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Sample records for bases synthesis characterization

  1. Boron-based nanostructures: Synthesis, functionalization, and characterization

    Science.gov (United States)

    Bedasso, Eyrusalam Kifyalew

    Boron-based nanostructures have not been explored in detail; however, these structures have the potential to revolutionize many fields including electronics and biomedicine. The research discussed in this dissertation focuses on synthesis, functionalization, and characterization of boron-based zero-dimensional nanostructures (core/shell and nanoparticles) and one-dimensional nanostructures (nanorods). The first project investigates the synthesis and functionalization of boron-based core/shell nanoparticles. Two boron-containing core/shell nanoparticles, namely boron/iron oxide and boron/silica, were synthesized. Initially, boron nanoparticles with a diameter between 10-100 nm were prepared by decomposition of nido-decaborane (B10H14) followed by formation of a core/shell structure. The core/shell structures were prepared using the appropriate precursor, iron source and silica source, for the shell in the presence of boron nanoparticles. The formation of core/shell nanostructures was confirmed using high resolution TEM. Then, the core/shell nanoparticles underwent a surface modification. Boron/iron oxide core/shell nanoparticles were functionalized with oleic acid, citric acid, amine-terminated polyethylene glycol, folic acid, and dopamine, and boron/silica core/shell nanoparticles were modified with 3-(amino propyl) triethoxy silane, 3-(2-aminoethyleamino)propyltrimethoxysilane), citric acid, folic acid, amine-terminated polyethylene glycol, and O-(2-Carboxyethyl)polyethylene glycol. A UV-Vis and ATR-FTIR analysis established the success of surface modification. The cytotoxicity of water-soluble core/shell nanoparticles was studied in triple negative breast cancer cell line MDA-MB-231 and the result showed the compounds are not toxic. The second project highlights optimization of reaction conditions for the synthesis of boron nanorods. This synthesis, done via reduction of boron oxide with molten lithium, was studied to produce boron nanorods without any

  2. [Synthesis and Characterization of a Sugar Based Electrolyte for Thin-film Polymer Batteries

    Science.gov (United States)

    1998-01-01

    The work performed during the current renewal period, March 1,1998 focused primarily on the synthesis and characterization of a sugar based electrolyte for thin-film polymer batteries. The initial phase of the project involved developing a suitable sugar to use as the monomer in the polymeric electrolyte synthesis. The monomer has been synthesized and characterized completely. Overall the yield of this material is high and it can be produced in relatively large quantity easily and in high purity. The scheme used for the preparation of the monomer is outlined along with pertinent yields.

  3. Synthesis and characterization of the polyaniline dopant Schiff base

    Directory of Open Access Journals (Sweden)

    Mirian Y. Matsumoto

    2012-06-01

    Full Text Available The Schiff base, N-salicilidenoanilina was used as dopant to induce polymerization of aniline and thus preparing polyaniline (PAni. The different conditions of preparation, including Schiff base structure, and the dosage of acidity reaction medium, were investigated to discuss the influence of these conditions relative conductivity of the resulting samples. The products were also characterized by Fourier transform infrared (FTIR, ultraviolet-visible (UV-Vis, electrochemical impedance spectroscopy (EIE. The results showed the synthesis conditions play an important in the formation and the final properties of the polyaniline

  4. Synthesis and Characterization of Two New p-tert-Butylcalix[4]-arene Schiff Bases

    Directory of Open Access Journals (Sweden)

    Saeed Taghvaee Ganjali

    2001-03-01

    Full Text Available Synthesis and characterization of two new Schiff bases of p-tertbuthylcalix[4]arene (H2L1 and HL2 is described. The synthesis of H2L1 and HL2 has been achieved by the condensation of salicylaldehyde with the amine group of upper rim monoamine p-tert-butylcalix[4]arene in ethanol. These compounds have been characterized on the basis of elemental analysis and spectral data. Solvatochromicity and fluorescence properties were observed and measured for H2L1 and HL2. Solvatochromicity of these ligands indicates their potential for NLO applications.

  5. Hydrothermal synthesis and characterization of zirconia based catalysts

    Science.gov (United States)

    Caillot, T.; Salama, Z.; Chanut, N.; Cadete Santos Aires, F. J.; Bennici, S.; Auroux, A.

    2013-07-01

    In this work, three equimolar mixed oxides ZrO2/CeO2, ZrO2/TiO2, ZrO2/La2O3 and a reference ZrO2 have been synthesized by hydrothermal method. The structural and surface properties of these materials have been fully characterized by X-ray diffraction, transmission electron microscopy, surface area measurement, chemical analysis, XPS, infrared spectroscopy after adsorption of pyridine and adsorption microcalorimetry of NH3 and SO2 probe molecules. All investigated mixed oxides are amphoteric and possess redox centers on their surface. Moreover, hydrothermal synthesis leads to catalysts with higher surface area and with better acid-base properties than classical coprecipitation method. Both Lewis and Brønsted acid sites are present on the surface of the mixed oxides. Compared to the other samples, the ZrO2/TiO2 material appears to be the best candidate for further application in acid-base catalysis.

  6. Synthesis, characterization and optimization of poly(p-phenylenediamine)-based organoclay composite for Cr(VI) remediation

    CSIR Research Space (South Africa)

    Mdlalose, L

    2017-04-01

    Full Text Available of these materials for environmental remediation. We report here the synthesis, characterization and application of a poly(para-phenylenediamine) (poly-pPD) organoclay-based composite for removal of Cr(VI) complexes from wastewater. Adsorption capacity...

  7. Synthesis, Characterization, Antimicrobial Activity and Antioxidant ...

    African Journals Online (AJOL)

    MBI

    2015-12-08

    Dec 8, 2015 ... Synthesis, Characterization, Antimicrobial Activity and Antioxidant. Studies of ... Transition metal complexes of Co(II) and Ni(II) with Schiff base ligand (HL) derived from condensation of 2- ..... 2-((5mercapto-1,3,4-thiadiazol-2-.

  8. Synthesis and characterization of homogeneous interstitial solutions of nitrogen and carbon in iron-based lattices

    DEFF Research Database (Denmark)

    Brink, Bastian Klüge

    work in synthesis and characterization of interstitial solutions ofnitrogen and carbon in iron-based lattices. In order to avoid the influences of gradients incomposition and residual stresses, which are typically found in treated surface layers,homogenous samples are needed. These were prepared from...

  9. Synthesis and characterization of semi-IPNs based on PVP and PLLA

    International Nuclear Information System (INIS)

    Camilo, A.P.R.; Mano, V.; Felisberti, M.I.

    2010-01-01

    The specific interest in the synthesis of semi-IPNs based on PLLA and PVP homopolymers due to the fact these are biodegradable and biocompatible, which allows us to infer applications in the medical field as sutures, implants, matrices for controlled release of drugs etc. The objective was to prepare a multicomponent material amphiphile in the form of semi-interpenetrating polymer networks, based on poly (L-lactide), PLLA, hydrophobic homopolymer, and poly (vinylpyrrolidone), PVP, hydrophilic component. The preparation of semi-IPN combined the polymerization and crosslinking of N-vinylpyrrolidone in the presence of poly (L-lactide). The products were characterized by spectroscopic and thermal methods. (author)

  10. SYNTHESIS AND CHARACTERIZATION OF N, N'-BIS-(3 ...

    African Journals Online (AJOL)

    user

    base complexes derived from Salicylaldehyde and histidine with some divalent transition metal ions. Furthermore, Syed (1993) reported the synthesis, characterization and biological evaluation of some. Schiff base metal complexes derived from Anthranilic acid-sugar and naturally occurring amino acid-sugar. Schiff bases ...

  11. Synthesis, characterization, thermal

    Directory of Open Access Journals (Sweden)

    Selma Bal

    2017-09-01

    Full Text Available This work explains the synthesis of a new azo-Schiff base compound, derived from condensation between N-ethylcarbazole-3-carbaldehyde and 1,3-diaminopropane, followed by azo coupling reaction with the diazonium salt of 2-amino-4-methyl phenol. The newly synthesized azo-Schiff base was further reacted with the acetate salts of Copper, Cobalt and Nickel to give three coordination compounds. All synthesized compounds have been characterized through spectral analysis. The coordination compounds have been examined for their thermal and catalytic features. Good and moderate yields were obtained for the oxidation of styrene and cyclohexene. Thermal features of the ligand and its complexes have been explained and the results obtained have supported the proposed structures.

  12. synthesis, characterization an complexes with schiff base co

    African Journals Online (AJOL)

    userpc

    active Ru(II) complexes with coordinating Schiff base were synthesiz lemental ... synthesis and stability of Schiff bases wh ... chelates with anticancer activity have also ..... iron.Inorg. Chem,23(1), 3-10. Kostova, I.; Sasa, L.(2013). Advances in.

  13. Synthesis and molecular characterization of chitosan based polyurethane elastomers using aromatic diisocyanate.

    Science.gov (United States)

    Zia, Khalid Mahmood; Anjum, Sohail; Zuber, Mohammad; Mujahid, Muhammad; Jamil, Tahir

    2014-05-01

    The present research work was performed to synthesize a new series of chitosan based polyurethane elastomers (PUEs) using poly(ɛ-caprolactone) (PCL). The chitosan based PUEs were prepared by step-growth polymerization technique using poly(ɛ-caprolactone) (PCL) and 2,4-toluene diisocyanate (TDI). In the second step the PU prepolymer was extended with different mole ratios of chitosan and 1,4-butane diol (BDO). Molecular engineering was carried out during the synthesis. The conventional spectroscopic characterization of the synthesized samples using FT-IR confirms the existence of the proposed chitosan based PUEs structure. Internal morphology of the prepared PUEs was studied using SEM analysis. The SEM images confirmed the incorporation of chitosan molecules into the PU backbone. Copyright © 2014 Elsevier B.V. All rights reserved.

  14. Synthesis and Characterization of Pine Needles Reinforced RF Matrix Based Biocomposites

    Directory of Open Access Journals (Sweden)

    A. S. Singha

    2008-01-01

    Full Text Available Synthesis and characterization of pine needles reinforced thermosetting resin (Resorcinol-Formaldehyde which is most suitable as composite matrix has been reported. The polycondensation reaction between resorcinol and formaldehyde (RF in different molar ratios has been applied to the synthesis of RF polymer matrix. A thermosetting resin based composite, containing approximately 10, 20, 30 and 40% of natural fiber by weight, has been obtained by adding pine needles to the Resorcinol-Formaldehyde (RF resin. The mechanical properties of randomly oriented intimately mixed particle reinforced (Pine needles composites were determined. Effect of fiber loading in terms of weight % on mechanical properties such as tensile, compressive, and flexural and wear properties have also been evaluated. The reinforcing of the resin with Pine needles was accomplished in particle size of 200 micron by employing optimized resin. Present work reveals that mechanical properties of the RF resin increases to extensive extent when reinforced with Pine needles. Thermal (TGA/DTA and morphological studies (SEM of the resin, fiber and polymer composites thus synthesized have also been carried out.

  15. Synthesis and structural characterization of a calcium coordination ...

    Indian Academy of Sciences (India)

    Synthesis and structural characterization of a calcium coordination polymer based on a μ3-bridging. tetradentate binding mode of glycine. SUBRAMANIAN NATARAJAN*a, BIKSHANDARKOIL R. SRINIVASANb , J. KALYANA SUNDARa, K. RAVIKUMARc , R.V. KRISHNAKUMARd , J. SURESHe,. aSchool of Physics, ...

  16. Synthesis and characterization of new optically active poly(amide ...

    African Journals Online (AJOL)

    Synthesis and characterization of new optically active poly(amide-imide)s based on N -trimellitimido- ... Bulletin of the Chemical Society of Ethiopia ... (DMAc), dimethyl sulfoxide (DMSO) and N-methyl-2-pyrrolidone (NMP) at room temperature.

  17. Synthesis and structural characterization of lithium

    Indian Academy of Sciences (India)

    synthesis and characterization of two new iminophos- phonamine ligands ... structures. 2.3 General synthetic method for ligands (1 and 2) ... 2.3b General method for the Synthesis of ligands ...... studies are currently underway in our laboratory.

  18. Synthesis and characterization of reactive dye-cassava mesocarp ...

    African Journals Online (AJOL)

    The synthesis of triazine based reactive dyes was carried out. The resultant dyes were characterized by thin layers chromatography, molecular weight, infrared and ultra- violet spectroscopy, and used in dyeing cassava mesocarp to produce dye modified cellulosic substrates. The dyed substrates were tested for dye fixation, ...

  19. Microwave Synthesis and Characterization of Waste Soybean Oil-Based Gemini Imidazolinium Surfactants with Carbonate Linkage

    Science.gov (United States)

    Tripathy, Divya Bajpai; Mishra, Anuradha

    Gemini surfactants are presently gaining attention due to their unusual self-assembling characteristics and incomparable interfacial activity. Current research work involves the cost-effective microwave (MW) synthesis of waste soybean oil-based gemini imidazolinium surfactants (GIS) having a carbonate linkage in its spacer moiety. Structural characterizations of the materials have been done using FT-IR, 1H-NMR and 13C-NMR. Using indigenous and natural material as base and MW as energy source for synthesizing the GIS with easily degradable chemical moiety make them to be labeled as green surfactants.

  20. SYNTHESIS, CHARACTERIZATION AND PHOTOCATALYTIC ...

    African Journals Online (AJOL)

    ISSN 1011-3924. © 2018 Chemical Society of Ethiopia and The Authors. Printed in Ethiopia ... SYNTHESIS, CHARACTERIZATION AND PHOTOCATALYTIC ACTIVITY OF .... cm−1 to determine the surface functional groups. 10 mg of sample ...

  1. Synthesis and characterization of organically linked ZnO nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Chory, Christine; Riedel, Ingo; Parisi, Juergen [Energy and Semiconductor Research Laboratory (EHF), University of Oldenburg, Carl-von Ossietzky-Strasse 9-11, 26129 Oldenburg (Germany); Kruska, Carsten; Heimbrodt, Wolfram [Department of Physics and Material Sciences Center, Philipps-University Marburg, Renthof 5, 35032 Marburg (Germany); Feser, Clemens [NEXT ENERGY - EWE Research Centre for Energy Technology e.V., Carl-von Ossietzky-Strasse 15, 26129 Oldenburg (Germany); Beenken, Wichard J.D. [Department of Theoretical Physics I, Ilmenau University of Technology, Weimarer Strasse 25, 98693 Ilmenau (Germany); Hoppe, Harald [Department of Experimental Physics I, Ilmenau University of Technology, Weimarer Strasse 32, 98693 Ilmenau (Germany)

    2012-11-15

    We report on the solution-based synthesis and characterization of three-dimensional networks of ZnO nanoparticles where the formation of structures is achieved by covalently linking the nanocrystals with bifunctional organic ligands. The colloidal synthesis will be presented with application of two ligands that vary in size and binding sites. Furthermore we report on structural characterization of dried powders and thin films by means of X-ray diffraction and electron microscopy in order to examine the regularity of the structures. We also present first investigations of the optical properties and electrical conductance behavior in lateral direction of the differently linked hybrid ZnO networks. (Copyright copyright 2012 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  2. Synthesis and characterization of organically linked ZnO nanoparticles

    International Nuclear Information System (INIS)

    Chory, Christine; Riedel, Ingo; Parisi, Juergen; Kruska, Carsten; Heimbrodt, Wolfram; Feser, Clemens; Beenken, Wichard J.D.; Hoppe, Harald

    2012-01-01

    We report on the solution-based synthesis and characterization of three-dimensional networks of ZnO nanoparticles where the formation of structures is achieved by covalently linking the nanocrystals with bifunctional organic ligands. The colloidal synthesis will be presented with application of two ligands that vary in size and binding sites. Furthermore we report on structural characterization of dried powders and thin films by means of X-ray diffraction and electron microscopy in order to examine the regularity of the structures. We also present first investigations of the optical properties and electrical conductance behavior in lateral direction of the differently linked hybrid ZnO networks. (Copyright copyright 2012 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  3. Novel synthesis and characterization of a collagen-based biopolymer initiated by hydroxyapatite nanoparticles.

    Science.gov (United States)

    Bhuiyan, D; Jablonsky, M J; Kolesov, I; Middleton, J; Wick, T M; Tannenbaum, R

    2015-03-01

    In this study, we developed a novel synthesis method to create a complex collagen-based biopolymer that promises to possess the necessary material properties for a bone graft substitute. The synthesis was carried out in several steps. In the first step, a ring-opening polymerization reaction initiated by hydroxyapatite nanoparticles was used to polymerize d,l-lactide and glycolide monomers to form poly(lactide-co-glycolide) co-polymer. In the second step, the polymerization product was coupled with succinic anhydride, and subsequently was reacted with N-hydroxysuccinimide in the presence of dicyclohexylcarbodiimide as the cross-linking agent, in order to activate the co-polymer for collagen attachment. In the third and final step, the activated co-polymer was attached to calf skin collagen type I, in hydrochloric acid/phosphate buffer solution and the precipitated co-polymer with attached collagen was isolated. The synthesis was monitored by proton nuclear magnetic resonance, infrared and Raman spectroscopies, and the products after each step were characterized by thermal and mechanical analysis. Calculations of the relative amounts of the various components, coupled with initial dynamic mechanical analysis testing of the resulting biopolymer, afforded a preliminary assessment of the structure of the complex biomaterial formed by this novel polymerization process. Copyright © 2015. Published by Elsevier Ltd.

  4. Boronate esters: Synthesis, characterization and molecular base receptor analysis

    Science.gov (United States)

    Gómez-Jaimes, Gelen; Barba, Victor

    2014-10-01

    The synthesis of three boronate esters obtained by reacting 4-fluorophenylboronic (1), 4-iodophenylboronic (2) and 3,4-chlorophenylboronic (3) acids with 2,4,5-trihidroxybenzaldehyde is reported. The structural characterization was determined by spectroscopic and spectrometric techniques. The boron atom was evaluated to acts as Lewis acid center in the reaction with pyridine (Py), triethylamine (TEA) and fluoride anion (F-). The titration method was followed by UV-Vis and 11B NMR spectroscopy; results indicate the good interaction with the fluoride ion but poor coordination towards pyridine in solution.

  5. Alternative chemical-based synthesis routes and characterization of nano-scale particles

    International Nuclear Information System (INIS)

    Brocchi, E.A.; Motta, M.S.; Solorzano, I.G.; Jena, P.K.; Moura, F.J.

    2004-01-01

    Different nano-scale particles have been synthesized by alternative routes: nitrates dehydratation and oxide, or co-formed oxides, reduction by hydrogen. Chemical-based synthesis routes are described and thermodynamics studies and kinetics data are presented to support the feasibility for obtaining single-phase oxides and co-formed two-phase oxides. In addition, the reduction reaction has been applied to successfully produce metal/ceramic nanocomposites. Structural characterization has been carried out by means of X-ray diffraction and, more extensively, transmission electron microscopy operating in conventional diffraction contrast mode (CTEM) and high-resolution mode (HRTEM). Nano-scale size distribution of oxide particles is well demonstrated together with their defect-free structure in the lower range, around 20 nm, size. Structural features related to the synthesized nano-composites are also presented

  6. Synthesis, characterization and potential utility of doped ceramics based catalysts

    Science.gov (United States)

    Sharma, Ritika; Yadav, Deepshikha; Singh, G. P.; Vyas, G.; Bhojak, N.

    2018-05-01

    Excessive utilization of petrol, diesel and other fossil fuels, continuous increase in their prices, and the big problem of carbon dioxide mission have encouraged scientists and technologist to find either new sources of energy or to develop technologies for the sustainable utilization of fuel. Biofuels are the only energy technologies that can resolve the problem of carbon dioxide emission in the atmosphere as well as reduce the amount of fossil fuel burned. Bio ethanol and biodiesel are the most common types of biofuel which are being used at present. Biodiesel has become more interesting for all the researchers in present scenario. Various feedstock viz. edible, nonedible oils, waste cooking oil, animal fat, algae etc, are using for the production of biodiesel worldwide according to their availability. Selection of efficient heterogeneous catalysts for biodiesel preparation still needs more attention of researchers. The present investigation deals with determination of synthesis, characterization and applications of doped ceramic based materials in different medium. Two of doped ceramic based catalysts which has been potentially used for the production of biodiesel. The Engine performance of biodiesel samples, made from industrial waste oils and ceramic based catalyst, have also been investigated and found up to satisfactory levels.

  7. Synthesis and characterization of thorium(IV) and uranium(IV) complexes with Schiff bases

    Energy Technology Data Exchange (ETDEWEB)

    Radoske, Thomas; Maerz, Juliane; Kaden, Peter; Patzschke, Michael; Ikeda-Ohno, Atsushi [Helmholtz-Zentrum Dresden-Rossendorf e.V., Dresden (Germany). Chemistry of the F-Elements

    2017-06-01

    We report herein the synthesis and characterization of several imine complexes of tetravalent thorium (Th(IV)) and uranium (U(IV)). The ligands investigated in this study are a Schiff base type, including the well-known salen ligand (H{sub 2}Le, Fig. 1). The complexation in solution was investigated by NMR measurements indicating paramagnetic effects of unpaired f-electrons of U(IV) on the ligand molecule. We also determined the solid-state molecular structures of the synthesized complexes by single crystal X-ray diffraction. The synthesized complexes show an eight-fold coordination geometry around the actinide center surrounded by two tetradentate ligands with 2N- and 2O-donor atoms.

  8. Synthesis and characterization of six-membered pincer ...

    Indian Academy of Sciences (India)

    0013167

    SUPPORTING INFORMATION. REGULAR ARTICLE. Synthesis and characterization of six-membered pincer nickelacycles and application in alkylation of benzothiazole. †. HANUMANPRASAD PANDIRI,a DIPESH M SHARMA,a RAJESH G GONNADEb and. BENUDHAR PUNJI*,a. aOrganometallic Synthesis and Catalysis ...

  9. Lanthanide phosphonates: Synthesis, thermal stability and magnetic characterization

    Energy Technology Data Exchange (ETDEWEB)

    Amghouz, Z., E-mail: amghouz.uo@uniovi.es [Departamentos de Quimica Fisica y Analitica y Quimica Organica e Inorganica, Universidad de Oviedo - CINN, 33006 Oviedo (Spain); Garcia, J.R.; Garcia-Granda, S. [Departamentos de Quimica Fisica y Analitica y Quimica Organica e Inorganica, Universidad de Oviedo - CINN, 33006 Oviedo (Spain); Clearfield, A. [Department of Chemistry, Texas A and M University, College Station, TX 77842-3012 (United States); Rodriguez Fernandez, J.; Pedro, I. de [CITIMAC, Facultad de Ciencias, Universidad de Cantabria, 39005 Santander (Spain); Blanco, J.A. [Departamento de Fisica, Universidad de Oviedo, 33007 Oviedo (Spain)

    2012-09-25

    Highlights: Black-Right-Pointing-Pointer Report of the complete series of lanthanide 1,4-phenylbis(phosphonate). Black-Right-Pointing-Pointer Synthesis under conventional hydrothermal synthesis or microwave-assisted hydrothermal synthesis. Black-Right-Pointing-Pointer Cation size is the key factor for the structural and particles size variations. Black-Right-Pointing-Pointer Thermal behaviour is characterized by unusual very high thermal stability. - Abstract: Series of novel organic-inorganic hybrids materials based on trivalent lanthanides (Ln = Y, La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu) and 1,4-phenylbis(phosphonate) obtained under hydrothermal conditions either by oven heat or microwave irradiation. The anhydrous compounds containing La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, and Ho, are isostructural. However, the compounds based on Y, Er, Tm, Yb, and Lu are hydrated and their structures have not yet been solved. The series of compounds are characterized by PXRD, TEM, SEM-EDX and thermal analyses (TG-MS and DSC). TEM study show a variable particles size with a minimum mean-particle size of ca. 30 nm. These compounds exhibit unusual very high thermal stability. The size of particles and the thermal stability are depending on lanthanide(III) cation features. All the investigated materials show paramagnetic behaviour. The magnetic susceptibility data follow a Curie-Weiss laws with paramagnetic effective moments in good agreement with those expected for Ln{sup 3+} free ions.

  10. Synthesis and characterization of iron cobalt (FECO) nanorods ...

    African Journals Online (AJOL)

    Synthesis and characterization of iron cobalt (FECO) nanorods prepared by simple ... shaped by increasing annealing temperature from room temperature to 800 ... Keywords: FeCo nanoparticles, sodium borohydrid, CTAB, chemical synthesis ...

  11. Hydrothermal synthesis, characterization and luminescent ...

    Indian Academy of Sciences (India)

    Home; Journals; Bulletin of Materials Science; Volume 39; Issue 4. Hydrothermal synthesis, characterization and luminescent properties of lanthanide-doped NaLaF 4 nanoparticles. JIGMET LADOL HEENA KHAJURIA SONIKA KHAJURIA ... Keywords. Citric acid; X-ray diffraction; down-conversion emission; energy transfer.

  12. Radiation synthesis and characterization of zinc phthalocyanine composite based on 2-hydroxyethyl methacrylate/methyl methacrylate copolymer

    International Nuclear Information System (INIS)

    Abdel Ghaffar, A.M.; Youssef, Tamer E.; Mohamed, Hanan H.

    2016-01-01

    The synthesis and characterization of new 2-hydroxyethyl methacrylate-co-methyl methacrylate/zinc phthalocyanine composite Poly(HEMA/MMA/ZnPc) is described for the first time in this study. The aim of this research is to present possibility of radiation synthesis of the newly zinc phthalocyanine composites as potential candidates for wide range of applications. Gel (%) and swelling for Poly(hydroxyethyl methacrylate) Poly(HEMA) and the based Poly(hydroxyethyl methacrylate/methyl methacrylate) copolymer Poly(HEMA/MMA) with different composition 100/0, 95/5, 90/10 and 80/20 wt % were evaluated. It was found that Poly(HEMA/MMA) copolymer with composition 95/5 wt % characterized by its high swelling property at pH 7.4. The prepared composites I and II Poly(HEMA/MMA/ZnPc) with composition (95/5/1 wt%) and (95/5/1.5 wt%) respectively have been characterized by FTIR and TGA. The effect of gamma irradiation on the chemical properties of composite I was described. It is observed that the Zinc phthalocyanine with low concentration 1 wt % enhance chemical, thermal properties and stabilization against gamma radiation of the prepared composite I. - Highlights: • The preparation of Poly(HEMA/MMA/ZnPc) by radiation forming modified composites. • The low concentration of ZcPc (1 or 1.5 wt %) lead to form outstanding properties. • These composites are a potential candidate for wide range of applications.

  13. Radiation synthesis and characterization of zinc phthalocyanine composite based on 2-hydroxyethyl methacrylate/methyl methacrylate copolymer

    Energy Technology Data Exchange (ETDEWEB)

    Abdel Ghaffar, A.M., E-mail: am_abdelghaffar@yahoo.com [Radiation Research of Polymer Chemistry Department, Industrial Irradiation Division, National Center for Radiation Research and Technology, Atomic Energy Authority P.O. Box 29, Nasr City, Cairo (Egypt); Youssef, Tamer E. [Applied Organic Chemistry Department, Chemical Industries Research Division, National Research Center, Dokki, Cairo, 12622 (Egypt); Chemical and Materials Engineering Department, Faculty of Engineering, King Abdulaziz University, P.O. Box 80204, Jeddah, 21589 (Saudi Arabia); Mohamed, Hanan H. [Chemistry Department, Faculty of Science, Helwan University, Ain Helwan, Cairo (Egypt)

    2016-08-01

    The synthesis and characterization of new 2-hydroxyethyl methacrylate-co-methyl methacrylate/zinc phthalocyanine composite Poly(HEMA/MMA/ZnPc) is described for the first time in this study. The aim of this research is to present possibility of radiation synthesis of the newly zinc phthalocyanine composites as potential candidates for wide range of applications. Gel (%) and swelling for Poly(hydroxyethyl methacrylate) Poly(HEMA) and the based Poly(hydroxyethyl methacrylate/methyl methacrylate) copolymer Poly(HEMA/MMA) with different composition 100/0, 95/5, 90/10 and 80/20 wt % were evaluated. It was found that Poly(HEMA/MMA) copolymer with composition 95/5 wt % characterized by its high swelling property at pH 7.4. The prepared composites I and II Poly(HEMA/MMA/ZnPc) with composition (95/5/1 wt%) and (95/5/1.5 wt%) respectively have been characterized by FTIR and TGA. The effect of gamma irradiation on the chemical properties of composite I was described. It is observed that the Zinc phthalocyanine with low concentration 1 wt % enhance chemical, thermal properties and stabilization against gamma radiation of the prepared composite I. - Highlights: • The preparation of Poly(HEMA/MMA/ZnPc) by radiation forming modified composites. • The low concentration of ZcPc (1 or 1.5 wt %) lead to form outstanding properties. • These composites are a potential candidate for wide range of applications.

  14. Synthesis, characterization and magnetic properties of selected Laves and MAX phases

    International Nuclear Information System (INIS)

    Hamm, Christin Maria

    2017-01-01

    In this work the rare-earth free Laves phases Ti 2 M 3 Si with M = Mn, Fe, Co, Ni were synthesized by microwave heating and were structurally and magnetically characterized. Furthermore, the solid solution Ti 2 (Co 1-x Fe x ) 3 Si was synthesized by arc melting and spark plasma sintering, as well as their magnetic behavior was studied. In addition to the Laves phases, the focus was on the synthesis and characterization of aluminum-based MAX phases. For the first time the ternary carbides were prepared by microwave heating. The phase-pure representation of MAX phases was particularly challenging for synthetic solid-state chemistry. The susceptor-assisted microwave heating allows the synthesis of high-quality samples, which was shown in this work on M 2 AlC (M = Ti, V, Cr) and V 4 AlC 3 . Furthermore, for the first time, the doping of these materials with Mn and Fe was successful. In addition to the structural characterization of the new phases, the microstructure and magnetic properties are discussed in this work. Using these doped compounds as well as the compound V 4 AlC 3 , it has been shown that field-activated synthesis, particularly susceptor-assisted microwave heating, are a very good synthesis method for compounds which are hard or sometimes not synthesized by conventional methods.

  15. Synthesis and characterization of a nanostructured matrix hydroxyapatite ceramic bone reconstruction

    International Nuclear Information System (INIS)

    Correa, P.; Camargo, N.H.A.; Silva, D.F.

    2012-01-01

    The nanostructured ceramics have been shown promise as biomaterials for bone reconstruction. Among calcium phosphates, hydroxyapatite Ca/P ratio = 1.67 mol stands out because of its crystallographic similarity with the mineral bone phase and biocompatibility. This work was based on synthesis and characterization of a nanostructured hydroxyapatite for use in reconstituting bone tissue. The synthesis method for obtaining the bioceramic powder occurred at process of dissolution/precipitation, involving CaO solid/liquid and phosphoric acid required for forming the composition of Ca/P = 1.67 mole. The material recovered from the synthesis was calcined at 900 ° C/2h, providing the hydroxyapatite powder nanometer. This was subjected to mechanical fragmentation process in mill attritor, providing a hydroxyapatite with modified surface morphology. The results presented relate to morphological characterization studies (SEM), mineralogical (XRD), chemical (FTIR) and particle size distribution, using the laser particle size analysis method. Such results showed the formation of hydroxyapatite phase and morphology satisfactory for use in reconstituting bone tissue

  16. SYNTHESIS AND CHARACTERIZATION OF BIO-BASED POLYESTER POLYOL

    Directory of Open Access Journals (Sweden)

    MİTHAT ÇELEBİ

    2016-11-01

    Full Text Available Polyurethanes are versatile polymeric materials and are usually synthesised by isocyanate reactions with polyols. Due to the variety of isocyanates and polyols, particularly polyols, polyurethanes can be easily tailored for wide applications, such as rigid and flexible foams, coatings, adhesives, and elastomers. Considerable efforts have been recently devoted to developing bio-based substitutes for petroleum-based polyuretahanes due to increasing concerns over the depletion of petroleum resources, environment, and sustainability. Polyester polyols based on aliphatic and aromatic dicarboxylic acids are one of the most important materials in polymer technologies. Large volume of plants oils are used as renewable resources to produce various chemicals which are industrially important to make soaps, cosmetic products, surfactants, lubricants, diluents, plasticizers, inks, agrochemicals, composite materials, food industry. This study introduces synthesis and properties of bio-based polyols from different renewable feedstocks including vegetable oils and derivatives. A comparison of bio-based polyol properties with their petroleum-based analogues were investigated.

  17. An Efficient Catalyst for the Synthesis of Schiff Bases

    International Nuclear Information System (INIS)

    Fareed, G.; Afza, N.; Kalhoro, M.A.

    2013-01-01

    An efficient high yielding synthesis of Schiff bases (1-17) is derived from condensation of 2-fluorenamine and 4-amino phenol with a variety of aldehydes catalyzed by dodecatungstosilicic acid P/sub 2/O/sub 5/ under solvent free conditions at room temperature. The catayst is found to be more efficient in terms of ease of reaction workup and high yields. This methodology contributes to an energy efficient, facile and environamental friendly synthesis for the preparation of Schiff bases. The structures of afforded Schiff bases were characterized by spectroscopic data and elemental analysis. (author)

  18. Synthesis, characterization and biological activity of C6-Schiff bases derivatives of chitosan.

    Science.gov (United States)

    Xu, Ruibo; Aotegen, Bayaer; Zhong, Zhimei

    2017-12-01

    C 6 -Schiff bases derivatives of chitosan were synthesized for the first time. C 2 -amino groups and C 3 -hydroxy groups were firstly protected by CuSO 4 ·5H 2 O, and the C 6 -hydroxy was then transformed into aldehyde, which then reacted with anilines through nucleophilic addition to introduce the CN group at C 6 -position in chitosan chain. Finally, C 6 -Schiff bases derivatives of chitosan were got by the deprotection of C 2 -NH 2 with cation exchange resin. The structures and properties of the new synthesized products were characterized by Fourier transform infrared spectroscopy, 13 C NMR, SEM image, and elemental analysis. The antibacterial activities of derivatives were tested in the experiment, and the results showed that the prepared chitosan derivatives had significantly improved antibacterial activity toward Staphylococcus aureus and Escherichia coli. The Cytotoxicity test showed that the prepared chitosan derivatives had low Cytotoxicity, compared with chitosan and C 2 -benzaldehyde Schiff bases of chitosan. This paper allowed a new method for the synthesis of Schiff bases of chitosan, which was enlightening. Copyright © 2017 Elsevier B.V. All rights reserved.

  19. Synthesis, characterization and comparison of polythiophene ...

    Indian Academy of Sciences (India)

    38

    Synthesis, characterization and comparison of polythiophene-carbon ... b Nanotechnology Research Institute, School of Chemical Engineering, Babol University of Technology, Babol, ..... The scan range was from −0.24 to 1.2 V in reference to.

  20. Synthesis and characterization of nano silicon and titanium nitride ...

    Indian Academy of Sciences (India)

    The characterization techniques indicated ... Scalable synthesis; microwave plasma; chemical synthesis; nanoparticles. 1. Introduction ... used but very few methods are available to produce silicon and titanium ... current (A). (m3/h). 1. Si. 2.1.

