawbacks of the well-established physical vapor deposition. The atomic layer deposition method (ALD) allows depositing films on the nanometer scale conformally both on three-dimensional objects as well as on large-area substrates. The present work therefore is concerned with the development of an ALD process to grow copper oxide films based on the metal-organic precursor bis(trin- butylphosphane)copper(I)acetylacetonate [({sup n}Bu{sub 3}P){sub 2}Cu(acac)]. This liquid, non-fluorinated {beta}-diketonate is brought to react with a mixture of water vapor and oxygen at temperatures from 100 to 160 C. Typical ALD-like growth behavior arises between 100 and 130 C, depending on the respective substrate used. On tantalum nitride and silicon dioxide substrates, smooth films and selfsaturating film growth, typical for ALD, are obtained. On ruthenium substrates, positive deposition results are obtained as well. However, a considerable intermixing of the ALD copper oxide with the underlying films takes place. Tantalum substrates lead to a fast self-decomposition of the copper precursor. As a consequence, isolated nuclei or larger particles are always obtained together with continuous films. The copper oxide films grown by ALD can be reduced to copper by vapor-phase processes. If formic acid is used as the reducing agent, these processes can already be carried out at similar temperatures as the ALD, so that agglomeration of the films is largely avoided. Also for an integration with subsequent

  12. Surface defects on the Gd{sub 2}Zr{sub 2}O{sub 7} oxide films grown on textured NiW technical substrates by chemical solution method

    Energy Technology Data Exchange (ETDEWEB)

    Zhao, Y., E-mail: yuezhao@sjtu.edu.cn [School of Electronic Information and Electrical Engineering, Shanghai Jiao Tong University, 200240 Shanghai (China); Department of Energy Conversion and Storage, Technical University of Denmark, 4000 Roskilde (Denmark); Opata, Yuri A. [Department of Energy Conversion and Storage, Technical University of Denmark, 4000 Roskilde (Denmark); Wu, W. [School of Electronic Information and Electrical Engineering, Shanghai Jiao Tong University, 200240 Shanghai (China); Grivel, J.C. [Department of Energy Conversion and Storage, Technical University of Denmark, 4000 Roskilde (Denmark)

    2017-02-15

    Epitaxial growth of oxide thin films has attracted much interest because of their broad applications in various fields. In this study, we investigated the microstructure of textured Gd{sub 2}Zr{sub 2}O{sub 7} films grown on (001)〈100〉 orientated NiW alloy substrates by a chemical solution deposition (CSD) method. The aging effect of precursor solution on defect formation was thoroughly investigated. A slight difference was observed between the as-obtained and aged precursor solutions with respect to the phase purity and global texture of films prepared using these solutions. However, the surface morphologies are different, i.e., some regular-shaped regions (mainly hexagonal or dodecagonal) were observed on the film prepared using the as-obtained precursor, whereas the film prepared using the aged precursor exhibits a homogeneous structure. Electron backscatter diffraction and scanning electron microscopy analyses showed that the Gd{sub 2}Zr{sub 2}O{sub 7} grains present within the regular-shaped regions are polycrystalline, whereas those present in the surrounding are epitaxial. Some polycrystalline regions ranging from several micrometers to several tens of micrometers grew across the NiW grain boundaries underneath. To understand this phenomenon, the properties of the precursors and corresponding xerogel were studied by Fourier transform infrared spectroscopy and coupled thermogravimetry/differential thermal analysis. The results showed that both the solutions mainly contain small Gd−Zr−O clusters obtained by the reaction of zirconium acetylacetonate with propionic acid during the precursor synthesis. The regular-shaped regions were probably formed by large Gd−Zr−O frameworks with a metastable structure in the solution with limited aging time. This study demonstrates the importance of the precise control of chemical reaction path to enhance the stability and homogeneity of the precursors of the CSD route. - Highlights: •We investigate microstructure

  13. Different apoptotic effects of [Pt(O,O'-acac)(γ-acac)(DMS)] and cisplatin on normal and cancerous human epithelial breast cells in primary culture.

