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Sample records for acetylacetone

  1. Photochemical transformation of vanadium(5) acetylacetonate complexes

    Energy Technology Data Exchange (ETDEWEB)

    Kuchmij, S.Ya.; Turchaninov, A.M.; Kryukov, A.I. (AN Ukrainskoj SSR, Kiev. Inst. Fizicheskoj Khimii)

    1980-08-01

    Photochemical transformations of mixed vanadium (5) complex formed as a result of interaction between ethylorthovanadate and acetylacetone which includes in the first coordination sphere vanadyl oxygen, two enolate-ions and enthoxygroup are studied spectrophotometrically and using ESR method. During irradiation of ethanol solutions of the complex a successive reduction of central atom with formation of acetyl-acetonate complexes of vanadium (4) and (3) takes place. At that the solvent is oxidated. In CCl/sub 4/ solution under the effect of UV irradiation ethoxygroup is replaced by chlorine ion with the formation of new mixed vanadium (5) complex, sensible to visible and UV radiation.

  2. Acetone and the precursor ligand acetylacetone : distinctly different electron beam induced decomposition?

    NARCIS (Netherlands)

    Warneke, Jonas; Van Dorp, Willem F.; Rudolf, Petra; Stano, Michal; Papp, Peter; Matejcik, Stefan; Borrmann, Tobias; Swiderek, Petra

    2015-01-01

    In focused electron beam induced deposition (FEBID) acetylacetone plays a role as a ligand in metal acetylacetonate complexes. As part of a larger effort to understand the chemical processes in FEBID, the electron-induced reactions of acetylacetone were studied both in condensed layers and in the ga

  3. The Electrochemical Synthesis of Transition-Metal Acetylacetonates

    Science.gov (United States)

    Long, S. R.; Browning, S. R.; Lagowski, J. J.

    2008-01-01

    The electrochemical synthesis of transition-metal acetylacetonates described here can form the basis of assisting in the transformation of an entry-level laboratory course into a research-like environment where all members of a class are working on the same problem, but where each member has a personal responsibility for the synthesis and…

  4. Infrared and Near-Infrared Spectroscopy of Acetylacetone and Hexafluoroacetylacetone.

    Science.gov (United States)

    Howard, Daryl L; Kjaergaard, Henrik G; Huang, Jing; Meuwly, Markus

    2015-07-23

    The infrared and near-infrared spectra of acetylacetone, acetylacetone-d8, and hexafluoroacetylacetone are characterized from experiment and computations at different levels. In the fundamental region, the intramolecular hydrogen bonded OH-stretching transition is clearly observed as a very broad band with substantial structure and located at significantly lower frequency compared to common OH-stretching frequencies. There is no clear evidence for OH-stretching overtone transitions in the near-infrared region, which is dominated by the CH-stretching overtones of the methine and methyl CH bonds. From molecular dynamics (MD) simulations, with a potential energy surface previously validated for tunneling splittings, the infrared spectra are determined and used in assigning the experimentally measured ones. It is found that the simulated spectrum in the region associated with the proton transfer mode is exquisitely sensitive to the height of the barrier for proton transfer. Comparison of the experimental and the MD simulated spectra establishes that the barrier height is around 2.5 kcal/mol, which favorably compares with 3.2 kcal/mol obtained from high-level electronic structure calculations.

  5. Solvents and supporting electrolytes for vanadium acetylacetonate flow batteries

    Science.gov (United States)

    Shinkle, Aaron A.; Pomaville, Timothy J.; Sleightholme, Alice E. S.; Thompson, Levi T.; Monroe, Charles W.

    2014-02-01

    Properties of supporting electrolytes and solvents were examined for use with vanadium acetylacetonate - a member of the class of metal(β-diketonate) active species - in non-aqueous redox flow batteries. Twenty supporting-electrolyte/solvent combinations were screened for ionic conductivity and supporting-electrolyte solubility. Hexane, tetrahydrofuran, and dimethylcarbonate solvents did not meet minimal conductivity and solubility criteria for any of the electrolytes used, which included tetraethylammonium tetrafluoroborate, tetrabutylammonium tetrafluoroborate, tetrabutylammonium hexafluorophosphate, and (1-butyl, 3-methyl)imidazolium bis(trifluoromethanesulfonyl)imide. Ionic conductivities and solubilities for solutions of these electrolytes passed screening criteria in acetonitrile and dimethylformamide solvents, in which maximum supporting-electrolyte and active-species solubilities were determined. Active-species electrochemistry was found to be reversible in several solvent/support systems; for some systems the voltammetric signatures of unwanted side reactions were suppressed. Correlations between supporting-solution properties and performance metrics suggest that an optimal solvent for a vanadium acetylacetonate RFB should have a low solvent molar volume for active-species solubility, and a high Hansen polarity for conductivity.

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

    CERN Document Server

    Ito, Y

    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.

  7. UV Spectral Analysis of the Chemical Modification and Photolysis of Acetylacetone Modified Alumina Aqueous Solution

    Institute of Scientific and Technical Information of China (English)

    Chengbin JING; Xiujian ZHAO; Haizheng TAO; Xina WANG; Aiyun LIU

    2004-01-01

    Acetylacetone was firstly introduced into the aqueous media with the presence of aluminum sec-butoxide and peptizator. It was confirmed that the UV (ultraviolet) absorption band of acetylacetone underwent 14 nm of red-shift due to the formation of the six-membered ring of the complex between alumina and acetylacetone in the aqueous solution. It was also found that the chemical modification can be dissociated by the UV irradiation with a wavelength shorter than 286 nm as a result of the excitation of π-π* transition in the complex.

  8. CAN Catalyzed Preparation of β-Enamino Ketones from Amines and Acetylacetone

    Institute of Scientific and Technical Information of China (English)

    Zheng DUAN; Ting LI; Xue Jie XUAN; Yang Jie WU

    2006-01-01

    A variety of β-enamino ketones were synthesized in high to excellent yields by reacting acetylacetone with amines in the presence of a catalytic amount of cerium(Ⅳ) ammonium nitrate(CAN) under ultrasonic irradiation.

  9. 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.

  10. Lanthanide Complexes with Acetylacetonate and 5,10,15,20-Tetra[para-(4-chlorobenzoyloxy)phenyl]porphyrin

    Institute of Scientific and Technical Information of China (English)

    2000-01-01

    @@ The lanthanide complexes of acetylacetonate and 5,10,15,20-tetra[para-(chlorobenzoyloxy)phenyl]porphyrin having a general formula Ln[(cbop)4p]acac(where Ln=Tb,Ho,Er,Tm;cbop=(4-chlorobenzoyloxy)phenyl;Hacac=acetylacetone;p=porphyrin) were prepared and characterized.The structure of the complexs was proposed.

  11. Radioactive Holmium Acetylacetonate Microspheres for Interstitial Microbrachytherapy: An In Vitro and In Vivo Stability Study

    NARCIS (Netherlands)

    Bult, W.; De Leeuw, H.; Steinebach, O.M.; Van der Bom, M.J.; Wolterbeek, H.T.; Heeren, R.M.A.; Bakker, C.J.G.; Van het Schip, A.D.; Hennink, W.E.; Nijsen, F.W.

    2011-01-01

    Purpose The clinical application of holmium acetylacetonate microspheres (HoAcAcMS) for the intratumoral radionuclide treatment of solid malignancies requires a thorough understanding of their stability. Therefore, an in vitro and an in vivo stability study with HoAcAcMS was conducted. Methods

  12. Radioactive holmium acetylacetonate microspheres for interstitial microbrachytherapy : an in vitro and in vivo stability study

    NARCIS (Netherlands)

    Bult, Wouter; de Leeuw, Hendrik; Steinebach, Olav M; van der Bom, Martijn J; Wolterbeek, Hubert Th; Heeren, Ron M A; Bakker, Chris J G; van Het Schip, Alfred D; Hennink, Wim E; Nijsen, J Frank W

    2012-01-01

    PURPOSE: The clinical application of holmium acetylacetonate microspheres (HoAcAcMS) for the intratumoral radionuclide treatment of solid malignancies requires a thorough understanding of their stability. Therefore, an in vitro and an in vivo stability study with HoAcAcMS was conducted. METHODS: HoA

  13. Operando study of iridium acetylacetonate decomposition on amorphous silica-alumina for bifunctional catalyst preparation.

    Science.gov (United States)

    Nassreddine, Salim; Bergeret, Gérard; Jouguet, Bernadette; Geantet, Christophe; Piccolo, Laurent

    2010-07-28

    The decomposition of iridium acetylacetonate Ir(acac)(3) impregnated on amorphous silica-alumina (ASA) has been investigated by combined thermogravimetry-differential thermal analysis-mass spectrometry (TG-DTA-MS) and by in situ X-ray diffraction (XRD). The resulting Ir/ASA hydrotreating catalysts have also been characterized by transmission electron microscopy (TEM). The effects of heating treatments under oxidative, reductive or inert gas flows are compared with each other and with similar experiments on ASA-supported acetylacetone (acacH). It is shown that Ir(acac)(3) undergoes exothermic combustion during calcination in air, leading to agglomerated IrO(2) particles. Conversely, direct reduction involves hydrogenolysis of the acac followed by hydrogenation of the ligand residues to alkanes and water. These two processes are catalyzed by Ir clusters, the gradual growth of which is followed in situ by XRD. The resulting nanoparticles are highly and homogeneously dispersed.

  14. STUDIES ON THE INITIATION MECHANISM OF CERIC ION AND ACETYLACETONE REDOX SYSTEM IN VINYL POLYMERIZATION

    Institute of Scientific and Technical Information of China (English)

    QIU Kunyuan; GUO Xinqiu; ZHANG Dong; FENG Xinde

    1991-01-01

    The initiation mechanism of acrylamide (AAM)polymerization using ceric ion/acetylacetone system as an initiator has been studied. The redox polymerization was revealed by the low value of overall activation energy ofAAm polymerization. The structure of free radicals formed from above-mentioned initiation sytem were detected by radical trapping and ESR spectra techniques and the end groups of polymers obtained were determined by FT-IR spectra analysis method. Based on these results the initiation mechanism is proposed.

  15. Metal Acetylacetonates as General Precursors for the Synthesis of Early Transition Metal Oxide Nanomaterials

    Directory of Open Access Journals (Sweden)

    Amanda L. Willis

    2007-01-01

    Full Text Available A versatile, convenient, and nontoxic solvothermal method for the synthesis of nanocrystalline iron, chromium, and manganese oxides is described. This method employs the reactions of metal acetylacetonate precursors and oxygen-containing solvents in a reaction to prepare metal oxide nanoparticles. Characterization of these nanocrystalline materials was carried out employing transmission electron microscopy (TEM, high-resolution TEM (HRTEM, X-ray diffraction (XRD, and elemental analysis.

  16. Metal Acetylacetonates as General Precursors for the Synthesis of Early Transition Metal Oxide Nanomaterials

    OpenAIRE

    Willis, Amanda L.; Zhuoying Chen; Jiaqing He; Yimei Zhu; Turro, Nicholas J.; Stephen O'Brien

    2007-01-01

    A versatile, convenient, and nontoxic solvothermal method for the synthesis of nanocrystalline iron, chromium, and manganese oxides is described. This method employs the reactions of metal acetylacetonate precursors and oxygen-containing solvents in a reaction to prepare metal oxide nanoparticles. Characterization of these nanocrystalline materials was carried out employing transmission electron microscopy (TEM), high-resolution TEM (HRTEM), X-ray diffraction (XRD), and elemental analysis.

  17. Double deuterated acetylacetone in neon matrices: infrared spectroscopy, photoreactivity and the tunneling process.

    Science.gov (United States)

    Gutiérrez-Quintanilla, Alejandro; Chevalier, Michèle; Crépin, Claudine

    2016-07-27

    The effect of deuteration of acetylacetone (C5O2H8) is explored by means of IR spectroscopy of its single and double deuterated isotopologues trapped in neon matrices. The whole vibrational spectra of chelated enols are very sensitive to the H-D exchange of the hydrogen atom involved in the internal hydrogen bond. UV excitation of double deuterated acetylacetone isolated in neon matrices induces the formation of four open enol isomers which can be divided into two groups of two conformers, depending on their formation kinetics. Within each group, one conformer is more stable than the other: slow conformer interconversion due to a tunneling process is observed in the dark at low temperature. Moreover, IR laser irradiation at the OD stretching overtone frequency is used to induce interconversion either from the most stable to the less stable conformer or the opposite, depending on the excitation wavelength. The interconversion process is of great help to assign conformers which are definitively identified by comparison between experimental and calculated IR spectra. Kinetic constants of the tunneling process at play are theoretically estimated and agree perfectly with experiments, including previous experiments with the totally hydrogenated acetylacetone [Lozada García et al., Phys. Chem. Chem. Phys., 2012, 14, 3450].

  18. Performance and Characterization for Blend Membrane of PES with Manganese(III Acetylacetonate as Metalorganic Nanoparticles

    Directory of Open Access Journals (Sweden)

    H. Abdallah

    2015-01-01

    Full Text Available This study describes the preparation, characterization, and evaluation of performance of blend Polyethersulfone (PES with manganese(III acetylacetonate Mn(acac3 to produce reverse osmosis blend membrane. The manganese(III acetylacetonate nanoparticles were prepared by a simple and environmentally benign route based on hydrolysis of KMnO4 followed by reaction with acetylacetone in rapid stirring rate. The prepared nanoparticle powder was dissolved in polymer solution mixture to produce RO PES/Mn(acac3 blend membrane, without any treatment of Polyethersulfone membrane surface. The membrane morphology, mechanical properties, and performance were presented. The scanning electron microscopy (SEM images have displayed a typical asymmetric membrane structure with a dense top layer due to the migration of Mn(acac3 nanoparticles to membrane surface during the phase inversion process. Contact angle measurements have indicated that the hydrophilicity of the membrane was improved by adding Mn(acac3. AFM images have proved excellent pores size distribution of blend membrane and lower surface roughness compared with bare PES. The desalination test was applied to blend membrane, where the blend membrane provided good performance; particularly, permeate flux was 24.2 Kg/m2·h and salt rejection was 99.5%.

  19. 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.

  20. Metal Organic Chemical Vapour Deposited Thin Films of Cobalt Oxide Prepared via Cobalt Acetylacetonate

    Institute of Scientific and Technical Information of China (English)

    C.U. Mordi; M.A. Eleruja; B.A. Taleatu; G.O. Egharevba; A.V. Adedeji; 0.0. Akinwunmi; B. Olofinjana; C. Jeynes; E.O.B. Ajayi

    2009-01-01

    The single solid source precursor, cobalt (Ⅱ) acetylacetonate was prepared and characterized by infrared spec-troscopy. Thin films of cobalt oxide were deposited on soda lime glass substrates through the pyrolysis (metal organic chemical vapour deposition (MOCVD)) of single solid source precursor, cobalt acetylaceto-nate, Co[C5H7O2]2 at a temperature of 420℃. The compositional characterization carried out by rutherford backscattering spectroscopy and X-ray diffraction (XRD), showed that the films have a stoichiometry of Co2O3 and an average thickness of 227±0.2 nm. A direct energy gap of 2.15±0.01 eV was calculated by the data obtained by optical absorption spectroscopy. The morphology of the films obtained by scanning electron mi-croscopy, showed that the grains were continuous and uniformly distributed at various magnifications, while the average grain size was less than 1 micron for the deposited thin films of cobalt oxide.

  1. Electrodeposition of uranium in dimethyl sulfoxide and its inhibition by acetylacetone as studied by EQCM

    Energy Technology Data Exchange (ETDEWEB)

    Shirasaki, K. [Institute for Materials Research, Tohoku University, Sendai, Miyagi 980-8577 (Japan)]. E-mail: kshira@imr.tohoku.ac.jp; Yamamura, T. [Institute for Materials Research, Tohoku University, Sendai, Miyagi 980-8577 (Japan); Herai, T. [Institute for Materials Research, Tohoku University, Sendai, Miyagi 980-8577 (Japan); Shiokawa, Y. [Institute for Materials Research, Tohoku University, Sendai, Miyagi 980-8577 (Japan)

    2006-07-20

    In the study of the all-uranium redox-flow battery with a high efficiency, electrochemical investigations of the negative electrode reaction, i.e. U(IV)/U(III) of uranium {beta}-diketone complexes, is necessary in aprotic solvents. In our recent studies, the uranium(IV) acelylacetonate, known to show the simplest voltammograms due to a quasi-reversible U(IV)/U(III) reaction at -2.6 V versus Fc/Fc{sup +} in the solvent with the small donor number, shows more complicated voltammograms in the solvents with the larger donor numbers such as dimethyl sulfoxide (DMSO). For U{sup 4+} ion without acetylacetone in such solvents, several researchers reported an electrodeposition at around -1.6 to -2 V versus Fc/Fc{sup +}, whereas its details have not known at all. Therefore in this study, the electrode reactions of the U(IV)/U(III) and the U(III)/U(0) reaction of U(dmso){sub 8}(ClO{sub 4}){sub 4} were investigated by direct monitoring of weight changes of a Au electrode during potential sweeps by using the EQCM, as well as the HMDE. Also, an inhibition of the uranium electrodeposition by an addition of the acetylacetone was investigated.

  2. AROMATIC AND HETEROCYCLIC NITRILES AND THEIR POLYMERS ⅩⅤⅢ. THE POLYMERIZATION KINETICS OF BENZONITRILE CATALYZED BY METAL ACETYLACETONATE

    Institute of Scientific and Technical Information of China (English)

    QIN Wei; HUANG Zhitang

    1993-01-01

    The bulk polymerization of benzonitrile catalyzed by Co (Ⅱ), Co (Ⅲ) and Fe(Ⅲ)acetylacetonate was studied. The results of kinetics study show that the rate of polymerization was proportional to first power of the concentration of catalyst and second power of the concentration of monomer.

  3. AROMATIC AND HETEROCYCLIC NITRILES AND THEIR POLYMERS XIX: THE POLYMERIZATION OF SUBSTITUTED BENZONITRILES CATALYZED BY COBALTIC ACETYLACETONATE

    Institute of Scientific and Technical Information of China (English)

    QIN Wei; HUANG Zhitang

    1996-01-01

    The polymerization kinetics of 4,4'-biphenyldicarbonitrile and other substituted benzonitriles catalyzed by cobaltic acetylacetonate was studied. The structure of polymer of different substituted benzonitrile was also determined. It is found that the rate of polymerization and the structure of polymer is greatly affected by the substituent of benzonitriles.

  4. Binary Diffusion Coefficients of Platinum(II) Acetylacetonate in Supercritical Carbon Dioxide.

    Science.gov (United States)

    Kong, Chang Yi; Siratori, Tomoya; Wang, Guosheng; Sako, Takeshi; Funazukuri, Toshitaka

    2013-11-14

    Binary diffusion coefficients (D12) and retention factors (k) of platinum(II) acetylacetonate at infinitesimal concentration in supercritical (sc) carbon dioxide (CO2) were measured by the chromatographic impulse response method with a poly(ethylene glycol) coated capillary column at temperatures from (308.15 to 343.15) K and pressures from (8.5 to 40.0) MPa, and D12 in liquid ethanol at temperatures from (298.15 to 333.15) K and atmospheric pressure by the Taylor dispersion method. As has been seen for our previously reported data on other metal complexes measured in sc CO2 and organic solvents, the D12 data in sc CO2 and liquid ethanol were represented by a function of temperature and solvent viscosity. The D12 values for metal complexes were not related to the solute molecular weights. The k values in sc CO2 were expressed by a function of temperature and CO2 density.

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

    Science.gov (United States)

    Wang, Lixi; Yang, Xiaojuan; Yang, Weimin; Zhang, Jing; Zhang, Qitu; Song, Bo; Wong, Chingping

    2017-03-01

    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)3 (RE = Ce, Dy, Tb) to achieve fine ZnO QDs and adjust their surface properties. RE(AcAc)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 (Eg) was also calculated to prove the surface modification effect. For the RE(AcAc)3/ZnO QDs complex materials, stable linkage occurs because of the affinity of sbnd COOH from acetylacetonate anionic ligand to zinc oxide surfaces, with attachment to the zinc oxide by hydrogen bonding between the protons of the hydroxyl groups on the surface of ZnO QDs and the π-system of acetylacetone.

  6. Synergistic Inhibition Effect of Zinc Acetylacetonate and Benzothiazole in Epoxy Coating on the Corrosion of Mild Steel

    Science.gov (United States)

    Amoozadeh, S. M.; Mahdavian, M.

    2015-06-01

    The corrosion inhibition effect of zinc acetylacetonate (ZAA) and benzothiazole (BTH) mixture was evaluated for mild steel in 3.5% NaCl solution. To this end, ZAA:BTH mixtures ranged from 6:1 to 1:6 mol ratios were examined by weight loss and open circuit potential to obtain optimal mole ratio. The optimal mixture of ZAA:BTH at 1:5 mol ratio showed a significant corrosion inhibition efficiency proved by electrochemical impedance spectroscopy and polarization studies. The addition of the optimal mixture of ZAA:BTH to epoxy coating showed a considerable increase of corrosion protection evaluated by salt spray exposure.

  7. Effect of magnesium acetylacetonate on the signal of organic forms of vanadium in graphite furnace atomic absorption spectrometry.

    Science.gov (United States)

    Kowalewska, Zofia; Welz, Bernhard; Castilho, Ivan N B; Carasek, Eduardo

    2013-01-15

    The aim of this work was to investigate the influence of magnesium acetylacetonate (MgA) on the signal of organic forms of vanadium in xylene solution by graphite furnace atomic absorption spectrometry. MgA alone or mixed with palladium acetylacetonate (PdA) was considered as a chemical modifier. It has been found that MgA does not improve, but decreases significantly the integrated absorbance of V in the form of alkyl-aryl sulfonates, acetylacetonates, porphyrins and in lubricating oils, while its effect is negligible in the case of "dark products" from petroleum distillation, i.e., heavy oil fractions and residues. The decrease is also observed in the presence of Pd. The MgA (or MgA+PdA) effect on the integrated absorbance of V has been studied using the following variants: different ways of modifier application, various pyrolysis temperature, additional application of air ashing, preliminary pretreatment with iodine and methyltrioctylammonium chloride, application of various graphite furnace heating systems (longitudinal or transverse) and various optical and background correction systems (medium-resolution line source spectrometer with deuterium background correction or high-resolution continuum source spectrometer). The experiments indicate formation of more refractory compounds as a possible reason for the decrease of the integrated absorbance for some forms of V in the presence of MgA. The application of MgA as a chemical modifier in V determination is not recommended. Results of this work have general importance as, apart from the intentional use of MgA as a modifier, organic Mg compounds, present in petroleum products for other reason (e.g. as an additive), can influence the signal of V compounds and hence the accuracy in V determination. Generally, petroleum products with known amount of V are recommended as standards; however, lubricating oils can be inadequate for "dark products" from petroleum distillation. In the case of unknown samples it is

  8. 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.

    2017-03-01

    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 Fe3O4 NPs is reduced to only 21% and 9% of the original cost when using 1,2-octanediol and cyclohexanol, respectively.

  9. Effect of chelating agent acetylacetone on corrosion protection properties of silane-zirconium sol-gel coatings

    Science.gov (United States)

    Yu, Mei; Liang, Min; Liu, Jianhua; Li, Songmei; Xue, Bing; Zhao, Hao

    2016-02-01

    The hybrid sol-gel coatings on AA2024-T3 were prepared with a silane coupling agent 3-glycidoxypropyltrimethoxysilane (GPTMS) and a metal alkoxide tetra-n-propoxyzirconium (TPOZ) as precursors. The effect of acetylacetone (AcAc) as a chelating agent on the corrosion protection properties of sol-gel coatings were evaluated and the optimal AcAc/TPOZ molar ratio was obtained. The sol-gel coatings were characterized by atomic force microscopy (AFM), scanning electron microscopy (SEM) and energy dispersive spectroscopy (EDS). The corrosion protection properties of the coatings were evaluated by means of potentiodynamic polarization study (PDS) and electrochemical impedance spectroscopy (EIS). It is demonstrated that AcAc avoids fast hydrolysis of TPOZ and benefits to form stable sols. The coating with AcAc/TPOZ molar ratio of 3 shows the best corrosion protection performance in 0.05 M NaCl solution.

  10. Reactions of 15-crown-5 and bis-15-crown-5 ethers with metal acetylacetonate ions in the gas phase

    Energy Technology Data Exchange (ETDEWEB)

    Timofeev, O.S.; Bogatskii, A.V.; Gren, A.I.; Lobach, A.V.; Nekarsov, Y.S.; Zagorevskii, D.V.

    1985-05-20

    A study was carried out on the ion-molecule reactions of ions arising in the dissociation of ferric, cobaltic, chromic, manganous, neodymium(II), gallium(III), and indium(III) acetylacetonates upon electron impact with 15-crown-5 and bis-15-crown-5. The ratio of the yields of (acac)x-1 /SUP M+L/ ions is determined by the case of reduction of M /SUP x+1+/ to M /SUP x+/ and for (acac)/sub 3/M complexes, this ratio decreases in the series Nd, In, GA > Cr > Fe, Co. The rate constant for the formation of acacCoL/sup +/ ions is greater than for acacFeL/sup +/ ions. The possibility of fixing transition metals in unstable oxidation states by crown ethers is demonstrated in the case of nickel.

  11. Transport of Indium, Gallium and Thallium Metal Ions Through Chromatographic Fiber Supported Solid Membrane in Acetylacetone Containing Mixed Solvents

    Institute of Scientific and Technical Information of China (English)

    Abaji Gaikwad

    2011-01-01

    The transport of metal ions of indium, gallium and thallium from source solution to receiving phase through the chromatographic fiber supported solid membrane in the acetylacetone (HAA) containing mixed solvent system has been explored. The fibers supported solid membranes were prepared with chemical synthesis from cellulose fibers and citric acid with the carboxylic acid ion exchange groups introduced. The experimental variables, such as concentration of metal ions (10^-2 to 10^-4 mol.L^-1) in the source solution, mixed solvent composition [for exampl, e, acetylacetone, (2,4-pentanedione), (HAA) 20% (by volume), 1,4-dioxane 10% to 60% and HC1 0.25 to 2 mol.L^-1] in the receiving phase and stirring speed (50-130 r.min ) of the bulk source and receiving phase, were explored. The efficiency of mixed solvents for the transport of metal ions from the source to receiving phase through the fiber supported solid membrane was evaluated. The combined ion exchange solvent extraction (CIESE) was observed effective for the selective transport of thallium, indium and gallium metal ions through fiber supported solid membrane in mixed solvents. The oxonium salt formation in the receiving phase enhances thallium, indium and gallium metal ion transport through solid membrane phase. The selective transport of thallium metal ions from source phase was observed from indium and gallium metal ions in the presence of hydrochloric acid in organic solvents in receiving phase. The separation of thallium metal ions from the binary mixtures of Be(II), Ti(IV), AI(III) Ca(II), Mg(II), K (I), La(III) and Y(III) was carried out in the mixed solvent system using cellulose fiber supported solid membrane.

  12. 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.

  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 and Photoluminescence of Cu[(PPh3)2](acac) (PPh3=Triphenylphosphine, acac = Acetylacetone)

    Institute of Scientific and Technical Information of China (English)

    2007-01-01

    A novel complex Cu(PPh3)2(acac) 1 (PPh3 = triphenylphosphine, acac = acetylacetone) was obtained by a solution reaction and structurally characterized by X-ray diffraction. The crystal belongs to monoclinic, space group P21/n with a = 13.7361(8), b = 12.8204(7), c =19.7638(13)(A), β = 95.946(2)°, C41H37CuO2P2, Mr= 687.19, V= 3461.7(4)(A)3, Z = 4, Dc = 1.319g/cm3, S = 1.067, μ(MoKα) = 0.758 mm-1, F(000) = 1432, R = 0.0403 and wR = 0.0990. Complex 1is characterized by an isolated structure. X-ray structure analysis of 1 shows that acac behaves as a chelating ligand and PPh3 coordinates as a monodentate ligand to the Cu(Ⅰ) atoms. Photoluminescent investigation reveals that the title complex displays a strong green-light emission.

  15. Thermal aging effect of vanadyl acetylacetonate precursor for deposition of VO{sub 2} thin films with thermochromic properties

    Energy Technology Data Exchange (ETDEWEB)

    Yu, Jung-Hoon [Department of Chemistry, Sungkyunkwan University, 440-746 Suwon (Korea, Republic of); Nam, Sang-Hun [Institute of Basic Science, Sungkyunkwan University, 440-746 Suwon (Korea, Republic of); Kim, Donguk; Kim, Minha [School of Electronic and Electrical Engineering, Sungkyunkwan University (Korea, Republic of); Seo, Hyeon Jin; Ro, Yu Hyeon [Department of Chemistry, Sungkyunkwan University, 440-746 Suwon (Korea, Republic of); Joo, Yong Tae [YOUNG DO Glass Industry Co., Ltd., Jeongeup (Korea, Republic of); Lee, Jaehyeong [School of Electronic and Electrical Engineering, Sungkyunkwan University (Korea, Republic of); Boo, Jin-Hyo, E-mail: jhboo@skku.edu [Department of Chemistry, Sungkyunkwan University, 440-746 Suwon (Korea, Republic of); Institute of Basic Science, Sungkyunkwan University, 440-746 Suwon (Korea, Republic of)

    2016-10-15

    Highlights: • 7 day aged VO(acac){sub 2} sol shows enhanced adhesivity on the SiO{sub 2} compared with non-aged sol. • The aging process has significantly affected the morphologies of VO{sub 2} films. • From the FT-IR spectra, thermal aging process provides the deformation of precursor. • The metal insulator transition (MIT) efficiency (ΔT{sub at2000} {sub nm}) reached a maximum value of 51% at 7 day aging. • Thermal aging process could shorten the aging time of sol solution. - Abstract: Thermochromic properties of vanadium dioxide (VO{sub 2}) have been studied extensively due to their IR reflection applications in energy smart windows. In this paper, we studied the optical switching property of VO{sub 2} thin film, depending on the thermal aging time of the vanadyl acetylacetonate (VO(acac){sub 2}) precursor. We found the alteration of the IR spectra of the precursor by tuning the aging time as well as heat treatments of the precursor. An aging effect of vanadium precursor directly affects the morphologies, optical switching property and crystallinity of VO{sub 2} films. The optimum condition was achieved at the 7 day aging time with metal insulator transition (MIT) efficiency of 50%.

  16. Efficient alkene epoxidation catalyzed by molybdenyl acetylacetonate supported on aminated UiO-66 metal−organic framework

    Energy Technology Data Exchange (ETDEWEB)

    Kardanpour, Reihaneh [Department of Chemistry, Catalysis Division, University of Isfahan, Isfahan 81746-73441 (Iran, Islamic Republic of); Tangestaninejad, Shahram, E-mail: stanges@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); Moghadam, Majid, E-mail: moghadamm@sci.ui.ac.ir [Department of Chemistry, Catalysis Division, University of Isfahan, Isfahan 81746-73441 (Iran, Islamic Republic of); Mohammadpoor-Baltork, Iraj; Zadehahmadi, Farnaz [Department of Chemistry, Catalysis Division, University of Isfahan, Isfahan 81746-73441 (Iran, Islamic Republic of)

    2015-03-15

    Metal–organic frameworks (MOFs) containing Mo Schiff base complexes were prepared by post-synthesis method and applied as efficient catalysts in the epoxidation of alkenes with tert-BuOOH. In this manner, UiO-66-NH{sub 2} (UiO=University of Oslo) MOF was reacted with salicylaldehyde and thiophene-2-carbaldehyde to produce bidentate Schiff bases. Then, the Schiff base ligands were used for immobilization of molybdenyl acetylacetonate. These new catalysts were characterized by FT-IR, UV–vis spectroscopic techniques, X-ray diffraction (XRD), BET, inductively coupled plasma atomic emission spectroscopy (ICP-AES) and field emission scanning electron microscopy (FE-SEM). These catalytic systems showed excellent activity in the epoxidation of alkenes such as cyclic and linear ones with tert-butyl hydroperoxide (TBHP) in 1,2-dichloroethane, and reused several times without any appreciable loss of their activity. - Graphical abstract: Efficient alkene epoxidation with TBHP catalyzed by heterogeneous and reusable molybdenum base catalysts is reported. - Highlights: • UiO-66-NH{sub 2} was modified with salicylaldehyde and thiophene-2-carbaldehyde. • The Schiff base groups were used for immobilization of MoO{sub 2}(acac){sub 2}. • The heterogeneous catalysts were prepared. • The prepared catalysts were used for epoxidation of alkenes. • Compared to other catalyst, our catalysts were more efficient and forceful.

  17. Acetylacetonate anchors for robust functionalization of TiO2 nanoparticles with Mn(II)-terpyridine complexes.

    Science.gov (United States)

    McNamara, William R; Snoeberger, Robert C; Li, Gonghu; Schleicher, James M; Cady, Clyde W; Poyatos, Macarena; Schmuttenmaer, Charles A; Crabtree, Robert H; Brudvig, Gary W; Batista, Victor S

    2008-10-29

    A novel class of derivatized acetylacetonate (acac) linkers for robust functionalization of TiO2 nanoparticles (NPs) under aqueous and oxidative conditions is reported. The resulting surface adsorbate anchors are particularly relevant to engineering photocatalytic and photovoltaic devices since they can be applied to attach a broad range of photosensitizers and photocatalytic complexes and are not affected by humidity. Acac is easily modified by CuI-mediated coupling reactions to provide a variety of scaffolds, including substituted terpy complexes (terpy = 2,2':6,2''-terpyridine), assembled with ligands coordinated to transition-metal ions. Since Mn-terpy complexes are known to be effective catalysts for oxidation chemistry, functionalization with Mn(II) is examined. This permits visible-light sensitization of TiO2 nanoparticles due to interfacial electron transfer, as evidenced by UV-vis spectroscopy of colloidal thin films and aqueous suspensions. The underlying ultrafast interfacial electron injection is complete on a subpicosecond time scale, as monitored by optical pump-terahertz probe transient measurements and computer simulations. Time-resolved measurements of the Mn(II) EPR signal at 6 K show that interfacial electron injection induces Mn(II) --> Mn(III) photooxidation, with a half-time for regeneration of the Mn(II) complex of ca. 23 s.

  18. 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.

  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

    Energy Technology Data Exchange (ETDEWEB)

    Kamakura, Nao, E-mail: minnie04_tb@yahoo.co.jp; Inui, Tetsuo; Kitano, Masaru; Nakamura, Toshihiro

    2014-03-01

    A new method for the separate determination of Chromium(III) (Cr(III)), Chromium(VI) (Cr(VI)), and Cr(III) acetylacetonate (Cr(acac){sub 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){sub 3} and Cr(III) were adsorbed on the CED, and Cr(VI) was adsorbed on the AED. The adsorbed Cr(acac){sub 3} was eluted with 50 mL of carbon tetrachloride, followed by the elution of Cr(III) with 50 mL of 3 mol L{sup −1} nitric acid. Cr(VI) was eluted with 50 mL of 3 mol L{sup −1} nitric acid. The chemical species of Cr eluted from the CED with carbon tetrachloride was identified as Cr(acac){sub 3} using infrared spectroscopy. The eluate of Cr(acac){sub 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){sub 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){sub 3} exhibited desirable results (96.0%–107%) when 5 μg of each species (50 μg L{sup −1}) was added to 100 mL water samples (i.e., tap water, rainwater, and bottled drinking water). In a humic acid solution, Cr(acac){sub 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

  1. Plasma assisted metal-organic chemical vapor deposition of hard chromium nitride thin film coatings using chromium(III) acetylacetonate as the precursor

    Energy Technology Data Exchange (ETDEWEB)

    Dasgupta, Arup; Kuppusami, P.; Lawrence, Falix; Raghunathan, V.S.; Antony Premkumar, P.; Nagaraja, K.S

    2004-06-15

    A new technique has been developed for depositing hard nanocrystalline chromium nitride (CrN) thin films on metallic and ceramic substrates using plasma assisted metal-organic chemical vapor deposition (PAMOCVD) technique. In this low temperature and environment-friendly process, a volatile mixture of chromium(III) acetylacetonate and either ammonium iodide or ammonium bifluoride were used as precursors. Nitrogen and hydrogen have been used as the gas precursors. By optimizing the processing conditions, a maximum deposition rate of {approx}0.9 {mu}m/h was obtained. A comprehensive characterization of the CrN films was carried out using X-ray diffraction (XRD), microhardness, and microscopy. The microstructure of the CrN films deposited on well-polished stainless steel (SS) showed globular particles, while a relatively smooth surface morphology was observed for coatings deposited on polished yittria-stabilized zirconia (YSZ)

  2. The electronic structure of the adducts of nickel(II) and cobalt(II) acetylacetonate with 2,2ʹ-dipyridyl by the method of quantum chemical modeling

    Science.gov (United States)

    Komissarov, A. A.; Korochentsev, V. V.; Vovna, V. I.

    2016-02-01

    The electronic structure of the nickel(II) and cobalt(II) bis-acetylacetonate with the additional 2,2ʹ-dipyridyl ligand is investigated using density functional theory calculations and X-ray photoelectron spectroscopy. Additional ligand effect on geometry, charges, electronic structure and X-ray photoelectron spectrum is studied. Our calculations show that the electron-donating ability of the 2,2ʹ-dipyridyl ligand is low. The computed data is compared with experimental data.

  3. Thermal co-decomposition of silver acetylacetonate and tin(II) hexafluoroacetylacetonate: Formation of carbonaceous Ag/Ag{sub x}Sn(x = 4 and 6.7)/SnO{sub 2} composites

    Energy Technology Data Exchange (ETDEWEB)

    Křenek, T.; Duchek, P. [Research Centre of New Technologies, University of West Bohemia, 30614 Plzeň (Czech Republic); Urbanová, M.; Pokorná, D. [Laboratory of Laser Chemistry, Institute of Chemical Process Fundamentals, ASCR v.v.i., 16502 Prague (Czech Republic); Bezdička, P.; Jakubec, I. [Institute of Inorganic Chemistry, ASCR v.v.i., 25068 Husinec-Řež (Czech Republic); Pola, M.; Čerstvý, R.; Kovářík, T. [Research Centre of New Technologies, University of West Bohemia, 30614 Plzeň (Czech Republic); Galiková, A. [Institute of Inorganic Chemistry, ASCR v.v.i., 25068 Husinec-Řež (Czech Republic); Pola, J., E-mail: pola@icpf.cas.cz [Institute of Inorganic Chemistry, ASCR v.v.i., 25068 Husinec-Řež (Czech Republic)

    2013-08-20

    Highlights: • Ag acetylacetonate increases thermal stability by mixing with Sn hexafluoroacetylacetonate. • Heated mixture of chelates yields a residue containing Ag, Sn, O and C elements. • Residues obtained at higher temperature contain Ag–Sn intermetallic compounds. - Abstract: Thermal co-decomposition of silver(I) acetylacetonate and tin(II) hexafluoroacetylacetonate has been examined by using thermal gravimetry, differential scanning calorimetry and complementary analyses of gaseous products and solid residues by Fourier transform infrared and Raman spectroscopy, X-ray diffraction and scanning electron microscopy. It is revealed that poorly stable silver(I) acetylacetonate mixed with tin(II) hexafluoroacetylacetonate does not undergo thermal decomposition at around 120 °C, but takes part in a room-temperature solid-state interaction with the Sn counterpart, which is ensued by an exothermal process at 109 °C and subsequent co-decomposition involving a pronounced stage at around 275 °C. All steps lead to carbonaceous Ag/SnO{sub 2} composites containing crystalline Ag at 200 °C, Ag and SnO{sub 2} at 400 °C, and Ag, SnO{sub 2}, Ag{sub 4}Sn and Ag{sub 6.7}Sn at 600 °C. The intermetallic Ag{sub 6.7}Sn compound is judged to arise from nanostructured environment of alloying Ag and Sn.

  4. Synthesis, spectral characterization and DNA binding of Schiff-base metal complexes derived from 2-amino-3-hydroxyprobanoic acid and acetylacetone.

    Science.gov (United States)

    Hosny, Nasser Mohammed; Hussien, Mostafa A; Radwan, Fatima M; Nawar, Nagwa

    2014-11-11

    Four new metal complexes derived from the reaction of Cu(II), Co(II), Ni(II) and Zn(II) acetates with the Schiff-base ligand (H3L) resulted from the condensation of the amino acid 2-amino-3-hydroxyprobanoic acid (serine) and acetylacetone have been synthesized and characterized by, elemental analyses, ES-MS, IR, UV-Vis., 1H NMR, 13C NMR, ESR, thermal analyses (TGA and DTG) and magnetic measurements. The results showed that the Schiff-base ligand acts as bi-negative tridentate through the azomethine nitrogen, the deprotonated carboxylate oxygen and the enolic carbonyl oxygen. The optical band gaps measurements indicated the semi-conducting nature of these complexes. Molecular docking was used to predict the binding between the Schiff base ligand with the receptor of prostate cancer mutant H874Y. The interactions between the Cu(II) complex and calf thymus DNA (CT-DNA) have been studied by UV spectra. The results confirm that the Cu(II) complex binds to CT-DNA in an intercalative mode.

  5. Optimization of the Energy Level Alignment between the Photoactive Layer and the Cathode Contact Utilizing Solution-Processed Hafnium Acetylacetonate as Buffer Layer for Efficient Polymer Solar Cells.

    Science.gov (United States)

    Yu, Lu; Li, Qiuxiang; Shi, Zhenzhen; Liu, Hao; Wang, Yaping; Wang, Fuzhi; Zhang, Bing; Dai, Songyuan; Lin, Jun; Tan, Zhan'ao

    2016-01-13

    The insertion of an appropriate interfacial buffer layer between the photoactive layer and the contact electrodes makes a great impact on the performance of polymer solar cells (PSCs). Ideal interfacial buffer layers could minimize the interfacial traps and the interfacial barriers caused by the incompatibility between the photoactive layer and the electrodes. In this work, we utilized solution-processed hafnium(IV) acetylacetonate (Hf(acac)4) as an effective cathode buffer layer (CBL) in PSCs to optimize the energy level alignment between the photoactive layer and the cathode contact, with the short-circuit current density (Jsc), open-circuit voltage (Voc), and fill factor (FF) all simultaneously improved with Hf(acac)4 CBL, leading to enhanced power conversion efficiencies (PCEs). Ultraviolet photoemission spectroscopy (UPS) and scanning Kelvin probe microscopy (SKPM) were performed to confirm that the interfacial dipoles were formed with the same orientation direction as the built-in potential between the photoactive layer and Hf(acac)4 CBL, benefiting the exciton separation and electron transport/extraction. In addition, the optical characteristics and surface morphology of the Hf(acac)4 CBL were also investigated.

  6. Spectral characterization, optical band gap calculations and DNA binding of some binuclear Schiff-base metal complexes derived from 2-amino-ethanoic acid and acetylacetone

    Science.gov (United States)

    Hussien, Mostafa A.; Nawar, Nagwa; Radwan, Fatima M.; Hosny, Nasser Mohammed

    2015-01-01

    Bi-nuclear metal complexes derived from the reaction of Cu(II), Co(II), Ni(II) and Zn(II) acetates with the Schiff-base ligand (H2L) resulted from the condensation of 2-amino-ethanoic acid (glycine) and acetylacetone have been synthesized and characterized by elemental analyses, Raman spectra, FT-IR, ES-MS, UV-Vis., 1H NMR, ESR, thermal analyses (TG, DTG and DTA) and magnetic measurements. The results showed that, the Schiff base ligand can bind two metal ions in the same time. It coordinates to the first metal ion as mono-negative bi-dentate through azomethine nitrogen and enolic carbonyl after deprotonation. At the same time, it binds to the second metal ion via carboxylate oxygen after deprotonation. The thermodynamic parameters E∗, ΔH∗, ΔG∗ and ΔS∗ have been calculated by Coats-Redfern (CR) and Horowitz-Metzger (HM) methods. The optical band gaps of the isolated complexes have been calculated from absorption spectra and the results indicated semi-conducting nature of the investigated complexes. The interactions between the copper (II) complex and calf thymus DNA (CT-DNA) have been studied by UV spectra. The results confirm that the Cu(II) complex binds to CT-DNA.

  7. New Ru(II)/Os(II)-polypyridyl complexes for coupling to TiO2 surfaces through acetylacetone functionality and studies on interfacial electron-transfer dynamics.

    Science.gov (United States)

    Banerjee, Tanmay; Biswas, Abul Kalam; Sahu, Tuhin Subhra; Ganguly, Bishwajit; Das, Amitava; Ghosh, Hirendra Nath

    2014-09-28

    New Ru(ii)- and Os(ii)-polypyridyl complexes have been synthesized with pendant acetylacetone (acac) functionality for anchoring on nanoparticulate TiO2 surfaces with a goal of developing an alternate sensitizer that could be utilized for designing an efficient dye-sensitized solar cell (DSSC). Time-resolved transient absorption spectroscopic studies in the femtosecond time domain have been carried out. The charge recombination rates are observed to be very slow, compared with those for strongly coupled dye molecules having catechol as the anchoring functionality. The results of such studies reveal that electron-injection rates from the metal complex-based LUMO to the conduction band of TiO2 are faster than one would expect for an analogous complex in which the chromophoric core and the anchoring moiety are separated with multiple saturated C-C linkages. Such an observation is rationalized based on computational studies, and a relatively smaller spatial distance between the dye LUMO and the TiO2 surface accounted for this. Results of this study are compared with those for analogous complexes having a gem-dicarboxy group as the anchoring functionality for covalent binding to the TiO2 surface to compare the role of binding functionalities on electron-transfer dynamics.

  8. Surface chemistry of copper metal and copper oxide atomic layer deposition from copper(ii) acetylacetonate: a combined first-principles and reactive molecular dynamics study.

    Science.gov (United States)

    Hu, Xiao; Schuster, Jörg; Schulz, Stefan E; Gessner, Thomas

    2015-10-28

    Atomistic mechanisms for the atomic layer deposition using the Cu(acac)2 (acac = acetylacetonate) precursor are studied using first-principles calculations and reactive molecular dynamics simulations. The results show that Cu(acac)2 chemisorbs on the hollow site of the Cu(110) surface and decomposes easily into a Cu atom and the acac-ligands. A sequential dissociation and reduction of the Cu precursor [Cu(acac)2 → Cu(acac) → Cu] are observed. Further decomposition of the acac-ligand is unfavorable on the Cu surface. Thus additional adsorption of the precursors may be blocked by adsorbed ligands. Molecular hydrogen is found to be nonreactive towards Cu(acac)2 on Cu(110), whereas individual H atoms easily lead to bond breaking in the Cu precursor upon impact, and thus release the surface ligands into the gas-phase. On the other hand, water reacts with Cu(acac)2 on a Cu2O substrate through a ligand-exchange reaction, which produces gaseous H(acac) and surface OH species. Combustion reactions with the main by-products CO2 and H2O are observed during the reaction between Cu(acac)2 and ozone on the CuO surface. The reactivity of different co-reactants toward Cu(acac)2 follows the order H > O3 > H2O.

  9. Evaluation of a synergetic effect between Rh as permanent chemical modifier and acetylacetone as complexing agent in Sc determination in sediment slurry samples by ETAAS

    Energy Technology Data Exchange (ETDEWEB)

    Flores, Araceli Veronica [Departamento de Quimica Analitica, Instituto de Quimica, Universidade Estadual de Campinas, P.O. Box 6154, 13084 971 Campinas, Sao Paulo (Brazil); Perez, Carlos Alberto [Laboratorio Nacional de Luz Sincrotron, P.O. Box 6192, 13084 971 Campinas, Sao Paulo (Brazil); Arruda, Marco Aurelio Zezzi [Departamento de Quimica Analitica, Instituto de Quimica, Universidade Estadual de Campinas, P.O. Box 6154, 13084 971 Campinas, Sao Paulo (Brazil)]. E-mail: zezzi@iqm.unicamp.br

    2005-02-14

    In the present work, scandium was determined in sediment slurry samples (from three different rivers) by electrothermal atomic absorption spectrometry (ETAAS). Slurries were prepared by weighting 100 mg of dry sediment samples ({<=}53 {mu}m particle sizes) and adding 6 ml of HCl:HNO{sub 3}:HF (3:1:2, v/v). Accurate results were only possible due to the synergetic effect between Rh as permanent chemical modifier and acetylacetone (Acac) as complexing agent. The same platform was used for 400 heating cycles. The performance of the chemical modification was evaluated by using scanning electron microscopy (SEM), synchrotron radiation X-ray fluorescence (SRXRF) and some figures of merit (precision and detectability). The best analytical conditions were attained using 1500 and 2550 deg. C as pyrolysis and atomization temperatures. The scandium content in the liquid phase of the slurries ranged from 61 to 73%, thus indicating, in this study, that both liquid and solid phases play an important role in slurry analyses. An amount of 5.0-20.0 {mu}g l{sup -1} Sc linear range as well as LOD and LOQ of 0.19 and 0.62 {mu}g l{sup -1}, respectively, were obtained under these conditions. The accuracy was checked by using microwave-assisted decomposition, and the results compared to those obtained with the proposed methodology (slurry analysis). By checking both sets of the results, there is no statistical difference at the 95% confidence levels.

  10. 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)

  11. Synthesis, interactions, molecular structure, biological properties and molecular docking studies on Mn, Co, Zn complexes containing acetylacetone and pyridine ligands with DNA duplex.

    Science.gov (United States)

    Thamilarasan, V; Sengottuvelan, N; Stalin, N; Srinivasan, P; Chakkaravarthi, G

    2016-07-01

    Three metal complexes (1-3) of the type [Mn(acac)2(py)·H2O] (1), [Co(acac)2(py)·H2O] (2) and [Zn(acac)2(py)·H2O] (3), [Where acac=acetylacetone, py=pyridine] were synthesized and characterized by spectral (UV-vis, FT-IR, ESI-mass) analysis. The structure of complex 2 has been determined by single crystal X-ray diffraction studies and the configuration of ligand-coordinated to metal(II) ion was well described as distorted octahedral coordination geometry. The interaction of the complexes with CT-DNA has been explored by absorption, fluorescence, circular dichromism spectroscopy, viscosity measurements and molecular docking studies. The intrinsic binding constant Kb of complexes 1-3 with CT-DNA obtained from UV-vis absorption spectral studies were 2.1×10(4), 2.1×10(5) and 1.98×10(4)M(-1), respectively, which revealed that the complexes could interact with CT-DNA through groove binding. The results indicated that the complexes (1-3) were able to bind to DNA with different binding affinity, in the order: 2>1>3. The interaction of the compounds with bovine serum albumins were also investigated using fluorescence methods and the gel electrophoresis assay demonstrates weak cleavage ability of the pBR322 plasmid DNA in the presence of the metal complexes (1-3) with various activators. Further, the in vitro cytotoxic effect of the complexes were examined on cancerous cell line, with human breast cancer cells MCF-7.

  12. Microwave Assisted Synthesis of N,N' - Bis (acetylacetone) - 1,2 -propenediimine and Its Co ( Ⅱ ) Complex%乙酰丙酮缩邻苯二胺及其Co(Ⅱ)配合物的微波合成

    Institute of Scientific and Technical Information of China (English)

    牛永盛; 李红春

    2011-01-01

    N,N' -Bis(acetylacetone) - 1,2- propenediimine and their cobalt complex were synthesized by microwave radicalization. The structures of as - prepared products were characterized by the infra - red, element analysis, magnetic spectrometer and meting point meter.%采用微波辐射方法合成了乙酰丙酮缩邻苯二胺Schiff碱及其Co(Ⅱ)金属配合物;通过红外光谱、元素分析、质谱、熔点仪对Schiff碱及其配合物进行了表征.

  13. Synthesis and characterization of Fe(II) β-diketonato complexes with relevance to acetylacetone dioxygenase: insights into the electronic properties of the 3-histidine facial triad.

    Science.gov (United States)

    Park, Heaweon; Baus, Jacob S; Lindeman, Sergey V; Fiedler, Adam T

    2011-12-05

    A series of high-spin iron(II) β-diketonato complexes have been prepared and characterized with the intent of modeling the substrate-bound form of the enzyme acetylacetone dioxygenase (Dke1). The Dke1 active site features an Fe(II) center coordinated by three histidine residues in a facial geometry--a departure from the standard 2-histidine-1-carboxylate (2H1C) facial triad dominant among nonheme monoiron enzymes. The deprotonated β-diketone substrate binds to the Fe center in a bidentate fashion. To better understand the implications of subtle changes in coordination environment for the electronic structures of nonheme Fe active sites, synthetic models were prepared with three different supporting ligands (L(N3)): the anionic (Me2)Tp and (Ph2)Tp ligands ((R2)Tp = hydrotris(pyrazol-1-yl)borate substituted with R-groups at the 3- and 5-pyrazole positions) and the neutral (Ph)TIP ligand ((Ph)TIP = tris(2-phenylimidazol-4-yl)phosphine). The resulting [(L(N3))Fe(acac(X))](0/+) complexes (acac(X) = substituted β-diketonates) were analyzed with a combination of experimental and computational methods, namely, X-ray crystallography, cyclic voltammetry, spectroscopic techniques (UV-vis absorption and (1)H NMR), and density functional theory (DFT). X-ray diffraction results for complexes with the (Me2)Tp ligand revealed six-coordinate Fe(II) centers with a bound MeCN molecule, while structures of the (Ph2)Tp and (Ph)TIP complexes generally exhibited five-coordinate geometries. Each [(L(N3))Fe(acac(X))](0/+) complex displays two broad absorption features in the visible region that arise from Fe(II)→acac(X) charge transfer and acac(X)-based transitions, consistent with UV-vis data reported for Dke1. These absorption bands, along with the Fe redox potentials, are highly sensitive to the identity of L(N3) and substitution of the β-diketonates. By interpreting the experimental results in conjunction with DFT calculations, detailed electronic-structure descriptions of the

  14. 乙酰丙酮比色法在流感病毒裂解疫苗游离甲醛含量测定中的应用%The application of acetylacetone colorimetric method for determination of free formaldehyde content in influenza vaccine (split virion)

    Institute of Scientific and Technical Information of China (English)

    方曼莉; 马雷钧; 郁佳俊; 封向明; 沈坚; 程鹏飞

    2014-01-01

    目的 验证乙酰丙酮比色法测定流感病毒裂解疫苗游离甲醛含量的可行性,并确认该法测定游离甲醛含量优于品红亚硫酸法. 方法 对乙酰丙酮比色法进行准确度、精密度、专属性、线性、耐用性验证,并将该法与品红亚硫酸法进行比较.结果 乙酰丙酮比色法的标准曲线具有可靠性,甲醛回收率为100.3%~100.9%,相对标准偏差(relative standard deviation,RSD)为0.49%.该法的精密度和专属性良好,实验间和实验内RSD均<5.0%,甲醛加样回收率均>99.0%.与品红亚硫酸法相比,该法的线性更好,偏差更小.结论 乙酰丙酮比色法可用于流感病毒裂解疫苗游离甲醛含量测定.%Objective To validate feasibility of using acetylacetone colorimetric method for determination of free formaldehyde content in influenza vaccine (split virion),and to confirm the acetylacetone colorimetric method was better than the magenta sulphurous acid colorimetric method.Methods The accuracy,precision,specificity,linearity and durability of the acetylacetone colorimetric method were validated.The acetylacetone colorimetric method was compared with the magenta sulphurous acid colorimetric method.Results The standard curve of the acetylacetone colorimetric method was reliable,recoveries of formaldehyde were 100.3%-100.9% and relative standard deviation (RSD) was 0.49%.The precision and specificity of the acetylacetone colorimetric method were good,RSDs of intra-assay and inter-assay were both <5.0% and recoveries of formaldehyde were >99.0%.The acetylacetone method had better linearity and lower deviation as compared with the magenta sulphurous acid colorimetric method.Conclusion The acetylacetone colorimetric method for the determination of free formaldehyde content in influenza vaccine (split virion) is feasible.

  15. 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

    Indian Academy of Sciences (India)

    N Raman; V Muthuraj; S Ravichandran; A Kulandaisamy

    2003-06-01

    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 structure of the complexes. From the data, it is found that all the complexes possess square-planar geometry. The EPR spectrum of the copper complex in DMSO at 300 K and 77 K was recorded and its salient features are reported. All the title complexes were screened for antimicrobial activity by the well diffusion technique using DMSO as solvent. The minimum inhibitory concentration (MIC) values were calculated at 37°C for a period of 24 h. It has been found that all the complexes are antimicrobially active and show higher activity than the free ligand.

  16. 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)

  17. Synthesis and characterization of fac-[M(CO)3(P)(OO)] and cis-trans-[M(CO)2(P)2(OO)] complexes (M = Re, (99m)Tc) with acetylacetone and curcumin as OO donor bidentate ligands.

    Science.gov (United States)

    Triantis, Charalampos; Tsotakos, Theodoros; Tsoukalas, Charalampos; Sagnou, Marina; Raptopoulou, Catherine; Terzis, Aris; Psycharis, Vassilis; Pelecanou, Maria; Pirmettis, Ioannis; Papadopoulos, Minas

    2013-11-18

    The synthesis and characterization of neutral mixed ligand complexes fac-[M(CO)3(P)(OO)] and cis-trans-[M(CO)2(P)2(OO)] (M = Re, (99m)Tc), with deprotonated acetylacetone or curcumin as the OO donor bidentate ligands and a phosphine (triphenylphosphine or methyldiphenylphosphine) as the monodentate P ligand, is described. The complexes were synthesized through the corresponding fac-[M(CO)3(H2O)(OO)] (M = Re, (99m)Tc) intermediate aqua complex. In the presence of phosphine, replacement of the H2O molecule of the intermediate complex at room temperature generates the neutral tricarbonyl monophosphine fac-[Re(CO)3(P)(OO)] complex, while under reflux conditions further replacement of the trans to the phosphine carbonyl generates the new stable dicarbonyl bisphosphine complex cis-trans-[Re(CO)2(P)2(OO)]. The Re complexes were fully characterized by elemental analysis, spectroscopic methods, and X-ray crystallography showing a distorted octahedral geometry around Re. Both the monophosphine and the bisphosphine complexes of curcumin show selective binding to β-amyloid plaques of Alzheimer's disease. At the (99m)Tc tracer level, the same type of complexes, fac-[(99m)Tc(CO)3(P)(OO)] and cis-trans-[(99m)Tc(CO)2(P)2(OO)], are formed introducing new donor combinations for (99m)Tc(I). Overall, β-diketonate and phosphine constitute a versatile ligand combination for Re(I) and (99m)Tc(I), and the successful employment of the multipotent curcumin as β-diketone provides a solid example of the pharmacological potential of this system.

  18. Transition metal complexes with thiosemicarbazide-based ligands. Part 51. Square-planar nickel(II complex with acetylacetone bis(S-n-propylisothiosemicarbazone (L. Crystal and molecular structure of [Ni(L-H]NCS and two isomorphic complexes [Ni(L-H]I·EtOH and [Ni(L-H]I·iPrOH

    Directory of Open Access Journals (Sweden)

    VUKADIN M. LEOVAC

    2006-06-01

    Full Text Available The template reaction of a warm methanolic solution of Ni(OAc2·4H2O, S-n-propylisothiosemicarbazide hydroiodide and acetylacetone yielded the needle- like, brown, diamagnetic complex [Ni(L–H]I·MeOH, and in the presence of an excess of NH 4NCS, brown, prismatic crystals of the complex [Ni(L–H]NCS (1, both compounds involving the monoanionic form of the ligand, acetylacetone bis(S-n-propylisothiosemicarbazone, L. Slow recrystallization fromMeOH, EtOH, iPrOH and Me2CO gave the corresponding monosolvent complexes [Ni(L–H]I·solvent, of which only those involving EtOH and iPrOH were suitable for structural analysis. The crystallographic parameters of [Ni(L–H]I·EtOH (2 and [Ni(L–H]I·iPrOH (3 are very similar to each other, showing their structures are isomorphic. The crystal structures of the title compounds consist of the independent ions: NCS-, or I-, and the chemically identical cation [Ni(L–H]+, where L–H is the monoanion resulting from deprotonation of the acetylacetone moiety, a tetradentate N4 ligand forming a square-planar coordination around a Ni(II ion. It was found that the isothiosemicarbazide fragment of the ligand has an imido form. The complex cations of the compounds [Ni(L–H]NCS and [Ni(L–H]I·EtOH exhibit significant difference only in the conformation of their propyl groups.

  19. Efeito da concentração do catalisador acetilacetonato férrico na cura de poliuretano à base de polibutadieno líquido hidroxilado (PBLH e diisocianato de isoforona (IPDI Effect of ferric acetylacetonate catalyst concentration on the cure of polyurethane based on hydroxy terminated polybutadiene and isophorone diisocyanate

    Directory of Open Access Journals (Sweden)

    Willian César Paterlini

    2002-05-01

    Full Text Available The reaction between hydroxy-terminated polybutadiene and isophorone diisocyanate constitutes the base of the curing process of the most composite solid propellant used in the propulsion of solid rocket propellant. In this work, differential scanning calorimetry and viscosity measurements were used to evaluate the effect of the ferric acetylacetonate catalyst concentration on the reaction between HTBR and IPDI. These analyses show one exotherm, which shifts to lower temperatures as the catalyst concentration increases. The viscosity analyses show that the increase of temperature causes, at first, a reduction in the mixture viscosity, reaching a minimum range called gelification region (increasing the crosslinking density.

  20. The sensitized reaction of non-ionic surfactant to acetylacetone spectrophotometry in the determination of trace formaldehyde in marine products%非离子表面活性剂OP增敏乙酰丙酮光度法测定海产品中的痕量甲醛

    Institute of Scientific and Technical Information of China (English)

    任淑华; 郭振良

    2013-01-01

    目的:建立快速、准确、灵敏测定海产品中甲醛的新方法.方法:在沸水浴中,痕量甲醛与乙酰丙酮能发生微弱的显色反应.实验发现,非离子表面活性剂OP对上述反应有较强的增敏作用,由此建立了一种测定痕量甲醛的新方法.结果:在测定条件下,溶液的最大吸收波长在412 nm,方法的检出限为0.11 μg/ml,相关系数为0.9993,九次空白实验的标准偏差为S=0.00365,相对标准偏差为RSD为0.376%,回收率在100% ~ 105%.结论:方法简单快速、选择性好,用于测定海产品中的甲醛时,测得结果与非增敏乙酰丙酮光度法及HPLC法的结果一致.%Objective: To develop a simple, exact and sensitive method for determination of trace formaldehyde in marine products. Methods: In boiling water bath, acetylacetone and formaldehyde could have a feeble colour reaction. The experiment was found that non - ionic surfactant OP could sensitize the colour reaction. Results: The maximum absorption wavelength was 412 nm. The detection limit was 0. 11 μg/ml. The correlation coefficient was 0.9993. The standard deviation and the relative standard deviation for nine blank were 0.00365 and 0.376%. The recoveries were in the range of 100% to 105% . Conclusion: The results obtained in the application of this method to the analysis of marine products were in consistency with those obtained by the acetylacetone spectrophotometry and the HPLC method.

  1. Synthesis and crystal structure of the Ag(I) complex with N,N′-bis(acetylacetone)-1,4-butanediamine%N,N′-双(乙酰丙酮)-1,4-丁二胺Schiff 碱Ag(I)配合物的合成及其晶体结构

    Institute of Scientific and Technical Information of China (English)

    赵文泽

    2016-01-01

    本文以1,4-丁二胺和乙酰丙酮进行缩合反应得到N,N′-双(乙酰丙酮)-1,4-丁二胺的 Schiff 碱配体L,然后将配体 L与AgNO3进行配位反应,得到配合物[Ag2(L)(NO3)2]n,并用元素分析,FT-IR和X-射线晶体衍射进行了表征。结果表明,配合物属于单斜晶系,空间群为 P21/c,晶体参数:a=0.73776(3)nm,b=1.52774(7)nm,c=0.96552(3)nm,β=106.6370(10),V=1.04269(7)nm3,Z=2,Dc=1.886 g·cm-3,R1=0.0443,wR2=0.1305.在配合物中,每个Ag( I)离子的配位模式均为扭曲四面体,分别与相邻配体的烯醇式氧原子,γ-C原子,两个硝酸根的氧原子配位,配体均表现为四齿配体,分别用两端β-酮亚胺单元的烯醇式氧原子,γ-C原子和四个Ag( I)离子配位形成一维链,一维链通过硝酸根和Ag( I)离子配位扩展形成三维网状结构。%The Schiff base ligand L[ N,N′-bis( acetylacetone)-1,4-butanediamine] was synthesized from condensation reaction of 1,4-butanediamine with acetylacetone. Ligand L was used for coordination with silver nitrate to obtain coordination complex[Ag2 ( L) ( NO3 ) 2 ] n;this complex was characterized by FT-IR spectroscopy,elemental analysis,and X-ray single-crystal diffraction anal-ysis. The results of structural analysis indicate that the complex crystallize in the monoclinic,space group P21/c,with the crystal cell parameters:a=0.73776(3)nm,b=1.52774(7)nm,c=0.96552(3)nm,β=106.6370(10),V=1042.69(7)nm3,Z=2,Dc=1. 886 g·cm-3 ,R1=0. 0443,wR2=0. 1305. The Complex coordination environment of Ag(Ⅰ) is a distorted tetrahedral geometry, being bound to oxygen atoms andγ-C atoms from two adjacent molecules of L as well as to two oxygen atoms from two bidentate ni-trate anion. Each L ligand links four metal atoms using both ends two oxygen atoms and γ-C atoms to generate a one-dimensional (1D)chain structure,A one-dimensional chain expanded into a three-dimensional(3D)network structure by nitrate coordinated Ag ( I) ion.