  1. A series of fluorene-based two-photon absorbing molecules: synthesis, linear and nonlinear characterization, and bioimaging

    Science.gov (United States)

    Andrade, Carolina D.; Yanez, Ciceron O.; Rodriguez, Luis; Belfield, Kevin D.

    2010-01-01

    The synthesis, structural, and photophysical characterization of a series of new fluorescent donor–acceptor and acceptor-acceptor molecules, based on the fluorenyl ring system, with two-photon absorbing properties is described. These new compounds exhibited large Stokes shifts, high fluorescent quantum yields, and, significantly, high two-photon absorption cross sections, making them well suited for two-photon fluorescence microscopy (2PFM) imaging. Confocal and two-photon fluorescence microscopy imaging of COS-7 and HCT 116 cells incubated with probe I showed endosomal selectivity, demonstrating the potential of this class of fluorescent probes in multiphoton fluorescence microscopy. PMID:20481596

  2. Synthesis, characterization, antimicrobial activity and molecular ...

    African Journals Online (AJOL)

    Synthesis, characterization, antimicrobial activity and molecular docking studies of combined pyrazol-barbituric acid pharmacophores. Assem Barakat, Bandar M. Al-Qahtani, Abdullah M. Al-Majid, M. Ali Mohammed Rafi Shaik, Mohamed H.M. Al-Agamy, Abdul Wadood ...

  3. synthesis and optical characterization of acid-doped polyaniline thin

    African Journals Online (AJOL)

    HOD

    SYNTHESIS AND OPTICAL CHARACTERIZATION OF ACID-DOPED. POLYANILINE THIN .... MATERIALS AND METHODS .... Characterization of Se Doped Polyaniline”,Current. Applied ... with Silver Nanoparticles”, Advances in Materials.

  4. Diclofenac-Based Hydrazones and Spirothiazolidinones: Synthesis, Characterization, and Antimicrobial Properties.

    Science.gov (United States)

    Kocabalkanlı, Ayşe; Cihan-Üstündağ, Gökçe; Naesens, Lieve; Mataracı-Kara, Emel; Nassozi, Mebble; Çapan, Gültaze

    2017-05-01

    We report here the synthesis, structural characterization, and biological evaluation of novel diclofenac-based hydrazone (4a-f) and spirothiazolidinone (5a-f, 6a-f) derivatives designed as potential antimicrobial agents. The compounds were evaluated in vitro for their antiviral activity against a wide spectrum of DNA and RNA viruses. They were further screened in vitro against different strains of bacteria and fungi. The hydrazone derivatives, 4a and 4c-f, were found to be active against herpesviruses (HSV-1, HSV-2, and HSV-1 TK - ), vaccinia virus, and Coxsackie B4 virus, with EC 50 values between 6.6 µg/mL and 14.7 μg/mL, and the selectivity index values were greater than 10 for 4a and 4f. The newly synthesized compounds (4-6) were inactive against the bacterial and the fungal strains tested, at levels below 2500, 1250, or 625 μg/mL. Interestingly, the key intermediate 3 with a free hydrazide moiety displayed antifungal properties against Candida albicans and C. parapsilosis at MIC values of 4.88 µg/mL and 78.12 μg/mL, respectively. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  5. Plasma-spray synthesis and characterization of ti-based nitride and oxide nanogranules

    Energy Technology Data Exchange (ETDEWEB)

    Antipas, Georgios S.E., E-mail: gantipas@metal.ntua.gr [School of Mining Engineering and Metallurgy, National Technical University of Athens, Athens (Greece)

    2014-09-15

    The synthesis of nanosized Ti-based nanogranules via plasma spraying is reported. The synthesis route involved use of both nitrogen and oxygen gases with varying results. In the case of nitrogen, a mixture of titanium nitrides were produced, yielding both the Ti2N and the sub-stoichiometric TiN0.61 compounds. In the case of oxygen, both the stoichiometric rutile and TiO ceramic phases were indexed. Based on EDS analysis, even fractional oxygen concentrations caused tungsten impurities which originated from the cathode electrode. The method yielded particle mass median sizes of the order of 15nm and the smallest particles detected were 5nm. (author)

  6. Photocatalytic semiconductors synthesis, characterization, and environmental applications

    CERN Document Server

    Hernández-Ramírez, Aracely

    2014-01-01

    This critical volume examines the different methods used for the synthesis of a great number of photocatalysts, including TiO2, ZnO and other modified semiconductors, as well as characterization techniques used for determining the optical, structural and morphological properties of the semiconducting materials. Additionally, the authors discuss photoelectrochemical methods for determining the light activity of the photocatalytic semiconductors by means of measurement of properties such as band gap energy, flat band potential and kinetics of hole and electron transfer. Photocatalytic Semiconductors: Synthesis, Characterization and Environmental Applications provide an overview of the semiconductor materials from first- to third-generation photocatalysts and their applications in wastewater treatment and water disinfection. The book further presents economic and toxicological aspects in the production and application of photocatalytic materials.

  7. Synthesis of new nano Schiff base complexes: X-ray crystallography ...

    African Journals Online (AJOL)

    This study presents synthesis and characterization of new nano uranyl Schiff base complexes. Electrochemistry of these complexes showed a quasireversible redox reaction without any successive reactions. Furthermore, X-ray crystallography exhibited that beside the coordination of tetradentate Schiff base, one solvent ...

  8. Synthesis, characterization and biological behavior of some Schiff's and Mannich base derivatives of Lamotrigine

    Directory of Open Access Journals (Sweden)

    A.A. Kulkarni

    2017-02-01

    Full Text Available A series of various Schiff's and Mannich base derivatives (N1–2 & ND1–6 of Lamotrigine with isatin and substituted isatin were synthesized to get more potent anticonvulsant agents. The starting material for the synthesis of various new Schiff's and Mannich base derivatives was isatin (1H-indole- 2, 3-dione which in turn was prepared from substituted isonitrosoacetanilide using aniline. Lamotrigine reacts with isatin & substituted isatin gave Schiff's bases (N1–2 which on reaction with various secondary amines (dimethylamine, diethylamine, morpholine produced Mannich bases (ND1–6. The structures of newly synthesized compounds were characterized by using TLC, UV, FT-IR, 1HNMR and studied for their anticonvulsant activity. Anticonvulsant activity of all the derivatives was evaluated by MES method using phenobarbitone sodium & Lamotrigine as standard drugs and % reduction of time spent by animals in extension, flexion, clonus, and stupor phase were noted. Compounds ND-4 and ND-6 showed significant anticonvulsant activity when compared with that of standard drugs. The remaining all compounds show moderate activity. Biological activity data of the synthesized derivatives revealed that, the synthesized derivatives are good anticonvulsant agents as compared to Lamotrigine.

  9. Synthesis, Spectroscopic and DFT Characterization of 4â-(4-tert ...

    African Journals Online (AJOL)

    In this work the synthesis, spectral characterization and non-linear optical properties of metal-free .... following literature methods23–26 The advantage of this method ..... Synthesis of phthalocyanine conjugates with gold nanoparticles and.

  10. Synthesis and characterization of dextran-coated iron oxide nanoparticles

    Science.gov (United States)

    Predescu, Andra Mihaela; Matei, Ecaterina; Berbecaru, Andrei Constantin; Pantilimon, Cristian; Drăgan, Claudia; Vidu, Ruxandra; Predescu, Cristian; Kuncser, Victor

    2018-03-01

    Synthesis and characterization of iron oxide nanoparticles coated with a large molar weight dextran for environmental applications are reported. The first experiments involved the synthesis of iron oxide nanoparticles which were coated with dextran at different concentrations. The synthesis was performed by a co-precipitation technique, while the coating of iron oxide nanoparticles was carried out in solution. The obtained nanoparticles were characterized by using scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction spectrometry, Fourier transform infrared spectroscopy and superconducting quantum interference device magnetometry. The results demonstrated a successful coating of iron oxide nanoparticles with large molar weight dextran, of which agglomeration tendency depended on the amount of dextran in the coating solution. SEM and TEM observations have shown that the iron oxide nanoparticles are of about 7 nm in size.

  11. New Dilated LMI Characterization for the Multiobjective Full-Order Dynamic Output Feedback Synthesis Problem

    Directory of Open Access Journals (Sweden)

    Zrida Jalel

    2010-01-01

    Full Text Available This paper introduces new dilated LMI conditions for continuous-time linear systems which not only characterize stability and performance specifications, but also, performance specifications. These new conditions offer, in addition to new analysis tools, synthesis procedures that have the advantages of keeping the controller parameters independent of the Lyapunov matrix and offering supplementary degrees of freedom. The impact of such advantages is great on the multiobjective full-order dynamic output feedback control problem as the obtained dilated LMI conditions always encompass the standard ones. It follows that much less conservatism is possible in comparison to the currently used standard LMI based synthesis procedures. A numerical simulation, based on an empirically abridged search procedure, is presented and shows the advantage of the proposed synthesis methods.

  12. Synthesis and characterization of castor oil-based polyurethane

    Indian Academy of Sciences (India)

    Polyurethane (PU) based on polyol, derived from castor oil has been synthesized and characterized for potential use as a base material for electrolytes. Transesterification process of castor oil formed a polyol with hydroxyl value of 190 mg KOH g–1 and molecular weight of 2786 g mol–1. The polyols together with 4 ...

  13. Synthesis and characterization of magnetite nanoparticles coated with lauric acid

    Energy Technology Data Exchange (ETDEWEB)

    Mamani, J.B., E-mail: javierbm@einstein.br [Instituto do Cérebro-InCe, Hospital Israelita Albert Einstein-HIAE, 05651-901 São Paulo (Brazil); Costa-Filho, A.J. [Faculdade de Filosofia, Ciências e Letras de Ribeirão Preto, Universidade de São Paulo, Ribeirão Preto (Brazil); Cornejo, D.R. [Instituto de Física Universidade de São Paulo, USP, São Paulo (Brazil); Vieira, E.D. [Instituto de Física, Universidade Federal de Goiás, Goiânia (Brazil); Gamarra, L.F. [Instituto do Cérebro-InCe, Hospital Israelita Albert Einstein-HIAE, 05651-901 São Paulo (Brazil)

    2013-07-15

    Understanding the process of synthesis of magnetic nanoparticles is important for its implementation in in vitro and in vivo studies. In this work we report the synthesis of magnetic nanoparticles made from ferrous oxide through coprecipitation chemical process. The nanostructured material was coated with lauric acid and dispersed in aqueous medium containing surfactant that yielded a stable colloidal suspension. The characterization of magnetic nanoparticles with distinct physico-chemical configurations is fundamental for biomedical applications. Therefore magnetic nanoparticles were characterized in terms of their morphology by means of TEM and DLS, which showed a polydispersed set of spherical nanoparticles (average diameter of ca. 9 nm) as a result of the protocol. The structural properties were characterized by using X-ray diffraction (XRD). XRD pattern showed the presence of peaks corresponding to the spinel phase of magnetite (Fe{sub 3}O{sub 4}). The relaxivities r{sub 2} and r{sub 2}* values were determined from the transverse relaxation times T{sub 2} and T{sub 2}* at 3 T. Magnetic characterization was performed using SQUID and FMR, which evidenced the superparamagnetic properties of the nanoparticles. Thermal characterization using DSC showed exothermic events associated with the oxidation of magnetite to maghemite. - Highlights: • Synthesis of magnetic nanoparticles coated with lauric acid • Characterization of magnetic nanoparticles • Morphological, structural, magnetic, calorimetric and relaxometric characterization.

  14. Synthesis and characterization of rare-earth-doped calcium tungstate nanocrystals

    Science.gov (United States)

    Suneeta, P.; Rajesh, Ch.; Ramana, M. V.

    2018-02-01

    In this paper, we report synthesis and characterization of rare-earth-ion-doped calcium tungstate (CaWO4) nanocrystals (NCs). Rare-earth ions, such as gadolinium (Gd), neodymium (Nd), praseodymium (Pr), samarium (Sm) and holmium (Ho), were successfully doped in the CaWO4 NCs by changing the synthesis conditions. The adopted synthesis route was found to be fast and eco-friendly. Structural characterizations, such as X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR) and compositional analysis, were performed using energy dispersive analysis of X-rays (EDAX) on as-synthesized NCs. The results indicate the size of the NCs ranging between 47 to 68nm and incorporation of rare-earth ions in CaWO4 NCs.

  15. Materials-by-design: computation, synthesis, and characterization from atoms to structures

    Science.gov (United States)

    Yeo, Jingjie; Jung, Gang Seob; Martín-Martínez, Francisco J.; Ling, Shengjie; Gu, Grace X.; Qin, Zhao; Buehler, Markus J.

    2018-05-01

    In the 50 years that succeeded Richard Feynman’s exposition of the idea that there is ‘plenty of room at the bottom’ for manipulating individual atoms for the synthesis and manufacturing processing of materials, the materials-by-design paradigm is being developed gradually through synergistic integration of experimental material synthesis and characterization with predictive computational modeling and optimization. This paper reviews how this paradigm creates the possibility to develop materials according to specific, rational designs from the molecular to the macroscopic scale. We discuss promising techniques in experimental small-scale material synthesis and large-scale fabrication methods to manipulate atomistic or macroscale structures, which can be designed by computational modeling. These include recombinant protein technology to produce peptides and proteins with tailored sequences encoded by recombinant DNA, self-assembly processes induced by conformational transition of proteins, additive manufacturing for designing complex structures, and qualitative and quantitative characterization of materials at different length scales. We describe important material characterization techniques using numerous methods of spectroscopy and microscopy. We detail numerous multi-scale computational modeling techniques that complements these experimental techniques: DFT at the atomistic scale; fully atomistic and coarse-grain molecular dynamics at the molecular to mesoscale; continuum modeling at the macroscale. Additionally, we present case studies that utilize experimental and computational approaches in an integrated manner to broaden our understanding of the properties of two-dimensional materials and materials based on silk and silk-elastin-like proteins.

  16. Synthesis and characterization of energetic thermoplastic elastomers for propellant formulations

    Directory of Open Access Journals (Sweden)

    Aparecida M. Kawamoto

    2009-01-01

    Full Text Available Synthesis and characterization of energetic ABA-type thermoplastic elastomers for propellant formulations has been carried out. Following the working plan elaborated, the synthesis and characterization of Poly 3- bromomethyl-3-methyl oxetane (PolyBrMMO, Poly 3- azidomethyl-3-methyl oxetane (PolyAMMO, Poly 3,3-bis-azidomethyl oxetane (PolyBAMO and Copolymer PolyBAMO/AMMO (by TDI end capping has been successfully performed. The thermoplastic elastomers (TPEs were synthesized using the chain elongation process PolyAMMO, GAP and PolyBAMO by diisocyanates. In this method 2.4-toluene diisocyanate (TDI is used to link block A (hard and mono- functional to B (soft and di-functional. For the hard A-block we used PolyBAMO and for the soft B-block we used PolyAMMO or GAP.This is a joint project set up, some years ago, between the Chemistry Division of the Institute of Aeronautics and Space (IAE - subordinated to the Brazilian Ministry of Defense - and the Fraunhofer Institut Chemische Technologie (ICT, in Germany. The products were characterized by different techniques as IR- and (1H,13CNMR spectroscopies, elemental and thermal analyses. New methodologies based on FT-IR analysis have been developed as an alternative for the determination of the molecular weight and CHNO content of the energetic polymers.

  17. Synthesis, characterization and antimicrobial activity of mixed ...

    African Journals Online (AJOL)

    Synthesis, characterization and antimicrobial activity of mixed ascorbic acid - nicotinamide metal complexes. ... The result of the antimicrobial studies showed that the mixed complexes have higher inhibitory activity than the original ligands against the tested bacteria and fungi species. KEY WORDS: Ascorbic acid, ...

  18. Green synthesis, characterization and antibacterial activity of copper ...

    African Journals Online (AJOL)

    Green synthesis, characterization and antibacterial activity of copper nanoparticles using L -ascorbic ... Journal Home > Vol 10, No 3 (2017) > ... In this study, simple, economical, convenient and environmentally-friendly chemical reduction ...

  19. Synthesis, Characterization and Applications in Catalysis of Polyoxometalate/Zeolite Composites

    Directory of Open Access Journals (Sweden)

    Frédéric Lefebvre

    2016-05-01

    Full Text Available An overview of the synthesis, characterization and catalytic applications of polyoxometalates/zeolites composites is given. The solids obtained by direct synthesis of the polyoxometalate in the presence of the zeolite are first described with their applications in catalysis. Those obtained by a direct mixing of the two components are then reviewed. In all cases, special care is taken in the localization of the polyoxometalate, inside the zeolite crystal, in mesopores or at the external surface of the crystals, as deduced from the characterization methods.

  20. Synthesis and characterization of a helicene-based imidazolium salt and its application in organic molecular electronics.

    Science.gov (United States)

    Storch, Jan; Zadny, Jaroslav; Strasak, Tomas; Kubala, Martin; Sykora, Jan; Dusek, Michal; Cirkva, Vladimir; Matejka, Pavel; Krbal, Milos; Vacek, Jan

    2015-02-02

    Herein we demonstrate the synthesis of a helicene-based imidazolium salt. The salt was prepared by starting from racemic 2-methyl[6]helicene, which undergoes radical bromination to yield 2-(bromomethyl)[6]helicene. Subsequent treatment with 1-butylimidazole leads to the corresponding salt 1-butyl-3-(2-methyl[6]helicenyl)-imidazolium bromide. The prepared salt was subsequently characterized by using NMR spectroscopy and X-ray analysis, various optical spectrometric techniques, and computational chemistry tools. Finally, the imidazolium salt was immobilized onto a SiO2 substrate as a crystalline or amorphous deposit. The deposited layers were used for the development of organic molecular semiconductor devices and the construction of a fully reversible humidity sensor. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. Design, Synthesis and Characterization of Polyethylene-Based Macromolecular Architectures by Combining Polyhomologation with Powerful Linking Chemistry

    KAUST Repository

    Alkayal, Nazeeha

    2016-01-01

    synthetic route towards well-defined polymethylene-based co/terpolymers, by combining the anthracene/maleimide Diels–Alder reaction with polyhomologation, is presented. For the synthesis of diblock copolymers the following approach was applied: (a) synthesis

  2. An efficient synthesis and spectroscopic characterization of Schiff bases containing 9,10-anthracenedione moiety

    Directory of Open Access Journals (Sweden)

    Fareed Ghulam

    2013-01-01

    Full Text Available A new method has been developed for the synthesis of novel Schiff bases containg anthraquinone moiety using dodeca-Tungstosilicic acid/P2O5 under solvent free conditions at room temperature. The reaction was completed in 1-3 minutes with excellent yields. This method was found to be more efficient, easy and hazardous free for the synthesis of azomethines. The development of these type of methadologies in synthetic chemistry may contribute to green chemistry. The structures of synthesized novel Schiff bases was elucidated using 1H-NMR, 13C-NMR, LCMS, FTIR and CHN analysis.

  3. Synthesis and Characterization of Colloidal Metal and Photovoltaic Semiconductor Nanocrystals

    KAUST Repository

    Abulikemu, Mutalifu

    2014-11-05

    Metal and semiconducting nanocrystals have received a great deal of attention from fundamental scientists and application-oriented researchers due to their physical and chemical properties, which differ from those of bulk materials. Nanocrystals are essential building blocks in the development of nanostructured devices for energy conversion. Colloidal metals and metal chalcogenides have been developed for use as nanocrystal inks to produce efficient solar cells with lower costs. All high-performing photovoltaic nanocrystals contain toxic elements, such as Pb, or scarce elements, such as In; thus, the production of solution-processable nanocrystals from earth-abundant materials using environmentally benign synthesis and processing methods has become a major challenge for the inorganic semiconductor-based solar field. This dissertation, divided into two parts, addresses several aspects of these emerging challenges. The first portion of the thesis describes the synthesis and characterization of nanocrystals of antimony sulfide, which is composed of non-scarce and non-toxic elements, and examines their performance in photovoltaic devices. The effect of various synthetic parameters on the final morphology is explored. The structural, optical and morphological properties of the nanocrystals were investigated, and Sb2S3 nanocrystal-based solid-state semiconductor-sensitized solar cells were fabricated using different deposition processes. We achieved promising power conversion efficiencies of 1.48%. The second part of the thesis demonstrates a novel method for the in situ synthesis and patterning of nanocrystals via reactive inkjet printing. The use of low-cost manufacturing approaches for the synthesis of nanocrystals is critical for many applications, including photonics and electronics. In this work, a simple, low-cost method for the synthesis of nanocrystals with minimum size variation and waste using reactive inkjet printing is introduced. As a proof of concept, the

  4. Synthesis and characterization of mangan oxide coated sand from Capkala kaolin

    Science.gov (United States)

    Destiarti, Lia; Wahyuni, Nelly; Prawatya, Yopa Eka; Sasri, Risya

    2017-03-01

    Synthesis and characterization of mangan oxide coated sand from quartz sand fraction of Capkala kaolin has been conducted. There were two methods on synthesis of Mangan Oxide Coated Sand (MOCS) from Capkala Kaolin compared in this research. Characterization of MOCS was done by using Scanning Electron Microscope/Energy Dispersive X-Ray Spectrometer (SEM/EDX) and X-Ray Diffraction (XRD). The MOCS was tested to reduce phosphate in laundry waste. The result showed that the natural sand had bigger agregates and a relatively uniform structural orientation while both MOCS had heterogen structural orientation and manganese oxide formed in cluster. Manganese in first and second methods were 1,93% and 2,63%, respectively. The XRD spectrum showed clear reflections at 22,80°, 36,04°, 37,60° and a broad band at 26,62° (SiO2). Based on XRD spectrum, it can be concluded that mineral constituents of MOCS was verified corresponding to pyrolusite (MnO2). The former MOCS could reduce almost 60% while the later could reduce 70% phosphate in laundry waste.

  5. Synthesis, characterization and behaviour of trans-bis (argininate) copper (II) to gamma radiation

    International Nuclear Information System (INIS)

    Pereira, A.B.

    1984-01-01

    The synthesis, the characterization and the behaviour to gamma radiation of trans-bis (argininate) copper (II) are presented. The synthesis is made from copper sulfate, sodium hydroxide and hydrochloride of L (+) arginine, in aqueous medium, and the characterization by infrared spectroscopy, visible and ultraviolet spectroscopy and elementary analysis. (C.G.C.)

  6. Synthesis and characterization of germa[n]pericyclynes.

    Science.gov (United States)

    Tanimoto, Hiroki; Nagao, Tomohiko; Nishiyama, Yasuhiro; Morimoto, Tsumoru; Iseda, Fumiyasu; Nagato, Yuko; Suzuka, Toshimasa; Tsutsumi, Ken; Kakiuchi, Kiyomi

    2014-06-14

    The synthesis and characterization of novel pericyclynes comprising germanium atoms and acetylenes, germa[n]pericyclynes, are described. The prepared germa[4]-, [6]-, and [8]pericyclynes were compared by (13)C NMR spectroscopy, X-ray crystallography, cyclic voltammetry, UV-visible spectroscopy, fluorescence emission spectroscopy, Raman spectroscopy, and density functional theory calculation analyses.

  7. Synthesis and characterization of irradiated injectable bone substitute paste based on hydroxyapatite

    International Nuclear Information System (INIS)

    Yessy Warastuti; Basril Abbas

    2011-01-01

    Synthesis and characterization of hydroxyapatite, chitosan and hydroxypropyl methylcellulose (HPMC) composite in injectable paste form have been done. The composite was synthesized by stirring hydroxyapatite, chitosan and HPMC until homogen. IBS paste was irradiated at the dose of 25 kGy (sterile dose). Characterization of IBS paste was conducted by measuring of the water content, identification of functional group with Fourier Transform Infra Red Spectrophotometer (FTIR), and identification of sample morphology with Scanning Electron Microscope Energy Dispersive Spectrophotometer (SEM EDS). The result showed that the water content of irradiated sample was higher than unirradiated sample due to water radiolysis. Several specific bands of IBS paste were identified, i.e., carbonate (CO 3 2- ), at 1420 cm -1 , phosphate (PO 4 3- ) at 1043 cm -1 , 605 cm -1 , 568 cm -1 and chitosan (NH 2 ) at 1599 cm -1 . There is no significant difference in absorbed band between irradiated and unirradiated samples. IBS paste has a microstructure with the size of 0.05 – 0.1 μm. Electron beam irradiation did not change the structure and morphology of sample. (author)

  8. Synthesis & Characterization of New bis-Symmetrical Adipoyl ...

    African Journals Online (AJOL)

    Full Title: Synthesis and Characterization of New bis-Symmetrical Adipoyl, Terepthaloyl, Chiral Diimido-di-L-alanine Diesters and Chiral Phthaloyl-L-alanine Ester of Tripropoxy p-tert-Butyl Calix[4]arene and Study of Their Hosting Ability for Alanine and Na+. Bis-symmetrical tripropoxy p-tert-butyl calix[4]arene esters were ...

  9. Polypyrrole-silver Nanocomposite: Synthesis and Characterization

    OpenAIRE

    D. M. Nerkar; S. V. Panse; S. P. Patil; S. E. Jaware; G. G. Padhye

    2016-01-01

    Polypyrrole-Silver (PPy-Ag) nanocomposite has been successfully synthesized by the chemical oxidative polymerization of pyrrole with iron (III) chloride as an oxidant, in the presence of a colloidal suspension of silver nanoparticles. Turkevich method (Citrate reduction method) was used for the synthesis of silver nanoparticles (Ag NPs). The silver nanoparticles were characterized by UV-Visible spectroscopy which showed an absorption band at 423 nm confirming the formation of nanoparticles. P...

  10. Synthesis and Characterization of Sn2+- based and Bi3+- based metal oxides for photocatalytic applications

    KAUST Repository

    Noureldine, Dalal

    2016-07-01

    The main challenge of water splitting technology is to develop stable, visible responsive photocatalysts that satisfy the thermodynamic requirements to achieve water redox reactions. This study investigates development of the semiconductors containing metals with s2d10 electronic configuration such as Sn2+ or Bi3+ which shifts the valence band position negatively. Efficient water splitting can, however, be only achieved by understanding the fundamental semiconductor properties of underlying processes. This work elucidates the semiconductor properties through two approaches: the first is to synthesize the materials of various stoichiometry in various forms (powders, thin film etc.) and the second is to perform a combined experimental-theoretical studies to determine the optoelectronic properties of the synthesized materials. The study includes the synthesis and characterization of a series of Bi3+ based semiconductors (Bi2Ti2O7, Bi12TiO20, and Bi4Ti3O12) to resolve inconsistencies in their optoelectronic properties. The crystal parameters and stoichiometry were confirmed by the Rietveld refinement and XRD measurements. These compounds showed a UV responsive absorption, high dielectric constants, and low electron and hole effective masses in one crystallographic reflecting their good charge separation and carrier diffusion properties. The approach showed to be accurate in determining the optoelectronic properties due to good agreement between experimental and theoretical values. The second study investigated the synthesis of SnNb2O6 and using flux assisted method which afforded control over the surface. Increasing the flux to reactant molar ratio resulted in a 2D platelets with anisotropic growth along bc plane as confirmed by XRD and SEM. The photocatalytic activity increased while increasing the flux to reactant ratio exceeding solid state synthesis. This method minimized the oxidation of the surface and formation of grain boundaries and enabled the synthesis of

  11. Synthesis and characterization of activated lithium fluoride with silver

    International Nuclear Information System (INIS)

    Encarnacion E, E. K.; Guerrero S, Z.; Reyes A, J.

    2017-10-01

    The present work shows part of the results obtained in the development of the research that has been carried out since 2015 entitled -Synthesis and characterization of new thermoluminescent materials for the radiation dosimetry and its applications in health-. In the development of this research, the synthesis of crystals of pure lithium fluoride (LiF) and activated with different concentrations of silver (LiF:Ag); synthesized samples are also presented using different temperatures, as well as varying the concentration of the solvent (water-ethanol). The synthesized materials were characterized through different techniques: scanning electron microscopy and X-ray diffraction. Specifically, the results of the calculation of the size of the LiF crystals are presented using the Scherrer equation. Within the results, a dependence on the size of the crystals is highlighted by means of the following factors: the amount of activator in the sample, the temperature at which the sample was synthesized, as well as the amount of solvent in the synthesis. The samples have a simple cubic crystalline phase. (Author)

  12. Synthesis and characterization of a new composite based on copper (II) and octa (aminopropil)silsesquioxane

    International Nuclear Information System (INIS)

    Magossi, M.S. de; Carmo, D.R. do

    2014-01-01

    In this work, a new compound based silsesquioxane and nitroprusside of copper was prepared starting from octa (aminopropyl)silsesquioxane following a new route of synthesis. The composite prepared as described ACCuN was preliminarily characterized by spectroscopic techniques, such as Infrared Spectroscopy in the Region of the Fourier transform (FTIR), Energy Dispersive X-ray (EDX), Scanning Electron Microscopy (SEM) and cyclic voltammetry (VC). The FTIR spectra showed absorption bands at 1106 cm"-"1 due to stretching Si-O-Si_(_ν_S_i_-_O_-_S_i_) characteristic of the structure of octa(aminopropylsilsesquioxane and absorption bands at 2063 cm"-"1 ascribed to the stretching NO_(_ν_N_-_O) and 2192 cm"-"1 attributed to the stretching C≡N_(_ν_≡N_). SEM and EDX observed cluster of cubic particles with an average size of approximately 241 nm, containing Si, O, N, Cu and Fe. Cyclic voltammogram of the material (ACCuN) showed a redox couple with average potential Eθ '= 0.73 V. (author)

  13. High temperature bismuth cuprate superconductors synthesis and characterization

    International Nuclear Information System (INIS)

    Mansori, M.; Satre, P.; Breandon, C.; Roubin, M.; Sebaoun, A.

    1993-01-01

    High temperature superconductor phases synthesis by coprecipitation in alkaline solution is reported. (Bi 1.6 Pb 0.4 )Sr 2 Ca 1 Cu 2 O 8+x and (Bi 1.6 Pb 0.4 )Sr 2 Ca 2 Cu 3 O 10+y noted (2212) and (2223) have been prepared and studied. From aqueous nitrate solutions of Bi, Pb, Sr, Ca and Cu and oxalic acid aqueous solution as well as ethylene glycol, using an organic base (the triethylamine), the pH was increased up to the path of the precipitation zone (pH = 10.5-11.2). This method assures a good granulometric homogeneity of powders. Thermal analysis and characterization of the different components produced during the synthesis have been studied by DTA (differential thermal analysis)- TGA (thermogravimetric analysis), X-ray diffraction at different temperatures and by Infrared spectroscopy with a Fourier transformation. The measurements of magnetic susceptibility for the 2212 (with and without lead) and 2223 (with lead) phases have permitted us to observe the critical temperatures of 84 K, 87 K and 114 K. (author). 29 refs., 2 figs., 4 tabs

  14. Synthesis and characterization of copper nanoparticles by using the exploding wire method

    International Nuclear Information System (INIS)

    Das, Rashmita; Das, Basanta Kumar; Shyam, Anurag

    2012-01-01

    During the past few years, the synthesis of copper nanoparticles has attracted much attention because of their huge potential for replacing the expensive nano silver inks utilized in conductive printing. This opens a new possibility in printed electronics. Copper-based inkjet inks can be used to form various devices such as solar cells, RF identification tags and electroluminescence devices. This paper describes controlled synthesis of pure copper nanoparticles, mainly by using the exploding wire method. A wire of 0.26 mm in diameter was exploded in a nitrogen environment. The sample was characterized by using X-ray diffraction (XRD) and atomic force microscopy (AFM). XRD revealed the presence of pure copper and AFM revealed the presence of nanoparticles with an average size of 55 nm.

  15. Magnetic ionic liquids: synthesis and characterization

    International Nuclear Information System (INIS)

    Medeiros, Anderson M.M.S.; Parize, Alexandre L.; Oliveira, Vanda M.; Neto, Brenno A.D.; Rubim, Joel C.

    2010-01-01

    The synthesis of magnetic ionic liquids (MILs) based on the stable dispersions of magnetic nanoparticles (MNPs) of γ-Fe 2 O 3 , Fe 3 O 4 , and CoFe 2 O 4 in the ionic liquid 1-n-butyl-3-methylimidazolium bis(trifluoromethanesulfonyl)imide (BMI.NTf 2 ) is reported. The MNPs were obtained by the coprecipitation method. The surface of the α-Fe 2 O 3 , Fe 3 O 4 , and CoFe 2 O 4 MNPs with mean sizes (XRD) of 9.3, 12.3, and 11.0 nm, respectively were functionalized by 1-n-butyl-3-(3'-trimethoxypropylsilane)- imidazolium chloride. The non functionalized and functionalized MNPs were further characterized by Raman, FTIR-ATR, and FTNIR spectroscopy and by TGA. The stability of the MILs was assigned to the formation of at least one monolayer of the surface modifier agent that mimics the structure of the BMI.NTf 2 IL. (author)

  16. Synthesis, structural and electrical characterizations of thermally ...

    African Journals Online (AJOL)

    Synthesis, structural and electrical characterizations of thermally evaporated Cu 2 SnS 3 thin films. ... The surface profilometer shows that the deposited films are rough. The XRD spectra identified the ... The electrical resistivity of the deposited Cu2SnS3 film is 2.55 x 10-3 Ωcm. The conductivity is in the order of 103 Ω-1cm-1.

  17. Combustion synthesis and structural characterization of Li–Ti mixed

    Indian Academy of Sciences (India)

    Combustion synthesis and structural characterization of Li–Ti mixed nanoferrites ... were prepared by combustion method at lower temperatures compared to the ... first time at low temperatures, using PEG which acts as a new fuel and oxidant.

  18. Synthesis and characterization of a cerebral radiotracer

    International Nuclear Information System (INIS)

    Ben hamouda, Salem

    2010-01-01

    The development of nuclear medicine is based on research of new radiopharmaceuticals, in particular, relying on technetium-99m, the most used radioisotope in terms of availability and low cost. A similar study on Rhenium (185/187Re) is essential for monitoring physico-chemical studies due to the high specific activity of technetium-99m. During this work, we have synthesized and labeled with technetium the N-methyl-4-hydroxy piperidinyl ferrocenyl carboxylate. The marking is done by exchange of ligands between the iron group of ferrocene and tricabonyl technetium core. We have succeeded to synthesis the N-methyl-4-hydroxy piperidinyl carboxyl cyclopentadienyl tricarbonyl rhenium (the molecular analogue of the technetium). We characterized it by MS, IR and NMR (1H, 13C) The structure of N-methyl-4-hydroxy piperidinyl carboxyl cyclopentadienyl tricarbonyl technetium is well justified.