    Science.gov (United States)

    Vetrugno, Carla; Muscella, Antonella; Fanizzi, Francesco Paolo; Cossa, Luca Giulio; Migoni, Danilo; De Pascali, Sandra Angelica; Marsigliante, Santo

    2014-11-01

    The aim of this study was to determine whether [platinum (Pt)(O,O'-acetylacetonate (acac))(γ-acac)(dimethylsulphide (DMS))] is differentially cytotoxic in normal and cancer cells, and to measure comparative levels of cytotoxicity compared with cisplatin in the same cells. We performed experiments on cancerous and normal epithelial breast cells in primary culture obtained from the same patients. The apoptotic effects [Pt(O,O'-acac)(γ-acac)(DMS)] and cisplatin in cancerous and normal breast cells were compared. Cancer cells were more sensitive to [Pt(O,O'-acac)(γ-acac)(DMS)] (IC50 = 5.22 ± 1.2 μmol·L(-1)) than normal cells (IC50 = 116.9 ± 8.8 μmol·L(-1)). However, the difference was less strong when cisplatin was used (IC50 = 96.0 ± 6.9 and 61.9 ± 6.1 μmol·L(-1) for cancer and normal cells respectively). Both compounds caused reactive oxygen species (ROS) production with different mechanisms: [Pt(O,O'-acac)(γ-acac)(DMS)] quickly activated NAD(P)H oxidase while cisplatin caused a slower formation of mitochondrial ROS. Cisplatin and [Pt(O,O'-acac)(γ-acac)(DMS)] caused activation of caspases, proteolysis of PARP and modulation of Bcl-2, Bax and Bid. [Pt(O,O'-acac)(γ-acac)(DMS)] also caused leakage of cytochrome c from the mitochondria. Overall, these processes proceeded more quickly in cells treated with [Pt(O,O'-acac)(γ-acac)(DMS)] compared with cisplatin. [Pt(O,O'-acac)(γ-acac)(DMS)] effects were faster and quantitatively greater in cancer than in normal cells. [Pt(O,O'-acac)(γ-acac)(DMS)] caused a fast decrease of mitochondrial membrane potential, especially in cancer cells. [Pt(O,O'-acac)(γ-acac)(DMS)] was specific to breast cancer cells in primary culture, and this observation makes this compound potentially more interesting than cisplatin. © 2014 The British Pharmacological Society.

  14. Different apoptotic effects of [Pt(O,O′-acac)(γ-acac)(DMS)] and cisplatin on normal and cancerous human epithelial breast cells in primary culture

    Science.gov (United States)

    Vetrugno, Carla; Muscella, Antonella; Fanizzi, Francesco Paolo; Cossa, Luca Giulio; Migoni, Danilo; De Pascali, Sandra Angelica; Marsigliante, Santo

    2014-01-01

    Background and Purpose The aim of this study was to determine whether [platinum (Pt)(O,O′-acetylacetonate (acac))(γ-acac)(dimethylsulphide (DMS))] is differentially cytotoxic in normal and cancer cells, and to measure comparative levels of cytotoxicity compared with cisplatin in the same cells. Experimental Approach We performed experiments on cancerous and normal epithelial breast cells in primary culture obtained from the same patients. The apoptotic effects [Pt(O,O′-acac)(γ-acac)(DMS)] and cisplatin in cancerous and normal breast cells were compared. Key Results Cancer cells were more sensitive to [Pt(O,O′-acac)(γ-acac)(DMS)] (IC50 = 5.22 ± 1.2 μmol·L−1) than normal cells (IC50 = 116.9 ± 8.8 μmol·L−1). However, the difference was less strong when cisplatin was used (IC50 = 96.0 ± 6.9 and 61.9 ± 6.1 μmol·L−1 for cancer and normal cells respectively). Both compounds caused reactive oxygen species (ROS) production with different mechanisms: [Pt(O,O′-acac)(γ-acac)(DMS)] quickly activated NAD(P)H oxidase while cisplatin caused a slower formation of mitochondrial ROS. Cisplatin and [Pt(O,O′-acac)(γ-acac)(DMS)] caused activation of caspases, proteolysis of PARP and modulation of Bcl-2, Bax and Bid. [Pt(O,O′-acac)(γ-acac)(DMS)] also caused leakage of cytochrome c from the mitochondria. Overall, these processes proceeded more quickly in cells treated with [Pt(O,O′-acac)(γ-acac)(DMS)] compared with cisplatin. [Pt(O,O′-acac)(γ-acac)(DMS)] effects were faster and quantitatively greater in cancer than in normal cells. [Pt(O,O′-acac)(γ-acac)(DMS)] caused a fast decrease of mitochondrial membrane potential, especially in cancer cells. Conclusions and Implications [Pt(O,O′-acac)(γ-acac)(DMS)] was specific to breast cancer cells in primary culture, and this observation makes this compound potentially more interesting than cisplatin. PMID:24990093

  15. Electronic state of ruthenium deposited onto oxide supports: An XPS study taking into account the final state effects

    International Nuclear Information System (INIS)

    Larichev, Yurii V.; Moroz, Boris L.; Bukhtiyarov, Valerii I.