  2. Metal-Acetylacetonate Synthesis Experiments: Which Is Greener?

    Science.gov (United States)

    Ribeiro, M. Gabriela T. C.; Machado, Adlio A. S. C.

    2011-01-01

    A procedure for teaching green chemistry through laboratory experiments is presented in which students are challenged to use the 12 principles of green chemistry to review and modify synthesis protocols to improve greenness. A global metric, green star, is used in parallel with green chemistry mass metrics to evaluate the improvement in greenness.…

  3. ORGANIC/INORGANIC SUPPORT FOR IMMOBILIZING IRON ( Ⅲ )ACETYLACETONATE AND BIS(IMINO) PYRIDYL LIGAND CATALYST SYSTEM FOR ETHYLENE POLYMERIZATION%无机/有机复合载体负载乙酰丙酮铁/双亚胺基吡啶催化剂及其乙烯聚合

    Institute of Scientific and Technical Information of China (English)

    吴晶; 历伟; 蒋斌波; 王靖岱; 阳永荣

    2012-01-01

    采用溶胶-凝胶法,将苯乙烯-丙烯酸共聚物( PSA)包覆于955 Davison硅胶上得到无机/有机复合微球载体,并在2,6-二[1-(2-异丙基苯基亚胺基)乙基]吡啶/Fe(acac)3均相催化剂中浸渍后得到负载型双亚胺基吡啶铁催化剂.该催化剂在生产高结晶度(72%)聚乙烯的同时,还能生产一定量的α-烯烃.考察了不同膜材料以及聚合条件(不同助催化剂,压力,温度,Al/Fe摩尔比)对聚合活性以及聚合产物性能的影响,发现温度对聚合产物的α-烯烃与聚乙烯的质量比影响最大,助催化剂类型既影响催化剂的活性,也对最终产物的性质有着很大的影响.氯化镁处理的PSA作为膜材料时,负载2,6-二[1-(2-异丙基苯基亚胺基)乙基]吡啶/Fe(acac)3所得到聚乙烯分子量较低(Mw=11.9×104),结晶度较大(72%),熔融指数MI较高(2.35 g/10min),可作为双峰聚乙烯中的低分子量部分加以利用.%An organic/inorganic support of immobilizing catalysts for ethylene polymerization was devised. The composition of the hybrid catalyst is as following: styrene and acrylic copolymer ( PSA ) is the organic part for binding iron ( HI ) acetylacetonate and bis( imino)pyridyl ligand catalyst,and Si02(Davison 955 silical gel) is the inorganic part. The inorganic part is coated by the organic part (PSA) by sol-gel method. The catalyst could produce not only high crystallinity (72% ) polyethylene, but also or-olefin. We considered the impact of different membrane materials and polymerization conditions (different cocatalyst,pressure,temperature,Al/Fe molar ratio) to the polymerization activity and properties of polymers and found that temperature had the greatest impact to the weight ratio of oligomer to PE. Because of the poor thermal stability of catalyst, the catalytic activity significantly attenuated with increasing temperature. When pressure increased, catalytic activity would increase too. The relationship of pressure and catalytic

  4. Influence of Acetylacetone on Photocatalytic Properties of TiO2 Thin Films Deposited on PMMA Substrates%乙酰丙酮对PMMA负载锐钛矿型TiO2薄膜及其光催化性能影响

    Institute of Scientific and Technical Information of China (English)

    张志清; 黄剑锋; 曹丽云; 吴建鹏

    2011-01-01

    The nanociystalline TiO2 solution was prepared using a microwave hydrotheimal process to treat precursor liquid which was obtained by control the hydrolysis of titanium-n-butoxide in the presence of excessive water and acetylacetone (AcAcH). Then nanociystalline TiO2 thin films were deposited on polymethylmethacrylate (PMMA) substrates by dip-coating process from TiO2 colloidal solution. The phase composition of TiO2 nanoparticles, morphologies and optical properties of TiO2 thin films deposited on PMMA substrates were characterized by X-ray diffraction (XRD), fourier transform infrared spectrometer (FTTR), transmission electron microscope (TEM), atomic force microscopy (AFM) and UV-vis spectroscopy. Meanwhile photocatalytic properties of TiO2 films were investigated by degradation of Rhodamine B ( RhB) under ultraviolet radiation. Trie results indicate that anatase TiO2 colloidal solution modified by AcAcH is disperse, uniform, deposit-free and the deposited TiO2 thin films are transparent, homogeneous and compact, and show high efficiency of photocatalysis. Rhodamine B has been degradated over 90% at 180 min%以钛酸丁酯作为钛源,水为溶剂,乙酰丙酮(AcAcH)为表面修饰剂,采用微波水热辅助溶胶-凝胶法制备了纳米晶二氧化钛水溶液,利用提拉镀膜法在聚合物聚甲基丙烯酸甲酯(PMMA)基板上沉积得到了透明TiO2纳米晶薄膜.通过X射线衍射(XRD)、红外光谱(FTIR)、透射电子显微镜(TEM)、原子力显微镜(AFM)和紫外-可见光吸收光谱(UV-Vis)等对TiO2纳米颗粒和薄膜的晶相组成、表面形貌及光学性能进行表征.同时通过紫外光光催化降解罗丹明B研究了TiO2薄膜的光催化性能.结果表明:通过引入乙酰丙酮,可以得到高度分散、晶相为锐钛矿型的TiO2水溶胶,在PMMA基板上沉积得到的薄膜表面平整、致密,具有良好的透光率,经过180 min紫外光照射,对罗丹明B的降解率达到90%以上.

  5. Electron beam irradiation of dimethyl-(acetylacetonate) gold(III) adsorbed onto solid substrates

    NARCIS (Netherlands)

    Wnuk, J.D.; Gorham, J.M.; Rosenberg, S.G.; Van Dorp, W.F.; Madey, T.E.; Hagen, C.W.; Fairbrother, D.H.

    2010-01-01

    Electron beam induced deposition of organometallic precursors has emerged as an effective and versatile method for creating two-dimensional and three-dimensional metal-containing nanostructures. However, to improve the properties and optimize the chemical composition of nanostructures deposited in t

  6. 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.

  7. Intratumoral administration of Holmium-166 Acetylacetonate Microspheres: antitumor efficacy and feasibility of multimodality imaging in renal cancer

    NARCIS (Netherlands)

    Bult, W.; Kroeze, S.G.C.; Elschot, M.; Seevinck, P.R.; Beekman, F.J.; De Jong, H.W.A.M.; Uges, D.R.A.; Kosterink, J.G.W.; Luijten, P.R.; Hennink, W.E.; et al.

    2013-01-01

    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 holmium-166 microsp

  8. Intratumoral administration of holmium-166 acetylacetonate microspheres: antitumor efficacy and feasibility of multimodality imaging in renal cancer.

    Directory of Open Access Journals (Sweden)

    Wouter Bult

    Full Text Available 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 holmium-166 microspheres ((166HoAcAcMS. This new technique locally ablates renal tumors through high-energy beta particles, while the gamma rays allow for nuclear imaging and the paramagnetism of holmium allows for MRI. METHODS: (166HoAcAcMS were administered intratumorally in orthotopic renal tumors (Balb/C mice. Post administration CT, SPECT and MRI was performed. At several time points (2 h, 1, 2, 3, 7 and 14 days after MS administration, tumors were measured and histologically analyzed. Holmium accumulation in organs was measured using inductively coupled plasma mass spectrometry. RESULTS: (166HoAcAcMS were successfully administered to tumor bearing mice. A striking near-complete tumor-control was observed in (166HoAcAcMS treated mice (0.10±0.01 cm(3 vs. 4.15±0.3 cm(3 for control tumors. Focal necrosis and inflammation was present from 24 h following treatment. Renal parenchyma outside the radiated region showed no histological alterations. Post administration CT, MRI and SPECT imaging revealed clear deposits of (166HoAcAcMS in the kidney. CONCLUSIONS: Intratumorally administered (166HoAcAcMS has great potential as a new local treatment of renal tumors for surgically unfit patients. In addition to strong cancer control, it provides powerful multimodality imaging opportunities.

  9. Fast determination of operational stability of the soluble acetylacetone-cleaving enzyme Dke1 in an enzyme membrane reactor.

    Science.gov (United States)

    Hofer, Hannes; Steiner, Walter

    2005-11-01

    The main aim of this study was the determination of the operational stability of soluble Dke1 (EC 1.13.11.50) in an enzyme membrane reactor. In order to calculate the half-life of soluble Dke1, the K (M) of oxygen must be known. The determination of this constant was done using progress curve analysis (K (M) = 260 micromol l(-1)). In a next step, the reactor system was studied by building a mathematical model for calculation of the reactor system, using Berkeley Madonna ver. 8.0.1 software. After that, the determination of the half-life of Dke1 under operational conditions at different temperatures (5, 10, 15, 25, 30, 35 degrees C) was performed. The quantitative criterion for stability was the value of the first-order rate constant of monomolecular inactivation. The experiments showed that soluble Dke1 is poorly stable. The half-life ranged from 308 min at 5 degrees C to 9 min at 35 degrees C. This method for determining the half-life is quite applicable for enzymes which are poorly stable. In addition, both the storage stability and the operational stability can be determined.

  10. Aerobic oxidation behavior of α-ionone catalyzed by N-hydroxyphthalimide combined with acetylacetone cobalt(Ⅱ)

    Institute of Scientific and Technical Information of China (English)

    TANG Rui-ren; ZHOU Ya-ping; GONG Nian-hua; ZHAO Yu

    2008-01-01

    A practical catalytic method to oxidize α-ionone with molecular oxygen using N-hydroxyphthalimide(NHPI) combined with acetylaeetone cobatt(Ⅱ) (Co(acac)2) was developed, and the probable catalytic mechanism was proposed. The influences of the reaction conditions on conversion of α-ionone and the selectivity of the major product (5-keto-ct-ionone) were investigated, and the technical parameters for 5-keto-α-ionone were optimized. The results show that the primary product is 5-keto-α-ionone, and by-products include epoxy-α-ionone, as well as rearrangement products 4-keto-β-ionone and epoxy-β-ionone, which are characterized by infrared spectra, proton nuclear magnetic resonance spectra, mass spectra and elemental analysis. The selectivity of 5-keto-α-ionone and the conversion of α-ionone are 55.0% and 97.0%, respectively, when 30%(molar fraction) NHPI, 1.0%(molar fraction) Co(acac)2 and no solvent are employed under O2 pressure of 1.0 MPa and the reaction temperature of 65℃ for 11 h. The procedure shows good reproducibility in the parallel experiments.

  11. Spectroscopic properties of the UO{sub 2}(ACAC){sub 2}.(H{sub 2}O)n:Eu{sup 3+}(ACAC=Acetylacetonate Ion)

    Energy Technology Data Exchange (ETDEWEB)

    Felinto, Maria Claudia F.C.; Luiz, Jose Eduardo M. Sa; Nakagawa, Fabio T. [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil); Brito, Hermi F. [Universidade de Sao Paulo (USP/IQ), SP (Brazil). Inst. de Quimica], E-mail: hefbrito@iq.usp.br; Teotonio, Ercules E.S. [Universidade Federal de Goias (UFG), Catalao, GO (Brazil)], E-mail: ercteot@gmail.com

    2007-07-01

    The uranyl ion possesses some properties, which makes it a potential component for a solar energy conversion system or biological application. It absorbs light in the shorter wavelength range of the solar spectrum, producing a relatively long-lived excited state. The excited state of uranyl ion has fluorescence peak at 520 nm, a property that makes it relatively convenient to investigate its reaction. The redox potential of the excited uranyl ion makes a powerful oxidizing agent. This may be of potential use in the photo generation of oxygen, which is of great importance for the photo cleavage of water. In this work, it is described the synthesis, characterization and spectroscopic study of the matrix UO{sub 2}(ACAC){sub 2}.(H{sub 2}O)n.(x% mol) Eu{sup 3+} (where x= 1, 3, 5 and 10). The compounds obtained were characterized by elementary analyses for determine the U{sup 6+} and Eu{sup 3+} concentrations, infrared spectra, thermal analyses, absorption in the UV-VIS range and luminescence spectra. The mainly bands in infrared spectra of the b-diketone observed in this work are {nu}{sub s} C=O in 1540 cm{sup -1}, {nu}{sub ass} C=O in 1540 cm{sup -1} and ns C=C in 1577 cm{sup -1}. In the emission spectra, transitions of the triplet 3{sup {pi}}{sub u} {yields} {sup 1}{sigma}{sub g} + was observed. The spectra of the uranyl matrix present behavior superimposed to doped 5% and 10% ones. The emission spectra of matrix doped with 1 and 3% showed a band shift to red region of spectrum light. (author)

  12. 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.

  13. Synthesis and crystal structure of the Schiff base derived from acetylacetone and benzidine%乙酰丙酮缩联苯胺席夫碱的合成及晶体结构

    Institute of Scientific and Technical Information of China (English)

    江光奇; 蔡杰; 杨建; 张云黔

    2008-01-01

    一个多世纪以来,己有大量有关席夫碱方面的文献报道。许多Schiff碱金属配合物因具有良好的抗肿瘤、抗病毒、杀菌抑霉等多种生物活性而得到了广泛应用;其特殊的催化行为以及在酶模拟方面的功效引起了化学家的普遍重视。席夫碱中,β-二酮类化合物是一类良好的金属螯合剂,因为它能够为金属提供两个键合点,形成稳定的六元螯合环,其与稀土离子形成的配合物具有稳定的化学性质和优异的发光性能,因而具有广泛的应用前景。乙酰丙酮是典型的β-二酮,它与不同胺类化合物缩合得到的Schiff碱具有较强的亲核性,容易与不同的金属离子进行配位,因此广泛地应用于金属离子分析测定和配位化合物的合成中。

  14. Narrow bandgap host material for high quantum efficiency yellow phosphorescent organic light-emitting diodes doped with iridium(III) bis(4-phenylthieno[3,2-c]pyridine)acetylacetonate

    Energy Technology Data Exchange (ETDEWEB)

    Yook, Kyoung Soo; Lee, Jun Yeob, E-mail: leej17@skku.edu

    2015-05-15

    A narrow bandgap host material, 4,5-di(9H-carbazol-9-yl)phthalonitrile (2CzPN), was used as a bipolar host material to improve the device performances of yellow phosphorescent organic light-emitting diodes(PHOLEDs). The device performances of the yellow PHOLEDs were optimized at a low doping concentration of 1%. A low turn-on voltage of 3.0 V and high quantum efficiency of 19.3% were achieved using the 2CzPN host material and no efficiency roll-off of the device was observed up to 1000 cd/m{sup 2} compared with 25% of reference device. - Highlights: • High quantum efficiency in yellow phosphorescent organic light-emitting diodes. • Narrow bandgap host material with donor–acceptor structure for low driving voltage. • Low optimum doping concentration of 1% for high quantum efficiency and power efficiency.

  15. Holmium nanoparticles : preparation and in vitro characterization of a new device for radioablation of solid malignancies

    NARCIS (Netherlands)

    Bult, Wouter; Varkevisser, Rosanne; Soulimani, Fouad; Seevinck, Peter R; de Leeuw, Hendrik; Bakker, Chris J G; Luijten, Peter R; van Het Schip, Alfred D; Hennink, Wim E; Nijsen, J Frank W

    2010-01-01

    PURPOSE: The present study introduces the preparation and in vitro characterization of a nanoparticle device comprising holmium acetylacetonate for radioablation of unresectable solid malignancies. METHODS: HoAcAc nanoparticles were prepared by dissolving holmium acetylacetonate in chloroform, follo

  16. An investigation of tautomeric equilibria by means of mass spectrometry

    DEFF Research Database (Denmark)

    Zamir, Lolita; Jensen, Bror Skytte; Larsen, Elfinn

    1969-01-01

    Changes in the mass spectra with inlet temperature were used in this work to demonstrate the dependence of keto-enol tautomerism of acetylacetone, 3-methyl acetylacetone and 3-allyl acetylacetone on temperature. The largest dependence of temperature were shown by the ion [M 42]+. arising from a M...

  17. Ultrasound-assisted dealumination of zeolite Y

    Indian Academy of Sciences (India)

    M Hosseini; M A Zanjanchi; B Ghalami-Choobar; H Golmojdeh

    2015-01-01

    We demonstrate a new procedure for dealumination of zeolite Y. The method employs a 28 KHz ultrasound bath and an ethanolic acetylacetone solution. Acetylacetone was used as chelating agent and ultrasound irradiation was used as extraction intensifier. Four types of samples, as-synthesized, ammoniumexchanged, acidic and neutralized zeolite were used for dealumination. Parts of the framework aluminumatoms are removed from their sites in the structure of zeolite Y upon the use of either acetylacetone on its own or simultaneous use of acetylacetone and ultrasound waves. Higher dealumination was observed for those samples subjected to both ultrasound irradiation and acetylacetone extraction.

  18. ОСОБЛИВОСТІ ІНІЦІЮВАННЯ ПОЛІМЕРИЗАЦІЇ СТИРОЛУ, ІНІЦІЙОВАНОЇ ГІДРОПЕРОКСИДОМ КУМОЛА В ПРИСУТНОСТІ АЦЕТИЛАЦЕТОНАТУ МІДІ(ІІ)

    OpenAIRE

    Grekova, A. V.; Ivanchenko, P. A.; Seifullina, I. I.; Skrypnik, L. V.

    2016-01-01

    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 findi...

  19. 乙酰丙酮分光光度法测定塑料中甲醛和六亚甲基四胺在食品模拟物中的迁移量%Acetylacetone Spectrophotometric Determination of Migration of Formaldehyde and Hexamethylenetetramine from Plastics into Food Simulants

    Institute of Scientific and Technical Information of China (English)

    朱晓艳; 陈少鸿; 刘在美; 曹国洲

    2009-01-01

    考察乙酰丙酮与甲醛的显色反应及六亚甲基四胺(HMTA)转化成甲醛的反应条件的影响并进行优化,建立乙酰丙酮分光光度法测定塑料中甲醛和HMTA在乙酸溶液中迁移量(以甲醛计)的方法.结果表明:线性范围可达0~15mg/L,检出限为0.09mg/L,HMTA对甲醛的甲均转化率为98.3%~100%,甲醛在HMTA溶液中的回收率为99.5%~101%.由9家实验室对水平为9.93mg/L(含HMTA)和7.01mg/L(不含HMTA)的样品进行协同实验,其重复性限r分别为0.707、0.112mg/L,再现性限R分别为2.094、1.516mg/L.

  20. Organometallics in High Energy Chemistry.

    Science.gov (United States)

    1983-10-31

    various transition metals. Design and synthesis of energetic ligands for subsequent complexation based on the acetylacetone (AcAc) backbone...coordination of beta- diketones and beta-keto esters as oxygen-donor chelating ligands . 1- 9 These complexes are generally prepared as mixed ligand complexes of...this still attractive concept was halted, however, in favor of the work on the..". synthesis and reactions of energetic acetylacetone ligands . The

  1. Characterization of precursor-based ZnO transport layers in inverted polymer solar cells

    NARCIS (Netherlands)

    Grossiord, N.; Bruyn, P. de; Moet, D.J.D.; Andriessen, R.; Blom, P.W.M.

    2014-01-01

    A wide range of characterization techniques are used to study spin-coated films of zinc oxide (ZnO) obtained from thermal decomposition of zinc acetylacetonate hydrate. Inverted organic solar cells with ZnO transport layers were prepared. Deposition conditions of the solution onto the substrate (e.g

  2. Coordination Complexes as Catalysts: The Oxidation of Anthracene by Hydrogen Peroxide in the Presence of VO(acac)[subscript 2

    Science.gov (United States)

    Charleton, Kimberly D. M.; Prokopchuk, Ernest M.

    2011-01-01

    A laboratory experiment aimed at students who are studying coordination chemistry of transition-metal complexes is described. A simple vanadyl acetylacetonate complex can be used as a catalyst in the hydrogen peroxide oxidation of anthracene to produce anthraquinone. The reaction can be performed under a variety of reaction conditions, ideally by…

  3. Catalyst-free Multicomponent Synthesis of β-Mercapto Diketones in Water%Catalyst-free Multicomponent Synthesis of β-Mercapto Diketones in Water

    Institute of Scientific and Technical Information of China (English)

    Li, Li; Liu, Bokai; WU, Qi; Lin, Xianfu

    2011-01-01

    A simple, efficient and eco-friendly route has been developed for the synthesis of fl-mercapto diketones via a multicomponent reaction of an aldehyde, acetylacetone and thiol in water. This methodology affords a number of β-mercapto diketone derivatives in moderate to good yields.

  4. Syntheses and Properties of Lanthanide Hydroxy-meso-tetra(p-chlorophenyl)porphyrin Complexes

    Institute of Scientific and Technical Information of China (English)

    YU Miao; YU Lian-xiang; JIAN Wen-ping; YANG Wen-sheng; LIU Guo-fa

    2004-01-01

    @@ Introduction The syntheses and characterization of porphyrins and metalloporphyrins have been studied extensively[1]. Hemoglobin, myoglobin or cytochrome P450, has been applied as a model compound[2]. Wong C. P. et al.[3] synthesized the first lanthanide porphyrin, acetylacetonate tetraphenylporphyrin europium, in 1974.

  5. 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

  6. 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

  7. KA1(SO4)2·12H2O catalyzed efficient synthesis of 3,4,6-trisubstituted 2-pyridone in water

    Institute of Scientific and Technical Information of China (English)

    Majid M.Heravi; Hossein A. Oskooie; Narges Karimi; Hoda Hamidi

    2011-01-01

    An efficient green protocol for the preparation 3,4,6-trisubstituted 2-pyridone of employing a condensation reaction of cyanoacetamide and acetylacetone in the presence of KAl(SO4)2·12H2O in water has been described. The present procedure offers advantage such as shorter reaction time, simple workup, and excellent yields.

  8. Synthesis and Photoluminescence of a New Red Phosphorescent Iridium(III) Quinoxaline Complex

    Institute of Scientific and Technical Information of China (English)

    Guo Lin ZHANG; Ze Hua LIU; Hai Qing GUO

    2004-01-01

    A new cyclometalated iridium(III) complex with the formula [Ir(DPQ)2(acac)] (DPQ= 2,3-diphenylquinoxaline; acac=acetylacetone) was prepared. The structure of the complex was confirmed by Elemental Analysis (EA), 1H NMR, and mass spectroscopy (MS). The UV-vis absorption and photoluminescent properties of the complex were investigated.

  9. 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...

  10. Circular serendipity: in situ ligand transformation for the self-assembly of an hexadecametallic [Cu(II)16] wheel.

    Science.gov (United States)

    Kostopoulos, Andreas K; Katsenis, Athanassios D; Frost, Jamie M; Kessler, Vadim G; Brechin, Euan K; Papaefstathiou, Giannis S

    2014-12-11

    A [Cu(II)16] wheel was isolated serendipitously from the reaction of acetylacetone dioxime with copper(ii) chloride and lanthanide ions in a reaction initially designed to produce heterometallic 3d-4f cages. The ligand has been transformed in situ to three different forms, all found within the [Cu16] wheel, with the original ligand completely absent.

  11. 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 structur

  12. 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.

    2010-01-01

    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 struc

  13. Fabrication of supported Ca-doped lanthanum niobate electrolyte layer and NiO containing anode functional layer by electrophoretic deposition

    DEFF Research Database (Denmark)

    Bozza, Francesco; Bonanos, Nikolaos

    2012-01-01

    The technique of electrophoretic deposition (EPD) has been applied for the preparation of a dense calcium-doped lanthanum niobate electrolyte film. La0.995Ca0.005NbO4 (LCN) powder was suspended in a solution of acetylacetone, iodine and water. The effects of suspension composition and deposition...

  14. Modified Sol-Gel Technique as a Cost-Effective Method of Ultradispersed Metal Oxide Powders Production

    Science.gov (United States)

    Vokhmintcev, K. V.; Konstantinov, O. V.; Belousov, V. V.

    2013-05-01

    A modified sol-gel technique was developed for fabrication of ultradispersed metal oxides powders of Bi2O3, CeO2, Cr2O3, Y2O3, ZnO2 and ZrO2. Hexamethylenetetramine, monoethanolamine and acetylacetone were used for the sol formation and gel stabilization.

  15. One-step growth of gold nanorods using a β-diketone reducing agent

    Science.gov (United States)

    Tollan, Christopher M.; Echeberria, Jon; Marcilla, Rebeca; Pomposo, José A.; Mecerreyes, David

    2009-07-01

    The synthesis and characterisation of gold nanorods have been carried out by reduction of the gold salt HAuCl4. This has been done using a single reducing agent, acetylacetone, rather than the two reducing agents, sodium borohydride and ascorbic acid, normally required by standard wet chemistry methods of gold nanorod formation. Using this novel method, the nanorods were synthesised at several different pH values which were found to greatly affect both the rate at which the nanorods form and their physical dimensions. The concentrations of acetylacetone and silver nitrate used relative to the gold salt were found to alter the aspect ratio of the nanorods formed. Rods with an average length of 42 nm and an aspect ratio of 4.6 can be easily and reproducibly formed at pH 10 using this method. Nanorods formed under optimum conditions were investigated using TEM.

  16. One-step growth of gold nanorods using a {beta}-diketone reducing agent

    Energy Technology Data Exchange (ETDEWEB)

    Tollan, Christopher M., E-mail: ctollan@cidetec.e [CIDETEC-Centre for Electrochemical Technologies, Parque Tecnologico de San Sebastian, New Materials Department (Spain); Echeberria, Jon [CEIT, Centro de Investigaciones Tecnicas de Guipuzcoa (Spain); Marcilla, Rebeca; Pomposo, Jose A.; Mecerreyes, David, E-mail: dmecerreyes@cidetec.e [CIDETEC-Centre for Electrochemical Technologies, Parque Tecnologico de San Sebastian, New Materials Department (Spain)

    2009-07-15

    The synthesis and characterisation of gold nanorods have been carried out by reduction of the gold salt HAuCl{sub 4}. This has been done using a single reducing agent, acetylacetone, rather than the two reducing agents, sodium borohydride and ascorbic acid, normally required by standard wet chemistry methods of gold nanorod formation. Using this novel method, the nanorods were synthesised at several different pH values which were found to greatly affect both the rate at which the nanorods form and their physical dimensions. The concentrations of acetylacetone and silver nitrate used relative to the gold salt were found to alter the aspect ratio of the nanorods formed. Rods with an average length of 42 nm and an aspect ratio of 4.6 can be easily and reproducibly formed at pH 10 using this method. Nanorods formed under optimum conditions were investigated using TEM.

  17. Facile fabrication of hierarchical SnO(2) microspheres film on transparent FTO glass.

    Science.gov (United States)

    Wang, Yu-Fen; Lei, Bing-Xin; Hou, Yuan-Fang; Zhao, Wen-Xia; Liang, Chao-Lun; Su, Cheng-Yong; Kuang, Dai-Bin

    2010-02-15

    Hierarchical SnO(2) microspheres consisting of nanosheets on the fluorine-doped tin oxide (FTO) glass substrates are successfully prepared via a facile hydrothermal synthesis process. The as-prepared novel microsphere films were characterized in detail by X-ray diffraction (XRD), field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), UV-vis diffuse reflectance spectroscopy. Moreover, SnO(2) nanoparticles with 30-80 nm in size covered on the surface of nanosheets/microspheres were also obtained by optimizing the hydrothermal reaction temperature, time, or volume ratio of acetylacetone/H(2)O. The detailed investigations disclose the experimental parameters, such as acetylacetone, NH(4)F, and seed layer play important roles in the morphology of hierarchical SnO(2) microspheres on the FTO glass. The formation process of SnO(2) microspheres is also proposed based on the observations of time dependent samples.

  18. NMR study of complexation in the catalyst - hydroperoxide, catalyst - alcohol, and catalyst - olefin - hydroperoxide systems

    Energy Technology Data Exchange (ETDEWEB)

    Azhikova, R.M.; Syroezhko, A.M.; Proskuryakov, V.A.

    1989-01-01

    On the basis of paramagnetic shifts and the broadening of NMR lines of hydroperoxide protons of cyclohexyl- and 1-methylcyclohexyl peroxides in haptane solution containing Mo(O) hexacarbonyl or Co(II) acetylacetonate, the authors have determined the heats of complexation and the lifetimes of hydroperoxide ligands in the metal - complex-former coordination sphere, and the activation energies of their emergence from the coordination sphere. They have determined the distances from the complex former of the central metal to the hydroxyl protons of the ligand (hydroperoxide, alcohol), and the hyperfine electron - nucleus interaction constants for the ligand hydroxyl protons in the complex. Molybdenum hexacarbonyl forms labile outer-sphere complexes with hydroperoxides and alcohols. However Co(II) acetylacetonate forms complexes that are stronger and intermediate between inner-sphere and outer-sphere complexes.

  19. 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)

  20. Cobalt-mediated radical polymerization of vinyl monomers: investigation of cobalt-coordination

    OpenAIRE

    2009-01-01

    Controlled Radical Polymerization techniques have been developed to obtain well-defined architectures and to control polymer parameters. Among these systems is Cobalt-Mediated Radical Polymerization (CMRP), which is based on the reversible deactivation of the growing radical chains with a cobalt complex, the cobalt (II) bis(acetylacetonate). The interest of this system is not only due to its ability to control the polymerization of very reactive monomers such as vinyl acetate (VAc) and N-viny...

  1. Deposition of copper selenide thin films and nanoparticles

    Science.gov (United States)

    Hu, Yunxiang; Afzaal, Mohammad; Malik, Mohammad A.; O'Brien, Paul

    2006-12-01

    A new method is reported for the growth of copper selenide thin films and nanoparticles using copper acetylacetonate and trioctylphosphine selenide. Aerosol-assisted chemical vapor deposition experiments lead to successful deposition of tetragonal Cu 2Se films. In contrast, hexadecylamine capped nanoparticles are composed of cubic Cu 2-xSe. The deposited materials are optically and structurally characterized. The results of this comprehensive study are described and discussed.

  2. Structural study of Ni- or Mg-based complexes incorporated within UiO-66-NH{sub 2} framework and their impact on hydrogen sorption properties

    Energy Technology Data Exchange (ETDEWEB)

    Žunkovič, E.; Mazaj, M. [Laboratory for Inorganic Chemistry and Technology, National Institute of Chemistry, Hajdrihova 19, 1000 Ljubljana (Slovenia); Mali, G. [Laboratory for Inorganic Chemistry and Technology, National Institute of Chemistry, Hajdrihova 19, 1000 Ljubljana (Slovenia); EN-FIST Centre of Excellence, Dunajska 156, 1000 Ljubljana (Slovenia); Rangus, M. [Laboratory for Inorganic Chemistry and Technology, National Institute of Chemistry, Hajdrihova 19, 1000 Ljubljana (Slovenia); Devic, T.; Serre, C. [Institut Lavoisier, UMR CNRS 8180, Université de Versailles Saint-Quentin-en-Yvelines, 78035 Versailles (France); Logar, N. Zabukovec, E-mail: natasa.zabukovec@ki.si [Laboratory for Inorganic Chemistry and Technology, National Institute of Chemistry, Hajdrihova 19, 1000 Ljubljana (Slovenia); CO-NOT Centre of Excellence, Hajdrihova 19, 1000 Ljubljana (Slovenia); University of Nova Gorica, Vipavska 13, 5000 Nova Gorica (Slovenia)

    2015-05-15

    Nickel and magnesium acetylacetonate molecular complexes were post-synthetically incorporated into microporous zirconium-based MOF (UiO-66-NH{sub 2}) in order to introduce active open-metal sites for hydrogen sorption. Elemental analysis, nitrogen physisorption and DFT calculations revealed that 5 molecules of Ni(acac){sub 2} or 2 molecules of Mg(acac){sub 2} were incorporated into one unit cell of UiO-66-NH{sub 2}. {sup 1}H–{sup 13}C CPMAS and {sup 1}H MAS NMR spectroscopy showed that, although embedded within the pores, both Ni- and Mg-complexes interacted with the UiO-66-NH{sub 2} framework only through weak van der Waals bonds. Inclusion of metal complexes led to the decrease of hydrogen sorption capacities in Ni-modified as well as in Mg-modified samples in comparison with the parent UiO-66-NH{sub 2}. The isosteric hydrogen adsorption enthalpy slightly increased in the case of Ni-modified material, but not in the case of Mg-modified analogue. - Graphical abstract: A post-synthesis impregnation of Mg- and Ni-acetylacetonate complexes performed on zirconium-based MOF UiO-66-NH{sub 2} does influence the hydrogen sorption performance with respect to the parent matrix. The structural study revealed that Mg- and Ni-acetylacetonate molecules interact with zirconium-terephthalate framework only by weak interactions and they are not covalently bonded to aminoterephthalate ligand. Still, they remain confined into the pores even after hydrogen sorption experiments. - Highlights: • Mg- and Ni-acetylacetonate molecules embedded in the pores of UiO-66-NH{sub 2} by PSM. • Molecules of complexes interact with framework only by van der Waals interactions. • Type/structure of deposited metal-complex impact hydrogen enthalpy of adsorption.

  3. Fabrication of Size-Tunable Metallic Nanoparticles Using Plasmid DNA as a Biomolecular Reactor.

    Science.gov (United States)

    Samson, Jacopo; Piscopo, Irene; Yampolski, Alex; Nahirney, Patrick; Parpas, Andrea; Aggarwal, Amit; Saleh, Raihan; Drain, Charles Michael

    2011-10-21

    Plasmid DNA can be used as a template to yield gold, palladium, silver, and chromium nanoparticles of different sizes based on variations in incubation time at 70 °C with gold phosphine complexes, with the acetates of silver or palladium, or chromium acetylacetonate. The employment of mild synthetic conditions, minimal procedural steps, and aqueous solvents makes this method environmentally greener and ensures general feasibility. The use of plasmids exploits the capabilities of the biotechnology industry as a source of nanoreactor materials.

  4. VO(acac)2 catalyzed condensation of o-phenylenediamine with aromatic carboxylic acids/aldehydes under microwave radiation affording benzimidazoles

    Institute of Scientific and Technical Information of China (English)

    Madhudeepa Dey; Krishnajyoti Deb; Siddhartha Sankar Dhar

    2011-01-01

    Vanadyl acetylacetonate, VO(acac)2, has been found to be very effective catalyst for synthesis of a variety of benzimidazoles under solvent-free condition. The methodology involves the exposure of a mixture of o-phenylenediamine and a selected aromatic carboxylic acid/aldehyde to microwave radiation without the use of any solvent or supporting agents. The benzimidazoles were obtained in quick time with high yields.

  5. Synthesis, characterization, and reactivity of pentamethylcyclopentadienyl complexes of divalent cobalt and nickel

    Energy Technology Data Exchange (ETDEWEB)

    Smith, Michael Edward [Univ. of California, Berkeley, CA (United States)

    1993-10-01

    The thesis is divided into the following 4 chapters: synthesis, characterization, and reactivity of trinuclear pentamethylcyclopentadienyl cobalt and nickel clusters with triply-bridging methylidyne groups; chemical and physical properties of pentamethylcyclopentadienyl acetylacetonate complexes of Co(II) and Ni(II); synthesis, characterization, and reactivity of pentamethylcyclopentadienyl halide complexes of Co and Ni; and crystallographic studies of distortions in metallocenes with C5-symmetrical cyclopentadienyl rings.

  6. Ozone Sensing Based on Palladium Decorated Carbon Nanotubes

    OpenAIRE

    2014-01-01

    Multiwall carbon nanotubes (MWCNTs) were easily and efficiently decorated with Pd nanoparticles through a vapor-phase impregnation-decomposition method starting from palladium acetylacetonates. The sensor device consisted on a film of sensitive material (MWCNTs-Pd) deposited by drop coating on platinum interdigitated electrodes on a SiO2 substrate. The sensor exhibited a resistance change to ozone (O3) with a response time of 60 s at different temperatures and the capability of detecting conc...

  7. Supported cobalt catalysts - preparation, characterization and reaction studies

    OpenAIRE

    Backman, Leif

    2009-01-01

    The aim of this work was to understand on the effect of thermal treatments, precursor and support on the interaction between the support and cobalt species, and further how the interaction affects the reducibility and dispersion of the catalyst. Silica and alumina supported cobalt catalysts were prepared, characterised and tested for catalytic activity. The catalysts were prepared by gas phase deposition techniques from cobalt acetylacetonate and cobalt carbonyl and by incipient wetness impre...

  8. Cyanate Ester Graphene Composites

    Science.gov (United States)

    2012-03-29

    weight Cu(II) acetylacetonate : nonylphenol • Mixture degassed at 300 mm/Hg 30 minutes at 90 °C and prior to pouring into silicone molds • Cure ...resin and well-understood; enables development of superior predictive models for failure; readily catalyzed to cure at reasonable temperatures BADCy Δ...Typical DSC Trace of CEs DISTRIBUTION A: Approved for public release. Distribution is unlimited. AFRL Public Affairs Clearance Number

  9. 5-Aminolevulinic acid and the hepatic oxidative stress in the early phase of experimental hexachlorobenzene intoxication Ácido delta-aminolevulinico e estresse oxidativo hepático na fase inicial da intoxicação experimental por hexaclorobenzeno

    OpenAIRE

    Tânia Cristina Higashi Sawada; Vanessa Vitoriano da Silva; Sonia Barros; Cristina Dislich Röpke; Silvia Berlanga de Moraes Barros

    2004-01-01

    This work evaluated the levels of 5-aminolevulinic acid (ALA) in the liver of rats exposed to different doses of HCB (25,50, and 100 mg/kg b.w. for 4 weeks) and correlated them with lipid peroxidation parameters. Levels of ALA were determined by high-pressure liquid chromatography after derivatization with acetylacetone and formaldehyde, followed by fluorescence detection. The methodology was carefully validated, nonetheless hepatic levels of ALA in all animals treated or not were below the d...

  10. Electro-active elastomer composite based on doped titanium dioxide Electro-active elastomer composite based on doped titanium dioxide

    OpenAIRE

    Kossi, Alaedine; Bossis, Georges; Persello, Jacques

    2015-01-01

    International audience; Recently, electro-active composites have been considered by several researchers because they exhibit an interesting change in their viscoelastic properties under an applied electric field. However, their relative elastic modulus change ΔG'=G'(E)-G'(0) is still low and rarely exceed 100 kPa. In this article, we demonstrated that, by synthesizing mesoporous aggregates of titanium dioxide (TiO2) and by adsorbing acetylacetone dipolar molecule (Acac) onto the TiO2 surface,...

  11. 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.

  12. Synthesis, characterization, and reactivity of pentamethylcyclopentadienyl complexes of divalent cobalt and nickel

    Energy Technology Data Exchange (ETDEWEB)

    Smith, M.E.

    1993-10-01

    The thesis is divided into the following 4 chapters: synthesis, characterization, and reactivity of trinuclear pentamethylcyclopentadienyl cobalt and nickel clusters with triply-bridging methylidyne groups; chemical and physical properties of pentamethylcyclopentadienyl acetylacetonate complexes of Co(II) and Ni(II); synthesis, characterization, and reactivity of pentamethylcyclopentadienyl halide complexes of Co and Ni; and crystallographic studies of distortions in metallocenes with C{sub 5}-symmetrical cyclopentadienyl rings.

  13. Preparation and Catalytic Properties of Iron-Cerium Phosphates with Sodium Dodecyl Sulfate

    OpenAIRE

    Hiroaki Onoda; Takeshi Sakumura

    2012-01-01

    Iron phosphate was prepared from iron nitrate and phosphoric acid with sodium dodecyl sulfate at various stirring hours. The chemical composition of the obtained samples was estimated from ICP and XRD measurements. Particle shape and size distribution were observed by SEM images and laser diffraction/scattering methods. Further, the catalytic activity was studied with the decomposition of the complex between formaldehyde, ammonium acetate, and acetylacetone. The peaks of FePO4 were observed i...

  14. Ligand-Free Synthesis of Tunable Size Ln:BaGdF5 (Ln = Eu3+ and Nd3+) Nanoparticles: Luminescence, Magnetic Properties, and Biocompatibility

    OpenAIRE

    Becerro, Ana Isabel; González-Mancebo, D.; Cantelar, Eugenio; Cussó, Fernando; Stepien, Grazyna; Fuente, J.M. de la; Ocaña, Manuel

    2016-01-01

    Bifunctional and highly uniform Ln:BaGdF5 (Ln = Eu3+ and Nd3+) nanoparticles have been successfully synthesized using a solvothermal method consisting of the aging at 120 °C of a glycerol solution containing the corresponding Lanthanide acetylacetonates and butylmethylimidazolium tetrafluoroborate. The absence of any surfactant in the synthesis process rendered hydrophilic nanospheres (with tunable diameter from 45 nm 85 nm, depending on the cations concentration of the starting solution) whi...

  15. Copper(II) complex of 3-cinnamalideneacetylacetone: Synthesis and characterisation

    Indian Academy of Sciences (India)

    A Veeraraj; P Sami; N Raman

    2000-10-01

    A bidentate ligand derived from cinnamaldehyde and acetylacetone and its copper(II) complex have been synthesized and characterized by elemental analysis, UV-Vis, IR, ESR and magnetic susceptibility measurements. Magnetic susceptibility measurements, ESR and electronic spectral data indicate the presence of six coordinated Cu(II) ion. The ligand and complex are tested for antibacterial activity against Pseudomonas aeroginosa. They are found to show the antibacterial activity

  16. Characterization of La0.995Ca0.005NbO4/Ni anode functional layer by electrophoretic deposition in a La0.995Ca0.005NbO4 electrolyte based PCFC

    DEFF Research Database (Denmark)

    Bozza, Francesco; Schafbauer, W.; Meulenberg, W.A.

    2012-01-01

    The Electrophoretic Deposition (EPD) technique has been applied to the preparation of a porous La0.995Ca0.005NbO4/Ni composite anode layer, deposited on a porous pre-sintered La0.995Ca0.005NbO4/Ni support. Powders of La0.995Ca0.005NbO4 and NiO were suspended in a solution of acetylacetone, iodine...

  17. Synthesis and spectral characterization of ternary mixed-vanadyl β-diketonate complexes with Schiff bases.

    Science.gov (United States)

    Baranwal, Balram Prasad; Tripathi, Kiran; Singh, Alok Kumar; Tripathi, Saurabh

    2012-06-01

    A new method to synthesize some mononuclear ternary oxovanadium(IV) complexes of the general formula [VO(β-dike)(SB)] (where Hβ-dike=acetylacetone; benzoylacetone or dibenzoylmethane, HSB=Schiff bases) has been explored by stepwise substitutions of acetylacetonate ion of VO(acac)(2) with Schiff bases. The substituted acetylacetone could be fractionated out with p-xylene as an azeotrope. The complexes were characterized by elemental analyses, molecular weight determinations, spectral (electronic, infrared, (1)H NMR, EPR and powder XRD) studies, magnetic susceptibility measurements and cyclic voltammetry. Molar conductance measurements indicated the complexes to be non-electrolytes in nitrobenzene. Bidentate chelating nature of β-diketones and Schiff base anions in the complexes was established by infrared and NMR spectra. Molecular weight determinations confirmed mononuclear nature of the complexes. The EPR spectra illustrated coupling of the unpaired electron with (51)V nucleus (I=7/2). Cyclic voltammograms of all the complexes displayed two-step oxidation processes. The oxidation peak potential corresponded to the quasireversible one-electron oxidation process of the metal center, yielding V(V) species. Transmission electron microscopy (TEM) indicated spherical particles of ∼200 nm diameter. The synthesized complexes are mixed-ligand complexes showing a considerable hydrolytic stability in which vanadium is having coordination number 5. A square pyramidal geometry around vanadium has been assigned in all the complexes.

  18. Study of the Gelling Process for the Preparation of Tin Oxide Materials Based on Tin Tetrabutoxide%Sn(OBun)4为前驱体制备SnO2材料中的溶胶-凝胶过程

    Institute of Scientific and Technical Information of China (English)

    黄瑞安; 侯立松; 赵启涛; 任叔华

    2005-01-01

    The gelling process in the preparation of tin oxide materials based on tin tetrabutoxide is studied. Sn(OBun)4 modified by two moles of acetylacetone (AcAc) has a stable six-member ring structure and is less susceptive to water. In a system with a lower molar ratio of acetylacetone to Sn(OBun)4 ([AcAc]/[Sn(OBun)4]<2.0) or a larger portion of water ([H2O]/[Sn(OBun)4]>2.5), colloidal suspension or white precipitation will take place. A system with molar ratios of both acetylacetone to Sn(OBun)4 and water to Sn(OBun)4 at 2.0 is transparent and olivaceous sol. As catalysts, hydrofluoric,hydrochloric, hydrobromic and acetic acids, and ammonia all accelerate the hydrolysis and condensation of Sn(OBun)4 during the sol-gel process. Light scattering measurement indicates that cluster size distribution in the sol system undergoes gradual broadening during the sol-gel transition.

  19. Characterization of microstructure and catalytic of cerium oxide obtained by colloidal solution; Caracterizacao da microestrutura e da atividade catalitica de oxido de cerio obtido por solucao coloidal

    Energy Technology Data Exchange (ETDEWEB)

    Senisse, C.A.L.; Bergmann, C.P.; Alves, A.K., E-mail: carolinasenisse@hotmail.com [Universidade Federal do Rio Grande do Sul (UFRGS), Porto Alege, RS (Brazil). Lab. de Materiais Ceramicos

    2012-07-01

    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)

  20. Synthesis of oxide and spinel nanocrystals for use in solid state lighting

    Science.gov (United States)

    Foley, Megan Elizabeth

    In this dissertation, microwave chemistry is employed to synthesize a variety of different crystalline nanoparticles (NPs). This introduction will describe the structures, properties and applications of the NPs studied within the dissertation, with a main focus being on ligand sensitization for the goal of enhanced luminescence. The use of metal acetylacetonate complexes to make Europium (III) doped Ytrrium (Y2O3) NPs is explored, where the acetylacetonate acts both as a source of oxygen for the synthesis of Y2O3, as well as an organic chromophore acting as an "antenna" for the absorption of light and subsequent excitation transfer to the incorporated Europium (III) (Chapter 2). Other host materials are investigated by method of metal acetylacetonate decomposition to synthesize a variety of different nanospinels, having the general formula AB2X4, with sulfide variants made by decomposition of diethyldithiocarbamate, (Chapter 3). The antenna ligand thenoyltrifluoroacetone (tta), which is known to undergo a Dexter energy transfer (DET) mechanism to efficiently sensitize Europium (III) emission, is used to determine the distance of energy transfer in Europium (III) doped nanospinels by passivating the surface of the nanospinel with a tta (Chapter 4). A variety of ligands are explored in order to optimize the sensitization efficiency in relation to the difference in energy between the singlet and triplet levels of the ligands versus the 5D0 and 5D4 energy levels of Europium (III) and Terbium (III) respectively (Chapter 5).

  1. 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)

  2. Fabrication of iron-platinum ferromagnetic nanoparticles

    Science.gov (United States)

    Elkins, Kevin Eugene

    Fabrication of chemically disordered FePt particles ranging from 2--9 nm with a precision of 1 nm has been achieved through modification of key process variables including surfactant concentration, heating rates and the type of iron precursor. In addition, the shape evolution of the FePt nanoparticles during particle growth can be manipulated to give cubic or rod geometries through changes to the surfactant injection sequence and solvent system. The primary method for synthesis of the disordered FePt nanoparticles is the polyol reduction reported by Fievet et al., which has been modified and used extensively for synthesis of differing nanoparticle systems. Our procedures use platinum acetylacetonate, iron pentacarbonyl or ferric acetylacetonate as precursors for the FePt alloy, oleic acid and oleyl amine for the surfactants, 1,2-hexadecanediol to assist with the reduction of the precursors and either dioctyl ether or phenyl ether for the solvent system. For iron pentacarbonyl based reactions, adjustment of heating rates to reflux temperatures from 1--15°C per minute allows control of FePt particle diameters from 3--8 nm. Substitution of iron pentacarbonyl with ferric acetylacetonate as the iron source results in 2 nm particles. A high platinum to surfactant ratio of 10 to 1 will yield 9 nm FePt particles when iron pentacarbonyl is used as the precursor. For use of these particles in advanced applications, the synthesized particles must be transformed to the L1o phase through annealing at temperatures above 500°C. Inhibition of particle sintering can be avoided through dispersion in a NaCl matrix at a weight ratio of 400 to 1 salt to fcc FePt particles. Production of L1o FePt nanoparticles with high magnetic anisotropy with this process has been successful, allowing the original size and size distribution of the particles.

  3. Synthesis and characterization of potential iron–platinum drugs and supplements by laser liquid photolysis

    Directory of Open Access Journals (Sweden)

    Forbes A

    2012-06-01

    Full Text Available Steven S Nkosi,1,2 Bonex W Mwakikunga,4 Elias Sideras-Haddad,2 Andrew Forbes1,31CSIR National Laser Centre, Pretoria, South Africa; 2DST/NRF Centre for Excellence in Strong Materials and School of Physics, University of the Witwatersrand, Johannesburg, 3School of Physics, University of KwaZulu-Natal, Durban, South Africa; 4DST/CSIR National Centre for Nano-Structured Materials, Pretoria, South AfricaAbstract: Highly crystalline nanospherical iron–platinum systems were produced by 248 nm laser irradiation of a liquid precursor at different laser fluences, ranging from 100–375 mJ/cm2. The influence of laser intensity on particle size, iron composition, and structure was systematically investigated. Different nanostructures of iron–platinum alloy and chemically disordered iron–platinum L10 phase were obtained without annealing. The prepared precursor solution underwent deep photolysis to polycrystalline iron–platinum nanoalloys through Fe(III acetylacetonate and Pt(II acetylacetonate. Fe(II and Pt(I acetylacetone decomposed into Fe0 and Pt0 nanoparticles. We found that the (001 diffraction peak shifted linearly to a lower angle, with the last peak shifting in opposition to the others. This caused the face-centered cubic L10 structure to change its composition according to laser fluence. The nanostructures were shown to contain iron and platinum only by energy-dispersive spectroscopy at several spots. The response of these iron–platinum nanoparticles to infrared depends on their stoichiometric composition, which is controlled by laser fluence.Keywords: nanostructures, iron, platinum, nanoparticles, laser liquid photolysis, composition

  4. Synthesis of novel glucose-based polymers and their applications as chiral stationary phases for high performance liquid chromatography

    Institute of Scientific and Technical Information of China (English)

    Tomoyuki IKAI; Takayuki YAMADA

    2016-01-01

    Two novel polymers containing glucose units as the main-chain that only differ in terms of their regioregularity were synthesized to evaluate their chiral recognition abilities as chiral stationary phases( CSPs) for high performance liquid chromatography( HPLC). The regioregular polymer( poly-5)shows clear resolution ability for the racemate of cobalt(Ⅲ)acetylacetonate( Co( acac)3 ),whereas the corresponding regioirregular polymer(poly-3)does not show any chiral recognition for Co(acac)3. The regioregular polymer main-chain seems to play an important role not only in providing an efficient interaction with the racemate but also in expressing the chiral recognition ability as a CSP for HPLC.

  5. Enhancement of Nitrite Reduction Kinetics on Electrospun Pd-Carbon Nanomaterial Catalysts for Water Purification.

    Science.gov (United States)

    Ye, Tao; Durkin, David P; Hu, Maocong; Wang, Xianqin; Banek, Nathan A; Wagner, Michael J; Shuai, Danmeng

    2016-07-20

    We report a facile synthesis method for carbon nanofiber (CNF) supported Pd catalysts via one-pot electrospinning and their application for nitrite hydrogenation. A mixture of Pd acetylacetonate (Pd(acac)2), polyacrylonitrile (PAN), and nonfunctionalized multiwalled carbon nanotubes (MWCNTs) was electrospun and thermally treated to produce Pd/CNF-MWCNT catalysts. The addition of MWCNTs with a mass loading of 1.0-2.5 wt % (to PAN) significantly improved nitrite reduction activity compared to the catalyst without MWCNT addition. The results of CO chemisorption confirmed that the addition of MWCNTs increased Pd exposure on CNFs and hence improved catalytic activity.

  6. Recubrimientos de Pd (Ag)-ZrO2 obtenidos por CVD para electrodos utilizados en la purificación electroquímica de aguas de desecho

    OpenAIRE

    Ferrétiz Anguiano, Jorge Luis

    2013-01-01

    In this research Pd – ZrO2 composite thin films were synthetized by Metalorganic Chemical Vapor Deposition (MOCVD) in order to obtain anticorrosive coatings for electrodes used in the technique of water treatment called Electrodyalisis. Coatings were deposited on AISI 304L stainless steel substrates in ratios of 10 – 90, 20 – 80 and 30 – 70 wt % Pd and Zr precursors (acetylacetonates) respectively, and temperatures of 450, 500 and 550 °C. Gas flows were adjusted at 130 cm3min-1 at ratio of 20...

  7. Lanthanide-containing polyimides

    Science.gov (United States)

    Stoakley, D. M.; St. Clair, Anne K.

    1987-01-01

    The preparation of a variety of lanthanide-containing polyimide films is described, and results of their characterization are presented. The properties investigated include the glass transition temperature, thermooxidative stability, magnetic susceptibility, and electrical conductivity of the polymer. Films containing lanthanide chlorides, fluorides, and sulfides are flexible, but those containing lanthanide nitrates are extremely brittle. The addition of lanthanide acetates and acetylacetonates caused immediate gelation of two of the synthesis-mixture ingredients. It was found that, in general, the addition of lanthanide to the polyimide increases the density and glass transition temperature of the polymer but slightly decreases the thermooxidative stability.

  8. Near-Monodisperse Ni-Cu Bimetallic Nanocrystals of Variable Composition: Controlled Synthesis and Catalytic Activity for H2 Generation

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Yawen; Huang, Wenyu; Habas, Susan E.; Kuhn, John N.; Grass, Michael E.; Yamada, Yusuke; Yang, Peidong; Somorjai, Gabor A.

    2008-07-22

    Near-monodisperse Ni{sub 1-x}Cu{sub x} (x = 0.2-0.8) bimetallic nanocrystals were synthesized by a one-pot thermolysis approach in oleylamine/1-octadecene, using metal acetylacetonates as precursors. The nanocrystals form large-area 2D superlattices, and display a catalytic synergistic effect in the hydrolysis of NaBH{sub 4} to generate H{sub 2} at x = 0.5 in a strongly basic medium. The Ni{sub 0.5}Cu{sub 0.5} nanocrystals show the lowest activation energy, and also exhibit the highest H{sub 2} generation rate at 298 K.

  9. Avaliação da "microverdura" de sínteses com a estrela verde

    Directory of Open Access Journals (Sweden)

    Rita C. C. Duarte

    2014-07-01

    Full Text Available This article reports a study to increase the overall greenness of chemical syntheses for first-year university laboratories. The separate evaluation of the micro-greenness of the three stages of synthesis (reaction, isolation and purification using the Green Star (GS was implemented and their respective contribution to overall greenness was investigated for two examples: syntheses of cobalt (III tris(acetylacetonate and potassium nitrilosulfonate. Results showed that the post-reaction (work-up steps are the most problematic for overall greenness. Greenness optimization can be achieved by combining the greenest procedures for each step obtained from different protocols available in the literature.

  10. Kinetische Untersuchungen zur Nucleophilie stabilisierter Carbanionen

    OpenAIRE

    2001-01-01

    1. In Anlehnung an Literaturvorschriften wurden die 7-aryl-2,6-di-tert-butylsubstituierten Chinonmethide 20a-d synthetisiert.1. In Anlehnung an Literaturvorschriften wurden die 7-aryl-2,6-di-tert-butylsubstituierten Chinonmethide 20a-d synthetisiert. 3. Durch Deprotonierung mit Kaliumethanolat als Base wurden die Kaliumsalze von Meldrumsäure (24a-K + ), Malonnitril (24b-K + ), Dimedon (24c-K + ), Cyanessigsäureethylester (24d-K + ), Acetylaceton (24e-K + ), Acetessigester (24f-K +...

  11. Synthesis and Photophysical Properties of Dy3+ and Gd3+ Polymeric Complexes with Functionalized Polybenzimidazole Containing β-Diketone Side Group

    Institute of Scientific and Technical Information of China (English)

    2007-01-01

    The polymeric ligand PBIa (functionalized polybenzimidazole containing β-diketone side group) was successfully synthesized via the reaction of polybenzimidazole (PBI) with 3-Br-acetylacetone in DMSO solvent using NaH as the deprotonation reagent. Its corresponding polymeric complexes of Dy3+ and Gd3+ were prepared and characterized by FT-IR, 1H NMR, molar conductance measurements, and thermal analysis. The photoluminescence properties and the probable mechanism of the Dy and Gd complexes were studied. The measurement and analysis of the thermal properties showed that these were thermal stable.

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

    DEFF Research Database (Denmark)

    Johannessen, Tue; Koutsopoulos, Sotiris

    2002-01-01

    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......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...

  13. 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...... with diameter 25-40 nm and specific surface area 27-43 m2/g. The crystallite size for both oxides, estimated from the XRD line broadening, is comparable to or slightly smaller than the primary particle diameter. The specific surface area increases and the primary particle size decreases with a decreasing flame...

  14. Synthesis of novel pyrazolylquinoxalines

    Energy Technology Data Exchange (ETDEWEB)

    Kim, Ho Sik [Catholoic University of Taegu-Hyosung, Gyongsan (Korea, Republic of); Kwag, Sam Tag [Pukyong National Univ., Pusan (Korea, Republic of)

    2000-06-01

    The reaction of 6-chloro-2-hydrazinoquinoxaline 4-oxide (10) with acetylacetone or dibenzoylmethane gave 6-chloro-2-(3,5-disubstituted pyrazol-1-yl)quinoxaline 4-oxide (11) through the intramolecular cyclization. The chlorination of compound 11 with phosphoryl chloride afforded 3,6-dichloro-2-(3,5-disubstituted pyrazol-l-yl)quinoxalines (12), whose reaction with hydrazine hydrate provided 6-chloro-3-hydrazino-2-(3,4-disubstituted pyrazol-l-yl)quinoxalines (13). The reaction of compound 13 with substituted benzaldehydes, benzenesulfonyl chloride, substituted benzoyl chlorides or acyl chlorides gave novel pyrazolylquinoxalines.

  15. Improved Low-Temperature Activity of V2O5-WO3/TiO2 for Denitration Using Different Vanadium Precursors

    OpenAIRE

    Lina Gan; Feng Guo; Jian Yu; Guangwen Xu

    2016-01-01

    This work tested two V2O5-WO3/TiO2 catalysts with different vanadium precursors for selective catalytic reduction (SCR) of flue gas NO using NH3 at 150–450 °C. While catalyst A was prepared using ammonium metavanadate (NH4VO3) through incipient impregnation, catalyst B was made according to the solvothermal method using vanadyl acetylacetonate (VO(acac)2) as the vanadium precursor. The catalytic evaluation for denitration was in a laboratory fixed bed reactor using simulated flue gas under co...

  16. Ozone sensing based on palladium decorated carbon nanotubes.

    Science.gov (United States)

    Colindres, Selene Capula; Aguir, Khalifa; Cervantes Sodi, Felipe; Vargas, Luis Villa; Salazar, José Moncayo; Febles, Vicente Garibay

    2014-04-14

    Multiwall carbon nanotubes (MWCNTs) were easily and efficiently decorated with Pd nanoparticles through a vapor-phase impregnation-decomposition method starting from palladium acetylacetonates. The sensor device consisted on a film of sensitive material (MWCNTs-Pd) deposited by drop coating on platinum interdigitated electrodes on a SiO₂ substrate. The sensor exhibited a resistance change to ozone (O₃) with a response time of 60 s at different temperatures and the capability of detecting concentrations up to 20 ppb. The sensor shows the best response when exposed to O3 at 120 °C. The device shows a very reproducible sensor performance, with high repeatability, full recovery and efficient response.

  17. Fabrication of Size-Tunable Metallic Nanoparticles Using Plasmid DNA as a Biomolecular Reactor

    Directory of Open Access Journals (Sweden)

    Charles Michael Drain

    2011-10-01

    Full Text Available Plasmid DNA can be used as a template to yield gold, palladium, silver, and chromium nanoparticles of different sizes based on variations in incubation time at 70 °C with gold phosphine complexes, with the acetates of silver or palladium, or chromium acetylacetonate. The employment of mild synthetic conditions, minimal procedural steps, and aqueous solvents makes this method environmentally greener and ensures general feasibility. The use of plasmids exploits the capabilities of the biotechnology industry as a source of nanoreactor materials.

  18. Effects of Palladium Loading on the Response of Thick Film Flame-made ZnO Gas Sensor for Detection of Ethanol Vapor

    OpenAIRE

    Sukon Phanichphant; Chaikarn Liewhiran

    2007-01-01

    ZnO nanoparticles doped with 0-5 mol% Pd were successfully produced in asingle step by flame spray pyrolysis (FSP) using zinc naphthenate and palladium (II)acetylacetonate dissolved in toluene-acetonitrile (80:20 vol%) as precursors. The effect ofPd loading on the ethanol gas sensing performance of the ZnO nanoparticles and thecrystalline sizes were investigated. The particle properties were analyzed by XRD, BET,AFM, SEM (EDS line scan mode), TEM, STEM, EDS, and CO-pulse chemisorptionmeasurem...

  19. Effects of Palladium Loading on the Response of a Thick Film Flame-made ZnO Gas Sensor for Detection of Ethanol Vapor

    OpenAIRE

    Liewhiran, Chaikarn; Phanichphant, Sukon

    2007-01-01

    ZnO nanoparticles doped with 0-5 mol% Pd were successfully produced in a single step by flame spray pyrolysis (FSP) using zinc naphthenate and palladium (II) acetylacetonate dissolved in toluene-acetonitrile (80:20 vol%) as precursors. The effect of Pd loading on the ethanol gas sensing performance of the ZnO nanoparticles and the crystalline sizes were investigated. The particle properties were analyzed by XRD, BET, AFM, SEM (EDS line scan mode), TEM, STEM, EDS, and CO-pulse chemisorption me...

  20. 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.

  1. Synthesis and characterization of graphene oxide composite with Fe3O4

    Directory of Open Access Journals (Sweden)

    Chuanyu Sun

    2015-09-01

    Full Text Available In the paper, a magnetic composite of graphene oxide (MGO has been successfully synthesized through decomposition of iron (III acetylacetonate in the mixture solution of triethylene glycol and graphene oxide (GO. Atomic force microscopy (AFM, transmission electron microscopy (TEM, X-ray diffraction (XRD and superconducting quantum interference device were used to characterize the material. The results show that the magnetic Fe3O4 nanoparticles modified graphene oxide composite with superparamagnetic properties, and magnetization saturation of 16.4 emu/g has been obtained. The MGO has a good sustained-release performance, and in vitro cytotoxicity confirming its secure use as a potential drug carrier.

  2. Preparation and characterization of perfluorosulfonic resin/titania hybrid transparent films

    Institute of Scientific and Technical Information of China (English)

    LI JianMei; XUE MinZhao; ZHANG YongMing; LIU YanGang

    2007-01-01

    Preparation and characterization of perfluoroaulfonic resin/titaniaorganic-inorganic hybrid films were presented. The transparent hybrid films were prepared by hydrothermal treatment at low temperature of a mixed solution of tetrabutyl titanata and perfluorosulfonic resin with the help of acetylacetone. The charactarization was carried out by SEM, XRD, FT-IR, UV-Vis and TGA. The results showed that the perfiuorosulfonic resin/titania hybrid transparent films were composed of titania particles dispersed in the perfluorosulfonic resin matrix very well and the titania was of anatase phase. Its diameter decreased with increasing weight ratio of titania to perfluorosulfonic resin.

  3. 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.

  4. 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.