  19. The Synthesis and Characterization of Gold-Core/LDH-Shell Nanoparticles

    Science.gov (United States)

    Rearick, Colton

    In recent years, the field of nanomedicine has progressed at an astonishing rate, particularly with respect to applications in cancer treatment and molecular imaging. Although organic systems have been the frontrunners, inorganic systems have also begun to show promise, especially those based upon silica and magnetic nanoparticles (NPs). Many of these systems are being designed for simultaneous therapeutic and diagnostic capabilities, thus coining the term, theranostics. A unique class of inorganic systems that shows great promise as theranostics is that of layered double hydroxides (LDH). By synthesis of a core/shell structures, e.g. a gold nanoparticle (NP) core and LDH shell, the multifunctional theranostic may be developed without a drastic increase in the structural complexity. To demonstrate initial proof-of-concept of a potential (inorganic) theranostic platform, a Au-core/LDH-shell nanovector has been synthesized and characterized. The LDH shell was heterogeneously nucleated and grown on the surface of silica coated gold NPs via a coprecipitation method. Polyethylene glycol (PEG) was introduced in the initial synthesis steps to improve crystallinity and colloidal stability. Additionally, during synthesis, fluorescein isothiocyanate (FITC) was intercalated into the interlayer spacing of the LDH. In contrast to the PEG stabilization, a post synthesis citric acid treatment was used as a method to control the size and short-term stability. The heterogeneous core-shell system was characterized with scanning electron microscopy (SEM), energy dispersive x-ray spectroscopy (EDX), dynamic light scattering (DLS), and powder x-ray diffraction (PXRD). A preliminary in vitro study carried out with the assistance of Dr. Kaushal Rege's group at Arizona State University was to demonstrate the endocytosis capability of homogeneously-grown LDH NPs. The DLS measurements of the core-shell NPs indicated an average particle size of 212nm. The PXRD analysis showed that PEG

  20. Synthesis and characterization of cadmium doped lead–borate ...

    Indian Academy of Sciences (India)

    Unknown

    Mater. Sci., Vol. 29, No. 1, February 2006, pp. 55–58. © Indian Academy of Sciences. 55. Synthesis and characterization of cadmium doped lead–borate glasses. A A ALEMI*, H SEDGHI†, A R MIRMOHSENI and V GOLSANAMLU. Department of Inorganic Chemistry, Faculty of Chemistry, University of Tabriz, Tabriz, Iran.

  1. Synthesis and characterization of fluorine compounds

    International Nuclear Information System (INIS)

    Martinez Carrillo, M.

    1991-01-01

    The ( 18 F) D-glucose, 2-deoxy fluorine ( 18 FDG) is a radio pharmaceutic that is used in nuclear medicine it is utilized mainly in the glucose metabolism. It allows recently to observe the tumors accumulation and growing. The obtention of this radio pharmaceutic can realize by a nucleophilic or electrophilic process through the use of different fluorinated agents obtained as intermediates for introducing the 18 F radionuclide in a final step of synthesis. The first methods already has been studied in the National Institute of Nuclear Research. The second one which is based this work and it was realized through the reaction of acetyl hypo fluorite (CH 3 COOF) with tri acetyl glucal (TAG) in turn they require the obtention of several fluorated compounds that they serve as intermediates for their obtention so that objective of this work was to find the adequate technique for the obtention of anhydride hydrofluoric acid (HF), KF.2 HF and elemental fluorine so as the design and construction of the systems and equipment used for carry out each one of the reactions. Moreover it was designed the system that will be used for the obtention of acetyl hypo fluoride and the synthesis of composite tetraacetilide 3,4,6 tri-D-glucopyranosil fluoride (TAG-F) for that finally by hydrolysis it was obtained the 2-deoxy fluoride-D-glucose (TAG) in inactive. In this system were realized several preliminary tests. The results are showed in the content of this work also the techniques for compounds characterization were given. (Author)

  2. Synthesis and characterization of new ionic liquids

    International Nuclear Information System (INIS)

    Oliveira, L.M.C. de; Mattedi, S.; Boaventura, J.S.; Iglesias, M.; Universidad de Santiago de Compostela

    2010-01-01

    In recent years, ionic liquids have been highlighted for its potential in various industrial applications. Among them, the salts of Broensted has a promising profile for the low toxicity, low cost and simple synthesis. This paper presents the synthesis and characterization of new salts of Bronsted with branched (lactate) or large chain anions (oleate) for future use as additives promoters of proton conductivity in fuel cells of ethanol. Experimental data were measured for density, sound velocity and conductivity of pure ionic liquids and mixtures. The density decreases linearly with increasing temperature, and sound velocity shows a similar trend, but not linear. The conductivity increases according to the Arrhenius model with activation energy less than 10 J/mol. Tests NMR, FTIR and TGA confirm ionic structure and thermal stability up to 165 deg C. (author)

  3. Refined Synthesis and Characterization of Controlled Diameter, Narrow Size Distribution Microparticles for Aerospace Research Applications

    Science.gov (United States)

    Tiemsin, Pacita I.; Wohl, Christopher J.

    2012-01-01

    Flow visualization using polystyrene microspheres (PSL)s has enabled researchers to learn a tremendous amount of information via particle based diagnostic techniques. To better accommodate wind tunnel researchers needs, PSL synthesis via dispersion polymerization has been carried out at NASA Langley Research Center since the late 1980s. When utilizing seed material for flow visualization, size and size distribution are of paramount importance. Therefore, the work described here focused on further refinement of PSL synthesis and characterization. Through controlled variation of synthetic conditions (chemical concentrations, solution stirring speed, temperature, etc.) a robust, controllable procedure was developed. The relationship between particle size and salt concentration, MgSO4, was identified enabling the determination of PSL diameters a priori. Suggestions of future topics related to PSL synthesis, stability, and size variation are also described.

  4. Combustion synthesis of TiB2-based cermets: modeling and experimental results

    International Nuclear Information System (INIS)

    Martinez Pacheco, M.; Bouma, R.H.B.; Katgerman, L.

    2008-01-01

    TiB 2 -based cermets are prepared by combustion synthesis followed by a pressing stage in a granulate medium. Products obtained by combustion synthesis are characterized by a large remaining porosity (typically 50%). To produce dense cermets, a subsequent densification step is performed after the combustion process and when the reacted material is still hot. To design the process, numerical simulations are carried out and compared to experimental results. In addition, physical and electrical properties of the products related to electrical contact applications are evaluated. (orig.)

  5. Synthesis and characterization of Taurine

    Directory of Open Access Journals (Sweden)

    B Bayarmaa

    2014-10-01

    Full Text Available Have been obtained 2-aminoethanesulfonic acid (taurine from ethanolamine, sulfuric acid and sodium sulfite during the synthesis in laboratory condition. The process involves two steps of reactions, the first was esterification of ethanolamine with sulfuric acid to produce the intermediate product of 2-aminoethyl ester which than was extended to the second step by sulfonation with sodium sulfite to produce 2-aminoethanesulfonic acid. Resulting product was analyzed using 1H-NMR, IR, FAB-MS analysis and examined purity characterizations of the synthesized products. DOI: http://dx.doi.org/10.5564/mjc.v14i0.200 Mongolian Journal of Chemistry 14 (40, 2013, p57-60

  6. Exploring the Fundamentals of Microreactor Technology with Multidisciplinary Lab Experiments Combining the Synthesis and Characterization of Inorganic Nanoparticles

    Science.gov (United States)

    Emmanuel, Noemie; Emonds-Alt, Gauthier; Lismont, Marjorie; Eppe, Gauthier; Monbaliu, Jean-Christophe M.

    2017-01-01

    Multidisciplinary lab experiments combining microfluidics, nanoparticle synthesis, and characterization are presented. These experiments rely on the implementation of affordable yet efficient microfluidic setups based on perfluoroalkoxyalkane (PFA) capillary coils and standard HPLC connectors in upper undergraduate chemistry laboratories.…

  7. Synthesis, Properties Characterization and Applications of Various Organobismuth Compounds

    Directory of Open Access Journals (Sweden)

    Jingfei Luan

    2011-05-01

    Full Text Available Organobismuth chemistry was emphasized in this review article due to the low price, low toxicity and low radioactivity characteristics of bismuth. As an environmentally-friendly class of organometallic compounds, different types of organobismuth compounds have been used in organic synthesis, catalysis, materials, etc. The synthesis and property characterization of many organobismuth compounds had been summarized. This review article also presented a survey of various applications of organobismuth compounds in organic transformations, as reagents or catalysts. The reactivity, reaction pathways and mechanisms of reactions with organobismuths were discussed. Less common and limiting aspects of organobismuth compounds were also briefly mentioned.

  8. SYNTHESIS AND CHARACTERIZATION OF NEW HALOGENATED CURCUMINOIDS

    Directory of Open Access Journals (Sweden)

    Eugenio Torres

    2013-12-01

    Full Text Available In this work a novel procedure of synthesis of compounds analogues to curcumin with halogens atoms in its structure is described, which can increase its solubility and biological activity. Four halogenated curcuminoids were obtained with great pharmacological interest, none of them reported in literature before. Synthesis was carried out by means of the aldol condensation assisted by microwaves of halogenated aromatic aldehydes and acetylacetona, using morpholine as basic catalyst, in absence of solvent, and the reaction just needed 1 min. The products were purified by treatment of the reaction mixture with methanol under ultrasound irradiation, followed by chromatographic column. All obtained compounds were characterized by infrared spectroscopy, nuclear magnetic resonance, quantitative elementary analysis and high resolution mass spectrometry. The RMN-1H data demonstrate in all structures of synthesized curcuminoids the enol form is the most favored.

  9. Synthesis and characterization of thermally oxidized ZnO films

    Indian Academy of Sciences (India)

    Administrator

    Synthesis and characterization of thermally oxidized ZnO films. A P RAMBU1,* and N IFTIMIE2 .... R. −. Δ. = = (1) where Ra is the sensor resistance in the air and Rg is the .... ple, Aida and coworkers (2006) reported that the total oxidation is ...

  10. Synthesis and characterization of semi-IPNs based on PVP and PLLA; Sintese e caracterizacao de semi-IPNs envolvendo os homopolimeros PVP e PLLA

    Energy Technology Data Exchange (ETDEWEB)

    Camilo, A.P.R.; Mano, V., E-mail: mano@ufsj.edu.b [Universidade Federal de Sao Joao del Rei (UFSJ), MG (Brazil). Dept. de Ciencias Naturais; Felisberti, M.I. [Universidade Estadual de Campinas (IQ/UNICAMP), SP (Brazil). Inst. de Quimica

    2010-07-01

    The specific interest in the synthesis of semi-IPNs based on PLLA and PVP homopolymers due to the fact these are biodegradable and biocompatible, which allows us to infer applications in the medical field as sutures, implants, matrices for controlled release of drugs etc. The objective was to prepare a multicomponent material amphiphile in the form of semi-interpenetrating polymer networks, based on poly (L-lactide), PLLA, hydrophobic homopolymer, and poly (vinylpyrrolidone), PVP, hydrophilic component. The preparation of semi-IPN combined the polymerization and crosslinking of N-vinylpyrrolidone in the presence of poly (L-lactide). The products were characterized by spectroscopic and thermal methods. (author)

  11. Synthesis and characterization of acrylate copolymer containing fluorescein functional group

    International Nuclear Information System (INIS)

    Hui, Guodong; Huang, Weiyun; Song, Yunzhao; Chen, Deben; Zhong, Anyong

    2013-01-01

    We report a novel method to fabricate fluorescent polymer (F-CPA) based on the esterification between acrylate copolymer (CPA) and fluorescein using N, N-dicyclohexylcarbodiimide (DCC)/4-dimethylaminopyridine (DMAP) as catalyst. The resulting copolymer was characterized by Fourier transform-infrared spectroscopy (FT-IR), gel permeation chromatography (GPC), differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), ultraviolet-visible spectroscopy (UV-Vis) and fluorescence spectroscopy. In addition, the influences of concentration, solvents, pH and metal cations (Cu"2"+, Fe"3"+ and Zn"2"+) on the fluorescent behaviors of F-CPA are discussed in detail. All those observations suggest that the synthesized F-CPA is an excellent luminescent macromolecular material with simple synthesis method and excellent solubility. Moreover, its sensitive fluorescence response behaviors to solvents, pH and metal cations make it to become a polymer-based probe

  12. Synthesis and characterization of amorphous cellulose from triacetate of cellulose

    International Nuclear Information System (INIS)

    Vega-Baudrit, Jose; Sibaja, Maria; Nikolaeva, Svetlana; Rivera A, Andrea

    2014-01-01

    It was carried-out a study for the synthesis and characterization of amorphous cellulose starting from cellulose triacetate. X-rays diffraction was used in order to obtain the cellulose crystallinity degree, also infrared spectroscopy FTIR was used. (author)

  13. Synthesis, Characterization and Applications of Ethyl Cellulose-Based Polymeric Calcium(II) Hydrogen Phosphate Composite

    Science.gov (United States)

    Mohammad, Faruq; Arfin, Tanvir; Al-Lohedan, Hamad A.

    2018-03-01

    The present report deals with the synthesis, characterization and testing of an ethyl cellulose-calcium(II) hydrogen phosphate (EC-CaHPO4) composite, where a sol-gel synthesis method was applied for the preparation of the composite so as to test its efficacy towards the electrochemical, biological, and adsorption related applications. The physical properties of the composite were characterized by using scanning electron microscopy (SEM), ultraviolet- visible (UV-Vis) spectroscopy, and fourier transform-infrared (FTIR) spectroscopy. On testing, the mechanical properties indicated that the composite is highly stable due to the cross-linked rigid framework and the enhanced interactions offered by the EC polymer supported for its binding very effectively. In addition, the conductivity of EC-CaHPO4 is completely governed by the transport mechanism where the electrolyte concentration has preference towards the adsorption of ions and the variations in the conductivity significantly affected the material's performance. We observed an increasing order of KCl > NaCl for the conductivity when 1:1 electrolytes were applied. Further, the material was tested for its usefulness towards the purification of industrial waste waters by removing harmful metal ions from the samples collected near the Aligarh city, India where the data indicates that the material has highest affinity towards Pb2+, Cu2+, Ni2+ and Fe3+ metal ions. Finally, the biological efficiency of the material was confirmed by means of testing the antibacterial activity against two gram positive (staphylococcus aureus and Bacillus thuringiensis) and two gram negative bacteriums (Pseudomonas aeruginosa and Patoea dispersa). Thus, from the cumulative study of outcomes, it indicates that the EC-CaHPO4 composite found to serve as a potential smart biomaterial due to its efficiency in many different applications that includes the electrical conductivity, adsorption capability, and antimicrobial activity.

  14. Characterization structural and morphology ZSM-5 zeolite by hydrothermal synthesis

    International Nuclear Information System (INIS)

    Silva, V.J.; Crispim, A.C.; Queiroz, M.B.; Laborde, H.M.; Rodrigues, M.G.F.; Menezes, R.R.

    2009-01-01

    Solid acids are catalytic materials commonly used in the chemical industry. Among these zeolites are the most important business processes including water treatment, gas separation, and cracking long hydrocarbon chains to produce high octane gasoline. Its synthesis, characterization and applications have been widely studied. The objective this study was to synthesize the ZSM-5 zeolite for future use in separation processes and catalysis. The zeolite ZSM-5 was prepared by hydrothermal synthesis at 170°C, using silica, deionized water and the director of structures (TPABr - tetrapropylammonium bromide). The materials were characterized by X ray diffraction (XRD), scanning electron microscopy (SEM) and semiquantitative chemical analysis by X ray fluorescence (XRF). According to the XRD was possible to observe the formation of ZSM-5 zeolite, with peaks intense and well defined. The SEM showed the formation of individual particles, clean, rounded shapes. (author)

  15. Polymer Brushes: Synthesis, Characterization, Applications

    Science.gov (United States)

    Advincula, Rigoberto C.; Brittain, William J.; Caster, Kenneth C.; Rühe, Jürgen

    2004-09-01

    Materials scientists, polymer chemists, surface physicists and materials engineers will find this book a complete and detailed treatise on the field of polymer brushes, their synthesis, characterization and manifold applications. In a first section, the various synthetic pathways and different surface materials are introduced and explained, followed by a second section covering important aspects of characterization and analysis in both flat surfaces and particles. These specific surface initiated polymerization (SIP) systems such as linear polymers, homopolymers, block copolymers, and hyperbranched polymers are unique compared to previously reported systems by chemisorption or physisorption. They have found their way in both large-scale and miniature applications of polymer brushes, which is covered in the last section. Such 'hairy' surfaces offer fascinating opportunities for addressing numerous problems of both academic and, in particular, industrial interest: high-quality, functional or protective coatings, composite materials, surface engineered particles, metal-organic interfaces, biological applications, micro-patterning, colloids, nanoparticles, functional devices, and many more. It is the desire of the authors that this book will be of benefit to readers who want to "brush-up on polymers".

  16. Uranium and thorium based phosphate matrix: synthesis, characterizations and lixiviation

    International Nuclear Information System (INIS)

    Dacheux, N.

    1995-03-01

    In the framework of the search for a ceramic material usable in the radioactive waste storage, uranium and thorium phosphates have been investigated. Their experimental synthesis conditions have been entirely reviewed, they lead to the preparation of four new compounds: U(UO 2 )(PO 4 ) 2 , U 2 O(PO 4 ) 2 , UCIPO 4 , 4H 2 O, and Th 4 (PO 4 ) 4 P 2 O 7 . Experimental evidenced are advanced for non existent compounds such as: U 3 (PO 4 ) 4 , U 2 O 3 P 2 O 7 and Th 3 (PO 4 ) 4 . Characterization by several techniques (X-rays and neutron powder diffractions, UV-Visible and Infra-red spectroscopies, XPS,...) were performed. The ab initio structure determination of U(UO 2 )(PO 4 ) 2 has been achieved by X-rays and refined by neutron diffractions. Through its physico-chemical analysis, we found that this compound was a new mixed valence uranium phosphate in which U 4+ and UO 2 2+ ions are ordered in pairs along parallel chains according to a new type of arrangement. Reaction mechanism, starting from UCIPO 4 , 4H 2 O and based on redox processes of uranium in solid state was set up. From two main matrices U(UO 2 )(PO 4 ) 2 and Th 4 (PO 4 ) 4 P 2 O 7 , solid solutions were studied. They consist of replacement of U(IV) by Th(IV) and reversely. The leaching tests on pure, loaded and doped matrices were performed in terms of storage time, pH of solutions, and determined by the use of solids labelled with 230 U or by the measurement of uranyl concentration by Laser-Induced Time-Resolved Spectro-fluorimetry. Average concentration of uranium in the liquid phase is around 10 -4 M to 10 -6 M. Taking into account the very low solubilities of the studied phosphate ceramics, we estimated their chemical performances promising as an answer to the important nuclear waste problem, if we compare them to the glasses used at the present time. (author)

  17. Synthesis and characterization of five-coordinated indium amidinates

    Energy Technology Data Exchange (ETDEWEB)

    Riahi, Yasaman

    2016-07-29

    The focus of this work is synthesis, characterization and exploring the reactivity of new indium amidinate compounds of the type R{sub 2}InX (R = R''NCR'NR''; R' = Ph, R'' = SiMe{sub 3}, iPr, dipp; X = Br, Cl) with the coordination number of five and R{sub 3}In (R = Me{sub 3}SiNCPhNSiMe{sub 3}) with the coordination number of six. By using amidinates as chelating ligands the electron deficiency of indium atom will be resolved. Additionally, by using different substituents the study of the different synthesized indium amidinates has become possible. The selected method for the synthesis allows the carbodiimides to react with organolithium compounds to get the corresponding lithium amidinates. Afterwards the resulting lithium amidinates take part in transmetalation reactions with InBr{sub 3} and InCl{sub 3}. The study of the reactivity of indium amidinate complexes including nucleophilic reactions as well as their reduction were also examined. Beside crystal structure analysis, nuclear magnetic resonance spectroscopy as well as elemental analysis has been applied to characterize the compounds.

  18. Synthesis and Characterization of Nano Scale YBCO

    International Nuclear Information System (INIS)

    Sukirman, E.; Wisnu AA; Yustinus P; Sahidin W, D.; Rina M, Th.

    2009-01-01

    Synthesis and characterization of the nano scale YBCO superconductor have been performed. The nano scale superconductor was synthesized from YBCO system (YBa 2 Cu 3 O 7-X ). Raw materials, namely Y 2 O 3 , BaCO 3 , and Cu°, were balanced and mixed with ethanol using magnetic steering as a churn in a beaker glass. Then, the precursor was calcined at T k = 900°C for 5 hours and repeated it until three times. The resulting precursor was ground by using High Energy Milling (HEM) for t = 0, 30, 50, 70, and 90 hour and hereinafter precursors are successively referred as YKM-00, YKM-30, YKM-50, YKM-70, and YKM-90. The resulting powders phase were characterized by means of x-ray diffraction technique using the Rietveld analysis method. Precursor of YKM-90 was pressed into pellets, and then sintered at various temperatures and periods. The sample phase was then characterized by using the Rietveld analysis method based on the x-ray diffraction data. The crystallites size were calculated using Scherrer formula. Results of analysis indicate that by minimizing crystallites size, period of sinter can be shortened from 10 to 1 hour, resulting crystallite size of D = 925 Å, critical current density of J c = 4 A / cm 2 , and can be grown of about 15 weight % of 211-phase in a matrix of 123-phase. The decrease of crystallite size will generate a change in physical properties dramatically, if the crystallite size of the material, D is smaller or equal to the coherence length of 10 Å. (author)

  19. Design, Synthesis and Characterization of Polyethylene-Based Macromolecular Architectures by Combining Polyhomologation with Powerful Linking Chemistry

    KAUST Repository

    Alkayal, Nazeeha

    2016-09-05

    Polyhomologation is a powerful method to prepare polyethylene-based materials with controlled molecular weight, topology and composition. This dissertation focuses on the discovery of new synthetic routes to prepare polyethylene-based macromolecular architectures by combining polyhomologation with highly orthogonal and efficient linking reactions such as Diels Alder, copper-catalyzed azide-alkyne cycloaddition (CuAAC), and Glaser. Taking advantage of functionalized polyhomologation initiators, as well as of the efficient coupling chemistry, we were able to synthesize various types of polymethylene (polyethylene)-based materials with complex architectures including linear co/terpolymers, graft terpolymers, and tadpole copolymers. In the first project, a facile synthetic route towards well-defined polymethylene-based co/terpolymers, by combining the anthracene/maleimide Diels–Alder reaction with polyhomologation, is presented. For the synthesis of diblock copolymers the following approach was applied: (a) synthesis of α-anthracene-ω-hydroxy-polymethylene by polyhomologation using tri (9 anthracene-methyl propyl ether) borane as the initiator, (b) synthesis of furan-protected-maleimide-terminated poly(ε-caprolactone) or polyethylene glycol and (c) Diels–Alder reaction between anthracene and maleimide-terminated polymers. In the case of triblock terpolymers, the α-anthracene-ω-hydroxy polymethylene was used as a macroinitiator for the ring-opening polymerization of D, L-lactide to afford an anthracene-terminated PM-b-PLA copolymer, followed by the Diels–Alder reaction with furan-protected maleimide-terminated poly (ε-caprolactone) or polyethylene glycol to give the triblock terpolymers. The synthetic methodology is general and potentially applicable to a range of polymers. The coupling reaction applied in the second project of this dissertation was copper-catalyzed “click” cycloaddition of azides and alkynes (CuAAC). Novel well-defined polyethylene-based

  20. Synthesis and Characterization of New Polyamides from 1,2-Bis hydrazine Derivatives

    International Nuclear Information System (INIS)

    Salaha, A.; Abdel-Bary, E.M.; Kandilea, N.G.

    2005-01-01

    Preparation of polyamides having different chemical structures allows obtaining new materials with different mechanical and physical properties. The difference in the chemical structure depends mainly on the starting reactants used in condensation polymerization of polyamides. In this paper the synthesis of new polyamides based on the condensation polymerization of 1,2- Bis(3-carboxyacryloyl or carboxybenzoyl) hydrazine derivatives and various diamines has been described. The polymers obtained were characterized using spectroscopic and X-ray analysis. Besides thermal stability and electrical conductivity have been evaluated and correlated with the chemical structure of the polyamides obtained

  1. Characterization of PDMS samples with variation of its synthesis parameters for tunable optics applications

    Science.gov (United States)

    Marquez-Garcia, Josimar; Cruz-Félix, Angel S.; Santiago-Alvarado, Agustin; González-García, Jorge

    2017-09-01

    Nowadays the elastomer known as polydimethylsiloxane (PDMS, Sylgard 184), due to its physical properties, low cost and easy handle, have become a frequently used material for the elaboration of optical components such as: variable focal length liquid lenses, optical waveguides, solid elastic lenses, etc. In recent years, we have been working in the characterization of this material for applications in visual sciences; in this work, we describe the elaboration of PDMSmade samples, also, we present physical and optical properties of the samples by varying its synthesis parameters such as base: curing agent ratio, and both, curing time and temperature. In the case of mechanical properties, tensile and compression tests were carried out through a universal testing machine to obtain the respective stress-strain curves, and to obtain information regarding its optical properties, UV-vis spectroscopy is applied to the samples to obtain transmittance and absorbance curves. Index of refraction variation was obtained through an Abbe refractometer. Results from the characterization will determine the proper synthesis parameters for the elaboration of tunable refractive surfaces for potential applications in robotics.

  2. Synthesis and Characterization of Novel Quaternary Thioaluminogermanates

    KAUST Repository

    Al-Bloushi, Mohammed

    2013-05-01

    Metal chalcogenides form an important class of inorganic materials, which include several technologically important applications. The design of metal chlcogenides is of technological interest and has encouraged recent research into moderate temperature solid-state synthetic methods for the single crystal growth of new materials. The aim of this project is the investigation and development of synthetic methodology for the synthesis of novel metal chlcogenides. The new inorganic compounds of the type “M(AlS2)(GeS2)” (M = Na and K) are new metal-chalcogenides, synthesized by the classical solid state approach. The characterization of these compounds was carried out by Scanning Electron Microscopy (SEM), Energy Dispersive X-ray Spectroscopy (EDS), Single crystal and powder X-ray diffraction, solid state Nuclear Magnetic Resonance (NMR), Ultraviolet-visible (UV-VIS), Infrared (IR) and Raman spectroscopy. These theses study the synthesis of metal chalcogenides through the use of standard chemical techniques. The systematic studies demonstrate the effect of the reactants ratio and reaction temperature on the synthesis and growth of the single crystals. Metal chalcogenides have several potential applications in gas separation, ion exchange, environmental remediation, and energy storage. Especially, the ion exchange materials have found\\tpossible applications in waste-water treatment, water softening, metal separation, and production of high purity water.

  3. Synthesis and characterization of acrylate copolymer containing fluorescein functional group

    Energy Technology Data Exchange (ETDEWEB)

    Hui, Guodong; Huang, Weiyun; Song, Yunzhao; Chen, Deben; Zhong, Anyong [Sichuan University, Chengdu (China)

    2013-08-15

    We report a novel method to fabricate fluorescent polymer (F-CPA) based on the esterification between acrylate copolymer (CPA) and fluorescein using N, N-dicyclohexylcarbodiimide (DCC)/4-dimethylaminopyridine (DMAP) as catalyst. The resulting copolymer was characterized by Fourier transform-infrared spectroscopy (FT-IR), gel permeation chromatography (GPC), differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), ultraviolet-visible spectroscopy (UV-Vis) and fluorescence spectroscopy. In addition, the influences of concentration, solvents, pH and metal cations (Cu{sup 2+}, Fe{sup 3+} and Zn{sup 2+}) on the fluorescent behaviors of F-CPA are discussed in detail. All those observations suggest that the synthesized F-CPA is an excellent luminescent macromolecular material with simple synthesis method and excellent solubility. Moreover, its sensitive fluorescence response behaviors to solvents, pH and metal cations make it to become a polymer-based probe.

  4. Synthesis and Characterization of Starch-based Aqueous Polymer Isocyanate Wood Adhesive

    Directory of Open Access Journals (Sweden)

    Shu-min Wang

    2015-09-01

    Full Text Available Modified starch was prepared in this work by acid-thinning and oxidizing corn starch with ammonium persulfate. Also, starch-based aqueous polymer isocyanate (API wood adhesive was prepared. The effect of the added amount of modified starch, styrene butadiene rubber (SBR, polymeric diphenylmethane diisocyanate (P-MDI, and the mass concentration of polyvinyl alcohol (PVOH on the bonding strength of starch-based API adhesives were determined by orthogonal testing. The starch-based API adhesive performance was found to be the best when the addition of modified starch (mass concentration 35% was 45 g, the amount of SBR was 3%, the PVOH mass concentration was 10%, and the amount of P-MDI was 18%. The compression shearing of glulam produced by starch-based API adhesive reached bonding performance indicators of I type adhesive. A scanning electron microscope (SEM was used to analyze the changes in micro-morphology of the starch surface during each stage. Fourier transform infrared spectroscopy (FT-IR was used to study the changes in absorption peaks and functional groups from starch to starch-based API adhesives. The results showed that during starch-based API adhesive synthesis, corn starch surface was differently changed and it gradually reacted with other materials.

  5. Synthesis and characterization of innovative insulation materials

    Directory of Open Access Journals (Sweden)

    Skaropoulou Aggeliki

    2018-01-01

    Full Text Available Insulation elements are distinguished in inorganic fibrous and organic foamed materials. Foamed insulation materials are of great acceptance and use, but their major disadvantage is their flammability. In case of fire, they tend to transmit the flame producing toxic gases. In this paper, the synthesis and characterization of innovative inorganic insulation materials with properties competitive to commercial is presented. Their synthesis involves the mixing of inorganic raw material and water with reinforcing agent or/and foaming agent leading to the formation of a gel. Depending on raw materials nature, the insulation material is produced by freeze drying or ambient drying techniques of the gel. The raw material used are chemically benign and abundantly available materials, or industrial by-products and the final products are non-toxic and, in some cases, non-flammable. Their density and thermal conductivity was measured and found 0.02-0.06 g/cm3 and 0.03-0.04 W/mK, respectively.

  6. Synthesis and characterization of a binary oxide ZrO2–TiO2 and its ...

    Indian Academy of Sciences (India)

    Administrator

    Synthesis and characterization of a binary oxide ZrO2–TiO2 and its application in ... Solar cells based on dye-sensitized TiO2 nanoparticles were first developed by Grätzel ... cells, resulting in high Jsc (short-circuit current density),. *Author for .... simple method to study dye sensitization of semiconduc- tors. It is found that the ...

  7. Carbon and oxide nanostructures. Synthesis, characterisation and applications

    Energy Technology Data Exchange (ETDEWEB)

    Yahya, Noorhana [Universiti Teknologi PETRONAS, Tronoh, Perak (Malaysia). Dept. of Fundamental and Applied Sciences

    2010-07-01

    This volume covers all aspects of carbon and oxide based nanostructured materials. The topics include synthesis, characterization and application of carbon-based namely carbon nanotubes, carbon nanofibres, fullerenes, carbon filled composites etc. In addition, metal oxides namely, ZnO, TiO2, Fe2O3, ferrites, garnets etc., for various applications like sensors, solar cells, transformers, antennas, catalysts, batteries, lubricants, are presented. The book also includes the modeling of oxide and carbon based nanomaterials. The book covers the topics: - Synthesis, characterization and application of carbon nanotubes, carbon nanofibres, fullerenes - Synthesis, characterization and application of oxide based nanomaterials. - Nanostructured magnetic and electric materials and their applications. - Nanostructured materials for petro-chemical industry. - Oxide and carbon based thin films for electronics and sustainable energy. - Theory, calculations and modeling of nanostructured materials. (orig.)

  8. Novel mesoporous composites based on natural rubber and hexagonal mesoporous silica: Synthesis and characterization

    Energy Technology Data Exchange (ETDEWEB)

    Nuntang, Sakdinun; Poompradub, Sirilux [Fuels Research Center, Department of Chemical Technology, Faculty of Science, Chulalongkorn University, Patumwan, Bangkok 10330 (Thailand); Butnark, Suchada [PTT Research and Technology Institute, PTT Public Company Limited, Wangnoi, Ayutthaya 13170 (Thailand); Yokoi, Toshiyuki; Tatsumi, Takashi [Division of Catalytic Chemistry, Chemical Resources Laboratory, Tokyo Institute of Technology, 4259 Nagatsuta, Midori-ku, Yokohama 226-8503 (Japan); Ngamcharussrivichai, Chawalit, E-mail: Chawalit.Ng@Chula.ac.th [Fuels Research Center, Department of Chemical Technology, Faculty of Science, Chulalongkorn University, Patumwan, Bangkok 10330 (Thailand); Center of Excellence on Petrochemical and Materials Technology (PETROMAT), Chulalongkorn University, Patumwan, Bangkok 10330 (Thailand)

    2014-02-14

    The present study is the first report on the synthesis and characterization of mesoporous composites based on natural rubber (NR) and hexagonal mesoporous silica (HMS). A series of NR/HMS composites were prepared in tetrahydrofuran via an in situ sol–gel process using tetraethylorthosilicate as the silica precursor. The physicochemical properties of the composites were characterized by various techniques. The effects of the gel composition on the structural and textural properties of the NR/HMS composites were investigated. The Fourier-transform infrared spectroscopy (FTIR) and {sup 29}Si magic angle spinning nuclear magnetic resonance ({sup 29}Si MAS NMR) results revealed that the surface silanol groups of NR/HMS composites were covered with NR molecules. The powder X-ray diffraction (XRD) and transmission electron microscopy (TEM) data indicated an expansion of the hexagonal unit cell and channel wall thickness due to the incorporation of NR molecules into the mesoporous structure. NR/HMS composites also possessed nanosized particles (∼79.4 nm) as confirmed by scanning electron microscopy (SEM) and particle size distribution analysis. From N{sub 2} adsorption–desorption measurement, the NR/HMS composites possessed a high BET surface area, large pore volume and narrow pore size distribution. Further, they were enhanced hydrophobicity confirmed by H{sub 2}O adsorption–desorption measurement. In addition, the mechanistic pathway of the NR/HMS composite formation was proposed. - Highlights: • NR molecules were incorporated into hexagonal meso-structure of HMS. • NR/HMS composites exhibited an expanded unit cell and channel wall thickness. • Nanosized NR/HMS composites with a lower particle size range were obtained. • NR/HMS had high surface area, large pore volume and narrow pore size distribution. • NR/HMS composites displayed an enhanced hydrophobicity.

  9. Graphene optoelectronics synthesis, characterization, properties, and applications

    CERN Document Server

    bin M Yusoff, Abdul Rashid

    2014-01-01

    This first book on emerging applications for this innovative material gives an up-to-date account of the many opportunities graphene offers high-end optoelectronics.The text focuses on potential as well as already realized applications, discussing metallic and passive components, such as transparent conductors and smart windows, as well as high-frequency devices, spintronics, photonics, and terahertz devices. Also included are sections on the fundamental properties, synthesis, and characterization of graphene. With its unique coverage, this book will be welcomed by materials scientists, solid-

  10. Synthesis and characterization of triangulene

    Science.gov (United States)

    Pavliček, Niko; Mistry, Anish; Majzik, Zsolt; Moll, Nikolaj; Meyer, Gerhard; Fox, David J.; Gross, Leo

    2017-05-01

    Triangulene, the smallest triplet-ground-state polybenzenoid (also known as Clar's hydrocarbon), has been an enigmatic molecule ever since its existence was first hypothesized. Despite containing an even number of carbons (22, in six fused benzene rings), it is not possible to draw Kekulé-style resonant structures for the whole molecule: any attempt results in two unpaired valence electrons. Synthesis and characterization of unsubstituted triangulene has not been achieved because of its extreme reactivity, although the addition of substituents has allowed the stabilization and synthesis of the triangulene core and verification of the triplet ground state via electron paramagnetic resonance measurements. Here we show the on-surface generation of unsubstituted triangulene that consists of six fused benzene rings. The tip of a combined scanning tunnelling and atomic force microscope (STM/AFM) was used to dehydrogenate precursor molecules. STM measurements in combination with density functional theory (DFT) calculations confirmed that triangulene keeps its free-molecule properties on the surface, whereas AFM measurements resolved its planar, threefold symmetric molecular structure. The unique topology of such non-Kekulé hydrocarbons results in open-shell π-conjugated graphene fragments that give rise to high-spin ground states, potentially useful in organic spintronic devices. Our generation method renders manifold experiments possible to investigate triangulene and related open-shell fragments at the single-molecule level.