    2011-01-01

    The electronic state of ruthenium in the supported Ru/EO x (EO x = MgO, Al 2 O 3 or SiO 2 ) catalysts prepared by with the use of Ru(OH)Cl 3 or Ru(acac) 3 (acac = acetylacetonate) and reduced with H 2 at 723 K is characterized by X-ray photoelectron spectroscopy (XPS) in the Ru 3d, Cl 2p and O 1s regions. The influence of the final state effects (the differential charging and variation of the relaxation energy) on the binding energy (BE) of Ru 3d 5/2 core level measured for supported Ru nanoparticles is estimated by comparison of the Fermi levels and the modified Auger parameters determined for the Ru/EO x samples with the corresponding characteristics of the bulk Ru metal. It is found that the negative shift of the Ru 3d 5/2 peak which is observed in the spectrum of ruthenium deposited onto MgO (BE = 279.5-279.7 eV) with respect to that of Ru black (BE = 280.2 eV) or ruthenium supported on γ-Al 2 O 3 and SiO 2 (BE = 280.4 eV) is caused not by the transfer of electron density from basic sites of MgO, as considered earlier, but by the differential charging of the supported Ru particles compared with the support surface. Correction for the differential charging value reveals that the initial state energies of ruthenium in the Ru/EO x systems are almost identical (BE = 280.5 ± 0.1 eV) irrespectively of acid-base properties of the support, the mean size of supported Ru crystallites (within the range of 2-10 nm) and the surface Cl content. The results obtained suggest that the difference in ammonia synthesis activity between the Ru catalysts supported on MgO and on the acidic supports is accounted for by not different electronic state of ruthenium on the surface of these oxides but by some other reasons.

  16. Neutron activation of microspheres containing 165Ho: theoretical and experimental radionuclidic impurities study

    International Nuclear Information System (INIS)

    Squair, Peterson L.; Pozzo, Lorena; Ivanov, Evandro; Osso Junior, Joao A.

    2011-01-01

    The 166 Ho microspheres are potentially interesting for medical applications for treatment of many tumors. The internal radionuclide therapy can use polymer or glass device that provides structural support for the radionuclide. After activation, beta minus emission of 166 Ho (T 1/2 =26.8h, β - E max =1.84 MeV, γ E p =80.6 keV) can be used for therapeutic purposes. The aim of this work is study the influence of radionuclide impurities between End of Bombardment (EOB) and the medical application. The appropriate specific activities and purity along decay should be adequate for their safe and efficient medical applications. The good practices on neutron activation techniques are choice a high purity target to avoid production of undesirable radionuclides and when possible with enriched targets to obtain higher specific activity. In this work the target used was Ho 2 O 3 and polymeric microspheres containing holmium acetylacetonate (HoAcAc) manufactured at the Biotechnology Center-IPEN/CNEN-SP. Three conditions were evaluated: preliminary test with 1.0x10 13 n.cm -2 s -1 for 1.0 hour; nowadays maximum capability of IEA-R1 reactor with 5.0x10 13 n.cm -2 s -1 for 64.0 hours and the ideal IEA-R1 operation with 5.0x10 13 n.cm -2 s -1 for 120.0 hours. Considering the sample with 99.9% 165 Ho purity and 0.1% for each impurities elements with its natural abundance, the highest radionuclidic impurity is the Lutetium followed by Ytterbium, Lanthanum and Cerium. The intrinsic radionuclidic impurity of 166 mHo is less relevant. This review is important to identify the radionuclidic purity characteristics of the preliminary studies with different time and flux irradiation. The data produced in this paper will help to define strategies for the production of 166 Ho radioisotope at IEA-R1 IPEN/CNEN-SP reactor. (author)

  17. Influence of different TiO{sub 2} blocking films on the photovoltaic performance of perovskite solar cells

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Chenxi; Luo, Yudan; Chen, Xiaohong, E-mail: xhchen@phy.ecnu.edu.cn; Ou-Yang, Wei; Chen, Yiwei; Sun, Zhuo; Huang, Sumei, E-mail: smhuang@phy.ecnu.edu.cn