  5. Syntheses, magnetic and spectral studies on polystyrene supported coordination compounds of bidentate and tetradentate Schiff bases

    Indian Academy of Sciences (India)

    D Kumar; P K Gupta; A Syamal

    2005-05-01

    The reaction of aminomethylated polystyrene (PSCH2-NH2) and 2-hydroxyacetanilide in DMF results in the formation of polystyrene-anchored monobasic bidentate Schiff base, PSCH2-LH (I). On the other hand, the reaction of chloromethylated polystyrene (PSCH2-Cl), 3-formylsalicylic acid, ethylenediamine and acetylacetone in DMF in presence of ethyl acetate (EA) and triethylamine (TEA) produces another polystyrene-anchored dibasic tetradentate Schiff base, PSCH2-L'H2 (II). Both I and II react with a number of di-, tri- and hexavalent metal ions like Co, Ni, Cu, Zn and Cd to form polystyreneanchored coordination compounds, and these have been characterized and discussed.

  6. Preparation and characterization of perfluorosulfonic resin/titania hybrid transparent films

    Institute of Scientific and Technical Information of China (English)

    2007-01-01

    Preparation and characterization of perfluorosulfonic resin/titania organic-inorganic hybrid films were presented. The transparent hybrid films were prepared by hydrothermal treatment at low temperature of a mixed solution of tetrabutyl titanate and perfluorosulfonic resin with the help of acetylacetone. The characterization was carried out by SEM,XRD,FT-IR,UV-Vis and TGA. The results showed that the perfluorosulfonic resin/titania hybrid transparent films were composed of titania particles dispersed in the perfluorosulfonic resin matrix very well and the titania was of anatase phase. Its diameter de-creased with increasing weight ratio of titania to perfluorosulfonic resin.

  7. Unconstrained Heterogeneous Colloidal Quantum Dots Embedded in GaAs/GaSb Nanovoids

    Science.gov (United States)

    2014-04-17

    layer at 510 C was grown. A III:V beam equivalent pressure ( BEP ) ratio of 1:6 was used to grow GaSb. The RHEED pattern was used to check for a (31...resulted in a smoothing of the surface, with continued growth for about 20 nm. A III:V BEP ratio of 1:10 was used for the GaAs growth. 3.2 Formation of...argon As – arsenic BEP – beam equivalent pressure BF – bright field Cd – cadmium Cd(acac)2 – cadmium acetylacetonate CdSe – cadmium selenide cm

  8. SYNTHETIC AND CATALYTIC PROPERTY STUDIES ON SILICA SUPPORTED BIS-(ACETYLACETONATO ) COBALT(Ⅱ) COMPLEXES

    Institute of Scientific and Technical Information of China (English)

    LI Xiaohu; LU Yun; LIN Sicong

    1992-01-01

    This paper reports mainly the preparation of silica supported acetylacetone ligands and their cobalt complexes, the characterization of their chemical structure, and the evaluation of their catalytic activity in the reaction for the preparation of ethers directly from alkanols and benzyl chloride. The results indicate that those silica supported β-diketone cobalt complexes (SACO) not only can simplify the reaction procedure of the ether preparation but also show a much higher catalytic activity in comparison with other homogeneous catalysts. In addition, SACO can be recovered and reused although their catalytic activity descend gradually as a result of the decrease in their cobalt content.

  9. Cobalt ion-containing epoxies

    Science.gov (United States)

    Stoakley, D. M.; St.clair, A. K.

    1983-01-01

    Varying concentrations of an organometallic cobalt complex were added to an epoxy system currently used by the aerospace industry as a composite matrix resin. Methods for combining cobalt (III) acetylacetonate with a tetraglycidyl 4,4 prime - diaminodiphenylmethane-based epoxy were investigated. The effects of increasing cobalt ion concentration on the epoxy cure were demonstrated by epoxy gel times and differential scanning calorimetry cure exotherms. Analysis on cured cobalt-containing epoxy castings included determination of glass transition temperatures by thermomechanical analysis, thermooxidative stabilities by thermogravimetric analysis, and densities in a density gradient column. Flexural strength and stiffness were also measured on the neat resin castings.

  10. Studying dispersions of ferroelectric nanopowders in dioctyl phthalate as dielectric media for capacitive electronic components

    Science.gov (United States)

    Gorokhovskii, A. V.; Gorshkov, N. V.; Burmistrov, I. N.; Goffman, V. G.; Tret'yachenko, E. V.; Sevryugin, A. V.; Fedorov, F. S.; Kovyneva, N. N.

    2016-06-01

    The electrical properties of dispersions of a powdered ferroelectric nanocomposite based on ilmenite (FeTiO3) and hollandite (K1.46Ti7.2Fe0.8O16) in dioctyl phthalate have been studied by impedance spectroscopy techniques in a frequency range of 10-1-106 Hz. The influence of stabilizing additives of cationic and anionic surfactants and iron acetylacetonate on the permittivity, conductivity, and dielectric losses was determined for dispersions containing 40 mass % of the solid composite. The influence of composition on the mechanisms of relaxation processes in the system is discussed.

  11. 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

    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...... 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...

  12. 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.

  13. Surface chemistry of a Cu(I) beta-diketonate precursor and the atomic layer deposition of Cu2O on SiO2 studied by x-ray photoelectron spectroscopy

    OpenAIRE

    Dhakal, Dileep; Waechtler, Thomas; E. Schulz, Stefan; Gessner, Thomas; Lang, Heinrich; Mothes, Robert; Tuchscherer, Andre

    2014-01-01

    This article has been published online on 21st May 2014, in Journal of Vacuum Science & Technology A: Vac (Vol.32, Issue 4): http://scitation.aip.org/content/avs/journal/jvsta/32/4/10.1116/1.4878815?aemail=author DOI: 10.1116/1.4878815 This article may be accessed via the issue's table of contents at this link: http://scitation.aip.org/content/avs/journal/jvsta/32/4?aemail=author The surface chemistry of the bis(tri-n-butylphosphane) copper(I) acetylacetonate, [(nBu3P)2Cu(a...

  14. Density Functional Theory Study of Atomic Layer Deposition of Zinc Oxide on Graphene.

    Science.gov (United States)

    Ali, Amgad Ahmed; Hashim, Abdul Manaf

    2015-12-01

    The dissociation of zinc ions (Zn(2+)) from vapor-phase zinc acetylacetonate, Zn(C5H7O2)2, or Zn(acac)2 and its adsorption onto graphene oxide via atomic layer deposition (ALD) were studied using a quantum mechanics approach. Density functional theory (DFT) was used to obtain an approximate solution to the Schrödinger equation. The graphene oxide cluster model was used to represent the surface of the graphene film after pre-oxidation. In this study, the geometries of reactants, transition states, and products were optimized using the B3LYB/6-31G** level of theory or higher. Furthermore, the relative energies of the various intermediates and products in the gas-phase radical mechanism were calculated at the B3LYP/6-311++G** and MP2/6-311 + G(2df,2p) levels of theory. Additionally, a molecular orbital (MO) analysis was performed for the products of the decomposition of the Zn(acac)2 complex to investigate the dissociation of Zn(2+) and the subsequent adsorption of H atoms on the C5H7O2 cluster to form acetylacetonate enol. The reaction energies were calculated, and the reaction mechanism was accordingly proposed. A simulation of infrared (IR) properties was performed using the same approach to support the proposed mechanism via a complete explanation of bond forming and breaking during each reaction step.

  15. 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

  16. A new copper(II) Schiff base complex containing asymmetrical tetradentate N2O2 Schiff base ligand: Synthesis, characterization, crystal structure and DFT study

    Science.gov (United States)

    Grivani, Gholamhossein; Baghan, Sara Husseinzadeh; Vakili, Mohammad; Khalaji, Aliakbar Dehno; Tahmasebi, Vida; Eigner, Václav; Dušek, Michal

    2015-02-01

    A new copper (II) Schiff base complex, CuL1, was prepared from the reaction of asymmetrical Schiff base ligand of L1 and Cu(OAC)2 (L1 = salicylidene imino-ethylimino-pentan-2-one). The Schiff base ligand, L1, and its copper (II) complex, CuL1, have been characterized by elemental analysis (CHN) and FT-IR and UV-vis spectroscopy. In addition, 1H NMR was employed for characterization of the ligand. Thermogrametric analysis of the CuL1 reveals its thermal stability and its decomposition pattern shows that it is finally decomposed to the copper oxide (CuO). The crystal structure of CuL1 was determined by the single crystal X-ray analysis. The CuL1 complex crystallizes in the monoclinic system, with space group P21/n and distorted square planar coordination around the metal ion. The Schiff base ligand of L1 acts as a chelating ligand and coordinates via two nitrogen and two oxygen atoms to the copper (II) ion with C1 symmetry. The structure of the CuL1 complex was also studied theoretically at different levels of DFT and basis sets. According to calculated results the Csbnd O bond length of the salicylate fragment is slightly higher than that in the acetylacetonate fragment of ligand, which could be interpreted by resonance increasing between phenyl and chelated rings in ligand in relative to the acetylacetonate fragment.

  17. 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.

  18. Synthesis, spectroscopic characterization and thermal studies of some lanthanide(Ⅲ) nitrate complexes with a hydrazo derivative of 4-aminoantipyrine

    Institute of Scientific and Technical Information of China (English)

    K. Mohanan; C.J. Athira; Y. Sindhu; M.S. Sujamol

    2009-01-01

    A heterocyclic ligand synthesized by the coupling of diazotized 4-aminoantipyrine with acetylacetone reacted with lanthanide(Ⅲ) nitrate to form complexes of the type [Ln(HAAP)2(NO3)3] where, Ln=La(Ⅲ), Ce(Ⅲ), Pr(Ⅲ), Nd(Ⅲ), Sm(Ⅲ), or Gd(Ⅲ) and HAAP=3-{[2-(N-1-pheny1-2,3-dimethylpyrazol-3-in-5-on-4-yl)]hydrazone}pent-2,3,4-trione. The ligand and metal complexes were characterized on the basis of elemental analysis, molar conductance, magnetic susceptibility measurements, UV-Visible, infrared, far infrared and proton NMR spectral data. The spectral data revealed that the ligand existed in the hydrazo form and coordinated to the metal ion without deproto-nation in a neutral tridentate manner, through carbonyl oxygen of pyrazolone ring, hydrazo nitrogen and carbonyl oxygen of the acetylace-tone moiety. The molar conductance values adequately supported their non-electrolytic nature. The ligand and the praseodymium(Ⅲ) com-plex were subjected to X-ray diffraction studies. Thermal decomposition behavior of the lanthanum(Ⅲ) complex was also examined.moiety.

  19. 黄铁矿和黄铜矿中铁铜钴镍的纸层析及定量测定

    Institute of Scientific and Technical Information of China (English)

    中国科学院贵阳地球化学研究所中心分析室

    1973-01-01

    The method of paper chromatography for the separation and quantitative determination of iron, copper, cobalt and nickel in pyrite and chalcopyrite is described.The three systems of ehromtograpbie solvents for the separation of iron, copper, cobalt and nickel on the 8×25 or 15×26 cm Whatman No. 3, involving acetone-hydrochloric acid-water, butanone-hydrochloric acid-water and acetone-acetylacetone-hydrochloric acid-water have been tested. As a developing system for the separation of this four elements in samples, the mixture of aoetone-acetylacetone-hydroehlorio acid-water is considered to be the best. After developing in a 30×40 cm glass dryer, the paper is dried in air and rendered the zone visible by treatment with 0.1% (W/V) rubeanic acid solution. The R1 values, colour reactions with this spray reagent and the eolour are given. A good paper chromatography of elements has been obtained. The elements are determined by colorimetrie method, with 1-nitroso-2-naphthol for cobalt,1-(2-pyridylozo)-2-naphthol for nickel, oxalic acid bis-cyelohexylidene hydrozide for copper, and sulfosalicylic acid for iron. In addition, iron and copper can also be determined by titration with potassium dichromate solution and iodimetry respectively.

  20. Optimization of process conditions for the production of TiO2–N film by sol–gel process using response surface methodology

    Indian Academy of Sciences (India)

    Rui Liu; Ching-Shieh Hsieh; Wein-Duo Yang; Hui-Yi Tsai

    2014-10-01

    TiO2–N film has been synthesized successfully through the sol–gel method. It is found that the anatase phase is formed at 400 °C and converted to rutile phase at 600 °C. The response surface methodology (RSM) and Box–Behnken design were employed to optimize the process conditions of sol–gel process. 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. The adjusted determination coefficient ($R^{2}_{\\text{Adj}}$) of the regression model was 0.9651, which indicated that the regression model is significant. By analysing the contour plots of response surface as well as solving the regression model, the optimized conditions were obtained as: 0.19 for molar ratio of surfactant to Ti, 2.01 for molar ratio of acetylacetone to Ti, 1.38 for molar ratio of water to Ti and 500 °C for calcination temperature. The predicted roughness of TiO2–N film for the optimized condition was calculated to be 41 nm. Confirmation experiments using the optimized conditions were performed, and a value about 43 nm was obtained. The experimental results are in good agreement with the predicted results.

  1. Surfactantless synthesis and textural properties of self-assembled mesoporous SnO{sub 2}

    Energy Technology Data Exchange (ETDEWEB)

    Velasquez, Celso [Departamento de QuImica, Universidad Autonoma Metropolitana-Iztapalapa, PO Box 55-534, Mexico, DF 09340 (Mexico); Ojeda, MarIa Luisa [Instituto de QuImica, UNAM, Circuito Exterior, Ciudad Universitaria, CP 04510, Mexico, DF (Mexico); Campero, Antonio [Departamento de QuImica, Universidad Autonoma Metropolitana-Iztapalapa, PO Box 55-534, Mexico, DF 09340 (Mexico); Esparza, Juan Marcos [Departamento de QuImica, Universidad Autonoma Metropolitana-Iztapalapa, PO Box 55-534, Mexico, DF 09340 (Mexico); Rojas, Fernando [Departamento de QuImica, Universidad Autonoma Metropolitana-Iztapalapa, PO Box 55-534, Mexico, DF 09340 (Mexico)

    2006-07-28

    Ordered surfactantless self-assembled, mesoporous SnO{sub 2} adsorbents, consisting of tubular voids of nanometric sizes, are prepared by the sol-gel processing of tin (IV) tetra-tert-amyloxide, Sn(OAm{sup t}){sub 4}, whose molecules have been previously chelated with acetylacetone in the absence of water, to modulate their reactivity and to promote an incipient self-assembling of -O-Sn-O oligomeric species; ultimately, the necessary amount of water to induce the hydrolysis-condensation reactions is added to this aged sol, then producing tubular pore templates within the SnO{sub 2} xerogel network. A collection of mesoporous SnO{sub 2} xerogels of assorted structural properties has been obtained after calcination in air of precursory gels proceeding from an aged mixture of Sn(OAm{sup t}){sub 4} and acetylacetone at temperatures in the range 200-1000 deg. C. N{sub 2} sorption isotherms measured on these SnO{sub 2} solids evidence mesoporous structures of diverse textural characteristics (i.e. pore widths of 3-50 nm and surface areas of 10-140 m{sup 2} g{sup -1}) in which voids virtually behave as if they are independent cylindrical pores during capillary condensation and evaporation.

  2. Synthesis and characterization of polyaluminocarbosilane as SiC ceramic precursor

    Institute of Scientific and Technical Information of China (English)

    余煜玺; 李效东; 曹峰; 冯春祥

    2004-01-01

    Polyaluminocarbosilane (PACS) was synthesized by the reaction of aluminum acetylacetonate(Al(AcAc)3) with polysilacarbosilane (PSCS), which was prepared by thermolysis and condensation of polydimeth-ylsilane (PDMS). The sublimation of Al(AcAc)3 could be avoided by the use of PSCS as reactant. The empiricalformula of PACS was SiC2.01 H7. 66 O0.13 Al0.02, which has the relative molecular mass of 2 265. When the reaction ofPSCS with Al(AcAc)3 proceeds, an enormous decrease in the number of Si-H bonds in PSCS is observed, at thesame time, gas acetylacetonate is a by-product of the reaction based on the ligands of Al(AcAc)3. The reactionmechanism is found to be related to the increase in the molecular mass of PACS by the cross-linking reaction ofSi-H bonds in PSCS with Al(AcAc)3, which leads to the formation of Si-Al bonds.

  3. Preparation of Ultrafine Fe-Pt Alloy and Au Nanoparticle Colloids by KrF Excimer Laser Solution Photolysis.

    Science.gov (United States)

    Watanabe, Masato; Takamura, Hitoshi; Sugai, Hiroshi

    2009-03-10

    We prepared ultrafine Fe-Pt alloy nanoparticle colloids by UV laser solution photolysis (KrF excimer laser of 248 nm wavelength) using precursors of methanol solutions into which iron and platinum complexes were dissolved together with PVP dispersant to prevent aggregations. From TEM observations, the Fe-Pt nanoparticles were found to be composed of disordered FCC A1 phase with average diameters of 0.5-3 nm regardless of the preparation conditions. Higher iron compositions of nanoparticles require irradiations of higher laser pulse energies typically more than 350 mJ, which is considered to be due to the difficulty in dissociation of Fe(III) acetylacetonate compared with Pt(II) acetylacetonate. Au colloid preparation by the same method was also attempted, resulting in Au nanoparticle colloids with over 10 times larger diameters than the Fe-Pt nanoparticles and UV-visible absorption peaks around 530 nm that originate from the surface plasmon resonance. Differences between the Fe-Pt and Au nanoparticles prepared by the KrF excimer laser solution photolysis are also discussed.

  4. Preparation of Ultrafine Fe–Pt Alloy and Au Nanoparticle Colloids by KrF Excimer Laser Solution Photolysis

    Directory of Open Access Journals (Sweden)

    Sugai Hiroshi

    2009-01-01

    Full Text Available Abstract We prepared ultrafine Fe–Pt alloy nanoparticle colloids by UV laser solution photolysis (KrF excimer laser of 248 nm wavelength using precursors of methanol solutions into which iron and platinum complexes were dissolved together with PVP dispersant to prevent aggregations. From TEM observations, the Fe–Pt nanoparticles were found to be composed of disordered FCC A1 phase with average diameters of 0.5–3 nm regardless of the preparation conditions. Higher iron compositions of nanoparticles require irradiations of higher laser pulse energies typically more than 350 mJ, which is considered to be due to the difficulty in dissociation of Fe(III acetylacetonate compared with Pt(II acetylacetonate. Au colloid preparation by the same method was also attempted, resulting in Au nanoparticle colloids with over 10 times larger diameters than the Fe–Pt nanoparticles and UV–visible absorption peaks around 530 nm that originate from the surface plasmon resonance. Differences between the Fe–Pt and Au nanoparticles prepared by the KrF excimer laser solution photolysis are also discussed.

  5. Preparation of amorphous aluminum oxide-hydroxide nanoparticles in amphiphilic silicone-based copolymer microemulsions.

    Science.gov (United States)

    Berkovich, Yana; Aserin, Abraham; Wachtel, Ellen; Garti, Nissim

    2002-01-01

    Organo-inorgano nanocomposites with colloidal dimensions have interesting optical, catalytic, and mechanical properties, particularly when such hybrids are reinforced with transition metal oxide nanoparticles. Nanoparticles with a mean size of 1.0-2.4 nm are obtained through hydrolysis of aluminum isopropoxide in the L(2) phase of amphiphilic (PDMS-POE) polydimethylsiloxane-polyoxyethylene Silwet L-7607-octanol/acetylacetone-water mixtures. The particle sizes are related weakly to the microemulsion composition: 0.8-1.2 nm for 20 wt% Silwet L-7607 and 2.0-2.4 nm for 50 wt% Silwet L-7607. Protection of the particles against aggregation is ensured through their confinement in the intraaggregate colloidal domains. Factors affecting the hydrolysis-condensation process of acetylacetone-complexed aluminum isopropoxide in copolymer-poor and copolymer-rich regions of PDMS-POE W/O microemulsions are studied by Fourier transform infrared spectroscopy, small angle X-ray scattering, and transmission electron microscopy. Prepared nanoparticulate dispersions possess long-term stability and form clear mixtures in different organic polar and nonpolar solvents.

  6. Mesoporous Titania Powders: The Role of Precursors, Ligand Addition and Calcination Rate on Their Morphology, Crystalline Structure and Photocatalytic Activity

    Directory of Open Access Journals (Sweden)

    Elisabetta Masolo

    2014-07-01

    Full Text Available We evaluate the influence of the use of different titania precursors, calcination rate, and ligand addition on the morphology, texture and phase content of synthesized mesoporous titania samples, parameters which, in turn, can play a key role in titania photocatalytic performances. The powders, obtained through the evaporation-induced self-assembly method, are characterized by means of ex situ X-Ray Powder Diffraction (XRPD measurements, N2 physisorption isotherms and transmission electron microscopy. The precursors are selected basing on two different approaches: the acid-base pair, using TiCl4 and Ti(OBu4, and a more classic route with Ti(OiPr4 and HCl. For both precursors, different specimens were prepared by resorting to different calcination rates and with and without the addition of acetylacetone, that creates coordinated species with lower hydrolysis rates, and with different calcination rates. Each sample was employed as photoanode and tested in the water splitting reaction by recording I-V curves and comparing the results with commercial P25 powders. The complex data framework suggests that a narrow pore size distribution, due to the use of acetylacetone, plays a major role in the photoactivity, leading to a current density value higher than that of P25.

  7. Effects of Paste Components on the Properties of Porous TiO2 Film for Dye-sensitized Solar Cells%浆料组成对染料敏化多孔TiO2太阳能电池性能的影响

    Institute of Scientific and Technical Information of China (English)

    康姣; 胡志强; 周红茹; 杨冬雪

    2011-01-01

    The TiO2 paste was obtained by ball milling,with varying amounts of PEG400,OP emulsifier and acetylacetone.Then the screen-printed technique was adopted to fabricate porous TiO2 film anode on substrate,and DSSC was assembled by TiO2 film anode.The experimental samples were investigated and measured by means of SEM ,XRD and electrochemical method.The effect of PEG400,OP emulsification,acetylacetone and ball milling time on DSSC properties was discussed by orthogonal experiment.The results indicate that the optimal component are PEG400 of 0.4mL,OP emulsifier of 0.02 mL,acetylacetone of 0.6mL and the ball milling time of 4h.The value of overall energy conversion efficiency η of DSSC of the optimal assembed is 3.44%.%在TiO2粉体中加入不同量的聚乙二醇400、OP乳化剂和乙酰丙酮,经球磨得到TiO2浆料,采用丝网印刷的工艺方法在基底上制备了多孔TiO2薄膜阳极,组装成DSSC.采用SEM、XRD和电化学工作站进行了表征及测试;利用正交实验探讨了浆料中聚乙二醇400、OP乳化剂、乙酰丙酮的量和球磨时间对DSSC光电性能的影响.研究结果表明,浆料的最佳配方是聚乙二醇400为0.4mL、OP乳化剂为0.02mL、乙酰丙酮为0.6mL和球磨时间为4h,由此可使制备的DSSC光电转化效率(η)达到3.44%.

  8. Chemistry of Cu(acac){sub 2} on Ni(110) and Cu(110) surfaces: Implications for atomic layer deposition processes

    Energy Technology Data Exchange (ETDEWEB)

    Ma Qiang; Zaera, Francisco [Department of Chemistry, University of California, Riverside, California 92521 (United States)

    2013-01-15

    The thermal chemistry of copper(II)acetylacetonate, Cu(acac){sub 2}, on Ni(110) and Cu(110) single-crystal surfaces was probed under vacuum by using x-ray photoelectron spectroscopy (XPS) and temperature programmed desorption (TPD). Some data for acetylacetone (Hacac, CH{sub 3}COCH{sub 2}COCH{sub 3}) adsorbed on Ni(110) are also reported as reference. Chemical transformations were identified in several steps covering a temperature range from 150 K to at least 630 K. The desorption of Hacac and a 3-oxobutanal (CH{sub 3}COCH{sub 2}CHO) byproduct was observed first at 150 and 180 K on Ni(110) and at 160 and 185 K on Cu(110), respectively. Partial loss of the acetylacetonate (acac) ligands and a likely change in adsorption geometry are seen next, with the possible production of HCu(acac), which desorbs at 200 and 235 K from the nickel and copper surfaces, respectively. Molecular Cu(acac){sub 2} desorption is observed on both surfaces at approximately 300 K, probably from recombination of Cu(acac) and acac surface species. The remaining copper atoms on the surface lose their remaining acac ligands to the substrate and become reduced directly to metallic copper. At the same time, the organic ligands follow a series of subsequent surface reactions, probably involving several C-C bond-scissions, to produce other fragments, additional Hacac and HCu(acac) in the gas phase in the case of the copper surface, and acetone on nickel. A significant amount of acac must nevertheless survive on the surface to high temperatures, because Hacac peaks are seen in the TPD at about 515 and 590 K and the C 1s XPS split associated with acac is seen up to close to 500 K. In terms of atomic layer deposition processes, this suggests that cycles could be design to run at such temperatures as long as an effective hydrogenation agent is used as the second reactant to remove the surface acac as Hacac. Only a small fraction of carbon is left behind on Ni after heating to 800 K, whereas more carbon

  9. 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.

  10. Investigation of the oxygen affinity of manganese(II, cobalt(II and nickel(II complexes with some tetradentate Schiff bases

    Directory of Open Access Journals (Sweden)

    Adel A.A. Emara

    2014-12-01

    Full Text Available Oxygen absorption–desorption processes for square planar Mn(II, Co(II and Mn(II complexes of tetradentate Schiff base ligands in DMF and chloroform solvents were investigated. The tetradentate Schiff base ligands were obtained by condensation reaction of ethylenediamine with salcyldehyde, o-hydroxyacetophenone or acetylacetone in the molar ratio 1:2. The square planar complexes were prepared by the reaction of the Schiff base ligands with Mn(II acetate, Co(II nitrate and Ni(II nitrate in dry ethanol under nitrogen atmosphere. The sorption processes were undertaken in the presence and absence of (pyridine axial-base in 1:1 M ratio of (pyridine:metal(II complexes. Complexes in DMF indicate significant oxygen affinity than in chloroform solvent. Cobalt(II complexes showed significant sorption processes compared to Mn(II and Ni(II complexes. The presence of pyridine axial base clearly increases oxygen affinity.

  11. Electrophoretic deposition of thin SOFC-electrolyte films on porous La{sub 0,75}Sr{sub 0,2}MnO{sub 3-{delta}} cathodes

    Energy Technology Data Exchange (ETDEWEB)

    Argirusis, C.; Damjanovic, T.; Borchardt, G. [Technische Univ. Clausthal, Fachbereich Physik, Metallurgie und Werkstoffwissenschaften, Clausthal-Zellerfeld (Germany)

    2004-07-01

    Solid oxide fuel cells with an electrode supported thin film electrolyte (electrolyte thickness 5 {mu}m < d < 20 {mu}m) are a promising alternative to electrolyte supported single cells because of decreased electrolyte resistance. The electrophoretic deposition (EPD) was performed on A-site deficient La{sub 0.75}Sr{sub 0.2}MnO{sub 3-{delta}} (ULSM) from three different suspensions: (Y{sub 2}O{sub 3}){sub 0.08}(ZrO{sub 2}){sub 0.92} (YSZ), (Ce{sub 0.9}Gd{sub 0.1})O{sub 1.955} (GDC) and La{sub 0.9}Sr{sub 0.1}Ga{sub 0.8}Mg{sub 0.2}O{sub 2.85} (LSGM) in acetylacetone and isopropanol. The thickness of the deposits was controlled by varying the conditions of the electrophoretic deposition. (orig.)

  12. 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.

  13. Photoresist-Free Fully Self-Patterned Transparent Amorphous Oxide Thin-Film Transistors Obtained by Sol-Gel Process

    Science.gov (United States)

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

    2014-04-01

    We demonstrated self-patterned solution-processed amorphous oxide semiconductor thin-film transistors (TFTs) using photosensitive sol-gels. The photosensitive sol-gels were synthesized by adding β-diketone compounds, i.e., benzoylacetone and acetylacetone, to sol-gels. The chemically modified photosensitive sol-gels showed a high optical absorption at specific wavelengths due to the formation of metal chelate bonds. Photoreactions of the modified solutions enabled a photoresist-free process. Moreover, Zn-Sn-O with a high Sn ratio, which is hard to wet-etch using conventional photolithography due to its chemical durability, was easily patterned via the self-patterning process. Finally, we fabricated a solution-processed oxide TFT that included fully self-patterned electrodes and an active layer.

  14. Epoxidação do óleo de soja com o sistema catalítico [MoO2(acac2]/TBHP EM [bmim][PF6

    Directory of Open Access Journals (Sweden)

    Maritana Farias

    2012-01-01

    Full Text Available Epoxidation of soybean oil was investigated using 1-n-butyl-3-methylimidazolium hexafluorophosphate [bmim][PF6] 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 ºC 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 ¹H NMR data.

  15. 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.

  16. Schiff bases of N-(2-aminoethyl)-3-aminopropyltrimethoxysilane and its silatranes: Synthesis and characterization

    Indian Academy of Sciences (India)

    Gurjaspreet Singh; Amandeep Saroa; Sadhika Khullar; Sanjay K Mandal

    2015-04-01

    This paper aims at the introduction of azomethine group by the condensation reaction of N-(2-aminoethyl)-3-aminopropyltrimethoxysilane with different compounds containing carbonyl group such as 2’-hydroxyacetophenone, salicylaldehyde, pyrrole-2-carboxaldehyde, acetylacetone and ethyl acetoacetate. Further, transesterification reaction of these Schiff base modified silanes with triethanolamine as a tripodal ligand leads to the synthesis of corresponding silatranes 1–5 bearing Schiff base functionalized long chain in the axial position. All the synthesized compounds are characterized by spectroscopic methods, elemental analysis and mass spectrometry. The authentication of Schiff base modified silatranes is scrutinized by single X-ray crystal structure of silatrane 1. The thermal stability of the five silatranes is studied by thermo-gravimetric analysis (TGA).

  17. 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-.

  18. 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.

  19. Coordination Chemistry of [Co(acac)2 ] with N-Doped Graphene: Implications for Oxygen Reduction Reaction Reactivity of Organometallic Co-O4 -N Species.

    Science.gov (United States)

    Han, Jongwoo; Sa, Young Jin; Shim, Yeonjun; Choi, Min; Park, Noejung; Joo, Sang Hoon; Park, Sungjin

    2015-10-19

    Hybridization of organometallic complexes with graphene-based materials can give rise to enhanced catalytic performance. Understanding the chemical structures within hybrid materials is of primary importance. In this work, archetypical hybrid materials are synthesized by the reaction of an organometallic complex, [Co(II) (acac)2 ] (acac=acetylacetonate), with N-doped graphene-based materials at room temperature. Experimental characterization of the hybrid materials and theoretical calculations reveal that the organometallic cobalt-containing species is coordinated to heterocyclic groups in N-doped graphene as well as to its parental acac ligands. The hybrid material shows high electrocatalytic activity for the oxygen reduction reaction (ORR) in alkaline media, and superior durability and methanol tolerance to a Pt/C catalyst. Based on the chemical structures and ORR experiments, the catalytically active species is identified as a Co-O4 -N structure.

  20. Colorimetric solvent indicators based on Nafion membranes incorporating nickel(II)-chelate complexes.

    Science.gov (United States)

    Hosokawa, Hitoshi; Funasako, Yusuke; Mochida, Tomoyuki

    2014-11-10

    To develop solvent-recognition films, Nafion membranes incorporating cationic nickel-chelate complexes, that is, [Ni(L(1))(L(2))](+) (HL(1) = acetylacetone, 2,2,6,6-tetramethyl-3,5-heptanedione; L(2) = N,N-diethylethylenediamine, N-butyl-N,N',N'-trimethylethylenediamine), were prepared. Immersion of the films in various solvents effected the color changes varying from red to pale blue green depending on the donor number of the solvents. The color change is based on an equilibrium shift between square-planar and solvent-coordinated octahedral geometries of the cations. The degree of the color change depended on the affinity of the incorporated complex to the solvent molecules. The films were robust and exhibited a reversible solvent response. The films exhibited thermochromism when a small amount of appropriate solvents were incorporated and changed from pale blue green at low temperatures to red at high temperatures.

  1. Issues Affecting the Synthetic Scalability of Ternary Metal Ferrite Nanoparticles

    Directory of Open Access Journals (Sweden)

    Lauren Morrow

    2015-01-01

    Full Text Available Ternary Mn-Zn ferrite (MnxZn1-xFe2O4 nanoparticles (NPs have been prepared by the thermal decomposition of an oleate complex, sodium dodecylbenzenesulfonate (SDBS mediated hydrazine decomposition of the chloride salts, and triethylene glycol (TREG mediated thermal decomposition of the metal acetylacetonates. Only the first method was found to facilitate the synthesis of uniform, isolable NPs with the correct Mn : Zn ratio (0.7 : 0.3 as characterized by small angle X-ray scattering (SAXS, transmission electron microscopy (TEM, and inductively coupled plasma-optical emission spectroscopy (ICP-OES. Scaling allowed for retention of the composition and size; however, attempts to prepare Zn-rich ferrites did not result in NP formation. Thermogravimetric analysis (TGA indicated that the incomplete decomposition of the metal-oleate complexes prior to NP nucleation for Zn-rich compositions is the cause.

  2. Synthesis of thiophene-linked pyrimidopyrimidines as pharmaceutical leads

    Indian Academy of Sciences (India)

    M B Siddesh; Basavaraj Padmashali; K S Thriveni; C Sandeep

    2014-05-01

    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 pyirmidopyirimidines 4a-e which on refluxing with POCl3 in presence of DMF produced compounds 5a-e. Nucleophilic substitution reactions on 5a-e were carried out with aniline to obtain 6a-e. The structures of the newly synthesised compounds have been confirmed by elemental analysis and spectral studies. Some selected compounds have been screened for antibacterial and analgesic activities.

  3. (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.

  4. Nickelacyclic-cobaltocene vs. nickelacyclic-nickelocene. Synthesis, X-ray structures, electron transfer activity, EPR spectroscopy, and theoretical calculations.

    Science.gov (United States)

    Buchalski, Piotr; Kamińska, Elzbieta; Piwowar, Katarzyna; Suwińska, Kinga; Jerzykiewicz, Lucjan; Rossi, Fulvio; Laschi, Franco; de Biani, Fabrizia Fabrizi; Zanello, Piero

    2009-06-01

    Reactions of 9-nickelafluorenyllithium with cobalt and nickel pentamethylcyclopentadienyl-acetylacetonates resulted in the formation of the novel nickelacyclic-cobaltocene 2 and nickelacyclic-nickelocene 3, respectively, in which the central metal atom is bonded to the nickelafluorenyl ring. On the basis of their redox propensity, compounds 2 and 3 were oxidized to the corresponding monocations [2](+) and [3](+). The crystal and molecular structures of both the redox couples were determined by single-crystal X-ray analysis. In spite of their structural similarity, they display a rather different electron transfer ability. To throw light on such an aspect, the pertinent redox couples have been examined by EPR spectroscopy and the nature of the frontier orbitals involved in the redox activity of the neutral precursors has been supported by extended Huckel theoretical calculations.

  5. Catalytic performance for CO{sub 2} conversion to methanol of gallium-promoted copper-based catalysts. Influence of metallic precursors

    Energy Technology Data Exchange (ETDEWEB)

    Toyir, Jamil; Ramirez de la Piscina, Pilar; Homs, Narcis [Departament de Quimica Inorganica, Facultat de Quimica, Universitat de Barcelona, Marti i Franques 1-11, 08028 Barcelona (Spain); Fierro, Jose Luis G. [Instituto de Catalisis y Petroleoquimica, C.S.I.C., Cantoblanco, 28049 Madrid (Spain)

    2001-11-28

    This study reports new gallium-promoted copper-based catalysts prepared by co-impregnation of methoxide-acetylacetonate (acac) precursors from methanolic solutions onto silica and zinc oxide supports. Catalyst performance in the CO{sub 2} hydrogenation to methanol was investigated at 2MPa and temperatures between 523 and 543K. A high activity and selectivity for ZnO-supported catalysts was found, which also showed a high stability in terms of both activity and selectivity. The maximum value for the activity was 378gMeOH/kgcath at 543K, with a selectivity of 88% towards methanol production. The high performance of these materials in the CO{sub 2} hydrogenation is related to the presence of Ga{sub 2}O{sub 3} promoter and highly dispersed Cu{sup +} species on the surface, determined by XPS and Auger on used catalysts.

  6. Synthesis, spectral, thermal and thermodynamic studies of oxovanadium(IV) complexes of Schiff bases derived from 3,4-diaminobenzoic acid with salicylaldehyde derivatives.

    Science.gov (United States)

    Mohammadi, Khosro; Niad, Mahmood; Irandoost, Amene

    2013-04-15

    Synthesis and evaluation of three new oxovanadium(IV) complexes, formed by the interaction of vanadyl acetylacetonate and the Schiff bases: 3,4-bis((E)-2-hydroxybenzylideneamino)benzoic acid (L(1)), 3,4-bis-((E)-2-hydroxy-3-methoxybenzylideneamino)benzoic acid (L(2)) and 3,4-bis((E)-2,4-dihydroxybenzylideneamino)benzoic acid (L(3)) in methanol. The complexes have been characterized and studied by IR spectra, UV-Vis spectroscopy and thermogravimetry in order to evaluate their thermal stability and thermal decomposition. According to the results discussed from TG curves, the order of thermal stability for the complexes is VOL(3)>VOL(1)>VOL(2). Their formation constants (Kf) were obtained by UV-Vis spectroscopic titration at 15, 25, 35 and 45 °C in methanol by SQUAD software. The trend of formation constants of the complexes as follows: VOL(3)>VOL(2)>VOL(1).

  7. Platinum-Iridium Alloy Films Prepared by MOCVD

    Institute of Scientific and Technical Information of China (English)

    WEI Yan; CHEN Li; CAI Hongzhong; ZHENG Xu; YANG Xiya; HU Changyi

    2012-01-01

    Platinum-Iridium alloy films were prepared by MOCVD on Mo substrate using metal-acetylacetonate precursors.Effects of deposition conditions on composition,microstructure and mechanical properties were determined.In these experimental conditions,the purities of films are high and more than 99.0%.The films are homogeneous and monophase solid solution of Pt and Ir.Weight percentage of platinum are much higher than iridium in the alloy.Lattice constant of the alloy changes with the platinum composition.Iridium composition showing an up-down-up trend at the precursor temperature of 190~230℃ and the deposition temperature at 400~550℃.The hardness of Pt-Ir alloys prepared by MOCVD is three times more than the alloys prepared by casting.

  8. 含铍碳化硅陶瓷先驱体聚铍碳硅烷的合成%Synthesis of Precursor of SiC ceramic containing beryllium

    Institute of Scientific and Technical Information of China (English)

    段曦东; 李文芳; 周珊; 杜作娟; 王超英; 黄小忠

    2012-01-01

    Beryllium acetylacetonate [Be(acac)2] was synthesized using beryllium hydroxide, sulfuric acid and acetylacetone as raw material. Beryllium acetylacetonate [Be(acac)2] reacted with polycarbosilane (PCS) with heating,resionoid product was produced. In the reaction, the beryllium acetylacetonate was consumed, the melting point was rised comparing to the onset polycarbosilane. The clement analysis shows there are some beryllium in the product, the gel permeation chromatography GPC ana-lysis shows the molecular of the product rised comparing to the onset polycarbosilane. Fourier transform infrared spectroscopy (FT- IR) analysis shows there are such chemical structures in PBeCS:Si(CH3 )2- CH2 -,-Si(CH3 ) · (H)-CH2-.1H-NMR shows the Si-H bond in the reagent was consumed. The reaction mechanism is inferred on the basis of analysis result, and the Si-H bond played a crucial role in the formation of the product. The experiment and theory analysis shows the product is a kind of polycarbosilane containing beryllium, which can be called polyberylliumocar-bosilane (PBeCS). After treated under 1200℃ the product PBeCS can be converted into the silicon carbide containing Beryllium.%以氢氧化铍、硫酸和乙酰丙酮为原料合成了乙酰丙酮铍(Be(acac)2).用乙酰丙酮铍和聚碳硅烷在加热的条件下反应一定时间,生成了树脂状的产物.反应中乙酰丙酮铍被消耗,生成产物熔点相对起始聚碳硅烷熔点升高.元素分析表明产物中含有铍元素,凝胶渗透色谱分析表明产物分子量相对起始聚碳硅烷向增大的方向发生变化.傅立叶红外光谱分析表明产物中主要存在如下结构:Si(CH3)2—CH2—,—Si(CH3)·(H)—CH2—.核磁共振1H-NMR分析表明反应物中Si—H键被消耗.根据分析结果推测了反应机理,Si—H键的消耗在产物的形成中起了重要作用.实验与理论分析表明先驱体产物是一种含铍聚碳硅烷,可以命名为聚铍碳硅烷(PBeCS).在1200℃的高

  9. High temperature stability of anatase in titania-alumina semiconductors with enhanced photodegradation of 2, 4-dichlorophenoxyacetic acid.

    Science.gov (United States)

    López-Granada, G; Barceinas-Sánchez, J D O; López, R; Gómez, R

    2013-12-15

    The incorporation of aluminum acetylacetonate as alumina source during the gelation of titanium alkoxide reduces the nucleation sites for the formation of large rutile crystals on temperatures ranging from 400 to 800°C. As a result, the aggregation of anatase crystals is prevented at high temperature. A relationship among the specific surface area, pore size, energy band gap, crystalline structure and crystallite size as the most relevant parameters are evaluated and discussed. According to the results for the photocatalytic degradation of 2,4-dichlorophenoxyacetic acid, the specific surface area, pore size, Eg band gap are not determinant in the photocatalytic properties. It was found that the anatase crystallite size is the mores important parameter affecting the degradation efficiency.

  10. 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.

  11. Reaction of Silane Alkoxide with Acid Anhydride as a Novel Synthetic Method for Organic-Inorganic Hybrid Materials

    Institute of Scientific and Technical Information of China (English)

    Masahiro Fujiwara

    2005-01-01

    @@ 1Introduction Sol-gel method is a potent method to produce new inorganic and organic-inorganic hybrid materials. The key step of this methodology is the hydrolysis of a metal alkoxide or other metal substrates such as acetylacetonates to form hydroxyl metal species, followed by their condensation to metal-oxygen-metal (M - O - M)bonds. In this process, the utilization of water, generally in excess, is essential and alcoholic solvents such as ethanol are often required to homogenize the solution when organic compounds coexist. As the common sol-gel method using water allows for limited uses of organic substrates due to their low solubility and stability in aqueous solution, modified variations of sol-gel method are required. Recently, some processes were reported for preparing metal oxides from metal alkoxides without the utilization of water.

  12. 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.

  13. 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.

  14. A selective nanocatalyst for an efficient Ugi reaction: Magnetically recoverable Cu(acac)2/NH2-T/SiO2@Fe3O4 nanoparticles

    Indian Academy of Sciences (India)

    Monireh Ghavami; Maryam Koohi; Mohammad Zaman Kassaee

    2013-11-01

    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 spectroscopy (XPS). Further characterizations are carried out by different techniques. Selectivity of this catalyst is demonstrated through one-pot synthesis of fourteen α-aminoacyl amides using Ugi four-component reaction of cyclohexyl isocyanide, acetic acid, amines and various aldehydes. Interestingly, all aromatic aldehydes react with short reaction times and high yields, but heteroaromatic aldehydes do not yield any product. Catalyst efficiency remains unaltered through three consecutive experiments.

  15. STUDY ON PROPERTIES OF CURED COMPOUND IN CYANATE EATER AND EPOXY CO-CURING SYSTEM%环氧树脂与氰酸酯共固化产物性能的研究

    Institute of Scientific and Technical Information of China (English)

    陈平; 程子霞; 金镇镐; 雷清泉

    2001-01-01

    The influence of composition on the curing kinetic parameter,electrical,mechanical,thermal properties and the glass transition temperature of cured compound of epoxy and cyanate ester co-curing system catalyzed by transition metal acetylacetone was studied by means of DSC,dielectric and dynamic mechanical methods in this paper.The results showed that the reactive energy and frequency factor of co-curing is found to increase with enhanced concentrations of cyanate ester of co-curing system.The glass transition temperature and thermal stability of cyanate ester and epoxy cured system is found to increase with enhanced concentrations of the cyanate ester under the same cured condition,addition of the cyanate ester will decrease the loss factor and dielectrical constant value as well.

  16. TiO{sub 2} thin films prepared by sol - gel method

    Energy Technology Data Exchange (ETDEWEB)

    Suciu, R C; Indrea, E; Silipas, T D; Dreve, S; Rosu, M C [National Institute for Research and Development of Isotopic and Molecular Technologies, 65-103 Donath, 400293 Cluj-Napoca (Romania); Popescu, V; Popescu, G; Nascu, H I, E-mail: ramona.suciu@itim-cj.r [Technical University of Cluj-Napoca, Physics Department, 15 C Daicoviciu, 400020 Cluj-Napoca (Romania)

    2009-08-01

    There is a growing awareness that titania (TiO{sub 2}) and TiO{sub 2}-based oxide systems are the most promising candidates for the development of photoelectrodes for photoelectrochemical cell (PEC) for solar-hydrogen production. The PEC is equipped with a single photoelectrode (photoanode) and cathode, both of which are immersed in an aqueous electrolyte. In this work we present a sol-gel method to prepare TiO{sub 2} thin films on ITO using tetraisopropoxides of titanium, acetylacetone, 1-butanol and Tween 80 as surfactant. The films were deposited on ITO coated glass slides by spray pyrolysis. UV-VIS spectra and fluorescence measurements were made for the solutions and films. X-ray diffraction was used for structural investigations and the morphology of the film was studied by Scanning Electron Microscopy.

  17. 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.

  18. 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.

  19. Simultaneous polymerization of Mg and Zr alkoxides

    Energy Technology Data Exchange (ETDEWEB)

    Mendez-Vivar, J.; Lara, V.H. [Univ. Autonoma Metropolitana-Iztapalapa, Depto. de Quimica, Mexico, D. F. (Mexico); Mendoza-Serna, R.; Ayala-Morales, A. [Facultad de Estudios Superiores Zaragoza, UNAM, Carrera de Ingenieria Quimica, Mexico, D. F. (Mexico); Bosch, P. [Inst. de Investigaciones en Materiales, UNAM Circuito Exterior, Mexico, D. F. (Mexico)

    2004-07-01

    The preparation of homogeneous MgO-ZrO{sub 2} ceramics by the sol-gel process is of interest because of its potential technological applications as dielectric materials in thin films and membranes. In this work we used magnesium methoxide and zirconium n-propoxide as precursors. The simultaneous polymerization of the alkoxides was performed via the sol-gel process, using acetylacetone (acacH) and isoeugenol (isoH) separately as the chelating agents, in order to control the hydrolysis and condensation steps. Spectroscopic studies have been performed on the sols, gels, xerogels and oxides, including Fourier transform infrared (FTIR) spectroscopy and small Angle X-ray Scattering (SAXS). (orig.)

  20. Direct Dry-Grinding Synthesis of Monodisperse Lipophilic CuS Nanoparticles.

    Science.gov (United States)

    Li, Yajuan; Scott, Julie; Chen, Yi-Tzai; Guo, Liangran; Zhao, Mingyang; Wang, Xiaodong; Lu, Wei

    2015-07-15

    Copper sulfide nanoparticles, effective absorbers of near-infrared light, are recently attracting broad interest as a photothermal coupling agent for cancer therapy. Lipophilic copper sulfide nanoparticles are preferred for high performance biomedical applications due to high tissue affinity. Synthesis of lipophilic copper sulfide nanoparticles requires complicated multi-step processes under severe conditions. Here, we describe a new synthetic process, developed by direct dry-grinding of copper(II) acetylacetonate with sulfur under ambient environment at low temperature. The formed CuS nanoparticles are of uniform size, ~10 nm in diameter, and are monodispersed in chloroform. Each covellite CuS nanocrystal surface is modified with oleylamine through hydrogen bonding between sulfur atoms and amine groups of oleylamine. The nanoparticles demonstrate near-infrared light absorption for photothermal applications. The synthetic methodology described here is more convenient and less extreme than previous methods, and should thus greatly facilitate the preparation of photothermal lipophilic copper sulfide nanomaterials for cancer therapy.

  1. 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.

  2. 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)

  3. Modified polymeric materials for durability in the atomic oxygen space environment

    Science.gov (United States)

    Kiefer, R. L.; Anderson, R. A.; Kim, M.-H. Y.; Thibeault, S. A.

    2003-08-01

    Organometallic compounds have been incorporated into organic polymers to improve their durability to the environment of the low earth orbit (LEO), particularly their resistance to erosion by atomic oxygen (AO). Bis(triphenyltin) oxide (BTO) was added to a thermoplastic polyetherimide, Ultem, and exposed on the Mir space station. The addition of the BTO to Ultem significantly reduced the mass loss in LEO. Aluminum acetylacetonate was added to a thermoset, PMDA-ODA polyimide. that is currently deployed on the International Space Station. Two films are placed in the ram direction exposed to AO and space radiation. Three films are placed in the wake direction and are exposed to space radiation but not AO. The doped films show superior resistance to AO.

  4. 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.

  5. Sol-Gel Assembly and Luminescence of SiO2/PEMA Hybrid Material Incorporated with Terbium Complex

    Institute of Scientific and Technical Information of China (English)

    闫冰; 游佳勇

    2002-01-01

    Ethyl methacrylate (EMA) doped with luminescent ternary terbium complex (Tb(acac)3*dam) with acetylacetone (Hacac) and diantipylmethane (dam) was incorporated into the microporous silica gel. With the polymerization of EMA, the hybrid material containing Tb(acac)3*dam was obtained. The hybrid material exhibited good toughness and transparency and higher thermal stability than that of the pure complex and pure polymer matrix. In the range of doping concentration of Tb(acac)3*dam (0.05%, 0.1%, 0.2%, 0.5%, 1.0%, 2.0% and 5.0%), emission intensity increases with the increasing of corresponding doping concentration and concentration quenching effect has not taken place.

  6. CuIn(S,Se){sub 2}thin film solar cells from nanocrystal inks: Effect of nanocrystal precursors

    Energy Technology Data Exchange (ETDEWEB)

    Ford, Grayson M.; Guo Qijie [School of Chemical Engineering and The Energy Center, Purdue University, 480 Stadium Mall Dr., West Lafayette, IN 47907 (United States); Agrawal, Rakesh, E-mail: agrawalr@purdue.edu [School of Chemical Engineering and The Energy Center, Purdue University, 480 Stadium Mall Dr., West Lafayette, IN 47907 (United States); Hillhouse, Hugh W., E-mail: h2@uw.edu [School of Chemical Engineering and The Energy Center, Purdue University, 480 Stadium Mall Dr., West Lafayette, IN 47907 (United States); Department of Chemical Engineering, University of Washington, Seattle WA 98105 (United States)

    2011-10-31

    CuIn(S,Se){sub 2} thin film solar cells are fabricated by selenizing CuInS{sub 2} nanocrystals synthesized using a variety of copper and indium precursors. Specifically, copper and indium acetates, acetylacetonates, iodides, chlorides and nitrates are investigated to determine the effect of precursors on electronic properties and device performance. Nanocrystal synthesis with each of these precursors can be optimized to yield similar nanocrystal composition, size and structure. In addition, dense chalcopyrite CuIn(S,Se){sub 2} thin films with micron sized grains at the surface are formed upon selenization regardless of precursor type. Surprisingly, solar cells fabricated from each nanocrystal ink have roughly the same carrier concentrations of 10{sup 16} to 10{sup 17} cm{sup -3} in the absorber layer and achieve active area efficiencies of approximately 5%.

  7. Blistering during the atomic layer deposition of iridium

    Energy Technology Data Exchange (ETDEWEB)

    Genevée, Pascal, E-mail: pascal-genevee@chimie-paristech.fr, E-mail: a.szeghalmi@uni-jena.de; Ahiavi, Ernest; Janunts, Norik; Pertsch, Thomas; Kley, Ernst-Bernhard; Szeghalmi, Adriana, E-mail: pascal-genevee@chimie-paristech.fr, E-mail: a.szeghalmi@uni-jena.de [Institut für Angewandte Physik, Friedrich-Schiller-Universität Jena, Max-Wien-Platz 1, 07743 Jena (Germany); Oliva, Maria [Fraunhofer IOF, Albert-Einstein-Strasse 7, 07743 Jena (Germany)

    2016-01-15

    The authors report on the formation of blisters during the atomic layer deposition of iridium using iridium acetylacetonate and oxygen precursors. Films deposited on fused silica substrates led to sparsely distributed large blisters while in the case of silicon with native oxide additional small blisters with a high density was observed. It is found that the formation of blisters is favored by a higher deposition temperature and a larger layer thickness. Postdeposition annealing did not have a significant effect on the formation of blisters. Finally, changing purge duration during the film growth allowed us to avoid blistering and evidenced that impurities released from the film in gas phase were responsible for the formation of blisters.

  8. X-ray diffraction and vibrational spectroscopic study of trans-bis(acetylacetonato)-bis(4-methylpyridine)cobalt(III)

    Science.gov (United States)

    Tayyari, Sayyed Faramarz; Habibi, Mohammad Hossien; Shojaee, Elahe; Jamialahmadi, Mina; Sammelson, Robert Erik; Wada, Koki; Suzuki, Takayoshi

    2015-03-01

    Trans-bis(acetylacetonato)-bis(4-methylpyridine)cobalt(III)hexafluorophosphate, [AMPC]PF6, was synthesized and characterized by X-ray diffraction and vibrational spectroscopy. The title compound C22H28N2O4Co crystallizes with Z = 2 in space group P-1 (#2). The molecular structure and vibrational spectra of this compound were investigated by means of density functional theory (DFT) calculations and the results were compared with the experimental data. The measured IR bands were interpreted in terms of the calculated vibrational normal modes and compared with the tris(acetylacetonate)Co(III) (Co(acac)3) and 4-methylpyridine (4-Mepy) vibrational spectra. The scaled theoretical wavenumbers and the structural parameters were in excellent agreement with the experimental data.

  9. Theoretical study, and infrared and Raman spectra of copper(II) chelated complex with dibenzoylmethane

    DEFF Research Database (Denmark)

    Nekoei, A.-R.; Vakili, M.; Hakimi-Tabar, M.

    2014-01-01

    assignment for Cu(dbm)2 in the literatures. Density functional theory (DFT) at the B3LYP level and also MP2 calculations using different basis sets, besides Natural Bond Orbital (NBO) and Atoms-in-Molecules (AIM) analyses, have been employed to investigate the effect of methyl substitution with the phenyl......There are some discrepancies in both the vibrational assignments and in the metal-ligand (M-L) bond strengths predicted in the previous studies on the copper (II) chelated complex of dibenzoylmethane, Cu(dbm)2. Also, there is a lack of theoretical structure, Raman spectrum and full vibrational...... group on the stabilities of bis(acetylacetonate) copper (II), Cu(acac)2, and Cu(dbm)2 complexes and the electron delocalization in their chelated rings. Measured solid phase infrared and Raman bands for Cu(dbm)2 complex have been interpreted in terms of the calculated vibrational modes and detailed...

  10. Electronic structure of planar-quasicycled organic molecules with intramolecular hydrogen bond

    Directory of Open Access Journals (Sweden)

    ALEXEI N. PANKRATOV

    2007-03-01

    Full Text Available By means of the HF/6-311G(d,p method, the electronic structure of the series of organic molecules, among which are malonaldehyde, acetylacetone, thiomalonaldehyde,’the derivatives of aniline 2-XC6H4NH2, phenol 2-XC6H4OH, benzenethiol 2-XC6H4SH (X = CHO, COOH, COO-, NO, NO2, OH, OCH3, SH, SCH3, F, Cl, Br, 8-hydroxyquinoline, 8-mercaptoquinoline, tropolone, has been studied. The intramolecular hydrogen bond (IHB has been established to lead to a local electron redistribution in quasicycle, and primarily to the electron density transfer between the direct IHB participants – from the hydrogen atom toward the proton-aceptor atom. On forming the IHB of the S–H···O type, the electron density in general decreases on the sulphohydryl hydrogen atom and increases on the sulphur atom.

  11. Synthesis and structural characterization of novel flower-like titanium dioxide nanostructures

    Energy Technology Data Exchange (ETDEWEB)

    Castaneda, Luis [Departamento de Ingenieria Electrica, Centro de Investigacion y de Estudios Avanzados del Instituto Politecnico Nacional CINVESTAV-IPN, SEES, Apartado Postal 14740, Mexico, DF, 07000 (Mexico); Departamento de Fisica y Matematicas, Division de Ciencia, Arte y Tecnologia, Universidad Iberoamericana, Av. Prolongacion Paseo de la Reforma 880, Santa Fe 012100, DF (Mexico); Terrones, Mauricio [Departamento de Fisica y Matematicas, Division de Ciencia, Arte y Tecnologia, Universidad Iberoamericana, Av. Prolongacion Paseo de la Reforma 880, Santa Fe 012100, DF (Mexico) and Advanced Materials Department, IPICYT, Camino a la Presa San Jose 2055, Col. Lomas, 4a. seccion, San Luis Potosi, 78216 (Mexico)]. E-mail: mterrones@ipicyt.edu.mx

    2007-03-01

    Titanium dioxide (TiO{sub 2}-anatase phase) films, consisting of agglomerated flower-like nanoparticles, have been synthesized using an ultrasonic spray pyrolysis method in conjunction with titanium (IV) oxide acetylacetonate (TiO(acac){sub 2}) and methanol at 550 deg. C. These films were subsequently thermally treated in air, at 950 deg. C for 6 h, and the flower-like particles were transformed into smooth surfaces mainly formed by the TiO{sub 2} rutile phase. In this letter, we characterized these structures using scanning electron microscopy, atomic force micrcoscopy, and low-angle X-ray diffraction measurements. It is proposed that these novel flower-like nanostructures, exhibiting a large number of exposed edges, will be important in the development of efficient gas sensor devices.

  12. Atomic layer deposition of cobalt carbide films and their magnetic properties using propanol as a reducing agent

    Science.gov (United States)

    Sarr, Mouhamadou; Bahlawane, Naoufal; Arl, Didier; Dossot, Manuel; McRae, Edward; Lenoble, Damien

    2016-08-01

    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.

  13. Effect of stabilizer on optical and structural properties of MgO thin films prepared by sol–gel method

    Indian Academy of Sciences (India)

    Z Bazhan; F E Ghodsi; J Mazloom

    2013-10-01

    The effects of monoethanolamine (MEA) and acetylacetone (ACAC) addition as stabilizer on the crystallization behaviour, morphology and optical properties of magnesium oxide were investigated using thermogravimetry (TG/DTG), X-ray diffraction (XRD), scanning electron microscopy (SEM), UV-Visible, photoluminescence (PL) and Fourier transform infrared (FTIR) spectroscopy. Stabilizer addition reduces transparency of the films. MgO films prepared at 500 °C showed weak orientation of (200). However, the films prepared by addition of stabilizer are amorphous. MgO powders were prepared for exhibiting the structural properties. The patterns of MgO powders showed a preferred orientation of (200). The addition of stabilizer causes a reduction in grain size. SEM micrographs show that a homogenous and crack-free film can be prepared at 500 °C and addition of stabilizer causes an increase in packing density.

  14. Fabrication of copper oxide-coated hollow waveguides for CO2 laser radiation.

    Science.gov (United States)

    Matsuura, Y; Miura, D; Miyagi, M

    1999-03-20

    Hollow fibers for transmitting CO(2) laser light were fabricated by the chemical vapor deposition (CVD) method. A dielectric film of copper oxide (Cu(2)O) was deposited upon the inside of a Ag-coated glass capillary by use of a metal acetylacetonate as the precursor. The waveguide, which was coated with Cu(2)O and had a bore diameter of 700 microm, showed a loss of 0.9 dB/m for CO(2) laser light. The Cu(2)O film deposited by CVD had high chemical and heat resistivity. Therefore a hollow fiber coated with copper oxide is suitable for high-power laser applications in a severe environment.

  15. Solvothermal synthesis and characterization of acicular -Fe2O3 nanoparticles

    Indian Academy of Sciences (India)

    S Basavaraja; D S Balaji; Mahesh D Bedre; D Raghunandan; P M Prithviraj Swamy; A Venkataraman

    2011-12-01

    Nanometer-sized -Fe2O3 particles have been prepared by a simple solvothermal method using ferric acetylacetonate as a precursor. The products were characterized by X-ray diffraction (XRD), energy dispersive X-ray microanalysis (EDAX), X-ray photoelectron spectroscopy (XPS), scanning electron microscopy (SEM), transition electron microscopy (TEM), infrared spectroscopy (IR) and thermal analysis (TG–DTA). XRD indicates that the product is single-phase -Fe2O3 with rhombohedral structure. Bundles of acicular shaped nanoparticles are seen in TEM images with an aspect ratio ∼ 12; typically 8–12 nm wide and over 150 nm long. The -Fe2O3 nanoparticles posses a high thermal stability, as observed on thermal analysis traces.

  16. 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.

  17. Improved electrical, optical, and structural properties of undoped ZnO thin films grown by water-mist-assisted spray pyrolysis

    Science.gov (United States)

    Martínez Pérez, L.; Aguilar-Frutis, M.; Zelaya-Angel, O.; Muñoz Aguirre, N.

    2006-08-01

    Undoped ZnO thin films were prepared using the ultrasonic spray pyrolysis deposition technique with zinc acetylacetonate dissolved in N,N-dimethylformamide as the source materials solution. The addition of water mist in a parallel flux to the spray solution stream was also used during deposition of the films. The addition of water mist improved the electrical characteristics of the ZnO films. Fresh ZnO samples were then thermally annealed in a H2 reducing atmosphere. X-ray diffraction patterns show mainly the wurzite crystalline ZnO phase in the films. An electrical resistivity ( ) of around 2.7 × 10-2 cm was measured at room temperature for the best undoped ZnO film. is approximately one order of magnitude lower than the resistivities found in undoped ZnO films obtained by means of similar non-vacuum deposition techniques.

  18. TiO2 thin films prepared by sol - gel method

    Science.gov (United States)

    Suciu, R. C.; Indrea, E.; Silipas, T. D.; Dreve, S.; Rosu, M. C.; Popescu, V.; Popescu, G.; Nascu, H. I.

    2009-08-01

    There is a growing awareness that titania (TiO2) and TiO2-based oxide systems are the most promising candidates for the development of photoelectrodes for photoelectrochemical cell (PEC) for solar-hydrogen production [1]. The PEC is equipped with a single photoelectrode (photoanode) and cathode, both of which are immersed in an aqueous electrolyte. In this work we present a sol-gel method to prepare TiO2 thin films on ITO using tetraisopropoxides of titanium, acetylacetone, 1-butanol and Tween 80 as surfactant. The films were deposited on ITO coated glass slides by spray pyrolysis. UV-VIS spectra and fluorescence measurements were made for the solutions and films. X-ray diffraction was used for structural investigations and the morphology of the film was studied by Scanning Electron Microscopy.

  19. Preparation of Fe3O4Spherical Nanoporous Particles Facilitated by Polyethylene Glycol 4000

    Directory of Open Access Journals (Sweden)

    Wang Li-Li

    2009-01-01

    Full Text Available Abstract Much interest has been attracted to the magnetic materials with porous structure because of their unique properties and potential applications. In this report, Fe3O4nanoporous particles assembled from small Fe3O4nanoparticles have been prepared by thermal decomposition of iron acetylacetonate in the presence of polyethylene glycol 4000. The size of the spherical nanoporous particles is 100–200 nm. Surface area measurement shows that these Fe3O4nanoporous particles have a high surface area of 87.5 m2/g. Magnetization measurement and Mössbauer spectrum indicate that these particles are nearly superparamagnetic at room temperature. It is found that the morphology of the products is greatly influenced by polyethylene glycol concentration and the polymerization degree of polyethylene glycol. Polyethylene glycol molecules are believed to facilitate the formation of the spherical assembly.

  20. Preparation and characterization of poly(glycidyl methacrylate)-grafted magnetic nanoparticles: Effects of the precursor concentration on polyol synthesis of Fe3O4 and [PMDETA]0/[CuBr2]0 ratios on SI-AGET ATRP

    Science.gov (United States)

    Jiang, Liping; Zhou, Xuyang; Wei, Guyun; Lu, Xiaoduo; Wei, Weiping; Qiu, Jianhua

    2015-12-01

    Polymer brushes based on poly(glycidyl methacrylate) (PGMA) have been successfully grafted from the surface of silica coated iron oxide (Fe3O4@SiO2) nanoparticles via surface-initiated activators generated by electron transfer atom transfer radical polymerization (SI-AGET ATRP). The size of the nanoparticles could be adjusted from 7.3 to 9.6 nm by varying the precursor concentration of iron(III) acetylacetonate. The Fe3O4 nanoparticles possessed a highly crystalline structure, and the saturation magnetization of the as-prepared magnetite was strongly related to the particle size. Furthermore, the grafted PGMA content on the magnetic nanoparticles could be controlled by varying the ligand to transition metal ratio in a N,N,N‧,N″,N″-pentamethyldiethylenetriamine (PMDETA)/CuBr2 catalyst system. The maximum grafted content was 23.1% at a ratio of [PMDETA]0/[CuBr2]0 = 2:1.