  11. Synthesis and characterization of LiFePO{sub 4} cathode preparation by low temperature method

    Energy Technology Data Exchange (ETDEWEB)

    Rajesh, Desapogu, E-mail: rajesh.desapogu@gmail.com; Srinivas Naik, V.; Sunandana, C.S., E-mail: sunandana@gmail.com

    2015-05-01

    We review in detail the physics and technology of the novel material LiFePO{sub 4}, a potential cathode material for Li-ion batteries. In the present work, nano crystalline LiFePO{sub 4} film has been synthesized in both powder and thin film forms from a non-aqueous sol–gel synthesis route based on oxalates of Li and Fe (II). Ferrous oxalate has been synthesized indigenously using a ferrous sulphate based chemical reaction and characterized. Nano powders and thin films of LiFePO{sub 4} have been fabricated and coated on stainless steel substrates with the aim of device development in future. The material has been characterized extensively by XRD for crystal structure, FESEM for microstructure, EDS for elemental analysis and FTIR for the internal modes of phosphate ion. Fe{sup 3+} impurity characterization has been done by using ESR.

  12. Synthesis and Characterization of Calcium Phosphate Powders for Biomedical Applications by Plasma Spray Coating

    OpenAIRE

    Sasidharan Pillai, Rahul

    2015-01-01

    This PhD work mainly focus on the synthesis and characterization of calcium phosphate powders for plasma spray coating. The preparation of high temperature phase stabilized βTCP and HA/βTCP powders for plasma spray coating applications has been the topic of investigation. Nowadays plasma sprayed coatings are widely used for biomedical applications especially in the dental and orthopaedic implantation field. Previously Ti based alloys were widely used for the orthopaedic and dental implant ap...

  13. Synthesis and characterization of the Cu2ZnSnS4 system for photovoltaic applications

    Science.gov (United States)

    Sánchez Pinzón, D. L.; Soracá Perez, G. Y.; Gómez Cuaspud, J. A.; López, E. Vera

    2017-01-01

    This paper focuses on the synthesis and characterization of a ceramic material based on the Cu2ZnSnS4 system, through the implementation of a hydrothermal route. For this purpose, we started from nitrate dissolutions in a 1.0mol L-1 concentration, which were mixed and treated in a teflon lined vessel steel at 280°C for 48h. The Physicochemical characterization of the solid was evaluated by means of ultraviolet visible spectroscopy (UV-VIS), X-ray diffraction (XRD), Raman spectroscopy, scanning and transmission electron microscopy (SEM-TEM) and solid state impedance spectroscopy (IS). The initial characterization through UV measurements confirms a Band-gap around 1.46eV obtained by the Kubelka-Munk method, which demonstrates the effectiveness of the synthesis method in the obtaining of a semiconductor material. The XRD results confirm the obtaining of a crystalline material of pure phase with tetragonal geometry and I-42m space group. The preferential crystalline orientation was achieved along (2 2 0) facet, with crystallite sizes of nanometric order (6.0nm). The morphological aspects evaluated by means electron microscopy, confirmed the homogeneity of the material, showing specifically a series of textural and surface properties of relevant importance. Finally, the electrical characterizations allow to validate the semiconductor behaviour of CZTS system for development of photovoltaic technologies.

  14. Magnetic zeolite NaA: synthesis, characterization based on metakaolin and its application for the removal of Cu2+, Pb2+.

    Science.gov (United States)

    Liu, Haibo; Peng, Shuchuan; Shu, Lin; Chen, Tianhu; Bao, Teng; Frost, Ray L

    2013-06-01

    The optimum parameters for synthesis of zeolite NaA based on metakaolin were investigated according to results of cation exchange capacity and static water adsorption of all synthesis products and selected X-ray diffraction (XRD). Magnetic zeolite NaA was synthesized by adding Fe3O4 in the precursor of zeolite. Zeolite NaA and magnetic zeolite NaA were characterized with scanning electron microscopy (SEM) and XRD. Magnetic zeolite NaA with different Fe3O4 loadings was prepared and used for removal of heavy metals (Cu(2+), Pb(2+)). The results show the optimum parameters for synthesis zeolite NaA are SiO2/Al2O3=2.3, Na2O/SiO2=1.4, H2O/Na2O=50, crystallization time 8h, crystallization temperature 95 °C. The addition of Fe3O4 makes the NaA zeolite with good magnetic susceptibility and good magnetic stability regardless of the Fe3O4 loading, confirming the considerable separation efficiency. Additionally, Fe3O4 loading had a little effect on removal of heavy metal by magnetic zeolite, however, the adsorption capacity still reaches 2.3 mmol g(-1) for Cu(2+), Pb(2+) with a removal efficiency of over 95% in spite of 4.7% Fe3O4 loading. This indicates magnetic zeolite can be used to remove metal heavy at least Cu(2+), Pb(2+) from water with metallic contaminants and can be separated easily after a magnetic process. Copyright © 2013 Elsevier Ltd. All rights reserved.

  15. Microwave hydrothermal synthesis and characterization of PZT 52/48 powders

    International Nuclear Information System (INIS)

    Teixeira, G.F.; Gasparotto, G.; Santos, N.A.; Zaghete, M.A.; Varela, J.A.; Longo, E.

    2009-01-01

    Full text: Lead Zirconate Titanate (PZT) is a ceramic witch has great interest because of their ferroelectric, piezoelectric, and other electrical properties. In this work Pb(ZrxTi1-x)O3 powders were synthesized by microwave hydrothermal synthesis (M-H) at 180°C without excess lead content. This method allows obtaining particles whit nanometer size, good stoichiometric controls, high purity and crystalline degree at low temperatures and short times of synthesis. Powders were synthesized with molar concentration of 0.15 mol.L -1 during different times: 30 min, 2, 4, 6 and 8 h. After that the powders were characterized by X-ray diffraction (XRD), Field Emission Gun (FEG) and photoluminescence (PL). Through analysis it is observed that the crystalline phase of PZT is obtained from 2 hours of synthesis and this same time also presents more intense PL emission. (author)

  16. Synthesis and characterization of an effective organic/inorganic hybrid green corrosion inhibitive complex based on zinc acetate/Urtica Dioica

    Science.gov (United States)

    Salehi, E.; Naderi, Reza; Ramezanzadeh, B.

    2017-02-01

    This study aims at synthesis and characterization of an effective corrosion inhibitive complex based on zinc acetate/Urtica Dioica (ZnA-U.D) for corrosion protection of mild steel in chloride solution. The chemical structure and morphology of the complex were characterized by Fourier transform infrared spectroscopy (FT-IR), UV-vis, thermal gravimetric analysis (TGA), X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM). The corrosion protection performance of the mild steel samples dipped in 3.5 wt.% NaCl solutions with and without ZnA-U.D extract was investigated by visual observations, open circuit potential (OCP) measurements, electrochemical impedance spectroscopy (EIS) and polarization test. Results revealed that the ZnA successfully chelated with organic inhibitive compounds (i.e Quercetin, Quinic acid, Caffeic acid, Hystamine and Serotonin) present in the U.D extract. The electrochemical measurements revealed the effective inhibition action of ZnA-U.D complex in the sodium chloride solution on the mild steel. The synergistic effect between Zn2+ and organic compounds present in the U.D extract resulted in protective film deposition on the steel surface, which was proved by SEM and XPS analyses.

  17. Electronic, electrical and magnetic ceramics synthesis and characterization

    International Nuclear Information System (INIS)

    Calix, V.S.; Saligan, P.P.; Naval, P.C.

    1989-01-01

    This paper describes the research and development activities of the Philippine Nuclear Research Institute (PNRI) on the synthesis and characterization of soft and hard ferrites and some beta alumina type superionic conductor materials. XRD, XRF and Moessbauer effect spectrometry are used to determine the structure phases, compositions and some magnetic properties of the materials. Effects of composition and preparation methods on the bulk electronic and magnetic properties are also discussed. (Auth.). 6 figs.; 3 tabs

  18. Synthesis and characterization of composites of mixed oxides of iron ...

    Indian Academy of Sciences (India)

    Home; Journals; Bulletin of Materials Science; Volume 34; Issue 4. Synthesis and characterization of composites of mixed oxides of iron and neodymium in polymer matrix of aniline–formaldehyde. Sajdha H N Sheikh B L Kalsotra N Kumar S Kumar. Volume 34 Issue 4 July 2011 pp 843-851 ...

  19. Naphthalene-based fluorophores: Synthesis characterization, and photophysical properties

    International Nuclear Information System (INIS)

    Feng Jinwu; Chen Xiaopeng; Han Qingchuan; Wang Hongbo; Lu Ping; Wang Yanguang

    2011-01-01

    U-type, 1,8-diarylnaphthalenes and 1,8-diarylethynylnaphthalenes were synthesized and their structures were characterized by spectroscopic methods. Emission performance of these compounds with donor and acceptor was largely depended upon the solvent polarity and environmental acidity, which implied that they might be used as solvent polarity sensors or pH sensors as well. Moreover, some 1,8-diarylnaphthalenes exhibited aggregation-induced emission enhancement (AIEE) based on their photophysical investigation and might be used as light emitting materials for optoelectronic applications. - Highlights: → 1,8-Diarylnaphthalenes and 1,8-diarylethynylnaphthalenes were synthesized. → Emission of these compounds depended on solvent polarity and environmental acidity. → Some 1,8-diarylnaphthalenes exhibited aggregation-induced emission enhancement.

  20. Colloidal phytosterols: synthesis, characterization and bioaccessibility

    NARCIS (Netherlands)

    Rossi, L.; Seijen ten Hoorn, J.W.M.; Melnikov, S.M.; Velikov, K.P.

    2010-01-01

    We demonstrate the synthesis of phytosterol colloidal particles using a simple food grade method based on antisolvent precipitation in the presence of a non-ionic surfactant. The resulting colloidal particles have a rod-like shape with some degree of crystallinity. The colloidal dispersions display

  1. Synthesis and Characterization Pectin-Carboxymethyl Chitosan crosslinked PEGDE as biosorbent of Pb(II) ion

    Science.gov (United States)

    Hastuti, Budi; Siswanta, Dwi; Mudasir; Triyono

    2018-01-01

    Pectin and chitosan are biodegradable polymers, potentially applied as a heavy metal adsorbents. Unfortunately both biosorbents pectin and chitosan have a weakness in acidic media. For this purpose required modified pectin and chitosan. The modified adsorben is intended to obtain a stable adsorbent and resistance under acid. The research was done by experimental method in laboratory. The stages of this research are the synthesis of carboxymethyl chitosan (CMC), synthesis of Pec-CMC-PEGDE film adsorbent, stabily test under acid, the characterization of active group using FTIR, stability characterization of Pec-CMC-PEGDE powder adsorbent using XRD, termo stability using DTA-TGA. The results of the research have shown that: pectin and CMC can be cross-linked using PEGDE crosslinking agent, the film adsorbent was stable under HCl 1 M, the film adsorbent have active group comprise of carboxylate and amine groups. The result of characterization using XRD, shows that the adsorbent is semi-crystalline. Base on termo stability, the film adsorbent Pec-CMC-PEGDE stable up to 600°C. The film can be applied as an adsobent of Pb (II) ion remediation. The optimum pH of pec-CMC-PEGDE in adsorbed of Pb(II) was reached at pH 5 with 99.99% absorbent adsorbed and of and adsorption capacity was 46.11 mg/g.

  2. Synthesis and characterization of an effective organic/inorganic hybrid green corrosion inhibitive complex based on zinc acetate/Urtica Dioica

    International Nuclear Information System (INIS)

    Salehi, E.; Naderi, Reza; Ramezanzadeh, B.

    2017-01-01

    Highlights: • An organic/inorganic hybrid green corrosion inhibitive pigment was synthesized and characterized. • Chemical structure and morphology of the hybrid complex were characterized. • Zinc acetate/Urtica Dioica showed effective inhibition action in saline solution on carbon steel. • The synergistic effect between Zn 2+ cations and inhibitive compounds existed in U.D resulted in protective film deposition on the steel surface. - Abstract: This study aims at synthesis and characterization of an effective corrosion inhibitive complex based on zinc acetate/Urtica Dioica (ZnA-U.D) for corrosion protection of mild steel in chloride solution. The chemical structure and morphology of the complex were characterized by Fourier transform infrared spectroscopy (FT-IR), UV–vis, thermal gravimetric analysis (TGA), X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM). The corrosion protection performance of the mild steel samples dipped in 3.5 wt.% NaCl solutions with and without ZnA-U.D extract was investigated by visual observations, open circuit potential (OCP) measurements, electrochemical impedance spectroscopy (EIS) and polarization test. Results revealed that the ZnA successfully chelated with organic inhibitive compounds (i.e Quercetin, Quinic acid, Caffeic acid, Hystamine and Serotonin) present in the U.D extract. The electrochemical measurements revealed the effective inhibition action of ZnA-U.D complex in the sodium chloride solution on the mild steel. The synergistic effect between Zn 2+ and organic compounds present in the U.D extract resulted in protective film deposition on the steel surface, which was proved by SEM and XPS analyses.

  3. Synthesis and characterization of an effective organic/inorganic hybrid green corrosion inhibitive complex based on zinc acetate/Urtica Dioica

    Energy Technology Data Exchange (ETDEWEB)

    Salehi, E.; Naderi, Reza [School of Metallurgy and Materials Engineering, College of Engineering, University of Tehran, P.O. Box 11155-4563, Tehran (Iran, Islamic Republic of); Ramezanzadeh, B., E-mail: ramezanzadeh@aut.ac.ir [Department of Surface Coatings and Corrosion, Institute for Color Science and Technology (ICST), PO 16765-654, Tehran (Iran, Islamic Republic of)

    2017-02-28

    Highlights: • An organic/inorganic hybrid green corrosion inhibitive pigment was synthesized and characterized. • Chemical structure and morphology of the hybrid complex were characterized. • Zinc acetate/Urtica Dioica showed effective inhibition action in saline solution on carbon steel. • The synergistic effect between Zn{sup 2+} cations and inhibitive compounds existed in U.D resulted in protective film deposition on the steel surface. - Abstract: This study aims at synthesis and characterization of an effective corrosion inhibitive complex based on zinc acetate/Urtica Dioica (ZnA-U.D) for corrosion protection of mild steel in chloride solution. The chemical structure and morphology of the complex were characterized by Fourier transform infrared spectroscopy (FT-IR), UV–vis, thermal gravimetric analysis (TGA), X-ray photoelectron spectroscopy (XPS) and scanning electron microscopy (SEM). The corrosion protection performance of the mild steel samples dipped in 3.5 wt.% NaCl solutions with and without ZnA-U.D extract was investigated by visual observations, open circuit potential (OCP) measurements, electrochemical impedance spectroscopy (EIS) and polarization test. Results revealed that the ZnA successfully chelated with organic inhibitive compounds (i.e Quercetin, Quinic acid, Caffeic acid, Hystamine and Serotonin) present in the U.D extract. The electrochemical measurements revealed the effective inhibition action of ZnA-U.D complex in the sodium chloride solution on the mild steel. The synergistic effect between Zn{sup 2+} and organic compounds present in the U.D extract resulted in protective film deposition on the steel surface, which was proved by SEM and XPS analyses.

  4. The Synthesis, Characterization and Catalytic Reaction Studies of Monodisperse Platinum Nanoparticles in Mesoporous Oxide Materials

    Energy Technology Data Exchange (ETDEWEB)

    Rioux, Robert M. [Univ. of California, Berkeley, CA (United States)

    2006-01-01

    A catalyst design program was implemented in which Pt nanoparticles, either of monodisperse size and/or shape were synthesized, characterized and studied in a number of hydrocarbon conversion reactions. The novel preparation of these materials enables exquisite control over their physical and chemical properties that could be controlled (and therefore rationally tuned) during synthesis. The ability to synthesize rather than prepare catalysts followed by thorough characterization enable accurate structure-function relationships to be elucidated. This thesis emphasizes all three aspects of catalyst design: synthesis, characterization and reactivity studies. The precise control of metal nanoparticle size, surface structure and composition may enable the development of highly active and selective heterogeneous catalysts.

  5. Synthesis and Characterization of Poly(Amidoamine Dendrimers Encapsulatd 198Au Nanoparticles

    Directory of Open Access Journals (Sweden)

    R. Ritawidya1,2

    2012-12-01

    Full Text Available Brachytherapy or internal radiotherapy is one of many methods used for treatment of cancer. This modality requires an agent with radionuclides that emits  or β particle with a proper energy. 198Au (99% β max = 0.96 MeV and t1/2 = 2.69 days is one of radionuclides that has been considered to be effective for the above-mentioned purpose. The purpose of this research was to synthesis and characterize poly(amidoamine (PAMAM G3.0 dendrimers encapsulated 198Au nanoparticles as a new brachytherapy agent. PAMAM G3.0 dendrimers encapsulated 198Au nanoparticles was successfully synthesized by a bottom-up method using sodium borohydride as a reductor. Purification was then performed by a size exclusion chromatography in order to separate large Au nanoparticles that were formed outside the cavity of PAMAM G3.0 dendrimers. Prior to the synthesis of PAMAM G3.0 dendrimers encapsulated 198Au nanoparticles, the synthetic procedure was first established by using a non-radioactive Au. The PAMAM G3.0 dendrimers encapsulated Au nanoparticles produced was then characterized by using an UV-Vis spectroscopy, a transmission electron microscopy (TEM, particle size analyzer (PSA, and an atomic absorption spectroscopy (AAS. Characterization results revealed that PAMAM G3.0 dendrimers encapsulated Au nanoparticles that were prepared from a reaction mixture of PAMAM G3.0 dendrimers and Au HAuCl4 with mol ratio of 2.8, was found to be a proper formula. It produced PAMAM G3.0 dendrimers encapsulated Au nanoparticles with diameter of 1.743 nm, spheris, uniform and drug loading value of 26.34%. This formula was then used in synthesis using radioactive Au, 198Au. Characterization results of PAMAM G3.0 dendrimers encapsulated 198Au nanoparticles gave a radiochemical purity of 99.4% and zero charge.

  6. Synthesis and characterization of dental composites

    Science.gov (United States)

    Djustiana, Nina; Greviana, Nadia; Faza, Yanwar; Sunarso

    2018-02-01

    During the last few decades, the increasing demands in esthetic dentistry have led to the development of dental composites material that provide similar appearance to the natural teeth. Recently, esthetic trend was an issue which increase the demand for teeth restorations that is similar with the origin. The esthetics of dental composite are more superior compared to amalgam, since its color look similar with natural teeth. Various dental composites have been developed using many type of fillers such as amorphous silica, quartz), borosilicate, Li-Sr-Ba-Al glass and oxide: zirconia and alumina. Researchers in Faculty of Dentistry University of Padjadjaran have prepared dental composites using zirconia-alumina-silica (ZAS) system as the filler. The aim is to improve the mechanical properties and the esthetic of the dental composites. The ZAS was obtained from chemical grade purity chemicals and Indonesia's natural sand as precursors its characterization were also presented. This novel method covers the procedure to synthesis and characterize dental composites in Padjadjaran University and some review about dental composites in global research.

  7. Synthesis, characterization and gas sensing performance of SnO2 ...

    Indian Academy of Sciences (India)

    Synthesis, characterization and gas sensing performance of SnO2 thin films prepared by spray pyrolysis. GANESH E PATIL, D D KAJALE, D N CHAVAN†, N K PAWAR††, P T AHIRE, S D SHINDE#,. V B GAIKWAD# and G H JAIN. ∗. Materials Research Laboratory, Arts, Commerce and Science College, Nandgaon 423 106, ...

  8. Synthesis, characterization, and application of novel biodegradable self-assembled 2-(N-phthalimido) ethyl-palmitate nanoparticles for cancer therapy

    Science.gov (United States)

    Kasoju, Naresh; Bora, Debajeet K.; Bhonde, Ramesh R.; Bora, Utpal

    2010-03-01

    We report the synthesis of novel biodegradable nanoparticles (NPs) which can kill the cancer cells without any additional drug loading. The NP was a self-assembled form of a phthalimide based conjugate, in which the phthalimide moiety was responsible for the anticancer activity. We describe the synthesis of a novel 2-(N-phthalimido) ethyl palmitate (PHEP-Pal) conjugate and subsequent preparation of NPs by a simple self assembly process. The successful synthesis of conjugate was confirmed by various characterization studies including nuclear magnetic resonance spectroscope, Fourier transform infrared spectroscope, TOF-liquid chromatography mass spectroscope, differential scanning calorimetry, and X-ray diffraction unit. The synthesis, shape, size, and size distribution of PHEP-Pal NPs were determined by transmission electron microscope, atomic force microscope, and dynamic light scattering technique. Finally, cell culture studies using A549 and HeLa cells were done to evaluate the anticancer effect of PHEP-Pal NPs, which demonstrated the potency of these NPs for use in cancer chemotherapy.

  9. Materials Research Society Symposium Proceedings Volume 635. Anisotropic Nanoparticles - Synthesis, Characterization and Applications

    National Research Council Canada - National Science Library

    Lyon, L

    2000-01-01

    This volume contains a series of papers originally presented at Symposium C, "Anisotropic Nanoparticles Synthesis, Characterization and Applications," at the 2000 MRS Fall Meeting in Boston, Massachusetts...

  10. Synthesis and Characterization of Stimuli Responsive Block Copolymers, Self-Assembly Behavior and Applications

    Energy Technology Data Exchange (ETDEWEB)

    Determan, Michael Duane [Iowa State Univ., Ames, IA (United States)

    2005-12-17

    The central theme of this thesis work is to develop new block copolymer materials for biomedical applications. While there are many reports of stimuli-responsive amphiphilic [19-21] and crosslinked hydrogel materials [22], the development of an in situ gel forming, pH responsive pentablock copolymer is a novel contribution to the field, Figure 1.1 is a sketch of an ABCBA pentablock copolymer. The A blocks are cationic tertiary amine methacrylates blocked to a central Pluronic F127 triblock copolymer. In addition to the prerequisite synthetic and macromolecular characterization of these new materials, the self-assembled supramolecular structures formed by the pentablock were experimentally evaluated. This synthesis and characterization process serves to elucidate the important structure property relationships of these novel materials, The pH and temperature responsive behavior of the pentablock copolymer were explored especially with consideration towards injectable drug delivery applications. Future synthesis work will focus on enhancing and tuning the cell specific targeting of DNA/pentablock copolymer polyplexes. The specific goals of this research are: (1) Develop a synthetic route for gel forming pentablock block copolymers with pH and temperature sensitive properties. Synthesis of these novel copolymers is accomplished with ATRP, yielding low polydispersity and control of the block copolymer architecture. Well defined macromolecular characteristics are required to tailor the phase behavior of these materials. (2) Characterize relationship between the size and shape of pentablock copolymer micelles and gel structure and the pH and temperature of the copolymer solutions with SAXS, SANS and CryoTEM. (3) Evaluate the temperature and pH induced phase separation and macroscopic self-assembly phenomenon of the pentablock copolymer. (4) Utilize the knowledge gained from first three goals to design and formulate drug delivery formulations based on the multi

  11. Modified Polyacrylic Acid-Zinc Composites: Synthesis, Characterization and Biological Activity

    Directory of Open Access Journals (Sweden)

    Mohammed Rafi Shaik

    2016-02-01

    Full Text Available Polyacrylic acid (PAA is an important industrial chemical, which has been extensively applied in various fields, including for several biomedical purposes. In this study, we report the synthesis and modification of this polymer with various phenol imides, such as succinimide, phthalimide and 1,8-naphthalimide. The as-synthesized derivatives were used to prepare polymer metal composites by the reaction with Zn+2. These composites were characterized by using various techniques, including NMR, FT-IR, TGA, SEM and DSC. The as-prepared PAA-based composites were further evaluated for their anti-microbial properties against various pathogens, which include both Gram-positive and Gram-negative bacteria and different fungal strains. The synthesized composites have displayed considerable biocidal properties, ranging from mild to moderate activities against different strains tested.

  12. Synthesis, characterization and catalytic activity of stable [(NHC)H][ZnXY2] (NHC=N-Heterocyclic carbene, X, Y=Cl, Br) species

    KAUST Repository

    Santoro, Orlando; Nahra, Fady; Cordes, David B.; Slawin, Alexandra M.Z.; Nolan, Steven P.; Cazin, Catherine S. J.

    2016-01-01

    The synthesis and characterization of imidazol(in)ium-based zinc(II) halide salts are reported. These compounds present interesting structural features and exhibit high stability. Their catalytic activity was explored in the methylation of amines with CO2 and PhSiH3.

  13. Synthesis, characterization and catalytic activity of stable [(NHC)H][ZnXY2] (NHC=N-Heterocyclic carbene, X, Y=Cl, Br) species

    KAUST Repository

    Santoro, Orlando

    2016-06-04

    The synthesis and characterization of imidazol(in)ium-based zinc(II) halide salts are reported. These compounds present interesting structural features and exhibit high stability. Their catalytic activity was explored in the methylation of amines with CO2 and PhSiH3.

  14. Nano-/micro metallic wire synthesis on Si substrate and their characterization

    International Nuclear Information System (INIS)

    Kaur, Jaskiran; Kaur, Harmanmeet; Singh, Surinder; Kanjilal, Dinakar; Chakarvarti, Shiv Kumar

    2014-01-01

    Nano-/micro wires of copper are grown on semiconducting Si substrate using the template method. It involves the irradiation of 8 um thick polymeric layer coated on Si with150 MeV Ni ion beam at a fluence of 2E8. Later, by using the simple technique of electrodeposition, copper nano-/micro wires were grown via template synthesis. Synthesized wires were morphologically characterized using SEM and electrical characterization was carried out by finding I-V plot

  15. Design, synthesis, and characterization of fluorine-free PAGs for 193-nm lithography

    Science.gov (United States)

    Liu, Sen; Glodde, Martin; Varanasi, Pushkara R.

    2010-04-01

    Photoacid generators (PAGs) are a key component in chemically amplified resists used in photolithography. Perfluorooctanesulfonates (PFOS) and other perfluoroalkylsulfonates (PFAS) have been well adopted as PAGs in 193 nm photoresist. Recently, concerns have been raised about their environmental impact due to their chemical persistency, bioaccumulation and toxicity. It is a general interest to find environmentally benign PAGs that are free of fluorine atoms. Here we describe the design, synthesis and characterization of a series of novel fluorine-free onium salts as PAGs for 193 nm photoresists. These PAGs demonstrated desirable physical and lithography properties when compared with PFAS-based PAGs for both dry and immersion exposures.

  16. Synthesis and characterization of novel curing agents for surface coatings based on acrylamide copolymers

    International Nuclear Information System (INIS)

    Patel, N. V.; Parmar, R. J.; Parmar, J. S.

    2003-01-01

    The acrylamide based curing agents were prepared form methyl methacrylate-acrylamide copolymers by further methylolation and subsequent etherification with butanol. These were characterized for their various physico-chemical characteristics. Various sets of these ACAs were blended with hydroxyl functional acrylic resin to prepare the staving compared with the conventional melamine-formaldehyde based curing agent containing compositions. The films were also characterized thermogravimetric analysis and IR-spectra. The result reveals that the properties of certain compositions based on ACAs were remarkably better than those of conventional melamine-formaldehyde based curing agent based coatings

  17. Synthesis and characterization of poly aniline for electrochemical biosensor construction

    International Nuclear Information System (INIS)

    Magalhaes, Gleice S.L.; Southgate, Erica F.; Alhadeff, Eliana M.; Guimaraes, Maria Jose O.C.

    2011-01-01

    Conductors polymers have many attractive interests to the industry due their highly technological applications. This work treats specially of polyaniline because it's large electrical conductivity, electrochemical properties, associate to the chemical stability in environmental conditions and synthesis facility. The main of this work is the application in a construction of an electrochemical biosensor for ethanol detection and quantification. Different conditions of synthesis of the conductor emeraldine polyaniline form were studied, investigated the influence of the dopant agent and the reactional environment conditions temperature on the reaction yield and conductivities. The polyaniline that showed the best conductivity were characterized by differential and thermal gravimetric analysis, infrared spectroscopy, X ray diffraction, and cycle voltammetry, comparing with the commercial polyaniline. (author)

  18. Synthesis and characterization of Au incorporated Alq3 nanowires

    Science.gov (United States)

    Khan, Mohammad Bilal; Ahmad, Sultan; Parwaz, M.; Rahul, Khan, Zishan H.

    2018-05-01

    We report the synthesis and characterization of pure and Au incorporated Alq3 nanowires. These nanowires are synthesized using thermal vapor transport method. The luminescence intensity of Au incorporated Alq3 nanowires are recorded to be higher than that of pure Alq3 nanowires, which is found to increase with the increase in Au concentration. Fluorescence quenching is also observed when Au concentration is increased beyond the certain limit.

  19. Synthesis and Characterization of Highly Intercalated Graphite Bisulfate

    Science.gov (United States)

    Salvatore, Marcella; Carotenuto, Gianfranco; De Nicola, Sergio; Camerlingo, Carlo; Ambrogi, Veronica; Carfagna, Cosimo

    2017-03-01

    Different chemical formulations for the synthesis of highly intercalated graphite bisulfate have been tested. In particular, nitric acid, potassium nitrate, potassium dichromate, potassium permanganate, sodium periodate, sodium chlorate, and hydrogen peroxide have been used in this synthesis scheme as the auxiliary reagent (oxidizing agent). In order to evaluate the presence of delamination, and pre-expansion phenomena, and the achieved intercalation degree in the prepared samples, the obtained graphite intercalation compounds have been characterized by scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDS), X-ray powder diffraction (XRD), infrared spectroscopy (FT-IR), micro-Raman spectroscopy ( μ-RS), and thermal analysis (TGA). Delamination and pre-expansion phenomena were observed only for nitric acid, sodium chlorate, and hydrogen peroxide, while the presence of strong oxidizers (KMnO4, K2Cr2O7) led to stable graphite intercalation compounds. The largest content of intercalated bisulfate is achieved in the intercalated compounds obtained from NaIO4 and NaClO3.

  20. Synthesis and Characterization of Lanthanum Complexes with Amino Acid Schiff Base

    Institute of Scientific and Technical Information of China (English)

    张秀英; 张有娟; 杨林

    2001-01-01

    Six new complexes of lanthanum with amino acid Schiff base ligands, A-F, were prepared in methanol-aqueous solution. The composition and properties of the title complexes were characterized by elemental analysis, molar conductance, infrared, electronic spectra, 1H NMR, thermogravimetric and differential thermal analysis.

  1. Synthesis, characterization and antioxidant activities of Schiff bases are of cholesterol

    OpenAIRE

    Madasamy Kumar; Tamilenthi Padmini; Kandasamy Ponnuvel

    2017-01-01

    A series of new cholesterol based Schiff base derivatives, namely cholesteryl-n-(4-((E)-(4′-cyanobiphenyl-4-ylimino)methyl)phenoxy)alkanoate (3a–j) have been synthesized and characterized by IR, NMR and mass spectral studies. In vitro antioxidant activities of these compounds were evaluated against super oxide anion radical, nitric oxide radical, DPPH radical and hydrogen peroxide and were compared with standard natural antioxidant, ascorbic acid. Our results reveal that these compounds exhib...

  2. Green synthesis and characterization of graphene nanosheets

    Energy Technology Data Exchange (ETDEWEB)

    Tavakoli, Farnosh [School of Chemistry, College of Science, University of Tehran, Tehran (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); Department of Inorganic Chemistry, Faculty of Chemistry, University of Kashan, Kashan, P. O. Box. 87317-51167, Islamic Republic of Iran (Iran, Islamic Republic of); Badiei, Alireza [School of Chemistry, College of Science, University of Tehran, Tehran (Iran, Islamic Republic of); Mohandes, Fatemeh [Department of Inorganic Chemistry, Faculty of Chemistry, University of Kashan, Kashan, P. O. Box. 87317-51167, Islamic Republic of Iran (Iran, Islamic Republic of)

    2015-03-15

    Highlights: • For the first time, we have synthesized graphene nanosheets in the presence of pomegranate juice. • Here pomegranate juice was used not only as reductant but also as capping agent. • FT-IR, XRD, SEM, EDS and TEM were used to characterize the samples. • According to TEM image, graphene nanosheet is individually exfoliated after stirring for 24 h. • As shown in the TEM image, graphene monolayer is obtained. - Abstract: For the first time, we have successfully synthesized graphene nanosheets in the presence of pomegranate juice. In this approach, pomegranate juice was used not only as reductant but also as capping agent to form graphene nanosheets. At first, the improved Hummer method to oxidize graphite for the synthesis of graphene oxide (GO) was applied, and then the as-produced graphene oxide was reduced by pomegranate juice to form graphene nanosheets. Fourier transformed infrared (FT-IR), X-ray powder diffraction (XRD), scanning electron microscopy (SEM), energy dispersive spectrometry (EDS), high resolution transmission electron microscopy (HRTEM), atomic force microscopy (AFM) and raman were used to characterize the samples. The results obtained from the characterization techniques proved high purity of the final products.

  3. Green synthesis and characterization of graphene nanosheets

    International Nuclear Information System (INIS)

    Tavakoli, Farnosh; Salavati-Niasari, Masoud; Badiei, Alireza; Mohandes, Fatemeh

    2015-01-01

    Highlights: • For the first time, we have synthesized graphene nanosheets in the presence of pomegranate juice. • Here pomegranate juice was used not only as reductant but also as capping agent. • FT-IR, XRD, SEM, EDS and TEM were used to characterize the samples. • According to TEM image, graphene nanosheet is individually exfoliated after stirring for 24 h. • As shown in the TEM image, graphene monolayer is obtained. - Abstract: For the first time, we have successfully synthesized graphene nanosheets in the presence of pomegranate juice. In this approach, pomegranate juice was used not only as reductant but also as capping agent to form graphene nanosheets. At first, the improved Hummer method to oxidize graphite for the synthesis of graphene oxide (GO) was applied, and then the as-produced graphene oxide was reduced by pomegranate juice to form graphene nanosheets. Fourier transformed infrared (FT-IR), X-ray powder diffraction (XRD), scanning electron microscopy (SEM), energy dispersive spectrometry (EDS), high resolution transmission electron microscopy (HRTEM), atomic force microscopy (AFM) and raman were used to characterize the samples. The results obtained from the characterization techniques proved high purity of the final products

  4. A short designed semi-aromatic organic nanotube – synthesis, chiroptical characterization, and host properties

    DEFF Research Database (Denmark)

    Wixe, Torbjörn; Christensen, Niels Johan; Lidin, Sven

    2014-01-01

    to molecular dynamics simulations in chloroform). The synthesis of the tube, a heptamer, is based on a series of Friedländer condensations and the use of pyrido[3,2-d]pyrimidine units as masked 2-amino aldehydes, as a general means to propagate organic tubular structures and the introduction of a methoxy group...... for modification toward solubility and functionalization are described. The electronic CD spectra of the tube and molecular intermediates are correlated with theoretical spectra calculated with time-dependent density functional theory to characterize the chirality of the tube. Both experimental (NMR...