    2016-12-01

    Highlights: • TiO{sub 2} blocking layer (BL) was synthesized using various methods. • Effect of BL characteristics on performance of perovskite solar cell was studied. • Charge transfer kinetics of perovskite solar cells with different BLs was explored. • We demonstrated efficient solar cells employing chemical bath deposition based BLs. - Abstract: Organolead trihalide perovskite materials have been successfully used as light absorbers in efficient photovoltaic (PV) cells. Cell structures based on mesoscopic metal oxides and planar heterojunctions have already demonstrated very impressive and brisk advances, holding great potential to grow into a mature PV technology. High power conversion efficiency (PCE) values have been obtained from the mesoscopic configuration in which a few hundred nano-meter thick mesoporous scaffold (e.g. TiO{sub 2} or Al{sub 2}O{sub 3}) infiltrated by perovskite absorber was sandwiched between the electron and hole transport layers. A uniform and compact hole-blocking layer is necessary for high efficient perovskite-based thin film solar cells. In this study, we investigated the characteristics of TiO{sub 2} compact layer using various methods and its effects on the PV performance of perovskite solar cells. TiO{sub 2} compact layer was prepared by a sol-gel method based on titanium isopropoxide and HCl, spin-coating of titanium diisopropoxide bis (acetylacetonate), screen-printing of Dyesol’s bocking layer titania paste, and a chemical bath deposition (CBD) technique via hydrolysis of TiCl{sub 4}, respectively. The morphological and micro-structural properties of the formed compact TiO{sub 2} layers were characterized by scanning electronic microscopy and X-ray diffraction. The analyses of devices performance characteristics showed that surface morphologies of TiO{sub 2} compact films played a critical role in affecting the efficiencies. The nanocrystalline TiO{sub 2} film deposited via the CBD route acts as the most efficient

  18. Preparation of hydrotalcite compounds using ultrasound irradiation to capture CO{sub 2}; Preparacion de compuestos tipo hidrotalcita utilizando irradiacion de ultrasonido para la captura de CO{sub 2}

    Energy Technology Data Exchange (ETDEWEB)

    Martinez, J.A.J.; Paredes, S.P.; Valenzuela, M.A.; Hernandez, M.L. [Instituto Politecnico Nacional, ESIQIE, Mexico, D.F. (Mexico)]. E-mail: sparedesc@ipn.com.mx

    2009-09-15

    Al-Mg hydrotalcite compounds (HTC) were prepared using co-precipitation, sol-gel and reconstruction of the structure with ultrasound-assisted irradiation. The interlaminar components for each method were nitrate, acetylacetonate ethoxide and metavanadate, respectively. Optimization of the synthesis was performed using x-ray diffraction. The effect of the different parameters on synthesis was studied, including pH, time and ultrasound irradiation power. In addition, for the reconstruction method, temperature and calcination time were evaluated. For all methods, ultrasound-assisted methods were found to be more efficient and economical than conventional methods reported (autoclave). They also have the advantage of being able to control properties such as crystallinity, porosity and the specific surface, which significantly depends on the preparation method, irradiation time and type of interlaminar component. These methods are intended to synthesize interlaminar anionic materials that are very scarce in nature with better properties than traditional adsorbents used for the capture of CO{sub 2}. [Spanish] Se prepararon compuestos tipo hidrotalcita Al-Mg por los metodos de: coprecipitacion, sol gel y reconstruccion de la estructura asistidos por irradiacion de ultrasonido. Los componentes interlaminares para cada metodo fueron respectivamente: nitrato, etoxido-acetilacetonato y metavanadato. La optimizacion de la sintesis, se efectuo mediante difraccion de rayos-X. Se estudio el efecto de diversos parametros en la sintesis: pH, tiempo y potencia de irradiacion de ultrasonido, ademas, para el metodo de reconstruccion se evaluaron la temperatura y el tiempo de calcinacion. En todos los casos se encontro que el empleo de metodos asistidos por ultrasonido resultan ser mas eficientes y economicos que los metodos convencionales reportados (autoclave), ademas tienen la ventaja, de poder controlar propiedades tales como: la cristalinidad, la porosidad y la superficie

  19. Nanocrystalline spinel ferrite (MFe2O4, M = Ni, Co, Mn, Mg, Zn) powders prepared by a simple aloe vera plant-extracted solution hydrothermal route