  1. 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.

  2. Validated spectrofluorimetric method for determination of selected aminoglycosides

    Science.gov (United States)

    Omar, Mahmoud A.; Ahmed, Hytham M.; Hammad, Mohamed A.; Derayea, Sayed M.

    2015-01-01

    New, sensitive, and selective spectrofluorimetric method was developed for determination of three aminoglycoside drugs in different dosage forms, namely; neomycin sulfate (NEO), tobramycin (TOB) and kanamycin sulfate (KAN). The method is based on Hantzsch condensation reaction between the primary amino group of aminoglycosides with acetylacetone and formaldehyde in pH 2.7 yielding highly yellow fluorescent derivatives measured emission (471 nm) and excitation (410 nm) wavelengths. The fluorescence intensity was directly proportional to the concentration over the range 10-60, 40-100 and 5-50 ng/mL for NEO, TOB and KAN respectively. The proposed method was applied successfully for determination of these drugs in their pharmaceutical dosage forms.

  3. Synthesis and characterization of spherical calcia stabilized zirconia nano-powders obtained by spray pyrolysis

    Energy Technology Data Exchange (ETDEWEB)

    Esparza-Ponce, H.E.; Reyes-Rojas, A.; Antunez-Flores, W.; Miki-Yoshida, M

    2003-02-25

    Fine, spherical Ca{sub 0.15}Zr{sub 0.85}O{sub 1.85} nano-powders were prepared by spray pyrolysis, starting from a mixed aqueous and ethylic solution of zirconium acetylacetonate and calcium acetate. The influence of solution concentration, furnace temperature, mass flow of carrier gas and voltage of precipitator on microstructure, average particles size and recovery percentage were evaluated. The powders were synthesized without sintering, and for adequate preparation conditions, were mostly spherical, solid and narrowly size distributed. Average particle size ranges between 40 and 350 nm. Transmission electron micrographs showed that crystalline calcia stabilized zirconia particles were constituted by small crystallites, their size varying between 2 and 40 nm. X-ray diffraction analysis shows that powders obtained at low temperature were amorphous; for higher temperatures ({approx}800 deg. C), it is found the presence of the tetragonal and cubic phases.

  4. One-Pot Synthesis of Disperse Dyes Under Microwave Irradiation: Dyebath Reuse in Dyeing of Polyester Fabrics

    Directory of Open Access Journals (Sweden)

    Huda M. Mahmoud

    2012-04-01

    Full Text Available A series of 4-hydroxyphenylazopyrazolopyrimidine disperse dyes were prepared via one-pot reactions of p-hydroxyphenylhydrazone, hydrazine hydrate, and acetylacetone or enaminones using microwave irradiation as an energy source. Structural assignments of the dyes were confirmed by X-ray crystallographic structure determination. Instead of discharging the dyebath after each dyeing cycle, the residual dyebath was spectrophotometrically analyzed and then pH readjusted for a repeat dyeing with longer time. Fastness of the dyed samples was measured after each recycle. Most of the dyed fabrics tested displayed good light fastness and excellent fastness to washing and perspiration. Finally, the biological activity of the synthesized dyes against Gram positive bacteria, Gram negative bacteria and yeast were evaluated.

  5. One-pot synthesis of disperse dyes under microwave irradiation: dyebath reuse in dyeing of polyester fabrics.

    Science.gov (United States)

    Al-Etaibi, Alya M; El-Apasery, Morsy A; Mahmoud, Huda M; Al-Awadi, Nouria A

    2012-04-10

    A series of 4-hydroxyphenylazopyrazolopyrimidine disperse dyes were prepared via one-pot reactions of p-hydroxyphenylhydrazone, hydrazine hydrate, and acetylacetone or enaminones using microwave irradiation as an energy source. Structural assignments of the dyes were confirmed by X-ray crystallographic structure determination. Instead of discharging the dyebath after each dyeing cycle, the residual dyebath was spectrophotometrically analyzed and then pH readjusted for a repeat dyeing with longer time. Fastness of the dyed samples was measured after each recycle. Most of the dyed fabrics tested displayed good light fastness and excellent fastness to washing and perspiration. Finally, the biological activity of the synthesized dyes against Gram positive bacteria, Gram negative bacteria and yeast were evaluated.

  6. Synthesis and characterization of starch-poly(methyl acrylate) graft copolymers using horseradish peroxidase.

    Science.gov (United States)

    Wang, Su; Wang, Qiang; Fan, Xuerong; Xu, Jin; Zhang, Ying; Yuan, Jiugang; Jin, Heling; Cavaco-Paulo, Artur

    2016-01-20

    Horseradish peroxidase (HRP)-mediated graft polymerization in the presence of hydrogen peroxide (H2O2) and acetylacetone (Acac) has been successfully applied to the synthesis of starch-poly(methyl acrylate) (PMA). The graft copolymer was characterized by Fourier transform infrared (FT-IR), elemental analysis, nuclear magnetic resonance ((1)H NMR and (13)C NMR), and differential scanning calorimetry (DSC). FT-IR, elemental analysis and NMR confirmed that methyl acrylate (MA) was grafted onto starch successfully. DSC results showed the graft reaction had changed the crystalline regions of the gelatinized starch. The effects of pH, MA content, HRP dosage, incubation temperature and time on grafting percentage (GP) and grafting efficiency (GE) were also investigated. The GP and GE under optimal conditions reached 30.21% and 45.13%, respectively.

  7. Characterization of the porosity of thin zirconium oxide coatings prepared at low temperatures

    Energy Technology Data Exchange (ETDEWEB)

    Ugas-Carrion, R. [Technische Universitaet Darmstadt, Department of Materials Science, Darmstadt (Germany); Sittner, F. [Technische Universitaet Darmstadt, Department of Materials Science, Darmstadt (Germany)], E-mail: sittner@ca.tu-darmstadt.de; Ochs, C.J.; Flege, S.; Ensinger, W. [Technische Universitaet Darmstadt, Department of Materials Science, Darmstadt (Germany)

    2009-01-30

    In this work we investigated the possibilities to reduce the porosity of thin protective zirconium oxide films deposited with the sol-gel technique at low temperatures. Electrochemical investigations showed that the concentration of the stabilizing agent acetylacetone is a crucial parameter for the protection performance of the zirconium oxide films and that it is possible to run the deposition process at much lower temperatures with the optimum stabilizer concentration. This allows the application of the process to sensitive substrates that cannot be treated at high temperatures and reduces energy costs as well. Characterization of the film structure with secondary ion mass spectrometry revealed that the stabilizing agent is responsible for the formation of a mixed oxide layer at the interface of substrate and coating. The thickness of this layer can be tuned with the concentration of the stabilizing agent.

  8. (Acetylacetonato-κ2O,O′(phthalocyaninato-κ4N(phenanthroline-κ2N,N′erbium(III

    Directory of Open Access Journals (Sweden)

    Hong-Feng Li

    2012-03-01

    Full Text Available The title complex, [Er(C32H16N8(C5H7O2(C12H8N2], possesses a mirror plane and the asymmetric unit is half of the molecule. The ErIII cation, lying on the mirror plane, is eight-coordinated by two O atoms from acetylacetone, two N (Nphen atoms from 1,10-phenanthroline and four isoindole N (Niso atoms from the phthalocyanine ligand in an antiprismatic geometry. The Er—N distances are in the range 2.376 (5–2.529 (4 Å and the Er—O distance is 2.272 (3 Å. Notably, the Er—Niso bonds are shorter than the Er—Nphen bonds, but longer than the Er—O bonds.

  9. Controlled Synthesis and Characterization of Monodisperse Fe3O4 Nanoparticles

    Institute of Scientific and Technical Information of China (English)

    SHI,Rongrong; GAO,Guanhua; YI,Ran; ZHOU,Kechao; QIU,Guanzhou; LIU,Xiaohe

    2009-01-01

    Monodisperse Fe3O4 nanoparticles were successfully synthesized through the thermal decomposition of iron acetylacetonate in octadecene solvent in the presence of oleic acid and oleylamine.The influences of experimental parameters,such as reacting temperature,amounts and kinds of surfactants,solvents,oleic acid and oleylamine,on the size and shape of monodisperse Fe3O4 nanoparticles were discussed.The phase structures,morphology,and size of the as-prepared products were investigated in detail by X-ray diffraction (XRD),transmission electron microscopy (TEM),selected area electron diffraction (SAED) and high-resolution transmission electron microscopy (HRTEM).Magnetic property was measured using a vibrating sample magnetometer (VSM) at room temperature,which revealed that Fe3O4 nanoparticles were of ferromagnetism with a saturation magnetization (Ms) of 74.0 emu/g and coercivity (Hc) of 72.6 Oe.

  10. Electrochemical and Reaction Bonding Processing of Thick ZrO2/Al2O3 Composite Coatings

    Institute of Scientific and Technical Information of China (English)

    WANGZhou-cheng; XIAOPing

    2004-01-01

    A novel technique combining electrophoretic deposition (EPD) and reaction bonding process (RBP) is developed to fabricate thick ZrO2/Al2O3 composite coatings. Mixed organic solvents are used here to make suspension containing yttria stablised zirconia (YSZ) and aluminium (Al). The results show that densely packed green form coatings are deposited using a mixture of ethanol and acetylacetone as suspension medium and ball milling for 48 hours. On subsequent heat treatment, melting and oxidation of aluminium in the green forms promote densification during sintering. By these means,thick, uniform and crack-free ZrO2/Al2O3 composite coatings have been fabricated on metal substrate.

  11. Electrochemical and Reaction Bonding Processing of Thick ZrO2/Al2O3 Composite Coatings

    Institute of Scientific and Technical Information of China (English)

    WANG Zhou-cheng; XIAO Ping

    2004-01-01

    A novel technique combining electrophoretic deposition (EPD) and reaction bonding process (RBP) is developed to fabricate thick ZrO2/Al2O3 composite coatings. Mixed organic solvents are used here to make suspension containing yttria stablised zirconia (YSZ) and aluminium (Al). The results show that densely packed green form coatings are deposited using a mixture of ethanol and acetylacetone as suspension medium and ball milling for 48 hours. On subsequent heat treatment, melting and oxidation of aluminium in the green forms promote densification during sintering. By these means,thick, uniform and crack-free ZrO2/Al2O3 composite coatings have been fabricated on metal substrate.

  12. Ozone Sensing Based on Palladium Decorated Carbon Nanotubes

    Directory of Open Access Journals (Sweden)

    Selene Capula Colindres

    2014-04-01

    Full Text Available Multiwall carbon nanotubes (MWCNTs were easily and efficiently decorated with Pd nanoparticles through a vapor-phase impregnation-decomposition method starting from palladium acetylacetonates. The sensor device consisted on a film of sensitive material (MWCNTs-Pd deposited by drop coating on platinum interdigitated electrodes on a SiO2 substrate. The sensor exhibited a resistance change to ozone (O3 with a response time of 60 s at different temperatures and the capability of detecting concentrations up to 20 ppb. The sensor shows the best response when exposed to O3 at 120 °C. The device shows a very reproducible sensor performance, with high repeatability, full recovery and efficient response.

  13. 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)

  14. Preparation of ITO transparent conductive film by sol-gel method

    Institute of Scientific and Technical Information of China (English)

    LI Zhi-hua; REN Dong-yan

    2006-01-01

    The ITO transparent conductive films were prepared on substrate of quartz glass by sol-gel method. The raw materials were nitrate indium, acetylacetone and the dopant of anhydrous chloride (SnCl4). The process from gel to crystalline film and the microstructure of the films were investigated by DTA-TG, XRD and SEM. The influence of preparation processes on the electricity performance of the films was also studied by four-probe apparatus. The results show that the crystallization process of ITO xerogel completes when the heat treatment temperature reaches 600 ℃. The ITO films possesses on vesicular structures accumulated by spherical particles, and both heat treatment temperature and cooling rate have important effects on the resistivity ofITO films.

  15. Acoplamento de cloreto de 4-nitrofenildiazônio com nucleófilos alifáticos: experimento integrado de síntese orgânica e cristalografia de raios X

    Directory of Open Access Journals (Sweden)

    Silvio Cunha

    2013-01-01

    Full Text Available 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.

  16. POLYMERIZATION OF γ-STEARYL-α,L-GLUTAMATE N-CARBOXYANHYDRIDE USING RARE EARTH COORDINATION CATALYSTS

    Institute of Scientific and Technical Information of China (English)

    Xiao-ping Hu; Jian Wu; Zhi-kang Xu; Lin-xian Feng

    2000-01-01

    A rare earth coordination system was first investigated as a new type of catalyst for the ring-opening polymerization of α-amino acid N-carboxyanhydrides (NCAs). The results for the polymerization of γ-stearyl-α,L-glutamate (SLG) NCA using neodymium acetylacetonate (Nd(acac)3)- or neodymium tris(2-ethylhexylphosphonate) (Nd(P204)3)-triethylaluminum-water as catalysts were compared with those using conventional catalysts. It was found that the helical poly(γ-stearyl-L-glutamate) with high molecular weight as well as narrow molecular weight distribution can be obtained in the presence of Nd(acac)3/AlEt3-1/2H2O. The polymer obtained was characterized by IR and NMR spectroscopy.

  17. Synthesis and photophysical properties of yellow-emitting iridium complexes. Effect of the temperature on the character of triplet emission.

    Science.gov (United States)

    Ivanov, P; Stanimirov, S; Kaloyanova, S; Petkov, I

    2012-11-01

    The parent study includes synthesis end photophysical characterization of four new phosphorescent cyclometalated iridium (III) complexes. The cyclometaled ligands used here are 2-(4-chlorophenyl)benzo[d]thiazole, 2(4isopropylphenyl)benzo[d] thiazole, 2-(4-methoxyphenyl)benzo[d]thiazole, 4-(benzo[d]thiazol-2-yl)-N,N-dimethylaniline. The auxiliary ligand is acetylacetone (Hacac). The photometric analyses show temperature dependence on phosphorescent spectra and the nature of the emitting state of the synthesized complexes. Using fluorescent and absorption spectroscopy we suggest an explanation of the observed effect points out the transition from ligand centered (LC) to MLCT main character of the emitting state. The quantitative photometric analysis states high phosphorescent quantum yields of the complexes in solution.

  18. Quantum molecular dynamics and molecular interactions studied by NMR and INS Nuclear magnetic resonance; Proton tunnelling; Hydrogen bond

    CERN Document Server

    Jones, N

    2002-01-01

    The wavefunction of a particle extends into the classically forbidden barrier region of the potential energy surface. The consequence of this partial delocalisation is the phenomenon of quantum tunnelling, an effect which enables a particle to penetrate a potential barrier of magnitude greater than the energy of the particle. The tunnelling probability is an exponential function of the particle mass. The effect is therefore an important contribution to the behaviour of light atoms, in particular the proton. The hydrogen bond has long been appreciated to be an essential component of many biological and chemical systems, and the proton transfer reaction in the hydrogen bond is fundamental to many of these processes. The proton behaviour in the hydrogen bonds of benzoic acid, acetylacetone and calix-4-arene has been studied. A variety of techniques, both experimental and computational, were adopted for the study of the three hydrogen bonded systems. The complementary spectroscopic techniques of inelastic neutron...

  19. Synthesis and ceramization of polycarbosilane containing beryllium

    Institute of Scientific and Technical Information of China (English)

    黄小忠; 周珊; 程勇; 杜作娟; 段曦东; 王超英

    2014-01-01

    Polycarbosilane containing beryllium (BPCS) precursors was prepared by the reaction of polycarbosilane (PCS) with beryllium acetylacetone (Be (acac)2). The analysis of structures and components of BPCS demonstrates that their main structures are basically the same as PCS. Ceramization of BPCS precursors shows that BPCS precursors are organic below 600 °C and inorganic at 800 °C. At 1400 °C, BPCS precursors convert into silicon carbide ceramics. The ceramization of different beryllium content precursors were studied, which show that beryllium plays an important role in the inhibition of crystalline grain growth ofβ-SiC at high temperature and it can adjust the dielectric constant of silicon carbide ceramics.

  20. 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)

  1. One-step hydrothermal synthesis of highly water-soluble secondary structural Fe3O4 nanoparticles

    Science.gov (United States)

    Yang, Xiwen; Jiang, Wei; Liu, Li; Chen, Binghua; Wu, Shixi; Sun, Danping; Li, Fengsheng

    2012-07-01

    Magnetite nanoparticles (MNPs) were prepared using the ferric acetylacetonate as the sole iron source in a facile hydrothermal route, while poly(acrylic acid) (PAA) was chosen as the stabilizer via one-step functionalized MNPs for better hydrophilic properties. The orthogonal was used in the paper for the experimental parameters optimization, including the solvent, the reaction time, the amount of stabilizer and the presynthesis. The obtained highly water dispersible MNPs with uniform size from about 50 to about 100 nm was individually composed of many monodisperse magnetite crystallites approximately 6 nm in size. And the MNPs show high magnetic properties, whose magnetite content was up to 76.76% and the saturation magnetization was 39.0 emu/g. Later the formation mechanism of MNPs was also discussed. Thus the MNPs proved to be very promising for biomedical applications.

  2. Pt nanoparticles on titania nanotubes prepared by vapor-phase impregnation-decomposition method

    Energy Technology Data Exchange (ETDEWEB)

    Encarnacion Gomez, C. [National Polytechnic Institute, Dept. of Metallurgical Eng., Mexico 07300 DF, AP 75-874 (Mexico); Vargas Garcia, J.R., E-mail: rvargasga@ipn.m [National Polytechnic Institute, Dept. of Metallurgical Eng., Mexico 07300 DF, AP 75-874 (Mexico); Toledo Antonio, J.A.; Cortes Jacome, M.A.; Angeles Chavez, C. [Petroleum Mexican Institute, Eje Central Lazaro Cardenas No. 152, Mexico 07730 DF (Mexico)

    2010-04-16

    Platinum (Pt) nanoparticles were prepared on titania nanotubes (TNTs) by vapor-phase impregnation-decomposition method using platinum acetylacetonate as precursor. TNTs and Pt precursor were mixed in 3:1 weight ratio before vapor-phase impregnation. The mixed powders were heated at 453 K for 10 min to evaporate the precursor in a horizontal tube quartz reactor at a total pressure of 66.6 kPa. Then, the impregnated TNTs were moved to a higher temperature zone (673 K) inside the tube reactor to achieve the precursor decomposition. HAADF-STEM observations, AAS and XPS results revealed that this method allows the formation of uniformly distributed Pt nanoparticles on the surface of TNTs with a narrow distribution of particle size (2.1 nm mean size). Pt nanoparticles remain mainly as Pt{sup 0} oxidation state with a Pt{sup 0}/Pt{sup 2+} atomic ratio of 3.9.

  3. Complexing properties of {alpha}-iso-saccharinate: thorium

    Energy Technology Data Exchange (ETDEWEB)

    Allard, S.; Ekberg, C. [Nuclear Chemistry - Department of Chemical and Biological Engineering, Chalmers University of Technology, SE-412 96 Goeteborg (Sweden)

    2005-07-01

    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 {sup 234}Th-{alpha}-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{sub 4} aqueous phase kept at pH 8 in a thermostated AKUFVE unit. Since the {alpha}-iso-saccharinic system consists of three species - the carboxylic {alpha}-iso-saccharinic acid, {alpha}-iso-saccharinate and {alpha}-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 {alpha}-iso-saccharinate form while at the same time being an excellent pH for the {sup 234}Th-acetylacetone complexation with very limited hydrolysis effect. The {alpha}- 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 {sup 234}Th and {sup 234}Pa had been reached. Two complexation constants were used to fit a distribution equation to the experimental data. (authors)

  4. Pure magnetic hard fct FePt nanoparticles: Chemical synthesis, structural and magnetic properties correlations

    Energy Technology Data Exchange (ETDEWEB)

    Suber, L., E-mail: lorenza.suber@ism.cnr.it [ISM-CNR, Area della Ricerca di Roma 1, Via Salaria km 29.300, 00015 Monterotondo Scalo, RM (Italy); Marchegiani, G. [ISM-CNR, Area della Ricerca di Roma 1, Via Salaria km 29.300, 00015 Monterotondo Scalo, RM (Italy); Olivetti, E.S.; Celegato, F.; Coïsson, M.; Tiberto, P. [INRIM, Electromagnetism Division, Strada delle Cacce 91, 10135 Torino (Italy); Allia, P. [DISAT Politecnico di Torino, Corso Duca degli Abruzzi 24, 10129 Torino (Italy); Barrera, G. [Dipartimento di Chimica, Università di Torino, Via Pietro Giuria 7, 10125 Torino (Italy); Pilloni, L. [UTTMAT-CHI, Via Anguillarese 10, 00123 S. Maria di Galeria, Roma (Italy); Barba, L. [IC-CNR, Area Science Park, SS 14 Km 163.5 Basovizza, 34149 Trieste (Italy); Padella, F. [UTTMAT-CHI, Via Anguillarese 10, 00123 S. Maria di Galeria, Roma (Italy); Cossari, P. [IGAG-CNR, Area della Ricerca di Roma 1, Via Salaria km 29.300, 00015 Monterotondo Scalo, RM (Italy); Chiolerio, A. [Istituto Italiano di Tecnologia, Center for Space Human Robotics, Corso Trento 21, 10129 Torino (Italy)

    2014-03-01

    FePt nanoparticles, containing a near-equal atomic percentage of Fe and Pt, with a face centered tetragonal structure (fct), are challenging for potential applications in high performance permanent magnets and high density data storage. In this study, we report on the chemical synthesis, carried out both solvothermally and hydrothermally in autoclave reacting iron (III) acetylacetonate and platinum (II) acetylacetonate with tri- or tetra-ethylene glycol, these employed as solvents, reducers and particle surface protecting agents as well. In both methods, a subsequent thermal treatment at high temperatures is necessary to transform the magnetic soft face centered cubic (fcc) phase to the hard fct one. Organic low-weight molecules, generally used to protect the nanoparticle surface and avoid particle aggregation, are decomposed by the thermal treatment resulting in particle aggregation and coalescence phenomena; on the contrary, in this case, a polymer matrix is formed as particle protecting agent and, by thermally treating the hydrothermally prepared nanoparticles up to 750 °C for 1 h, the pure magnetic hard fct phase is obtained while preserving the nanostructure. A detailed study is carried out on FePt nanoparticle structure (fcc and fct phases) and correlated to the magnetic properties of the system. - Highlights: • fct FePt nanoparticles for hard magnetic nanotechnology applications. • Influence of synthesis parameters on the precursor fcc FePt nanoparticle structure. • Easy hydrothermal method for preparing pure fct FePt nanoparticles. • Monitoring the role of temperature and time on the FePt fcc–fct phase transformation. • Correlation between FePt nanoparticle structural and magnetic properties.

  5. 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.

  6. Highly efficient orange and red organic light-emitting diodes with iridium(III) complexes bearing benzothiazole cyclometallate ligands as emitters

    Energy Technology Data Exchange (ETDEWEB)

    Li, Ming [College of Chemistry, Sichuan University, Chengdu, 610064 (China); 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); Dai, Jun [College of Chemistry, Sichuan University, Chengdu, 610064 (China); Lu, Zhi-yun, E-mail: luzhiyun@scu.edu.cn [College of Chemistry, Sichuan University, Chengdu, 610064 (China); Huang, Yan [College of Chemistry, Sichuan University, Chengdu, 610064 (China); Yu, Jun-sheng, 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); Luo, Shuai [College of Chemistry, Sichuan University, Chengdu, 610064 (China); Su, Shi-jian, E-mail: mssjsu@scut.edu.cn [State Key Laboratory of Luminescent Materials and Devices and Institute of Polymer Optoelectronic Materials and Devices, South China University of Technology, Guangzhou, 510640 (China)

    2012-12-30

    Two iridium complexes bearing benzothiazole cyclometallate ligands, bis[2-(3 Prime ,5 Prime -di-tert-butylbiphenyl-4-yl)benzothiazolato-N,C{sup 2 Prime }]iridium(III) (acetylacetonate) [(tbpbt){sub 2}Ir(acac)] and bis[2-(9,9-dimethyl-9H-fluoren-2-yl)benzothiazolato-N,C{sup 2 Prime }]iridium(III) (acetylacetonate) [(fbt){sub 2}Ir(acac)], have been evaluated as orange and red electrophosphorescent materials. Both X-ray crystallographic analysis and photophysical results indicate that they possess alleviated self-quenching characteristics due to the existence of steric bulky ligands. As a result, phosphorescent organic light-emitting diodes (PhOLEDs) based on them show high performance even in heavily-doped level ({>=} 15 wt.%). The (tbpbt){sub 2}Ir(acac)-based PhOLED gives efficient orange emission with peak current efficiency of 26.9 cd/A (1280 cd/m{sup 2}) at doping ratio of 15 wt.%, while the 15 wt.% (fbt){sub 2}Ir(acac)-doped device emits efficient red light with Commission Internationale de l'Eclairage coordinates of (0.63, 0.36), and peak current and external quantum efficiency of 28.5 cd/A (1210 cd/m{sup 2}) and 15.6%, respectively. Moreover, all these heavily-doped PhOLEDs exhibit low efficiency roll-off at relatively high current density. - Highlights: Black-Right-Pointing-Pointer Two iridium complexes with bulky ligands are developed as orange/red emitter. Black-Right-Pointing-Pointer Organic light-emitting diodes using these phosphors show low efficiency roll-off. Black-Right-Pointing-Pointer High performance devices could be achieved under high doping ratio of {>=} 15 wt.%. Black-Right-Pointing-Pointer The high device efficiencies arise from the reduced self-quenching of the phosphors.

  7. 基于量子点的正方块状二氧化钛纳米晶的形成分析%Synthesis of titania nanosquare via recrystalization of titanium monoxide nanodots

    Institute of Scientific and Technical Information of China (English)

    丁晓坤

    2012-01-01

    二氧化钛是目前为止较理想的半导体光电材料,多用于光催化及太阳能电池.本文利用水热法合成正方块状锐钛矿结构的纳米二氧化钛单晶颗粒,并利用TEM表征其形成过程.这些纳米颗粒平均尺度为50 nm,暴露出较高比例的(001)高能面.通过实验进一步发现该纳米晶的形成源于液相中均匀分布的一氧化钛量子点,其形成是一个聚集-相变-重结晶的过程,最终在氟离子作用下形成正方块状单晶二氧化钛纳米颗粒.%This paper reported a new synthesis route of anatase nanosquare TiO2 single crystal with exposed (001) facet. The nanocrystals were prepared by solid Titanium Oxy Acetylacetoneate dispersed in mixed solvent of acetylacetone and ethanol, followed by a hydrothermal treatment in NH4F solution with PVP added. After heated at 160℃ in different days, it was found that the nanosquares formed from titanium monoxide nanodots in a process of aggregation, phase transform and recrystallization. The final nanosquare TiO2 was formed under the action of fluorin ions with the size of 30 -50 nm and exposed (001) facet.

  8. 含Zn2+的金属有机骨架材料对碳酸二苯酯与1,4-丁二醇酯交换反应的催化性能%Transesterification Between Diphenyl Carbonate and 1,4-Butanediol Catalyzed by Metal-Organic Framework Based on Zn2 +

    Institute of Scientific and Technical Information of China (English)

    王丽苹; 王公应; 汪帆; 刘品华; 徐晓林; 贺池先

    2013-01-01

    采用溶剂热法制备了Zn2+和对苯二甲酸组合形成的金属有机骨架材料(MOF),并用X射线衍射(XRD)和红外光谱(FT-IR)对其进行了表征.研究了MOF对碳酸二苯酯(DPC)与1,4-丁二醇(1,4-BD)酯交换反应合成聚碳酸酯二醇(PCDL)的催化活性,并与乙酰丙酮氧钛(TiO(acac)2)、乙酰丙酮锌(Zn(acac)2)和锌铝类水滑石(Zn-Al-CO3 LDH)等催化剂进行了比较.结果显示,MOF是该酯交换反应的良好催化剂.在优化的反应条件下,获得了数均分子量为3470,羟基值为35.2mg KOH/g的PCDL.%Metal-organic framework (MOF) based on Zn2+ and terephthalic acid was prepared and characterized with X-ray diffraction (XRD) and Fourier transform infrared spectroscopy (FT-IR). The catalytic activity of MOF for the transesterification between diphenyl carbonate (DPC) and 1,4-butanediol (1,4-BD) to polycarbonate diol (PCDL) was investigated, and was compared with that of catalysts such as titaniumoxide acetylacetonate (TiO(acac)2), zinc acetylacetonate (Zn(acac)2) and Zn-Al-CO3 layered double hydroxides (Zn-Al-CO3 LDH). The results show that MOF is an efficient catalyst for the transesterification. Under optimal reaction conditions, PCDL with number average molecular weight (-Mn) of 3470 and hydroxyl value of 35.2 mg KOH/g was synthesized.

  9. 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)

  10. Zirconium doped TiO2 thin films deposited by chemical spray pyrolysis

    Science.gov (United States)

    Juma, A.; Oja Acik, I.; Oluwabi, A. T.; Mere, A.; Mikli, V.; Danilson, M.; Krunks, M.

    2016-11-01

    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 TiO2 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 TiO2 thin films were uniform and homogeneous showing much smaller grains than the undoped TiO2 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 TiO2 film from 5.9 to 1.1 nm. An XRD study of samples with the highest Zr amount showed the ZrTiO4 phase started forming after annealing at 800 °C. The optical band gap for TiO2 decreased from 3.3 eV to 3.0 eV after annealing at 800 °C but for the TiO2: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.

  11. 高黏度指数聚α-烯烃合成润滑油的制备方法%A synthesis method of poly-alpha-olefins with high viscosity index

    Institute of Scientific and Technical Information of China (English)

    杨晓明; 丁洪生; 王丽

    2012-01-01

    以AlCl3 -乙酰丙酮络合物为催化剂,1-辛烯为原料齐聚合成了聚α-烯烃合成润滑油.考察了AlCl3物质的量分数、n(AlCl3)∶n(乙酰丙酮)、反应温度及反应时间对聚α-烯烃合成润滑油收率和性能的影响.结果表明,最佳工艺条件为AlCl3物质的量分数4%,n(AlCl3)∶n(乙酰丙酮)=2∶1,反应温度25℃,反应时间4h,此条件下,可以合成黏度指数为173和凝点- 40℃的聚α-烯烃合成润滑油.%Poly-alpha-olefins synthetic lubricant (PAO) was synthesized with aluminium chloride-acety-lacetone complex as the catalyst, and 1-octene as the raw material. The influence of mole fractions of AlCl3, molar ratio of AlCl3 to acetylacetone, reaction temperature and reaction time on the yield and properties of the PAO was investigated. The results showed that PAO with viscosity index of 173 and condensation point of - 40 t was synthesized under the optimum process condition as follows: AlCl3 mole fraction 4% ,n( AlCl3): n( acetylacetone) =2: 1,reaction temperature 25? and reaction time 4 h.

  12. Chemical modification of titanium isopropoxide for producing stable dispersion of titania nano-particles

    Energy Technology Data Exchange (ETDEWEB)

    Mahata, S. [National Institute of Science and Technology, Berhampur, Orissa (India); Mondal, B., E-mail: bnmondal@rediffmail.com [Centre for Advanced Materials Processing, Central Mechanical Engineering Research Institute, Durgapur 713 209 (India); Mahata, S.S. [National Institute of Science and Technology, Berhampur, Orissa (India); Usha, K. [Bengal College of Engineering and Technology, Durgapur (India); Mandal, N.; Mukherjee, K. [Centre for Advanced Materials Processing, Central Mechanical Engineering Research Institute, Durgapur 713 209 (India)

    2015-02-01

    Stable colloidal TiO{sub 2} nano-particles are synthesized through the controlled hydrolysis of chemically modified titanium (Ti) isopropoxide with acetylacetone and acetic acid whereas ammonium salts of poly(acrylic acid) is used as a dispersing agent. Acetylacetone and acetic acid used as chelating ligand to retard the hydrolysis and condensation rates. The process is found promising for producing homogeneous aqueous phase colloidal dispersion of TiO{sub 2} particles. Fourier transformed infrared and nuclear magnetic resonance spectra reveal the formation of monodentate bridging of ligands with Ti-isopropoxide. UV–Vis spectroscopy confirms the effective adsorption of poly(acrylic acid) within the modified Ti precursor. Zeta potential of modified titanium isopropoxide precursor is measured to understand its stability in different pH. The thermal stability of the precursors modified with different chelating ligands and dispersing agent has been studied using thermo-gravimetric in conjunction to differential thermal analysis (TG-DTA). Phase formation behavior and the morphological features of the synthesized particles are studied using X-ray diffraction and electron microscopy techniques. The sizes of the anatase phase particles are found in the range of 12–20 nm. - Highlights: • Nanosized colloidal TiO{sub 2} is prepared by controlled hydrolysis of Ti-isopropoxide. • Effect of chelating and dispersing agent on stability of colloidal TiO{sub 2} is studied. • Phase, morphology and stability of colloidal TiO{sub 2} are investigated. • The sizes of synthesized TiO{sub 2} particles are found in the range of 12–20 nm. • Suitable chelating and dispersing agent can improve particle loading in sol.

  13. 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.

  14. 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.

  15. Synthesis of PEO-PPO-PEO coated multi-functional CoFeAu nanoparticles by polyol process%Polyol法制备 PEO-PPO-PEO包裹的多功能CoFeAu纳米粒子

    Institute of Scientific and Technical Information of China (English)

    邵红琴; 张晓燕; 侯澎; 吴君华; 刘红玲

    2013-01-01

      采用Polyol合成法,以三嵌段共聚物PEO-PPO-PEO为表面活性剂,以1,2-十六烷二醇为还原剂,乙酰丙酮钴(Ⅱ)、乙酰丙酮铁(Ⅱ)和醋酸金为前驱体,成功合成了CoFeAu纳米粒子.傅立叶变换红外光谱(FT-IR)分析证实了共聚物PEO-PPO-PEO包裹在CoFeAu纳米颗粒表面,X射线衍射仪(XRD)测试得出该纳米粒子是面心立方晶体结构、晶格参数为0.406 nm、结晶性能好.紫外可见近红外分光光度计吸收光谱仪和振动样品磁强计(VSM )测试证明了该纳米粒子兼具良好的光学和磁学特性.该多功能CoFeAu纳米粒子有望在催化材料、磁材料、光电和生物医药等方面发挥有益作用.%CoFeAu nanoparticles were successfully synthesized by polyol process with the use of poly(ethylene oxide)-poly(propylene oxide)-poly(ethylene oxide) (PEO-PPO-PEO) as the sur-factant ,C14 H29CH(OH)CH2OH as the reducing agent ,cobalt acetylacetonate ,iron acetylacet-onate and gold acetate as precursors .The FT-IR study confirmed the PEO-PPO-PEO molecules on the surface of the CoFeAu nanoparticles .The X-ray diffraction identified the crystallograph-ic parameter 0 .406 nm of the face-centered cubic structure and showed the nanoparticles have good crystallinity .Whereas a UV-Vis near IR spectrophotometer and a vibrating sample mag-netometer were respectively applied to prove the good optical and magnetic properties of the CoFeAu nanoparticles .Such multi-functional CoFeAu nanoparticles show promising applica-tions in the catalytic ,magnetic ,photoelectric and biomedical fields .

  16. 多功能NiFeAu纳米粒子的合成与表征%Synthesis and characterization of multi-functional NiFeAu nanoparticles

    Institute of Scientific and Technical Information of China (English)

    张晓燕; 金邻豫; 侯澎; 吴君华; 李敏; 刘红玲

    2012-01-01

    采用一罐纳米乳液法,以聚乙二醇聚丙二醇聚乙二醇(PEOPPO-PEO)三嵌段共聚物为表面活性剂,通过还原前驱体乙酰丙酮镍、乙酰丙酮铁(Ⅱ)和醋酸金,成功制备了NiFeAu纳米粒子.采用透射电镜和X射线衍射仪分析了NiFeAu纳米粒子的形貌和结构;采用傅立叶变换红外光谱仪分析了三嵌段共聚物在NiFeAu纳米颗粒表面的覆盖情况;采用紫外-可见吸收光谱仪和振动样品磁强计测试了纳米粒子的光学和磁学特性.结果表明,三嵌段共聚物成功地结合于NiFeAu纳米颗粒表面;所制备的纳米粒子粒径分布较窄、结晶性能良好,并兼具光学和磁学特性.%NiFeAu nanoparticles were successfully synthesized via a one-pot nanoemulsion route involving simultaneous reduction of precursors nickel acetylacetonate, iron( II ) acetylacetonate and gold acetate in the presence of poly(ethylene glycol)-poly(propylene glycol)-poly(ethylene glycol) triblock copolymer (denoted as PEOPPOPEO) as the surfactant. The morphology and structure of as-prepared nanoparticles were analyzed by transmission electron microscopy and X-ray diffraction. The coverage of the triblock copolymer on the surface of as-prepared nanoparticles was examined by Fourier transform infrared spectrometry; and the optical and magnetic properties of the nanoparticles were investigated using an ultraviolet-visible light ab-sorbance spectrometer and a vibrating sample magnetometer, respectively. Results indicate that PEO-PPOPEO triblock copolymer is successfully combined onto the surface of the inorganic nanoparticles. As-prepared NiFeAu nanoparticles have a narrow size distribution and good crystallinity; and they possess optical and magnetic properties as well, showing promising applications as multi-functional materials in the fields of optical and biomedical engineering.

  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. Synthesis of magnetic cobalt ferrite nanoparticles with controlled morphology, monodispersity and composition: the influence of solvent, surfactant, reductant and synthetic conditions

    Science.gov (United States)

    Lu, Le T.; Dung, Ngo T.; Tung, Le D.; Thanh, Cao T.; Quy, Ong K.; Chuc, Nguyen V.; Maenosono, Shinya; Thanh, Nguyen T. K.

    2015-11-01

    In our present work, magnetic cobalt ferrite (CoFe2O4) nanoparticles have been successfully synthesised by thermal decomposition of Fe(iii) and Co(ii) acetylacetonate compounds in organic solvents in the presence of oleic acid (OA)/ oleylamine (OLA) as surfactants and 1,2-hexadecanediol (HDD) or octadecanol (OCD-ol) as an accelerating agent. As a result, CoFe2O4 nanoparticles of different shapes were tightly controlled in size (range of 4-30 nm) and monodispersity (standard deviation only at ca. 5%). Experimental parameters, such as reaction time, temperature, surfactant concentration, solvent, precursor ratio, and accelerating agent, in particular, the role of HDD, OCD-ol, and OA/OLA have been intensively investigated in detail to discover the best conditions for the synthesis of the above magnetic nanoparticles. The obtained nanoparticles have been successfully applied for producing oriented carbon nanotubes (CNTs), and they have potential to be used in biomedical applications.In our present work, magnetic cobalt ferrite (CoFe2O4) nanoparticles have been successfully synthesised by thermal decomposition of Fe(iii) and Co(ii) acetylacetonate compounds in organic solvents in the presence of oleic acid (OA)/ oleylamine (OLA) as surfactants and 1,2-hexadecanediol (HDD) or octadecanol (OCD-ol) as an accelerating agent. As a result, CoFe2O4 nanoparticles of different shapes were tightly controlled in size (range of 4-30 nm) and monodispersity (standard deviation only at ca. 5%). Experimental parameters, such as reaction time, temperature, surfactant concentration, solvent, precursor ratio, and accelerating agent, in particular, the role of HDD, OCD-ol, and OA/OLA have been intensively investigated in detail to discover the best conditions for the synthesis of the above magnetic nanoparticles. The obtained nanoparticles have been successfully applied for producing oriented carbon nanotubes (CNTs), and they have potential to be used in biomedical applications. Electronic

  19. High energy sodium based room temperature flow batteries

    Science.gov (United States)

    Shamie, Jack

    As novel energy sources such as solar, wind and tidal energies are explored it becomes necessary to build energy storage facilities to load level the intermittent nature of these energy sources. Energy storage is achieved by converting electrical energy into another form of energy. Batteries have many properties that are attractive for energy storage including high energy and power. Among many different types of batteries, redox flow batteries (RFBs) offer many advantages. Unlike conventional batteries, RFBs store energy in a liquid medium rather than solid active materials. This method of storage allows for the separation of energy and power unlike conventional batteries. Additionally flow batteries may have long lifetimes because there is no expansion or contraction of electrodes. A major disadvantage of RFB's is its lower energy density when compared to traditional batteries. In this Thesis, a novel hybrid Na-based redox flow battery (HNFB) is explored, which utilizes a room temperature molten sodium based anode, a sodium ion conducting solid electrolyte and liquid catholytes. The sodium electrode leads to high voltages and energy and allows for the possibility of multi-electron transfer per molecule. Vanadium acetylacetonate (acac) and TEMPO have been investigated for their use as catholytes. In the vanadium system, 2 electrons transfers per vanadium atom were found leading to a doubling of capacity. In addition, degradation of the charged state was found to be reversible within the voltage range of the cell. Contamination by water leads to the formation of vanadyl acetylacetonate. Although it is believed that vanadyl complex need to be taken to low voltages to be reduced back to vanadium acac, a new mechanism is shown that begins at higher voltages (2.1V). Vanadyl complexes react with excess ligand and protons to reform the vanadium complex. During this reaction, water is reformed leading to the continuous cycle in which vanadyl is formed and then reduced back

  20. Fabrication and kinetics study of nano-Al/NiO thermite film by electrophoretic deposition.

    Science.gov (United States)

    Zhang, Daixiong; Li, Xueming

    2015-05-21

    Nano-Al/NiO thermites were successfully prepared as film by electrophoretic deposition (EPD). For the key issue of this EPD, a mixture solvent of ethanol-acetylacetone (1:1 in volume) containing 0.00025 M nitric acid was proved to be a suitable dispersion system for EPD. The kinetics of electrophoretic deposition for both nano-Al and nano-NiO were investigated; the linear relation between deposition weight and deposition time in short time and parabolic relation in prolonged time were observed in both EPDs. The critical transition time between linear deposition kinetics and parabolic deposition kinetics for nano-Al and nano-NiO were 20 and 10 min, respectively. The theoretical calculation of the kinetics of electrophoretic deposition revealed that the equivalence ratio of nano-Al/NiO thermites film would be affected by the behavior of electrophoretic deposition for nano-Al and nano-NiO. The equivalence ratio remained steady when the linear deposition kinetics dominated for both nano-Al and nano-NiO. The equivalence ratio would change with deposition time when deposition kinetics for nano-NiO changed into parabolic kinetics dominated after 10 min. Therefore, the rule was suggested to be suitable for other EPD of bicomposites. We also studied thermodynamic properties of electrophoretic nano-Al/NiO thermites film as well as combustion performance.

  1. 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.

  2. Electrophoretic deposition on non-conducting substrates: The case of YSZ film on NiO-YSZ composite substrates for solid oxide fuel cell application

    Energy Technology Data Exchange (ETDEWEB)

    Besra, Laxmidhar [Colloids and Materials Chemistry Department, Regional Research Laboratory (CSIR), Bhubaneswar 751013, Orissa (India); Compson, Charles; Liu, Meilin [School of Materials Science and Engineering, Georgia Institute of Technology, 771 Ferst Drive, Atlanta, GA 30332-0245 (United States)

    2007-11-08

    This paper report the results of our investigation on electrophoretic deposition (EPD) of YSZ particles from its suspension in acetylacetone onto a non-conducting NiO-YSZ substrate. In principle, it is not possible to carry out electrophoretic deposition on non-conducting substrates. In this case, the EPD of YSZ particles on a NiO-YSZ substrate was made possible through the use of an adequately porous substrate. The continuous pores in the substrates, when saturated with the solvent, helped in establishing a ''conductive path'' between the electrode and the particles in suspension. Deposition rate was found to increase with increasing substrate porosity up to a certain value. The higher the applied voltage, the faster the deposition. For a given applied voltage, there exists a threshold porosity value below which EPD becomes practically impossible. An SOFC constructed on bi-layers of NiO-YSZ/YSZ with YSZ layer thickness of 40 {mu}m exhibited an open circuit voltage (OCV) of 0.97 V at 650 C and peak power density of 263.8 mW cm{sup -2} at 850 C when tested with H{sub 2} as fuel and ambient air as oxidant. (author)

  3. Electrophoretic deposition of Y{sub 2}O{sub 3}-stabilized ZrO{sub 2} electrolyte films in solid oxide fuel cells

    Energy Technology Data Exchange (ETDEWEB)

    Ishihara, Tatsumi; Sato, Keiji; Takita, Yusaku [Oita Univ. (Japan). Dept. of Applied Chemistry

    1996-04-01

    An electrophoretic deposition (EPD) method was applied for the preparation of yttria-stabilized zirconia (YSZ) films for solid oxide fuel cell (SOFC) applications. Dense YSZ films with uniform thickness can be readily prepared with the EPD method by using acetylacetone or acetone as a solvent. The open-circuit voltages of SOFC, for which the YSZ films were prepared by the EPD method, increased with increasing repetitions of deposition and sintering. It was found that the open-circuit voltage exceeded 1.0 V after five repetitions. When the planar SOFC was fabricated using La{sub 0.6}Sr{sub 0.4}MnO{sub 3} as a cathode, and electroless plating Pt as an anode, the open-circuit voltage and the maximum power density attained were 1.03 V and 1.84 W{center_dot}cm{sup {minus}2}, respectively. Consequently, it became evident that the electrophoretic deposition was a suitable processing route for the formation of gas-tight YSZ films with thickness less than 10 {micro}m.

  4. Electrophoretic deposition on non-conducting substrates: The case of YSZ film on NiO-YSZ composite substrates for solid oxide fuel cell application

    Science.gov (United States)

    Besra, Laxmidhar; Compson, Charles; Liu, Meilin

    This paper report the results of our investigation on electrophoretic deposition (EPD) of YSZ particles from its suspension in acetylacetone onto a non-conducting NiO-YSZ substrate. In principle, it is not possible to carry out electrophoretic deposition on non-conducting substrates. In this case, the EPD of YSZ particles on a NiO-YSZ substrate was made possible through the use of an adequately porous substrate. The continuous pores in the substrates, when saturated with the solvent, helped in establishing a "conductive path" between the electrode and the particles in suspension. Deposition rate was found to increase with increasing substrate porosity up to a certain value. The higher the applied voltage, the faster the deposition. For a given applied voltage, there exists a threshold porosity value below which EPD becomes practically impossible. An SOFC constructed on bi-layers of NiO-YSZ/YSZ with YSZ layer thickness of 40 μm exhibited an open circuit voltage (OCV) of 0.97 V at 650 °C and peak power density of 263.8 mW cm -2 at 850 °C when tested with H 2 as fuel and ambient air as oxidant.

  5. 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.

  6. Nonaqueous magnetic nanoparticle suspensions with controlled particle size and nuclear magnetic resonance properties.

    Science.gov (United States)

    Meledandri, Carla J; Stolarczyk, Jacek K; Ghosh, Swapankumar; Brougham, Dermot F

    2008-12-16

    We report the preparation of monodisperse maghemite (gamma-Fe2O3) nanoparticle suspensions in heptane, by thermal decomposition of iron(III) acetylacetonate in the presence of oleic acid and oleylamine surfactants. By varying the surfactant/Fe precursor mole ratio during synthesis, control was exerted both over the nanocrystal core size, in the range from 3 to 6 nm, and over the magnetic properties of the resulting nanoparticle dispersions. We report field-cycling 1H NMR relaxation analysis of the superparamagnetic relaxation rate enhancement of nonaqueous suspensions for the first time. This approach permits measurement of the relaxivity and provides information on the saturation magnetization and magnetic anisotropy energy of the suspended particles. The saturation magnetization was found to be in the expected range for maghemite particles of this size. The anisotropy energy was found to increase significantly with decreasing particle size, which we attribute to increased shape anisotropy. This study can be used as a guide for the synthesis of maghemite nanoparticles with selected magnetic properties for a given application.

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

    Science.gov (United States)

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

    2016-06-01

    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 Å), and low electrical resistivity (4.2 × 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 × 107, 0.43 V/decade, 0.7 V, and 2.1 cm2/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.

  8. Synthesis and Characterization of Dinuclear Metal Complexes Stabilized by Tetradentate Schiff Base Ligands

    Directory of Open Access Journals (Sweden)

    Eid A. Abdalrazaq

    2010-01-01

    Full Text Available Problem statement: The synthesis, spectroscopic properties and theoretical calculations of acetylacetonimine and acetylacetanilidimine Schiff-base ligands, L1H and L2H, respectively and their dinuclear complexes of the type [M2LnCl2(H2O2], where n = 1 or 2, M = Co(II, Ni(II, Cu(II, Zn(II and Cd(II are described. Approach: The new tetradentate dianion Schiff base ligand which was used as stabilizers for the complexes were prepared by condensation of hydrazine with acetylacetone or acetylacetanilide. The dinuclear complexes of theses ligands were synthesized by treating an ethanolic solution of the prepared ligand with hydrated metal salts in molar ratio of 1:2 (L:M. Results: The ligand and their dinuclear metal complexes were characterized by CHN elemental analysis, FT-IR, UV-Vis, 1HNMR (for the ligands, conductivity, magnetic susceptibility and theoretical calculation by using MM2 modeling program. Conclusion: The reaction of these ligands in a 1:2 (L:M afford dinuclear M(II metal complexes with tetrahedral arrangement around Co(II, Zn(II and Cd(II and square planar around Ni(II and Cu(II.

  9. Role of the coordination center in photocurrent behavior of a tetrathiafulvalene and metal complex dyad.

    Science.gov (United States)

    Sun, Yong-Gang; Ji, Shu-Fang; Huo, Peng; Yin, Jing-Xue; Huang, Yu-De; Zhu, Qin-Yu; Dai, Jie

    2014-03-17

    Small organic molecule-based compounds are considered to be promising materials in photoelectronics and high-performance optoelectronic devices. However, photoelectron conversion research based on functional organic molecule and metal complex dyads is very scarce. We design and prepare a series of compounds containing a tetrathiafulvalene (TTF) moiety substituted with pyridylmethylamide groups of formulas [Ni(acac)2L]·2CH3OH (1), [Cu2I2L2]·THF·2CH3CN (2), and [MnCl2L2]n·2nCH3CH2OH (3) (L = 4,5-bis(3-pyridylmethylamide)-4',5'-bimethylthio-tetrathiafulvalene, acac = acetylacetone) to study the role of the coordination center in photocurrent behavior. Complex 1 is a mononuclear species, and complex 2 is a dimeric species. Complex 3 is a two-dimensional (2-D) coordination polymer. Spectroscopic and electrochemical properties of these complexes indicate that they are electrochemically active materials. The tetrathiafulvalene ligand L is a photoelectron donor in the presence of electron acceptor methylviologen. The effect of metal coordination centers on photocurrent response behavior is examined. The redox-active metal coordination centers should play an important role in improvement of the photocurrent response property. The different morphologies of the electrode films reflect the dimensions in molecular structures of the coordination compounds.

  10. Film properties of alumina passivation layer for silicon solar cells prepared by spin-coating method

    Energy Technology Data Exchange (ETDEWEB)

    Watanabe, Ryosuke, E-mail: rwatanabe@st.seikei.ac.jp; Kawashima, Mizuho; Saito, Yoji

    2015-09-01

    We prepared alumina passivation films deposited by a sol-gel wet process for silicon substrates. Aluminum acetylacetonate was used as a precursor, and the solution was spin-coated onto silicon substrates. Calcination temperature dependence of the passivation quality of the films was evaluated mainly by measuring effective lifetime using a photo conductance decay technique and capacitance–voltage measurements. Also, X-ray photoelectron spectroscopy and Fourier transform infrared spectroscopy were carried out to evaluate film properties. A large amount of negative fixed charge density (Q{sub f} = − 3.1 × 10{sup 12} cm{sup −2}) exists in the films calcined at 300 °C. On the other hand, a long effective lifetime of 400 μs was obtained for the sample calcined at 600 °C, and the passivation films had a large amount of positive fixed charge density (Q{sub f} = 3.6 × 10{sup 12} cm{sup −2}) with a low interface state density. - Highlights: • Alumina passivation films for silicon solar cells were prepared by spin-coating. • Electronic properties and the quality of passivation films were investigated. • Carrier lifetime was enhanced for the samples that were calcined above 400 °C. • The films calcined at 300 °C have high amount of negative fixed charge.

  11. Sensing Characteristics of Flame-Spray-Made Pt/ZnO Thick Films as H2 Gas Sensor

    Directory of Open Access Journals (Sweden)

    Nittaya Tamaekong

    2009-08-01

    Full Text Available Hydrogen sensing of thick films of nanoparticles of pristine, 0.2, 1.0 and 2.0 atomic percentage of Pt concentration doped ZnO were investigated. ZnO nanoparticles doped with 0.2–2.0 at.% Pt were successfully produced in a single step by flame spray pyrolysis (FSP technique using zinc naphthenate and platinum(II acetylacetonate as precursors dissolved in xylene. The particle properties were analyzed by XRD, BET, SEM and TEM. Under the 5/5 (precursor/oxygen flame condition, ZnO nanoparticles and nanorods were observed. The crystallite sizes of ZnO spheroidal and hexagonal particles were found to be ranging from 5 to 20 nm while ZnO nanorods were seen to be 5–20 nm wide and 20–40 nm long. ZnO nanoparticles paste composed of ethyl cellulose and terpineol as binder and solvent respectively was coated on Al2O3 substrate interdigitated with gold electrodes to form thin films by spin coating technique. The thin film morphology was analyzed by SEM technique. The gas sensing properties toward hydrogen (H2 was found that the 0.2 at.% Pt/ZnO sensing film showed an optimum H2 sensitivity of ~164 at hydrogen concentration in air of 1 volume% at 300 °C and a low hydrogen detection limit of 50 ppm at 300 °C operating temperature.

  12. 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.

  13. Preparation and Characterization of Modified-ZrO2 Catalysts for the Reaction of CO Hydrogenation

    Institute of Scientific and Technical Information of China (English)

    Qingjie Ge; A. Kiennemann; A.C. Roger; Wenzhao Li; Hengyong Xu

    2004-01-01

    ZrO2 in different structures and CexZr4-xO8 solid solutions have been prepared by a sol-gel related method with propionic acid as the solvent. The results of their characterization and CO hydrogenation performance evaluation show that t-ZrO2 has better catalytic performance for CO hydrogenation to hydrocarbon than m-ZrO2. Cerium (Ⅲ) acetate and zirconium (Ⅳ) acetylacetonate have been chosen as the most suitable starting materials for CexZr4-xO8 solid solution preparation. Ce-Zr reducibility properties are increased by the incorporation of zirconium oxide in the ceria structure. Ce2Zr2O8 exhibits a higher activity, lower methane selectivity and higher iso-C4 selectivity than tetragonal ZrO2. This implies that the formation mechanism of C4 hydrocarbons, especially that for the iso-C4 fraction is different over Ce2Zr2O8 and t-ZrO2.

  14. Experimental and theoretical study on one-pot, three-component route to 2H-indazolo[2,1-b]phthalazine-triones catalyzed by nano-alumina sulforic acid

    Science.gov (United States)

    Kiasat, Ali Reza; Noorizadeh, Siamak; Ghahremani, Mahboubeh; Saghanejad, Seyed Jafar

    2013-03-01

    A simple, efficient, and high yielding one-pot protocol for the synthesis of 2H-indazolo[2,1-b]phthalazine-trione derivatives has been developed by three-component coupling of phthalhydrazide, dimedone and some aromatic aldehydes in ecofriendly neat conditions promoted by nano-γ-alumina sulforic acid. This protocol avoids the use of expensive catalysts, toxic solvents and chromatographic separation. Also the proposed protocol was extended to the linear β-diketone (acetylaceton) instead of cyclic diketone (dimedone). The generality and functional tolerance of this convergent and environmentally benign method is demonstrated. The nature of each step of the suggested mechanism for this condensation reaction is also identified through Density Functional Theory (DFT) calculations using B3LYP/6-31G** level of theory. It is shown that the first step is charge controlled; whereas the second one is controlled by frontier molecular orbitals. The 1H and 13C chemical shift values together with the structural parameters of the title compound have been also computed and the scaled values have been compared with the corresponding experimental NMR and X-ray spectra. As a result, the calculated spectroscopic data and optimized geometry show a good agreement with the experimental results.

  15. Synthesis and characterization of oxo-bridged, trinuclear, six-coordinate mixed-carboxylato complexes of chromium (III)

    Science.gov (United States)

    Baranwal, B. P.; Fatma, Talat

    2005-08-01

    Mixed-carboxylato β-diketonato complexes of chromium (III) (R=C13H27, C15H31 or C17H35 and L=CH3OH) [Cr3O(OOCR)3(dike)3L3]+ have been synthesized by enforced substitution reactions of [Cr3O(OOCCH3)7(H2O)] first with straight chain fatty acids (myristic, palmitic or stearic acid) and then with β-diketones (Hβ-dike) like acetylacetone(Hacac) or benzoylacetone(Hbzac) in toluene under reflux. These are new type of oxo-bridged chromium(III) complexes in which one ligand is a fatty acid while the other one is a β-diketone. The complexes were characterized by elemental analyses, spectral (infrared, electronic, FAB mass and powder XRD) studies, molar conductance and magnetic susceptibility measurements. Bridging coordination modes for both carboxylate and β-diketonate anions were indicated by presence of νasym(Cr3O) vibrations in the infrared spectra. Trinuclear nature of the complexes and their structural features have been discussed on the basis of physicochemical studies.

  16. Curcumin as the OO bidentate ligand in "2 + 1" complexes with the [M(CO)3]+ (M = Re, 99mTc) tricarbonyl core for radiodiagnostic applications.

    Science.gov (United States)

    Sagnou, Marina; Benaki, Dimitra; Triantis, Charalampos; Tsotakos, Theodoros; Psycharis, Vassilis; Raptopoulou, Catherine P; Pirmettis, Ioannis; Papadopoulos, Minas; Pelecanou, Maria

    2011-02-21

    The synthesis and characterization of "2 + 1" complexes of the [M(CO)(3)](+) (M = Re, (99m)Tc) core with the β-diketones acetylacetone (complexes 2, 8) and curcumin (complexes 5, 10 and 6, 11) as bidentate OO ligands, and imidazole or isocyanocyclohexane as monodentate ligands is reported. The complexes were synthesized by reacting the [NEt(4)](2)[Re(CO)(3)Br(3)] precursor with the β-diketone to generate the intermediate aqua complex fac-Re(CO)(3)(OO)(H(2)O) that was isolated and characterized, followed by replacement of the labile water by the monodentate ligand. All complexes were characterized by mass spectrometry, NMR and IR spectroscopies, and elemental analysis. In the case of complex 2, bearing imidazole as the monodentate ligand, X-ray analysis was possible. The chemistry was successfully transferred at (99m)Tc tracer level. The curcumin complexes 5 and 6, as well as their intermediate aqua complex 4, that bear potential for radiopharmaceutical applications due to the wide spectrum of pharmacological activity of curcumin, were successfully tested for selective staining of β-amyloid plaques of Alzheimer's disease. The fact that the complexes maintain the affinity of the mother compound curcumin for β-amyloid plaques prompts for further exploration of their chemistry and biological properties as radioimaging probes.

  17. Synthesis and Conformational Behavior of Rhodium(I) Metallohosts Derived from Diphenylglycoluril.

    Science.gov (United States)

    Coolen, Hein K. A. C.; van Leeuwen, Piet W. N. M.; Nolte, Roeland J. M.

    1996-07-12

    The design and synthesis of molecules containing both a substrate-binding cavity and a nearby catalytically active metal center is a useful approach to the development of synthetic systems that function according to the principles of enzymes. To this end the receptor molecule 2a, derived from diphenylglycoluril, was functionalized with triaryl phosphite ligands to give the receptor ligand 2d. Exchange reactions of 2d with (diketonate)Rh(CO)(2), (diketone = acetylacetone, dibenzoylmethane, or dipivaloylmethane) led to the formation of the metallohosts 3a-c, respectively. The properties and conformational behavior of these metal complexes were studied by NMR techniques. Reaction of compounds 3 with H(2) in the presence of a small excess of additional triphenyl phosphite yields the rhodium(I) hydride complex 5. The metallohosts are capable of binding dihydroxybenzene guests in their cavities by hydrogen bonding and pi-pi stacking interactions. On binding a substrate the conformational behavior of hosts 3a-c was affected considerably.

  18. Polymeric microspheres for radionuclide synovectomy containing neutron-activated holmium-166.

    Science.gov (United States)

    Mumper, R J; Mills, B J; Ryo, U Y; Jay, M

    1992-03-01

    Poly-L-lactic acid (PLA) microspheres containing neutron-activated 166Ho were investigated as potential agents for radionuclide synovectomy. Stable 165Ho, complexed to acetylacetone (AcAc), was incorporated into PLA spheres by the solvent evaporation technique. Spheres prepared with the optimal mean particle size of 7.2 microns (range 2-13 microns) containing 25.4% 165Ho-AcAc (9.1% 165Ho) were irradiated in a high neutron flux to produce 31.1-36.0 mCi 166Ho. In vitro human plasma studies showed that the irradiated spheres retained 99.0 +/- 0.01% of the 166Ho at 314 hr. In-vivo retention studies were conducted by administering irradiated PLA spheres with 257-591 microCi 166Ho into the joint space of normal rabbits (n = 6). Biodistribution analysis and gamma camera analysis showed 166Ho retention in the joint space after 120 hr of 97.7% +/- 0.8% and 98.2% +/- 2.4%, respectively, with no uptake by the lymph nodes. The ease with which the PLA spheres can be made in the optimal size range for later irradiation and their ability to retain the 166Ho make them attractive agents for radionuclide synovectomy.

  19. Metal oxide films on glass and steel substrates

    CERN Document Server

    Sohi, A M

    1987-01-01

    in the pH8 electrolyte supports the view that the rate limiting reduction reaction is possibly oxygen (or water) reduction although some contribution from an organic 'impurity' cannot be ruled out. Coatings of Fe sub 3 O sub 4 on mild steel have been prepared by CVD using pneumatic spraying techniques and the corrosion behaviour of coated electrodes in organic-phosphate electrolyte (pH8) has been examined. A variety of thin (10-1000nm) metal oxide films have been deposited on flat glass substrates by the pyrolysis of an aerosol of metal acetylacetonates in a suitable carrier. The optical characteristics and thickness of the films have been measured and particular interest has centered on the use of a novel pin on disc apparatus to measure the physical durability of such thin films. Characteristic friction/penetration force traces have been established for 1st Series transition metal oxide films and some ranking in terms of 'hardness' established. The use of SnO sub 2 - coated glass for electrodes in a light m...

  20. Series of dinuclear and tetranuclear lanthanide clusters encapsulated by salen-type and β-diketionate ligands: single-molecule magnet and fluorescence properties.

    Science.gov (United States)

    Sun, Wen-Bin; Han, Bing-Lu; Lin, Po-Heng; Li, Hong-Feng; Chen, Peng; Tian, Yong-Mei; Murugesu, Muralee; Yan, Peng-Fei

    2013-10-07

    Three dinuclear [Ln2H2OL(1)2(acac)2]·solvent (1, Ln = Gd, solvent = 2CH2Cl2; 2, Ln = Tb, no solvent; 3, Ln = Er, solvent = (C2H5)2O), and two tetranuclear lanthanide clusters [Ln4(μ3-OH)2L(2)2(acac)6]·2(solvent) (4, Ln = Tb, solvent = CH3OH; 5, Ln = Dy, solvent = CH3CN) were characterized in terms of structure, fluorescence and magnetism. The dinuclear lanthanide complexes were constructed by a rigid salen-type ligand H2L(1) = N,N'-bis(salicylidene)-o-phenylenediamine and β-diketonate (acac = acetylacetonate) ligands, while the tetranuclear clusters were formed from the flexible ligand H2L(2) = N,N'-bis(salicylidene)-1,2-ethanediamine. Crystal structure analysis indicates that the rigid ligand favors the double-decker sandwich structure (Ln2L(1)2), in which the two lanthanide ions have different coordination numbers and geometry, while the more flexible ligand (H2L(2)) leads to planar tetranuclear clusters. The relationship between their respective magnetic anisotropy and ligand-field geometries and their fluorescence properties was investigated. The Dy and Tb-containing clusters exhibit typical visible fluorescence properties, and single-molecule magnet behavior is seen in complex 5.

  1. Solid-phase spectrophotometric determination of nickel in water and vegetable samples at sub-mug l(-1) level with o-carboxylphenyldiazoaminoazobenzene loaded XAD-4.