  5. Phosphates based pigments for new anti-corrosion application: Synthesis and characterization

    Science.gov (United States)

    Tbib, B.; Eddya, M.; El-Hami, K.

    2018-02-01

    Our study focused on pyrophosphates SrZn1-xMxP2O7 using four series by substituting M with manganese (Mn), cobalt (Co), nickel (Ni), and copper (Cu). They were prepared by reaction in the solid state at 1000 °C for 24 hours and then characterized by X-ray diffraction, which showed that the obtained products are pure. The characterization by UV-visible spectroscopy was used to explain the color of the obtained materials and the optical properties showing the optical energy gap and disorder of these materials. Potential application could be done using the new anti-corrosion pigments based on phosphates.

  6. Synthesis, characterization and antioxidant activities of Schiff bases are of cholesterol

    Directory of Open Access Journals (Sweden)

    Madasamy Kumar

    2017-01-01

    Full Text Available A series of new cholesterol based Schiff base derivatives, namely cholesteryl-n-(4-((E-(4′-cyanobiphenyl-4-yliminomethylphenoxyalkanoate (3a–j have been synthesized and characterized by IR, NMR and mass spectral studies. In vitro antioxidant activities of these compounds were evaluated against super oxide anion radical, nitric oxide radical, DPPH radical and hydrogen peroxide and were compared with standard natural antioxidant, ascorbic acid. Our results reveal that these compounds exhibit excellent radical scavenging activities.

  7. Synthesis, characterization and electrochemical properties of 4.8 V LiNi{sub 0.5}Mn{sub 1.5}O{sub 4} cathode material in lithium-ion batteries

    Energy Technology Data Exchange (ETDEWEB)

    Chi, Le Ha [Faculty of Engineering Physics and NanoTechnology, College of Technology, 144 Xuan Thuy Road, Hanoi (Viet Nam)] [Vietnamese Academy of Science and Technology, 18 Hoang Quoc Viet Street, Cau Giay District, Hanoi (Viet Nam); Dinh, Nguyen Nang [Faculty of Engineering Physics and NanoTechnology, College of Technology, 144 Xuan Thuy Road, Hanoi (Viet Nam); Brutti, Sergio, E-mail: sergio.brutti@uniroma1.i [Department of Chemistry, University of Rome ' La Sapienza' , P.le Aldo Moro 5, 00185 Rome (Italy); Scrosati, Bruno [Department of Chemistry, University of Rome ' La Sapienza' , P.le Aldo Moro 5, 00185 Rome (Italy)

    2010-07-15

    In this work the synthesis of a nickel doped cubic manganese spinel has been studied for application as cathode material in secondary lithium batteries. Six different experimental approaches have been tested in order to carry out a screening of the various possible synthetic routes. The used synthetic strategies were wet chemistry (WC), solid state (SS), combustion synthesis (CS), cellulose-based sol-gel synthesis (SG-C), ascorbic acid-based sol-gel synthesis (SG-AA) and resorcinol/formaldehyde-based sol-gel synthesis (SG-RF). The goal of our study is to obtain insights about how the synthesis conditions can be modified in order to achieve a material with improved electrochemical performances in such devices, especially in high current operating regimes. The synthesized materials have been characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) with energy dispersive spectroscopy (EDS), atomic absorption, inductively coupled plasma (ICP-MS) atomic emission spectroscopy, surface area measurements and tested as high voltage cathodes in Li-ion electrochemical devices.

  8. Synthesis and dosimetric characterization of LiF-MgF2, doped with Lu

    International Nuclear Information System (INIS)

    Gonzalez, Pedro R.; Nieto, Ana L.; Cruz-Zaragoza, Epifanio; Furetta, Claudio

    2013-01-01

    The results of the synthesis and characterization of dosimetric thermoluminescent material based on the composition LiF-MgF 2 1:1 (Z eff = 9.7) doped Lu 3+ ions, developed at the National Institute of Nuclear Research, Mexico are presented. The TL material synthesis was carried out using the technique of casting solid substances, preparations were made with dopant concentrations of 0.25, 0.83, 1.00 and 2.00 mol%, the 1 mol% resulted in increased sensitivity to radiation. Its brightness curve has the TL peak intensity at 330 deg C when irradiated to 1000 Gy, whereas when irradiated greater than 2500 Gy, occurs at 230 ° C, also has a peak of smaller maximum intensity at 140 ° C. Microstructural characterization of the obtained material was performed using the techniques of scanning electron microscopy and X-ray diffraction Kinetic parameters of the curves of brightness of the material is performed by the deconvolution method using the sequential quadratic programming algorithm, developed in the same institute. This new TL material complies fully with international standards to be used as dosimetry system in medical physics, research and industry, as its TL response (total integrated under the curve) to 60 Co gamma radiation, presents linearity between 1 and 5000 Gy , while the response of commercial TLD dosimeter-100 used as a reference, is only linear up to 10 Gy

  9. Electrospun V2O5 composite fibers: Synthesis, characterization and ammonia sensing properties

    International Nuclear Information System (INIS)

    Modafferi, V.; Trocino, S.; Donato, A.; Panzera, G.; Neri, G.

    2013-01-01

    In the present work, vanadium oxide (V 2 O 5 ) fibers have been investigated for monitoring ammonia (NH 3 ) at ppb levels in air. A simple sol gel-based electrospinning process has been applied for the synthesis of vanadium oxide/polyvinyl acetate (PVAc) and vanadium oxide/polyvinylpyrrolidone (PVP) composite fibers. Composite fibers doped with platinum (Pt) have been also prepared. The pure and Pt-doped metal oxide phase has been subsequently obtained by removing the polymer binder at high temperature in air. The samples have been widely studied to characterize their morphological and microstructural properties by X-Ray Diffraction, Fourier Transform InfraRed spectroscopy, X-ray Photoelectron Spectroscopy, and Scanning Electron Microscopy investigations. The application of the produced fibers in highly sensitive ammonia resistive sensors has been demonstrated. The influence of the nature of polymer binder and platinum addition on the sensing performances of the V 2 O 5 fibers has been investigated and discussed.V 2 O 5 fibers produced by using PVP as a polymer binder have shown higher sensitivity toward ammonia at ppb concentrations than fibers obtained with PVAc. Pt-doped samples have shown a lower response compared to un-doped samples. - Highlights: • Synthesis of vanadium oxide composite fibers by electrospinning • Physical and chemical characterization of prepared samples • Investigation of the sensing properties to ppb concentrations of ammonia in air

  10. Nanostructured carbon-supported Pd electrocatalysts for ethanol oxidation: synthesis and characterization

    Science.gov (United States)

    Gacutan, E. M.; Climaco, M. I.; Telan, G. J.; Malijan, F.; Hsu, H. Y.; Garcia, J.; Fulo, H.; Tongol, B. J.

    2012-12-01

    The need to lower the construction cost of fuel cells calls for the development of non-Pt based electrocatalysts. Among others, Pd has emerged as a promising alternative to Pt for fuel cell catalysis. This research aims to investigate the synthesis and characterization of nanostructured Pd-based catalysts dispersed on carbon support as anode materials in direct ethanol fuel cells. For the preparation of the first Pd-based electrocatalyst, palladium nanoparticles (NPs) were synthesized via oleylamine (OAm)-mediated synthesis and precursor method with a mean particle size of 3.63 ± 0.59 nm as revealed by transmission electron microscopy (TEM). Carbon black was used as a supporting matrix for the OAm-capped Pd NPs. Thermal annealing and acetic acid washing were used to remove the OAm capping agent. To evaluate the electrocatalytic activity of the prepared electrocatalyst towards ethanol oxidation, cyclic voltammetry (CV) studies were performed using 1.0 M ethanol in basic medium. The CV data revealed the highest peak current density of 11.05 mA cm-2 for the acetic acid-washed Pd/C electrocatalyst. Meanwhile, the fabrication of the second Pd-based electrocatalyst was done by functionalization of the carbon black support using 3:1 (v/v) H2SO4:HNO3. The metal oxide, NiO, was deposited using precipitation method while polyol method was used for the deposition of Pd NPs. X-ray diffraction (XRD) analysis revealed that the estimated particle size of the synthesized catalysts was at around 9.0-15.0 nm. CV results demonstrated a 36.7% increase in the catalytic activity of Pd-NiO/C (functionalized) catalyst towards ethanol oxidation compared to the non-functionalized catalyst.

  11. Multifunctional material based on ionic transition metal complexes and gold-silica nanoparticles: synthesis and photophysical characterization for application in imaging and therapy.

    Science.gov (United States)

    Ricciardi, Loredana; Martini, Matteo; Tillement, Olivier; Sancey, Lucie; Perriat, Pascal; Ghedini, Mauro; Szerb, Elisabeta I; Yadav, Yogesh J; La Deda, Massimo

    2014-11-01

    A new combination of luminescent ionic transition-metal complexes (M = Ru(II) or Ir(III)) with gold silica-based nanoparticles (GSNPs) gives a promising nanomaterial for application in biomedical fields. Herein we report the synthesis and the photophysical properties of Ru(II) and Ir(III) complexes doped gold core-polysiloxane shell particles prepared by microemulsion method and characterized by Transmission Electron Microscopy, Dynamic Light Scattering and UV-Vis spectroscopy. The cytotoxicity and photodynamic activity of the obtained 50 nm-diameter nanoparticles were evaluated in vitro, providing noteworthy results. Furthermore, their intrinsic phosphorescence allows the localization of the photosensitizing nanoparticles into the cytosol of tumor cells by fluorescence confocal microscope. These valuable features designate them as multifunctional nanoplatforms for theranostic purposes.

  12. Synthesis and Characterization of a Novel Ammonia Gas Sensor Based on PANI-PVA Blend Thin Films

    Directory of Open Access Journals (Sweden)

    D. B. DUPARE

    2008-06-01

    Full Text Available The polyaniline - polyvinyl alcohol blend films were synthesized by oxidative polymerization using chemical synthesis route. The polyaniline films were synthesized using optimized concentration of monomer aniline, hydrochloric acid as a dopant using ammonium peroxy-disulphate as a oxidant and insulating addative matrix polyvinyl alcohol on glass substrate for development of ammonia sensor. The formation of PANI- PVA blend films show good uniform surface morphology at 10ºc temperature, maintained at constant temperature bath. The synthesized PANI-PVA blend thin films were characterized by analyzing UV-Visible and FTIR spectra. The SEM study ensures that the thin films are uniform and porous in nature. The I-V characterization shows ohmic behaviour and also determines conductivity of the films. The response time of PANI-PVA blend thin films show that excellent behavior for 50-800 ppm and higher range of ammonia gas. This study reveals that PANI-PVA blend thin films provide a polymer matrix with very good mechanical strength, environmental stability, uniformity in surface, porous morphology and high conductivity, which are suitable for ammonia gas sensing.

  13. Synthesis and characterization of the monomer 2,2'-dialylbisphenol-A (ABFA) for production of proton exchange membranes based on sulphonated poly(arylene ether sulphone)s reticulated

    International Nuclear Information System (INIS)

    Souza, Julio C.; Souza, Carlos H.F.B.; Silva, Maria Elisa S.R.; Sousa, Ricardo G.; Freitas, Roberto F.S.; Silva, Claudio Homero F.

    2011-01-01

    In the present work, a methodology of synthesis and characterization of the monomer 2,2'- dialylbisphenol A was developed, aiming at getting a precursor, with adequate purity, for obtaining cross-linked membranes based on sulfonated poly(arylene ether sulfone)s. The monomer 2,2'- dialylbisphenol A was obtained through Claisen rearrangement of the 2,2-Bis(4-alyloxiphenyl)propane, synthesized from Bisphenol A. All the products and reagents were characterized by Fourier Transform infrared spectroscopy, Thermo-gravimetric analysis and High-performance liquid chromatography. The thermal Claisen rearrangement process was conducted by using Differential Scanning Calorimetry technique, from a factorial experiment planning, with temperature and time being the variables. The above cited techniques were used for monitoring the Claisen rearrangement and for the characterization of the final product. The best results yield an ABFA purity between 85 and 90%. The obtained results suggest that, in the studied range, polymerization and degradation of the monomer ABFA occur, simultaneously to its formation. (author)

  14. Synthesis, purification and characterization of [3,5 - T] p-aminobenzoic acid

    International Nuclear Information System (INIS)

    Corol-Cucu, Delia-Irina; Chiper, Diana; Mihaila, V.; Negoita, N.

    2000-01-01

    This paper refers to the synthesis, purification and characterization of [3,5-T] p-aminobenzoic acid (PAB,H' vitamine). The p-aminobenzoic acid is used in the treatment of rheumatic arthritis and dermatological affections. The advantage of tritium labelling of p-aminobenzoic acid is that some biomedical important aspects of collagen's behaviour are made clear. The PAB stimulate the grow of intestinal bacteria so necessary to synthesis of some vitamins (bio tine, pantothenic acid). Tritium is the only radioactive isotope of hydrogen. Several steps have to be carried out in the synthesis of the final product as well as to study its biological behavior. For the labelling of PAB one prefers the substitution of bromine from PAB-3,5-Br with tritium because of simplicity of reaction and the easy synthesis of halogen compound. The first step in synthesis is the protection of NH 2 group through acetylation of PAB. After that PAB is bromated into the 3 and 5 position with elementary bromine. The raw compound is purified and recrystallized and characterized through thin layer chromatography.The tritium labelling is performed through substitution of bromine from bromate derivative, using Pd/C (10% Pd) as catalyst and low basic conditions for the neutralization of HBr resulting from reaction. After the separation of PAB-3,5-T through filtration, the catalyst remains on the filter paper and the labelled compound goes in aqueous solution. PAB-3,5-T is purified through thin layer chromatography with the solvent system n-BuOH:NH 4 OH(25%):H 2 O:EtOH (8:1:2:2,5, v/v) with silica gel GF 254 as support. The determination of activity is carried out with LSC (Liquid Scintillation Counter). A 98% purity was determined through TLC in the same conditions while determination of activity distribution was performed with a 2π Berthold scanner with gas running and without window. The chemical concentration has been measured through UV spectrophotometry and by comparing extinction with

  15. Sol – Gel synthesis and characterization of magnesium peroxide nanoparticles

    International Nuclear Information System (INIS)

    Jaison, J; Chan, Y S; Ashok raja, C; Balakumar, S

    2015-01-01

    Magnesium peroxide is an excellent source of oxygen in agriculture applications, for instance it is used in waste management as a material for soil bioremediation to remove contaminants from polluted underground water, biological wastes treatment to break down hydrocarbon, etc. In the present study, sol-gel synthesis of magnesium peroxide (MgO 2 ) nanoparticles is reported. Magnesium peroxide is odourless; fine peroxide which releases oxygen when reacts with water. During the sol-gel synthesis, the magnesium malonate intermediate is formed which was then calcinated to obtain MgO 2 nanoparticles. The synthesized nanoparticles were characterized using Thermo gravimetric -Differential Thermal Analysis (TG- DTA), X-Ray Diffraction studies (XRD) and High Resolution Transmission Electron Microscope (HRTEM). Our study provides a clear insight that the formation of magnesium malonate during the synthesis was due to the reaction between magnesium acetate, oxalic acid and ethanol. In our study, we can conclude that the calcination temperature has a strong influence on particle size, morphology, monodispersity and the chemistry of the particles. (paper)

  16. Synthesis and characterization of 4-[(E)-(-2,5 ...

    African Journals Online (AJOL)

    The synthesis of 4-[(E)-(-2,5- dimethoxybenzylidene)amino] benzoic acid. Schiff base, SBDAB was carried out inorder to determine its inhibitory efficiency at higher temperature using weight loss and gasometric techniques. The results showed that the inhibition efficiency of the studied Schiff base increased with increase in ...

  17. Synthesis and characterization of bulk Cu2ZnSnX4 (X: S, Se) via thermodynamically supported mechano-chemical process

    International Nuclear Information System (INIS)

    Pareek, Devendra; Balasubramaniam, K.R.; Sharma, Pratibha

    2015-01-01

    Materials with the general formula, Cu 2 ZnSnX 4 (CZTX; X: Group 16 elements), with X being S/Se, have been receiving considerable attention due to their utility as an absorber layer in solar photovoltaics (PV). This paper reports on the synthesis of CZTSe and CZTS nanocrystalline powders at low temperatures, starting from elemental metal and chalcogen powders, via the low cost, scalable technique of ball milling. The prepared samples were well characterized using the different characterization tools. XRD, Raman, SEM and TEM studies confirm the formation of single-phase, stoichiometric, nano-crystalline kesterite CZTS and CZTSe powders. The low temperature phase selection of the complex quaternary compound in this system is seen as a direct consequence of the thermodynamic facilitation, coupled with the capability of mechano-chemical synthesis to aid in overcoming kinetic constraints. The optical bandgap of the various samples of CZTS was observed in the range of 1.4–1.6 eV and corresponding values for CZTSe was observed to be in the range of 1.08–1.18 eV. Our work provides a pathway for developing cheap, scalable, and ink-based techniques for low cost solar PV. - Graphical abstract: Display Omitted - Highlights: • A scalable route for synthesis of near phase pure CZTS/Se nano-crystals has been demonstrated. • Stoichiometric CZTS and CZTSe were synthesized via mechano-chemical synthesis route. • Synthesis at near room temperature is supported by thermodynamic calculations

  18. Synthesis and characterization of novel silver nanoparticles using Chamaemelum nobile extract for antibacterial application

    Science.gov (United States)

    Erjaee, Hoda; Rajaian, Hamid; Nazifi, Saeed

    2017-06-01

    The present study reports green synthesis of silver nanoparticles (AgNPs) at room temperature using aqueous Chamaemelum nobile extract for the first time. The effect of silver nitrate concentration, quantity of the plant extract and the reaction time on particle size was optimized and studied by UV-Vis spectroscopy and dynamic light scattering. The appearance of brownish color with λ max of 422 nm confirmed the formation of AgNPs. Synthesized nanoparticles were further characterized by Fourier transform infrared spectroscopy, x-ray diffraction and transmission electron microscopy. In addition, antimicrobial activity of the AgNPs against Escherichia coli, Salmonella typhimurium, Staphylococcus aureus and Bacillus subtilis was evaluated based on the inhibition zone using the disc-diffusion assay and measurement of minimal inhibition concentration and minimal bactericidal concentration by standard microdilution method. In conclusion, synthesis of nanoparticle with aqueous Chamaemelum nobile extract is simple, rapid, environmentally benign and inexpensive. Moreover, these synthesized nanoparticles exhibit significant antibacterial activity.

  19. Synthesis and Characterization of Block Copolymers with Unique Chemical Functionalities and Entropically-Hindering Moieties

    Science.gov (United States)

    2017-08-14

    methanol as a function of chemistry , morphology and hydration levels. Accomplishments: This section is included in the "upload" section. Training...Copolymer Blend Membranes.” In Press, Polymer Engineering and Science, DOI: 10.1002 /pen.24508, 2017. 5. M. Pérez-Pérez and D. Suleiman. “Synthesis and...Synthesis and Characterization of Sulfonated Amine Block Copolymers for Energy Efficient Applications". Chemical Engineering Symposium, University of

  20. Quaternized Carboxymethyl Chitosan-Based Silver Nanoparticles Hybrid: Microwave-Assisted Synthesis, Characterization and Antibacterial Activity

    Directory of Open Access Journals (Sweden)

    Siqi Huang

    2016-06-01

    Full Text Available A facile, efficient, and eco-friendly approach for the preparation of uniform silver nanoparticles (Ag NPs was developed. The synthesis was conducted in an aqueous medium exposed to microwave irradiation for 8 min, using laboratory-prepared, water-soluble quaternized carboxymethyl chitosan (QCMC as a chemical reducer and stabilizer and silver nitrate as the silver source. The structure of the prepared QCMC was characterized using Fourier transform infrared (FT-IR and 1H nuclear magnetic resonance (NMR. The formation, size distribution, and dispersion of the Ag NPs in the QCMC matrix were determined using X-ray diffraction (XRD, X-ray photoelectron spectroscopy (XPS, ultraviolet-visible (UV-Vis, transmission electron microscopy (TEM, and field emission scanning electron microscope (FESEM analysis, and the thermal stability and antibacterial properties of the synthesized QCMC-based Ag NPs composite (QCMC-Ag were also explored. The results revealed that (1 QCMC was successfully prepared by grafting quaternary ammonium groups onto carboxymethyl chitosan (CMC chains under microwave irradiation in water for 90 min and this substitution appeared to have occurred at -NH2 sites on C2 position of the pyranoid ring; (2 uniform and stable spherical Ag NPs could be synthesized when QCMC was used as the reducing and stabilizing agent; (3 Ag NPs were well dispersed in the QCMC matrix with a narrow size distribiution in the range of 17–31 nm without aggregation; and (4 due to the presence of Ag NPs, the thermal stability and antibacterial activity of QCMC-Ag were dramatically improved relative to QCMC.

  1. Quaternized Carboxymethyl Chitosan-Based Silver Nanoparticles Hybrid: Microwave-Assisted Synthesis, Characterization and Antibacterial Activity.

    Science.gov (United States)

    Huang, Siqi; Wang, Jing; Zhang, Yang; Yu, Zhiming; Qi, Chusheng

    2016-06-17

    A facile, efficient, and eco-friendly approach for the preparation of uniform silver nanoparticles (Ag NPs) was developed. The synthesis was conducted in an aqueous medium exposed to microwave irradiation for 8 min, using laboratory-prepared, water-soluble quaternized carboxymethyl chitosan (QCMC) as a chemical reducer and stabilizer and silver nitrate as the silver source. The structure of the prepared QCMC was characterized using Fourier transform infrared (FT-IR) and ¹H nuclear magnetic resonance (NMR). The formation, size distribution, and dispersion of the Ag NPs in the QCMC matrix were determined using X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), ultraviolet-visible (UV-Vis), transmission electron microscopy (TEM), and field emission scanning electron microscope (FESEM) analysis, and the thermal stability and antibacterial properties of the synthesized QCMC-based Ag NPs composite (QCMC-Ag) were also explored. The results revealed that (1) QCMC was successfully prepared by grafting quaternary ammonium groups onto carboxymethyl chitosan (CMC) chains under microwave irradiation in water for 90 min and this substitution appeared to have occurred at -NH₂ sites on C2 position of the pyranoid ring; (2) uniform and stable spherical Ag NPs could be synthesized when QCMC was used as the reducing and stabilizing agent; (3) Ag NPs were well dispersed in the QCMC matrix with a narrow size distribiution in the range of 17-31 nm without aggregation; and (4) due to the presence of Ag NPs, the thermal stability and antibacterial activity of QCMC-Ag were dramatically improved relative to QCMC.

  2. Synthesis and characterization of tantalum organometallic complexes. Catalytic activity for olefins

    International Nuclear Information System (INIS)

    Baley, A.S.

    1990-11-01

    Synthesis of monoaryloxy (alcoxy) neopentyl compounds is investigated. The tantalum-oxygen bond is formed by two parallel ways from TaCl 5 or TaR 2 Cl 3 with R = neopentyl and the tantalum carbon bond from a neopentyl derivative of the main series. Some compounds were isolated and characterized by NMR, elemental analysis and sometimes X-ray structure, some others are characterized in solution only. Catalytic effect is tested by ethylene dimerization and olefin polymerization. Reactivity of tantalum aryloxy neopentyl in respect to complexing and chelating ligands is studied for preparation of neopentylidene complexes

  3. Synthesis and Application of Graphene Based Nanomaterials

    Science.gov (United States)

    Peng, Zhiwei

    Graphene, a two-dimensional sp2-bonded carbon material, has recently attracted major attention due to its excellent electrical, optical and mechanical properties. Depending on different applications, graphene and its derived hybrid nanomaterials can be synthesized by either bottom-up chemical vapor deposition (CVD) methods for electronics, or various top-down chemical reaction methods for energy generation and storage devices. My thesis begins with the investigation of CVD synthesis of graphene thin films in Chapter 1, including the direct growth of bilayer graphene on insulating substrates and synthesis of "rebar graphene": a hybrid structure with graphene and carbon or boron nitride nanotubes. Chapter 2 discusses the synthesis of nanoribbon-shaped materials and their applications, including splitting of vertically aligned multi-walled carbon nanotube carpets for supercapacitors, synthesis of dispersable ferromagnetic graphene nanoribbon stacks with enhanced electrical percolation properties in magnetic field, graphene nanoribbon/SnO 2 nanocomposite for lithium ion batteries, and enhanced electrocatalysis for hydrogen evolution reactions from WS2 nanoribbons. Next, Chapter 3 discusses graphene coated iron oxide nanomaterials and their use in energy storage applications. Finally, Chapter 4 introduces the development, characterization, and fabrication of laser induced graphene and its application as supercapacitors.

  4. Synthesis and characterization of binder-free Cr3C2 coatings on nickel-based alloys for molten fluoride salt corrosion resistance

    International Nuclear Information System (INIS)

    Brupbacher, Michael C.; Zhang, Dajie; Buchta, William M.; Graybeal, Mark L.; Rhim, Yo-Rhin; Nagle, Dennis C.; Spicer, James B.

    2015-01-01

    Under various conditions, chromium carbides appear to be relatively stable in the presence of molten fluoride salts and this suggests that their use in corrosion resistant coatings for fluoride salt environments could be beneficial. One method for producing these coatings is the carburization of sprayed Cr coatings using methane-containing gaseous precursors. This process has been investigated for the synthesis of binder-free chromium carbide coatings on nickel-based alloy substrates for molten fluoride salt corrosion resistance. The effects of the carburization process on coating microstructure have been characterized using X-ray diffraction (XRD) and scanning electron microscopy (SEM) in conjunction with energy dispersive spectroscopy (EDS). Both plasma-sprayed and cold-sprayed Cr coatings have been successfully converted to Cr 3 C 2 , with the mechanism of conversion being strongly influenced by the initial porosity in the as-deposited coatings

  5. Novel metallomesogenic polyurethanes: Synthesis, characterization and properties

    International Nuclear Information System (INIS)

    Senthilkumar, Natarajan; Narasimhaswamy, Tanneru; Kim, Il-Jin

    2012-01-01

    A series of tetradentate Schiff base metallomesogenic diols were synthesized from two simple dihydroxy benzenes. The metallomesogenic diol was constructed from three ring containing mesogen linked through ester and azomethine with terminal hydroxy group. This upon complexation with copper(II) formed metallomesogenic diol with varying terminal chain length. A series of metallomesogenic polyurethanes were synthesized using these metallomesogenic diols as chain extenders for the prepolymers based on polytetramethylene glycol (PTMG) of varying molecular weight (M n = 650, 2000) and 2,4-toluene diisocyanate (TDI), or 4,4′-methylene bis(phenyl isocyanate) (MDI). The molar ratio of metallomesogenic diol and PTMG were varied in the polyurethane to find their role in liquid crystalline and mechanical properties. Extensive characterization of all metallomesogenic compounds and intermediates were carried out by FT-IR, 1 H and 13 C NMR, EPR, VSM, Mass (EI and FAB) and UV–visible spectroscopy. Hot stage polarizing microscope and differential scanning calorimetry were used to ensure the phase characteristics such as nature of phase, melting and clearing temperatures and phase range. The appearance of enantiotropic smectic A phases indicated high molecular polarizability of the core due to the metal ion. - Highlights: ► Design and synthesis of metallomesogenic diols. ► Metallomesogenic polyurethanes were prepared using these diols as chain extenders. ► Liquid crystalline and mechanical properties were studied. ► A square pyramidal structure for the copper(II) complexes have been proposed. ► Polyurethanes exhibited enantiotropic smectic A phases.

  6. Glucose Synthesis in a Protein-Based Artificial Photosynthesis System.

    Science.gov (United States)

    Lu, Hao; Yuan, Wenqiao; Zhou, Jack; Chong, Parkson Lee-Gau

    2015-09-01

    The objective of this study was to understand glucose synthesis of a protein-based artificial photosynthesis system affected by operating conditions, including the concentrations of reactants, reaction temperature, and illumination. Results from non-vesicle-based glyceraldehyde-3-phosphate (GAP) and glucose synthesis showed that the initial concentrations of ribulose-1,5-bisphosphate (RuBP) and adenosine triphosphate (ATP), lighting source, and temperature significantly affected glucose synthesis. Higher initial concentrations of RuBP and ATP significantly enhanced GAP synthesis, which was linearly correlated to glucose synthesis, confirming the proper functions of all catalyzing enzymes in the system. White fluorescent light inhibited artificial photosynthesis and reduced glucose synthesis by 79.2 % compared to in the dark. The reaction temperature of 40 °C was optimum, whereas lower or higher temperature reduced glucose synthesis. Glucose synthesis in the vesicle-based artificial photosynthesis system reconstituted with bacteriorhodopsin, F 0 F 1 ATP synthase, and polydimethylsiloxane-methyloxazoline-polydimethylsiloxane triblock copolymer was successfully demonstrated. This system efficiently utilized light-induced ATP to drive glucose synthesis, and 5.2 μg ml(-1) glucose was synthesized in 0.78-ml reaction buffer in 7 h. Light-dependent reactions were found to be the bottleneck of the studied artificial photosynthesis system.

  7. CdTe and CdSe quantum dots: synthesis, characterizations and applications in agriculture

    International Nuclear Information System (INIS)

    Ung, Thi Dieu Thuy; Tran, Thi Kim Chi; Pham, Thu Nga; Nguyen, Quang Liem; Nguyen, Duc Nghia; Dinh, Duy Khang

    2012-01-01

    This paper highlights the results of the whole work including the synthesis of highly luminescent quantum dots (QDs), characterizations and testing applications of them in different kinds of sensors. Concretely, it presents: (i) the successful synthesis of colloidal CdTe and CdSe QDs, their core/shell structures with single- and/or double-shell made by CdS, ZnS or ZnSe/ZnS; (ii) morphology, structural and optical characterizations of the synthesized QDs; and (iii) testing examples of QDs as the fluorescence labels for agricultural-bio-medical objects (for tracing residual pesticide in agricultural products, residual clenbuterol in meat/milk and for detection of H5N1 avian influenza virus in breeding farms). Overall, the results show that the synthesized QDs have very good crystallinity, spherical shape and strongly emit at the desired wavelengths between ∼500 and 700 nm with the luminescence quantum yield (LQY) of 30–85%. These synthesized QDs were used in fabrication of the three testing fluorescence QD-based sensors for the detection of residual pesticides, clenbuterol and H5N1 avian influenza virus. The specific detection of parathion methyl (PM) pesticide at a content as low as 0.05 ppm has been realized with the biosensors made from CdTe/CdS and CdSe/ZnSe/ZnS QDs and the acetylcholinesterase (AChE) enzymes. Fluorescence resonance energy transfer (FRET)-based nanosensors using CdTe/CdS QDs conjugated with 2-amino-8-naphthol-6-sulfonic acid were fabricated that enable detection of diazotized clenbuterol at a content as low as 10 pg ml −1 . For detection of H5N1 avian influenza virus, fluorescence biosensors using CdTe/CdS QDs bound on the surface of chromatophores extracted and purified from bacteria Rhodospirillum rubrum were prepared and characterized. The specific detection of H5N1 avian influenza virus in the range of 3–50 ng μl −1 with a detection limit of 3 ng μL −1 has been performed based on the antibody-antigen recognition. (review)

  8. Synthesis and characterization of triglyceride based thermosetting polymers

    Science.gov (United States)

    Can, Erde

    2005-07-01

    Plant oils, which are found in abundance in all parts of the world and are easily replenished annually, have the potential to replace petroleum as a chemical feedstock for making polymers. Within the past few years, there has been growing interest to use triglycerides as the basic constituent of thermosetting polymers with the necessary rigidity, strength and glass transition temperatures required for engineering applications. Plant oils are not polymerizable in their natural form, however various functional groups that can polymerize can easily be attached to the triglyceride structure making them ideal cross-linking monomers for thermosetting liquid molding resins. Through this research project a number of thermosetting liquid molding resins based on soybean and castor oil, which is a specialty oil with hydroxyls on its fatty acids, have been developed. The triglyceride based monomers were prepared via the malination of the alcoholysis products of soybean and castor oil with various polyols, such as pentaerythritol, glycerol, and Bisphenol A propoxylate. The malinated glycerides were then cured in the presence of a reactive diluent, such as styrene, to form rigid glassy materials with a wide range of properties. In addition to maleate half-esters, methacrylates were also introduced to the glyceride structure via methacrylation of the soybean oil glycerolysis product with methacrylic anhydride. This product, which contains methacrylic acid as by-product, and its blends with styrene also gave rigid materials when cured. The triglyceride based monomers were characterized via conventional spectroscopic techniques. Time resolved FTIR analysis was used to determine the curing kinetics and the final conversions of polymerization of the malinated glyceride-styrene blends. Dynamic Mechanical Analysis (DMA) was used to determine the thermomechanical behavior of these polymers and other mechanical properties were determined via standard mechanical tests. The use of lignin

  9. Schiff Bases of Benzothiazol-2-ylamine and Thiazolo[5,4-b] pyridin-2-ylamine as Anticonvulsants: Synthesis, Characterization and Toxicity Profiling.

    Science.gov (United States)

    Shukla, Rashmi; Singh, Ajeet P; Sonar, Pankaj K; Mishra, Mudita; Saraf, Shailendra K

    2016-01-01

    Schiff bases have a broad spectrum of biological activities like antiinflammatory, analgesic, antimicrobial, anticonvulsant, antitubercular, anticancer, antioxidant, anthelmintic and so forth. Thus, after a thorough perusal of literature, it was decided to conjugate benzothiazol-2-ylamine/thiazolo [5, 4-b] pyridin-2-ylamine with aromatic and heteroaromatic aldehydes to get a series of Schiff bases. Synthesis, characterization, in-silico toxicity profiling and anticonvulsant activity of the Schiff bases of Benzothiazol-2-ylamine and Thiazolo [5, 4-b] pyridin-2-ylamine. Aniline/4-aminopyridine was converted to the corresponding thiourea derivatives, which were cyclized to obtain benzothiazol-2-ylamine/thiazolo [5, 4-b] pyridin-2-ylamine. Finally, these were condensed with various aromatic and heteroaromatic aldehydes to obtain Schiff bases of benzothiazol-2-ylamine and thiazolo [5, 4-b] pyridin-2-ylamine. The synthesized compounds were characterized and screened for their anticonvulsant activity using maximal electroshock (MES) test and isoniazid (INH) induced convulsions test. In-silico toxicity profiling of all the synthesized compounds was done through "Lazar" and "Osiris" properties explorer. Majority of the compounds were more potent against MES induced convulsions than INH induced convulsions. Schiff bases of benzothiazol-2-ylamine were more effective than thiazolo [5, 4-b] pyridin-2-ylamine against MES induced convulsions. The compound benzothiazol-2-yl-(1H-indol-2-ylmethylene)-amine (VI) was the most potent member of the series against both types of convulsions. Compound VI exhibited the most significant activity profile in both the models. The compounds did not exhibit any carcinogenicity or acute toxicity in the in-silico studies. Thus, it may be concluded that the Schiff bases of benzothiazol-2-ylamine exhibit the potential to be promising and non-toxic anticonvulsant agents.