    International Nuclear Information System (INIS)

    Phumying, Santi; Labuayai, Sarawuth; Swatsitang, Ekaphan; Amornkitbamrung, Vittaya; Maensiri, Santi

    2013-01-01

    Graphical abstract: This figure shows the specific magnetization curves of the as-prepared MFe 2 O 4 (M = Ni, Co, Mn, Mg, Zn) powders obtained from room temperature VSM measurement. These curves are typical for a soft magnetic material and indicate hysteresis ferromagnetism in the field ranges of ±500 Oe, ±1000 Oe, and ±2000 Oe for the CoFe 2 O 4 , MgFe 2 O 4 and MnFe 2 O 4 respectively, whereas the samples of NiFe 2 O 4 and ZnFe 2 O 4 show a superparamagnetic behavior. Highlights: ► Nanocrystalline MFe 2 O 4 powders were synthesized by a novel hydrothermal method. ► Metal acetylacetonates and aloe vera plant-extracted solution are used. ► This biosynthetic route is very simple and provides high-yield oxide nanomaterials. ► XRD and TEM results indicate that the prepared samples have only spinel structure. ► The maximum M s of 68.9 emu/g at 10 kOe were observed for the samples of MnFe 2 O 4 . - Abstract: Nanocrystalline spinel ferrite MFe 2 O 4 (M = Ni, Co, Mn, Mg, Zn) powders were synthesized by a novel hydrothermal method using Fe(acac) 3 , M(acac) 3 (M = Ni, Co, Mn, Mg, Zn) and aloe vera plant extracted solution. The X-ray diffraction and selected-area electron diffraction results indicate that the synthesized nanocrystalline have only spinel structure without the presence of other phase impurities. The crystal structure and morphology of the spinel ferrite powders, as revealed by TEM, show that the NiFe 2 O 4 and CoFe 2 O 4 samples contain nanoparticles, whereas the MnFe 2 O 4 and MgFe 2 O 4 samples consist of many nanoplatelets and nanoparticles. Interestingly, the ZnFe 2 O 4 sample contains plate-like structure of networked nanocrystalline particles. Room temperature magnetization results show a ferromagnetic behavior of the CoFe 2 O 4 , MnFe 2 O 4 and MgFe 2 O 4 samples, whereas the samples of NiFe 2 O 4 and ZnFe 2 O 4 exhibit a superparamagnetic behavior

  20. Influence of the process parameters on the spray pyrolysis technique, on the synthesis of gadolinium doped-ceria thin film

    International Nuclear Information System (INIS)

    Halmenschlager, C.M.; Neagu, R.; Rose, L.; Malfatti, C.F.; Bergmann, C.P.

    2013-01-01

    Graphical abstract: Gas-tight CGO made by spray pyrolysis suitable to be used as SOFC electrolyte. Display Omitted Highlights: ► Dense and crystalline CGO films deposited by spray pyrolysis on various substrates. ► Solvent did not have a strong influence on the film microstructure, defect concentration or thickness. ► The substrate did not have a strong influence on the film microstructure, defect concentration or thickness. ► Films with at least 2.5 μm of thickness presented high impermeability. ► The films obtained are suitable to use as a SOFC electrolyte. -- Abstract: This work presents the results of a process of optimization applied to gadolinia-doped ceria (Ce 0.8 Gd 0.2 O 1.9−x , or CGO) thin films, deposited by spray pyrolysis (SP). Spray pyrolysis is a high thermal deposition method that combines material deposition and heat treatment. This combination is advantageous since the post-deposition heat treatment step is not necessary. However, stresses are solidified in the coating during the deposition, which may lead to the initiation of a crack in the coating. The aim of this work was to achieve thin, dense, and continuous CGO coatings, which may be used as gas separation membranes and as a solid state electrochemical interfaces. Dense, flat, low-defect substrates such as silica slides, silicon mono crystal wafers, and porous substrates were used as substrates in this work. Cerium ammonium nitrate and gadolinium acetylacetonate were dissolved in ethanol and butyl carbitol to form a precursor solution that was sprayed on the heated substrates. Process parameters such as solvent composition, deposition rate and different heating regimes were analyzed. The microstructure was analyzed by secondary electron microscopy (SEM) and was found that thin, dense, and defect-free films could be produced on dense and porous substrates. The results obtained show that it is possible to obtain a CGO dense film deposited by spray pyrolysis. X-ray diffraction