    Science.gov (United States)

    Liu, Yongwen; Chang, Xijun; Wang, Sui; Guo, Yong; Din, Bingjun; Meng, Shuangming

    2004-09-08

    A highly sensitive and selective solid-phase spectrophotometric method for the determination of sub-mugl(-1) level nickel(II) is described. Nickel(II) was sorbed on a styrene-divinylbenzene-type resin Amberlite XAD-4 as a Ni(II)-o-carboxylphenyldiazoaminoazobenzene (o-CDAA) complex. At pH 9.0, resin phase absorbances at 588 and 800nm were measured directly with an apparent molar absorptivity of 2.95x10(7)gmol(-1)cm(-1). The linear range of the determination was 1.2-41mugg(-1) resin. The detection limit and the quantification limit were found to be 0.24 and 0.76mugg(-1) resin, respectively. The relative standard deviation of 10 replicate determinations of 1.0mug nickel(II) in 100ml sample was of 1.5%. The tolerance limit of coexistent ions was also investigated. Most of them are in tolerable amount. For practical analyses, 1ml acetylacetone used can eliminate the interferences caused by Cu and Fe. The procedure was validated by analysis a certified water reference material (GBW 08618 Beijing, China) and a tomato leaf certified reference material (GBW 08402 Beijing, China) with the results in agreement with the certified values. The method was applied to the determination of nickel(II) in water and vegetable samples with satisfactory results.

  2. Synthesis of indium oxi-sulfide films by atomic layer deposition: The essential role of plasma enhancement

    Directory of Open Access Journals (Sweden)

    Cathy Bugot

    2013-11-01

    Full Text Available This paper describes the atomic layer deposition of In2(S,O3 films by using In(acac3 (acac = acetylacetonate, H2S and either H2O or O2 plasma as oxygen sources. First, the growth of pure In2S3 films was studied in order to better understand the influence of the oxygen pulses. X-Ray diffraction measurements, optical analysis and energy dispersive X-ray spectroscopy were performed to characterize the samples. When H2O was used as the oxygen source, the films have structural and optical properties, and the atomic composition of pure In2S3. No pure In2O3 films could be grown by using H2O or O2 plasma. However, In2(S,O3 films could be successfully grown by using O2 plasma as oxygen source at a deposition temperature of T = 160 °C, because of an exchange reaction between S and O atoms. By adjusting the number of In2O3 growth cycles in relation to the number of In2S3 growth cycles, the optical band gap of the resulting thin films could be tuned.

  3. 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.

  4. Effects of water chemistry on decolorization in three photochemical processes: Pro and cons of the UV/AA process.

    Science.gov (United States)

    Wu, Bingdang; Yin, Ran; Zhang, Guoyang; Yu, Chao; Zhang, Shujuan

    2016-11-15

    The poor selectivity of hydroxyl radicals is a major restriction in the practical application of the UV/H2O2 process for dyeing wastewater treatment. As an alternative, the target-selective UV/acetylacetone (AA) process was found highly efficient for dye decolorization. For the proper selection and application of the two photochemical processes, the effects of water matrices, including common inorganic anions (Cl(-), SO4(2-), NO3(-), HCO3(-)), natural organic matter, metal cations (Mg(2+), Mn(2+), Cu(2+), Fe(3+), Cr(3+)), and temperature, on the photo-degradation of an azo dye, Acid Orange 7 (AO7), were systematically investigated. The experimental results demonstrate that the UV/AA process was more sensitive to inner filter effect. NO3(-), Cu(2+), and Fe(3+) were all detrimental to the UV/AA process, whereas at certain concentrations they were beneficial to the UV/H2O2 process. However, even with severe inhibitory effects, the decolorization efficiency of the UV/AA process was still several times higher than that of the UV/H2O2 process. The results are helpful for us to better understand the mechanisms behind the UV/AA process and may shed light on the application of UV-based advanced oxidation processes for wastewater treatment.

  5. Nickel(II) complexes having Imidazol-2-ylidene-N′-phenylurea ligand in the coordination sphere – syntheses and solid state structures

    Indian Academy of Sciences (India)

    Kishor Naktode; Abhinanda Kundu; Sudeshna Saha; Hari Pada Nayek; Tarun K Panda

    2015-08-01

    We report the syntheses and structural studies of two nickel(II) complexes of imidazol-2-ylidene- N'-phenylureate ligand of composition [{ImBu NCON(H)Ph}2 Ni(acac)2] (1) and [(C6H5NH2)2 Ni(acac)2] [ImMes NCON(H)Ph] (2). The nickel complex 1 was readily prepared by the reaction of nickel(II) acetylacetonate [Ni(acac) 2 ] with imidazol-2-ylidene-N'-phenylureate ligand [ImBu NCON(H)Ph] (L1) in THF under reflux condition for 72 h. The nickel complex 2 was obtained by the reaction of [Ni(acac)2], mesityl derivative of imidazol-2-ylidene-N′-phenylureate ligand [ImMes NCON(H)Ph] (L2) in the presence of aniline as base under reflux condition in THF. Both the paramagnetic complexes have been characterized by FT-IR spectroscopy and elemental analyses. Solid-state structures of both the new complexes were established by single crystal X-ray diffraction analysis. In the molecular structures of complexes 1 and 2, each nickel(II) ion is six fold coordinated and form a distorted octahedral geometry. The optical properties of both complexes have been explored. The Hirshfeld surfaces are used to view and analyze the intermolecular contacts in crystalline state for complex 2.

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

    Directory of Open Access Journals (Sweden)

    María Luz Carrera Jota

    2013-02-01

    Full Text Available 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.

  7. 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.

  8. Characterization of titanium dioxide nanoparticles dispersed in organic ligand solutions by using a diffusion-ordered spectroscopy-based strategy.

    Science.gov (United States)

    Van Lokeren, Luk; Maheut, Géraldine; Ribot, François; Escax, Virginie; Verbruggen, Ingrid; Sanchez, Clément; Martins, José C; Biesemans, Monique; Willem, Rudolph

    2007-01-01

    Diffusion-ordered NMR spectroscopy (DOSY NMR) is presented as a tool for the determination of the diffusion coefficients of organic ligands in suspensions of titanium dioxide nanoparticles. The nanoparticles were prepared by a sol-gel process by hydrolysis and condensation reactions of titanium tetra-n-butoxide in the presence of pentane-2,4-dione (acacH: acetylacetone), as well as para-toluenesulfonic acid (pTsA) and n-butanol (nBuOH). NMR spectroscopic studies were performed in various deuterated solvents, on both dispersed xerosols and diluted sols. The bipolar-pulsed field gradient longitudinal eddy-current delay (LED) pulse sequence was used for data acquisition. The data were processed by inverse Laplace transformation (ILT), by using a maximum entropy algorithm, to afford 2D DOSY spectra. Different diffusion regimes for organic ligands in the bound and unbound states were successfully discriminated, more particularly in [D3]acetonitrile, thus allowing assessment of their interactions with the nanoparticles.

  9. A Nonaqueous Approach to the Preparation of Iron Phosphide Nanowires

    Directory of Open Access Journals (Sweden)

    She Houde

    2010-01-01

    Full Text Available Abstract Previous preparation of iron phosphide nanowires usually employed toxic and unstable iron carbonyl compounds as precursor. In this study, we demonstrate that iron phosphide nanowires can be synthesized via a facile nonaqueous chemical route that utilizes a commonly available iron precursor, iron (III acetylacetonate. In the synthesis, trioctylphosphine (TOP and trioctylphosphine oxide (TOPO have been used as surfactants, and oleylamine has been used as solvent. The crystalline structure and morphology of the as-synthesized products were characterized by powder X-ray diffraction (XRD and transmission electron microscopy (TEM. The obtained iron phosphide nanowires have a typical width of ~16 nm and a length of several hundred nanometers. Structural and compositional characterization reveals a hexagonal Fe2P crystalline phase. The morphology of as-synthesized products is greatly influenced by the ratio of TOP/TOPO. The presence of TOPO has been found to be essential for the growth of high-quality iron phosphide nanowires. Magnetic measurements reveal ferromagnetic characteristics, and hysteresis behaviors below the blocking temperature have been observed.

  10. Fluorinated alcohols as promoters for the metal-free direct substitution reaction of allylic alcohols with nitrogenated, silylated, and carbon nucleophiles.

    Science.gov (United States)

    Trillo, Paz; Baeza, Alejandro; Nájera, Carmen

    2012-09-01

    The direct allylic substitution reaction using allylic alcohols in 1,1,1,3,3,3-hexafluoroisopropanol (HFIP) and 2,2,2-trifluoroethanol (TFE) as reaction media is described. The developed procedure is simple, works under mild conditions (rt, 50 and 70 °C), and proves to be very general, since different nitrogenated nucleophiles and carbon nucleophiles can be used achieving high yields, especially when HFIP is employed as solvent and aromatic allylic alcohols are the substrates. Thus, sulfonamides, carbamates, carboxamides, and amines can be successfully employed as nitrogen-based nucleophiles. Likewise, silylated nucleophiles such as trimethylsilylazide, allyltrimethylsilane, trimethylsilane, and trimethylsilylphenylacetylene give the corresponding allylic substitution products in high yields. Good results for the Friedel-Crafts adducts are also achieved with aromatic compounds (phenol, anisole, indole, and anilines) as nucleophiles. Particularly interesting are the results obtained with electron-rich anilines, which can behave as nitrogenated or carbon nucleophiles depending on their electronic properties and the solvent employed. In addition, 1,3-dicarbonyl compounds (acetylacetone and Meldrum's acid) are also successfully employed as soft carbon nucleophiles. Studies for mechanism elucidation are also reported, pointing toward the existence of carbocationic intermediates and two working reaction pathways for the obtention of the allylic substitution product.

  11. Sol-gel synthesis of mesoporous assembly of Nd 2O 3 nanocrystals with the aid of structure-directing surfactant

    Science.gov (United States)

    Sreethawong, Thammanoon; Chavadej, Sumaeth; Ngamsinlapasathian, Supachai; Yoshikawa, Susumu

    2008-01-01

    The aim of this work was to demonstrate a simple route to synthesize mesoporous assembly of nanocrystalline neodymium oxide (Nd 2O 3) with predominant pore size distribution in the mesopore region, which was successfully done for the first time under mild conditions by a modified sol-gel process with the aid of structure-directing surfactant. Properly manipulated hydrolysis and condensation steps of neodymium n-butoxide modified with acetylacetone in the presence of laurylamine hydrochloride surfactant aqueous solution were performed to obtain the assembled Nd 2O 3 nanocrystal. Various techniques, including thermogravimetric and differential thermal analyses (TG-DTA), X-ray diffraction (XRD), N 2 adsorption-desorption, Brunauer-Emmett-Teller (BET) surface area analysis, Barrett-Joyner-Halenda (BJH) pore size distribution analysis, scanning electron microscopy (SEM), transmission electron microscopy (TEM), and selected-area electron diffraction (SAED), were used to characterize the synthesized Nd 2O 3 nanocrystal. The N 2 adsorption-desorption isotherm of the synthesized Nd 2O 3 nanocrystal calcined at 500 °C exhibited single hysteresis loop with IUPAC type IV-like pattern, indicating the existence of foremost mesopore. BJH pore size distribution result revealed that the synthesized Nd 2O 3 nanocrystals possessed mostly mesopore due to their assembly with a small extent of macropore, resulting in very small mean pore diameter in the mesopore region. The particle size determined from both SEM and TEM micrographs was also extremely small of approximately 10 nm.

  12. A simple route utilizing surfactant-assisted templating sol-gel process for synthesis of mesoporous Dy2O3 nanocrystal.

    Science.gov (United States)

    Sreethawong, Thammanoon; Chavadej, Sumaeth; Ngamsinlapasathian, Supachai; Yoshikawa, Susumu

    2006-08-01

    A simple route of combined sol-gel process with surfactant-assisted templating technique was successfully employed for the first time to synthesize nanocrystalline mesoporous Dy(2)O(3) with narrow monomodal pore size distribution under mild conditions. The nanocrystalline Dy(2)O(3) with monomodal mesoporous characteristic was ultimately achieved by controlling the hydrolysis and condensation steps of dysprosium n-butoxide modified with acetylacetone in the presence of laurylamine hydrochloride surfactant aqueous solution. The synthesized material was methodically characterized by thermogravimetry and differential thermal analysis (TG-DTA), X-ray diffraction (XRD), scanning electron microscopy (SEM), high resolution transmission electron microscopy (HRTEM), selected-area electron diffraction (SAED), N(2) adsorption-desorption, Brunauer-Emmett-Teller (BET) surface area analysis, and Barrett-Joyner-Halenda (BJH) pore size distribution analysis. The particle size of the synthesized Dy(2)O(3) in nanosized range obtained from the SEM and HRTEM micrographs was in good accordance with the crystallite size estimated from the XRD result. The N(2) adsorption-desorption result exhibited hysteresis pattern with single loop, indicating the existence of monomodal mesopore. The extremely narrow pore size distribution with mean pore diameter in the mesopore region of the synthesized Dy(2)O(3) was also confirmed by the BJH result.

  13. Spectral, NLO, Fluorescence, and Biological Activity of Knoevenagel Condensate of β-Diketone Ligands and Their Metal(II Complexes

    Directory of Open Access Journals (Sweden)

    S. Sumathi

    2011-01-01

    Full Text Available 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, H1NMR, mass and ESR spectral studies. Conductivity measurements reveal that all the complexes are nonelectrolytic in nature. Spectroscopic and other analytical data of the complexes suggest square planar geometry for copper(II, cobalt(II, and nickel(II complexes of 3-(3-phenylallylidenepentane-2,4-dione and octahedral geometry for other metal(II complexes. The redox behaviors 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 bacteria and fungus. 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 was found to have considerable effect compared to that of urea and KDP.

  14. 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).

  15. Fabrication of copper nanorods by low-temperature metal organic chemical vapor deposition

    Institute of Scientific and Technical Information of China (English)

    ZHANG Ying; Frank Leung-Yuk Lam; HU Xijun; YAN Zifeng

    2006-01-01

    Copper nanorods have been synthesized in mesoporous SBA-15 by a low-temperature metal organic chemical vapor deposition (MOCVD)employing copper (Ⅱ) acetylacetonate, Cu(acac)2,and hydrogen as a precursor and reactant gas, respectively. The hydrogen plays an important role in chemical reduction of oganometallic precursor which enhances mass transfer in the interior of the SBA-15 porous substrate. Such copper nanostructures are of great potentials in the semiconductor due to their unusual optical, magnetic and electronic properties.In addition, it has been found that chemically modifying the substrate surface by carbon deposition is crucial to such synthesis of copper nanostructures in the interior of the SBA-15, which is able to change the surface properties of SBA-15 from hydrophilic to hydrophobic to promote the adsorption of organic cupric precursor. It has also been found that the copper nanoparticles deposited on the external surface are almost eliminated and the copper nanorods are more distinct while the product was treated with ammonia. This approach could be achieved under a mild condition: a low temperature (400℃) and vacuum (2 kPa) which is extremely milder than the conventional method. It actually sounds as a foundation which is the first time to synthesize a copper nanorod at a mild condition of a low reaction temperature and pressure.

  16. Low-loaded Pd/{alpha}-Al{sub 2}O{sub 3} catalysts: Influence of metal particle morphology on hydrogenation of buta-1,3-diene and hydrogenation and isomerization of but-1-ene

    Energy Technology Data Exchange (ETDEWEB)

    Goetz, J.; Touroude, R. [Universite Louis Pasteur, Strasbourg (France); Volpe, M.A. [Planta Piloto de Ingeneria Quimica, Bahia Blanca (Argentina)

    1996-12-01

    Buta-1,3-diene hydrogenation and but-1-ene hydrogenation and isomerization were studied on low-loaded Pd/{alpha}-Al{sub 2}O{sub 3} catalysts (0.1-0.3 wt.%) prepared from palladium acetylacetonate (Pd(C{sub 5}H{sub 7}O{sub 2}){sub 2}). Deuterium tracer study, hydrogen chemisorption, transmission electron microscopy, and X-ray photoelectron spectroscopy analysis were used to establish the relationships between metal-support interactions, particle shapes, and buta-1,3-diene and but-1-ene hydrogenation and isomerization mechanisms. It was found that the hydrogenation reaction rates (turnover frequencies) are similar for buta-1,3-diene and but-1-ene, but 10 times lower for the 0.1% Pd catalyst compared to the 0.3% Pd catalyst. However, the 0.1% Pd catalyst has a high activity for the isomerization reaction which leads to 98% selectivity in isomers for the but-1-ene reaction. This unusual specific activity is explained considering that the 0.1% Pd catalyst contains flat particles in strong interaction with the support, as was deduced from several characterization methods, while the 0.3% Pd catalyst has more rugged bulk type particles after H{sub 2} treatments because they are not interacting with the support. 33 refs., 7 figs., 5 tabs.

  17. Continuous determination of the Zr-Fe-Y Content by EDTA titrimetry%EDTA滴定法连续测定锆-铁-钇含量

    Institute of Scientific and Technical Information of China (English)

    袁履璀; 向斌; 赵娜

    2013-01-01

    In order to accurately measure the content of Zr, Fe and Y in the acidic solution which produced by recycling waste zirconium-yttrium ceramics, the influences of the iron ion masking agent including acetylacetone, triethanolamine, citric acid and the indicator such as arsenazo M hydrate, methyl thymol blue and xylenol orange on the determination results were investigated in this paper. Finally, a satisfactory result has been achieved by EDTA titrimetry when xylenol orange and hydroxylamine hydrochloride acted as the only indicator and reducing agent, respectively. The RSD was smaller than 2% .%探讨了准确测定废旧锆钇陶瓷回收时产生的酸性溶液中锆、铁、钇的含量时,乙酰丙酮、三乙醇胺和柠檬酸等铁离子掩蔽剂,以及偶氮砷Ⅲ、甲基百里酚蓝和二甲酚橙等指示剂对测定结果的影响,确定仅以二甲酚橙为指示剂,盐酸羟胺为还原剂,用EDTA滴定法连续测定了溶液中的锆、铁、钇含量,测定结果的RSD <2%.

  18. 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.

  19. Spectroscopic studies on Solvatochromism of mixed-chelate copper(II) complexes using MLR technique.

    Science.gov (United States)

    Golchoubian, Hamid; Moayyedi, Golasa; Fazilati, Hakimeh

    2012-01-01

    Mixed-chelate copper(II) complexes with a general formula [Cu(acac)(diamine)]X where acac=acetylacetonate ion, diamine=N,N-dimethyl,N'-benzyl-1,2-diaminoethane and X=BPh(4)(-), PF(6)(-), ClO(4)(-) and BF(4)(-) have been prepared. The complexes were characterized on the basis of elemental analysis, molar conductance, UV-vis and IR spectroscopies. The complexes are solvatochromic and their solvatochromism were investigated by visible spectroscopy. All complexes demonstrated the positive solvatochromism and among the complexes [Cu(acac)(diamine)]BPh(4)·H(2)O showed the highest Δν(max) value. To explore the mechanism of interaction between solvent molecules and the complexes, different solvent parameters such as DN, AN, α and β using multiple linear regression (MLR) method were employed. The statistical results suggested that the DN parameter of the solvent plays a dominate contribution to the shift of the d-d absorption band of the complexes.

  20. Synthesis, characterization, DNA binding, cleavage activity and cytotoxicity of copper(II) complexes.

    Science.gov (United States)

    Li, Mei-Jin; Lan, Tao-Yu; Cao, Xiu-Hui; Yang, Huang-Hao; Shi, Yupeng; Yi, Changqing; Chen, Guo-Nan

    2014-02-21

    Three new mononuclear copper(II) complexes, [Cu(L2)](2+) (1), [Cu(acac)(L)](+) (2), and [Cu(acac-Cl)(L)](+) (3) (L = 2-(4-pyridine)oxazo[4,5-f]1,10-phenanthroline (4-PDOP); acac = acetylacetone; acac-Cl = 3-chloroacetylacetone), have been synthesized and characterized by elemental analysis, high resolution mass spectrometry (Q-TOF), and IR spectroscopy. Two of the complexes were structurally characterized by single-crystal X-ray diffraction techniques. Their interactions with DNA were studied by UV-vis absorption and emission spectra, viscosity, thermal melting, DNA unwinding assay and CD spectroscopy. The nucleolytic cleavage activity of the compounds was carried out on double stranded pBR322 circular plasmid DNA by using a gel electrophoresis experiment in the presence and absence of an oxidant (H2O2). Active oxygen intermediates such as hydroxyl radicals and hydrogen peroxide generated in the presence of L and complexes 1-3 may act as active species for the DNA scission. The cytotoxicity of the complexes against HepG2 cancer cells was also studied.

  1. Effect of Counterion on the Solvatochromic Properties of Heteroleptic Chelate Copper(II Complexes

    Directory of Open Access Journals (Sweden)

    Hamid Golchoubian

    2013-01-01

    Full Text Available A series of heteroleptic chelate copper(II complexes of the type [Cu(L(acac]X where acac = acetylacetonate; L = N,N′-1,6-bis(2-fluorophenyl-2,5-diazahexane; X=CIO4-, BPh4-, PF6-, and BF4- have been prepared and characterized by elemental analyses, IR and UV-Vis spectroscopies, and molar conductance measurements. The prepared complexes are fairly soluble in a large number of organic solvents and show positive solvatochromism. Among the complexes [Cu(L(acac]ClO4, it is demonstrated the most solvatochromism. A multiparametric equation has been utilized to explain the solvent effect on the d-d transition of the complexes using SPSS/PC software. To explore the mechanism of interaction between solvent molecules and the complexes, different solvent parameters such as DN, AN, α, ET(30, π*, and β using stepwise multiple linear regression (SMLR method were employed. The results demonstrated that the donor power of the solvent plays the most important role in the solvatochromism of the compounds.

  2. Modulation of Intersystem Crossing Rate by Minor Ligand Modifications in Cyclometalated Platinum(II) Complexes.

    Science.gov (United States)

    Shafikov, Marsel Z; Kozhevnikov, Dmitry N; Bodensteiner, Michael; Brandl, Fabian; Czerwieniec, Rafał

    2016-08-01

    Photophysical properties of four new platinum(II) complexes comprising extended ppy (Hppy = 2-phenylpyridine) and thpy (Hthpy = 2-(2'-thienyl)pyridine) cyclometalated ligands and acetylacetonate (acac) are reported. Substitution of the benzene ring of Pt-ppy complexes 1 and 2 with a more electron-rich thiophene of Pt-thpy complexes 3 and 4 leads to narrowing of the HOMO-LUMO gap and thus to a red shift of the lowest energy absorption band and phosphorescence band, as expected for low-energy excited states of the intraligand/metal-to-ligand charge transfer character. However, in addition to these conventional spectral shifts, another, at first unexpected, substitution effect occurs. Pt-thpy complexes 3 and 4 are dual emissive showing fluorescence about 6000 cm(-1) (∼0.75 eV) higher in energy relative to the phosphorescence band, while for Pt-ppy complexes 1 and 2 only phosphorescence is observed. For dual-emissive complexes 3 and 4, ISC rates kISC are estimated to be in order of 10(9)-10(10) s(-1), while kISC of Pt-ppy complexes 1 and 2 is much faster amounting to 10(12) s(-1) or more. The relative intensities of the fluorescence and phosphorescence signals of Pt-thpy complexes 3 and 4 depend on the excitation wavelength, showing that hyper-intersystem crossing (HISC) in these complexes is observably significant.

  3. Intermediate temperature single-chamber methane fed SOFC based on Gd doped ceria electrolyte and La 0.5Sr 0.5CoO 3- δ as cathode

    Science.gov (United States)

    Morales, M.; Piñol, S.; Segarra, M.

    Single-chamber fuel cells with electrodes supported on an electrolyte of gadolinium doped ceria Ce 1- xGd xO 2- y with x = 0.2 (CGO) 200 μm thickness has been successfully prepared and characterized. The cells were fed directly with a mixture of methane and air. Doped ceria electrolyte supports were prepared from powders obtained by the acetyl-acetonate sol-gel related method. Inks prepared from mixtures of precursor powders of NiO and CGO with different particle sizes and compositions were prepared, analysed and used to obtain optimal porous anodes thick films. Cathodes based on La 0.5Sr 0.5CoO 3 perovskites (LSCO) were also prepared and deposited on the other side of the electrolyte by inks prepared with a mixture of powders of LSCO, CGO and AgO obtained also by sol-gel related techniques. Both electrodes were deposited by dip coating at different thicknesses (20-30 μm) using a commercial resin where the electrode powders were dispersed. Finally, electrical properties were determined in a single-chamber reactor where methane, as fuel, was mixed with synthetic air below the direct combustion limit. Stable density currents were obtained in these experimental conditions. Temperature, composition and flux rate values of the carrier gas were determinants for the optimization of the electrical properties of the fuel cells.

  4. Synthesis of Three-Dimensional Agaric-like Biomorphic TiO2 by a Facile Method with Coscinodiscus sp.Frustule

    Institute of Scientific and Technical Information of China (English)

    ZHANG Qianqian; CHEN Ran; LI Ling

    2012-01-01

    The paper aims to expand the application of natural marine algae.Marine diatoms,which have intricate frustule structures,can serve as bio-template for preparing three-dimensional materials.A simple and effective approach to synthesize the corrugated agaric-like biomorphic TiO2 templated with frustule of Coscinodiscus sp.is reported.In the sol-gel preparation process,the titania-coating on the frustule is prepared through the deposition and condensation with the aid of acetylacetone (acac) as a controlling agent to make the precursor Ti(BuO)4 hydrolyze slowly.The as-prepared titania-coated frustule and biomorphic TiO2 is characterized by scanning electron microscopy (SEM) attached with energy dispersive X-ray spectrometer (EMAX) and X-ray diffraction (XRD).The microstructure of the corresponding titania nanoparticles appears to be sphere with the diameters distributed around 10-20nm.The templating process is repeated for three cycles.Subsequently,the three-dimensional freestanding corrugated agaric-like biomorphic TiO2 structure is obtained by a selective removal in the NaOH solution.As far as we known,the 3D freestanding corrugated agaric-like biomorphic TiO2 with greatly increased surface area is obtained for the first time.

  5. Cobalt- and iron-based nanoparticles hosted in SBA-15 mesoporous silica and activated carbon from biomass: Effect of modification procedure

    Science.gov (United States)

    Tsoncheva, Tanya; Genova, Izabela; Paneva, Daniela; Dimitrov, Momtchil; Tsyntsarski, Boyko; Velinov, Nicolay; Ivanova, Radostina; Issa, Gloria; Kovacheva, Daniela; Budinova, Temenujka; Mitov, Ivan; Petrov, Narzislav

    2015-10-01

    Ordered mesoporous silica of SBA-15 type and activated carbon, prepared from waste biomass (peach stones), are used as host matrix of nanosized iron and cobalt particles. The effect of preparation procedure on the state of loaded nanoparticles is in the focus of investigation. The obtained materials are characterized by Boehm method, low temperature physisorption of nitrogen, XRD, UV-Vis, FTIR, Mossbauer spectroscopy and temperature programmed reduction with hydrogen. The catalytic behaviour of the samples is tested in methanol decomposition. The dispersion, oxidative state and catalytic behaviour of loaded cobalt and iron nanoparticles are successfully tuned both by the nature of porous support and the metal precursor used during the samples preparation. Facile effect of active phase deposition from aqueous solution of nitrate precursors is assumed for activated carbon support. For the silica based materials the catalytic activity could be significantly improved when cobalt acetylacetonate is used during the modification. The complex effect of pore topology and surface functionality of different supports on the active phase formation is discussed.

  6. 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.

  7. 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.

  8. Synthesis, Crystal Structure and Properties of Complex VO(C12H12N2O2)(C13H10NO2)

    Institute of Scientific and Technical Information of China (English)

    MA Dong-sheng; Gao Shan; HUO Li-hua; GAO Jing-sheng

    2004-01-01

    Complex VO(C12H12N2O2)(C13H10NO2)(C12H12N2O2-2=acetylacetone benzoylhydrozanate, C13H10NO_2=N-phenylbenzohydroxamate) was synthesized and characterized by means of elemental analysis, IR and UV spectroscopies, cyclic voltammetry and single crystal X-ray diffraction. The complex crystallized in the monoclinic system with space group P21/n and the crystal cell parameters a=1.3003(1) nm, b=0.88836(6) nm, c=2.0196(2) nm, β=95.065(8)°, V=2.3238(3) nm3, Mr=495.40 and Z=4. The two oxygen and one nitrogen atoms of the tridentate hydrazone ligand coordinate to the vanadium atom, forming an equatorial plane. And the coordinated vanadium atom exhibits a distorted octahedral geometry. The atom in the transposition to the oxo O atom is the carbonyl oxygen atom of the hydroxamate ligand in the complex. The half-wave redox potential of the title complex in the three different solvents positively shifts in the order of CH2Cl2

  9. Fabrication of LaAlO3 film by sol-gel process with corresponding inorganic

    Institute of Scientific and Technical Information of China (English)

    殷明志; 汪敏强; 姚熹

    2004-01-01

    Well-cubic perovskite lanthanum aluminate (LaAlO3) film on (110) silicon substrate was fabricated by sol-gel method with corresponding inorganic salts. Lanthanum acetate and aluminum acetate glacial acetic acid solutions were prepared via ligand exchange starting from lanthanum nitrate hexahydrate and aluminum nitrate hexahydrate after being refluxed. (CH3CO)2O removed nitrates and the crystallized H2O completely, acetylacetone (AcAc) was partially bidentated with metallic ion of the metallic acetates and formed La(OAc)3(x(AcAc)x, which were hydrolyzed into La(AcAc)3(x(OH)x by adding 10 ml 0.4% methyl cellulose (MCL) solution. The La(AcAc)3(x(OH)x, polymerizing and combining with MCL, formed the LaAlO3 sol precursor with heteropolymeric structure and formed film easily. The epitaxial LaAlO3 film on Si(110) substrate was crystallized after being annealed in thermal annealing furnace for 650(750 (C/30 min. The morphologies and microstructures were characterized. The refractive index of the LAO film was 1.942 to 2.007; the dielectric constant and the dissipation factors were estimated to be 23(26 and 2.1(10(4 ( 2.4(10(4 respectively.

  10. Fabrication of LaAlO3 film by sol-gel process with corresponding inorganic

    Institute of Scientific and Technical Information of China (English)

    殷明志; 汪敏强; 姚熹

    2004-01-01

    Well-cubic perovskite lanthanum aluminate (LaAl03) film on (110) silicon substrate was fabricated by sol-gel method with corresponding inorganic salts. Lanthanum acetate and aluminum acetate glacial acetic acid solutions were prepared via ligand exchange starting from lanthanum nitrate hexahydrate and aluminum nitrate hexahydrate after being refluxed. (CH3CO)2O removed nitrates and the crystallized H2O completely, acetylacetone (AcAc) was partially bidentated with metallic ion of the metallic acetates and formed La(OAc)3-x(AcAc)x, which were hydrolyzed into La(AcAc)3-x(OH)x by adding 10 ml 0.4% methyl cellulose (MCL) solution. The La(AcAc)3-x(OH)x, polymerizing and combining with MCL,formed the LaA1O3 sol precursor with heteropolymeric structure and formed film easily. The epitaxial LaA1O3 film on Si(110) substrate was crystallized after being annealed in thermal annealing furnace for 650-750 ℃/30 min. The morphologies and microstructures were characterized. The refractive index of the LAO film was 1.942 to 2.007; the dielectric constant and the dissipation factors were estimated to be 23-26 and 2.1×10-4-2.4x10-4 respectively.

  11. Assembly, characterization, and electrochemical properties of immobilized metal bipyridyl complexes on silicon(111) surfaces.

    Science.gov (United States)

    Lattimer, Judith R C; Blakemore, James D; Sattler, Wesley; Gul, Sheraz; Chatterjee, Ruchira; Yachandra, Vittal K; Yano, Junko; Brunschwig, Bruce S; Lewis, Nathan S; Gray, Harry B

    2014-10-28

    Silicon(111) surfaces have been functionalized with mixed monolayers consisting of submonolayer coverages of immobilized 4-vinyl-2,2'-bipyridyl (1, vbpy) moieties, with the remaining atop sites of the silicon surface passivated by methyl groups. As the immobilized bipyridyl ligands bind transition metal ions, metal complexes can be assembled on the silicon surface. X-ray photoelectron spectroscopy (XPS) demonstrates that bipyridyl complexes of [Cp*Rh], [Cp*Ir], and [Ru(acac)2] were formed on the surface (Cp* is pentamethylcyclopentadienyl, acac is acetylacetonate). For the surface prepared with Ir, X-ray absorption spectroscopy at the Ir LIII edge showed an edge energy as well as post-edge features that were essentially identical with those observed on a powder sample of [Cp*Ir(bpy)Cl]Cl (bpy is 2,2'-bipyridyl). Charge-carrier lifetime measurements confirmed that the silicon surfaces retain their highly favorable photoelectronic properties upon assembly of the metal complexes. Electrochemical data for surfaces prepared on highly doped, n-type Si(111) electrodes showed that the assembled molecular complexes were redox active. However the stability of the molecular complexes on the surfaces was limited to several cycles of voltammetry.

  12. Single-Site Zeolite-Anchored Organoiridium Carbonyl Complexes: Characterization of Structure and Reactivity by Spectroscopy and Computational Chemistry.

    Science.gov (United States)

    Martinez-Macias, Claudia; Chen, Mingyang; Dixon, David A; Gates, Bruce C

    2015-08-10

    A family of HY zeolite-supported cationic organoiridium carbonyl complexes was formed by reaction of Ir(CO)2 (acac) (acac=acetylacetonate) to form supported Ir(CO)2 complexes, which were treated at 298 K and 1 atm with flowing gas-phase reactants, including C2 H4 , H2 , (12) CO, (13) CO, and D2 O. Mass spectrometry was used to identify effluent gases, and infrared and X-ray absorption spectroscopies were used to characterize the supported species, with the results bolstered by DFT calculations. Because the support is crystalline and presents a nearly uniform array of bonding sites for the iridium species, these were characterized by a high degree of uniformity, which allowed a precise determination of the species involved in the replacement, for example, of one CO ligand of each Ir(CO)2 complex with ethylene. The supported species include the following: Ir(CO)2 , Ir(CO)(C2 H4)2 , Ir(CO)(C2 H4), Ir(CO)(C2 H5), and (tentatively) Ir(CO)(H). The data determine a reaction network involving all of these species.

  13. 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.

  14. 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.

  15. 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}.

  16. The Structure and Magnetic Properties Metal-carbon Nanocomposites FeCo / C on Based of Polyacrylonitrile

    Directory of Open Access Journals (Sweden)

    L.V. Kozhitov

    2014-07-01

    Full Text Available For the first time in the conditions of the IR pyrolysis precursor based on polyacrylonitrile, cobalt acetate and acetylacetonate iron (ratio of metals in precursors Fe : Co = 3 : 1 metal-carbon nanocomposites have been obtained, which are carbon matrix with graphite-like structure, containing buried her nanoparticles of intermetallids of FeCo. It is shown that the phase formation FeCo occurs in the temperature range of obtaining 500-600 degrees centigrade, at T ≤ 500 degrees centigrade are only two distinct phases metals: HCC-With and BCC Fe. In the structure of nanocomposites obtained at T ≥ 600 degrees centigrade, at the same time there are nanoparticles of intermetallides and FeCo little content phase fсс-Co or solid solution of cobalt. It is determined that the composition of a metal component nanocomposite satisfies the ratio of Fe, Co, originally specified.

  17. Helicenes as All-in-One Organic Materials for Application in OLEDs: Synthesis and Diverse Applications of Carbo- and Aza[5]helical Diamines.

    Science.gov (United States)

    Jhulki, Samik; Mishra, Abhaya Kumar; Chow, Tahsin J; Moorthy, Jarugu Narasimha

    2016-06-27

    A set of eight helical diamines were designed and synthesized to demonstrate their relevance as all-in-one materials for multifarious applications in organic light-emitting diodes (OLEDs), that is, as hole-transporting materials (HTMs), EMs, bifunctional hole transporting + emissive materials, and host materials. Azahelical diamines function very well as HTMs. Indeed, with high Tg values (127-214 °C), they are superior alternatives to popular N,N'-di(1-naphthyl)-N,N'-diphenyl-(1,1'-biphenyl)-4,4'-diamine (NPB). All the helical diamines exhibit emissive properties when employed in nondoped as well as doped devices, the performance characteristics being superior in the latter. One of the carbohelical diamines (CHTPA) serves the dual function of hole transport as well as emission in simple double-layer devices; the efficiencies observed were better by quite some margin than those of other emissive helicenes reported. The twisting endows helical diamines with significantly high triplet energies such that they also function as host materials for red and green phosphors, that is, [Ir(btp)2 acac] (btp=2-(2'-benzothienyl)pyridine; acac=acetylacetonate) and [Ir(ppy)3 ] (ppy=2-phenylpyridine), respectively. The results of device fabrications demonstrate how helicity/ helical scaffold may be diligently exploited to create molecular systems for maneuvering diverse applications in OLEDs.

  18. Synthesis,Crystal Structure and Thermal Stability of(Diacetylacetone)(diimidazole)Nickel(Ⅱ)Complex

    Institute of Scientific and Technical Information of China (English)

    建方方; 庞蕾; 肖海连; 孙萍萍

    2004-01-01

    The title compound, [Ni(acac)2(Im)2] (acac = acetylacetone), has been obtained by the reaction of Ni(acac)2 with imidazole ligand in the ethanol solvent. The blue crystal is of triclinic, space group Pī with a = 7.472(2), b = 9.456(2), c = 13.823(3)A, α = 85.55(3), β = 89.03(3), γ = 80.63(3)o, C16H22N4NiO4, Mr = 393.09, V = 960.7(3)A3, Z = 2, Dc = 1.359 g/cm3, F(000) = 412, μ = 1.036 mm-1, R = 0.0549 and wR = 0.1615. The crystal structure consists of two disconnected structural units. Each Ni atom coordinated by two N atoms from two imidazole ligands and four O atoms from two acetylactone ligands adopts a slightly distorted octahedron. The structure characterization was performed by means of IR, UV, TG, elemental analysis and single-crystal X-ray analysis. The thermal gravity (TG) data indicate that thermal decomposition of the title compound takes place in two steps, and the residue is NiO.

  19. Size dependence of the magnetic relaxation and specific power absorption in iron oxide nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Lima, E. [CONICET and Instituto de Nanociencia y Nanotecnologia and Centro Atomico Bariloche (Argentina); Torres, T. E. [University of Zaragoza, Instituto de Nanociencia de Aragon (INA) and Departamento de Fisica de la Materia Condensada and Laboratorio de Microscopias Avanzadas (LMA) (Spain); Rossi, L. M. [Instituto de Quimica, Universidade de Sao Paulo (Brazil); Rechenberg, H. R. [Instituto de Fisica, Universidade de Sao Paulo (Brazil); Berquo, T. S. [Institute of Rock Magnetism, University of Minnesota (United States); Ibarra, A. [University of Zaragoza, INA and LMA (Spain); Marquina, C. [CSIC, Universidad de Zaragoza, Departamento de Fisica de la Materia Condensada and Instituto de Ciencia de Materiales de Aragon (ICMA) (Spain); Ibarra, M. R. [University of Zaragoza, INA and Departamento de Fisica de la Materia Condensada and LMA (Spain); Goya, G. F., E-mail: goya@unizar.es [University of Zaragoza, INA and Departamento de Fisica de la Materia Condensada (Spain)

    2013-05-15

    In this study, magnetic and power absorption properties of a series of iron oxide nanoparticles with average sizes Left-Pointing-Angle-Bracket d Right-Pointing-Angle-Bracket ranging from 3 to 23 nm were reported. The nanoparticles were prepared by thermal decomposition of Iron(III) acetylacetonate in organic media. From the careful characterization of the magnetic and physicochemical properties of these samples, the specific power absorption (SPA) values experimentally found were numerically reproduced, as well as their dependence with particle size, using a simple model of Brownian and Neel relaxation at room temperature. SPA experiments in ac magnetic fields (H{sub 0} = 13 kA/m and f = 250 kHz) indicated that the magnetic and rheological properties played a crucial role determining the heating efficiency at different conditions. A maximum SPA value of 344 W/g was obtained for a sample containing nanoparticles with Left-Pointing-Angle-Bracket d Right-Pointing-Angle-Bracket = 12 nm and dispersion {sigma} = 0.25. The observed SPA dependence with particle diameter and their magnetic parameters indicated that, for the size range and experimental conditions of f and H studied in this study, both Neel and Brown relaxation mechanisms are important to the heat generation observed.

  20. Enhanced efficiency in mixed host red electrophosphorescence devices

    Energy Technology Data Exchange (ETDEWEB)

    Su Zisheng; Li Wenlian, E-mail: wllioel@yahoo.com.cn; Chu Bei, E-mail: beichu@163.com

    2011-06-01

    Enhanced efficiency of red phosphorescent organic light-emitting devices is observed by using a bis[2-(2'-benzothienyl)pyridinato-N,C{sup 3'}] iridium(acetylacetonato) doped 4,4'-N,N'-dicarbazole-biphenyl (CBP) and 1,3,5-tris(N-phenylbenzimidazole-2-yl)benzene (TPBI) mixed host emitting layer. The CBP:TPBI mixed host device shows a maximum external quantum efficiency of 9.1%, which is dramatically improved compared to that of the CBP (6.6%) and TPBI (5.4%) single host devices. Such a mixed host strategy can also be exploited in red phosphor dibenzo[f,h]quinoxaline iridium (acetylacetonate) doped devices. Investigations reveal that the position of charge carrier recombination zone of the mixed host devices predominantly locates in the electron blocking layer/emitting layer interface. The efficiency enhancement is attributed to the optimized hole and electron injection balance and hence increased charge carrier recombination rate in the emitting layer.

  1. 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.

  2. Synthesis and Structural Characterization of a Copper Complex with Furaldehyde Salicylylhydrazone

    Institute of Scientific and Technical Information of China (English)

    DU Kang-Kai; LIU Shi-Xiong

    2008-01-01

    The copper complex Cu(C12H9N2O3)2 has been synthesized by the reaction of furaldehyde salicylylhydrazone (Hfs) and copper acetylacetonate and characterized by X-ray crystal diffraction and spectroscopic studies. The crystal crystallizes in space group P21/n with a =5.9765(3), b = 15.7196(9), c = 12.0514(6) A, β= 101.618(3)°,V= 1109.0(1) A3,C24H18CuN4O6,M, = 521.96, Z= 2, Dc = 1.563 g/cm3, μ =1.035 mm-1,F(000) = 534, R = 0.0373 and wR =0.1058 for 2283 observed reflections (Ⅰ 20(Ⅰ)). The copper atom has a square-planar CuN2O2 coordination and should be in an oetahedral coordination if considering Cu-O (phenol) with distances of 2.796(2) A as weak bonds. The neighboring copper complex molecules are linked together by these weak Cu-O (phenol) bonds, resulting in an extended 1D chain. The title com-pound exhibits paramagnetie property and fluorescence behavior at room temperature supported by the EPR and fluorescence spectra.

  3. Theoretical study, and infrared and Raman spectra of copper(II) chelated complex with dibenzoylmethane.

    Science.gov (United States)

    Nekoei, A-R; Vakili, M; Hakimi-Tabar, M; Tayyari, S F; Afzali, R; Kjaergaard, H G

    2014-07-15

    There are some discrepancies in both the vibrational assignments and in the metal-ligand (M-L) bond strengths predicted in the previous studies on the copper (II) chelated complex of dibenzoylmethane, Cu(dbm)2. Also, there is a lack of theoretical structure, Raman spectrum and full vibrational assignment for Cu(dbm)2 in the literatures. Density functional theory (DFT) at the B3LYP level and also MP2 calculations using different basis sets, besides Natural Bond Orbital (NBO) and Atoms-in-Molecules (AIM) analyses, have been employed to investigate the effect of methyl substitution with the phenyl group on the stabilities of bis(acetylacetonate) copper (II), Cu(acac)2, and Cu(dbm)2 complexes and the electron delocalization in their chelated rings. Measured solid phase infrared and Raman bands for Cu(dbm)2 complex have been interpreted in terms of the calculated vibrational modes and detailed assignment has been presented. We concluded that, theoretically, the results of charge transfer studies, and experimentally, in-phase symmetric O-Cu-O stretching mode of these complexes are very useful measures for M-L bond strength. The electron delocalization in the chelated rings and the M-L bond strength in Cu(dbm)2 are concluded to be higher than those in Cu(acac)2. The calculated geometries and vibrational results are in good agreement with the experimental data.

  4. 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...... is examined by X-ray powder diffraction, determination of the specific surface area by the BET-method, determination of the copper dispersion in the reduced catalyst by a novel N2O-method, by transmission electron microscopy, and by test of the catalytic properties in a catalytic micro-reactor. A low peak...... 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...

  5. 脂肪乳中甘油测定方法的建立%A method for determination of glycerin in fat emulsion

    Institute of Scientific and Technical Information of China (English)

    孙婧

    2015-01-01

    Objective To establish a new method for the determination of glycerin in fat emulsion.Method Glycerin was oxidized by sodium periodate to generate formaldehyde,which in turn reacted with acetylacetone to produce a derivative with ultraviolet absorption property,which was determined using ultraviolet speetrophotometer.Result This method showed high recovery (100.04% in the linear range of content) and good precision.Conclusion This method is reliable in determining the concentration of glycerin in fat emulsion.%目的 建立一种脂肪乳中甘油含量测定的方法.方法 甘油可以被高碘酸钠氧化生成甲醛,甲醛与乙酰丙酮反应生成的衍生物有紫外吸收,采用紫外分光光度计测定衍生物的吸光度.结果 在测定的含量线性范围内,回收率为100.04%,方法精密度良好.结论 该方法可以准确地测定脂肪乳中的甘油含量.

  6. Chemical vapor deposition and analysis of thermally insulating ZrO{sub 2} layers on injection molds

    Energy Technology Data Exchange (ETDEWEB)

    Atakan, Burak; Khlopyanova, Victoria; Mausberg, Simon; Kandzia, Adrian; Pflitsch, Christian [Thermodynamik (IVG) and Cenide, Universitaet Duisburg-Essen, Lotharstr. 1, 47057 Duisburg (Germany); Mumme, Frank [Kunststoff-Institut Luedenscheid, Karolinenstrasse 8, 58507 Luedenscheid (Germany)

    2015-07-15

    High quality injection molding requires a precise control of cooling rates. Thermal barrier coating (TBC) of zirconia with a thickness of 20-40 μm on polished stainless steel molds could provide the necessary insulating effect. This paper presents results of zirconia deposition on stainless steel substrates using chemical vapor deposition (CVD) aiming to provide the process parameters for the deposition of uniform zirconia films with such a thickness. The deposition was performed with zirconium (IV) acetylacetonate (Zr(C{sub 5}H{sub 7}O{sub 2}){sub 4}) as precursor and synthetic air as co-reactant, which allows deposition at temperatures below 600 C. The experiments were carried out in a hot-wall reactor at pressures between 7.5 mbar and 500 mbar and in a temperature range from 450 C to 600 C. Important growth parameters were characterized and growth rates between 1 and 2.5 μm/h were achieved. Thick and well adhering zirconia layers of 38 μm could be produced on steel within 40 h. The transient heat transfer rate upon contact with a hot surface was also evaluated experimentally with the thickest coatings. These exhibit a good TBC performance. (copyright 2015 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  7. [Procedure for determination of individual sensitivity to antitumor drugs].

    Science.gov (United States)

    Abduvaliev, A A; Gil'dieva, M S; Tatarskiĭ, V P

    2006-05-01

    The present paper proposes to employ the cultured tumor cells of the breast and chick fibroblasts after long-term cultivation (for above 24 days) to determine their individual drug sensitivity and, as a criterion of cell damage, to use the percent of destruction of the cell layer formed in the wells 24 hours after drug insertion. It also presents the comparative results of tests of 2 cellular models that have been used to determine the in vitro sensitivity of the cells of breast cancer and chick fibroblasts to melfalan and its complex compound with copper acetylacetonate - MOK*M. At the same time, the cytotoxic activity of MOK*M and melfalan against tumor cells has been not shown to differ greatly (16.02+/-1.85 and 15.71+/-0.65% cell layer destruction, respectively), but the same activity of MOK*M against the model of intact cells (chick fibroblasts) was much less (15.23+/-1.97%) than that of melfalan (95.39+/-1.11%). The test system proposed by the authors is of certain informative value and it may be used for the determination of the individual sensitivity of tumor cells to antitumor drugs.

  8. Influence of the utilized precursors on the morphology and properties of YBa{sub 2}Cu{sub 3}O{sub 7−y} superconducting nanostructures

    Energy Technology Data Exchange (ETDEWEB)

    Alikhanzadeh-Arani, Sima [Plasma Physics Research Center, Science and Research Branch, Islamic Azad University, Tehran, Islamic Republic of Iran (Iran, Islamic Republic of); Salavati-Niasari, Masoud, E-mail: salavati@kashanu.ac.ir [Institute of Nano Science and Nano Technology, University of Kashan, Kashan, P.O. Box 87317-51167, Islamic Republic of Iran (Iran, Islamic Republic of); Almasi-Kashi, Mohammad [Department of Physics, University of Kashan, Kashan, 87317-51167, Islamic Republic of Iran (Iran, Islamic Republic of)

    2013-05-15

    Highlights: ► YBa{sub 2}Cu{sub 3}O{sub 7−x} (Y-123) nanoparticles was synthesized by solid state processing. ► Inorganic precursor was used in the synthesis of YBa{sub 2}Cu{sub 3}O{sub 7−x}. ► The effect of calcinations on morphology and particle size were investigated. -- Abstract: In order to prevent agglomeration of high temperature ceramic material, the solid state processing based on new and appropriate yttrium complex precursors without applying surfactant has been suggested. These have been prepared by a reaction of yttrium acetate with three coordination compositions, acetylacetone, 2-hydroxo-1-naphthaldehyde and salicylaldehyde, for forming yttrium complex types. It was found that the size and morphology of products are clearly dependent on the type of utilized precursor because the organic ligands around yttrium center in these novel precursors act like a protecting agent. Magnetic susceptibility measurements showed that T{sub c} of the superconducting nanoparticles is from 82 K to 88.4 K. The crystalline structures of the nanoparticles remained in orthorhombic symmetry. Characterizations of specimens were performed using scanning electron microscopy and transmission electron microscopy, supported by other techniques including XRD diffraction, energy dispersive X-ray, FT-IR spectrum and magnetic susceptibility measurements.

  9. Chromium and Ruthenium-Doped Zinc Oxide Thin Films for Propane Sensing Applications

    Science.gov (United States)

    Gómez-Pozos, Heberto; González-Vidal, José Luis; Torres, Gonzalo Alberto; Rodríguez-Baez, Jorge; Maldonado, Arturo; de la Luz Olvera, María; Acosta, Dwight Roberto; Avendaño-Alejo, Maximino; Castañeda, Luis

    2013-01-01

    Chromium and ruthenium-doped zinc oxide (ZnO:Cr) and (ZnO:Ru) thin solid films were deposited on soda-lime glass substrates by the sol-gel dip-coating method. A 0.6 M solution of zinc acetate dihydrate dissolved in 2-methoxyethanol and monoethanolamine was used as basic solution. Chromium (III) acetylacetonate and Ruthenium (III) trichloride were used as doping sources. The Ru incorporation and its distribution profile into the films were proved by the SIMS technique. The morphology and structure of the films were studied by SEM microscopy and X-ray diffraction measurements, respectively. The SEM images show porous surfaces covered by small grains with different grain size, depending on the doping element, and the immersions number into the doping solutions. The sensing properties of ZnO:Cr and ZnO:Ru films in a propane (C3H8) atmosphere, as a function of the immersions number in the doping solution, have been studied in the present work. The highest sensitivity values were obtained for films doped from five immersions, 5.8 and 900, for ZnO:Cr and ZnO:Ru films, respectively. In order to evidence the catalytic effect of the chromium (Cr) and ruthenium (Ru), the sensing characteristics of undoped ZnO films are reported as well. PMID:23482091

  10. Chromium and Ruthenium-Doped Zinc Oxide Thin Films for Propane Sensing Applications

    Directory of Open Access Journals (Sweden)

    Maximino Avendaño-Alejo

    2013-03-01

    Full Text Available Chromium and ruthenium-doped zinc oxide (ZnO:Cr and (ZnO:Ru thin solid films were deposited on soda-lime glass substrates by the sol-gel dip-coating method. A 0.6 M solution of zinc acetate dihydrate dissolved in 2-methoxyethanol and monoethanolamine was used as basic solution. Chromium (III acetylacetonate and Ruthenium (III trichloride were used as doping sources. The Ru incorporation and its distribution profile into the films were proved by the SIMS technique. The morphology and structure of the films were studied by SEM microscopy and X-ray diffraction measurements, respectively. The SEM images show porous surfaces covered by small grains with different grain size, depending on the doping element, and the immersions number into the doping solutions. The sensing properties of ZnO:Cr and ZnO:Ru films in a propane (C3H8 atmosphere, as a function of the immersions number in the doping solution, have been studied in the present work. The highest sensitivity values were obtained for films doped from five immersions, 5.8 and 900, for ZnO:Cr and ZnO:Ru films, respectively. In order to evidence the catalytic effect of the chromium (Cr and ruthenium (Ru, the sensing characteristics of undoped ZnO films are reported as well.

  11. 3,4-Dihydroxy-1,6-bis(4-methoxyphenyl)hexa-2,4-diene-1,6-dione, its 4-methylphenyl analogue, and a potassium salt of 2-hydroxy-4-(4-methoxyphenyl)-4-oxobut-2-enoic acid.

    Science.gov (United States)

    Nye, Luke; Turnbull, Mark M; Wikaira, Jan L

    2013-11-01

    Reaction of 4-methoxyacetophenone with diethyl oxalate under basic conditions produced 3,4-dihydroxy-1,6-bis(4-methoxyphenyl)hexa-2,4-diene-1,6-dione, C20H18O6, (1). The molecules lie across a crystallographic inversion centre and intramolecular hydrogen bonding, similar to acetylacetone, is observed, confirming that the molecule is in the di-enol-dione tautomeric form. Additional O-H...O hydrogen bonds link the molecules into chains parallel to the b axis. The structure is compared with that of redetermined 4-methylphenyl compound 3,4-dihydroxy-1,6-bis(4-methylphenyl)hexa-2,4-diene-1,6-dione, C20H18O4, (2), which crystallizes in a similar fashion. The salt, catena-poly[[μ2-2-hydroxy-4-(4-methoxyphenyl)-4-oxobut-2-enoato-κ(3)O(1),O(2):O(4)][μ2-2-hydroxy-4-(4-methoxyphenyl)-4-oxobut-2-enoic acid-κ(2)O(1):O(4)]potassium], [K(C11H9O5)(C11H10O5)]n, (3), was isolated as a by-product of the synthesis of (1). The two organic species are linked by a strong hydrogen bond between the carboxylic acid and carboxylate groups. They are further stabilized and linked into a double-chain structure via the seven-coordinate potassium ion.

  12. Multiple magnetic relaxation processes, magnetocaloric effect and fluorescence properties of rhombus-shaped tetranuclear rare earth complexes.

    Science.gov (United States)

    Gao, Hong-Ling; Jiang, Li; Liu, Shuang; Shen, Hai-Yun; Wang, Wen-Min; Cui, Jian-Zhong

    2016-01-07

    Seven new tetranuclear rare earth (RE) complexes [RE4(acac)4L6(μ3-OH)2] (HL = 5-(4-fluorobenzylidene)-8-hydroxylquinoline; acac = acetylacetonate; RE = Y (1), Eu (2), Gd (3), Tb (4), Dy (5), Tm (6) and Lu (7)) have been synthesized and completely characterized. Complex exhibits multiple zero-field slow magnetic relaxation processes typical of Single Molecule Magnets (SMMs). Two distinct slow magnetic relaxation processes, with effective energy barriers of Ueff = 48 K for the slow relaxation (SR) process and Ueff = 121 K for the fast relaxation (FR) process, are mainly attributed to the presence of two crystallographically independent Dy(III) sites. The magnetocaloric effect (MCE) was detected as -ΔSm(T) = 20.8 J kg(-1) K(-1) for complex . The fluorescence properties of complexes 1, 2, 4, 5 and 7 were also investigated. Complexes 2, 4 and 5 show the characteristic peaks for their corresponding RE(III) center, while complexes 1 and 7 show similar emission peaks to the Schiff base ligand when they are excited at the appropriate wavelength.

  13. 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.

  14. Synthesis of indium oxi-sulfide films by atomic layer deposition: The essential role of plasma enhancement.

    Science.gov (United States)

    Bugot, Cathy; Schneider, Nathanaëlle; Lincot, Daniel; Donsanti, Frédérique

    2013-01-01

    This paper describes the atomic layer deposition of In2(S,O)3 films by using In(acac)3 (acac = acetylacetonate), H2S and either H2O or O2 plasma as oxygen sources. First, the growth of pure In2S3 films was studied in order to better understand the influence of the oxygen pulses. X-Ray diffraction measurements, optical analysis and energy dispersive X-ray spectroscopy were performed to characterize the samples. When H2O was used as the oxygen source, the films have structural and optical properties, and the atomic composition of pure In2S3. No pure In2O3 films could be grown by using H2O or O2 plasma. However, In2(S,O)3 films could be successfully grown by using O2 plasma as oxygen source at a deposition temperature of T = 160 °C, because of an exchange reaction between S and O atoms. By adjusting the number of In2O3 growth cycles in relation to the number of In2S3 growth cycles, the optical band gap of the resulting thin films could be tuned.

  15. Unconventional Synthesis of γ-Fe2O3: Excellent Low-Concentration Ethanol Sensing Performance

    Science.gov (United States)

    Naskar, Atanu; Narjinary, Mousumi; Kundu, Susmita

    2016-09-01

    This study reports on a simple unconventional procedure for synthesis of γ-Fe2O3 nanopowder and its fabrication as a resistive ethanol sensor. γ-Fe2O3 powder having an average particle size of ˜15 nm was prepared by thermal decomposition of iron(III) acetylacetonate. Platinum incorporation (0.5-1.5 wt.%) was also carried out for enhancing sensing performance. The powders were characterized using an x-ray diffractometer, x-ray photoelectron spectroscopy, Brunauer-Emmett-Teller surface area, field area scanning electron microscopy, transmission electron microscopy along with energy dispersion x-ray analyses. Sensor fabricated from pure γ-Fe2O3 exhibited excellent ethanol sensing performance at concentrations down to 1 ppm, having a great demand in medical diagnosis and food-processing industries. The response observed for pure γ-Fe2O3 (˜75% for 1 ppm ethanol) was enhanced ˜10% after 1 wt.% Pt impregnation. Sensors were quite stable and selective towards ethanol vapour detection. A possible mechanism for high sensing performance has been discussed.

  16. (2Z,2′Z,4E,4′E-4,4′-(Cyclohexane-1,2-diyldinitrilodipent-2-en-2-ol

    Directory of Open Access Journals (Sweden)

    Zhi-Rong Qu

    2008-05-01

    Full Text Available A new tetradentate chiral Schiff base ligand, C16H26N2O2, has been synthesized by the reaction of acetylacetone with (1R,2R-(−-1,2-diaminocyclohexane. Both of the molecules in the asymmetric unit are of the same chirality (R configuration, since the absolute configuration was determined by the starting reagent (1R,2R-(−-1,2-diaminocyclohexane. The six-membered cyclohexane ring is in a chair conformation, and the substituents are equatorial in the most stable conformation (trans-cyclohexyl. At the ring substituents, large conjugated —C=N—CH=C—OH systems exist, resulting from the original ketone converted into the enol form. With H atoms excluded, the atoms of each substituent lie in the same plane. The two molecules in the asymmetric unit have almost the same structure, with slight differences in the torsion angles between the substituents and the cyclohexane ring; the corresponding N1—(C—C—Ccyclohexane torsion angles are −177.2 (3 and 179.3 (4° in one molecule and −176.5 (3 and 178.4 (4° in the other. Two intramolecular O—H...N hydrogen bonds exist in each molecule.

  17. Structural models of vanadate-dependent haloperoxidases and their reactivity

    Indian Academy of Sciences (India)

    Mannar R Maurya

    2006-11-01

    Vanadium(V) complexes with hydrazone-based ONO and ONN donor ligands that partly model active-site structures of vanadate-dependent haloperoxidases have been reported. On reaction with [VO(acac)2] (Hacac = acetylacetone) under nitrogen, these ligands generally provide oxovanadium(IV) complexes [VO(ONO)X] (X = solvent or nothing) and [VO(acac)(ONN)], respectively. Under aerobic conditions, these oxovanadium(IV) species undergo oxidation to give oxovanadium(V), dioxovanadium (V) or -oxobis{oxovanadium(V)} species depending upon the nature of the ligand. Anionic and neutral dioxovanadium(V) complexes slowly deoxygenate in methanol to give monooxo complexes [VO(OMe)(MeOH)(ONO)]. The anionic complexes [VO2(ONO)]- can also be converted in situ on acidification to oxohydroxo complexes [VO(OH)(HONO)]+ and to peroxo complexes [VO(O2)(ONO)]-, and thus to the species assumed to be intermediates in the haloperoxidases activity of the enzymes. In the presence of catechol (H2cat) and benzohydroxamic acid (H2bha), oxovanadium (IV) complexes, [VO (acac)(ONN)] gave mixed-chelate oxovanadium(V) complexes [VO(cat)(ONN)] and [VO(bha)(ONN)] respectively. These complexes are not very stable in solution and slowly convert to the corresponding dioxo species [VO2(ONN)] as observed by 51V NMR and electronic absorption spectroscopic studies.

  18. Effect of solvent on the extraction of lanthanides with picrolonic acid

    Energy Technology Data Exchange (ETDEWEB)

    Ali, A.; Saeed, M.M. [Pakistan Institute of Nuclear Science and Technology (PINSTECH), Islamabad (Pakistan). Chemistry Div.; Rehman, H. [Pakistan Institute of Nuclear Science and Technology (PINSTECH), Islamabad (Pakistan). Central Analytical Facility Div.; Anwar, J. [Punjab Univ., Lahore (Pakistan). Inst. of Chemistry

    2010-07-01

    Extraction of Eu(III), Tb(III) and Lu(III), as representatives of lanthanides, has been studied with picrolonic acid [1-p-nitrophenyl-3-methyl-4-nitro-5-pyrazolone (HPA)] as extractant in various solvents such as acetylacetone (ACAC), 1-octanol (ONL), n-hexanol (HNL), 1-butanol (nBNL), 2-butanol (iBNL), cyclohexanone (CHN), n-butyl ether (BE), di(1,2-dichloroethyl)ether (DCEE), diisobutylketone (DIBK), benzene and toluene from aqueous solution of pH 1-2, having ionic strength of 0.01 mol dm{sup -3} (K{sup +}/H{sup +}, Cl{sup -}). The composition of the extracted adduct has been determined as M(PA){sub 3} except in DCEE where it is M(PA){sub 3}.(HPA). Extraction constants (log K{sub ex}) were calculated and on the basis of log K{sub ex}, the role of diluents in the extraction process has been discussed. The solvents with respect to their extractability of the rare earth metal ions can be arranged in the order ACAC > DIBK > BE> DCEE > ONL > HNL > CHN. (orig.)

  19. Planar tetranuclear Dy(III) single-molecule magnet and its Sm(III), Gd(III), and Tb(III) analogues encapsulated by salen-type and β-diketonate ligands.

    Science.gov (United States)

    Yan, Peng-Fei; Lin, Po-Heng; Habib, Fatemah; Aharen, Tomoko; Murugesu, Muralee; Deng, Zhao-Peng; Li, Guang-Ming; Sun, Wen-Bin

    2011-08-01

    The syntheses, structures, and magnetic properties are reported for four new lanthanide clusters [Sm(4)(μ(3)-OH)(2)L(2)(acac)(6)]·4H(2)O (1), [Gd(4)(μ(3)-OH)(2)L(2)(acac)(6)]·4CH(3)CN (2), and [Ln(4)(μ(3)-OH)(2)L(2)(acac)(6)]·2H(2)L·2CH(3)CN (3, Ln = Tb; 4, Ln = Dy) supported by salen-type (H(2)L = N,N'-bis(salicylidene)-1,2-cyclohexanediamine) and β-diketonate (acac = acetylacetonate) ligands. The four clusters were confirmed to be essentially isomorphous by infrared spectroscopy and single-crystal X-ray diffraction. Their crystal structures reveal that the salen-type ligand provides a suitable tetradentate coordination pocket (N(2)O(2)) to encapsulate lanthanide(III) ions. Moreover, the planar Ln(4) core is bridged by two μ(3)-hydroxide, four phenoxide, and two ketonate oxygen atoms. Magnetic properties of all four compounds have been investigated using dc and ac susceptibility measurements. For 4, the static and dynamic data indicate that the Dy(4) complex exhibits slow relaxation of the magnetization below 5 K associated with single-molecule magnet behavior.