  10. Synthesis and characterization of anisotropic magnetic hydrogels

    Energy Technology Data Exchange (ETDEWEB)

    Hinrichs, Stephan, E-mail: stephan.hinrichs@chemie.uni-hamburg.de; Nun, Nils; Fischer, Birgit, E-mail: birgit.fischer@chemie.uni-hamburg.de

    2017-06-01

    Multiresponsive hydrogels are an interesting new class of materials. They offer the advantage, that they respond to different stimuli like temperature, pH and magnetic fields. By this they can change their properties which makes the hydrogels ideal candidates for many applications in the technical as well as medical field. Here we present the synthesis and characterization of hydrogels - micro- as well as macrogels - which consist of an iron oxide core, varying in phase and morphology, embedded in a thermoresponsive polymer, consisting of poly N-isopropylacrylamide. By using dynamic light scattering we investigated the thermoresponsive properties. In addition we were able to follow the formation of the macrogel by monitoring the shear viscosity.

  11. Nanostructured carbon-supported Pd electrocatalysts for ethanol oxidation: synthesis and characterization

    International Nuclear Information System (INIS)

    Gacutan, E M; Tongol, B J; Climaco, M I; Telan, G J; Malijan, F; Hsu, H Y; Garcia, J; Fulo, H

    2012-01-01

    The need to lower the construction cost of fuel cells calls for the development of non-Pt based electrocatalysts. Among others, Pd has emerged as a promising alternative to Pt for fuel cell catalysis. This research aims to investigate the synthesis and characterization of nanostructured Pd-based catalysts dispersed on carbon support as anode materials in direct ethanol fuel cells. For the preparation of the first Pd-based electrocatalyst, palladium nanoparticles (NPs) were synthesized via oleylamine (OAm)-mediated synthesis and precursor method with a mean particle size of 3.63 ± 0.59 nm as revealed by transmission electron microscopy (TEM). Carbon black was used as a supporting matrix for the OAm-capped Pd NPs. Thermal annealing and acetic acid washing were used to remove the OAm capping agent. To evaluate the electrocatalytic activity of the prepared electrocatalyst towards ethanol oxidation, cyclic voltammetry (CV) studies were performed using 1.0 M ethanol in basic medium. The CV data revealed the highest peak current density of 11.05 mA cm −2 for the acetic acid-washed Pd/C electrocatalyst. Meanwhile, the fabrication of the second Pd-based electrocatalyst was done by functionalization of the carbon black support using 3:1 (v/v) H 2 SO 4 :HNO 3 . The metal oxide, NiO, was deposited using precipitation method while polyol method was used for the deposition of Pd NPs. X-ray diffraction (XRD) analysis revealed that the estimated particle size of the synthesized catalysts was at around 9.0–15.0 nm. CV results demonstrated a 36.7% increase in the catalytic activity of Pd–NiO/C (functionalized) catalyst towards ethanol oxidation compared to the non-functionalized catalyst. (paper)

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

    Science.gov (United States)

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

    2017-06-01

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

  13. Robotics-based synthesis of human motion

    KAUST Repository

    Khatib, O.; Demircan, E.; De Sapio, V.; Sentis, L.; Besier, T.; Delp, S.

    2009-01-01

    The synthesis of human motion is a complex procedure that involves accurate reconstruction of movement sequences, modeling of musculoskeletal kinematics, dynamics and actuation, and characterization of reliable performance criteria. Many of these processes have much in common with the problems found in robotics research. Task-based methods used in robotics may be leveraged to provide novel musculoskeletal modeling methods and physiologically accurate performance predictions. In this paper, we present (i) a new method for the real-time reconstruction of human motion trajectories using direct marker tracking, (ii) a task-driven muscular effort minimization criterion and (iii) new human performance metrics for dynamic characterization of athletic skills. Dynamic motion reconstruction is achieved through the control of a simulated human model to follow the captured marker trajectories in real-time. The operational space control and real-time simulation provide human dynamics at any configuration of the performance. A new criteria of muscular effort minimization has been introduced to analyze human static postures. Extensive motion capture experiments were conducted to validate the new minimization criterion. Finally, new human performance metrics were introduced to study in details an athletic skill. These metrics include the effort expenditure and the feasible set of operational space accelerations during the performance of the skill. The dynamic characterization takes into account skeletal kinematics as well as muscle routing kinematics and force generating capacities. The developments draw upon an advanced musculoskeletal modeling platform and a task-oriented framework for the effective integration of biomechanics and robotics methods.

  14. Robotics-based synthesis of human motion

    KAUST Repository

    Khatib, O.

    2009-05-01

    The synthesis of human motion is a complex procedure that involves accurate reconstruction of movement sequences, modeling of musculoskeletal kinematics, dynamics and actuation, and characterization of reliable performance criteria. Many of these processes have much in common with the problems found in robotics research. Task-based methods used in robotics may be leveraged to provide novel musculoskeletal modeling methods and physiologically accurate performance predictions. In this paper, we present (i) a new method for the real-time reconstruction of human motion trajectories using direct marker tracking, (ii) a task-driven muscular effort minimization criterion and (iii) new human performance metrics for dynamic characterization of athletic skills. Dynamic motion reconstruction is achieved through the control of a simulated human model to follow the captured marker trajectories in real-time. The operational space control and real-time simulation provide human dynamics at any configuration of the performance. A new criteria of muscular effort minimization has been introduced to analyze human static postures. Extensive motion capture experiments were conducted to validate the new minimization criterion. Finally, new human performance metrics were introduced to study in details an athletic skill. These metrics include the effort expenditure and the feasible set of operational space accelerations during the performance of the skill. The dynamic characterization takes into account skeletal kinematics as well as muscle routing kinematics and force generating capacities. The developments draw upon an advanced musculoskeletal modeling platform and a task-oriented framework for the effective integration of biomechanics and robotics methods.

  15. Microwave-assisted synthesis and micellization behavior of soy-based copoly(2-oxazoline)s

    OpenAIRE

    Hoogenboom, Richard; Leenen, Mark A. M.; Huang, Haiying; Fustin, Charles-Andr?; Gohy, Jean-Fran?ois; Schubert, Ulrich S.

    2006-01-01

    Polymers based on renewable resources are promising candidates for replacing common organic polymers, and thus, for reducing oil consumption. In this contribution we report the microwave-assisted synthesis of block and statistical copolymers from 2-ethyl-2-oxazoline and 2-?soy alkyl?-2-oxazoline via a cationic ring-opening polymerization mechanism. The synthesized copolymers were characterized by gel permeation chromatography and 1H-NMR spectroscopy. The micellization of these amphiphilic cop...

  16. Octalithium plumbate as breeding blanket ceramic: Neutronic performances, synthesis and partial characterization

    International Nuclear Information System (INIS)

    Colominas, S.; Palermo, I.; Abellà, J.; Gómez-Ros, J.M.; Sanz, J.; Sedano, L.

    2012-01-01

    Highlights: ► Definition of a suitable configuration for the Li 8 PbO 6 breeding blanket design. ► Demonstration of the feasibility of Li 8 PbO 6 as a breeding material. ► Synthesis optimization in the Li 8 PbO 6 production. ► Characterization of Li 8 PbO 6 by X-ray phase analysis is discussed. - Abstract: A neutronic assessment of the performances of a helium-cooled Li 8 PbO 6 breeding blanket (BB) for the conceptual design of a DEMO fusion reactor is given. Different BB configurations have been considered in order to minimize the amount of beryllium required for neutron multiplication, including the use of graphite as reflector material. The calculated neutronic responses: tritium breeding ratio (TBR), power deposition in TF coils and power amplification factor, indicate the feasibility of Li 8 PbO 6 as breeding material. Furthermore, the synthesis and characterization of Li 8 PbO 6 by X-ray phase analysis are also discussed.

  17. Synthesis and characterization of thiolated polymers based on polyhydroxyethylakrylate and 3-mercaptopropylmethoxysilane

    Directory of Open Access Journals (Sweden)

    G. Irmukhametova

    2012-03-01

    Full Text Available In the presented paper thiolated polymer based on nonionic polyhydroxyethylmethacrylate (PHEMA and 3-mercaptopropyltrimethoxysilane (MPTS was obtained and characterized. Results of Raman-spectroscopy and Elman’s assay showed the presence of thiol groups in the modified polymer.

  18. Synthesis and characterization of superabsorbent hydrogel based ...

    African Journals Online (AJOL)

    The hydrogels structure was characterized by Fourier transform infrared (FTIR) spectroscopy, scanning electron microscopy (SEM) and thermogravimetric analysis (TGA). The effect of grafting variables, that is, AA/AN weight ratio and concentration of MBA and APS, was systematically optimized to achieve a hydrogel with ...

  19. Colloidal synthesis and characterization of Bi2S3 nanoparticles for photovoltaic applications

    International Nuclear Information System (INIS)

    Piras, R; Aresti, M; Saba, M; Marongiu, D; Mula, G; Quochi, F; Mura, A; Bongiovanni, G; Cannas, C; Mureddu, M; Ardu, A; Ennas, G; Musinu, A; Calzia, V; Mattoni, A

    2014-01-01

    Bismuth sulfide is a promising n-type semiconductor for solar energy conversion. We have explored the colloidal synthesis of Bi 2 S 3 nanocrystals, with the aim of employing them in the fabrication of solution-processable solar cells and to replace toxic heavy metals chalcogenides like PbS or CdS, that are currently employed in such devices. We compare different methods to obtain Bi 2 S 3 colloidal quantum dots, including the use of environmentally benign reactants, through organometallic synthesis. Different sizes and shapes were obtained according to the synthesis parameters and the growth process has been rationalized by comparing the predicted morphology with systematic physical-chemistry characterization of nanocrystals by X-ray diffraction, FT-IR spectroscopy, Transmission Electron Microscopy (TEM)

  20. Synthesis and characterization of dihexyldithiocarbamate as a chelating agent in extraction of gold(III)

    Energy Technology Data Exchange (ETDEWEB)

    Fatimah, Soja Siti, E-mail: soja-sf@upi.edu [Departemen Pendidikan Kimia, Universitas Pendidikan Indonesia, Jl. Dr. Setiabudhi No. 229, Bandung 40154 (Indonesia); Department of Chemistry, Faculty of Mathematics and Natural Sciences, Padjadjaran University, Jl. Raya Bandung-Sumedang, Km. 21, Jatinangor (Indonesia); Bahti, Husein H.; Hastiawan, Iwan [Department of Chemistry, Faculty of Mathematics and Natural Sciences, Padjadjaran University, Jl. Raya Bandung-Sumedang, Km. 21, Jatinangor (Indonesia); Permanasari, Anna [Departemen Pendidikan Kimia, Universitas Pendidikan Indonesia, Jl. Dr. Setiabudhi No. 229, Bandung 40154 (Indonesia)

    2016-02-08

    The use of dialkyldithiocarbamates as chelating agents of transition metals have been developing for decades. Many chelating agents have been synthesized and used in the extraction of the metals. Studies on particular aspects of extraction of the metals, such as the effect of increasing hydrophobicity of chelating agents on the effectiveness of the extraction, have been done. However, despite the many studies on the synthesis and applications of this type of chelating agents, interests in the aspect of molecular structure of the synthesized ligands and of their complexes, have been limited. This study aimed at synthesizing and characterizing dihexylthiocarbamate, and using the ligand for the extraction of gold III). Characterization of the ligand and of its metal complex were done by using elemental analysis, DTG, and spectroscopic methods to include NMR, ({sup 1}H, and {sup 13}C), FTIR, and MS-ESI. Data on the synthesis, characterization, and the application of the ligand as a chelating agent are presented.

  1. Synthesis and characterization of dihexyldithiocarbamate as a chelating agent in extraction of gold(III)

    Science.gov (United States)

    Fatimah, Soja Siti; Bahti, Husein H.; Hastiawan, Iwan; Permanasari, Anna

    2016-02-01

    The use of dialkyldithiocarbamates as chelating agents of transition metals have been developing for decades. Many chelating agents have been synthesized and used in the extraction of the metals. Studies on particular aspects of extraction of the metals, such as the effect of increasing hydrophobicity of chelating agents on the effectiveness of the extraction, have been done. However, despite the many studies on the synthesis and applications of this type of chelating agents, interests in the aspect of molecular structure of the synthesized ligands and of their complexes, have been limited. This study aimed at synthesizing and characterizing dihexylthiocarbamate, and using the ligand for the extraction of gold III). Characterization of the ligand and of its metal complex were done by using elemental analysis, DTG, and spectroscopic methods to include NMR, (1H, and 13C), FTIR, and MS-ESI. Data on the synthesis, characterization, and the application of the ligand as a chelating agent are presented.

  2. Radiation synthesis and characterization of new hydrogels based on acrylamide copolymers cross-linked with 1-allyl-2-thiourea

    Energy Technology Data Exchange (ETDEWEB)

    Sahiner, Nurettin [Department of Chemistry, Faculty of Science, Hacettepe University, Beytepe Campus, 0653 Ankara (Turkey); Malci, Savas [Department of Chemistry, Faculty of Science, Hacettepe University, Beytepe Campus, 0653 Ankara (Turkey); Celikbicak, Oemuer [Department of Chemistry, Faculty of Science, Hacettepe University, Beytepe Campus, 0653 Ankara (Turkey); Kantoglu, Oemer [Ankara Nuclear Research Center, Turkish Atomic Energy Authority, 06983 Ankara (Turkey); Salih, Bekir [Department of Chemistry, Faculty of Science, Hacettepe University, Beytepe Campus, 0653 Ankara (Turkey)]. E-mail: bekir@hacettepe.edu.tr

    2005-10-01

    Poly(acrylamide-1-allyl-2-thiourea) hydrogels, Poly(AA-AT), were synthesized by gamma irradiation using {sup 60}Co {gamma} source in different irradiation dose and at different 1-allyl-2-thiourea content in the monomer mixture. For the characterization of the hydrogels, Fourier transform infrared spectrometer (FT-IR), thermogravimetric analyzer (TGA), elemental analyzer and the swellability of the hydrogels were used. It was noted that 1-allyl-2-thiourea in the synthesized hydrogels was increased by the increasing the content of the 1-allyl-2-thiourea in the irradiation monomer mixture and increasing the radiation dose for the hydrogel synthesis. sis.

  3. Synthesis and characterization of M-type barium hexferrite by ultrasonic inter-dispersion of chemical precipitate

    International Nuclear Information System (INIS)

    Garcia Junior, E.S.; Gomes Junior, G.G.; Ogasawara, T.

    2010-01-01

    This work is concerned with the study the synthesis and characterization of M-type barium hexaferrite powder by chemical precipitation type and ultrasonic interdispersion of precursor materials Fe(OH) 3 and Ba(OH) 2 ,separately and ultrasonic inter-dispersion, followed by drying and calcining. In order to guide the experimental work was carried out a preliminary thermodynamic analysis of the system Ba-Fe-H 2 O at 25 deg C. The study shows that the phase formation of M-type barium hexaferrite is obtained at a calcination at 1000 deg C, characterized by X-ray diffraction, the grain growth of the final product of synthesis depending on the calcination temperature is visible by SEM. The synthesis method developed in this research is an option to achieve the results that would be obtained if the co-precipitation of ferric and barium hydroxide was thermodynamically possible, where you can get crystallization of barium hexaferrite in a calcination at 1000 deg C. (author)

  4. Designing Selectivity in Metal-Semiconductor Nanocrystals: Synthesis, Characterization, and Self-Assembly

    Science.gov (United States)

    Pavlopoulos, Nicholas George

    This dissertation contains six chapters detailing recent advances that have been made in the synthesis and characterization of metal-semiconductor hybrid nanocrystals (HNCs), and the applications of these materials. Primarily focused on the synthesis of well-defined II-VI semiconductor nanorod (NR) and tetrapod (TP) based constructs of interest for photocatalytic and solar energy applications, the research described herein discusses progress towards the realization of key design rules for the synthesis of functional semiconductor nanocrystals (NCs). As such, a blend of novel synthesis, advanced characterization, and direct application of heterostructured nanoparticles are presented. The first chapter is a review summarizing the design, synthesis, properties, and applications of multicomponent nanomaterials composed of disparate semiconductor and metal domains. By coupling two compositionally distinct materials onto a single nanocrystal, synergistic properties can arise that are not present in the isolated components, ranging from self-assembly to photocatalysis. For semiconductor nanomaterials, this was first realized in the ability to tune nanomaterial dimensions from 0-D quantum dot (QD) structures to cylindrical (NR) and branched (TP) structures by exploitation of advanced colloidal synthesis techniques and understandings of NC facet reactivities. The second chapter is focused on the synthesis and characterization of well-defined CdSe-seeded-CdS (CdSe CdS) NR systems synthesized by overcoating of wurtzite (W) CdSe quantum dots with W-CdS shells. 1-dimensional NRs have been interesting constructs for applications such as solar concentrators, optical gains, and photocatalysis. Through synthetic control over CdSe CdS NR systems, materials with small and large CdSe seeds were prepared, and for each seed size, multiple NR lengths were prepared. Through transient absorption studies, it was found that band alignment did not affect the efficiency of charge localization

  5. An electrochemical procedure coupled with a Schiff base method; application to electroorganic synthesis of new nitrogen-containing heterocycles

    International Nuclear Information System (INIS)

    Dowlati, Bahram; Othman, Mohamed Rozali

    2013-01-01

    The synthesis of Nitrogen-containing heterocycles has been achieved using chemical and electrochemical methods, respectively. The direct chemical synthesis of nucleophiles proceeds through the Schiff base chemical reaction. This procedure offers an alternate reaction between dicarbonyl compounds and diamines leads to the formation of products. The results indicate that the Schiff base chemical method for synthesis of the product has successfully performed in excellent overall yield. In the electrochemical step, a series of Nitrogen-containing compounds were electrosynthesized. Various parameters such as the applied potential, pH of the electrolytic solution, cell configuration and also purification techniques, were carried out to optimize the yields of corresponding products. New Nitrogen-containing heterocycle derivatives were synthesized using an electrochemical procedure coupled with a Schiff base as a facile, efficient and practical method. The products have been characterized after purification by IR, 1 H NMR, 13 C NMR and ESI-MS 2

  6. Synthesis and characterization of boehmites obtained from gibbsite in presence of different environments

    Energy Technology Data Exchange (ETDEWEB)

    Denigres Filho, Ricardo Wilson Nastari; Rocha, Gisele de Araujo; Vieira-Coelho, Antonio Carlos, E-mail: acvcoelh@usp.br [Universidade de Sao Paulo (LPSS/EP/USP), SP (Brazil). Departamento de Engenharia Metalurgica e de Materiais. Laboratorio de Materias-Primas Particuladas; Montes, Celia Regina [Centro de Energia Nuclear na Agricultura (NUPEGEL/CENA/USP), Piracicaba, SP (Brazil). Nucleo de Pesquisas Geoquimicas e Geofisicas da Listosfera

    2016-05-15

    In this study, results related to boehmite synthesis by hydrothermal processes starting from a Bayer commercial gibbsite are reported. The processes have been conducted from aqueous suspensions with initial acidic or alkaline pH, without or with acetate ion, at 160 deg C for 72h to 168h. The final materials were characterized by X-ray diffraction (XRD), thermal methods (DTA and TGA) and scanning electron microscopy (SEM). The influence of the synthesis conditions on the morphology of the boehmite crystals obtained from the gibbsite at different hydrothermal processes are discussed. (author)

  7. Synthesis, characterization and a.c. magnetic analysis of magnetite nanoparticles

    International Nuclear Information System (INIS)

    Riani, P.; Napoletano, M.; Canepa, F.

    2011-01-01

    In the last years, the study of Fe-based magnetic nanoparticles (MNP) has attracted increasing interest either for the physical properties shown by nanosized materials (electric and magnetic properties are strongly affected by dimension and surface effects) either for the different technological applications of these materials (catalysis, drug delivery, magnetic resonance imaging, contaminants removal from groundwater, new exchange coupled magnets, soft nanomagnets for high frequency applications, etc.). In this article, the results obtained in the synthesis and characterization of the Fe 3 O 4 MNP is reported. The magnetite nanoparticles were synthesized by a modified Massart method. Structural characterization was performed using X-ray diffraction analysis and a complete morphological and dimensional study was carried out by means of Transmission Electron Microscopy, and a.c. magnetic susceptibility measured as a function of the frequency of the applied magnetic field. Diameters of the superparamagnetic Fe 3 O 4 nanoparticles are ranging from 2 to 10 nm, as evidenced by all the techniques employed. The size distribution of the hydrated aggregates in solution has been obtained by quantitative analysis of the frequency dependence of the a.c. susceptibility. The mathematical approach adopted will be described and all the obtained results will be compared and discussed.

  8. Synthesis and structural characterization of some trisulfide analoges of thiouracil-based antithyroid drugs

    Science.gov (United States)

    Bhabak, Krishna P.; Bhowmick, Debasish

    2012-08-01

    Thiourea-based antithyroid drugs are effectively used for the treatment of hyperthyroidism. In this paper, we describe the synthesis of new trisulfides (11-12) from the commonly used thiourea-based antithyroid drugs such as 6-n-propyl-2-thiouracil (PTU) and 6-methyl-2-thiouracil (MTU) in the reaction with I2/KI system. Structural analysis by single crystal X-ray diffraction studies revealed the stabilization of trisulfides by a lactam-lactim tautomerism facilitating effective intramolecular as well as intermolecular non-covalent interactions. Although the structures of both trisulfides were found to be quite similar, a notable difference in the intermolecular interactions was observed between compounds 11 and 12 leading to different structural patterns. Structural stabilization of these trisulfides by tautomerism followed by intramolecular as well as intermolecular H-bonds makes these molecules as perfect examples in molecular recognition with self-complementary donor and acceptor units within a single molecule.

  9. Enzymatic preparation and characterization of soybean lecithin-based emulsifiers

    International Nuclear Information System (INIS)

    Reddy Jala, R.C.; Chen, B.; Li, H.; Zhang, Y.; Cheong, L.Z.; Yang, T.; Xu, X.

    2016-01-01

    Simple enzymatic methods were developed for the synthesis of lysolecithin, glycerolyzed lecithin and hydrolyzed lecithin. The products were characterized in terms of their acetone insoluble matter, hexane insoluble matter, moisture, phospholipid distribution and fatty acid composition. The HLB value ranges of different products with different acid values were detected. The efficiency of optimally hydrolyzed lecithin was examined at high calcium ion, low pH, and aqueous solutions and compared with commercially available standard lecithin-based emulsifiers. Overall, lysolecithin powder was proven to be the best emulsifier even at strong and medium acidic conditions. [es

  10. Synthesis and characterization of ferrous phosphate (vivianite) and its behavior in aqueous media

    International Nuclear Information System (INIS)

    Diaz F, J.C.

    2003-01-01

    The synthesis and characterization of materials that can be useful in Environmental Chemistry is very important because their characteristics are exposed and its behavior in chemical phenomena as the sorption in aqueous media is understand to use it in the human being benefit. With the object of using, in a future, the octa hydrated ferrous phosphate (vivianite) as a potential candidate for matrix confinement in contention walls for the storage of radioactive waste of long half life, it was synthesized and it characterized physico chemically and their properties of surface of this compound were evaluated. Presently work was carried out the synthesis and structural characterization of the iron phosphate II by infrared spectroscopy with having Fourier transform, high vacuum scanning electron microscopy, X-ray diffraction, thermal gravimetric analysis, the BET multipoint surface area and Moessbauer spectroscopy; as well as, the determination between aqueous media of the isoelectric point and the density of sites of surface of the compound. The octa hydrated ferrous phosphate was obtained pure. The results indicate that the product corresponds to the prospective mineral, the vivianite. The thermal gravimetric analysis demonstrated that the ferrous phosphate is a stable salt after the lost of water. The isoelectric point is since an important parameter because allows to know the behavior of the surface of the material in aqueous systems, in this case the isoelectric point, of the octa hydrated ferrous phosphate, in distilled water is of pH 4.20 and in solution of potassium nitrate 0.5 M is of pH = 3.75. This indicates that the material has an amphoteric surface depending on the pH. On the other hand, the density of active sites of surface obtained by titrations acid-base is of 20 sites by nm 2 . (Author)

  11. The Heeger & Bergen Pyramid Based Texture Synthesis Algorithm

    Directory of Open Access Journals (Sweden)

    Thibaud Briand

    2014-11-01

    Full Text Available This contribution deals with the Heeger-Bergen pyramid-based texture analysis/synthesis algorithm. It brings a detailed explanation of the original algorithm tested on many characteristic examples. Our analysis reproduces the original results, but also brings a minor improvement concerning non-periodic textures. Inspired by visual perception theories, Heeger and Bergen proposed to characterize a texture by its first-order statistics of both its color and its responses to multiscale and multi-orientation filters, namely the steerable pyramid. The Heeger-Bergen algorithm consists in the following procedure: starting from a white noise image, histogram matchings are performed to the noise alternatively in both the image domain and steerable pyramid domain, so that the corresponding histograms match the ones of the input texture.

  12. Development of Hydrotalcite Based Cobalt Catalyst by Hydrothermal and Co-precipitation Method for Fischer-Tropsch Synthesis

    Directory of Open Access Journals (Sweden)

    Muhammad Faizan Shareef

    2017-10-01

    Full Text Available This paper presents the effect of a synthesis method for cobalt catalyst supported on hydrotalcite material for Fischer-Tropsch synthesis. The hydrotalcite supported cobalt (HT-Co catalysts were synthesized by co-precipitation and hydrothermal method. The prepared catalysts were characterized by using various techniques like BET (Brunauer–Emmett–Teller, SEM (Scanning Electron Microscopy, TGA (Thermal Gravimetric Analysis, XRD (X-ray diffraction spectroscopy, and FTIR (Fourier Transform Infrared Spectroscopy. Fixed bed micro reactor was used to test the catalytic activity of prepared catalysts. The catalytic testing results demonstrated the performance of hydrotalcite based cobalt catalyst in Fischer-Tropsch synthesis with high selectivity for liquid products. The effect of synthesis method on the activity and selectivity of catalyst was also discussed. Copyright © 2017 BCREC Group. All rights reserved Received: 3rd November 2016; Revised: 26th February 2017; Accepted: 9th March 2017; Available online: 27th October 2017; Published regularly: December 2017 How to Cite: Sharif, M.S., Arslan, M., Iqbal, N., Ahmad, N., Noor, T. (2017. Development of Hydrotalcite Based Cobalt Catalyst by Hydrothermal and Co-precipitation Method for Fischer-Tropsch Synthesis. Bulletin of Chemical Reaction Engineering & Catalysis, 12(3: 357-363 (doi:10.9767/bcrec.12.3.762.357-363

  13. Synthesis and characterization of covalent diphenylalanine nanotube-folic acid conjugates

    DEFF Research Database (Denmark)

    León, John Jairo Castillo; Rindzevicius, Tomas; Wu, Kaiyu

    2014-01-01

    Herein, we describe the synthesis and characterization of a covalent nanoscale assembly formed between diphenylalanine micro/nanotubes (PNT) and folic acid (FA). The conjugate was obtained via chemical functionalization through coupling of amine groups of PNTs and carboxylic groups of FA. The sur...... for applications in the detection and diagnosis of cancer or tropical diseases such as leishmaniasis and as a carrier nanosystem delivering drugs to malignant tumors that overexpress folate receptors....

  14. Synthesis and characterization of polyphosphazene electrolytes including cyclic ether side groups

    Science.gov (United States)

    Fiedler, Carsten; Luerssen, Bjoern; Lucht, Brett; Janek, Juergen

    2018-04-01

    This paper presents the synthesis and detailed characterization of two polyphosphazene based polymers, including different cyclic ether side groups. The final polymers were obtained by a well-known method employing a living cationic polymerization and subsequent nucleophilic substitution. The synthesized polymers Poly [(1,3-dioxane-5-oxy) (1,3-dioxolane-4-methoxy)phosphazene] (DOPP) and Poly[bis(2-Tetrahydro-3-furanoxy)phosphazene] (THFPP) were mixed with varied amounts of lithium bis(trifluoromethane)sulfonamide (LiTFSI) and the interactions between the salt and the polymer chains were studied by Fourier transform infrared (FT-IR) and differential scanning calorimetry (DSC) measurements. Electrochemical characterization was performed by electrochemical impedance spectroscopy (EIS) and direct current polarization in the temperature range of 20-60 °C. These measurements were utilized to calculate the lithium transference number (t+), the lithium conductivity (σ) and its activation energy in order to elucidate the lithium transport behavior. Relatively high lithium transference numbers of 0.6 (DOPP) and 0.7 (THFPP) at 60 °C are found and reveal maximum lithium conductivities of 2.8·10-6 Sṡcm-1 and 9.0·10-7 Sṡcm-1 for DOPP and THFPP at 60 °C, respectively.

  15. Synthesis and characterization of nanocomposites based on polyurethane in aqueous dispersions with non-modified hydrophilic clays

    International Nuclear Information System (INIS)

    Miranda, G.S.; Delpechi, M.C.; Santo, W.L.E.

    2010-01-01

    Several studies involving the formation of polyurethane nanocomposites employing clays of montmorillonite modified. This involves the presence of quaternary ammonium salts, the cation exchange needed to increase the interlayer space of clays that incorporate more than one step to the process, generates a higher cost. In this paper the synthesis of nanocomposite polyurethanes dispersed in water allowed not only the production of materials less harmful to the environment, but also the incorporation of hydrophilic clays, calcium and sodium in nature, without any modifications. Dispersions produced from 0.5, 1.0 and 2.5% clay (on the mass of prepolymer) were characterized in terms of total solids content, the films obtained by casting were evaluated for adhesiveness, diffraction X-rays, scanning electron microscopy. Most systems showed intercalated and partially exfoliated structures. (author)

  16. Synthesis and Characterization of Magnesium Substituted Aluminophosphate Molecular Sieves with AEL Structure

    Institute of Scientific and Technical Information of China (English)

    Benjing Xu; Ling Qian; Xinmei Liu; Chunmin Song; Zifeng Yan

    2004-01-01

    MAPO-11 molecular sieves were synthesized by hydrothermal methods. The influence of precursor of magnesium, Mg/Al ratio, synthesis temperature, synthesis time and the type of template on the formation and properties of MAPO-11 molecular sieves was examined. The samples were characterized by the techniques of X-ray diffraction (XRD), scanning electron microscopy (SEM), thermogravimetric/differential thermogravimetric analysis (TG-DGA), etc. The results show that the shape and size of crystal were influenced by the precursor of Mg, the Mg/Al ratio and the type of template, and the TG-DGA analysis shows that MAPO-11 molecular sieves as-synthesized have poor thermal stability.

  17. Synthesis and characterization of hydroxyapatite crystals: a review study on the analytical methods

    NARCIS (Netherlands)

    Koutsopoulos, S.

    2002-01-01

    For the synthesis of hydroxyapatite crystals from aqueous solutions three preparation methods were employed. From the experimental processes and the characterization of the crystals it was concluded that aging and precipitation kinetics are critical for the purity of the product and its

  18. Preliminary characterization of propellants based on p(GA/BAMO) and pAMMO binders

    Energy Technology Data Exchange (ETDEWEB)

    Barbieri, Ugo; Polacco, Giovanni [Department of Chemical Engineering, University of Pisa (Italy); Keicher, Thomas [Fraunhofer-Institut fuer Chemische Technologie (ICT), Pfinztal (Germany); Massimi, Roberto [AVIO S.p.A., Roma (Italy)

    2009-10-15

    In previous papers, the synthesis and characterization of OH-terminated glycidyl azide-r-(3,3-bis(azidomethyl)oxetane) copolymers (GA/BAMO) and poly-3-azidomethyl-3-methyl oxetane (pAMMO) by azidation of their respective polymeric substrates were described. The main objective was the preparation of amorphous azido-polymers, as substitutes of hydroxy-terminated polybutadiene (HTPB) in new formulations of energetic propellants. Here, the subsequent characterization of both the binders is presented. First of all, several isocyanates were checked in order to optimize the curing reaction, and then two small-scale formulations of a propellant, based on aluminium and ammonium perchlorate, were prepared and characterized. Finally, the mechanical properties and burning rate were compared to those of a similar propellant based on HTPB as binder. (Abstract Copyright [2009], Wiley Periodicals, Inc.)

  19. Selective recognition of palladium based on functional mono phthalocyanines; synthesis, characterization and photophysical properties

    Energy Technology Data Exchange (ETDEWEB)

    Yaraşir, M. Nilüfer; Aytekin, Ahmet [Department of Chemistry, Sakarya University, TR54187 Serdivan, Sakarya (Turkey); Kandaz, Mehmet, E-mail: mkandaz@sakarya.edu.tr [Department of Chemistry, Sakarya University, TR54187 Serdivan, Sakarya (Turkey); Güney, Orhan [Istanbul Technical University, Department of Chemistry, 34469 Maslak, Istanbul (Turkey)

    2016-09-15

    We report the synthesis and photophysical properties of 4,5-bis(2-((Z)-(3-hydroxynaphthalen-2-yl) methyleneamino)phenylthio)phthalonitrile ligand (SB) and its star-type functional zincphthalocyanine (SB-ZnPc) compound obtained by the condensation of 2,3,9,10,16,17,23,24-octakis-(2-aminophenylthio)zincphthlocyanines (A-ZnPc) and 1-hydroxy-2-naphthaldehyde (HNA). Each compound was purified and characterized by elemental analysis, FTIR, {sup 1}H NMR, {sup 13}C NMR, UV/vis and MS (Maldi-TOF) spectral data. SB-ZnPc bearing fluorescent SB moieties on the periphery shows selective palladium ion sensing behavior by acting as hard core upon interaction. Electronic spectra of the SB-ZnPc displays pronounced changes in both absorption and fluorescence spectra upon interaction with Pd{sup 2+} ion. The fluorescence of the SB-ZnPc compound is effectively quenched by treatment with Pd{sup 2+} in THF solution. The solvent effect on the photophysical properties of the SB-ZnPc and interference effect of foreign metal ions were also investigated.

  20. Synthesis and Spectroscopic Characterization of Two Tetrasubstituted Cationic Porphyrin Derivatives

    Directory of Open Access Journals (Sweden)

    Newton M. Barbosa Neto

    2011-07-01

    Full Text Available An imidazolium tetrasubstituted cationic porphyrin derivative (the free base and its Zn(II complex with five-membered heterocyclic groups in the meso-positions were synthesized using microwave irradiation, and the compounds obtained characterized by 1H-NMR and mass spectrometry. We observed that under microwave irradiation the yield is similar to when the synthesis is performed under conventional heating, however, the time required to prepare the porphyrins decreases enormously. In order to investigate the electronic state of these compounds, we employed UV-Vis and fluorescence spectroscopy combined with quantum chemical calculations. The results reveal the presence, in both compounds, of a large number of electronic states involving the association between the Soret and a blue-shifted band. The Soret band in both compounds also shows a considerable solvent dependence. As for emission, these compounds present low quantum yield at room temperature and no solvent influence on the fluorescence spectra was observed.

  1. Synthesis characterization, and properties of rubber lattices; a review

    International Nuclear Information System (INIS)

    Khan, S.M.; Chughtai, A.; Sattar, A.