  20. Preparation of magnetite aqueous dispersion for magnetic fluid hyperthermia

    Energy Technology Data Exchange (ETDEWEB)

    Kikuchi, Teppei; Kasuya, Ryo [Graduate School of Environmental Studies, Tohoku University, 6-6-20, Aramaki, Aoba, Aoba-ku, Sendai 980-8579 (Japan); Endo, Shota; Nakamura, Akira; Takai, Toshiyuki [Institute of Development, Aging and Cancer, Tohoku University, 4-1 Seiryo-cho, Aramaki-Aoba, Aoba-ku, Sendai 980-8575 (Japan); Metzler-Nolte, Nils [Faculty of Chemistry and Biochemistry, Ruhr-University Bochum, Universitaetstrasse 150, D-44801 Bochum (Germany); Tohji, Kazuyuki [Graduate School of Environmental Studies, Tohoku University, 6-6-20, Aramaki, Aoba, Aoba-ku, Sendai 980-8579 (Japan); Balachandran, Jeyadevan, E-mail: jeyadevan.b@mat.usp.ac.j [Department of Material Science, School of Engineering, University of Shiga Prefecture, 2500, Hassaka-cho, Hikone-City, Shiga 522-8533 (Japan)

    2011-05-15

    An aqueous magnetic suspension was prepared by dispersing amphiphilic co-polymer-coated monodispersed magnetite nanoparticles synthesized through thermal decomposition of iron acetylacetonate (Fe(acac){sub 3}) in a mixture of oleic acid and oleylamine. The average diameter of narrow-size-distributed magnetite nanoparticles varied between 5 and 12 nm depending on the experimental parameters such as reaction temperature, metal salt concentration and oleic acid/oleylamine ratio. Though the as-synthesized particles were coated with oleate and were dispersible in organic solvent, their surfaces were modified using amphiphilic co-polymers composed of poly(maleic anhydride-alt-1-octadecene) and polyethylene glycol-methyl ether and made dispersible in water. Infrared spectra of the sample indicated the existence of -COOH groups on the surface for further conjugation with biomolecules for targeted cancer therapy. - Research Highlights: Preparation of magnetite nanoparticles suitable for in vivo magnetic fluid hyperthermia. Thermal decomposition of Fe(acac){sub 3} in a mixture of oleic acid and oleylamine. Monodispersed magnetite particles with average sizes varying between 5 and 12 nm. Modification of the hydrophobic particle surface with amphiphilic co-polymers. These surface modified particles have carboxyl groups and polyethylene glycol.

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

    Science.gov (United States)

    Torres-Huerta, A. M.; Domínguez-Crespo, M. A.; Ramírez-Meneses, E.; Vargas-García, J. R.

    2009-02-01

    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.

  2. 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.

  3. Superparamagnetic iron oxide nanoparticles coated with different polymers and their MRI contrast effects in the mouse brains

    Science.gov (United States)

    Xie, Songbo; Zhang, Baolin; Wang, Lei; Wang, Jun; Li, Xuan; Yang, Gao; Gao, Fabao

    2015-01-01

    PEG and PEG/PEI modified superparamagnetic iron oxide nanoparticles (SPIONs) were synthesized by the thermal decomposition of iron (III) acetylacetonate (Fe(acac)3) in poly (ethylene glycol) (PEG) containing poly (ethylene imine) (PEI) (0 or 0.3 g). PEG/PEI-SPIONs were coated with Tween 80 (PEG/PEI/Tween 80-SPIONs). Fourier transform infrared spectroscopy (FTIR) analyses indicated that PEG, PEG/PEI and PEG/PEI/Tween 80 were attached to the surfaces of the SPIONs. The PEG-SPIONs, PEG/PEI-SPIONs and PEG/PEI/Tween 80-SPIONs performed excellent colloidal stability in the phosphate buffered saline (PBS), and in deionized water with the mean hydrodynamic sizes of 19.5, 21.0, 24.0 nm and the zeta potentials of -5.0, 35.0, 19.0 mV, respectively. All the SPIONs showed low cytotoxicity assessed by the MTT assay. In vivo magnetic resonance imaging (MRI) of the Kunming (KM) mouse brains were performed, the PEG-SPIONs, PEG/PEI-SPIONs and PEG/PEI/Tween 80-SPIONs exhibited vascular imaging effects in bulbus olfactorius, frontal cortex, temporal, thalamus and brain stem of the mouse brains after 24 h intravenous injection of the nanoparticles. The SPIONs have potentials as MRI contrast agents in the mouse brains.

  4. Description of the blocking index programs; Descriptif des programmes de calcul des index de blocage anticyclonique

    Energy Technology Data Exchange (ETDEWEB)

    Parey, S. [Departement Environnement, Service Applications de l`Electricite et Environnement, Direction des Etudes et Recherches, Electricite de France (EDF), 92 - Clamart (France)

    1997-09-01

    The work is conducted in the framework of the European programme SIDDACLICH (SImulation, Diagnosis and Direction of the Anthropogenic CLImate CHange), co-ordinated by DKRZ (Deutsches Klimarechenzentrum) of Hamburg. This project aims to perform and analyze climatic simulations with coupled models in order to study detection and impact of possible climate change linked to human activities. EDF/R and D D contribution to this project is limited to the delivery of diagnosis programs concerning acetylacetone blocking detection, in order to permit the evaluation of the impact of climate change on this type of situation from the results of coupled simulations performed in the project. First, two blocking indexes had been coded from works of Mullen and Kaas and Branstator, reported in the literature and applied to evaluate the impact of the augmentation of CO{sub 2} gas atmospheric concentration on a situation of this type, staring from the results of different equilibrium simulation results of atmospheric only simulations performed in the framework of a previous programme on Anthropogenic Climate Change. Then, these indexes have been confronted with a more commonly used index, the Tibaldi et al. index, using a long series of data covering the period 1963-1988, in order to have an idea of the situations detected by each index for the Euro-Atlantic sector in winters for which the situation is well known. (authors) 9 refs., 6 figs.

  5. Fabrication and structure characterization of ITO transparent conducting film by sol-gel technique

    Institute of Scientific and Technical Information of China (English)

    LI Zhi-hua; REN Dong-yan

    2007-01-01

    Using In(NO3)3-5H2O and acetylacetone as raw materials and anhydrous SnCl4 as dopant, the transparent conducting indium tin oxide(ITO) films were prepared by sol-gel and dip-coating technique. The phase transformation, structure properties and physical properties (sheet resistance and transmittance) of the films were investigated by DTA-TG, XRD, SEM, four-probe method and UV-Vis spectrometry. The results indicate that it is feasible to fabricate ITO films on the quartz substrates by sol-gel technique, and the ITO films are formed by accumulating of particles with the size of several decades of nanometers. The prepared ITO film has cubic bixbyite structure, and (111) is its preferred plane. After five-times dip-coating, the ITO film has a thickness less than 150 nm, a sheet resistance of 110 Ω/□, a resistivity of 1.65×10-3 Ω-cm and a transparency of 90%.

  6. /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.

  7. 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.

  8. Shape controlled hydrothermal synthesis and characterization of LiFePO4 for lithium ion batteries.

    Science.gov (United States)

    Yu, Yang; Li, Qianwen; Ma, Yanmei; Zhang, Xing; Zhu, Yongchun; Qian, Yitai

    2013-02-01

    Various LiFePO4 microstructures were synthesized via hydrothermal or solvothermal routes using different additives. In an aqueous solution, LiFePO4 spindles whose length was about 2 microm were obtained with the assistance of polyvinyl pyrrolidone (PVP). As PVP and P2O7(4-) added in water, ellipsoidal LiFePO4 particles which composed of nanoparticles around 100 nm in diameter were obtained. If the additive was cetyltrimethyl ammonium bromide (CTAB), sheet-like LiFePO4 crystals with the width of 100 nm were prepared. In the mixed solvents of water together with ethanol or acetylacetone, when adding CTAB or polyethylene glycol (20000), LiFePO4 plates or nanoparticles were obtained. The ellipsoidal LiFePO4 had the best electrochemical properties among all these products. It is found that the annealed samples were significantly better than the corresponding unannealed ones. Take the ellipsoidal LiFePO4 for example, the initial discharge capacity of annealed (161 mAh/g) was much higher than the unannealed ones (85 mAh/g) at 0.1 C and the former cell still could deliver a capacity of 143 mAh/g after 30 cycles.

  9. 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.

  10. The effects of exposure in space on two high-performance polymers

    Energy Technology Data Exchange (ETDEWEB)

    Kiefer, Richard L., E-mail: rlkief@wm.ed [Department of Chemistry, College of William and Mary, P.O. Box 8795, Williamsburg, VA 23185 (United States); Gabler, William J.; Hovey, Michael T. [Department of Chemistry, College of William and Mary, P.O. Box 8795, Williamsburg, VA 23185 (United States); Thibeault, Sheila A. [Advanced Materials and Processing Branch, NASA Langley Research Center, Hampton, VA 23681 (United States)

    2011-02-15

    Films of a polyimide, poly(pyromellitimide-1,4-diphenyl ether), and a poly(etherimide), commercial Ultem, both pure and with additives were exposed to the low earth orbit (LEO) space environment on several missions of the Materials on the International Space Station Experiment (MISSE). The additives, which contained aluminum or boron, were designed to interact with atomic oxygen to form a protective metal oxide coating. A polyimide film containing 10% aluminum acetylacetonate (Al(acac){sub 3}) survived an exposure of nearly four year while an adjacent pure film was completely eroded. After exposure in space, films containing aluminum showed an enhanced amount of the element on the surface along with an enhanced amount of oxygen. Boron-containing films showed no enhancement of the element after exposure. The temperature of 10% mass loss increased with space exposure for films containing aluminum but decreased for those containing boron. The glass transition temperature (T{sub g}) increased after space exposure for polyimide films containing Al(acac){sub 3}.

  11. The effects of exposure in space on two high-performance polymers

    Science.gov (United States)

    Kiefer, Richard L.; Gabler, William J.; Hovey, Michael T.; Thibeault, Sheila A.

    2011-02-01

    Films of a polyimide, poly(pyromellitimide-1,4-diphenyl ether), and a poly(etherimide), commercial Ultem ®, both pure and with additives were exposed to the low earth orbit (LEO) space environment on several missions of the Materials on the International Space Station Experiment (MISSE). The additives, which contained aluminum or boron, were designed to interact with atomic oxygen to form a protective metal oxide coating. A polyimide film containing 10% aluminum acetylacetonate (Al(acac) 3) survived an exposure of nearly four year while an adjacent pure film was completely eroded. After exposure in space, films containing aluminum showed an enhanced amount of the element on the surface along with an enhanced amount of oxygen. Boron-containing films showed no enhancement of the element after exposure. The temperature of 10% mass loss increased with space exposure for films containing aluminum but decreased for those containing boron. The glass transition temperature ( Tg) increased after space exposure for polyimide films containing Al(acac) 3.

  12. TREG coated iron oxide nanoparticles as contrast agent for MRI in-vivo use

    Science.gov (United States)

    Gutierrez-Garcia, Eric; Hidalgo-Tobon, Silvia; Lopez, Ciro; Gonzalez-Rodriguez, Roberto; Coffer, Jeffery; De Celis Alonso, Benito; Dies Suarez, Pilar; Obregon, Manuel; Perez-Pena, Mario; Platas-Neri, Diana; Mendez-Rojas, Miguel

    2014-11-01

    Super-paramagnetic iron oxide nanoparticles (SPIONs) are of interest due to their great potential applications in diverse fields such as biomedicine. In this work we have prepared SPION nanoparticles using the polyol technique and characterized the magnetic properties of them for MRI in-vivo use. Nanoparticle preparation: All reagents were purchased from commercial sources (Sigma-Aldrich, St. Louis, USA) Iron (III) acetylacetonate, [Fe(acac)3], was used as the iron oxide precursor and thermally decomposed at high temperatures in triethyleneglycol (TREG). Nano-sized magnetite particles were prepared by an adaptation of the method proposed by Wei Cai et al[1-3]. A healthy rabbit was scanned on a clinical 1.5 T Philips MR scanner. Images were taken in 2D mode with a mFFE sequence. Relaxation time T2 was obtained from the MR images using a Matlab algorithm where the signal intensity decay was calculated at each image and then adjusted to a mono-exponential curve. Images were obtained before contrast injection, 24 hours and 36 hours following SPIONs administration. Signal decay at different Echo times for the prepared magnetic SPIONs, before and after contrast injection was measured. It was visualized a concentration of the agent contrast in brain and liver and the results were compared with images obtained from histopathology.

  13. Photocatalytic activity enhancement of TiO{sub 2} films by micro and nano-structured surface modification

    Energy Technology Data Exchange (ETDEWEB)

    Bizarro, M., E-mail: monserrat@iim.unam.mx [Instituto de Investigaciones en Materiales, Universidad Nacional Autonoma de Mexico, A.P. 70-360, Coyoacan 04510, D.F. (Mexico); Tapia-Rodriguez, M.A. [Instituto de Investigaciones en Materiales, Universidad Nacional Autonoma de Mexico, A.P. 70-360, Coyoacan 04510, D.F. (Mexico); Ojeda, M.L. [Departamento de Ciencias Naturales y Exactas, Universidad de Guadalajara, Centro Universitario de los Valles, C.P. 46600 Ameca, Jalisco (Mexico); Alonso, J.C.; Ortiz, A. [Instituto de Investigaciones en Materiales, Universidad Nacional Autonoma de Mexico, A.P. 70-360, Coyoacan 04510, D.F. (Mexico)

    2009-04-01

    Titanium oxide thin films were deposited by spin coating using a precursor solution of titanium oxide (IV) acetylacetonate. To increase the contact surface area of the films, TiO{sub 2} microspheres were added to the surface of the films. These spheres were 2 {mu}m in diameter and formed agglomerates on the surface. They did not spread uniformly across the substrate, creating different roughnesses and morphologies along the surface of films. Photocatalytic properties of the samples were tested by the degradation of a methyl orange solution. The degradation performance was compared between plain films, films with microspheres and films covered with commercial TiO{sub 2} P25 powder. The results indicate that the samples that were surface modified with TiO{sub 2} microspheres present a photodegradation reaction rate 62 times higher than that obtained for plain TiO{sub 2} films. The rate of reaction of the samples covered with P25 was 2 times greater than that obtained for the samples with microspheres, but the adhesion to the film was better in the case of microspheres. Moreover, samples with microspheres could be reused several times maintaining the same structural and photocatalytic properties.

  14. Research on Raman-scattering and Fabrication of Multilayer Thin Film with Different Structures and Components Based on Pt/Ti/Si3N4/SiO2/Si Substrate

    Institute of Scientific and Technical Information of China (English)

    Qiu-lin Tan; Wen-dong Zhang; Chen-yang Xue; Jun Liu; Jun-hong Li; Ji-jun Xiong

    2009-01-01

    Using the same conditions and various starting materials, such as lead acetate trihydrate, tetrabulyl titanate, zirconium n-butoxide, and acetylacetone, two kinds of solid precursors, lead zirconate titanate (PZT, Zr/Ti=15/85) and lead titanate (PT), were fabricated. With three different combinations, namely, PZT, PT/PZT-PZT/PT, and PT/PZT/-/PZT/PT, three multilayer thin films were deposited on three Pt-Ti-Si3N4-SiO2-Si substrates by a modified sol-gel process. The fabrication process of the thin films is discussed in detail. We found that there is a large built-in stress in the thin film, which can be diminished by annealing at 600 ℃, when the gel is turned into solid material through drying and sintering. The Raman scattering spectra of the films with different compositions and structures were investigated. With the help of X-ray diffraction (XRD) analyzer and Raman scattering spectra analyzer, it was found that the thin films with the PT/PZT-PZT/PT structure have reasonable crystallinity and less residual stress. XRD testing shows that the diffraction pattern of the multilayer film results from the superimposition of the PZT and PT patterns. This leads to the conclusion that the PT/PZT-PZT/PT multilayer thin film has a promising future in pyroelectric infrared detectors with high performance.

  15. Structural diversity in binuclear complexes of alkaline earth metal ions with 4,6-diacetylresorcinol

    Science.gov (United States)

    Shebl, Magdy; Khalil, Saied M. E.; Taha, A.; Mahdi, M. A. N.

    2012-11-01

    A new series of binuclear and mixed-ligand complexes with the general formula: [M 2(LO)yClz]; where M = Mg(II), Ca(II), Sr(II) and Ba(II); H2L = 4,6-diacetylresorcinol, the secondary ligand L' = acetylacetone (acac), 8-hydroxyquinoline (8-HQ) or 2,2'-bipyridyl (Bipy), n = 0-2, m = 1, 2, x = 0, 1, 2, 4, y = 0, 2, 4, 5 and z = 0-2; have been synthesized. They have been characterized by the analytical and spectral methods (IR, 1H NMR and mass) as well as TGA and molar conductivity measurements. The spectroscopic and conductance data suggested that the H2L ligand behaves as a neutral, monobasic or dibasic tetradentate ligand, depending on the basicity of the secondary ligand, through the two phenolic and two carbonyl groups. Binuclear octahedral geometry has been assigned to all of the prepared complexes in various molar ratios 2:2; 2:2:2; 1:2:1 and 1:2:4 (L:M:L'). Molecular orbital calculations were performed for the ligands and their complexes using Hyperchem 7.52 program on the bases of PM3 level and the results were correlated with the experimental data. The ligand and some of its alkaline metal(II) complexes showed antibacterial activity towards some of Gram-positive and Gram-negative bacteria, yeast (Candida albicans) and fungus (Aspergillus fumigatus).

  16. 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.

  17. 聚铝碳硅烷的制备及应用进展%Preparation and Application of Polyalumincarbosilane

    Institute of Scientific and Technical Information of China (English)

    黎阳

    2012-01-01

    The properties of silicon carbide (SiC) ceramics fibers and SiC ( Al) ceramics fibers were introduced. The methods for preparing polyalumincarbosilane by reacting polycarbosilane, polysilacarbosilane or polydimethysilane with aluminum acetylacetonate, the chemical structures, and applications ( for the preparation of high-temperature resistant ceramics fibers and light-emitting ceramics films) of polyalumincarbosilane were reviewed. The advantages and disadvantages of the different preparation methods were reviewed. The existing problems required be addressed and the future research directions were discussed and proposed.%介绍了碳化硅(SiC)陶瓷纤维、含铝SiC陶瓷纤维的特点,综述了用聚碳硅烷、聚硅碳硅烷、聚二甲基硅烷与乙酰丙酮铝反应制备聚铝碳硅烷先驱体的合成方法,聚铝碳硅烷的化学结构及在制备耐超高温陶瓷纤维和发光陶瓷薄膜中的应用,评述了各种制备工艺的优缺点,提出了当前工作中需要解决的问题,并展望了今后的发展趋势.

  18. Preparation and characterization of lead zirconate titanate ceramic fibers with alkoxide-based sol-gel route

    Energy Technology Data Exchange (ETDEWEB)

    Mai Manfang; Lin Cheng; Xiong Zhaoxian; Xue Hao; Chen Lifu [Department of Materials Science and Engineering, College of Materials, Xiamen University, Xiamen 361005 (China)], E-mail: zxxiong@xmu.edu.cn

    2009-03-01

    Lead zirconate titanate (PZT) fibers with diameters from 10{mu}m to 40{mu}m were prepared via a sol-gel route. Several kinds of chemicals were used, including lead acetate trihydrate, zirconium n-butoxide and titanium n-butoxide, in addition to butanol as a solvent. As a water source for hydrolysis reaction, Pb(CH{sub 3}COO){sub 2}{center_dot}3H{sub 2}O was directly used without further adding of water or catalyst conventionally. Acetylacetonate and acetate were added as stabilization agents to obtain stable sols for fiber drawing. The gel-to-ceramic conversion was characterized with thermal analysis, infrared spectroscopy and X-ray diffraction. A pure perovskite phase was obtained after heat treatment at 650 deg. C for 1h. By using scanning electron microscope (SEM), it was observed that a lower rate of heat treatment resulted in a denser microstructure of the fibers. The relative permittivity and the P-E hysteresis loop of the crystalline PZT fibers were also measured and discussed in the paper.

  19. Preparation and characterization of lead zirconate titanate ceramic fibers with alkoxide-based sol-gel route

    Science.gov (United States)

    Mai, Manfang; Lin, Cheng; Xiong, Zhaoxian; Xue, Hao; Chen, Lifu

    2009-03-01

    Lead zirconate titanate (PZT) fibers with diameters from 10μm to 40μm were prepared via a sol-gel route. Several kinds of chemicals were used, including lead acetate trihydrate, zirconium n-butoxide and titanium n-butoxide, in addition to butanol as a solvent. As a water source for hydrolysis reaction, Pb(CH3COO)2·3H2O was directly used without further adding of water or catalyst conventionally. Acetylacetonate and acetate were added as stabilization agents to obtain stable sols for fiber drawing. The gel-to-ceramic conversion was characterized with thermal analysis, infrared spectroscopy and X-ray diffraction. A pure perovskite phase was obtained after heat treatment at 650°C for 1h. By using scanning electron microscope (SEM), it was observed that a lower rate of heat treatment resulted in a denser microstructure of the fibers. The relative permittivity and the P-E hysteresis loop of the crystalline PZT fibers were also measured and discussed in the paper.

  20. Direct dry-grinding synthesis of monodisperse lipophilic CuS nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Li, Yajuan; Scott, Julie; Chen, Yi-Tzai; Guo, Liangran; Zhao, Mingyang; Wang, Xiaodong [Department of Biomedical and Pharmaceutical Sciences, College of Pharmacy, The University of Rhode Island, Kingston, RI 02881 (United States); Lu, Wei, E-mail: weilu@uri.edu [Department of Biomedical and Pharmaceutical Sciences, College of Pharmacy, The University of Rhode Island, Kingston, RI 02881 (United States); School of Pharmacy, Fudan University, Shanghai 201203 (China)

    2015-07-15

    Copper sulfide nanoparticles, effective absorbers of near-infrared light, are recently attracting broad interest as a photothermal coupling agent for cancer therapy. Lipophilic copper sulfide nanoparticles are preferred for high performance biomedical applications due to high tissue affinity. Synthesis of lipophilic copper sulfide nanoparticles requires complicated multi-step processes under severe conditions. Here, we describe a new synthetic process, developed by direct dry-grinding of copper(II) acetylacetonate with sulfur under ambient environment at low temperature. The formed CuS nanoparticles are of uniform size, ∼10 nm in diameter, and are monodispersed in chloroform. Each covellite CuS nanocrystal surface is modified with oleylamine through hydrogen bonding between sulfur atoms and amine groups of oleylamine. The nanoparticles demonstrate near-infrared light absorption for photothermal applications. The synthetic methodology described here is more convenient and less extreme than previous methods, and should thus greatly facilitate the preparation of photothermal lipophilic copper sulfide nanomaterials for cancer therapy. - Highlights: • We make lipophilic CuS nanoparticles by mechanical grinding method in large scale. • The reaction condition is studied to obtain high yield and uniform size. • The synthesis does not need nitrogen protection or high temperature. • Lipophilic CuS nanoparticles show significant near-infrared absorbance.

  1. Kinetics and mechanism of interaction of some bioactive ligands with cis-diaqua(cis-1,2-diaminocyclohexane)platinum(II) in aqueous medium

    Indian Academy of Sciences (India)

    P Karmakar; S Ray; S Mallick; B K Bera; A Mandal; S Mondal; A K Ghosh

    2013-09-01

    The substitution reaction of cis-[Pt(cis-dach)(H2O)2]2+ (where `dach’ is cis-1,2-diaminocyclohexane) with 2-thiouracil (S, N), 1,2-cyclohexanedionedioxime (N, N) and acetylacetone (O, O) were studied in aqueous solution in 0.10 M NaClO4 under pseudo-first order conditions as a functions of concentration, pH and temperature using UV-Vis spectrophotometry. The substitution reaction proceeds via rapid outer sphere association complex formation, followed by two slow consecutive steps. The first of these involves ligand-assisted deaquation, while second involves chelation as the second aqua ligand is displaced. The association equilibrium constant (KE) for the outer sphere complex formation has been evaluated together with rate constants for the two subsequent steps. The rate constants increase with increasing ligand concentration and the evaluated activation parameters for all reactions suggest an associative substitution mechanism for both the aqua ligand substitution processes. The product of the reaction has been characterized by IR, NMR and ESI-MS spectral analysis; which throws more light on the mechanistic behaviour of platinum(II) antitumour complexes.

  2. 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)

  3. Photooxidation of Furfural with Phthalocyanine-sensitized TiO2 Particle Under Xenon Lamp

    Institute of Scientific and Technical Information of China (English)

    2007-01-01

    Copper phthalocyanine was selected as the photosensitizer to sensitize TiO2 in this experiment with furfural as the target pollutant. The composite catalysts (TiO2/CuPC) obtained showed a great activity under a xenon lamp. By experiments, the optimal preparation conditions of the composite catalysts were set as follows: the CuPC loading mass fraction was 1.5% , the mass fraction of acetylacetone was 0. 3% , and the stirring time was 10 h. UV-Vis diffuse reflectance spectra, XRD, and BET were used to characterize the properties of the composite catalysts, which showed that after loading CuPC on TiO2, the composite catalyst retained the same crystal structure as pure TiO2 and the wavelength range of its absorption spectrum was broadened to 600-700 nm while its surface area was smaller than that of the pure TiO2. Under the optimal conditions, 20 mg/L furfural solution was degraded by nearly 90% and TOC by about 70%. When the catalyst was reused 6 times, the activity of the catalyst was still retained by about 75%.

  4. New Synthetic Method of 1,5-diaryl-1,4-pentadiene-3-one%1,5-二芳基-1,4-戊二烯-3-酮类化合物的新合成方法

    Institute of Scientific and Technical Information of China (English)

    尹彦冰; 许钱; 尹官武; 裴爽

    2013-01-01

    A new synthetic method of 1,5-diaryl-1,4-pentadiene-3-one was developed by using acetylacetone and aromatic aldehydes as substrate , sodium hydroxide as catalyst and ethanol as solvent .The structure of the compounds were characterized by NMR and IR.The results showed that the yield of the product was above 90% when 10% sodi-um hydroxide solution was used as catalyst .Compared with the conventional methods , the new synthetic method has several advantages, such as the simple raw materials, the mild reaction conditions, and the high yield of production .%  以乙酰丙酮、芳醛为原料,乙醇为溶剂,氢氧化钠为催化剂的条件下合成了一系列1,5-二芳基-1,4-戊二烯-3-酮类化合物,用核磁、红外等测试手段对化合物进行了表征。结果表明:在10%的氢氧化钠溶液的催化下,产物的产率均在90%以上,与传统的方法相比,该方法具有反应条件温和、操作简单及产率高等优点。

  5. Relaxivity enhancement of aquated Tris(β-diketonate)gadolinium(III) chelates by confinement within ultrashort single-walled carbon nanotubes.

    Science.gov (United States)

    Law, Justin J; Guven, Adem; Wilson, Lon J

    2014-01-01

    Ultrashort single-walled carbon nanotubes loaded with gadolinium ions (gadonanotubes) have been previously shown to exhibit extremely high T1 -weighted relaxivities (>100 mm(-1) s(-1) ). To further examine the effect of nanoconfinement on the relaxivity of gadolinium-based contrast agents for magnetic resonance imaging, a series of ultrashort single-walled carbon nanotube (US-tube) materials internally loaded with gadolinium chelates have been prepared and studied. US-tubes were loaded with Gd(acac)3  · 2H2 O, Gd(hfac)3  · 2H2 O, and Gd(thd)3 (acac = acetylacetone, hfac = hexafluoroacetylacetone, thd = tetramethylheptanedione). The longitudinal relaxivities of the prepared materials determined at 25°C in a 1.5 T field were 103 mm(-1) s(-1) for Gd(acac)3  · 2H2 O@US-tubes, 105 mm(-1) s(-1) for Gd(hfac)3  · 2H2 O@US-tubes and 26 mm(-1) s(-1) for Gd(thd)3 @US-tubes. Compared with the relaxivities obtained for the unloaded chelates (<10 mm(-1) s(-1) ) as well as accounting for the T1 reduction observed for the empty US-tubes, the boost in relaxivity for chelate-loaded US-tubes is attributed to confinement within the nanotube and depends on the number of coordinated water molecules.

  6. Electrophoretic deposition of BaTiO{sub 3}/CoFe{sub 2}O{sub 4} multiferroic composite films

    Energy Technology Data Exchange (ETDEWEB)

    Zhou Dongxiang; Jian Gang [Department of Electronic Science and Technology, Huazhong University of Science and Technology, Wuhan, 430074 (China); Zheng Yanan, E-mail: tjuhust@gmail.com [Department of Electronic Science and Technology, Huazhong University of Science and Technology, Wuhan, 430074 (China); Gong Shuping; Shi Fei [Department of Electronic Science and Technology, Huazhong University of Science and Technology, Wuhan, 430074 (China)

    2011-06-15

    Electrophoretic deposition was utilized for preparation of BaTiO{sub 3}/CoFe{sub 2}O{sub 4} multiferroic composite thick films on indium-tin oxide substrates. The suspensions for electrophoretic experiments were prepared by dispersing BaTiO{sub 3} and CoFe{sub 2}O{sub 4} nanoparticles with different molar ratios into solvents composed of ethanol and acetylacetone. Polyvinyl butyral was added to the suspensions in order to enhance the adhesion and strength of deposit and prevent cracking. The zeta potential values of BaTiO{sub 3}/CoFe{sub 2}O{sub 4} suspensions were measured to be 26.4-36.9 mV. The experiment results showed that deposited films were obtained only when the applied electric field was larger than a certain critical value. XRD and SEM analysis depicted the presence of constituent phases in composite films. The percolation threshold of composite films was improved through dispersing ferromagnetic phase into ferroelectric phase. Therefore, the ferroelectric properties of composite thick films were maintained when the ferromagnetic properties were enhanced significantly with increasing CFO content.

  7. Electrophoretic deposition of BaTiO 3/CoFe 2O 4 multiferroic composite films

    Science.gov (United States)

    Zhou, Dongxiang; Jian, Gang; Zheng, Yanan; Gong, Shuping; Shi, Fei

    2011-06-01

    Electrophoretic deposition was utilized for preparation of BaTiO 3/CoFe 2O 4 multiferroic composite thick films on indium-tin oxide substrates. The suspensions for electrophoretic experiments were prepared by dispersing BaTiO 3 and CoFe 2O 4 nanoparticles with different molar ratios into solvents composed of ethanol and acetylacetone. Polyvinyl butyral was added to the suspensions in order to enhance the adhesion and strength of deposit and prevent cracking. The zeta potential values of BaTiO 3/CoFe 2O 4 suspensions were measured to be 26.4-36.9 mV. The experiment results showed that deposited films were obtained only when the applied electric field was larger than a certain critical value. XRD and SEM analysis depicted the presence of constituent phases in composite films. The percolation threshold of composite films was improved through dispersing ferromagnetic phase into ferroelectric phase. Therefore, the ferroelectric properties of composite thick films were maintained when the ferromagnetic properties were enhanced significantly with increasing CFO content.

  8. Novel composite Zr/PBI-O-PhT membranes for HT-PEFC applications

    Directory of Open Access Journals (Sweden)

    Mikhail S. Kondratenko

    2013-08-01

    Full Text Available Novel composite membranes for high temperature polymer-electrolyte fuel cells (HT-PEFC based on a poly[oxy-3,3-bis(4′-benzimidazol-2″-ylphenylphtalide-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(acac4 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.

  9. 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.

  10. 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.

  11. 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

    2017-03-17

    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.

  12. Mangiferin loaded magnetic PCEC microspheres: preparation, characterization and antitumor activity studies in vitro.

    Science.gov (United States)

    Xiao, WenJing; Hou, Jun; Ma, Jie; Yu, BoTao; Ren, JianDong; Jin, WeiHua; Wu, Juan; Zheng, DeZhi; Fan, KaiHua

    2014-09-30

    Mangiferin is a promising effective chemopreventive agent against various tumors. However, its clinical use is limited by poor water solubility and low bioavailability. In this article, mangiferin loaded magnetic PCEC microspheres (MG-MS) were designed, characterized and the antitumor activity of MG-MS was evaluated in vitro. The magnetic nanoparticles (MNP) were synthesized via the high-temperature reaction of iron acetylacetonate in phenyl ether in the presence of oleic acid and oleylamine. Poly (ε-caprolactone)-poly (ethyleneglycol)-poly (ε-caprolactone) (PCL-PEG-PCL, PCEC) copolymers were formed by ring-opening copolymerization of ε-CL initiated by PEG-diol using Sn(Oct)2 as a catalyst and MG-MS were prepared by solvent diffusion method. MNP, PCEC copolymer, and MG-MS were characterized by GPC, TEM, XRD, FT-IR, (1)H-NMP and Malvern Laser Particle Sizer. Meanwhile, the antiproliferative activity in vitro and in vitro release behavior of this microspheres were studied in detail. The results indicate that the obtained magnetic microspheres might have great potential as an effective carrier for mangiferin used in cancer chemotherapy.

  13. Improved electrical, optical, and structural properties of undoped ZnO thin films grown by water-mist-assisted spray pyrolysis

    Energy Technology Data Exchange (ETDEWEB)

    Perez, L.Martinez [Centro de Investigacion en Ciencia Aplicada y Tecnologia Avanzada del Instituto Politecnico Nacional, Legaria 694, Col. Irrigacion, C.P. 11500 Mexico D.F. (Mexico); Unidad Profesional Interdisciplinaria en Ingenieria y Tecnologias Avanzadas del Instituto Politecnico Nacional, Av. IPN No. 2580, Col. Barrio La Laguna Ticoman, C.P. 07340 Mexico D.F. (Mexico); Aguilar-Frutis, M. [Centro de Investigacion en Ciencia Aplicada y Tecnologia Avanzada del Instituto Politecnico Nacional, Legaria 694, Col. Irrigacion, C.P. 11500 Mexico D.F. (Mexico); Zelaya-Angel, O. [Centro de Investigacion y de Estudios Avanzados del Instituto Politecnico Nacional, Av. IPN 2508, Col. San Pedro Zacatenco, 07000 Mexico D.F. (Mexico); Munoz Aguirre, N. [Instituto Mexicano del Petroleo, Eje Central Lazaro Cardenas no. 152, Col. San Bartolo Atepehuacan, 07730 Mexico D.F. (Mexico)

    2006-08-15

    Undoped ZnO thin films were prepared using the ultrasonic spray pyrolysis deposition technique with zinc acetylacetonate dissolved in N,N-dimethylformamide as the source materials solution. The addition of water mist in a parallel flux to the spray solution stream was also used during deposition of the films. The addition of water mist improved the electrical characteristics of the ZnO films. Fresh ZnO samples were then thermally annealed in a H{sub 2} reducing atmosphere. X-ray diffraction patterns show mainly the wurzite crystalline ZnO phase in the films. An electrical resistivity ({rho}) of around 2.7 x 10{sup -2} {omega}cm was measured at room temperature for the best undoped ZnO film. {rho} is approximately one order of magnitude lower than the resistivities found in undoped ZnO films obtained by means of similar non-vacuum deposition techniques. (copyright 2006 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  14. Phase- and morphology-controlled synthesis of cobalt sulfide nanocrystals and comparison of their catalytic activities for hydrogen evolution

    Science.gov (United States)

    Pan, Yuan; Liu, Yunqi; Liu, Chenguang

    2015-12-01

    Colalt sulfide nanocrystals (NCs), including dandelion-like Co9S8 and sphere-like Co3S4, have been synthesized via a thermal decomposition approach using cobalt acetylacetonate as the cobalt source, 1-dodecanethiol as the sulfur source and oleic acid or oleylamine as the high boiling organic solvent. It is found that the molar ratio of the Co:S precursor and the species of solvent play an important role in the control of phase and morphology of cobalt sulfide nanostructures. The phase structure and morphology of the as-synthesized nickel sulfide NCs are characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscope (SEM), energy dispersive spectrum (EDS) mapping, X-ray photoelectron spectroscopy (XPS) and N2 adsorption-desorption. Then we further compare the electrocatalytic activity and stability of as-synthesized cobalt sulfide NCs for hydrogen evolution reaction (HER). The results show that sphere-like Co3S4 exhibits better electrocatalytic activity than the dandelion-like Co9S8 NCs for HER, which can be attributed to the difference of phase structure and morphology. The sphere-like Co3S4 NCs have large surface area and high electrical conductivity, both are beneficial to enhance the catalytic activity. This study indicates that the crystalline phase structure and morphology of cobalt sulfide NCs are important for designing HER electrocatalysts with high efficiency and good stability.

  15. MOCVD of Cobalt Oxide Using Co-Actylacetonate As Precursor: Thin Film Deposition and Study of Physical Properties

    Directory of Open Access Journals (Sweden)

    S.M. Jogade

    2011-01-01

    Full Text Available Metal Organic Chemical Vapor Deposition (MOCVD is the deposition method of choice for achieving conformal uniform (composition and thickness continuous thin films over the micron geometry topology necessary for implementing advanced devices. Thin films of cobalt oxide were prepared by MOCVD technique on alumina substrate using a cobalt acetylacetonate as precursor. The thin films of cobalt oxide were deposited on alumina substrate by MOCVD at four different temperatures viz 490 °C, 515 °C, 535 °C, 565 °C. The as deposited samples are uniform and well adherent to the substrate. Thickness of the cobalt oxide film is maximum at temperature 535 °C. The crystalline and phase composition of films were examined by X-ray diffraction. The XRD reveals the crystalline nature with cubic in structure for all the samples. The surface morphology of the films were studied by scanning electron microscopy. The SEM image shows well defined closely packed grains for all the samples. The hexagonal shape of grains are observed for sample at temperature 515 °C. Raman spectroscopy shows Fm3m, 225 space groups for cobalt oxide thin films deposited on alumina substrate.

  16. Unconventional Synthesis of γ-Fe2O3: Excellent Low-Concentration Ethanol Sensing Performance

    Science.gov (United States)

    Naskar, Atanu; Narjinary, Mousumi; Kundu, Susmita

    2017-01-01

    This study reports on a simple unconventional procedure for synthesis of γ-Fe2O3 nanopowder and its fabrication as a resistive ethanol sensor. γ-Fe2O3 powder having an average particle size of ˜15 nm was prepared by thermal decomposition of iron(III) acetylacetonate. Platinum incorporation (0.5-1.5 wt.%) was also carried out for enhancing sensing performance. The powders were characterized using an x-ray diffractometer, x-ray photoelectron spectroscopy, Brunauer-Emmett-Teller surface area, field area scanning electron microscopy, transmission electron microscopy along with energy dispersion x-ray analyses. Sensor fabricated from pure γ-Fe2O3 exhibited excellent ethanol sensing performance at concentrations down to 1 ppm, having a great demand in medical diagnosis and food-processing industries. The response observed for pure γ-Fe2O3 (˜75% for 1 ppm ethanol) was enhanced ˜10% after 1 wt.% Pt impregnation. Sensors were quite stable and selective towards ethanol vapour detection. A possible mechanism for high sensing performance has been discussed.

  17. Microspheres of polyester loaded with Holmium-165: effect of gamma irradiation on the polymeric structure

    Energy Technology Data Exchange (ETDEWEB)

    Azevedo, Mariangela de Burgos M. de; Pires, Geovanna; Lira, Rafael A. de; Geraldes, Adriana N.; Nascimento, Nanci; Melo, Vitor Hugo Soares de, E-mail: mbmazevedo@ipen.br [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil); Kodama, Yasko [Instituto de Pesquisas Energeticas e Nucleares (IPEN/CNEN-SP), Sao Paulo, SP (Brazil). Centro de Biotecnologia

    2011-07-01

    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)

  18. Synthesis of Bridged Bis(β-ketoiminate) compounds%桥联的双β-酮亚胺化合物的合成

    Institute of Scientific and Technical Information of China (English)

    谢光勇; 徐晓航; 李龙; 刘公毅; 张爱清

    2013-01-01

      对二甲苯与N-溴代丁二酰亚胺反应合成对二溴甲基苯,后者与乙酰丙酮反应合成1,4-二(2',2'-二乙酰基乙烷基)苯,再与取代苯胺反应,较高收率合成了5种新型的苯二亚甲基桥联的双β-酮亚胺化合物;并通过1H NMR、IR和元素分析对产物进行了表征。%Five novel xylylene-bridged bis (β-ketoiminate ) compounds were synthesized with high yields by substituted anilines reacted with 1, 4-( 2′, 2′-acetonyethyl ) benzene which was synthesized with acetylacetone and p-dibromomethylbenzene prepared with p-Xylene and NBS. All the title compounds reported were characterized by 1 H NMR, IR and elemental analysis.

  19. 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.

  20. Production and characterization of 166Ho polylactic acid microspheres.

    Science.gov (United States)

    Yavari, Kamal; Yeganeh, Ehsan; Abolghasemi, Hossein

    2016-01-01

    Microsphere and particle technology with selective transport of radiation represents a new generation of therapeutics. Poly-L-lactic acid (PLLA) microspheres loaded with holmium-166 acetylacetonate ((166)Ho-PLLA-MS) are novel microdevices. In this research, (165)HoAcAc-PLLA microparticles were prepared by the solvent evaporation technique. Microspheres were irradiated at Tehran Research Reactor. The diameter and surface morphologies were characterized by particle sizer and scanning electron microscopy before and after irradiation. The complex stability, radiochemical purity, and in vivo biodistribiotion were checked in the final solution up to 3 days. In this study, (166)Ho-PLLA spherical particles with a smooth surface and diameter of 20-40 µm were obtained, which were stable in vitro and in vivo studies. Neutron irradiation did not damage the particles. The ease with which the PLLA spheres could be made in the optimal size range for later irradiation and their ability to retain the (166)Ho provided good evidence for their potential use in radioembolization.

  1. Pt-free carbon-based fuel cell catalyst prepared from spherical polyimide for enhanced oxygen diffusion

    Science.gov (United States)

    Nabae, Yuta; Nagata, Shinsuke; Hayakawa, Teruaki; Niwa, Hideharu; Harada, Yoshihisa; Oshima, Masaharu; Isoda, Ayano; Matsunaga, Atsushi; Tanaka, Kazuhisa; Aoki, Tsutomu

    2016-03-01

    The development of a non-precious metal (NPM) fuel cell catalyst is extremely important to achieve globalization of polymer electrolyte fuel cells due to the cost and scarcity of platinum. Here, we report on a NPM cathode catalyst prepared by the pyrolysis of spherical polyimide nanoparticles that contain small amounts of Fe additive. 60 nm diameter Fe-containing polyimide nanoparticles were successfully synthesized by the precipitation polymerization of pyromellitic acid dianhydride and 1,3,5-tris(4-aminophenyl)benzene with Fe(acac)3 (acac = acetylacetonate) as an additive. The particles were subsequently carbonized by multistep pyrolysis to obtain the NPM catalyst while retaining the small particle size. The catalyst has good performance and promising durability for fuel cell applications. The fuel cell performance under a 0.2 MPa air atmosphere at 80 °C of 1.0 A cm‑2 at 0.46 V is especially remarkable and better than that previously reported.

  2. 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)

  3. 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)

  4. 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.

  5. Determination of acidity constants of enolisable compounds by capillary electrophoresis.

    Science.gov (United States)

    Mofaddel, N; Bar, N; Villemin, D; Desbène, P L

    2004-10-01

    Research on the structure-activity relationships of molecules with acidic carbon atoms led us to undertake a feasibility study on the determination of their acidity constants by capillary electrophoresis (CE). The studied molecules had diverse structures and were tetronic acid, acetylacetone, diethylmalonate, Meldrum's acid, 3-methylrhodanine, nitroacetic acid ethyl ester, pyrimidine-2,4,6-trione, 3-oxo-3-phenylpropionic acid ethyl ester, 1-phenylbutan-1,3-dione, 5,5-dimethylcyclohexan-1,3-dione and homophthalic anhydride. The p Ka range explored by CE was therefore very large (from 3 to 12) and p Ka values near 12 were evaluated by mathematical extrapolations. The analyses were carried out in CZE mode using a fused silica capillary grafted (or not) with hexadimethrine. Owing to the electrophoretic behaviour of these compounds according to the pH, their acidity constants could be evaluated and appeared in perfect agreement with the literature data obtained, a few decades ago, by means of potentiometry, spectrometry or conductimetry. The p Ka of homophthalic anhydride and 3-methylrhodanine were evaluated for the first time.

  6. Synthesis, structure characterization and biological activity of selected metal complexes of sulfonamide Schiff base as a primary ligand and some mixed ligand complexes with glycine as a secondary ligand

    Science.gov (United States)

    Sharaby, Carmen M.; Amine, Mona F.; Hamed, Asmaa A.

    2017-04-01

    The current work reports synthesis of metal complexes and mixed ligand complexes of a novel sulfonamide Schiff base ligand (HL) resulted from the condensation of sulfametrole [N‧-(4-methoxy-1,2,5-thiadiazol-3-yl]sulfanilamide and acetyl-acetone as a primary ligand and glycine as a secondary ligand. The metal complexes and mixed ligand complexes of HL Schiff base ligand were synthesized and characterized using different physicochemical studies as elemental analyses, mass spectra, conductivity measurement, IR spectra, 1H NMR spectra, UV-vis Spectra, solid reflectance, magnetic susceptibility, thermal analyses (TGA and DTA) and their microbial and anticancer activities. The spectroscopic data of the complexes suggest their 1:2(L1:M) complex structures and 1:2:2(L1:L2:M) mixed ligand complex structures, where L1 = HL and L2 = glycine. Also, the spectroscopic studies suggested the octahedral structure for all complexes. The synthesized Schiff base, its metal and mixed ligand complexes were screened for their bacterial, antifungal and anticancer activity. The activity data show that the metal complexes and mixed ligand complexes exhibited promising microbial and anticancer activities than their parent HL Schiff base ligand, also the data show that the mixed ligand complexes more effective than the metal complexes.

  7. A facile microwave synthetic route for ferrite nanoparticles with direct impact in magnetic particle hyperthermia.

    Science.gov (United States)

    Makridis, A; Chatzitheodorou, I; Topouridou, K; Yavropoulou, M P; Angelakeris, M; Dendrinou-Samara, C

    2016-06-01

    The application of ferrite magnetic nanoparticles (MNPs) in medicine finds its rapidly developing emphasis on heating mediators for magnetic hyperthermia, the ever-promising "fourth leg" of cancer treatment. Usage of MNPs depends largely on the preparation processes to select optimal conditions and effective routes to finely tailor MNPs. Microwave heating, instead of conventional heating offers nanocrystals at significantly enhanced rate and yield. In this work, a facile mass-production microwave hydrothermal synthetic approach was used to synthesize stable ferromagnetic manganese and cobalt ferrite nanoparticles with sizes smaller than 14 nm from metal acetylacetonates in the presence of octadecylamine. Prolonging the reaction time from 15 to 60 min, led to ferrites with improved crystallinity while the sizes are slight increased. The high crystallinity magnetic nanoparticles showed exceptional magnetic heating parameters. In vitro application was performed using the human osteosarcoma cell line Saos-2 incubated with manganese ferrite nanoparticles. Hyperthermia applied in a two cycle process, while AC magnetic field remained on until the upper limit of 45 °C was achieved. The comparative results of the AC hyperthermia efficiency of ferrite nanoparticles in combination with the in vitro study coincide with the magnetic features and their tunability may be further exploited for AC magnetic hyperthermia driven applications.

  8. A zeolite-supported molecular ruthenium complex with eta6-C6H6 ligands: chemistry elucidated by using spectroscopy and density functional theory.

    Science.gov (United States)

    Ogino, Isao; Chen, Mingyang; Dyer, Jason; Kletnieks, Philip W; Haw, James F; Dixon, David A; Gates, Bruce C

    2010-07-05

    An essentially molecular ruthenium-benzene complex anchored at the aluminum sites of dealuminated zeolite Y was formed by treating a zeolite-supported mononuclear ruthenium complex, [Ru(acac)(eta(2)-C(2)H(4))(2)](+) (acac=acetylacetonate, C(5)H(7)O(2)(-)), with (13)C(6)H(6) at 413 K. IR, (13)C NMR, and extended X-ray absorption fine structure (EXAFS) spectra of the sample reveal the replacement of two ethene ligands and one acac ligand in the original complex with one (13)C(6)H(6) ligand and the formation of adsorbed protonated acac (Hacac). The EXAFS results indicate that the supported [Ru(eta(6)-C(6)H(6))](2+) incorporates an oxygen atom of the support to balance the charge, being bonded to the zeolite through three Ru-O bonds. The supported ruthenium-benzene complex is analogous to complexes with polyoxometalate ligands, consistent with the high structural uniformity of the zeolite-supported species, which led to good agreement between the spectra and calculations at the density functional theory level. The calculations show that the interaction of the zeolite with the Hacac formed on treatment of the original complex with (13)C(6)H(6) drives the reaction to form the ruthenium-benzene complex.

  9. 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.)

  10. Rapid synthesis of novel flowerlike K0.46Mn2O4(H2O)1.4 hierarchical architectures and their catalytic degradation of formaldehyde in aqueous solution

    Science.gov (United States)

    Ahmed, Khalid Abdelazez Mohamed; Huang, Kaixun

    2014-04-01

    Novel flower-like birnessite type manganese oxide hierarchical architectures were hydrothermally synthesized from KMnO4 solution using sodium fluorite as a reductant in sulfuric acid medium at low temperature. X-ray diffraction (XRD), Fourier transform infrared (FT-IR) and X-ray photoelectron (XPS) spectroscopes confirm that the composition of the as-fabricated product. Field emission scanning electron microscopy (FE-SEM), transmission electron microscopy (TEM), selected area electron diffraction (SA-ED), high resolution transmission electron microscopy (HR-TEM) and N2 adsorption-desorption isotherm reveal that the as-synthesized sample exhibits a microsized flower-like crystal with dense nanoleaves standing on their surfaces, polycrystalline, monoclinic phase structure and high BET surface area. On the basis of time-dependent experimental results, a possible mechanism for the formation of flowerlike structures is speculated. Their capability of catalytic degradation of formaldehyde solution with oxygen air bubbles were studied by using an acetylacetone calorimetric spectra, total organic carbon (TOC) method and turnover number (TON). In addition, the birnessite nanoflower is stable during the reaction and can be used repeatedly.

  11. Sol-gel based sensor for selective formaldehyde determination.

    Science.gov (United States)

    Bunkoed, Opas; Davis, Frank; Kanatharana, Proespichaya; Thavarungkul, Panote; Higson, Séamus P J

    2010-02-01

    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 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.

  12. Separation and quantitation of methenamine in urine by ion-pair extraction.

    Science.gov (United States)

    Strom, J G; Jun, H W

    1986-04-01

    An ion-pair extraction technique is described for separating methenamine, a urinary tract antibacterial agent, from formaldehyde in human urine samples. Separation conditions are developed from extraction constants for the methenamine-bromocresol green ion-pair. The technique involves adsorption of the ion-pair onto a silica cartridge and elution with methylene chloride:1-pentanol (95:5). Methenamine is freed from the ion-pair by the addition of excess tetrabutylammonium iodide and converted to formaldehyde (determined spectrophotometrically) by reaction with ammonia and acetylacetone. Linear standard plots were obtained from urine containing methenamine which was diluted to 10-160 micrograms/mL. The lower limit of detection was 6 micrograms/mL of methenamine. Absolute recovery from urine was greater than or equal to 94.5%. The precision (CV) of detection of methenamine in the presence of formaldehyde was less than 2%, and less than or equal to 4.5% for the detection of formaldehyde in the presence of methenamine. No interferences were noted. The applicability of the method was demonstrated by analysis of human urine levels of both methenamine and formaldehyde following oral administration of a methenamine salt to a volunteer.

  13. High capacity magnetic mesoporous carbon-cobalt composite adsorbents for removal of methylene green from aqueous solutions.

    Science.gov (United States)

    Dai, Mingzhi; Vogt, Bryan D

    2012-12-01

    Mesoporous carbons containing cobalt nanoparticles are synthesized by tri-or quad-constituent self assembly of Pluronic F127, phenol-formaldehyde oligomer (resol), cobalt acetylacetonate (acac), and optionally tetraethyl orthosilicate (TEOS, optional). Upon pyrolysis in N(2) atmosphere, the resol provides sufficient carbon yield to maintain the ordered structure, while decomposition of the Co(acac) yields cobalt nanoparticles. To provide increased surface area, the dispersed silicate from condensation of TEOS can be etched after carbonization to yield micropores, Without silica templated micropores, the surface area decreases as the cobalt content increases, but there is a concurrent increase in the volume-average pore diameter (BHJ) and a dramatic increase in the adsorption capacity of methylene green with the equilibrium adsorption capacity from 2 to 90 mg/g with increasing Co content. Moreover, the surface area and pore size of mesoporous composites can be dramatically increased by addition of TEOS and subsequent etching. These composites exhibit extremely high adsorption capacity up to 1151 mg/g, which also increases with increases in the Co content. Additionally, the inclusion of cobalt nanoparticles provides magnetic separation from aqueous suspension. The in situ synthesis of the Co nanoparticles yields to a carbon shell that can partially protect the Co from leaching in acidic media; after 96 h in 2 M HCl, the powders remain magnetic.

  14. Synthesis of porous carbon nanofiber with bamboo-like carbon nanofiber branches by one-step carbonization process

    Science.gov (United States)

    Yoo, Seung Hwa; Joh, Han-Ik; Lee, Sungho

    2017-04-01

    Porous carbon nanofibers (PCNFs) with CNF branches (PCNF/bCNF) were synthesized by a simple heat treatment method. Conventional methods to synthesize this unique structure usually follow a typical route, which consists of CNF preparation, catalyst deposition, and secondary CNF growth. In contrast, our method utilized a one-step carbonization process of polymer nanofibers, which were electrospun from a one-pot solution consisted of polyacrylonitrile, polystyrene (PS), and iron acetylacetonate. Various structures of PCNF/CNF were synthesized by changing the solution composition and molecular weight of PS. It was verified that the content and molecular weight of PS were critical for the growth of catalyst particles and subsequent growth of CNF branches. The morphology, phase of catalyst, and carbon structure of PCNF/bCNF were analyzed at different temperature steps during carbonization. It was found that pores were generated by the evaporation of PS and the catalyst particles were formed on the surface of PCNF at 700 °C. The gases originated from the evaporation of PS acted as a carbon source for the growth of CNF branches that started at 900 °C. Finally, when the carbonization process was finished at 1200 °C, uniform and abundant CNF branches were formed on the surface of PCNF.

  15. Synthesis, spectroscopic characterization, electrochemical behaviour and thermal decomposition studies of some transition metal complexes with an azo derivative

    Science.gov (United States)

    Sujamol, M. S.; Athira, C. J.; Sindhu, Y.; Mohanan, K.

    2010-01-01

    Complexes of manganese(II), cobalt(II), nickel(II), copper(II) and zinc(II) with a novel heterocyclic azo derivative, formed by coupling diazotized 2-amino-3-carbethoxy-4,5-dimethylthiophene with acetylacetone were synthesized and characterized on the basis of elemental analyses, molar conductance, magnetic susceptibility measurements, UV-vis, IR, 1H NMR and EPR spectral data. Spectral studies revealed that the ligand existed in an internally hydrogen bonded azo-enol form rather than the keto-hydrazone form and coordinated to the metal ion in a tridentate fashion. Analytical data revealed that all the complexes exhibited 1:1 metal-ligand ratio. On the basis of electronic spectral data and magnetic susceptibility measurements, suitable geometry was proposed for each complex. The nickel(II) complex has undergone facile transesterification reaction when refluxed in methanol for a long period. The ligand and the copper(II) complex were subjected to X-ray diffraction study. The electrochemical behaviour of copper(II) complex was investigated by cyclic voltammetry. The thermal behaviour of the same complex was also examined by thermogravimetry.

  16. Analysis and pollution sources speculations of toxic gases in a secondary fiber paper mill.

    Science.gov (United States)

    Tong, Xin; Liu, Zhang; Chen, Xiao Q; Shen, Wen H

    2016-11-09

    This paper quantitatively investigates the compositions of the gaseous pollutants in the ambient air of a secondary fiber paper mill. Total volatile organic compounds (TVOC), formaldehyde (HCHO), sulfur compounds (H2S), and hydrocarbon compounds (CxHy) were analyzed on six sampling sites with photo-ionisation detector, acetylacetone spectrophotometric method, and gas detector. The results revealed that, the high levels of TVOC and CxHy were detected at the wet end of paper machine and the office area, respectively; all the H2S contents on the six sites exceeded the limit (0.06 mg m(-3)) seriously; the HCHO concentrations at other five sites were out of the limit (0.10 mg m(-3)) except for the wastewater treatment plant. Furthermore, the necessary discussions about the possible pollution sources were considered on the process flow, the chemical agents used, and the ambient conditions in the paper mill. For the sake of air pollution control in paper mills, these remarkable results and analysis lay some technical basis in the following researches that should attract more attentions.

  17. Synthesis and characterization of phosphorescent platinum complexes containing phenylpyridazine

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Sang Jin; Kang, Seok; Lee, Seung Hee; Hwang, Kwang Jin; Park, Noh Kil; Kim, Young Sik

    2004-01-05

    Synthesis and characterization of a series of square planar Pt(II)-phenylpyridazine complexes are reported. The complexes have the general structure of (C-N)Pt(O-O), where HC-N is 3-phenyl-pyridazine (ppdz), 3-(3'-trifluoromethylphenyl)pyridazine (3'tfmppdz), 3-(3'-methoxyphenyl)-pyridazine (3'meoppdz), 3-(4'-methoxyphenyl)pyridazine (4'meoppdz), or 3-phenyl-6-chloro-pyridazine (6Clppdz) and HO-O is acetylacetone (Hacac). Reaction of K{sub 2}PtCl{sub 4} with a HC-N ligand forms the dimer, (C-N)Pt({mu}-Cl){sub 2}Pt(C-N), which is cleaved with Hacac to give the corresponding monomer, (C-N)Pt(O-O). The emission characteristics of these complexes are governed by the substituents of the cyclometalating ligands, showing emission {lambda}{sub max} values from 508 to 610 nm. Strong spin-orbit coupling of the platinum atom allows for the formally forbidden mixing of the {sup 1}MLCT with the {sup 3}MCLT and {sup 3}({pi}-{pi}*) states.

  18. Preparation of magnetic carbon nanotubes with hierarchical copper silicate nanostructure for efficient adsorption and removal of hemoglobin

    Science.gov (United States)

    Zhang, Min; Wang, Yongtao; Zhang, Yanwei; Ding, Lei; Zheng, Jing; Xu, Jingli

    2016-07-01

    The controllable synthesis of materials with the desired structure and dimensionality is of great significance in material science. In this work, the hierarchical CNTs/Fe3O4@copper silicate (CNTs/Fe3O4@CuSilicate) composites were synthesized via a simple chemical conversion route by using CNTs/Fe3O4@SiO2 nanocables as template. Firstly, magnetic CNTs composites (CNTs/Fe3O4) were synthesized by the high temperature decomposition process using the iron acetylacetonate as raw materials. Then a layer of SiO2 can be easily coated on the magnetic CNTs by the stöber method, which were then converted into CNTs/Fe3O4@CuSilicate composites by hydrothermal reaction between the silica shell and copper ions in alkaline solution. The resulting CNTs/Fe3O4@CuSilicate composites hold merits such as magnetic responsivity, good dispersibility, and large specific surface area. Moreover, the CNTs/Fe3O4@copper silicate composites have strong affinity toward bovine hemoglobin (BHb), which were successfully applied to convenient, efficient, and fast removal of abundant proteins (HHb and HSA) in human blood.

  19. I mproved Synthesis of 1 H, 4 H -3,6-dinitropyrazolo [ 4,3-C ] pyrazole%3,6-二硝基吡唑[4,3-c]并吡唑的合成工艺改进

    Institute of Scientific and Technical Information of China (English)

    易文斌; 朱春琳; 王金星; 张怡; 蔡春

    2011-01-01

    1 H,4H-3,6-dinitropyrazolo [4,3-C] pyrazole (DNPP) was synthesized from acetylacetone via monocyclization,diazotization, bicyclization, nitration, oxidation, and decarboxylative nitration. The overall yield of DNPP was 11.3% and 4%higher than that reported before. The synthesis of 4-amino-3,5-dimethylpyrazole was carried out by one-pot method which shows a number of advantages in comparison with the procedure adapted in the literature, including eliminating the use of mixture acid and iron power, shorting the reaction time (from 72 h to 24 h), improving the yield (from 79.1% to 92.0% ), and simplifying the post-treatment. In addition, both nitration and decarboxylative nitration were studied.%3,6-二硝基吡唑[4,3-c]并吡唑(DNPP),是一种新型氮杂环含能材料.以乙酰丙酮为原料,经环化、重氮化、双环构建、硝化、氧化、脱羧硝化等反应合成了DNPP,得率为1 3.3%,比文献值提高了4%.考察了一锅法制备中间体4-氨基-3,5-二甲基吡唑的合成工艺、硝化工艺和脱羧硝化工艺.

  20. Examples of UV-Vis profiles use as tool for evidence of the metallophthalocyanines transformation

    Science.gov (United States)

    Kubiak, Ryszard; Dyrda, Gabriela; Ejsmont, Krzysztof

    2017-02-01

    The UV-Vis spectra for a set of MPcs (Mmetal, Pc = phthalocyanine ligand), i.e.: In(III)PcI (1), Hf(IV)PcI2Pht (Pht = phthalonitrile) (2), Sn(II)Pc (3), Sn(IV)PcI2(4), and Ge(IV)PcI2(5) have been examined in two solvents, O-donative acetylacetone, and non-coordinative benzene. The UV-Vis spectra in Hacac solution of 1,2 and 4,5 shows that the axially ligated iodine atoms are replaced by (acac)- anions of the solvent, whereas in 3 the oxygen donors of the solvent causing the auto-oxidation of Sn(II) to Sn(IV) ions and as a result the Sn(II)Pc is transformed into the Sn(IV)Pc(acac)2. The chloride complexes of the 1-5 compounds are formed at Hacac solution after acidification by hydrochloric acid, however each compound solution behaviors specifically. The UV-Vis spectra collected for the studied compounds at benzene solvent both before and after the solution acidization clearly indicate that the respective Q band character (besides 3) remains practically unchanged. The presence of the Cl- ions at the Sn(II)Pc solution in benzene results in the formation of Sn(IV)PcCl2.

  1. Electroless plating of ultrathin palladium films: self-initiated deposition and application in microreactor fabrication

    Science.gov (United States)

    Muench, Falk; Oezaslan, Mehtap; Svoboda, Ingrid; Ensinger, Wolfgang

    2015-10-01

    We present new electroless palladium plating reactions, which can be applied to complex-shaped substrates and lead to homogeneous, dense and conformal palladium films consisting of small nanoparticles. Notably, autocatalytic and surface-selective metal deposition could be achieved on a wide range of materials without sensitization and activation pretreatments. This provides a facile and competitive route to directly deposit well-defined palladium nanofilms on e.g. carbon, paper, polymers or glass substrates. The reactions proceed at mild conditions and are based on easily accessible chemicals (reducing agent: hydrazine; metal source: PdCl2; ligands: ethylenediaminetetraacetic acid (EDTA), acetylacetone). Additionally, the water-soluble capping agent 4-dimethylaminopyridine (DMAP) is employed to increase the bath stability, to ensure the formation of small particles and to improve the film conformity. The great potential of the outlined reactions for micro- and nanofabrication is demonstrated by coating an ion-track etched polycarbonate membrane with a uniform Pd film of approximately 20 nm thickness. The as-prepared membrane is then employed as a highly miniaturized flow reactor, using the reduction of 4-nitrophenol with NaBH4 as a model reaction.

  2. 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.

  3. Deposition and characterization of ZnO films using microplasma at atmospheric pressure

    Energy Technology Data Exchange (ETDEWEB)

    Thejaswini, H.C.; Agasanapura, B.; Hopwood, J., E-mail: hopwood@ece.tufts.edu

    2016-03-31

    Zinc oxide (ZnO) films were deposited on room-temperature Si(100) by microwave-induced microplasma at one atmosphere. The precursor used in this work was zinc acetylacetonate hydrate (Zn(acac){sub 2}{sup .}xH{sub 2}O) sublimed at 54 °C into flowing helium. The deposition rate was estimated to be 400 nm/min. The films were visually transparent and FTIR spectroscopy confirms the presence of the Zn-O stretching vibration at 410 cm{sup −1}. Raman spectroscopy reveals that the films have the 437 cm{sup −1} Raman band typical of a wurtzite crystal structure. Cross sectional scanning electron microscopy shows columnar growth with individual column widths of approximately 0.5 μm. Scale-up using arrays of microplasmas is considered. - Highlights: • ZnO thin films were deposited on silicon and KBr at atmospheric pressure • Cold microplasma dissociates Zn(acac){sub 2} precursor and removes organics • The growth temperature does not exceed 23 °C • Deposition rates of 400 nm/min • ZnO composition is verified by FTIR and Raman spectroscopy.

  4. Size and shape effects on magnetic properties of Ni nanoparticles

    Institute of Scientific and Technical Information of China (English)

    Xuemin He; Huigang Shi

    2012-01-01

    Pure Ni nanoparticles ranging in size from 24 to 200nm are prepared via thermal decomposition of nickel acetylacetonate in oleylamine.The as-prepared Ni particles change from spherical to dendritic or starlike with increasing precursor concentration.The particles are stable because the organic coating occurs in situ.Magnetic measurement reveals that all the Ni nanoparticles are ferromagnetic and show ferromagnetic-paramagnetic transitions at their Curie points.The saturation magnetization Ms is sizedependent,with a maximum value of 52.01 and 82.31 emu/g at room temperature and 5 K,respectively.The coercivity decreases at first and then increases with increasing particle size,which is attributed to the competition between size effect and shape anisotropy.The Curie temperature Tc is 593,612,622,626 and 627 K for the 24,50,96,165 and 200 nm Ni nanoparticles,respectively.A theoretical model is proposed to explain the size-dependence of Ni nanoparticle Curie temperature.

  5. Anion exchange membrane prepared from simultaneous polymerization and quaternization of 4-vinyl pyridine for non-aqueous vanadium redox flow battery applications

    Science.gov (United States)

    Maurya, Sandip; Shin, Sung-Hee; Sung, Ki-Won; Moon, Seung-Hyeon

    2014-06-01

    A simple, single step and environmentally friendly process is developed for the synthesis of anion exchange membrane (AEM) by simultaneous polymerization and quaternization, unlike the conventional membrane synthesis which consists of separate polymerization and quaternization step. The membrane synthesis is carried out by dissolving polyvinyl chloride (PVC) in cyclohexanone along with 4-vinyl pyridine (4VP) and 1,4-dibromobutane (DBB) in the presence of thermal initiator benzoyl peroxide, followed by film casting to get thin and flexible AEMs. The membrane properties such as ion exchange capacity, ionic conductivity and swelling behaviour are tuned by varying the degree of crosslinking. These AEMs exhibit low vanadium permeability, while retaining good dimensional and chemical stability in an electrolyte solution, making them appropriate candidates for non-aqueous vanadium acetylacetonate redox flow battery (VRFB) applications. The optimized membrane displays ion exchange capacity and ionic conductivity of 2.0 mequiv g-1 and 0.105 mS cm-1, respectively, whereas the efficiency of 91.7%, 95.7% and 87.7% for coulombic, voltage and energy parameter in non-aqueous VRFB, respectively. This study reveals that the non-aqueous VRFB performance is greatly influenced by membrane properties; therefore the optimal control over the membrane properties is advantageous for the improved performance.

  6. Increasing the energy density of the non-aqueous vanadium redox flow battery with the acetonitrile-1,3-dioxolane-dimethyl sulfoxide solvent mixture

    Science.gov (United States)

    Herr, T.; Fischer, P.; Tübke, J.; Pinkwart, K.; Elsner, P.

    2014-11-01

    Different solvent mixtures were investigated for non-aqueous vanadium acetylacetonate (V(acac)3) redox flow batteries with tetrabutylammonium hexafluorophosphate as the supporting electrolyte. The aim of this study was to increase the energy density of the non-aqueous redox flow battery. A mixture of acetonitrile, dimethyl sulfoxide and 1-3-dioxolane nearly doubles the solubility of the active species. The proposed electrolyte system was characterized by Raman and FT-IR spectroscopy, cyclic voltammetry, electrochemical impedance spectroscopy and charge-discharge set-up. Spectroscopic methods were applied to understand the interactions between the solvents used and their impact on the solubility. The potential difference between oxidation and reduction of V(acac)3 measured by cyclic voltammetry was about 2.2 V. Impedance spectroscopy showed an electrolyte resistance of about 2400 Ω cm2. Experiments in a charge-discharge test cell achieved coulombic and energy efficiencies of ∼95% and ∼27% respectively. The highest discharge power density was 0.25 mW cm-2.

  7. Trace level determination of beryllium in natural and flavored mineral waters after pre-concentration using activated carbon.

    Science.gov (United States)

    Kılınç, Ersin; Bakırdere, Sezgin; Yaman, Mehmet

    2011-04-01

    The concentrations of beryllium (Be) in natural and flavored mineral water samples were determined by flame atomic absorption spectrophotometer (FAAS) after pre-concentration based on the complexation of Be(+2) with a mixture of acetylacetone (pentane-2,4-dione) plus morin (3,5,7,2',4'-pentaoxyflavone) and adsorption on activated carbon. The adsorbed complex was eluted with 1.5 ml of 2.0 M HNO(3) and evaporated to dryness. After adding 1.5 ml of 2 M HNO(3) and centrifuging, Be in acid solution was determined by FAAS. To remove a number of metals present in water, EDTA was used as a chelating agent. Beryllium in mineral water samples was pre-concentrated by 500-fold, taking 750 ml as initial sample and 1.5 ml as the final volume. The relative standard deviations were sufficiently low for practical purposes and recoveries were up to 85%. Spiking experiments were performed in real samples to establish accuracy and recoveries. The limits of detection and quantification were 0.01 and 0.03 ng ml(-1), respectively. Twenty samples were analyzed for their beryllium content using optimum parameters. The highest concentration of beryllium was found to be 0.94 ± 0.15 ng ml(-1) in a natural mineral water, while beryllium was not detected in five samples.

  8. Structural characteristics of Al{sub 2}O{sub 3} thin films prepared by spray pyrolysis

    Energy Technology Data Exchange (ETDEWEB)

    Guzman-Mendoza, J.; Garcia-Hipolito, M. [Instituto de Investigaciones en Materiales, UNAM, Coyoacan, DF (Mexico); Posgrado en Tecnologia Avanzada, CICATA-IPN (Legaria), DF (Mexico); Aguilar-Frutis, M. [Centro de Investigacion en Ciencia Aplicada y Tecnologia Avanzada, CICATA-IPN (Legaria), DF (Mexico); Falcony-Guajardo, C. [Departamento de Fisica, CINVESTAV-IPN, DF (Mexico)

    2001-12-17

    The crystalline and structural characteristics of aluminium oxide (Al{sub 2}O{sub 3}) thin films deposited by ultrasonic spray pyrolysis have been analysed using conventional and high resolution transmission electron microscopy. The aluminium oxide films were deposited on silicon (100) wafers, using a solution of aluminium acetylacetonate in dimethylformamide. The films were deposited with and without the addition of water mist generated in parallel to the spraying solution. The substrate temperatures during deposition of the films were in the range of 500-650 deg. C. The results indicate that the thin films deposited without water mist have an amorphous structure, while those films deposited with the addition of water mist show a two-face nature, formed by small crystallites embedded in an amorphous matrix. The crystalline phase has been determined, through the indexing of the electron diffraction patterns. It is found that it corresponds to 5Al{sub 2}O{sub 3}{center_dot}H{sub 2}O in a Tohdite hexagonal structure with unit cell lattice constants a=5.575 A and c=8.76 A. (author). Letter-to-the-editor.

  9. One-step hydrothermal synthesis of highly water-soluble secondary structural Fe{sub 3}O{sub 4} nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Yang Xiwen [National Special Superfine Powder Engineering Research Center, Nanjing University of Science and Technology, Nanjing 210094 (China); Jiang Wei, E-mail: yangxw0610@yahoo.cn [National Special Superfine Powder Engineering Research Center, Nanjing University of Science and Technology, Nanjing 210094 (China); Liu Li; Chen Binghua; Wu Shixi; Sun Danping; Li Fengsheng [National Special Superfine Powder Engineering Research Center, Nanjing University of Science and Technology, Nanjing 210094 (China)

    2012-07-15

    Magnetite nanoparticles (MNPs) were prepared using the ferric acetylacetonate as the sole iron source in a facile hydrothermal route, while poly(acrylic acid) (PAA) was chosen as the stabilizer via one-step functionalized MNPs for better hydrophilic properties. The orthogonal was used in the paper for the experimental parameters optimization, including the solvent, the reaction time, the amount of stabilizer and the presynthesis. The obtained highly water dispersible MNPs with uniform size from about 50 to about 100 nm was individually composed of many monodisperse magnetite crystallites approximately 6 nm in size. And the MNPs show high magnetic properties, whose magnetite content was up to 76.76% and the saturation magnetization was 39.0 emu/g. Later the formation mechanism of MNPs was also discussed. Thus the MNPs proved to be very promising for biomedical applications. - Highlights: Black-Right-Pointing-Pointer MNPs are prepared in a low-temperature hydrothermal synthesis procedure. Black-Right-Pointing-Pointer Synthesis of MNPs is hybridized with their in situ surface functionalization. Black-Right-Pointing-Pointer Each of the secondary structural MNPs is composed of monodisperse primary particles. Black-Right-Pointing-Pointer The resulting MNPs show good magnetic properties combining that of primary one. Black-Right-Pointing-Pointer The size of MNPs is controllable and the mechanism is elaborated.

  10. Progammed synthesis of magnetic mesoporous silica coated carbon nanotubes for organic pollutant adsorption

    Science.gov (United States)

    Tong, Yue; Zhang, Min; Xia, Peixiong; Wang, Linlin; Zheng, Jing; Li, Weizhen; Xu, Jingli

    2016-05-01

    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, N2 adsorption-desorption and VSM. The well-designed mesoporous magnetic nanotubes had a large specific area, a highly open mesoporous structure and high magnetization. Firstly, SiO2-coated maghemite/CNTs nanoparticles (CNTs/Fe3O4@SiO2 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 SiO2, respectively. The CNTs/Fe3O4@SiO2 composites revealed a core-shell structure, Then, CNTs/Fe3O4@mSiO2 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.

  11. Secondary brown carbon formation via the dicarbonyl imine pathway: nitrogen heterocycle formation and synergistic effects.

    Science.gov (United States)

    Kampf, C J; Filippi, A; Zuth, C; Hoffmann, T; Opatz, T

    2016-07-21

    Dicarbonyls are known to be important precursors of so-called atmospheric brown carbon, significantly affecting aerosol optical properties and radiative forcing. In this systematic study we report the formation of light-absorbing nitrogen containing compounds from simple 1,2-, 1,3-, 1,4-, and 1,5-dicarbonyl + amine reactions. A combination of spectrophotometric and mass spectrometric techniques was used to characterize reaction products in solutions mimicking atmospheric particulates. Experiments with individual dicarbonyls and dicarbonyl mixtures in ammonium sulfate and glycine solutions demonstrate that nitrogen heterocycles are common structural motifs of brown carbon chromophores formed in such reaction systems. 1,4- and 1,5-dicarbonyl reaction systems, which were used as surrogates for terpene ozonolysis products, showed rapid formation of light-absorbing material and products with absorbance maxima at ∼450 nm. Synergistic effects on absorbance properties were observed in mixed (di-)carbonyl experiments, as indicated by the formation of a strong absorber in ammonium sulfate solutions containing acetaldehyde and acetylacetone. This cross-reaction oligomer shows an absorbance maximum at 385 nm, relevant for the actinic flux region of the atmosphere. This study demonstrates the complexity of secondary brown carbon formation via the imine pathway and highlights that cross-reactions with synergistic effects have to be considered an important pathway for atmospheric BrC formation.

  12. Metal-organic chemical vapour deposition of lithium manganese oxide thin films via single solid source precursor

    Directory of Open Access Journals (Sweden)

    Oyedotun K.O.

    2015-12-01

    Full Text Available Lithium manganese oxide thin films were deposited on sodalime glass substrates by metal organic chemical vapour deposition (MOCVD technique. The films were prepared by pyrolysis of lithium manganese acetylacetonate precursor at a temperature of 420 °C with a flow rate of 2.5 dm3/min for two-hour deposition period. Rutherford backscattering spectroscopy (RBS, UV-Vis spectrophotometry, X-ray diffraction (XRD spectroscopy, atomic force microscopy (AFM and van der Pauw four point probe method were used for characterizations of the film samples. RBS studies of the films revealed fair thickness of 1112.311 (1015 atoms/cm2 and effective stoichiometric relationship of Li0.47Mn0.27O0.26. The films exhibited relatively high transmission (50 % T in the visible and NIR range, with the bandgap energy of 2.55 eV. Broad and diffused X-ray diffraction patterns obtained showed that the film was amorphous in nature, while microstructural studies indicated dense and uniformly distributed layer across the substrate. Resistivity value of 4.9 Ω·cm was obtained for the thin film. Compared with Mn0.2O0.8 thin film, a significant lattice absorption edge shift was observed in the Li0.47Mn0.27O0.26 film.

  13. Thermal, spectroscopic, and solvent influence studies on mixed-ligand copper(II) complexes containing the bulky ligand: Bis[ N-( p-tolyl)imino]acenaphthene

    Science.gov (United States)

    El-Ayaan, Usama; Gabr, I. M.

    2007-05-01

    Four mixed-ligand copper(II) complexes containing the rigid bidentate nitrogen ligand bis[ N-( p-tolyl)imino]acenaphthene (abb. p-Tol-BIAN) ligand are reported. These complexes, namely [Cu( p-Tol-BIAN) 2](ClO 4) 21, [Cu( p-Tol-BIAN)(acac)](ClO 4) 2, [Cu( p-Tol-BIAN)Cl 2] 3 and [Cu( p-Tol-BIAN)(AcOH) 2](ClO 4) 24 (where acac, acetylacetonate and AcOH, acetic acid) have been prepared and characterized by elemental analysis, spectroscopic, magnetic and molar conductance measurements. ESR spectra suggest a square planar geometry for complexes 1 and 2. In complexes 3 and 4, a distorted tetrahedral arrangement around copper(II) centre was suggested. Solvatochromic behavior of all studied complexes indicates strong solvatochromism of their solutions. The observed solvatochromism is mainly due to the solute-solvent interaction between the chelate cation and the solvent molecules. Thermal properties and decomposition kinetics of all complexes are investigated. The kinetic parameters ( E, A, Δ H, Δ S and Δ G) of all thermal decomposition stages have been calculated using the Coats-Redfern and other standard equations.

  14. Synthesis, structural and solvent influence studies on solvatochromic mixed-ligand copper(II) complexes with the rigid nitrogen ligand: bis[ N-(2,4,6-trimethylphenyl)imino]acenaphthene

    Science.gov (United States)

    El-Ayaan, Usama; Murata, Fumiko; El-Derby, Soheir; Fukuda, Yutaka

    2004-04-01

    Three mixed-ligand copper (II) complexes containing the rigid bidentate nitrogen ligand bis[ N-(2,4,6-trimethylphenyl)imino]acenaphthene (abbr. 2,4,6-Me 3C 6H 2-BIAN) and β-diketonate (dike) ligands are reported and characterized. These complexes namely, [Cu(dike)(2,4,6-Me 3C 6H 2-BIAN)]ClO 4 {where dike=acac (acetylacetonate), bzac (benzoylacetonate) or (dibm) dibenzoylmethanate}have been synthesized and characterized by elemental analysis, spectroscopic, magnetic and molar conductance measurements. In addition to their high solubility in various organic solvents, these three complexes show a color change on going from one solvent to another, that is, strong solvatochromism of their solutions. The observed solvatochromism is mainly due to the solute-solvent interaction between the chelate cation and the solvent molecules. Reported also are the X-ray crystal structures of the free 2,4,6-Me 3C 6H 2-BIAN ligand and the [Cu(acac)(2,4,6-Me 3C 6H 2-BIAN)]ClO 4 complex.

  15. 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.

  16. Simultaneous observation of low temperature 4f-4f and 3d-3d emission spectra in a series of Cr(III)(ox)Ln(III) assembly

    CERN Document Server

    Subhan, M A; Suzuki, T; Choi, J H; Kaizaki, S

    2003-01-01

    We report here the low temperature emission spectra in the heterometal dinuclear 3d-4f assembled molecular system [(acac) sub 2 Cr sup I sup I sup I (mu-ox)Ln sup I sup I sup I (HBpz sub 3) sub 2] (Cr(ox)Ln:acac sup - =acetylacetonate, ox sup 2 sup - =oxalate, HBpz sub 3 sup - =hydrotris(pyrazol-1-yl)borate; Ln=La, Nd, Ho, Er , Tm and Yb) in comparison with those of Na[Cr(acac) sub 2 (ox)] and [(HBpz sub 3) sub 2 Ln(mu-ox)Ln(HBpz sub 3) sub 2](Ln=Nd and Er). From 10 to 150 K the Cr(ox)Ln complexes show a broad emission band around 800 nm from the sup 2 E state of Cr(III) moiety. At room temperature no sup 2 E- sup 4 A sub 2 emission was observed in the Cr(ox)Ln except for the La and Lu complexes. On warming from 10 to 300 K rapid quenching of the sup 2 E- sup 4 A sub 2 emission of Cr(III) is suggested to result from the energy transfer from Cr to Ln in the Cr(ox)Ln. The excitation spectra and the life-time were also measured with monitoring the 4f-4f emission peaks of the Cr(ox)Yb complex.

  17. Atmospheric Pressure Low Temperature Plasma System for Additive Manufacturing

    Science.gov (United States)

    Burnette, Matthew; Staack, David

    2016-09-01

    There is growing interest in using plasmas for additive manufacturing, however these methods use high temperature plasmas to melt the material. We have developed a novel technique of additive manufacturing using a low temperature dielectric barrier discharge (DBD) jet. The jet is attached to the head of a 3D printer to allow for precise control of the plasma's location. Various methods are employed to deposit the material, including using a vaporized precursor or depositing a liquid precursor directly onto the substrate or into the plasma via a nebulizer. Various materials can be deposited including metals (copper using copper (II) acetylacetonate), polymers (PMMA using the liquid monomer), and various hydrocarbon compounds (using alcohols or a 100% methane DBD jet). The rastering pattern for the 3D printer was modified for plasma deposition, since it was originally designed for thermoplastic extrusion. The design constraints for fill pattern selection for the plasma printer are influenced by substrate heating, deposition area, and precursor consumption. Depositions onto pressure and/or temperature sensitive substrates can be easily achieved. Deposition rates range up to 0.08 cm3/hr using tris(2-methoxyethoxy)(vinyl)silane, however optimization can still be done on the system to improve the deposition rate. For example higher concentration of precursor can be combined with faster motion and higher discharge powers to increase the deposition rate without overheating the substrate.

  18. 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.

  19. Hierarchical nanostructured NiCo2O4 as an efficient bifunctional non-precious metal catalyst for rechargeable zinc-air batteries

    Science.gov (United States)

    Prabu, Moni; Ketpang, Kriangsak; Shanmugam, Sangaraju

    2014-02-01

    A nickel-doped cobalt oxide spinel structure is a promising non-precious metal electrocatalyst for oxygen evolution and oxygen reduction in rechargeable metal-air batteries and water electrolyzers operating with alkaline electrolytes. One dimensional NiCo2O4 (NCO) nanostructures were prepared by using a simple electrospinning technique with two different metal precursors (metal nitrate/PAN and metal acetylacetonate/PAN). The effect of precursor concentration on the morphologies was investigated. Single-phase, NCO with an average diameter of 100 nm, porous interconnected fibrous morphology was revealed by FESEM and FETEM analysis. The hierarchical nanostructured 1D-spinel NiCo2O4 materials showed a remarkable electrocatalytic activity towards oxygen reduction and evolution in an aqueous alkaline medium. The extraordinary bi-functional catalytic activity towards both ORR and OER was observed by the low over potential (0.84 V), which is better than that of noble metal catalysts [Pt/C (1.16 V), Ru/C (1.01 V) and Ir/C (0.92 V)], making them promising cathode materials for metal-air batteries. Furthermore, the rechargeable zinc-air battery with NCO-A1 as a bifunctional electrocatalyst displays high activity and stability during battery discharge, charge, and cycling processes.A nickel-doped cobalt oxide spinel structure is a promising non-precious metal electrocatalyst for oxygen evolution and oxygen reduction in rechargeable metal-air batteries and water electrolyzers operating with alkaline electrolytes. One dimensional NiCo2O4 (NCO) nanostructures were prepared by using a simple electrospinning technique with two different metal precursors (metal nitrate/PAN and metal acetylacetonate/PAN). The effect of precursor concentration on the morphologies was investigated. Single-phase, NCO with an average diameter of 100 nm, porous interconnected fibrous morphology was revealed by FESEM and FETEM analysis. The hierarchical nanostructured 1D-spinel NiCo2O4 materials showed a

  20. 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

  1. 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

  2. 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

  3. Behavior of the potential antitumor V(IV)O complexes formed by flavonoid ligands. 3. Antioxidant properties and radical production capability.

    Science.gov (United States)

    Sanna, Daniele; Ugone, Valeria; Fadda, Angela; Micera, Giovanni; Garribba, Eugenio

    2016-08-01

    The radical production capability and the antioxidant properties of some V(IV)O complexes formed by flavonoid ligands were examined. In particular, the bis-chelated species of quercetin (que), [VO(que)2](2-), and morin (mor), [VO(mor)2], were evaluated for their capability to reduce the stable radical 1,1-diphenyl-2-picrylhydrazyl (DPPH) and produce the hydroxyl radical (•)OH by Fenton-like reactions, where the reducing agent is V(IV)O(2+). The results were compared with those displayed by other V(IV)O complexes, such as [VO(H2O)5](2+), [VO(acac)2] (acac=acetylacetonate) and [VO(cat)2](2-) (cat=catecholate). The capability of the V(IV)O flavonoids complexes to reduce DPPH is much larger than that of the V(IV)O species formed by non-antioxidant ligands and it is due mainly to the flavonoid molecule. Through the 5,5-dimethyl-1-pyrroline N-oxide (DMPO) spin trapping assay of the hydroxyl radical it was possible to demonstrate that in acidic solution V(IV)O(2+) has an effectiveness in producing (•)OH radicals comparable to that of Fe(2+). When V(IV)O complexes of flavonoids were taken into account, the amount of hydroxyl radicals produced in Fenton-like reactions depends on the specific structure of the ligand and on their capability to reduce H2O2 to give (•)OH. Both the formation of reactive oxygen species (ROS) under physiological conditions by V(IV)O complexes of flavonoid ligands and their radical scavenging capability can be put in relationship with their antitumor effectiveness and it could be possible to modulate these actions by changing the features of the flavonoid coordinated to the V(IV)O(2+) ion, such as the entity, nature and position of the substituents and the number of phenolic groups.

  4. A Facile Synthesis of MPd (M=Co, Cu) Nanoparticles and Their Catalysis for Formic Acid Oxidation

    Energy Technology Data Exchange (ETDEWEB)

    Mazumder, Vismadeb [Brown University; Chi, Miaofang [ORNL; Mankin, Max [Brown University; Liu, Yi [Brown University; Metin, Onder [Ataturk University; Sun, Daohua [Xiamen University, China; More, Karren Leslie [ORNL; Sun, Shouheng [Brown University

    2012-01-01

    Monodisperse CoPd nanoparticles (NPs) were synthesized and studied for catalytic formic acid (HCOOH) oxidation (FAO). The NPs were prepared by coreduction of Co(acac)2 (acac = acetylacetonate) and PdBr2 at 260 C in oleylamine and trioctylphosphine, and their sizes (5-12 nm) and compositions (Co10Pd90 to Co60Pd40) were controlled by heating ramp rate, metal salt concentration, or metal molar ratios. The 8 nm CoPd NPs were activated for HCOOH oxidation by a simple ethanol wash. In 0.1 M HClO4 and 2 M HCOOH solution, their catalytic activities followed the trend of Co50Pd50 > Co60Pd40 > Co10Pd90 > Pd. The Co50Pd50 NPs had an oxidation peak at 0.4 V with a peak current density of 774 A/gPd. As a comparison, commercial Pd catalysts showed an oxidation peak at 0.75 V with peak current density of only 254 A/gPd. The synthesis procedure could also be extended to prepare CuPd NPs when Co(acac)2 was replaced by Cu(ac)2 (ac = acetate) in an otherwise identical condition. The CuPd NPs were less active catalysts than CoPd or even Pd for FAO in HClO4 solution. The synthesis provides a general approach to Pd-based bimetallic NPs and will enable further investigation of Pd-based alloy NPs for electro-oxidation and other catalytic reactions.

  5. Highly Phosphorescent Iridium Complex for Organic Light Emitting Diodes%高效磷光铱配合物的合成及电致发光性能研究

    Institute of Scientific and Technical Information of China (English)

    李春香; 胡嘉伟; 孙培培; 潘毅; 郑建鸿

    2007-01-01

    合成了一种含苯并噻唑结构配体的环金属化铱配合物(ffbi)2Ir(acac),(其中ffbi为1-(4-氟苄基)-2-(4-氟苯基)苯并咪唑,acac 为乙酰丙酮),并以其作为发光体,制备了有机电致发光器件.结果表明该配合物具有强磷光发光特性,器件发绿色光.其中结构为TCTA(40nm)/CBP:Ir(6.3%,30nm)/BCP(10nm)/Alq(40nm)的电致发光器件在12V电压下最大发光亮度达41499 cd·m-2,在8V电压下,最大外量子效率达5.7%.%A bis-cyclometalated iridium complex(ffbi)2Ir(acac)(ffbi=l-(4-fluorobenzyl)-2-(4-fluorophenyl)benzimidazole,acac=acetylacetone)containing benzimidazole-based ligand has been synthesized and used as an emitter in organic light emitting diodes(OLEDs).The results showed that this complex had a strong phosphorescent character and the EL devices based on this complex emitted green light.For the device with the structure of TCTA(40nm)/CBP:Ir(6.3%,30nm)/BCP(10nm)/Alq(40nm),the maximum brightness reached 41499 cd·m-2 at a voltage of 12 V and the maximum external efficiency reached 5.7%at a voltage of 8 V.

  6. Thermal and sonochemical synthesis of porous (Ce,Zr)O2 mixed oxides from metal β-diketonate precursors and their catalytic activity in wet air oxidation process of formic acid.

    Science.gov (United States)

    Cau, Camille; Guari, Yannick; Chave, Tony; Larionova, Joulia; Nikitenko, Sergey I

    2014-07-01

    Porous (Ce0.5Zr0.5)O2 solid solutions were prepared by thermolysis (T=285 °C) or sonolysis (20 kHz, I=32 W cm(-2), Pac=0.46 W mL(-1), T=200 °C) of Ce(III) and Zr(IV) acetylacetonates in oleylamine or hexadecylamine under argon followed by heat treatment of the precipitates obtained in air at 450 °C. Transmission Electron Microscopy images of the samples show nanoparticles of ca. 4-6 nm for the two synthetic approaches. The powder X-ray diffraction, scanning electron microscopy, energy dispersive X-ray and μ-Raman spectroscopy of solids obtained after heat treatment indicate the formation of (Ce0.5Zr0.5)O2 solid solutions with a metastable tetragonal crystal structure for the two synthetic routes. The specific surface area of the samples varies between 78 and 149 m(2) g(-1) depending on synthesis conditions. The use of Barrett-Joyner-Halenda and t-plot methods reveal the formation of mixed oxides with a hybrid morphology that combines mesoporosity and microporosity regardless of the method of preparation. Platinum nanoparticles were deposited on the surface of the mixed oxides by sonochemical reduction of Pt(IV). It was found that the materials prepared by sonochemistry exhibit better resistance to dissolution during the deposition process of platinum. X-ray photoelectron spectroscopy analysis shows the presence of Pt(0) and Pt(II) on the surface of mixed oxides. Porous (Ce0.5Zr0.5)O2 mixed oxides loaded with 1.5%wt. platinum exhibit high activity in catalytic wet air oxidation of formic acid at 40 °C.

  7. Exploitation of pulsed flows for on-line dispersive liquid-liquid microextraction: Spectrophotometric determination of formaldehyde in milk.

    Science.gov (United States)

    Nascimento, Carina F; Brasil, Marcos A S; Costa, Susana P F; Pinto, Paula C A G; Saraiva, Maria Lúcia M F S; Rocha, Fábio R P

    2015-11-01

    Formaldehyde is often added to foods as a preservative, but it is highly toxic to humans, having been identified as a carcinogenic substance. It has also been used for the adulteration of milk in order to diminish the bacteria count and increase the shelf life of the product. Herein, we present a green dispersive liquid-liquid microextraction procedure in a flow-batch system for the determination of formaldehyde in milk. Pulsed flows were exploited for the first time to improve the dispersion of the extractant in the aqueous phase. The Hantzsch reaction was used for the derivatization of formaldehyde and the product was extracted with the ionic liquid (IL) trihexyltetradecylphosphonium chloride with methanol as the disperser. The flow-batch chamber was made of stainless steel with the facility for resistive heating to speed up the derivatization reaction. Spectrophotometric measurements were directly carried out in the organic phase using an optical fiber spectrophotometer. The limit of detection and coefficient of variation were 100 μg L(-1) and 3.1% (n=10), respectively, with a linear response from 0.5 to 5.0 mg L(-1), described by the equation A=0.088+0.116CF (mg L(-1)) in which A is absorbance and CF is formaldehyde concentration in mg L(-1). The estimated recoveries of formaldehyde from spiked milk samples ranged from 91% to 106% and the slopes of the analytical curves obtained with reference solutions in water or milk were in agreement, thus indicating the absence of matrix effects. Accuracy was demonstrated by the agreement of the results with those achieved by the reference fluorimetric procedure at the 95% confidence level. The proposed procedure allows for 10 extractions per hour, with minimized reagent consumption (120 μL of IL and 3.5 μL acetylacetone) and generation of only 6.7 mL waste per determination, which contribute to the eco-friendliness of the procedure.

  8. A new route for the synthesis of titanium silicalite-1

    Energy Technology Data Exchange (ETDEWEB)

    Vasile, Aurelia, E-mail: aurelia_vasile@yahoo.com [Laboratory of Materials Chemistry, Faculty of Chemistry, ' Al.I. Cuza' University of Iasi, B-dul Carol I, No. 11, 700506 Iasi (Romania); Busuioc-Tomoiaga, Alina Maria [Laboratory of Materials Chemistry, Faculty of Chemistry, ' Al.I. Cuza' University of Iasi, B-dul Carol I, No. 11, 700506 Iasi (Romania); Catalysis Research Department, ChemPerformance SRL, Iasi 700337 (Romania)

    2012-01-15

    Graphical abstract: Well-prepared TS-1 was synthesized by an innovative procedure using inexpensive reagents such as fumed silica and TPABr as structure-directing agent. This is the first time when highly crystalline TS-1 is obtained in basic medium, using sodium hydroxide as HO{sup -} ion source required for the crystallization process. Hydrolysis of titanium source has been prevented by titanium complexation with acetylacetone before structuring gel. Highlights: Black-Right-Pointing-Pointer TS-1 was obtained using cheap reagents as fumed silica and tetrapropylammonium bromide. Black-Right-Pointing-Pointer First time NaOH was used as source of OH{sup -} ions required for crystallization process. Black-Right-Pointing-Pointer The hydrolysis Ti alkoxides was controlled by Ti complexation with 2,4-pentanedione. -- Abstract: A new and efficient route using inexpensive reagents such as fumed silica and tetrapropylammonium bromide is proposed for the synthesis of titanium silicalite-1. High crystalline titanium silicalite-1 was obtained in alkaline medium, using sodium hydroxide as HO{sup -} ion source required for the crystallization process. Hydrolysis of titanium source with formation of insoluble oxide species was prevented by titanium complexation with before structuring gel. The final solids were fully characterized by powder X-ray diffraction, scanning electron microscopy, Fourier transform infrared, ultraviolet-visible diffuse reflectance, Raman and atomic absorption spectroscopies, as well as nitrogen sorption analysis. It was found that a molar ratio Ti:Si of about 0.04 in the initial reaction mixture is the upper limit to which well formed titanium silicalite-1 with channels free of crystalline or amorphous material can be obtained. Above this value, solids with MFI type structure containing both Ti isomorphously substituted in the network and extralattice anatase nanoparticles inside of channels is formed.

  9. 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.

  10. 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.

  11. 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.

  12. In vitro inhibitory effect of tetrahydrocurcuminoids on Fusarium proliferatum growth and fumonisin B₁ biosynthesis.

    Science.gov (United States)

    Coma, Véronique; Portes, Elise; Gardrat, Christian; Richard-Forget, Florence; Castellan, Alain

    2011-02-01

    Many plant pathogens produce toxic metabolites when growing on food and feed. Some antioxidative components seem to prevent fungal growth and mycotoxin formation. Recently, we synthesized a new class of powerful antioxidative compounds, i.e. tetrahydrocurcuminoids, and its structure/antioxidant activity relationships have been established. The South West of France produces large amounts of corn, which can be infected by Fusarium species, particularly F. proliferatum. In this context, the efficiency of tetrahydrocurcuminoids, which can be obtained from natural curcuminoids, was investigated to control in vitro the growth of F. proliferatum and the production of its associated mycotoxin, fumonisin B₁. The relation between structure and antifungal activity was studied. Tetrahydrocurcumin (THC1), with two guaiacyl phenolic subunits, showed the highest inhibitory activity (measured as radial growth on agar medium) against the F. proliferatum development (67% inhibition at a concentration of 13.6 µmol ml⁻¹). The efficiencies of THC2 (36% at a concentration of 11.5 µmol ml⁻¹), which contains syringyl phenolic units, and THC3 (30% at a concentration of 13.6 µmol ml⁻¹), which does not have any substituent on the aromatic rings, were relatively close. These results indicate that the simultaneous presence of guaiacyl phenols and the enolic function of the β-diketone moiety play an important role in the inhibition mechanisms. The importance of this combination was confirmed using n-propylguaiacol and acetylacetone as molecular models. Under the same conditions, ferulic acid and eugenol, other natural phenolic antioxidants, were less efficient in inhibiting fungal growth. THC1 also reduced fumonisin B₁ production in liquid medium by approximately 35, 50 and 75% at concentrations of 0.8, 1.3, and 1.9 µmol ml⁻¹, respectively. These very low inhibitory concentrations show that tetrahydrocurcuminoids could be one of the most promising biobased molecules for the

  13. Highly efficient electrophosphorescence devices based on iridium complexes with high efficiency over a wide range of current densities

    Energy Technology Data Exchange (ETDEWEB)

    Zhang Liying; Li Bin; Hong Ziruo [Key Laboratory of Excited State Processes, Changchun Institute of Optics, Fine Mechanics and Physics, Changchun 130033 (China); Chen Ping; Liu Shiyong [State Key Lab of Integrated Optoelectronics, Jilin University, Changchun 130023 (China)], E-mail: lib020@ciomp.ac.cn, E-mail: syliu@mail.jlu.edu.cn

    2008-12-21

    Three new luminescent cyclometalated iridium (II I) complexes are successfully synthesized. The cyclometalated ligand used here is 2-(2-fluorophenyl)-benzothiazole (F-BT). The auxiliary ligands are acetylacetone (acac), 1,1,1-trifluoroacetylaceton (3F-acac), 1,1,1,5,5,5-hexafluoroacetylacetone (6F-acac), respectively. All complexes exhibit bright photoluminescence at room temperature. Organic light-emitting diodes are fabricated by doping the iridium (III) complexes in 4, 4' -N, N'-dicarbazole-biphenyl (CBP), and the device characteristics are investigated. Among these devices, the performances of the optimized devices based on 1 at high current density are among the best reported for devices with iridium (III) complexes as emitters. EL efficiencies show weak dependence on doping concentration and current density. The optimized device exhibits a peak current efficiency of 28.5 cd A{sup -1} and a power efficiency of 11.2 lm W{sup -1}, respectively, at 20 mA cm{sup -2}, an efficiency of 22.7 cd A{sup -1} at 100 mA cm{sup -2}, 80% of the maximum, can be achieved. Short triplet decay time of 1 measured in solid films is supposed to be responsible for the minor loss in EL efficiency, which suggests depressed triplet-triplet annihilation and site saturation of the phosphor. Efficient exciton formation on the molecules of 1 by direct charge trapping and confinement within the emissive layer also make for outstanding electrophosphorescent performances.

  14. 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.

  15. SYNTHESIS AND IN VITRO ANTIPROLIFERATIVE ACTIVITY OF NOVEL 2-ARYLIDENEAMINOBENZIMIDAZOLE DERIVATIVES.

    Science.gov (United States)

    Nowicka, Anna; Liszkiewicz, Hanna; Nawrocka, Wanda P; Wietrzyk, Joanna; Sadowska, Joanna

    2015-01-01

    A new class of Mannich bases 9-26, derivatives of 2-amino-1H-benzimidazole, were obtained in the condensation of Schiff bases 1-4 or 2-benzylaminobenzimidazoles 5-8 with selected secondary amines: morpholine, piperidine, N-methylpiperazine, N-phenylpiperazine, 1-(2-pyridyl)piperazine, 1(2-methoxyphenyl)piperazine, 1-(2-pyrimidinyl)piperazine and formaldehyde in ethanol. The pyrimido[1,2-albenzimidazole derivatives 27-29 have been synthesized in the reactions of Schiff base 2 with selected compounds containing active methylene group: acetylacetone, benzoylacetone and malononitrile. The structures 1-29 were confirmed by the results of elementary analysis and their IR, 1H- and 13C-NMR spectra. The products 1-29 are of interest for biological studies and can be substrates for further synthesis. All compounds were screened against the cells of MV4-11 human leukemia and then the most active of them 5, 7, 9-16, 24-26, 28, 29 were tested towards human T47D breast and A549 lung cancer cells as well as normal mouse fibroblasts (BALB/3T3). The most active compound against the cancer cell lines was 4-amino-3-cyano-2-(4-hydroxyphenylene)-1,2-dihydropyrimi-do[1,2-a]benzimidazole (29) (IC50 0.23 ± 0.05 µg/mL against MV4-11 cells) showing in parallel very low cytotoxicity towards mouse fibroblasts. Cisplatin was the control drug.

  16. Synthesis and evaluation of antitumor activity ofsome thiazolo[4,5-b]pyridines

    Directory of Open Access Journals (Sweden)

    Ogurtsov V. V.

    2012-09-01

    Full Text Available Aim. To synthesize a series of novel 3H-thiazolo[4,5-b]pyridine-2-ones by structural modification of the core heterocycle in its N3- and N6-positions and to evaluate their anticancer activity in vitro on several tumor cell lines. Methods. Organic synthesis, 1H-NMR spectroscopy, trypan blue cell viability assay. Results. A new convenient synthetic approach was developed and optimized conditions were studied for the reaction of preparation of 3H- thiazolo[4,5-b]pyridin-2-one derivatives. 5,7-Dimethyl-3H-thiazolo[4,5-b]pyridin-2-one and 6-phenylazo-5,7- dimethyl-3H-thiazolo[4,5-b]pyridin-2-one were obtained by [3 + 3]cyclocondensation of 4-iminothiazolidone- 2 with acetylacetone and phenylazoacetylacetone in methanol medium in the presence of sodium methylate. They were used as starting compounds for further structural modification of the core thiazolo[4,5-b]pyridine heterocycle in its 3- and 6-positions. On the basis of in vitro cytotoxicity studies of synthesized compounds several structure-functional relationships underlying anticancer potential of 5,7-dimethyl-3H-thiazolo[4,5-b]pyridin- 2-one derivatives were identified. Conclusions. 3H-thiazolo[4,5-b]pyridin-2-one can be considered as a promising molecular scaffold for rational design of potential anticancer drug candidates. Introduction of phenylazo substitute at C6-position of 3H-thiazolo[4,5-b]pyridin-2-one proved to be the most efficient, as it led to 3-fold increase of its anticancer potential.

  17. Facile and straightforward synthesis of superparamagnetic reduced graphene oxide-Fe3O4 hybrid composite by a solvothermal reaction.

    Science.gov (United States)

    Liu, Yue-Wen; Guan, Meng-Xue; Feng, Lan; Deng, Shun-Liu; Bao, Jian-Feng; Xie, Su-Yuan; Chen, Zhong; Huang, Rong-Bin; Zheng, Lan-Sun

    2013-01-18

    A superparamagnetic reduced graphene oxide-Fe(3)O(4) hybrid composite (rGO-Fe(3)O(4)) was prepared via a facile and straightforward method through the solvothermal reaction of iron (III) acetylacetonate (Fe(acac)(3)) and graphene oxide (GO) in ethylenediamine (EDA) and water. By this method, chemical reduction of GO as well as the formation of Fe(3)O(4) nanoparticles (NPs) can be achieved in one step. The Fe(3)O(4) NPs are firmly deposited on the surfaces of rGO, avoiding their reassembly to graphite. The rGO sheets prevent the agglomeration of Fe(3)O(4) NPs and enable a uniform dispersion of these metal oxide particles. The size distribution and coverage density of Fe(3)O(4) NPs deposited on rGO can be controlled by varying the initial mass ratio of GO and iron precursor, Fe(acac)(3). With an initial mass ratio of GO and Fe(acac)(3) of 5:5, the surfaces of rGO sheets are densely covered by spherical Fe(3)O(4) NPs with an average size of 19.9 nm. The magnetic-functionalized rGO hybrid exhibits a good magnetic property and the specific saturation magnetization (M(s)) is 13.2 emu g(-1). The adsorption test of methylene blue from aqueous solution demonstrates the potential application of this rGO-Fe(3)O(4) hybrid composite in removing organic dyes from polluted water.

  18. 溶胶凝胶法制备( Ba0.3Sr0.7)(Zn1/3Nb2/3)O3微波介质陶瓷薄膜%FABRICATION OF ( Ba0.3Sr0.7 ) ( Zn1/3Nb2/3 ) O3 MICROWAVE DIELECTRIC CERAMIC THIN FILMS BY SOL-GEL

    Institute of Scientific and Technical Information of China (English)

    杨龙; 王锐; 石锋

    2012-01-01

    Inexpensive metal nitrates and barium acetate instead of metal alkoxides were used as raw materials, and high quality sol was obtained by utilization of acetylacetone and citric acid. Microwave dielectric ceramic (Ba0 3Sr0 7) (Zn1/3Nb2/3) O3 thin film was fabricated on Pt/Ti/SiO2/Si substrates by spin -coating, then annealed in the environment of oxygen. X - ray diffraction ( XRD) , Fourier transform infrared spectrometer (FTIR) , and scanning electron microscope ( SEM) were used to study the microstructures and morphological properties of the thin film. The results revealed that the main phases of the thin film were (Ba0 3Sr0 7) (Zn1/3Nb2/3) O3 with less second phase. The thin film was compact in surface and well crystallized without crack.%以柠檬酸和乙酰丙酮为络合剂和稳定剂,金属硝酸盐为起始原料制备溶胶.采用甩胶旋涂法在Pt/Ti/SiO2/Si基片上制膜并在O2环境下退火,重复3次制得所需薄膜.采用XRD,FTIR和SEM分析薄膜的结晶性,微观结构和表面形貌.结果表明:制备的薄膜主晶相为(Ba0.3Sr0.7)(Zn1/3Nb2/3)O3,伴有少量的第二相,同时,薄膜表面致密,无气孔,结晶良好,结晶颗粒均匀分布于薄膜的表面.

  19. A low-cost cementite (Fe3C) nanocrystal@N-doped graphitic carbon electrocatalyst for efficient oxygen reduction.

    Science.gov (United States)

    Wu, Tianxing; Zhang, Haimin; Zhang, Xian; Zhang, Yunxia; Zhao, Huijun; Wang, Guozhong

    2015-11-01

    In this work, chitosan whiskers (CWs) were first extracted using low-cost and earth-abundant crab shells as materials by a series of chemical processes, and then assembled into chitosan whisker microspheres (CWMs) via a simple photochemical polymerization approach. Subsequently, a cementite (Fe3C) nanocrystal@N-doped graphitic carbon (Fe3C@NGC) nanocomposite was successfully fabricated by high temperature pyrolysis of CWMs adsorbed with ferric acetylacetonate (Fe(acac)3) at 900 °C. It was found that a suitable growth atmosphere generated inside CWMs during high temperature pyrolysis is critically important to form Fe3C nanocrystal cores, concurrently accompanying a structural transformation from chitosan whiskers to mesoporous graphitic carbon shells with natural nitrogen (N) doping properties, resulting in the formation of a core-shell structure Fe3C@NGC nanocomposite. The resulting samples were evaluated as electrocatalysts for oxygen reduction reaction (ORR). In comparison with sole N-doped graphitic carbon without Fe3C nanocrystals obtained by direct pyrolysis of chitosan whisker microspheres at 900 °C (CWMs-900), Fe3C@NGC showed significantly improved ORR catalytic activity. The tolerance to fuel cell molecules (e.g., methanol) and the durability of Fe3C@NGC are obviously superior to commercial Pt/C catalysts in alkaline media. The high ORR performance of Fe3C@NGC could be due to its large surface area (313.7 m(2) g(-1)), a synergistic role of Fe3C nanocrystals, N doping in graphitic carbon creating more catalytic active sites, and a porous structure of the nanocomposite facilitating mass transfer to efficiently improve the utilization of these catalytic active sites.

  20. Thermodynamic modeling to analyse composition of carbonaceous coatings of MnO and other oxides of manganese grown by MOCVD

    Indian Academy of Sciences (India)

    Sukanya Dhar; A Varade; S A Shivashankar

    2011-02-01

    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 functions of CVD parameters. For the process conduced in argon ambient, the analysis predicts the simultaneous deposition of MnO and elemental carbon in 1:3 molar proportion, over a range of temperatures. The analysis predicts also that, if CVD is carried out in oxygen ambient, even a very low flow of oxygen leads to the complete absence of carbon in the film deposited oxygen, with greater oxygen flow resulting in the simultaneous deposition of two different manganese oxides under certain conditions. The results of thermodynamic modeling have been verified quantitatively for lowpressure CVD conducted in argon ambient. Indeed, the large excess of carbon in the deposit is found to constitute a MnO/C nanocomposite, the associated cauliflower-like morphology making it a promising candidate for electrode material in supercapacitors. CVD carried out in oxygen flow, under specific conditions, leads to the deposition of more than one manganese oxide, as expected from thermodynamic analysis (and forming an oxide–oxide nanocomposite). These results together demonstrate that thermodynamic analysis of the MOCVD process can be employed to synthesize thin films in a predictive manner, thus avoiding the inefficient trial-and-error method usually associated with MOCVD process development. The prospect of developing thin films of novel compositions and characteristics in a predictive manner, through the appropriate choice of CVD precursors and process conditions, emerges from the present work.

  1. 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.

  2. Synthesis and catalytic properties of iron - cerium phosphates with surfactant Síntese e propriedades catalíticas de ferro-fosfato de cério com surfactante

    Directory of Open Access Journals (Sweden)

    H. Onoda

    2013-03-01

    Full Text Available Iron phosphate was prepared from iron nitrate and phosphoric acid with a surfactant, pentaethylene glycol mono dodecyl ether. The chemical composition of the obtained samples was estimated from ICP and XRD measurements. Particle shape and size distribution were observed by SEM images and laser diffraction / scattering methods. Further, the catalytic activity was studied with the decomposition of the complex between formaldehyde, ammonium acetate, and acetylacetone. The peaks of FePO4 were observed in XRD patterns of samples prepared in Fe/Ce=10/0 and then heated at 600 ºC. Other samples were amorphous in XRD patterns. Iron-cerium phosphates had high catalytic activity for the decomposition of the complex.Fosfato de ferro foi preparado a partir do nitrato de ferro e ácido fosfórico com um surfactante éter monododecil pentaetileno glicol. A composição química das amostras obtidas foi estimada a partir de medidas por ICP e DRX. A distribuição e forma das partículas foram observadas por imagens de MEV e o pelo método de espalhamento de laser. A atividade catalítica foi estudada com a decomposição do complexo entre formaldeido, acetato de amônio e acetilacetona. Os picos de FePO4 foram observados nos padrões de DRX das amostras preparadas Fe/Ce=10/0 e então aquecidas a 600 ºC. Outras amostras foram de padrões de DRX amorfo. Ferro-fosfatos de cério tiveram alta atividade catalítica para a decomposição do complexo.

  3. Optically active mixed phthalocyaninato-porphyrinato rare-earth double-decker complexes: synthesis, spectroscopy, and solvent-dependent molecular conformations.

    Science.gov (United States)

    Zhang, Xiaomei; Muranaka, Atsuya; Lv, Wei; Zhang, Yuexing; Bian, Yongzhong; Jiang, Jianzhuang; Kobayashi, Nagao

    2008-01-01

    Reaction between the optically active metal-free phthalocyanine with a pi system with noncentrosymmetrical C(2) [corrected] symmetry ((S)- and (R)-H(2){Pc(OBNP)(2)}; OBNP=binaphthylphthalocyanine) and half-sandwich complexes [M(III)(acac)(TClPP)] (M=Y, Eu; TClPP=meso-tetrakis(4-chlorophenyl)porphyrinate; acac=acetylacetonate), which were generated in situ from [M(acac)(3)].n H(2)O and H(2)(TClPP) in n-octanol at reflux, provided the first optically active protonated mixed phthalocyaninato-porphyrinato rare-earth double-decker complexes [M(III)H{Pc(OBNP)(2)}(TClPP)] (M=Y, Eu) in good yield. In addition to electronic absorption spectroscopy and magnetic circular dichroism results, circular dichroism shows different spectroscopic features of these mixed-ring rare-earth double-decker compounds in different solvents, such as DMF and CHCl(3), which was well-reproduced on the basis of time-dependent density functional theory calculation results for the yttrium species (S)-[Y(III){Pc(OBNP)(2)}(Por)](-) (Por=porphyrinate, which is obtained by removing the four chlorophenyl groups from the TClPP ligand) in terms of the change in the rotation angle between the two macrocyclic ligands in the double-decker molecules. These results revealed the solvent-dependent nature of the molecular conformation of mixed-ring rare-earth double-decker complexes, which suggests a new way of tuning the optical and the electrochemical properties of sandwich-type bis(tetrapyrrole)-metal double-decker complexes in solution by changing the solvent.

  4. Synthesis and characterization of Fe{sub 0.6}Zn{sub 0.4}Fe{sub 2}O{sub 4} ferrite magnetic nanoclusters using simple thermal decomposition method

    Energy Technology Data Exchange (ETDEWEB)

    Sharifi, Ibrahim; Zamanian, Ali, E-mail: a-zamanian@merc.ac.ir; Behnamghader, Aliasghar

    2016-08-15

    This paper presents experimental results regarding the effect of the quantity of solvent on formation of the Fe–Zn ferrite nanoparticles during thermal decomposition. A ternary system of Fe{sub 0.6}Zn{sub 0.4}Fe{sub 2}O{sub 4} has been synthesized by a thermal decomposition method using metal acetylacetonate in high temperature boiling point solvent and oleic acid. The X-ray diffraction study was used to determine phase purity, crystal structure, and average crystallite size of iron–zinc ferrite nanoparticles. The average crystallite size of nanoparticles was increased from 13 nm to 37 nm as a result of reducing the solvent from 30 ml to 10 ml in a synthesis batch. The diameter of particles and morphology of the particles were determined by transmission electron microscopy (TEM) and field emission scanning electron microscope (FESEM). Mid and far Fourier transform infrared (FT-IR) measurement confirmed monophasic spinel structure of ferrite. Furthermore, the DC magnetic properties of the samples were studied using the vibrating sample magnetometer (VSM). The largest Fe–Zn ferrite nanoparticles exhibited a relatively high saturation magnetization of 96 emu/g. Moreover, Low-field AC susceptibility measurement indicated blocking temperature of nanoparticles around 170–200 K. - Highlights: • Narrow dispersed nanoclusters Fe–Zn ferrites prepared by a simple thermal decomposition route. • Increase of solvent content in reaction cause reduce the size of nanoparticles. • The XRD parameters are refined by the Rietveld method. • Saturation magnetization increases while coercivity decreases with increasing the particle size of ferrites.

  5. 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.

  6. 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.

  7. 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

  8. Synthesis and characterization of ZnO/CuInS{sub 2} nanocomposite and investigation of their photocatalytic properties under visible light irradiation

    Energy Technology Data Exchange (ETDEWEB)

    Fakhri, H., E-mail: hanieh_fakhrie@yahoo.com; Mahjoub, A.R., E-mail: mahjouba@modares.ac.ir; Khavar, A.H. Cheshme

    2014-11-01

    Highlights: • The CuInS{sub 2} nanocrystals have been successfully synthesized by the new reflux route. • The effect of surfactant on the morphology was investigated. • The effect of morphology of ZnO on the photocatalytic activity was investigated. • The optimal pH was obtained for photocatalytic process. - Abstract: In this work, CuInS{sub 2} (CIS) nanoparticles were synthesized via a simple and efficient reflux route and were composite with different nanostructures of ZnO by a thermal treatment process. The particle size of 56 nm was obtained using cupper acetylacetonate (Cu(acac){sub 2}), thioacetamide (C{sub 2}H{sub 5}NS), indium(III) chloride tetrahydrate (InCl{sub 3}·4H{sub 2}O) and ethylene glycol as a solvent at the reaction time of 90 min. The product was characterized by X-ray powder diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM) and ultraviolet–visible spectroscopy (UV–vis). SEM images presented the particle morphology of the CIS sample and flower-like, narcis and particle morphologies for the ZnO samples in the arranged reaction conditions. The band gap energy of 1.55 eV estimated by the diffuse reflectance spectroscopy (DRS) for CIS nanoparticles, exhibited that this product can be appropriate for photocatalytic activity in the visible region of solar spectrum. Photocatalytic activity of ZnO/CIS nanocomposite was determined by photodegradation of crystal violet under visible light irradiation. Results showed that the presence of the CIS nanoparticles improves the efficiency of the photocatalytic activity of ZnO and the removal efficiency up to 100%, which prove capability of CIS nanoparticles to depredate crystal violet from aqueous solution. In this paper, the effects of morphology of ZnO nanostructures and initial pH of solution on the photocatalytic activity are investigated.

  9. Synthesis and characterization of ZnO/CuInS2 nanocomposite and investigation of their photocatalytic properties under visible light irradiation

    Science.gov (United States)

    Fakhri, H.; Mahjoub, A. R.; Khavar, A. H. Cheshme

    2014-11-01

    In this work, CuInS2 (CIS) nanoparticles were synthesized via a simple and efficient reflux route and were composite with different nanostructures of ZnO by a thermal treatment process. The particle size of 56 nm was obtained using cupper acetylacetonate (Cu(acac)2), thioacetamide (C2H5NS), indium(III) chloride tetrahydrate (InCl3·4H2O) and ethylene glycol as a solvent at the reaction time of 90 min. The product was characterized by X-ray powder diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), scanning electron microscopy (SEM) and ultraviolet-visible spectroscopy (UV-vis). SEM images presented the particle morphology of the CIS sample and flower-like, narcis and particle morphologies for the ZnO samples in the arranged reaction conditions. The band gap energy of 1.55 eV estimated by the diffuse reflectance spectroscopy (DRS) for CIS nanoparticles, exhibited that this product can be appropriate for photocatalytic activity in the visible region of solar spectrum. Photocatalytic activity of ZnO/CIS nanocomposite was determined by photodegradation of crystal violet under visible light irradiation. Results showed that the presence of the CIS nanoparticles improves the efficiency of the photocatalytic activity of ZnO and the removal efficiency up to 100%, which prove capability of CIS nanoparticles to depredate crystal violet from aqueous solution. In this paper, the effects of morphology of ZnO nanostructures and initial pH of solution on the photocatalytic activity are investigated.

  10. Nanostructured copper, chromium, and tin oxide multicomponent materials as catalysts for methanol decomposition: 11C-radiolabeling study.

    Science.gov (United States)

    Tsoncheva, Tanya; Sarkadi-Priboczki, Eva; Dimitrov, Momtchil; Genova, Izabela

    2013-01-01

    Copper and chromium modified tin oxide nanocomposites were obtained via incipient wetness impregnation of high surface area nanosized SnO(2) with the corresponding metal acetylacetonates and their further decomposition in air. Powder X-ray diffraction (XRD), Nitrogen physisorption, UV-Vis, and Temperature-programmed reduction (TPR) with hydrogen were applied for the samples characterization. The catalytic activity of the obtained materials was tested in methanol conversion. A new approach based on the selective coverage of the surface with (11)C-methanol was used for the characterization of the catalytic sites. It was demonstrated that the products distribution could be controlled by the surface coverage with methanol and the role of different active sites was discussed. The modification of SnO(2) with copper oxide increased the activity in methanol decomposition to CO(2)via dioxymethylene intermediates, but the catalyst suffered considerable loss of activity due to the reduction transformations by the reaction medium and formation of an inactive intermetallic alloy. The modification with chromium changed the acid-basic properties of SnO(2) by the formation of Cr(2)O(3) nanoparticles as well as anchored to the support chromate species. The former particles facilitated the formation of dimethyl ether (DME), while the latter species converted methanol predominantly to hydrocarbons. The fraction of chromate species increased in Cu-Cr-Sn oxide multicomponent nanocomposites and promoted the formation of hydrocarbons over DME at low temperatures, while at higher temperatures, the activity of the copper species leading to CO(2) formation was more pronounced.

  11. Improved Low-Temperature Activity of V2O5-WO3/TiO2 for Denitration Using Different Vanadium Precursors

    Directory of Open Access Journals (Sweden)

    Lina Gan

    2016-02-01

    Full Text Available This work tested two V2O5-WO3/TiO2 catalysts with different vanadium precursors for selective catalytic reduction (SCR of flue gas NO using NH3 at 150–450 °C. While catalyst A was prepared using ammonium metavanadate (NH4VO3 through incipient impregnation, catalyst B was made according to the solvothermal method using vanadyl acetylacetonate (VO(acac2 as the vanadium precursor. The catalytic evaluation for denitration was in a laboratory fixed bed reactor using simulated flue gas under conditions of a gas hourly space velocity (GHSV of 40,000 h−1 and an NH3/NO molar ratio of 0.8. Without SO2 and water vapor in the flue gas at 200 °C, the realized NO conversion was 56% for catalyst A but 80% for B. The presence of 350 ppm SO2 and 10 vol. % water vapor in the flue gas slightly reduced the NO conversion over catalyst B, and its activity was stable in a 108-h continuous test at temperatures varying from 450 °C to 220 °C. Via fourier transformation infrared spectroscopy (FT-IR and thermogravimetric (TG analysis, it was shown that over catalyst B a dynamic balance between the formation and decomposition of ammonium sulfite or sulfate is built possibly at temperatures as low as 220 °C. For this catalyst there was a higher surface atomic concentration of vanadium and a higher ratio of V4+/(V4+ + V5+, while the NH3 adsorption test revealed more acidic sites on catalyst B. The study discloses a potentially new approach to prepare a V2O5-WO3/TiO2 catalyst with good performance for SCR of flue gas NO at 220–300 °C.

  12. Comparison between sol-gel derived and classic methods for the elaboration process of DSA Ta/IrO{sub 2} electrodes

    Energy Technology Data Exchange (ETDEWEB)

    Massot, L.; Palau, P.; Savall, A.; Taxil, P. [Paul-Sabatier Univ., Toulouse (France). Chemical Engineering Lab.

    2006-07-01

    This paper investigated the oxygen evolution of inert anodes in acidic media. The electrodes were composed of a tantalum (Ta) substrate with a catalyst coating of iridium oxide (IrO{sub 2}). Two methods were used to obtain the catalyst coating: (1) a Sol-Gel derived method using iridium acetylacetonate ([CH{sub 3}COCH=COCH{sub 3}]{sub 3}Ir) dissolved in an isopropanol-acetic acid mixture, and (2) iridium chloride (IrCl{sub 4}) dissolved in an ethanol-isopropanol mixture as an iridium oxide precursor. The electrodes were then characterized and compared using thermogravimetric measurements of the precursors. Results of the study showed that the new precursor derived from the Sol-Gel method was more reactive as the IrO{sub 2}3 formation temperature was lower. A higher amount of heat generated by cracking and combustion of the organic compounds was released during the decomposition of the Sol-Gel precursor salts. The enthalpy of conversion into the oxide measured by differential sweeping calorimetry was -15580 J/g in the case of the Sol-Gel derived method and -74.7 J/g in the case of the traditional method. However, the electrodes prepared by the Sol-Gel method were not stable, and the service lives of the electrodes were 4 times less significant than those of the electrodes prepared using the other method due to the low stability of metal iridium under polarization. It was also noted that the fine catalyst particles were less stable during a gaseous evolution. Results indicated that a rise in the thermal processing temperatures may facilitate the formation of iridium oxide, but would involve a more significant oxidation of the substrate. It was concluded that the Sol-Gel method is not suitable for the preparation of Ta/IrO{sub 2} electrodes when the oxidation number of the iridium oxide precursor is 3. 3 refs., 1 tab., 1 fig.

  13. Catalytic nanomedicine technology: copper complexes loaded on titania nanomaterials as cytotoxic agents of cancer cell.

    Science.gov (United States)

    Lopez, Tessy; Ortiz-Islas, Emma; Guevara, Patricia; Gómez, Esteban

    2013-01-01

    The anticancer properties of pure copper (II) acetate and copper (II) acetylacetonate, alone and loaded on functionalized sol-gel titania (TiO(2)), were determined in four different cancer cell lines (C6, RG2, B16, and U373), using increasing concentrations of these compounds. The copper complexes were loaded onto the TiO(2) network during its preparation by the solgel process. Once copper-TiO(2) materials were obtained, these were characterized by several physical-chemical techniques. An in vitro copper complex-release test was developed in an aqueous medium at room temperature and monitored by ultraviolet spectroscopy. The toxic effect of the copper complexes, alone and loaded on TiO(2), was determined using a cell viability 3(4,5-dimethylthiazol-2-yl)-2,5-diphenyl-tetrazolium bromide (MTT) assay, when cancer cells were treated with increasing concentrations (15.75-1000 mg/mL) of these. Characterization studies revealed that the addition of copper complexes to the TiO(2) sol-gel network during its preparation, did not generate changes in the molecular structure of the complexes. The surface area, pore volume, and pore diameter were affected by the copper complex additions and by the crystalline phases obtained. The kinetic profiles of both copper complexes released indicated two different stages of release: The first one was governed by first-order kinetics and the second was governed by zero-order kinetics. The cell viability assay revealed a cytotoxic effect of copper complexes, copper-TiO(2), and cisplatin in a dose-dependent response for all the cell lines; however, the copper complexes exhibited a better cytotoxic effect than the cisplatin compound. TiO(2) alone presented a minor cytotoxicity for C6 and B16 cells; however, it did not cause any toxic effect on the RG2 and U373 cells, which indicates its high biocompatibility with these cells.

  14. Thermochemical properties and contribution groups for ketene dimers and related structures from theoretical calculations.

    Science.gov (United States)

    Morales, Giovanni; Martínez, Ramiro

    2009-07-30

    This research's main goals were to analyze ketene dimers' relative stability and expand group additivity value (GAV) methodology for estimating the thermochemical properties of high-weight ketene polymers (up to tetramers). The CBS-Q multilevel procedure and statistical thermodynamics were used for calculating the thermochemical properties of 20 cyclic structures, such as diketenes, cyclobutane-1,3-diones, cyclobut-2-enones and pyran-4-ones, as well as 57 acyclic base compounds organized into five groups. According to theoretical heat of formation predictions, diketene was found to be thermodynamically favored over cyclobutane-1,3-dione and its enol-tautomeric form (3-hydroxycyclobut-2-enone). This result did not agree with old combustion experiments. 3-Hydroxycyclobut-2-enone was found to be the least stable dimer and its reported experimental detection in solution may have been due to solvent effects. Substituted diketenes had lower stability than substituted cyclobutane-1,3-diones with an increased number of methyl substituents, suggesting that cyclobutane-1,3-dione type dimers are the major products because of thermodynamic control of alkylketene dimerization. Missing GAVs for the ketene dimers and related structures were calculated through linear regression on the 57 acyclic base compounds. Corrections for non next neighbor interactions (such as gauche, eclipses, and internal hydrogen bond) were needed for obtaining a highly accurate and precise regression model. To the best of our knowledge, the hydrogen bond correction for GAV methodology is the first reported in the literature; this correction was correlated to MP2/6-31Gdagger and HF/6-31Gdagger derived geometries to facilitate its application. GAVs assessed by the linear regression model were able to reproduce acyclic compounds' theoretical thermochemical properties and experimental heat of formation for acetylacetone. Ring formation and substituent position corrections were calculated by consecutively

  15. 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)

  16. Synthesis of ZnO@γ-Fe2O3 core-shell nanocomposites by a facile thermal decomposition approach and their application in photocatalytic degradation of congo red

    Science.gov (United States)

    Yadav, Sudheer Kumar; Jeevanandam, P.