    2008-01-01

    Latex is a stable dispersion of polymeric material in an aqueous medium. Lattices are present in natural as well as in synthetic forms. The range of applications of latex is extensive in carpet underlay, fabric back-coating, paper and paints coatings, adhesive, binder, leather finish, floor polish, waterproof clothing, bounded fiber, pigment printing, latex thread, cement and asphalt, foam scraps binders, can closure, thickeners, box toes and shoes counters, sealant and mastics, modifiers, protein reduction, enzyme treatment and peroxide vulcanization. In this review we are presenting synthesis, characterization, properties, manufacturing and processing of latex. (author)

  2. Synthesis and Characterization of Biscoumarin and Benzopyrano Dicoumarin Derivatives

    International Nuclear Information System (INIS)

    Nik Khairunissa' Nik Abdullah Zawawi; Muhammad Taha; Norizan Ahmat; Nor Hadiani Ismail; Nik Khairunissa' Nik Abdullah Zawawi; Muhammad Taha; Norizan Ahmat; Nor Hadiani Ismail

    2016-01-01

    The wide-ranging biological activities of 4-hydroxycoumarin have stimulated considerable interest in this class of compounds, and various biscoumarin derivatives have been synthesized. Recently, a number of methods have been reported for the synthesis of biscoumarin by the reaction of 4-hydroxycoumarin and various aldehydes in the presence of catalysts. In the present study, a new series of biscoumarin and benzopyrano dicoumarin were synthesized and physically characterized by nuclear magnetic resonane ( 1 H and 13 C NMR), fourier transform infrared spectroscopy (FTIR), mass spectrometry (MS) and melting point. (author)

  3. Synthesis, structure characterization and catalytic activity of nickel tungstate nanoparticles

    International Nuclear Information System (INIS)

    Pourmortazavi, Seied Mahdi; Rahimi-Nasrabadi, Mehdi; Khalilian-Shalamzari, Morteza; Zahedi, Mir Mahdi; Hajimirsadeghi, Seiedeh Somayyeh; Omrani, Ismail

    2012-01-01

    Graphical abstract: NiWO 4 nanoparticles were prepared via precipitation technique. Experimental parameters of procedure were optimized statistically. Highlights: ► NiWO 4 spherical nanoparticles were synthesized via direct precipitation method. ► Taguchi robust design was used for optimization of synthesis reaction parameters. ► Composition and structural properties of NiWO 4 nanoparticles were characterized. ► EDAX, XRD, SEM, FT-IR, UV–vis and photoluminescence techniques were employed. ► Catalytic activity of the product in a cyclo-addition reaction was investigated. - Abstract: Taguchi robust design was applied to optimize experimental parameters for controllable, simple and fast synthesis of nickel tungstate nanoparticles. NiWO 4 nanoparticles were synthesized by precipitation reaction involving addition of nickel ion solution to the tungstate aqueous reagent and then formation of nickel tungstate nucleolus which are insoluble in aqueous media. Effects of various parameters such as nickel and tungstate concentrations, flow rate of reagent addition and reactor temperature on diameter of synthesized nickel tungstate nanoparticles were investigated experimentally by the aid of orthogonal array design. The results for analysis of variance (ANOVA) showed that particle size of nickel tungstate can be effectively tuned by controlling significant variables involving nickel and tungstate concentrations and flow rate; while, temperature of the reactor has a no considerable effect on the size of NiWO 4 particles. The ANOVA results proposed the optimum conditions for synthesis of nickel tungstate nanoparticles via this technique. Also, under optimum condition nanoparticles of NiWO 4 were prepared and their structure and chemical composition were characterized by means of EDAX, XRD, SEM, FT-IR spectroscopy, UV–vis spectroscopy, and photoluminescence. Finally, catalytic activity of the nanoparticles in a cycloaddition reaction was examined.

  4. Synthesis, structure characterization and catalytic activity of nickel tungstate nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Pourmortazavi, Seied Mahdi, E-mail: pourmortazavi@yahoo.com [Faculty of Material and Manufacturing Technologies, Malek Ashtar University of Technology, Tehran (Iran, Islamic Republic of); Rahimi-Nasrabadi, Mehdi, E-mail: rahiminasrabadi@gmail.com [Department of Chemistry, Imam Hossein University, Tehran (Iran, Islamic Republic of); Khalilian-Shalamzari, Morteza [Department of Chemistry, Imam Hossein University, Tehran (Iran, Islamic Republic of); Zahedi, Mir Mahdi; Hajimirsadeghi, Seiedeh Somayyeh [Islamic Azad University, Varamin Pishva Branch, Varamin (Iran, Islamic Republic of); Omrani, Ismail [Department of Chemistry, Imam Hossein University, Tehran (Iran, Islamic Republic of)

    2012-12-15

    Graphical abstract: NiWO{sub 4} nanoparticles were prepared via precipitation technique. Experimental parameters of procedure were optimized statistically. Highlights: Black-Right-Pointing-Pointer NiWO{sub 4} spherical nanoparticles were synthesized via direct precipitation method. Black-Right-Pointing-Pointer Taguchi robust design was used for optimization of synthesis reaction parameters. Black-Right-Pointing-Pointer Composition and structural properties of NiWO{sub 4} nanoparticles were characterized. Black-Right-Pointing-Pointer EDAX, XRD, SEM, FT-IR, UV-vis and photoluminescence techniques were employed. Black-Right-Pointing-Pointer Catalytic activity of the product in a cyclo-addition reaction was investigated. - Abstract: Taguchi robust design was applied to optimize experimental parameters for controllable, simple and fast synthesis of nickel tungstate nanoparticles. NiWO{sub 4} nanoparticles were synthesized by precipitation reaction involving addition of nickel ion solution to the tungstate aqueous reagent and then formation of nickel tungstate nucleolus which are insoluble in aqueous media. Effects of various parameters such as nickel and tungstate concentrations, flow rate of reagent addition and reactor temperature on diameter of synthesized nickel tungstate nanoparticles were investigated experimentally by the aid of orthogonal array design. The results for analysis of variance (ANOVA) showed that particle size of nickel tungstate can be effectively tuned by controlling significant variables involving nickel and tungstate concentrations and flow rate; while, temperature of the reactor has a no considerable effect on the size of NiWO{sub 4} particles. The ANOVA results proposed the optimum conditions for synthesis of nickel tungstate nanoparticles via this technique. Also, under optimum condition nanoparticles of NiWO{sub 4} were prepared and their structure and chemical composition were characterized by means of EDAX, XRD, SEM, FT-IR spectroscopy, UV

  5. Synthesis of samarium complexes with the derivative binder of Schiff Quinolinic base. Characterization and photophysical study

    International Nuclear Information System (INIS)

    Lucas H, J.

    2016-01-01

    In this work we determined the metal: binder stoichiometry of the species formed during the UV/Vis spectrophotometric titration of the derivative binder of Schiff quinolinic base, L1 with the samarium nitrate pentahydrate in methanol. Statistical analysis of the data allowed proposing the metal: binder stoichiometry for the synthesis of the complexes which was one mole of samarium salt by 2.5 moles of binder and thus favor the formation of complexes with 1M: 1L and 1M: 2L stoichiometries. They were synthesized in aqueous-organic medium (water-ethanol), isolated and purified two complexes with stoichiometry 1 Sm: 1 L1, complex 1 and 1 Sm: 2 L1, complex 2. The overall yield of the reaction was 76%. The characterization of the formed complexes was performed by visible ultraviolet spectrometry (UV/Vis), nuclear magnetic resonance, X-ray photoelectron spectroscopy (XP S), thermal gravimetric analysis with differential scanning calorimetry (TGA/DSC), and radial distribution function. These complexes were studied by fluorescence and emission phosphorescence at variable temperature. Spectroscopic techniques used in both solution and solid demonstrated the formation and stability of these complexes. In addition XP S indicated that in both complexes the samarium retains its oxidation state 3+. Luminescence studies indicated that there is intra-binding charge transfer which decreases the transfer of light energy from the binder to the samarium. Based on the experimental results, L1 binder molecules and complexes 1 and 2 were modeled that demonstrated the proposed Nc for each complex, as well as allowed to visualize the structural arrangement of the molecules, complexes and binder. (Author)

  6. Synthesis, characterization and magnetic properties of room-temperature nanofluid ferromagnetic graphite

    OpenAIRE

    Souza, N. S.; Sergeenkov, S.; Speglich, C.; Rivera, V. A. G.; Cardoso, C. A.; Pardo, H.; Mombru, A. W.; Rodrigues, A. D.; de Lima, O. F.; Araujo-Moreira, F. M.

    2009-01-01

    We report the chemical synthesis route, structural characterization, and physical properties of nanofluid magnetic graphite (NFMG) obtained from the previously synthesized bulk organic magnetic graphite (MG) by stabilizing the aqueous ferrofluid suspension with an addition of active cationic surfactant. The measured magnetization-field hysteresis curves along with the temperature dependence of magnetization confirmed room-temperature ferromagnetism in both MG and NFMG samples. (C) 2009 Americ...

  7. Electrochemical synthesis and characterization of copper (I oxide

    Directory of Open Access Journals (Sweden)

    Bugarinović Sanja J.

    2009-01-01

    Full Text Available The quest and need for clean and economical energy sources have increased interest in the development of thin film cells technologies. Electrochemical deposition is an attractive method for synthesis of thin films. It offers the advantages of low synthesis temperature, low cost and high purity. Copper (I oxide or cuprous oxide is an oxide semiconductor which is used as the anodic material in the form of thin film in lithium batteries and solar cells. The cathodic process of synthesis of cuprous oxide thin film is carried out in a potentiostatic mode from the organic electrolyte. The process parameters are chosen in that way to accomplish maximum difference between the potentials at which Cu2O and CuO are obtained. The electrochemical characterization was carried out by cyclic voltammetry. The electrodeposition techniques are particularly well suited for the deposition of single elements but it is also possible to carry out simultaneous depositions of several elements and syntheses of well-defined alternating layers of metals and oxides with thicknesses down to a few nm. Nanomaterials exhibit novel physical properties and play an important role in fundamental research. In addition, cuprous oxide is commonly used as a pigment, a fungicide, and an antifouling agent for marine paints. It is insoluble in water and organic solvents. This work presents the examinations of the influence of bath, temperature, pH and current density on the characteristics of electrochemically synthesized cuprous oxide. In the 'classic' process of synthesis, which is carried out under galvanostatic conditions on the anode, the grain size of the powder decreases with the increase in current density while the grain colour becomes lighter. The best commercial quality of the Cu2O (grain size, colour, content of choride was obtained at the temperature of 80°C, concentration of NaCl of 3 mol/dm3 and current density of 400 A/m2.

  8. SYNTHESIS, SPECTRAL CHARACTERIZATIONS AND ...

    African Journals Online (AJOL)

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    A series of 4-chloro-2-[(arylmethylidene)amino]phenols (1–11) including methoxy group ... The structures of the Schiff bases were characterized by FT-IR, .... The characteristic ν(C-H) modes of ring residues are observed at near 3050 cm–1.

  9. Synthesis and Characterization of Thermoelectric Oxides at Macro- and Nano-scales

    Science.gov (United States)

    Ma, Feiyue

    Thermoelectric materials can directly convert a temperature difference into electrical voltage and vice versa. Due to this unique property, thermoelectric materials are widely used in industry and scientific laboratories for temperature sensing and thermal management applications. Waste heat harvesting, another potential application of thermoelectric materials, has long been limited by the low conversion efficiency of the materials. Potential high temperature applications, such as power plant waste heat harvesting and combustion engine exhaust heat recovery, make thermoelectric oxides a very promising class of thermoelectric materials. In this thesis, the synthesis and characterization of thermoelectric oxide materials are explored. In the first part of this thesis, the measurement methodologies and instrumentation processes employed to investigate different thermoelectric properties, such as the Seebeck coefficient and carrier concentration at the bulk scale and the thermal conductivity at the nanoscale, are detailed. Existing scientific and engineering challenges associated with these measurements are also reviewed. To overcome such problems, original parts and methodologies have been designed. Three fully functional systems were ultimately developed for the characterization of macroscale thermoelectric properties as well as localized thermal conductivity. In the second part of the thesis, the synthesis of NaxCo 2O4, a thermoelectric oxide material, is discussed. Modification of both composition and structure were carried out so as to optimize the thermoelectric performance of NaxCo2O4. Nanostructuring methods, such as ball milling, electrospinning, auto-combustion synthesis, and core-shell structure fabrication, have been developed to refine the grain size of NaxCo2O4 in order to reduce its thermal conductivity. However, the structure of the nanostructured materials is very unstable at high temperature and limited improvement on thermoelectric performance is

  10. Synthesis of Fluorinated Amphiphilic Block Copolymers Based on PEGMA, HEMA, and MMA via ATRP and CuAAC Click Chemistry

    Directory of Open Access Journals (Sweden)

    Fatime Eren Erol

    2014-01-01

    Full Text Available Synthesis of fluorinated amphiphilic block copolymers via atom transfer radical polymerization (ATRP and Cu(I catalyzed Huisgen 1,3-dipolar cycloaddition (CuAAC was demonstrated. First, a PEGMA and MMA based block copolymer carrying multiple side-chain acetylene moieties on the hydrophobic segment for postfunctionalization was carried out. This involves the synthesis of a series of P(HEMA-co-MMA random copolymers to be employed as macroinitiators in the controlled synthesis of P(HEMA-co-MMA-block-PPEGMA block copolymers by using ATRP, followed by a modification step on the hydroxyl side groups of HEMA via Steglich esterification to afford propargyl side-functional polymer, alkyne-P(HEMA-co-MMA-block-PPEGMA. Finally, click coupling between side-chain acetylene functionalities and 2,3,4,5,6-pentafluorobenzyl azide yielded fluorinated amphiphilic block copolymers. The obtained polymers were structurally characterized by 1H-NMR, 19F-NMR, FT-IR, and GPC. Their thermal characterizations were performed using DSC and TGA.

  11. Electrochemical synthesis of nanosized TiO2 nanopowder involving choline chloride based ionic liquids

    International Nuclear Information System (INIS)

    Anicai, Liana; Petica, Aurora; Patroi, Delia; Marinescu, Virgil; Prioteasa, Paula; Costovici, Stefania

    2015-01-01

    Highlights: • TiO 2 nanopowder electrochemically prepared using choline chloride based ionic liquids. • The new proposed method allowed high anodic synthesis efficiencies of minimum 92%. • High surface area of the electrochemically synthesized titania nanopowders. • Enhanced photocatalytic activity. - Abstract: The paper presents some experimental results regarding the electrochemical synthesis of TiO 2 nanopowders through anodic dissolution of Ti metal in choline chloride based eutectic mixtures (DES). A detailed characterization of the obtained titania has been performed, using various techniques, including XRD, Raman spectroscopy, XPS, SEM associated with EDX analysis, BET and UV–vis diffuse reflectance spectra. The anodic behavior of Ti electrode in DES has been also investigated. The photoreactivity of the synthesized materials was evaluated for the degradation of Orange II dye under UV (λ = 365 nm) and visible light irradiation. An anodic synthesis efficiency of minimum 92% has been determined. The as-synthesized TiO 2 showed amorphous structure and a calcination post-treatment at temperatures between 400 and 600 °C yielded anatase. The anodically obtained nanocrystalline oxides have crystallite sizes of 8–18 nm, a high surface area and enhanced photocatalytic effect

  12. Synthesis and characterization of noble metal–titania core–shell nanostructures with tunable shell thickness

    Directory of Open Access Journals (Sweden)

    Bartosz Bartosewicz

    2017-10-01

    Full Text Available Core–shell nanostructures have found applications in many fields, including surface enhanced spectroscopy, catalysis and solar cells. Titania-coated noble metal nanoparticles, which combine the surface plasmon resonance properties of the core and the photoactivity of the shell, have great potential for these applications. However, the controllable synthesis of such nanostructures remains a challenge due to the high reactivity of titania precursors. Hence, a simple titania coating method that would allow better control over the shell formation is desired. A sol–gel based titania coating method, which allows control over the shell thickness, was developed and applied to the synthesis of Ag@TiO2 and Au@TiO2 with various shell thicknesses. The morphology of the synthesized structures was investigated using scanning electron microscopy (SEM. Their sizes and shell thicknesses were determined using tunable resistive pulse sensing (TRPS technique. The optical properties of the synthesized structures were characterized using UV–vis spectroscopy. Ag@TiO2 and Au@TiO2 structures with shell thickness in the range of ≈40–70 nm and 90 nm, for the Ag and Au nanostructures respectively, were prepared using a method we developed and adapted, consisting of a change in the titania precursor concentration. The synthesized nanostructures exhibited significant absorption in the UV–vis range. The TRPS technique was shown to be a very useful tool for the characterization of metal–metal oxide core–shell nanostructures.

  13. Synthesis and Characterization of High Aluminum Zeolite X from Technical Grade Materials

    Directory of Open Access Journals (Sweden)

    Seyed Kamal Masoudian

    2013-06-01

    Full Text Available Zeolites are widely used as ion exchangers, adsorbents, separation materials and catalyst due to their well-tailored and highly-reproducible structures; therefore, the synthesis of zeolite from low grade resources can be interested. In the present work, high aluminum zeolite X was prepared from mixing technical grade sodium aluminate and sodium silicate solutions at temperatures between 70°C and 100°C. The synthesized zeolite X was characterized by SEM and X-ray methods according to ASTM standard procedures. The results showed that aging of the synthesis medium at the room temperature considerably increased the selectivity of zeolite X formation. On the other hand, high temperature of reaction mixture during crystallization formed zeolite A in the product; therefore, it decreased the purity of zeolite X. In addition, it was found that increasing H2O/Na2O and decreasing Na2O/SiO2 molar ratios in the reaction mixture resulted product with higher purity. © 2013 BCREC UNDIP. All rights reservedReceived: 7th January 2013; Revised: 7th April 2013; Accepted: 19th April 2013[How to Cite: Masoudian, S. K., Sadighi, S., Abbasi, A. (2013. Synthesis and Characterization of High Alu-minum Zeolite X from Technical Grade Materials. Bulletin of Chemical Reaction Engineering & Catalysis, 8 (1: 54-60. (doi:10.9767/bcrec.8.1.4321.54-60][Permalink/DOI: http://dx.doi.org/10.9767/bcrec.8.1.4321.54-60] | View in  |

  14. Synthesis and characterization of functionalized methacrylates for coatings and biomedical applications

    Science.gov (United States)

    Shemper, Bianca Sadicoff

    The research presented in this dissertation involves the design of polymers for biomaterials and for coatings applications. The development of non-wettable, hard UV-curing, or reactive coatings is discussed. The biomaterials section involves the syntheses of linear and star-like polymers of the functionalized monomer poly(propylene glycol) monomethacrylate (PPGM) via atom transfer radical polymerization (ATRP) (Chapter II). Its copolymerization with a perfluoroalkyl ethyl methacrylate monomer (1H,1H,2H,2H-heptadecafluorodecyl methacrylate) and the syntheses of linear and star-like amphiphilic copolymers containing the fluorinated monomer and poly(ethyleneglycol) methyl ether methacrylate (MPEGMA) are discussed in Chapter III. The four-arm amphiphilic block copolymer obtained showed unique associative properties leading to micellization in selective solvents. Chapter IV includes research involving the design of films with low surface energy by incorporating fluorine into the polymer. The synthesis, characterization and polymerization of a perfluoroalkylether-substituted methacrylic acid (C8F7) are discussed, and the properties of coatings obtained after its photopolymerization on different substrates are evaluated to confirm formation of low-surface energy polymeric coatings. Subsequently, hard coatings based on methyl (alpha-hydroxymethyl)acrylate (MHMA) were prepared via photopolymerization using UV-light. Firstly, mechanistic investigations into the photopolymerization behavior of (alpha-hydroxymethyl)acrylates (RHMA's) are reported (Chapter V). RHMA derivatives were photopolymerized with various multifunctional acrylates and methacrylates and the effect of crosslinker type and degree of functionality on photopolymerization rates and conversions was investigated. Then, in Chapter VI the synthesis of a series of new crosslinkers is described and their photopolymerization kinetics was investigated in bulk. The effect of these novel crosslinkers on the

  15. Synthesis and characterization of boron nitrides nanotubes

    International Nuclear Information System (INIS)

    Ferreira, T.H.; Sousa, E.M.B.

    2010-01-01

    This paper presents a new synthesis for the production of boron nitride nanotubes (BNNT) from boron powder, ammonium nitrate and hematite tube furnace CVD method. The samples were subjected to some characterization techniques as infrared spectroscopy, thermal analysis, X-ray diffraction and scanning electron microscopy and transmission. By analyzing the results can explain the chemical reactions involved in the process and confirm the formation of BNNT with several layers and about 30 nanometers in diameter. Due to excellent mechanical properties and its chemical and thermal stability this material is promising for various applications. However, BNNT has received much less attention than carbon nanotubes, it is because of great difficulty to synthesize appreciable quantities from the techniques currently known, and this is one of the main reasons this work.(author)

  16. Controlling Magnetic and Ferroelectric Order Through Geometry: Synthesis, Ab Initio Theory, Characterization of New Multi-Ferric Fluoride Materials

    Energy Technology Data Exchange (ETDEWEB)

    Halasyamani, Shiv [Univ. of Houston, TX (United States); Fennie, Craig [Cornell Univ., Ithaca, NY (United States)

    2016-11-03

    We have focused on the synthesis, characterization, and ab initio theory on multi-functional mixed-metal fluorides. With funding from the DOE, we have successfully synthesized and characterized a variety of mixed metal fluoride materials.

  17. Enzymatic preparation and characterization of soybean lecithin-based emulsifiers

    Directory of Open Access Journals (Sweden)

    R. C. Reddy Jala

    2016-12-01

    Full Text Available Simple enzymatic methods were developed for the synthesis of lysolecithin, glycerolyzed lecithin and hydrolyzed lecithin. The products were characterized in terms of their acetone insoluble matter, hexane insoluble matter, moisture, phospholipid distribution and fatty acid composition. The HLB value ranges of different products with different acid values were detected. The efficiency of optimally hydrolyzed lecithin was examined at high calcium ion, low pH, and aqueous solutions and compared with commercially available standard lecithin-based emulsifiers. Overall, lysolecithin powder was proven to be the best emulsifier even at strong and medium acidic conditions.

  18. Synthesis and characterization of iron-cobalt (FeCo) alloy nanoparticles supported on carbon

    DEFF Research Database (Denmark)

    Koutsopoulos, Sotiris; Barfod, Rasmus; Eriksen, Kim Michael

    2017-01-01

    of the alloy nanoparticles differed depending on the preparation method. When the wet impregnation technique of acetate precursor salts of Fe and Co were used for the synthesis, the size of FeCo alloy nanoparticles was approximately 13 nm. FeCo alloy nanoparticles were characterized by crystallography (XRD...

  19. Synthesis, purification and physico-chemical characterization of the deuterized chloroform

    International Nuclear Information System (INIS)

    Mihaila, Vasile; Chiper, Diana

    1999-01-01

    This work refers to deuterized chloroform synthesis and purification methods. Three preparation methods of deuterized chloroform are presented. In the first method the direct chlorination of methane (CH 4 + 3Cl 2 ) in the presence of light and in an oxygen-free atmosphere results in CHCl 3 + 3HCl. The method's drawback is that the resulting product is impure, being obtained also secondary chlorinated compounds, such as CHCl, CH 2 Cl 2 and CCl 4 . The second method consists in chlorination of acetaldehyde or acetone, in basic catalysis and in halogen excess (α substitution with direct synthesis of trihalogen compound), followed by a haloform reaction (hydrolytic splitting) in the presence of chlorinated lime. This method makes use of decarbolyzing of trichlor acetate acid (as a sodium salt), what results in CL 3 CH + NaHCO 3 . This method is the most suitable for the deuterized chloroform synthesis, since the reaction takes place in absence of other hydrogen atoms (protons) and in deuterized water of 99.87% purity, according to the following reaction: Cl 3 C-COONa → (D 2 O) → Cl 2 CD + NaDCO 3 . Another advantage is that this method avoids the synthesis of secondary products, which could entail additional purifications (distillations, rectification, a.s.o.). The deuterized chloroform is separated from the deuterized sodium bicarbonate aqueous solution by washing with deuterized water, in a liquid to liquid separating funnel. After separation, deuterized chloroform is dried in nitrogen atmosphere. The characterization of the final product is carried out by nuclear magnetic resonance spectrometry. (authors)

  20. Synthesis and characterization of sulfonic acid membranes based on interpenetrating polymer networks for application in fuel cells; Sintese e caracterizacao de membranas sulfonadas baseadas em redes polimericas interpenetrantes para aplicacao em celulas a combustivel

    Energy Technology Data Exchange (ETDEWEB)

    Blanco, Lyzed Toloza; Loureiro, Felipe A.M.; Rocco, Ana Maria [Grupo de Materiais Condutores e Energia, Escola de Quimica, Universidade Federal do Rio de Janeiro (UFRJ), RJ (Brazil)], e-mail: amrocco@eq.ufrj.br; Pereira, Robson Pacheco [Instituto de Ciencias Exatas, Universidade Federal Fluminense (UFF), Volta Redonda, RJ (Brazil)

    2011-07-01

    In the present work, the synthesis and characterization of sulfonic membranes based on interpenetrating polymer networks (IPN). In order to obtain such systems, the diglycidyl ether of bisphenol A (DGEBA) was polymerized in presence of polyethyleneimine (PEI). These membranes were submitted to sulfonation reactions, originating IPN-SO{sub 3}H membranes. The characterization by FTIR evidenced the formation of a Semi-IPN structure, while sulfonation reactions resulted in systems containing -SO{sub 3}H groups covalently bonded to the chains. The membranes exhibited water retention up to 200 degree C, in a temperature range sufficient for application in PEMFC under hydration. (author)

  1. Chemical synthesis, characterization and evaluation of antimicrobial properties of Cu and its oxide nanoparticles

    CSIR Research Space (South Africa)

    Motlatle, Abesach M

    2016-10-01

    Full Text Available of Nanoparticle Research, vol. 18: DOI: 10.1007/s11051-016-3614-8 Chemical synthesis, characterization and evaluation of antimicrobial properties of Cu and its oxide nanoparticles Motlatle AM Kesevan Pillai S Scriba MR Ray SS ABSTRACT: Cu...

  2. Game-based verification and synthesis

    DEFF Research Database (Denmark)

    Vester, Steen

    and the environment behaves. Synthesis of strategies in games can thus be used for automatic generation of correct-by-construction programs from specifications. We consider verification and synthesis problems for several well-known game-based models. This includes both model-checking problems and satisfiability...... can be extended to solve finitely-branching turn-based games more efficiently. Further, the novel concept of winning cores in parity games is introduced. We use this to develop a new polynomial-time under-approximation algorithm for solving parity games. Experimental results show that this algorithm...... corresponds directly to a program for the corresponding entity of the system. A strategy for a player which ensures that the player wins no matter how the other players behave then corresponds to a program ensuring that the specification of the entity is satisfied no matter how the other entities...

  3. Synthesis and characterization of new polyamino-cyclodextrin materials.

    Science.gov (United States)

    Lo Meo, Paolo; D'Anna, Francesca; Gruttadauria, Michelangelo; Riela, Serena; Noto, Renato

    2012-01-10

    With the aim of the synthesis of chemically modified cyclodextrins bearing polyamine pendant groups, potentially useful as capping agents for the preparation of nanosized metal systems or as auxiliaries for gene transfection, the reaction between the heptakis-(6-iodo)-(6-deoxy)-β-cyclodextrin and various polyamines has been explored. This synthetic approach allows obtaining materials constituted by mixtures of cyclodextrins, having different degrees of substitution, which were satisfactorily characterized by means of various complementary techniques (ESI-MS, NMR, potentiometric titration). The products obtained were successfully subjected to preliminary tests for their binding abilities towards suitable organic guests and as capping agents for the preparation of stable silver nanoparticles. Copyright © 2011 Elsevier Ltd. All rights reserved.

  4. Synthesis and characterization of sugar based low molecular weight gelators and the preparation of chiral sulfinamides

    Science.gov (United States)

    Mangunuru, Hari Prasad Reddy

    Low molecular weight gelators (LMWGs) have received considerable attention in the field of chemistry from last few decades. These compounds form self-assembled fibrous networks like micelles, cylindrical, sheets, fibers, layers and so on. The fibrous network entraps the solvent and forms gel, because of the self-assembly phenomenon and their demonstrated potential uses in a variety of areas, ranging from environmental to medicinal applications. Sugars are good starting materials to synthesize the new class of LMWG's, because these are different from some expensive materials, these are natural products. We have synthesized and characterized the LMGS's based on D-glucose and D-glucosamine. D-glucosamine is the versatile starting material to make different peptoids and triazoles. Several series of compounds were synthesized using compounds 1-3 as starting material and studied the gelation behavior all the compounds. We have studied the self-assembling properties of a new class of tripeptoids, synthesized by one-pot Ugi reaction from simple starting materials. Among the focused library of tripeptoids synthesized, we found that several efficient low molecular weight organogelators were obtained for aqueous DMSO and ethanol mixtures. We have also synthesized and characterized a series of monosaccharide triazole derivatives. These compounds were synthesized from N-acetyl glucosamine and D-glucose via a Cu(I) catalyzed azide/alkyne cycloaddition reaction (CuAAc). The compounds have been screened for their gelation properties and several efficient low molecular weight organo/hydro gelators were obtained, among these compounds, five per-acetyl glucosamine derivatives and one peracetyl glucose derivative were able to form gels in water. These new molecules are expected to be useful in drug delivery and tissue engineering.*. Asymmetric synthesis of chiral amines is a challenging in synthetic organic chemistry. The development of new catalysts for asymmetric organic

  5. Controlled synthesis of phase-pure zeolitic imidazolate framework Co-ZIF-9

    NARCIS (Netherlands)

    Öztürk, Z.; Hofmann, J.P.; Lutz, M.; Mazaj, M.; Zabukovec Logar, N.; Weckhuysen, B.M.

    2015-01-01

    The synthesis of phase-pure Co-ZIF-9, an important cobalt-based zeolitic imidazolate framework, could be achieved by modification of the reported synthesis procedure through pH adjustment of the starting synthesis mixture. The phase-pure Co-ZIF-9 material obtained has been characterized by a

  6. Nano-ilmenite FeTiO3 : synthesis and characterization

    OpenAIRE

    Raghavender, A. T.; Hoa Hong, Nguyen; Lee, Kyu Joon; Jung, Myung-Hwa; Skoko, Z.; Vasilevskiy, Mikhail; Cerqueira, M. F.; Samantilleke, A. P.

    2013-01-01

    In general, ilmenite FeTiO3 is synthesized by solid-state reaction at very high pressure and high temperature. Synthesis of FeTiO3 is not an easy task as the Fe2+ ions are not stable. Therefore, it is really challenging to prepare this material. In this work nano-ilmenite FeTiO3 was synthesized by the sol-gel method. Structural, optical and magnetic characterizations were performed. The bandgap of FeTiO3 was determined to be 2.8 eV showing FeTiO3 as suitable wide bandgap material for technolo...

  7. High pressure and microwave based synthesis of transition metal pnictides

    Energy Technology Data Exchange (ETDEWEB)

    Pobel, Roman Rupert

    2016-04-11

    The goal of this thesis was to explore the possibilities of synthetic methods that are not very common in current transition metal pnictide research. The substitution of the Ca-site in CaFe{sub 2}As{sub 2} with rare earth elements such as Pr the has been reported to induce superconductivity. However, some inconsistencies in the data suggested a non-intrinsic origin of the observed diamagnetic signal. Furthermore a solubility limit of 13% was found when prepared in an electrical furnace thus leaving a huge part of the physical phase diagram inaccessible. A high pressure/high temperature synthesis was developed to allow access to the whole doping range and an in-depth characterization of this compound was carried out. During the experiments concerning the high pressure synthesis of Ca{sub 1-x}Pr{sub x}Fe{sub 2}As{sub 2} the new ternary iron arsenide CaFe{sub 5}As{sub 3} was identified and classified as a member of the Ca{sub n(n+1)/2}(Fe{sub 1-x}M{sub x}){sub (2+3n)}M'{sub n(n-1)/2}As{sub (n+1)(n+2)/2} (n = 1-3; M =Nb, Pd, Pt; M' = □, Pd, Pt) family. The complete solid solution Ca{sub 1-x}Pr{sub x}Fe{sub 5}As{sub 3} (O ≤ x ≤ 1) was prepared and physically characterized. Furthermore, several useful techniques were developed to aid in future high pressure based investigations of transition metal pnictides. The second part of this thesis concerns a completely different, but equally promising synthetic approach. Microwave based synthesis is a well-established technique in many solution based fields, such as organic, medicinal or nano chemistry. For solid state and materials research several parameters and particularities have to be considered. But when successful, it allows for the reduction of reaction time by several orders of magnitude. It has very rarely been applied in the preparation of pnictides and on1y once in the context of pnictide superconductor research. The possibilities of this method were explored and employed in the preparation of several

  8. Synthesis and characterization of N-t-BOC protected pyrrole-sulfur oligomers and polymers

    NARCIS (Netherlands)

    Groenendaal, L.; Pieterse, K.; Vekemans, J.A.J.M.; Meijer, E.W.

    1997-01-01

    The synthesis and characterization of a new class of pyrrole-sulfur compounds is described. These compounds are designed to be precursors for an organic analogue of poly(sulfur nitride). Poly(N-t-BOC-2.5-pyrrolyl sulfide) was prepared from N-t-BOC-2,5-dibromopyrrole by first lithiating this compound

  9. Synthesis and characterization of carbon nanotube from coconut shells activated carbon

    Science.gov (United States)

    Melati, A.; Hidayati, E.

    2016-03-01

    Carbon nanotubes (CNTs) have been explored in almost every single cancer treatment modality, including drug delivery, lymphatic targeted chemotherapy, photodynamic therapy, and gene therapy. They are considered as one of the most promising nanomaterial with the capability of both detecting the cancerous cells and delivering drugs or small therapeutic molecules to the cells. CNTs have unique physical and chemical properties such as high aspect ratio, ultralight weight, high mechanical strength, high electrical conductivity, and high thermal conductivity. Coconut Shell was researched as active carbon source on 500 - 600°C. These activated carbon was synthesized becomes carbon nanotube and have been proposed as a promising tool for detecting the expression of indicative biological molecules at early stage of cancer. Clinically, biomarkers cancer can be detected by CNT Biosensor. We are using pyrolysis methods combined with CVD process or Wet Chemical Process on 600°C. Our team has successfully obtained high purity, and aligned MWCNT (Multi Wall Nanotube) bundles on synthesis CNT based on coconut shells raw materials. CNTs can be used to cross the mammalian cell membrane by endocytosis or other mechanisms. SEM characterization of these materials have 179 nm bundles on phase 83° and their materials compound known by using FTIR characterization.