    2016-07-01

    ZnO@γ-Fe2O3 core-shell nanocomposites were synthesized by a facile thermal decomposition approach. ZnO nanorods were first synthesized by calcination of zinc acetate at 300 °C, in air. γ-Fe2O3 nanoparticles were then deposited on the surface of ZnO nanorods by the thermal decomposition of iron acetylacetonate at 200 °C in diphenyl ether. The structure, composition, optical and magnetic properties of the nanocomposites were studied using an array of techniques. XRD results suggest the presence of γ-Fe2O3 nanoparticles and ZnO, and FE-SEM images indicate formation of shell of iron oxide on the ZnO nanorods. Transmission electron microscopy studies clearly show that ZnO possesses rod morphology (length = 1.1 ± 0.1 μm, diameter = 40.1 ± 7 nm) and TEM images of the ZnO@γ-Fe2O3 nanocomposites show uniform shell of γ-Fe2O3 coated on the ZnO nanorods and thickness of the γ-Fe2O3 shell varies from 10 to 20 nm. Diffuse reflectance spectra of ZnO@γ-Fe2O3 nanocomposites reveal extended optical absorption in the visible range (400-600 nm) and photoluminescence spectra indicate that the ZnO@γ-Fe2O3 nanocomposites exhibit enhanced defect emission. The ZnO@γ-Fe2O3 core-shell nanocomposites show superparamagnetic behaviour at room temperature. The core-shell nanocomposites exhibit enhanced visible-light driven photocatalytic degradation of congo red in an aqueous solution as compared to pure ZnO nanorods and γ-Fe2O3 nanoparticles. The enhanced photocatalytic activity is attributed to good visible-light absorption and effective charge separation at the interface of ZnO@γ-Fe2O3 core-shell nanocomposites.

  17. Superparamagnetic gamma-Fe2O3@SiO2 nanoparticles: a novel support for the immobilization of [VO(acac)2].

    Science.gov (United States)

    Pereira, Clara; Pereira, André M; Quaresma, Pedro; Tavares, Pedro B; Pereira, Eulália; Araújo, João P; Freire, Cristina

    2010-03-21

    This work reports a detailed investigation about the physicochemical properties of superparamagnetic gamma-Fe(2)O(3) nanomaterial synthesized by the co-precipitation method and coated with two silica shells, and its application as support for the immobilization of oxovanadium(IV) acetylacetonate ([VO(acac)(2)]). The influence of the silica coatings on the surface composition and physicochemical interactions of the core-shell nanocomposites is discussed based on the combination of several techniques: electron microscopy techniques (SEM and TEM with EDS), DLS, powder XRD, XPS, FTIR and magnetic characterization. The identity of the iron oxide, gamma-Fe(2)O(3), was confirmed by XPS, FTIR and by the Rietveld refinement of the PXRD pattern. The results obtained by electron microscopy techniques, XRD and magnetization indicated that the gamma-Fe(2)O(3) nanoparticles are superparamagnetic and present an average size of approximately 6.5 nm. The first silica coating leads to a core-shell nanomaterial with an average particle size of 21 nm and upon the second coating, the average size increases to 240 nm. Magnetic measurements revealed that the silica-coated nanomaterials maintain the superparamagnetic state at room temperature, although with an expected reduction of the magnetization saturation due to the increase of the silica shell thickness. Furthermore, a numerical fit of the temperature dependence of magnetization was performed to determine the core size distribution and the effect of the silica coatings on the dipolar magnetic interactions. [VO(acac)(2)] was covalently immobilized on the surface of the silica-coated magnetic nanoparticles functionalized with amine groups, as confirmed by chemical analysis and XPS. In a proof-of-principle experiment, we demonstrated the catalytic performance of the novel magnetic hybrid nanomaterial in the epoxidation of geraniol, which presented high selectivity towards the 2,3-epoxygeraniol product and easy recovery by magnetic

  18. Monomeric malonate precursors for the MOCVD of HfO2 and ZrO2 thin films.

    Science.gov (United States)

    Pothiraja, Ramasamy; Milanov, Andrian; Parala, Harish; Winter, Manuela; Fischer, Roland A; Devi, Anjana

    2009-01-28

    New Hf and Zr malonate complexes have been synthesized by the reaction of metal amides with different malonate ligands (L = dimethyl malonate (Hdmml), diethyl malonate (Hdeml), di-tert-butyl malonate (Hdbml) and bis(trimethylsilyl) malonate (Hbsml)). Homoleptic eight-coordinated monomeric compounds of the type ML4 were obtained for Hf with all the malonate ligands employed. In contrast, for Zr only Hdmml and Hdeml yielded the eight-coordinated monomeric compounds of the type ML4, while using the bulky Hdbml and Hbsml ligands resulted into mixed alkoxo-malonato six-coordinated compounds of the type [ML2(OR)2]. Single crystal X-ray diffraction studies of all the compounds are presented and discussed, and they are found to be monomeric. The complexes are solids and in solution, they retain their monomeric nature as evidenced by NMR measurements. Compared to the classical beta-diketonate complexes, [M(acac)4] and [M(thd)4] (M = Hf, Zr; acac: acetylacetonate; thd: tetramethylheptadione), the new malonate compounds are more volatile, decompose at lower temperatures and have lower melting points. In particular, the homoleptic diethyl malonate complexes of Hf and Zr melt at temperatures as low as 62 degrees C. In addition, the compounds are very stable in air and can be sublimed quantitatively. The promising thermal properties makes these compounds interesting for metal-organic chemical vapor deposition (MOCVD). This was demonstrated by depositing HfO2 and ZrO2 thin films successfully with two representative Hf and Zr complexes.

  19. Sintering of SiO{sub 2}-Al{sub 2}O{sub 3}-TiO{sub 2} and SiO{sub 2}-Al{sub 2}O{sub 3}-ZrO{sub 2} obtained by the sol-gel process

    Energy Technology Data Exchange (ETDEWEB)

    Mendoza-Serna, R.; Loyo-Arnaud, E.; Martinez-Fuentes, S.S.; Munoz-Duran, R.; Valdez-Castro, L. [Facultad de Estudios Superiores Zaragoza, UNAM, Mexico, D. F. (Mexico); Mendez-Vivar, J. [Univ. Autonoma Metropolitana-Iztapalapa, Depto. de Quimica, Mexico, D. F. (Mexico)

    2004-07-01

    An experimental strategy was developed to obtain Si-Al-Ti and Si-Al-Zr transparent sols via the sol-gel process. Acetylacetone (2, 4 pentanedione, acacH) and itaconic anhydride (2-methylenesuccinic anhydride, anhH) were employed separately as chelating agents to stabilize Al, Ti and Zr precursors, in order to slow down the chemical reactivity, avoiding precipitation. The molar ratio chelating agent/M (M: Al, Ti, and Zr) was 2.0. The starting materials were Si(OEt){sub 4} (TEOS), Ti(OEt){sub 4} (OEt: OCH{sub 2}CH{sub 3}), Al(OBu{sup s}){sub 3} (OBu{sup s}: C{sub 2}H{sub 5}CH(CH{sub 3})O) and Zr(OPr{sup n}){sub 4} (OPr{sup n}: OCH{sub 2}CH{sub 2}CH{sub 3}). The molar ratio Si:Al:Ti or Zr was 80:7:13, respectively. The sols were clear and homogeneous at macroscopic scale during gelation. The gels were dried at 423 K for 24 h in air. Xerogels were calcined at 673, 773, 873 and 1123 K for 24 h in air. The samples were analyzed by X-ray diffraction and found to be amorphous up to 873 K. The solids calcined have small pore size (micro and mesopores). The solids were also studied by scanning electron microscopy (SEM), and X-ray diffraction (XRD) to compare the influence of size and structure of the chelating agent in the particle size and the crystallite size distribution. (orig.)

  20. 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.

  1. Highly active nanocrystalline TiO(2) photoelectrodes.

    Science.gov (United States)

    Paronyan, Tereza M; Kechiantz, A M; Lin, M C

    2008-03-19

    A simple method for the fabrication of highly photoactive nanocrystalline two-layer TiO(2) electrodes for solar cell applications is presented. Diluted titanium acetylacetonate has been used as a precursor for covering SnO(2):F (FTO) films with dense packed TiO(2) nanocrystallites. The nanoporous thick TiO(2) film follows the dense packed thin TiO(2) film as a second layer. For the latter, amorphous TiO(2) nanoparticles have been successfully synthesized by a sol-gel technique in an acidic environment with pHTiO(2) gel of pH 5 was obtained; this pH value is higher than the recently reported value of 3.1 (Park et al 2005 Adv. Mater. 17 2349-53). Highly interconnected, nanoporous, transparent and active TiO(2) films have been fabricated from the pH 5 gel. SEM, AFM and XRD analyses have been carried out for investigation of the crystal structure and the size of nanoparticles as well as the surface morphology of the films. Investigation of the photocurrent-voltage characteristics has shown improvement in cell performance along with the modification of the surface morphology, depending on pH of the TiO(2) gel. Increasing the pH of the gel from 2.1 to 5 enhanced the overall conversion efficiency of the dye-sensitized solar cells by approximately 30%. An energy conversion efficiency of 8.83% has been achieved for the cell (AM1.5, 100  mWcm(-2) simulated sunlight) compared to 6.61% efficiency in the absence of ammonia in the TiO(2) gel.

  2. 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.

  3. Synthesis, spectroscopic studies, molecular modeling and antimicrobial activity of binuclear Co(II) and Cu(II) complexes of 4,6-diacetylresorcinol

    Science.gov (United States)

    Shebl, Magdy; Khalil, Saied M. E.; Taha, A.; Mahdi, M. A. N.

    2013-09-01

    Reactions of 4,6-diacetylresorcinol with different cobalt(II) and copper(II) salts viz., OAc-, Cl-, NO3- and SO42-, yielded a new series of binuclear metal complexes. Reactions of the ligand with these metal ions in the presence of a secondary ligand (L‧) [O,O-donor; acetylacetone, N,O-donor; 8-hydroxyquinoline or N,N-donor; 1,10-phenanthroline and N,N,N‧,N‧-tetramethylethylenediamine] in 1:2:2 (L:M:L‧) molar ratio yielded mixed-ligand complexes with different molar ratios. The metal complexes were characterized by elemental and thermal analyses, IR, electronic, ESR and mass spectra as well as conductivity and magnetic susceptibility measurements. The analytical and spectroscopic data suggested that the H2L ligand behaves as a neutral, monobasic or dibasic tetradentate ligand, depending on the type of the anion and secondary ligand used, through the two phenolic and two carbonyl groups. Electronic spectra, magnetic and conductivity measurements showed that all complexes are octahedral with non-electrolytic nature. The profile of ESR spectra of copper(II) complexes suggested the octahedral geometry and the spin Hamiltonian parameters of the complexes were calculated and discussed. Molecular orbital calculations were performed for metal complexes using Hyperchem 7.52 program on the bases of PM3 level and the results correlated with the experimental data. The free ligand and some of its metal complexes showed antimicrobial activity towards some of Gram-positive and Gram-negative bacteria, yeast (Candida albicans) and fungus (Aspergillus fumigatus).

  4. Iron pyrite thin films synthesized from an Fe(acac)3 ink.

    Science.gov (United States)

    Seefeld, Sean; Limpinsel, Moritz; Liu, Yu; Farhi, Nima; Weber, Amanda; Zhang, Yanning; Berry, Nicholas; Kwon, Yon Joo; Perkins, Craig L; Hemminger, John C; Wu, Ruqian; Law, Matt

    2013-03-20

    Iron pyrite (cubic FeS2) is a promising candidate absorber material for earth-abundant thin-film solar cells. Here, we report on phase-pure, large-grain, and uniform polycrystalline pyrite films that are fabricated by solution-phase deposition of an iron(III) acetylacetonate molecular ink followed by sequential annealing in air, H2S, and sulfur gas at temperatures up to 550 °C. Phase and elemental compositions of the films are characterized by conventional and synchrotron X-ray diffraction, Raman spectroscopy, Auger electron spectroscopy, secondary ion mass spectrometry, and X-ray photoelectron spectroscopy (XPS). These solution-deposited films have more oxygen and alkalis, less carbon and hydrogen, and smaller optical band gaps (E(g) = 0.87 ± 0.05 eV) than similar films made by chemical vapor deposition. XPS is used to assess the chemical composition of the film surface before and after exposure to air and immersion in water to remove surface contaminants. Optical measurements of films rich in marcasite (orthorhombic FeS2) show that marcasite has a band gap at least as large as pyrite and that the two polymorphs share similar absorptivity spectra, in excellent agreement with density functional theory models. Regardless of the marcasite and elemental impurity contents, all films show p-type, weakly activated transport with curved Arrhenius plots, a room-temperature resistivity of ~1 Ω cm, and a hole mobility that is too small to measure by Hall effect. This universal electrical behavior strongly suggests that a common defect or a hole-rich surface layer governs the electrical properties of most FeS2 thin films.

  5. 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)

  6. Hierarchical self-assembly of nanoparticles in polymer matrix and the nature of the interparticle interaction

    Science.gov (United States)

    Lin, Yu-Chiao; Chen, Chun-Yu; Chen, Hsin-Lung; Hashimoto, Takeji; Chen, Show-An; Li, Yen-Cheng

    2015-06-01

    Using small angle X-ray scattering (SAXS), we elucidated the spatial organization of palladium (Pd) nanoparticles (NPs) in the polymer matrix of poly(2-vinylpyridine) (P2VP) and the nature of inter-nanoparticle interactions, where the NPs were synthesized in the presence of P2VP by the reduction of palladium acetylacetonate (Pd(acac)2). The experimental SAXS profiles were analysed on the basis of a hierarchical structure model considering the following two types of interparticle potential: (i) hard-core repulsion only (i.e., the hard-sphere interaction) and (ii) hard-core repulsion together with an attractive potential well (i.e., the sticky hard-sphere interaction). The corresponding theoretical scattering functions, which were used for analysing the experimental SAXS profiles, were obtained within the context of the Percus-Yevick closure and the Ornstein-Zernike equation in the fundamental liquid theory. The analyses revealed that existence of the attractive potential well is indispensable to account for the experimental SAXS profiles. Moreover, the morphology of the hybrids was found to be characterized by a hierarchical structure with three levels, where about six primary NPs with the diameter of ca. 1.8 nm (level one) formed local clusters (level two), and these clusters aggregated to build up a large-scale mass-fractal structure (level three) with the fractal dimension of ca. 2.3. The scattering function developed here is of general use for quantitatively characterizing the morphological structures of polymer/NP hybrids and, in particular, for exploring the interaction potential of the NPs on the basis of the fundamental liquid theory.

  7. XRF法测定PTA生产中Co(Ⅲ)和Co(Ⅱ)含量%XRF determination of Co(Ⅲ) and Co( Ⅱ ) contents during PTA production

    Institute of Scientific and Technical Information of China (English)

    薛月霞; 李人杰

    2011-01-01

    Co( Ⅲ ) and Co( Ⅱ ) can be separated by extraction process due to the different water solubility of their chelates obrained by reacting with acetylacetone. The Co( Ⅲ ) and Co( Ⅱ ) contents of p -xylene (PX) liquid phase oxidation system were determined by X-ray fluorescene spectrometry (XRF). The results showed that the recovery of standard addition was 92% 109% and the relative standard deviation was 3.5% -4.2% when the operating current and time were 20 μA and 100 s, respectively. This XRF analysis method can be applied in the practical production due to its high accuracy and precision.%利用Co(Ⅱ)、Co(Ⅲ)与乙酰丙酮生成的螯合物的不同水溶性,通过萃取将Co(Ⅱ)、Co(Ⅲ)进行分离,应用X射线荧光光谱仪(XRF)测定对二甲苯(PX)液相氧化反应中的Co(Ⅱ)和Co(Ⅲ)含量.结果表明:XRF的操作电流为20μA,测试时间为100 s时,测定PX中的Co(Ⅱ)和Co(Ⅲ)含量,其加标回收率为92%~109%,相对标准偏差为3.5%~4.2%.该XRF分析方法准确度和精密度较高,可应用于生产实际中.

  8. 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.

  9. 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.

  10. 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%.

  11. Ultrasonic spray-pyrolyzed CuCrO2 thin films

    Science.gov (United States)

    Sánchez-Alarcón, R. I.; Oropeza-Rosario, G.; Gutierrez-Villalobos, A.; Muro-López, M. A.; Martínez-Martínez, R.; Zaleta-Alejandre, E.; Falcony, C.; Alarcón-Flores, G.; Fragoso, R.; Hernández-Silva, O.; Perez-Cappe, E.; Mosqueda Laffita, Yodalgis; Aguilar-Frutis, M.

    2016-05-01

    In this paper the optical, structural and electrical properties of CuCrO2 thin films deposited by ultrasonic spray pyrolysis at temperatures from 400 to 600 °C in steps of 50 °C are presented. Copper and chromium acetylacetonates were chosen as sources of Cu and Cr, respectively, and N,N-dimethylformamide was used as the solvent. X-ray results confirmed that the films as deposited showed the CuCrO2 phase without any post-deposition thermal annealing. The surface morphology was observed to be mirror like, and as the films were deposited at different temperatures, they gradually revealed the presence of small crystallites. The best film’s optical percentage transmission (in the visible region), about 58%, was obtained in films deposited at 450 °C, and the highest band gap energy (3.17 eV) was measured in films deposited at 400 °C. The electrical properties of the films were obtained by the Hall effect. A hole concentration in the range 1019-1021 cm-3, conductivity as high as 35 S cm-1, and mobility lower than 1 cm2 V-1 s-1 were obtained in the films. p-type conductivity was confirmed using the hot point probe arrangement, and the Seebeck coefficient was estimated. The hole conductivity is thought to be due to excess oxygen in the films. Finally, the minimum energy required to transfer carriers from acceptor level to the valence band in the films was estimated by impedance spectroscopy.

  12. Cobalt(III) complexes as potential anticancer agents: Physicochemical, structural, cytotoxic activity and DNA/protein interactions.

    Science.gov (United States)

    Thamilarasan, V; Sengottuvelan, N; Sudha, A; Srinivasan, P; Chakkaravarthi, G

    2016-09-01

    Cobalt(III) complexes (1-3) such as [Co(acac)(bpy)(N3)2·H2O] 1, [Co(acac)(en)(N3)2] 2, and [Co(acac)(2-pic)(N3)2] 3 (where, acac=acetylacetone, bpy=2.2'-bipyridine, en=ethylenediamine, 2-pic=2-picolylamine and NaN3=sodium azide) were synthesized and characterized. The structure of complexes (1-3) has been determined by single crystal X-ray diffraction studies and the configuration around cobalt(III) ion was distorted octahedral coordination geometry. Density functional theory calculations were performed to examine the molecular geometry and frontier molecular orbital properties of complexes (1-3). DNA binding properties of the cobalt(III) complexes with calf thymus DNA (CT-DNA) were investigated by UV-visible absorption, fluorescence, circular dichroism spectroscopy and viscosity measurements. The docking studies showed the preferred orientation of sterically acceptable Co(III) complexes (1, 2) inside the DNA through the mode of intercalation, whereas complex 3 exhibited minor groove binding modes. The intrinsic binding constants Kb of complexes (1-3) with CT-DNA were in the following order 1>3>2. Complexes (1-3) exhibit a good binding propensity to bovine serum albumin (BSA) and gel electrophoresis assay demonstrated that the complexes (1-3) promote the cleavage of the pBR322 DNA in the presence of 3-mercaptopropionic acid (MPA) and cleavage process was found to proceed by singlet oxygen cleavage mechanism. Further, the in vitro cytotoxicity studies of complexes (1-3) were tested on human breast cancer cell line (MCF-7).

  13. 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)

  14. Synthesis of hybrid metal-organic frameworks of {FexMyM'1-x-y}-MIL-88B and the use of anions to control their structural features.

    Science.gov (United States)

    Choi, Sora; Cha, Wonhee; Ji, Hoyeon; Kim, Dooyoung; Lee, Hee Jung; Oh, Moonhyun

    2016-09-22

    The controlled formation of metal-organic frameworks (MOFs) or coordination polymers (CPs) with suitable components and structural features is one of the most important themes in MOF research. In particular, the reliable preparation of hybrid MOFs containing more than two different kinds of metal ions or organic linkers and a comprehensive understanding of the structural flexibility of MOFs are the central issues for the production of MOFs with the desired properties. We report the synthesis of micro-sized hybrid MOF particles [also known as coordination polymer particles (CPPs)] containing two or three kinds of metal ions in each particle: {FexMyM'1-x-y}-MIL-88B (MIL stands for Materials of Institut Lavoisier, M and M' = Ga, Co, or Mn). Scanning electron microscopy images revealed the formation of well-defined uniform micro-sized hexagonal rods, and energy-dispersive X-ray spectroscopy and elemental mapping images verified the simultaneous incorporation of two or three kinds of metal ions within the CPPs. Interestingly, the structural features of CPPs made from MIL-88B were controlled by altering the anions involved in the structure. Incorporating large acetylacetonate anions within the structure resulted in the closed MIL-88B structure with a small cell volume. However, the open MIL-88B structure with a large cell volume was obtained when small chloride anions were incorporated. The intermediate semi-open MIL-88B structure was also prepared using nitrate anions. Three different structural forms of MIL-88B were verified by powder X-ray diffraction, whole pattern fitting, and thermogravimetric analysis.

  15. 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.

  16. 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.

  17. In situ X-ray Rietveld analysis of Ni-YSZ solid oxide fuel cell anodes during NiO reduction in H{sub 2}

    Energy Technology Data Exchange (ETDEWEB)

    Reyes Rojas, A [Centro de Investigacion en Materiales Avanzados SC, Miguel de Cervantes 120, Complejo Industrial Chihuahua, Cd. de Chihuahua, Chihuahua (Mexico); Facultad de Quimica, Universidad Autonoma del Estado de Mexico, Toluca (Mexico); Esparza-Ponce, H E [Centro de Investigacion en Materiales Avanzados SC, Miguel de Cervantes 120, Complejo Industrial Chihuahua, Cd. de Chihuahua, Chihuahua (Mexico); Fuentes, L [Centro de Investigacion en Materiales Avanzados SC, Miguel de Cervantes 120, Complejo Industrial Chihuahua, Cd. de Chihuahua, Chihuahua (Mexico); Lopez-Ortiz, A [Centro de Investigacion en Materiales Avanzados SC, Miguel de Cervantes 120, Complejo Industrial Chihuahua, Cd. de Chihuahua, Chihuahua (Mexico); Keer, A [Centro de Investigacion en Materiales Avanzados SC, Miguel de Cervantes 120, Complejo Industrial Chihuahua, Cd. de Chihuahua, Chihuahua (Mexico); Reyes-Gasga, J [Instituto de Fisica, UNAM. Apartado Postal 20-364. 01000 Mexico DF (Mexico)

    2005-07-07

    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 {yields} Ni-YSZ) at 800 deg. C for 8 h in a tubular reactor furnace using 10% H{sub 2}/N{sub 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{sup -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.

  18. Indium tin oxide thin films elaborated by sol-gel routes: The effect of oxalic acid addition on optoelectronic properties

    Energy Technology Data Exchange (ETDEWEB)

    Kesim, Mehmet Tumerkan; Durucan, Caner, E-mail: cdurucan@metu.edu.tr

    2013-10-31

    Single layer indium tin oxide (ITO) thin films were deposited on glass using modified sol-gel formulations. The coating sols were prepared using indium (InCl{sub 3}∙ 4H{sub 2}O) and tin salts (SnCl{sub 4}∙ 5H{sub 2}O). The stable sols were obtained using ethanol (C{sub 2}H{sub 5}OH) and acetylacetone (C{sub 5}H{sub 8}O{sub 2}) as solvents and by the addition of oxalic acid dihydrate (C{sub 2}H{sub 2}O{sub 4}∙ 2H{sub 2}O) in different amounts. The effect of oxalic acid content in the sol formulation and post-coating calcination treatment (in air at 300–600 °C) on electrical/optical properties of ITO films have been reported. It was shown that film formation efficiency, surface coverage and homogeneity were all enhanced with oxalic acid addition. Oxalic acid modification also leads to a significant improvement in electrical conductivity without affecting the film thickness (45 ± 3 nm). ITO films exhibiting high transparency (≈ 93%, visible region) with a sheet resistance as low as 3.8 ± 0.4 kΩ/sqr have been formed by employing coating sols with optimized oxalic acid amount. The mechanisms and factors affecting the functional performance of oxalic acid-modified films have been thoroughly discussed and related to the microstructural and chemical characteristic of the films achieved by oxalic acid addition. - Highlights: • A solution-based method for processing indium tin oxide (ITO) thin film is reported. • Oxalic acid (OAD) modification leads to a highly compacted film microstructure. • Bulk resistivity of a single layer OAD-modified ITO film was determined as 0.02 Ωcm. • Thin films with transparency values higher than 90% were produced.

  19. Manganese(III) Schiff base complexes: chemistry relevant to the copolymerization of epoxides and carbon dioxide.

    Science.gov (United States)

    Darensbourg, Donald J; Frantz, Eric B

    2007-07-23

    Schiff base complexes of the form (acacen)Mn(III)X (acacen = N,N'-bis(acetylacetone)-1,2-ethylenediimine), where X = OAc, Cl, or N(3), have been evaluated for their ability to couple CO(2) and cyclohexene oxide in the presence of a variety of cocatalysts to provide cyclic or polycarbonates. These complexes proved to be ineffective at catalyzing this process; however, valuable information related to the coordination chemistry of these manganese Schiff bases was elucidated. Of importance, mechanistic findings as revealed by comprehensive studies involving structurally related (salen)CrX and (salen)CoX complexes strongly support the requirement of six-coordinate metal species for the effective copolymerization of CO(2) and epoxides. In the case of these Mn(III) complexes, it was determined that in chloroform or toluene solution a five-coordinate species was greatly favored over a six-coordinate species even in the presence of 20 equiv or more of various Lewis bases. Significantly epoxide monomers such as propylene oxide and cyclohexene oxide displayed no tendency to bind to these (acacen)MnX derivatives, even when used as solvents. Only in the case of excessive quantities of heterocyclic amines such as pyridine, DMAP, and DBU was spectral evidence of a six-coordinate Mn derivative observed in solution. X-ray crystal structures are provided for many of the complexes involved in this study, including the one-dimensional polymeric structures of [(acacen)MnOAc x 2H(2)O](n), [(acacen)MnN(3)](n) (mu(1,3)-N(3)), and a rare mixed bridging species [(acacen)MnN(3)](n) (mu(1,3)-N(3)/mu(1,1)-N(3)). In addition, a structure was obtained in which the unit cell contains both a (acacen)MnN(3)(DMAP) and a (acacen)MnN(3) species.

  20. On the Critical Effect of the Metal (Mo vs. W) on the [3+2] Cycloaddition Reaction of M3 S4 Clusters with Alkynes: Insights from Experiment and Theory.

    Science.gov (United States)

    Bustelo, Emilio; Gushchin, Artem L; Fernández-Trujillo, M Jesús; Basallote, Manuel G; Algarra, Andrés G

    2015-10-12

    Whereas the cluster [Mo3 S4 (acac)3 (py)3 ](+) ([1](+) , acac=acetylacetonate, py=pyridine) reacts with a variety of alkynes, the cluster [W3 S4 (acac)3 (py)3 ](+) ([2](+) ) remains unaffected under the same conditions. The reactions of cluster [1](+) show polyphasic kinetics, and in all cases clusters bearing a bridging dithiolene moiety are formed in the first step through the concerted [3+2] cycloaddition between the C≡C atoms of the alkyne and a Mo(μ-S)2 moiety of the cluster. A computational study has been conducted to analyze the effect of the metal on these concerted [3+2] cycloaddition reactions. The calculations suggest that the reactions of cluster [2](+) with alkynes feature ΔG(≠) values only slightly larger than its molybdenum analogue, however, the differences in the reaction free energies between both metal clusters and the same alkyne reach up to approximately 10 kcal mol(-1) , therefore indicating that the differences in the reactivity are essentially thermodynamic. The activation strain model (ASM) has been used to get more insights into the critical effect of the metal center in these cycloadditions, and the results reveal that the change in reactivity is entirely explained on the basis of the differences in the interaction energies Eint between the cluster and the alkyne. Further decomposition of the Eint values through the localized molecular orbital-energy decomposition analysis (LMO-EDA) indicates that substitution of the Mo atoms in cluster [1](+) by W induces changes in the electronic structure of the cluster that result in weaker intra- and inter-fragment orbital interactions.

  1. Complicating osteomyelitis imaged with Tc-99m MDP, In-111 granulocytes, and Ga-67 citrate

    Energy Technology Data Exchange (ETDEWEB)

    Schauwecker, D.S.; Park, H.M.; Mock, B.H.; Burt, R.W.; Kernick, C.B.; Ruoff, A.C. III; Sinn, H.J.; Wellman, H.N.; Vamc, R.L.R.

    1984-01-01

    Gallium-67 and 3-phase bone scan (3P) studies, though very sensitive, are not very specific in evaluating suspected osteomyelitis (OM) which is superimposed upon other diseases that cause increased bone turnover (IBT). The authors compared In-111 acetylacetone labeled granulocytes (In-111) GRAN) with 3P in 57 such patients; 29 of these patients had Ga-67 studies as well. In-111 GRAN had a sensitivity of 100% in acute OM, 62% in chronic OM, and a specificity of 96%. Gallium-67 ruled out OM when the study was normal; it diagnosed OM when the relative uptake of Ga-67 exceeded the uptake of Tc-99m MDP, or when the skeletal distribution of Ga-67 was different from that of the TC-99m MDP. Unfortunately, these criteria were met in only 28% of the subjects. The simple approach of increased Ga-67 activity meant OM gave a sensitivity of 100%, but an unacceptable specificity of 38%. Chronic cellulitis or long-standing decubiti were seldom detected by IN-111 GRAN. Clinically obvious soft tissue infections or cellulitis were seen with In-111 GRAN 27% of the time, and 17% of the time with Ga-67. The authors conclude that when added to 3P, In-111 GRAN provided more useful information than did Ga-67. A combination of all 3 studies did not significantly increase the diagnostic yield. Performing In-111 GRAN without 3P in patients with IBT is not recommended since the 3P provides anatomic information that aids in the differentiation of OM from soft tissue infections.

  2. Enhancement of oxygen reduction activity of nanoshell carbons by introducing nitrogen atoms from metal phthalocyanines

    Energy Technology Data Exchange (ETDEWEB)

    Ozaki, Jun-ichi, E-mail: jozaki@cee.gunma-u.ac.j [Department of Chemical and Environmental Engineering, Graduate School of Engineering, Gunma University, 1-5-1, Tenjin-cho, Kiryu, Gunma 376-8515 (Japan); Tanifuji, Shin-ichi; Furuichi, Atsuya; Yabutsuka, Katsutoshi [Department of Chemical and Environmental Engineering, Graduate School of Engineering, Gunma University, 1-5-1, Tenjin-cho, Kiryu, Gunma 376-8515 (Japan)

    2010-02-15

    Nanoshell carbon is a type of catalytically grown nanocarbon with a hollow, round, shell-like structure, with a diameter in the range of approximately 20-50 nm. It has been shown to possess the electrocatalytic activity for oxygen reduction reaction (ORR) and is also expected to be a non-Pt catalyst for polymer electrolyte fuel cells. This paper reports the synergetic enhancement of the ORR activity of nanoshell carbons caused by the coexistence of nitrogen atoms. The nanoshell carbons were prepared by the carbonization of furan resin in the presence of acetylacetonates (AAs) and of phthalocyanines (Pcs), which contained Fe, Co, and Ni. The Pc-derived nanoshells (MP-T series; M = Co or Fe, T = carbonization temperature) showed higher ORR activities than the AA-derived nanoshells (MA-T series; M = Co or Fe, T = carbonization temperature) when the same metal elements were employed. An XPS study revealed that nitrogen species were introduced to the surface of the nanoshells when Pcs were used as the nanoshell-forming catalysts, and that no metal species remained on the nanoshells. Principally, the ORR activity of the carbons was governed by the presence of the nanoshells and further enhancement could be achieved by the introduction of nitrogen atoms. 0.78 V of OCV and 0.21 W cm{sup -2} of the maximum power density were observed for a fuel cell whose MEA consisted of 3CoP1000 cathode and a commercial Pt/C anode, when it was operated at 80 deg. C under a pressurized condition of 0.35 MPa.

  3. Study of atomic layer deposition of indium oxy-sulfide films for Cu(In,Ga)Se{sub 2} solar cells

    Energy Technology Data Exchange (ETDEWEB)

    Bugot, Cathy, E-mail: cathy-externe.bugot@edf.fr [Institut de Recherche et Développement sur l' Energie Photovoltaïque (IRDEP, UMR 7174 CNRS-EDF-Chimie Paristech), Chatou (France); Schneider, Nathanaelle [Institut de Recherche et Développement sur l' Energie Photovoltaïque (IRDEP, UMR 7174 CNRS-EDF-Chimie Paristech), Chatou (France); Bouttemy, Muriel; Etcheberry, Arnaud [Institut Lavoisier de Versailles, UMR 8180 (CNRS-UVSQ), Versailles (France); Lincot, Daniel; Donsanti, Frédérique [Institut de Recherche et Développement sur l' Energie Photovoltaïque (IRDEP, UMR 7174 CNRS-EDF-Chimie Paristech), Chatou (France)

    2015-05-01

    This paper explores the growth mechanism of plasma enhanced atomic layer deposition of In{sub 2}(S,O){sub 3} films. The films were deposited using indium acetylacetonate (In(acac){sub 3}), hydrogen sulfide (H{sub 2}S) and Ar/O{sub 2} plasma as oxygen precursor. The films were characterized using X-ray reflectometry, spectrophotometry, energy dispersive X-ray spectroscopy and X-ray photoelectron spectroscopy. To understand the growth mechanism and especially the interactions between Ar/O{sub 2} plasma and In{sub 2}(S,O){sub 3} growing film, in-situ analyses were performed using quadrupole mass spectrometry. In-situ qualitative analysis revealed good correlation between the species detected in vapor phase and thin film properties. High concentrations of atomic and molecular oxygen were measured in the vapor phase during O{sub 2} plasma pulses. Significant decrease of these species could be observed by varying the plasma power from 2600 to 300 W, while the optical band gap remained at high values (> 2.6 eV). The analysis of the O{sub 2}-free/Ar plasma process showed that some of these oxygen species originate either from the indium precursor or from the substrate surface. This study explains the high oxygen content of the films, and allows us to reduce and control it. Generally, this report provides keys to understand the effect of plasma reactivity for the elaboration of oxide based materials. - Highlights: • In{sub 2}(S,O){sub 3} films were synthesized by plasma enhanced atomic layer deposition. • Growth mechanism was studied via gas phase analysis by Quadrupole Mass Spectrometry. • Good correlation between the vapor phase species and thin films properties was observed. • The film compositions and band gaps can be controlled by varying the plasma power.

  4. Development of a biocompatible magnetic nanofluid by incorporating SPIONs in Amazonian oils

    Science.gov (United States)

    Gaspar, André S.; Wagner, Friedrich E.; Amaral, Vítor S.; Costa Lima, Sofia A.; Khomchenko, Vladimir A.; Santos, Judes G.; Costa, Benilde F. O.; Durães, Luísa

    2017-02-01

    Higher quality magnetic nanoparticles are needed for use as magnetic nanoprobe in medical imaging techniques and cancer therapy. Moreover, the phytochemistry benefits of some Amazonian essential oils have sparked great interest for medical treatments. In this work, a magnetic nanoprobe was developed, allying the biocompatibility and superparamagnetism of iron oxide nanoparticles (SPIONs) with benefits associated with Amazonian oils from Copaiba and Andiroba trees. SPIONs were obtained by two thermal decomposition procedures and different amounts of precursors (iron acetylacetonates). Their characterization was accomplished by Fourier transform infrared spectroscopy, thermogravimetric analysis, transmission electron microscopy (TEM), X-ray diffraction (XRD), Mössbauer spectroscopy and magnetization. The obtained nanoparticles composition and magnetic properties were not affected by the relative proportion of iron(II) and iron(III) in the precursor system. However, when changing the reducing and stabilizing agents the coating layer shows different compositions/relative weight - the more promising SPIONs have a coating mainly composed by oleylamine and an iron oxide:coating wt% ratio of 55:45. Nanoparticles size distributions were very narrow and centred in the average size of 6-7 nm. Cellular assays confirmed the biocompatibility of SPIONs and their effective internalization in human colon cancer cells. Mössbauer/XRD results indicated maghemite as their main iron oxide phase, but traces of magnetite proved to be present. Magnetization saturations of 57 emu/g at 5 K and 42 emu/g at 300 K were achieved. With incorporation of SPIONs into Copaiba and Andiroba essential oils, these values show a 4-fold decrease, but the supermagnetic behaviour is preserved providing the effective formation of a nanofluid.

  5. Boosting the photocurrent density of p-type solar cells based on organometal halide perovskite-sensitized mesoporous NiO photocathodes.

    Science.gov (United States)

    Wang, Huan; Zeng, Xianwei; Huang, Zhanfeng; Zhang, Wenjun; Qiao, Xianfeng; Hu, Bin; Zou, Xiaoping; Wang, Mingkui; Cheng, Yi-Bing; Chen, Wei

    2014-08-13

    The p-n tandem design of a sensitized solar cell is a novel concept holding the potential to overcome the efficiency limitation of conventional single-junction sensitized solar cells. Significant improvement of the photocurrent density (Jsc) of the p-type half-cell is a prerequisite for the realization of a highly efficient p-n tandem cell in the future. This study has demonstrated effective photocathodes based on novel organometal halide perovskite-sensitized mesoporous NiO in liquid-electrolyte-based p-type solar cells. An acceptably high Jsc up to 9.47 mA cm(-2) and efficiency up to 0.71% have been achieved on the basis of the CH3NH3PbI3/NiO solar cell at 100 mW cm(-2) light intensity, which are significantly higher than those of any previously reported liquid-electrolyte-based p-type solar cells based on sensitizers of organic dyes or inorganic quantum dots. The dense blocking layer made by spray pyrolysis of nickel acetylacetonate holds the key to determining the current flow direction of the solar cells. High hole injection efficiency at the perovskite/NiO interface and high hole collection efficiency through the mesoporous NiO network have been proved by time-resolved photoluminescence and transient photocurrent/photovoltage decay measurements. The limitation of these p-type solar cells primarily rests with the adverse light absorption by the NiO mesoporous film; the secondary limitation arises from the highly viscous ethyl acetate-based electrolyte, which is helpful for the solar cell stability but hinders fluent diffusion into the pore channels, giving rise to a nonlinear dependence of Jsc on the light intensity.

  6. Validation of a standardised method for determining beryllium in human urine at nanogram level.

    Science.gov (United States)

    Devoy, Jérôme; Melczer, Mathieu; Antoine, Guillaume; Remy, Aurélie; Heilier, Jean-François

    2013-10-01

    The potential toxicity of beryllium at low levels of exposure means that a biological and/or air monitoring strategy may be required to monitor the exposure of subjects. The main objective of the work presented in this manuscript was to develop and validate a sensitive and reproducible method for determining levels of beryllium in human urine and to establish reference values in workers and in non-occupationally exposed people. A chelate of beryllium acetylacetonate formed from beryllium(II) in human urine was pre-concentrated on a SPE C18 cartridge and eluted with methanol. After drying the eluate, the residue was solubilised in nitric acid and analysed by atomic absorption spectrometry and/or inductively coupled plasma mass spectrometry. The proposed method is 4 to 100 times more sensitive than other methods currently in routine use. The new method was validated with the concordance correlation coefficient test for beryllium concentrations ranging from 10 to 100 ng/L. Creatinine concentration, urine pH, interfering compounds and freeze-thaw cycles were found to have only slight effects on the performance of the method (less than 6%). The effectiveness of the two analytical techniques was compared statistically with each other and to direct analysis techniques. Even with a detection limit of 0.6 ng/L (obtained with inductively coupled plasma mass spectrometry), the method is not sensitive enough to detect levels in non-occupationally exposed persons. The method performance does however appear to be suitable for monitoring worker exposure in some industrial settings and it could therefore be of use in biological monitoring strategies.

  7. Hypersensitivity in the 4f-4f absorption spectra of tris (acetylacetonato) neodymium(III) complexes with imidazole and pyrazole in non-aqueous solutions. Effect of environment on hypersensitive transitions

    Energy Technology Data Exchange (ETDEWEB)

    Ansari, Anees A.; Ilmi, Rashid [Department of Chemistry, Jamia Millia Islamia, New Delhi 110025 (India); Iftikhar, K., E-mail: kiftikhar.ch@jmi.ac.in [Department of Chemistry, Jamia Millia Islamia, New Delhi 110025 (India)

    2012-01-15

    The optical absorption spectra of [Nd(acac){sub 3}(H{sub 2}O){sub 2}].H{sub 2}O, [Nd(acac){sub 3}(im){sub 2}] and [Nd(acac){sub 3}(pz){sub 2}] (where acac is the anion of acetylacetone, im is imidazole and pz is pyrazole) complexes in the visible region have been analyzed. The transition {sup 4}G{sub 5/2} <- {sup 4}I{sub 9/2} located near the middle of the visible region (17,500 cm{sup -1}) is hypersensitive. Its behavior is in sharp contrast to many other typically weak and consistently unvaried, normal 4f-4f transitions. It is overlapped by a less intense transition {sup 2}G{sub 7/2} <- {sup 4}I{sub 9/2}. The band shapes of the hypersensitive transition show remarkable changes on passing from aqueous solution to various non-aqueous solutions, which is the result of changes in the environment about the Nd(III) ion in the various solutions and suggests coordination of a solvent molecules. Pyridine has been found especially effective in promoting 4f-4f electric-dipole intensity. The DMSO invades the complexes and replaces the water molecules and heterocyclic amines from the coordination sphere. Two DMSO molecules coordinate and the complexes acquire similar structure, [Nd(acac){sub 3}(DMSO){sub 2}] in solution. The oscillator strength and the band shape of the hypersensitive transition of all the complexes remains the same in this solvent. The IR spectra and the NMR spectra of the complexes have also discussed. - Highlights: > Structurally similar eight-coordinate complexes of neodymium are synthesized. > The 4f-4f absorption spectra are investigated in non-aqueous solvents. > Methanol, isopropanol and acetonitrile are coordinating solvents. > Pyridine and DMSO are coordinating solvents by replacing the ancillary ligands. > Pyridine is most effective in promoting the 4f-4f intensity.

  8. 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)

  9. Controllable Synthesis of Monodispersed Middle and Heavy Rare Earth Oxysulfide Nanoplates Based on the Principles of HSAB Theory%基于软硬酸碱理论的单分散中重稀土硫氧化物纳米板的可控合成

    Institute of Scientific and Technical Information of China (English)

    顾均; 丁祎; 柯俊; 张亚文; 严纯华

    2013-01-01

    Based on the theory of hard and soft acids and bases, trivalent ions of middle and heavy rare earths belong to very hard acids, which possess weak affinity towards S2- ions but strong affinity to O2- ions. So it is difficult to synthesize middle and heavy rare earth oxysulfide nano-materials through the thermolysis method in high-boiling-point organic solvent. In this article, monodispersed oxysulfide nanoplates of Y, Eu, Gd, Er and Yb were synthesized through this thermolysis method we developed. Both sodium-doped and undoped rare earth oxysulfide nanoplates could be prepared, and the doping of sodium ions could promote the crystallization of the nanoplates. Rare earth acetylacetonates were used as metal precursors and H2S gas as the sulfurizing reagent. The reactions were conducted in oleylamine at 280 °C for 1 hour. The thermogravimetric analysis of the precursor showed that the initial decomposition temperature of the rare earth acetylacetonates is about 200 'C, which is much lower than that of rare earth oleates. The transmission electron microscopy observation and energy dispersive X-ray analyses of the intermediate products during the synthesis of the nanoplates showed that rare earth oxide nanoplates formed firstly at about 220 °C, and these nanoplates transformed to oxysulfide nanoplates gradually during the temperature ramping period. Density functional theory calculation was used to compare the total free energy of the oxide and oxysulfide of different rare earth elements. According to this thermodynamical comparison, we concluded that, from light rare earths to heavy rare earths, higher chemical potential of sulfur is needed to obtain the oxysulfide rather than oxide. On one hand, H2S gas has higher sulphurizing power than sulfur. On the other hand, a comparatively low reaction temperature favors the dissolving of H2S in oleylamine. As a result, the chemical potential of sulfur in synthetic system could be effectively increased by using rare earth

  10. Synthesis and Characterization of In (acac)3 and Sn (acac)2 Cl2%In(acac)3和 Sn(acac)2 Cl2的合成及表征

    Institute of Scientific and Technical Information of China (English)

    喻德翔; 郑萍; 常桥稳; 赵群

    2014-01-01

    This paper introduced the synthesis methods of two important raw materials (In(acac)3 and Sn(acac)2 Cl2 )for the synthesis of nanoparticles ITO (Indium Tin Oxides).By InCl3 ·4H2 O as raw material under stirring at pH =9.0 in citric acid solution,In(acac)3 was synthesized;and by SnCl4 ·4H2 O and acetylacetone as raw materials,refluxing in toluene,Sn(acac)2 Cl2 was prepared.The synthesized prod-ucts were characterized through NMR,crystal -XRD.The effects of various experimental conditions on the synthesis reaction were discussed and the best condition was established as citric acid solution with a concen-tration of 84mmol·L -1 ,pH value of 9.0.By toluene as the best solvent for preparation of Sn (acac)2 Cl2 .%介绍了化学法制备氧化铟锡(ITO)纳米材料的两个重要合成原料 In(acac)3和 Sn (acac)2 Cl2的合成方法。以 InCl3·4H2 O 为原料,在 pH 值为9.0的柠檬酸溶液中制备 In(acac)3;以SnCl4·5H2 O 与乙酰丙酮为原料,在甲苯溶剂中加热回流制备 Sn(acac)2 Cl2。通过 IR、NMR、XRD 检测手段对合成的产物进行表征分析。讨论了各种实验条件对合成反应的影响,总结出 In(acac)3的最佳合成条件是:柠檬酸浓度为84 mmol·L -1,pH 值为9.0;制取 Sn(acac)2 Cl2的最佳溶剂是甲苯。

  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. Photo-induced DNA cleavage activity and remarkable photocytotoxicity of lanthanide(III) complexes of a polypyridyl ligand.

    Science.gov (United States)

    Hussain, Akhtar; Gadadhar, Sudarshan; Goswami, Tridib K; Karande, Anjali A; Chakravarty, Akhil R

    2012-01-21

    Lanthanide(III) complexes [Ln(pyphen)(acac)(2)(NO(3))] (1, 2), [Ln(pydppz)(acac)(2)(NO(3))] (3, 4) and [La(pydppz)(anacac)(2)(NO(3))] (5), where Ln is La(III) (in 1, 3, 5) and Gd(III) (in 2, 4), pyphen is 6-(2-pyridyl)-1,10-phenanthroline, pydppz is 6-(2-pyridyl)-dipyrido[3,2-a:2',3'-c]phenazine, anacac is anthracenylacetylacetonate and acac is acetylacetonate, were prepared, characterized and their DNA photocleavage activity and photocytotoxicity studied. The crystal structure of complex 2 displays a GdO(6)N(3) coordination. The pydppz complexes 3-5 show an electronic spectral band at ~390 nm in DMF. The La(III) complexes are diamagnetic, while the Gd(III) complexes are paramagnetic with seven unpaired electrons. The molar conductivity data suggest 1 : 1 electrolytic nature of the complexes in aqueous DMF. They are avid binders to calf thymus DNA giving K(b) in the range of 5.4 × 10(4)-1.2 × 10(6) M(-1). Complexes 3-5 efficiently cleave supercoiled DNA to its nicked circular form in UV-A light of 365 nm via formation of singlet oxygen ((1)O(2)) and hydroxyl radical (HO˙) species. Complexes 3-5 also exhibit significant photocytotoxic effect in HeLa cancer cells giving respective IC(50) value of 0.16(±0.01), 0.15(±0.01) and 0.26±(0.02) μM in UV-A light of 365 nm, while they are less toxic in dark with an IC(50) value of >3 μM. The presence of an additional pyridyl group makes the pydppz complexes more photocytotoxic than their dppz analogues. FACS analysis of the HeLa cells treated with complex 4 shows apoptosis as the major pathway of cell death. Nuclear localization of complex 5 having an anthracenyl moiety as a fluorophore is evidenced from the confocal microscopic studies.

  13. Photophysical and photocatalytic properties of Bi{sub 2}MNbO{sub 7} (M = Al, In, Ga, Fe) thin films prepared by dip-coating

    Energy Technology Data Exchange (ETDEWEB)

    Ropero-Vega, J.L., E-mail: jlropero@ciencias.uis.edu.co [Centro de Investigaciones en Catalisis - CICAT, Universidad Industrial de Santander - UIS, Sede Guatiguara Km. 2 via El Refugio, C.P. 681011, Piedecuesta (Santander) (Colombia); Rosas-Barrera, K.L. [Grupo de Investigaciones en Minerales, Biohidrometalurgia y Ambiente - GIMBA, Universidad Industrial de Santander - UIS, Sede Guatiguara Km. 2 via El Refugio, C.P. 681011, Piedecuesta (Santander) (Colombia); Pedraza-Avella, J.A. [Centro de Investigaciones en Catalisis - CICAT, Universidad Industrial de Santander - UIS, Sede Guatiguara Km. 2 via El Refugio, C.P. 681011, Piedecuesta (Santander) (Colombia); Laverde-Catano, D.A., E-mail: dlaverde@uis.edu.co [Grupo de Investigaciones en Minerales, Biohidrometalurgia y Ambiente - GIMBA, Universidad Industrial de Santander - UIS, Sede Guatiguara Km. 2 via El Refugio, C.P. 681011, Piedecuesta (Santander) (Colombia); Pedraza-Rosas, J.E. [Grupo de Investigaciones en Minerales, Biohidrometalurgia y Ambiente - GIMBA, Universidad Industrial de Santander - UIS, Sede Guatiguara Km. 2 via El Refugio, C.P. 681011, Piedecuesta (Santander) (Colombia); Nino-Gomez, M.E. [Centro de Investigaciones en Catalisis - CICAT, Universidad Industrial de Santander - UIS, Sede Guatiguara Km. 2 via El Refugio, C.P. 681011, Piedecuesta (Santander) (Colombia)

    2010-10-25

    In this work we report the preparation and characterization of Bi{sub 2}MNbO{sub 7} (M = Al, Ga, In, Fe) transparent thin films on glass slides. The films were obtained by dip-coating using bismuth(III) acetate, niobium(V) ethoxide and the corresponding metal(III) acetylacetonate precursors. Crystal structure and elemental analysis were performed by X-ray diffraction (XRD) and energy dispersive X-ray fluorescence (EDXRF). The band-gap energy (E{sub g}) of the semiconductor films was estimated by UV-vis spectroscopy. Their photocatalytic activity was evaluated in the degradation of methyl orange (MeO) in aqueous solution. The presence of a crystalline phase in the Bi-M-Nb-O (M = Al, Ga, In, Fe) systems with pyrochlore-type structure was suggested by the diffraction peak at 2{theta} {approx} 29.01. The elemental proportion in the Bi-Ga-Nb-O film fits better to the stoichiometric ratio in Bi{sub 2}MNbO{sub 7}. The estimated E{sub g} values were: Bi{sub 2}FeNbO{sub 7} (2.47 eV) < Bi{sub 2}GaNbO{sub 7} (2.67 eV) < Bi{sub 2}AlNbO{sub 7} (2.79 eV) < Bi{sub 2}InNbO{sub 7} (3.01 eV) and the calculated kinetic parameter t{sub 1/2} were: Bi{sub 2}GaNbO{sub 7} (239 min) < Bi{sub 2}AlNbO{sub 7} (278 min) < Bi{sub 2}InNbO{sub 7} (296 min) < Bi{sub 2}FeNbO{sub 7} (319 min). These results indicate that a slight band-gap narrowing has a positive effect in the photocatalytic properties but those further than E{sub g} < 2.5 eV has a detrimental effect.

  14. Electronic state of ruthenium deposited onto oxide supports: An XPS study taking into account the final state effects

    Science.gov (United States)

    Larichev, Yurii V.; Moroz, Boris L.; Bukhtiyarov, Valerii I.

    2011-12-01

    The electronic state of ruthenium in the supported Ru/EOx (EOx = MgO, Al2O3 or SiO2) catalysts prepared by with the use of Ru(OH)Cl3 or Ru(acac)3 (acac = acetylacetonate) and reduced with H2 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 3d5/2 core level measured for supported Ru nanoparticles is estimated by comparison of the Fermi levels and the modified Auger parameters determined for the Ru/EOx samples with the corresponding characteristics of the bulk Ru metal. It is found that the negative shift of the Ru 3d5/2 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-Al2O3 and SiO2 (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/EOx 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.

  15. The effect of precursors salts on surface state of Pd/Al2O3 and Pd/CeO2/Al2O3 catalysts

    Directory of Open Access Journals (Sweden)

    André L. Guimarães

    2004-12-01

    Full Text Available The influence of the precursors on the promoting effect of ceria on Pd/Al2O3 catalyst, when ceria is coated over alumina was studied. The reaction of propane oxidation proceeded under different feed conditions and the surface active sites were characterized by X-ray photoelectron spectroscopy (XPS and in situ diffuse reflectance spectroscopy (DRS. XPS and DRS results show that PdO/Pd0 interface are the active sites independent of the precursor, while the catalysts containing CeO2 showed formation of palladium species in the highest oxidation state, probably PdO2 (338 eV after the oxidation of propane. Besides, the O/Al and O/Ce ratios evidenced the increase of oxygen storage in the presence of CeO2. In addition, the precursor acetylacetonate favors the oxygen storage in the lattice.Estudo da influência dos precursores sobre os catalisadores de Pd/Al2O3 promovidos com céria ancorado sobre a alumina. A oxidação do propano foi feita sob diferentes condições de alimentação sendo caracterizados os sítios superficiais por Espectroscopia Fotoeletrônica de raios X (XPS e por Refletância Difusa em ''situ''. Resultados de XPS e DRS mostraram a formação de interfaces de PdO/Pd0 como sendo os sítios ativos, independentes do precursor utilizado na preparação, enquanto que os catalisadores contendo CeO2 mostraram a formação de espécies de paládio com estado de oxidação mais altos, provavelmente PdO2 (338 eV após a oxidação do propano. Além disso, as razões O/Al e O/Ce evidenciaram um aumento de oxigênio armazenado na presença de CeO2. O precursor acetilacetonato favoreceu o armazenamento de oxigênio na rede.

  16. Chelate Ring Size Effect as a Factor of Selective Fluorescent Recognition of Zn(2+) Ions by Pyrrolo[2,3-b]quinoxaline with a Substituted 2-Pyridyl Group Receptor.

    Science.gov (United States)

    Ostrowska, Katarzyna; Musielak, Bogdan; Szneler, Edward; Dudek, Łukasz; Gryl, Marlena; Stadnicka, Katarzyna

    2015-09-01

    Analysis of the spectral properties and structural differences of two turn-on ratiometric fluorescent receptors for Zn(2+) and Cd(2+) ions, derivatives of pyrrolo[2,3-b]quinoxaline (2), and earlier published 3 (Ostrowska et al. CrystEngComm 2015, 17, 498-502) was performed. Both ligands are E/Z push-pull olefins interconverting at room temperature, with barriers to rotation about enamine double bonds, from E to Z isomers of 19.3 ± 0.1 and 16.9 ± 0.3 kcal/mol and from Z to E of 16.9 ± 0.3 and 15.7 ± 0.2 kcal/mol, respectively. Diastereoisomers (E)-2 and (Z)-2 were isolated and characterized by X-ray structural analysis. The formation of complexes by (E/Z)-2 with acetates and acetylacetonates of Zn(2+) and Cd(2+) was monitored by UV-vis, fluorescence, and (1)H NMR titrations in acetonitrile, respectively. X-ray structural analysis for isolated [(E)-2]2Zn in relation to earlier published (E)-3-ZnOAc revealed the formation of a six-coordinated zinc ion with six- and four-membered bis-chelate rings by (E)-2. The chelate effect increases the ligand affinity for Zn(2+) (log β12 = 12.45) and causes the elongation of nitrogen-metal bonds. Extension of the coordination cavity size allows coordination of a cadmium ion. The introduction of a flexible ethylene linker between the fluorophore and ionophore pyridyl groups in 3 significantly affects the selectivity of zinc-ion recognition. The distorted tetrahedral geometry of (E)-3-ZnOAc with a four-coordinated zinc ion appears to be the most preferred because of the short donor-zinc distance with a 1:1 binding mode. The formation of the small coordination cavity size with six-membered bis-chelate rings provides an effective overlap of zinc and donor orbitals, precluding the coordination of a cadmium ion in the same manner as zinc.

  17. Sonochemical precipitation of amorphous uranium phosphates from trialkyl phosphate solutions and their thermal conversion to UP2O7.

    Science.gov (United States)

    Doroshenko, Iaroslav; Zurkova, Jana; Moravec, Zdenek; Bezdicka, Petr; Pinkas, Jiri

    2015-09-01

    Insoluble amorphous precipitates containing uranyl and phosphate ions are obtained by sonication of solutions of three uranyl precursors, UO2(X)2, X=NO3, CH3COO, CH3C(O)CHC(O)CH3 (acetylacetonate, acac), in triesters of phosphoric acid, OP(OR)3, R=Me (trimethyl phosphate, TMP), Et (triethyl phosphate, TEP). TMP and TEP are used as high-boiling solvents and they serve also as a source of phosphate anions. Sonolysis experiments were carried out under flow of Ar at 40°C on a Sonics and Materials VXC 500W system (f=20 kHz, Pac=0.49 W cm(-3)). Powder X-ray diffraction (PXRD) reveals amorphous character of all obtained precipitates. The presence of uranyl and phosphate is evidenced by IR spectroscopy and ICP-OES analysis reveals the content of both U (38.6-43.4 wt%) and P (11.0-13.6 wt%). The thermal behavior of the substances was studied by TG/DSC analysis, which shows weight losses in the range of 19.21-24.08%. On heating the amorphous precipitates to 1000°C, crystalline uranium diphosphate UP2O7 is obtained in all cases as the only crystalline phase. Uranyl(VI) is reduced during thermolysis to U(IV) as there is no characteristic vibration of UO2(2+) in the IR spectra of solid UP2O7 products. The ICP-OES analysis of U and P content in precipitates allowed us to calculate the efficiency of precipitation of uranium from mother liquor and to compare it with the efficiency calculated from the data received by the PXRD and TG/DSC analyses. The efficiency of the uranium removal attained by our sonoprecipitation procedure was typically 30-35%. These sonochemical precipitation reactions providing insoluble uranium phosphates may be potentially interesting models for the description of behavior of uranium-containing waste or reprocessing streams.

  18. 溴酸钾-苯酚红体系催化动力学光度法测定食品中的痕量甲醛%Determination of Trace Formaldehyde in Foods with Catalytic Kinetic Spectrophotometry in Potassium Bromate-Phenol Red System

    Institute of Scientific and Technical Information of China (English)

    严进

    2015-01-01

    A catalytic spectrophotometric method for the determination of trace formaldehyde is established based on the inhibitory effect of formaldehyde on the oxidation of phenol red by potassium bromate in H2SO4 medium. The optimum kinetic condition of the catalytic reaction has been investigated. The wavelength for the determination is 380 nm, and the linear range for determination of formaldehyde is 0.02~0.32 μg/mL with the detection limit of 6.10×10-9 g/mL.v The results from the studies suggest that the catalytic reaction is zero-or-der and the apparent activation energy of this reaction is 38.87 kJ/mol,and the apparent rate constant is k=9.1×10-4s-1. The procedure has been used to determine formaldehyde in foods, with the relative standard devi-ation of below 3.9%and the average recovery of 96.3 %~105.5 %. Results obtained by this method are con-sistent with the results found by the acetylacetone photometry.%基于溴酸钾在硫酸介质中可氧化苯酚红,甲醛的加入催化该氧化反应的进行,从而使溴酸钾氧化苯酚红的速度明显加快,据此建立了测定食品中痕量甲醛的新催化动力学分光光度法,并研究了该催化褪色反应的最佳动力学条件和参数。在测定波长380 nm下,测定方法的线性范围0.02~0.32滋g/mL,检出限为6.10×10-9 g/mL。催化反应为动力学零级反应,表现活化能为38.87 kJ/mol,催化反应速率常数k=9.1×10-4s-1。运用所建立的方法测定食品中痕量甲醛,相对标准偏差小于3.9%,回收率在96.3%~105.5%,表明该方法测得的结果与乙酰丙酮光度法所测结果一致。

  19. Secondary brown carbon - Formation of light-absorbing compounds in atmospheric particulates from selected dicarbonyls and amines

    Science.gov (United States)

    Kampf, Christopher; Filippi, Alexander; Hoffmann, Thorsten

    2015-04-01

    One of the main open questions regarding organic compounds in atmospheric chemistry today is related to the formation of optically-active compounds and the occurrence of so called brown carbon (Andreae and Gelencsér, 2006). While organic compounds in ambient fine particles for decades have been assumed to not absorb solar radiation, thus resulting in a net cooling effect on climate (IPCC, 2007), it is now generally accepted that a continuum of light-absorbing carbonaceous species is present in fine aerosols (Pöschl, 2003). In this study, light-absorbing compounds from reactions between dicarbonyl compounds, i.e., glyoxal, methylglyoxal, acetylacetone, 2,3-butanedione, 2,5-hexanedione, and glutaraldehyde, and amine species, i.e., ammonia and glycine, were investigated at atmospherically relevant concentrations in bulk solution experiments mimicking atmospheric particulates. Product analyses were performed using UV/Vis spectrophotometry and (ultra) high performance liquid chromatography coupled to diode array detection and ion trap mass spectrometry (HPLC-DAD-ESI-MS/MS), as well as ultra-high resolution (Orbitrap) mass spectrometry (UHPLC-ESI-HRMS/MS). We demonstrate that light-absorbing compounds are formed from a variety of atmospherically relevant dicarbonyls via particle phase reactions with amine nucleophiles. Single dicarbonyl and mixed dicarbonyl experiments were performed and products were analyzed. The reaction products are suggested to be cyclic nitrogen containing compounds such as imidazoles or dihydropyridines as well as open chain compounds resulting from aldol condensation reactions. Further, the reactive turnover was found to be higher at increasing pH values. The aforementioned processes may be of higher relevance in regions with high aerosol pH, e.g., resulting from high ammonia emissions as for example in northern India (Clarisse et al., 2009). References Andreae, M.O., and Gelencsér, A. (2006): Black carbon or brown carbon? The nature of light

  20. The Preparation of TiO2 Thin Films with Level Sedimentation and Its Properties%液位沉降法制备 Ti O2薄膜及其性能研究

    Institute of Scientific and Technical Information of China (English)

    殷天兰; 武光明; 高德文; 丁尧; 姚天宇

    2014-01-01

    以钛酸丁酯为前驱液,无水乙醇为溶剂,乙酰丙酮为稳定剂,制备了 T iO 2溶胶,采用液位沉降法在清洁的玻璃衬底上镀制T iO 2薄膜。研究了添加剂聚乙二醇(1000)、p H、衬底温度对 T iO 2溶胶在玻璃基板上附着性的影响;研究了液位沉降速度、容器倾角以及溶胶附着性对T iO 2薄膜厚度的影响。考察了TiO2薄膜的表面形貌、晶相、光催化性能。结果表明,采用PEG与 Ti4+的质量比为1,不调节pH的TiO2溶胶,在沉降速度为7 cm/min ,容器倾角为30°所制得的TiO2薄膜的光催化性能最好,光照3 h时其光催化降解率高达52.1%。%TiO2 sol was prepared with butyl titanate as precursor solution ,anhydrous ethanol as solvent ,acetylacetone as the stabilizer .TiO2 thin film was coated on a clean glass substrate by level sedimentation method .The effect of Polyethylene glycol (1 000) as the additives ,pH and the substrate temperature on the adhesion between TiO 2 sol and the glass substrate was studied . The influence of level sedimentation velocity ,container angle and the adhesion on TiO2 thin film thickness was also studied .The surface morphology ,crystal phase ,and the photocatalytic per-formance of TiO2 thin films were researched too .The results showed that when the PEG with Ti4+ mass ratio was 1 ,the pH value was not adjusted ,the settling velocity was 7 cm/min ,the container angle was 30° ,the photocatalytic properties of TiO2 thin film was the best ,which was as high as 52.1% after being lighted for 3 hours .