  10. Synthesis and characterization of sulfur-functionalized silica nanocapsules as mercury adsorbents

    Science.gov (United States)

    Palaniappan, Thenappan; Saman, Norasikin; Mat, Hanapi; Johari, Khairiraihanna

    2017-12-01

    Sulfur functionalized silica nanocapsules (S-SiNC) was successfully synthesized and characterized as a potential adsorbent for industrial applications. The synthesis of S-SiNC was carried out using the mircoemulsion templating method using cetyltrimethylammonium bromide (CTAB) as cationic surfactant, toluene as co-solvent, ammonia solution as catalyst, and tetraethylorthosilicate (TEOS) as the silica base. The S-SiNC adsorbent was characterized using Transmission Electron Microscope, Fourier Transformed Infra Red spectroscopy and nitrogen adsorption/desorption analysis. The physical and chemical properties of the SiNC changed as a result of the functionalization, hence affecting the extent of Hg(II) adsorption. The S-SiNCs were also tested in mercury ion [Hg(II)] adsorption via batch adsorption process with variation in initial Hg (II) concentration. It was found that there is a significant improvement in Hg(II) adsorption performance after being functionalized with elemental sulfur. The highest Hg(II) adsorption capacity was obtained for S-SiNC (107.875 mg/g), which significantly outperformed the blank SiNC. The experimental data obtained was found to be fitting well to the Langmuir isotherm model (R2= 0.979) compared to Freundlich isotherm model. Thus, the results demonstrated the potential application of sulfur functionalized silica nanocapsules as adsorbent in industrial applications.

  11. Synthesis, characterization, bioactivity and potential application of phenolic acid grafted chitosan: A review.

    Science.gov (United States)

    Liu, Jun; Pu, Huimin; Liu, Shuang; Kan, Juan; Jin, Changhai

    2017-10-15

    In recent years, increasing attention has been paid to the grafting of phenolic acid onto chitosan in order to enhance the bioactivity and widen the application of chitosan. Here, we present a comprehensive overview on the recent advances of phenolic acid grafted chitosan (phenolic acid-g-chitosan) in many aspects, including the synthetic method, structural characterization, biological activity, physicochemical property and potential application. In general, four kinds of techniques including carbodiimide based coupling, enzyme catalyzed grafting, free radical mediated grafting and electrochemical methods are frequently used for the synthesis of phenolic acid-g-chitosan. The structural characterization of phenolic acid-g-chitosan can be determined by several instrumental methods. The physicochemical properties of chitosan are greatly altered after grafting. As compared with chitosan, phenolic acid-g-chitosan exhibits enhanced antioxidant, antimicrobial, antitumor, anti-allergic, anti-inflammatory, anti-diabetic and acetylcholinesterase inhibitory activities. Notably, phenolic acid-g-chitosan shows potential applications in many fields as coating agent, packing material, encapsulation agent and bioadsorbent. Copyright © 2017 Elsevier Ltd. All rights reserved.

  12. Synthesis and characterization of ceramic pigments based on oxides of chromium and iron, on TiO2

    International Nuclear Information System (INIS)

    Silva, E.M. da; Galvao, S.B.; Paskocimas, C.A.

    2011-01-01

    This work used oxides of chromium and iron, as precursors of the synthesis of ceramic pigments. The synthesis is based on the dissolution of citric acid as a complexing agent, addition of metal oxides, such as ion chromophores; polymerization with ethylene glycol and doping with titanium oxide. Passing through pre-calcination, breakdown, calcination at different temperatures (900 and 1100 ° C), resulting in pigments: green for pigment chrome deposited on TiO 2 and orange for iron on TiO 2 . Noticing an increase in the opacity with increasing temperature. The thermal analysis (TG and DTA), evaluated their thermal behavior, the XRD revealed the formation of crystalline phases as Iron Titanate and Chrome Titanate; SEM showed the formation of hexagonal particles for both oxides. Thus, the synthesized oxides were within the requirements for application as ceramic pigments. (author)

  13. Straightforward high-pressure synthesis and characterization of indium-based thiospinels: photocatalytic potential for hydrogen production

    Energy Technology Data Exchange (ETDEWEB)

    Falcon, Horacio [Instituto de Ciencia de Materiales de Madrid, CSIC, Cantoblanco (Spain); NANOTEC (Centro de Investigacion en Nanociencia y Nanotecnologia), Universidad Tecnologica Nacional-Facultad Regional Cordoba, Cordoba (Argentina); Tartaj, Pedro; Alonso, Jose Antonio [Instituto de Ciencia de Materiales de Madrid, CSIC, Cantoblanco (Spain); Vaquero, Fernando; Navarro, Rufino M.; Fierro, Jose Luis G. [Instituto de Catalisis y Petroleoquimica, CSIC, Cantoblanco, Madrid (Spain); Bolletta, Juan P.; Paoli, Juan M. de; Carbonio, Raul E. [INFIQC - CONICET, Departamento de Fisicoquimica, Facultad de Ciencias Quimicas, Universidad Nacional de Cordoba (Argentina); Fernandez-Diaz, Maria Teresa [Institut Laue Langevin, Grenoble (France)

    2016-04-15

    Ternary chalcogenides (AB{sub 2}X{sub 4}) based on the spinel structure are gaining a great deal of attention because of the possibility of tuning their magnetic and optoelectronic properties not only by changing chemical composition but also by altering their degree of inversion. Here we report a rapid high-pressure synthetic method for the synthesis of MIn{sub 2}S{sub 4} powders starting from commercially available solid sulfides. We prove the versatility of our method by reporting the synthesis of six members of the MIn{sub 2}S{sub 4} family (M = Mn, Fe, Co, Ni, Zn, and Cd) under high-pressure conditions (3.5 GPa); these compounds show complete to moderate degrees of inversion. Furthermore, this family covers a spectral region that includes visible band gaps. Interestingly, the structural refinement carried out by X-ray and neutron diffraction allows one to establish positive correlations between the gap and different parameters, including the degree of inversion. Finally, as a proof-of-concept, these ternary chalcogenides show moderate photocatalytic hydrogen production from aqueous solutions. (Copyright copyright 2016 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  14. Synthesis and characterization of lanthanide-based luminescent nanoparticles: toward new bio-labels

    International Nuclear Information System (INIS)

    Lechevallier, Severine

    2010-01-01

    This work deals with the development of luminescent nanoparticles (NPs) suitable as bio-labels. Inorganic NPs have been synthesized, in which luminescent ion (Eu 3+ in most of cases) is substituting ions of the oxide host matrix. NPs of Ln(OH)CO 3 :Eu 3+ (Ln = Y or Gd), Ln 2 O 3 :Eu 3+ , Ln 2 O 2 S:Eu 3+ and SiO 2 :Eu 3+ have been characterized by the way of TGA, WAXS-XRD, TEM, IR and photoluminescence (PL) techniques. The controlled precipitation using urea as precipitating agent is the way chosen and optimized to obtain spherical and monodispersed in size (150±15 nm) NPs. These particles of amorphous lanthanide hydroxycarbonate can directly be used as luminescent bio-labels or after their conversion in oxide or oxi-sulfide. For the silica particles, the synthesis by aerosol pyrolysis has been used. The obtained particles are spherical with a main diameter of 350 nm. In a second step, the surface of the inorganic NPs has been modified, in order to graft amino-reactive functions. Several modification ways have been explored: with APTES (aminopropyltriethoxysilane), with TEOS (tetra-ethoxysilane) and then APTES, or with a TEOS/APTES mixture. The same characterizations techniques have been applied to the modified particles, and chemical analysis, solid state NMR and XPS. DLS and ζ-potential of the NPs dispersed in water have also been measured. These analyses have been completed by the evaluation of the number of accessible amine functions by coupling with FITC (fluorescein isothiocyanate). The direct modification of oxides (Y 2 O 3 or Gd 2 O 3 ) with APTES is the best way, and an homogenous layer of 1 nm with a high number of accessible amine can be graft. Finally, to move toward luminescent bio-labelling in biological medium, the luminescence of the NPs has been observed and analyzed using: - A spectro-fluorimeter, after their dispersion in water; - A fluorescence microscope, on glass slides, under broad band excitation; - A confocal microscope, under laser

  15. Synthesis and Characterization of Soy-Based Polyurethane Foam with Utilization of Ethylene Glycol in Polyol

    Directory of Open Access Journals (Sweden)

    Flora Elvistia Firdaus

    2014-08-01

    Full Text Available The use of vegetable oils on replacing petroleum has attracted attention of many researchers. The chemical structure of vegetable oils are different from petrochemicals, so the structure of soybean oil has to be chemicallymodified through its unsaturated fatty acid chain in triglyceride. Atwo step process was conducted for the preparationof soy-polyol in designated temperatures; 50 °C, 60 °C, and 70 °C. Ethylene glycol (EG as co-reagent was taking part in soy-polyol synthesis, and the soy-polyol was used as a sole polyol for polyurethane synthesis. Referred to the previous study, the existence of EG in polyurethane synthesis can improved physical properties of polyurethane foam. The aim of this research is using soy-derived polyol for petro-polyol replacement aligned with drop-off of petro-derived reagent; EG. One step process was applied for the foam synthesis.The ingredients for foam synthesis; soy-polyol, Toluene diisocyanate (TDI: a mixture of 2.4 and 2.6 isomers in ratio of 80:20 (TDI T-80, surfactant, and distilled water. The synergize of stoichiometry ratio of co-reagent EG to soy-epoxide with best temperature, with the absence of EG in polyurethane formula can produce an ultimate property of polyurethane foam. 

  16. Synthesis of Zinc Diethyldithiocarbamate (ZDEC) and Structure Characterization using Decoupling 1H NMR

    International Nuclear Information System (INIS)

    Sujarit, Jenjira; Phutdhawong, Weerachai

    2003-10-01

    A synthesis of zinc diethyldithiocarbamate (ZDEC) has been studied. The optimization mole ratio of the synthetic process was 2: 2: 2: 1 of diethylamine, carbondisulfide, sodium hydroxide, and zinc chloride. Characterization was carried out mainly by analyzing its spectroscopic properties especially decoupling 1 H NMR technique. ZDEC was obtained in 48.5% yield

  17. Design, synthesis, and characterization of novel fine-particle, unsupported catalysts for coal liquefaction

    Energy Technology Data Exchange (ETDEWEB)

    Klein, M.T.

    1991-12-30

    The purpose of this work is to investigate the kinetics-assisted design, synthesis and characterization of fme-pardcle, unsupported catalysts for coal liquefaction. The goal is to develop a fundamental understanding of coal catalysis and catalysts that will, in turn, allow for the specification of a novel optimal catalyst for coal liquefaction.

  18. Synthesis and Complete Antimicrobial Characterization of CEOBACTER, an Ag-Based Nanocomposite.

    Directory of Open Access Journals (Sweden)

    O E Jaime-Acuña

    Full Text Available The antimicrobial activity of silver nanoparticles (AgNPs is currently used as an alternative disinfectant with diverse applications, ranging from decontamination of aquatic environments to disinfection of medical devices and instrumentation. However, incorporation of AgNPs to the environment causes collateral damage that should be avoided. In this work, a novel Ag-based nanocomposite (CEOBACTER was successfully synthetized. It showed excellent antimicrobial properties without the spread of AgNPs into the environment. The complete CEOBACTER antimicrobial characterization protocol is presented herein. It is straightforward and reproducible and could be considered for the systematic characterization of antimicrobial nanomaterials. CEOBACTER showed minimal bactericidal concentration of 3 μg/ml, bactericidal action time of 2 hours and re-use capacity of at least five times against E. coli cultures. The bactericidal mechanism is the release of Ag ions. CEOBACTER displays potent bactericidal properties, long lifetime, high stability and re-use capacity, and it does not dissolve in the solution. These characteristics point to its potential use as a bactericidal agent for decontamination of aqueous environments.

  19. Synthesis and Complete Antimicrobial Characterization of CEOBACTER, an Ag-Based Nanocomposite

    Science.gov (United States)

    Vasquez-Peña, M.; Raymond-Herrera, O.; Villavicencio-García, H.; Petranovskii, V.; Vazquez-Duhalt, R.; Huerta-Saquero, A.

    2016-01-01

    The antimicrobial activity of silver nanoparticles (AgNPs) is currently used as an alternative disinfectant with diverse applications, ranging from decontamination of aquatic environments to disinfection of medical devices and instrumentation. However, incorporation of AgNPs to the environment causes collateral damage that should be avoided. In this work, a novel Ag-based nanocomposite (CEOBACTER) was successfully synthetized. It showed excellent antimicrobial properties without the spread of AgNPs into the environment. The complete CEOBACTER antimicrobial characterization protocol is presented herein. It is straightforward and reproducible and could be considered for the systematic characterization of antimicrobial nanomaterials. CEOBACTER showed minimal bactericidal concentration of 3 μg/ml, bactericidal action time of 2 hours and re-use capacity of at least five times against E. coli cultures. The bactericidal mechanism is the release of Ag ions. CEOBACTER displays potent bactericidal properties, long lifetime, high stability and re-use capacity, and it does not dissolve in the solution. These characteristics point to its potential use as a bactericidal agent for decontamination of aqueous environments. PMID:27824932

  20. PAMAM dendrimer-coated iron oxide nanoparticles: synthesis and characterization of different generations

    International Nuclear Information System (INIS)

    Khodadust, Rouhollah; Unsoy, Gozde; Yalcın, Serap; Gunduz, Gungor; Gunduz, Ufuk

    2013-01-01

    This study focuses on the synthesis and characterization of different generations (G 0 –G 7 ) of polyamidoamine (PAMAM) dendrimer-coated magnetic nanoparticles (DcMNPs). In this study, superparamagnetic iron oxide nanoparticles were synthesized by co-precipitation method. The synthesized nanoparticles were modified with aminopropyltrimethoxysilane for dendrimer coating. Aminosilane-modified MNPs were coated with PAMAM dendrimer. The characterization of synthesized nanoparticles was performed by X-ray diffraction, X-ray photoelectron spectroscopy (XPS), Fourier transform infrared spectroscopy (FTIR), transmission electron microscopy (TEM), dynamic light scattering, and vibrating sample magnetometry (VSM) analyses. TEM images demonstrated that the DcMNPs have monodisperse size distribution with an average particle diameter of 16 ± 5 nm. DcMNPs were found to be superparamagnetic through VSM analysis. The synthesis, aminosilane modification, and dendrimer coating of iron oxide nanoparticles were validated by FTIR and XPS analyses. Cellular internalization of nanoparticles was studied by inverted light scattering microscopy, and cytotoxicity was determined by XTT analysis. Results demonstrated that the synthesized DcMNPs, with their functional groups, symmetry perfection, size distribution, improved magnetic properties, and nontoxic characteristics could be suitable nanocarriers for targeted cancer therapy upon loading with various anticancer agents.

  1. Droplet-based microfluidic method for synthesis of microparticles

    CSIR Research Space (South Africa)

    Mbanjwa, MB

    2012-10-01

    Full Text Available Droplet-based microfluidics has, in recent years, received increased attention as an important tool for performing numerous methods in modern day chemistry and biology such as the synthesis of hydrogel microparticles. Hydrogels have been used in many..., in recent years, received increased attention as an important tool for performing numerous methods in modern day chemistry and biology, such as synthesis of hydrogel microparticles. CONCLUSION AND OUTLOOK The droplet-based microfluidic method offers...

  2. Electrochemical synthesis of nanosized TiO{sub 2} nanopowder involving choline chloride based ionic liquids

    Energy Technology Data Exchange (ETDEWEB)

    Anicai, Liana, E-mail: lanicai@itcnet.ro [POLITEHNICA University of Bucharest, Center of Surface Science and Nanotechnology, Splaiul Independentei 313, Bucharest, 060042 (Romania); Petica, Aurora [Leather and Footwear Research Institute (ICPI), Ion Minulescu 93, Bucharest, 031215 (Romania); Patroi, Delia; Marinescu, Virgil; Prioteasa, Paula [INCDIE ICPE-Advanced Research, Splaiul Unirii 313, Bucharest (Romania); Costovici, Stefania [POLITEHNICA University of Bucharest, Center of Surface Science and Nanotechnology, Splaiul Independentei 313, Bucharest, 060042 (Romania)

    2015-09-15

    Highlights: • TiO{sub 2} nanopowder electrochemically prepared using choline chloride based ionic liquids. • The new proposed method allowed high anodic synthesis efficiencies of minimum 92%. • High surface area of the electrochemically synthesized titania nanopowders. • Enhanced photocatalytic activity. - Abstract: The paper presents some experimental results regarding the electrochemical synthesis of TiO{sub 2} nanopowders through anodic dissolution of Ti metal in choline chloride based eutectic mixtures (DES). A detailed characterization of the obtained titania has been performed, using various techniques, including XRD, Raman spectroscopy, XPS, SEM associated with EDX analysis, BET and UV–vis diffuse reflectance spectra. The anodic behavior of Ti electrode in DES has been also investigated. The photoreactivity of the synthesized materials was evaluated for the degradation of Orange II dye under UV (λ = 365 nm) and visible light irradiation. An anodic synthesis efficiency of minimum 92% has been determined. The as-synthesized TiO{sub 2} showed amorphous structure and a calcination post-treatment at temperatures between 400 and 600 °C yielded anatase. The anodically obtained nanocrystalline oxides have crystallite sizes of 8–18 nm, a high surface area and enhanced photocatalytic effect.

  3. Synthesis and characterization of ruthenium-decorated nanoporous platinum materials

    International Nuclear Information System (INIS)

    Peng Xinsheng; Koczkur, Kallum; Chen, Aicheng

    2007-01-01

    We report on the synthesis of novel three-dimensional nanoporous Pt-Ru bimetallic networks by decorating nanoporous Pt networks with Ru using a hydrothermally assisted precipitating process. Scanning electron microscopy (SEM) and energy dispersive x-ray spectroscopy (EDS) were used to characterize the morphology and the composition of the nanoporous Pt-Ru networks formed. X-ray diffraction analysis confirmed that, after protected annealing treatment, Pt-Ru bimetallic material was formed. The electrocatalytic activity of the synthesized nanoporous Pt-Ru networks was characterized using electrochemical oxidation of methanol as a probe. The electrocatalytic activity of the nanoporous Pt networks significantly increases with the increments of decorated Ru and reaches the highest value with 41% of Ru. The peak current of methanol oxidation on the nanoporous Pt-Ru(41%) bimetallic networks is over 180% higher than that on the nanoporous Pt networks without Ru decoration. This is very desirable for fuel cell development and electrochemical sensor design

  4. Synthesis and characterization of cobalt sulfide nanoparticles by sonochemical method

    Science.gov (United States)

    Muradov, Mustafa B.; Balayeva, Ofeliya O.; Azizov, Abdulsaid A.; Maharramov, Abel M.; Qahramanli, Lala R.; Eyvazova, Goncha M.; Aghamaliyev, Zohrab A.

    2018-03-01

    Convenient and environmentally friendly synthesis of Co9S8/PVA, CoxSy/EG and CoxSy/3-MPA nanocomposites were carried out in the presence of ultrasonic irradiation by the liquid phase synthesis of the sonochemical method. For the synthesis, cobalt acetate tetrahydrate [Co(CH3COO)2·4H2O] and sodium sulfide (Na2S·9H2O) were used as a cobalt and sulfur precursor, respectively. Polyvinyl alcohol (PVA), ethylene glycol (EG) and 3-mercaptopropionic acid (3-MPA) were used as a capping agent and surfactant. The structural, optical properties and morphology of nanocomposites were characterized using X-ray diffractometer (XRD), Ultraviolet/Visible Spectroscopy (UV-Vis), Fourier-transform infrared spectroscopy (FTIR) and scanning electron microscopy (SEM). The optical band gap of Co9S8/PVA is 1.81 eV and for CoxSy/EG is 2.42 eV, where the direct band gap of bulk cobalt sulfide is (0.78-0.9 eV). The wide band gap indicates that synthesised nanocomposites can be used in the fabrication of optical and photonic devices. The growth mechanisms of the Co9S8, CoS2 and Co3S4 nanoparticles were discussed by the reactions. The effects of sonication time and annealing temperature on the properties of the nanoparticles have been studied in detail.

  5. Synthesis and Physicochemical Characterization of Mesoporous SiO2 Nanoparticles

    Directory of Open Access Journals (Sweden)

    Dharani Das

    2014-01-01

    Full Text Available There exists a knowledge gap in understanding potential toxicity of mesoporous silica nanoparticles. A critical step in assessing toxicity of these particles is to have a wide size range with different chemistries and physicochemical properties. There are several challenges when synthesizing mesoporous silica nanoparticles over a wide range of sizes including (1 nonuniform synthesis protocols using the same starting materials, (2 the low material yield in a single batch synthesis (especially for particles below 60–70 nm, and (3 morphological instability during surfactant removal process and surface modifications. In this study, we synthesized a library of mesoporous silica nanoparticles with approximate particle sizes of 25, 70, 100, 170, and 600 nm. Surfaces of the silica nanoparticles were modified with hydrophilic-CH2–(CH22–COOH and relatively hydrophobic-CH2–(CH210–COOH functional groups. All silica nanoparticles were analysed for morphology, surface functionality, surface area/pore volume, surface organic content, and dispersion characteristics in liquid media. Our analysis revealed the synthesis of a spectrum of monodisperse bare and surface modified mesoporous silica nanoparticles with a narrow particle size distribution and devoid of cocontaminants critical for toxicity studies. Complete physicochemical characterization of these synthetic mesoporous silica nanoparticles will permit systematic toxicology studies for investigation of structure-activity relationships.

  6. Eco-friendly green synthesis of silver nanoparticles using salmalia malabarica: synthesis, characterization, antimicrobial, and catalytic activity studies

    Science.gov (United States)

    Murali Krishna, I.; Bhagavanth Reddy, G.; Veerabhadram, G.; Madhusudhan, A.

    2016-06-01

    An economically viable and "green" process has been developed for the synthesis of silver nanoparticles (AgNPs) with an average size of 7 nm using non-toxic and renewable salmalia malabarica gum (SMG) as reducing and capping agent without using any chemical reducing agent. The effect of various parameters such as concentration of SMG and silver nitrate and reaction time for the synthesis of AgNPs was studied. The synthesized AgNPs are systematically characterized by UV/Vis spectroscopy, Fourier transform infrared spectroscopy, X-ray diffraction and Transmission electron microscopy. The resultant SMG-capped AgNPs are highly stable and had significant antibacterial action on both Escherichia coli ( E. coli) and Staphylococcus aureus ( S. aureus). The catalytic action of the SMG-capped AgNPs to initiate the reduction of 4-nitrophenol (4-NP) in the presence of NaBH4 has also been reported. The kinetics of the reaction was found to be of pseudo-first-order with respect to the 4-NP.

  7. Synthesis and characterization of Ag nanowires: Improved performance in dye sensitized solar cells

    Directory of Open Access Journals (Sweden)

    Safia A. Kazmi

    2016-09-01

    Full Text Available Development of highly efficient dye-sensitized solar cells (DSSCs with good photovoltaic parameters is an active research area of current global interest. Recently, one dimensional nanomaterial, such as nanorods and nanotubes has replaced the nanoparticles used in DSSCs anode because of their ability to improve the electron transport leading to enhanced electron collection efficiency. In the present work, rapid synthesis of silver nanowires (AgNWs was done. The XRD characterization was performed to confirm the formation and size of synthesized AgNWs. It was observed that FWHM of the diffraction peaks was increased with AgNWs concentration in TiO2. The synthesized TiO2AgNWs nanocomposite was used as the photo anode of Dye sensitized solar cell. The I–V characteristics of the solar cell were drawn using standard conditions. It was observed that TiO2AgNWs based solar cells have significantly increased photocurrent density resulting in improved conversion efficiency as compared to pure TiO2 based DSSC.

  8. Synthesis and characterization of polyaniline–Fe@C magnetic nanocomposite powder

    Energy Technology Data Exchange (ETDEWEB)

    Fleaca, C.T., E-mail: claudiufleaca@yahoo.com [National Institute for Lasers, Plasma and Radiation Physics (NILPRP), Atomistilor 409, R-077125 Magurele (Romania); “Politehnica” University of Bucharest, Faculty of Applied Sciences, Physics Department, Independentei 313, Bucharest (Romania); Dumitrache, F. [National Institute for Lasers, Plasma and Radiation Physics (NILPRP), Atomistilor 409, R-077125 Magurele (Romania); “Politehnica” University of Bucharest, Faculty of Applied Sciences, Physics Department, Independentei 313, Bucharest (Romania); Morjan, I.; Niculescu, A.-M.; Sandu, I. [National Institute for Lasers, Plasma and Radiation Physics (NILPRP), Atomistilor 409, R-077125 Magurele (Romania); Ilie, A. [National Institute for Lasers, Plasma and Radiation Physics (NILPRP), Atomistilor 409, R-077125 Magurele (Romania); University of Bucharest, Physics Faculty, Atomistilor 405, Magurele (Romania); Stamatin, I.; Iordache, A. [3NanoSAE Research Center, University of Bucharest, Atomistilor 405, Magurele (Romania); Vasile, E. [“Politehnica” University of Bucharest, Faculty of Applied Chemistry and Materials Science, Gh. Polizu. 1-7, Bucharest (Romania); Prodan, G. [“Ovidius” University, Nanotechnology and Alternative Energy Sources Institute, Mamaia 124, Constanta (Romania)

    2016-06-30

    Highlights: • Carbon-encapsulated Fe–Fe{sub x}C nanoparticles were synthesized by laser pyrolysis. • Fe–C@PANI was obtained by redox polymerization in aqueous acid suspension. • The composite show low coercivity and 6 emu/g saturation magnetization. • Electric and redox behavior of Fe–C@PANI is similar with those of pure PANI. - Abstract: We report the synthesis of novel magnetic nanocomposite based on polyaniline (PANI) matrix and Fe–C nanoparticles. These hydrophobic Fe–Fe{sub x}C@C nanoparticles (having diameters under 20 nm) were synthesized by laser pyrolysis from Fe(CO){sub 5} and C{sub 2}H{sub 4}/H{sub 2} and dispersed in water using sodium carboxymethylcellulose, followed by the PANI coating using ultrasonication-assisted oxidative polymerization of aniline hydrochloride. The structure of the resulted composite was characterized by Transmission Electron Microscopy, X-ray diffraction and also by Raman and Infrared spectroscopy. The composite powder shows ferromagnetic behavior with low coercivity and 6.4 emu/g saturation magnetization, having also electric and electrochemical behavior similar with pure PANI reference.

  9. Synthesis and Characterization of C-Cinnamal Calix [4] Resorsinarena from Cinnamon Oil Waste West Sumatra

    Science.gov (United States)

    Etika, S. B.; Nasra, E.; Rilaztika, I.

    2018-04-01

    Synthesis and characterization of compound C-Cinnamal Calix [4] Resorsinarena (CCCR) of cinnamon oil waste have been done. This study was aimed to synthesis and characterize C-Cinnamal Calix [4] Resorsinarena from cinnamaldehyde violated cinnamon oil waste. C-Cinnamal Calix [4] Resorsinarena was synthesized by electrophilic substitution reaction of cinnamaldehyde isolated by the acid and resorcinol at 77oC temperature for 2 hour. The data analysis spectrum UV-VIS and FT-IR showed that the compound isolated cinnamaldehyde same as pure cinnamaldehyde compound. The characterization of C-Cinnamal Calix [4] Resorsinarena in the form of reddish-colored solids with melting point 3580C by using UV-VIS showed the presence of double bond, FT-IR showed the absorption at the wave number 3323,94 cm-1 indicating the ‑OH group, the wave number 1610,94 cm-1 showed the vibration C=C, the strong region absorption of 1500,86 cm-1 indicating the presence of an aromatic ring, the at 1442,88 cm-1 wave number indicating the presence of CH3.

  10. Synthesis and characterization of nanocomposites ZnO / polypyrrole for anti corrosive application

    International Nuclear Information System (INIS)

    Valenca, D.P.; Bouchonneau, N.; Vieira, M.R.S.; Alves, K.G.B.; Melo, C.P. de; Urtiga Filho, S.L.

    2014-01-01

    Nanoparticles of metal oxides and conductive polymers have been investigated as alternative additives in corrosion protection of oxidizable metals. In this hybrid nanocomposites work Polypyrrole-ZnO were synthesized and characterized as a potential application as industrial paint anti corrosive additive. The different steps of the synthesis and characterization of nanocomposites are described. The nanocomposites were obtained from the emulsion polymerization of aqueous solutions of pyrrole and sodium dodecyl sulfate containing ZnO nanoparticles dispersed in the mass. The nanoparticles were characterized by scanning electron microscopy and transmission, dynamic light scattering, diffraction of X-rays and techniques of infrared spectroscopy. From the characterization techniques, it was possible to determine the average size of nanoparticles of ZnO and ZnO-Polypyrrole. The peaks in the diffraction pattern of X-rays observed in the nanocomposite were the same as in ZnO, confirming the presence of ZnO in the composite. (author)

  11. The synthesis and characterization of biotin-silver-dendrimer nanocomposites as novel bioselective labels

    Energy Technology Data Exchange (ETDEWEB)

    Maly, J; Lampova, H; Semeradtova, A; Stofik, M [Faculty of Science, University of J E Purkynje, 40096 Usti nad Labem (Czech Republic); Kovacik, L, E-mail: malyjalga@seznam.c [Institute of Cellular Biology and Pathology, First Faculty of Medicine, Charles University in Prague (Czech Republic)

    2009-09-23

    This paper presents a synthesis of a novel nanoparticle label with selective biorecognition properties based on a biotinylated silver-dendrimer nanocomposite (AgDNC). Two types of labels, a biotin-AgDNC (bio-AgDNC) and a biotinylated AgDNC with a poly(ethylene)glycol spacer (bio-PEG-AgDNC), were synthesized from a generation 7 (G7) hydroxyl-terminated ethylenediamine-core-type (2-carbon core) PAMAM dendrimer (DDM) by an N,N'-dicyclohexylcarbodiimide (DDC) biotin coupling and a NaBH{sub 4} silver reduction method. Synthesized conjugates were characterized by several analytical methods, such as UV-vis, FTIR, AFM, TEM, ELISA, HABA assay and SPR. The results show that stable biotinylated nanocomposites can be formed either with internalized silver nanoparticles (AgNPs) in a DMM polymer backbone ('type I') or as externally protected ('type E'), depending on the molar ratio of the silver/DMM conjugate and type of conjugate. Furthermore, the selective biorecognition function of the biotin is not affected by the AgNPs' synthesis step, which allows a potential application of silver nanocomposite conjugates as biospecific labels in various bioanalytical assays, or potentially as fluorescence cell biomarkers. An exploitation of the presented label in the development of electrochemical immunosensors is anticipated.

  12. NONLINEAR OPTICAL MOLECULAR CRYSTAL BASED ON 2,6-DIAMINOPYRIDINE: SYNTHESIS AND CHARACTERIZATION

    Directory of Open Access Journals (Sweden)

    I. M. Pavlovetc

    2014-05-01

    Full Text Available The paper deals with investigation of a new nonlinear optical material based on nonlinear optical chromophore (4-Nitrophenol and aminopyridine (2,6-Diaminopyridine. Calculation results are presented for molecular packing in the crystalline compound, based on the given components. According to these results the finite material must have a noncentrosymmetric lattice, which determines the presence of the second order nonlinear optical response. Investigations carried out in this work confirm these calculations. Results of experiments are given describing the co-crystallization of these components and the following re-crystallization of the obtained material. In order to get a monocrystal form, the optimal conditions for the synthesis of molecular crystals based on these components are determined. Sufficiently large homogeneous crystals are obtained, that gave the possibility to record their spectra in the visible and near infrared parts of the spectrum, to determine their nonlinear optical properties and the level of homogeneity. Their optical (optical transmission and optical laser damage threshold and nonlinear optical properties are presented. For observation and measurement of the nonlinear optical properties an installation was built which implements the comparative method for measurements of nonlinear optical properties. A potassium titanyl oxide phosphate crystal was used as a sample for comparison. Results are given for the conversion efficiency of the primary laser radiation in the second optical harmonic relative to the signal obtained on the potassium titanyl oxide phosphate crystal. Obtained results show that the molecular co-crystal based on 2,6-Diaminopyridine is a promising nonlinear optical material for generating the second optical harmonic on the Nd: YAG laser (532 nm.

  13. Synthesis, Characterization, and Ultrafast Dynamics of Metal, Metal Oxide, and Semiconductor Nanomaterials

    OpenAIRE

    Wheeler, Damon Andreas

    2013-01-01

    SYNTHESIS, CHARACTERIZATION, AND ULTRAFAST DYNAMICS OF METAL, METAL OXIDE, AND SEMICONDUCTOR NANOMATERIALSABSTRACTThe optical properties of each of the three main classes of inorganic nanomaterials, metals, metal oxides, and semiconductors differ greatly due to the intrinsically different nature of the materials. These optical properties are among the most fascinating and useful aspects of nanomaterials with applications spanning cancer treatment, sensors, lasers, and solar cells. One techn...

  14. Self-Assembled Structures of PMAA-PMMA Block Copolymers : Synthesis, Characterization, and Self-Consistent Field Computations

    NARCIS (Netherlands)

    Li, Feng; Schellekens, Mike; de Bont, Jens; Peters, Ron; Overbeek, Ad; Leermakers, Frans A. M.; Tuinier, Remco

    2015-01-01

    Block copolymers composed of methacrylic acid (MAA) and methyl methacrylate (MMA) blocks are interesting candidates for replacing surfactants in emulsion polymerization methods. Here the synthesis and experimental characterization of well-defined PMAA-PMMA block copolymers made via RAFT

  15. Self-assembled structures of PMAA-PMMA block copolymers: Synthesis, characterization, and self-consistent field computations

    NARCIS (Netherlands)

    Li, F.; Schellekens, J.; Bont, de J.A.M.; Peters, R.; Overbeek, A.; Leermakers, F.A.M.; Tuinier, R.

    2015-01-01

    Block copolymers composed of methacrylic acid (MAA) and methyl methacrylate (MMA) blocks are interesting candidates for replacing surfactants in emulsion polymerization methods. Here the synthesis and experimental characterization of well-defined PMAA–PMMA block copolymers made via RAFT

  16. Synthesis and characterization of related substances of Azilsartan Kamedoxomil

    Directory of Open Access Journals (Sweden)

    Maddi N. V. D. Harikiran

    2017-03-01

    Full Text Available Azilsartan Kamedoxomil is an AT1-subtype angiotensin II receptor blocker (ARB. During the laboratory synthesis of Azilsartan Kamedoxomil, four related substances of Azilsartan Kamedoxomil were observed and identified. These were 2-Ethoxy-3-[[4-[2- [4-[(5-methyl-2-oxo-1,3-dioxol-4-ylmethyl]-5-oxo-1,2,4-oxadiazol-3-yl]phenyl]phenyl] methyl] benzimidazole-4-carboxylic acid (azilsartan N-medoxomil, 9, (5-methyl-2-oxo- 1,3-dioxol-4-ylmethyl 2-ethoxy-3-[[4-[2-[4-[(5-methyl-2-oxo-1,3-dioxol-4-ylmethyl]-5- oxo-1,2,4-oxadiazol-3-yl]phenyl]phenyl] methyl] benzimidazole-4-carboxylate (azilsartan dimedoxomil, 10, (5-methyl-2-oxo-1,3-dioxo-4-ylmethyl 1-[2’-(4,5-dihydro-5-oxo-4H- 1,2,4-oxadiazol-3-ylbiphenyl-4-yl]methyl]-2-methoxy-1H-benzimidazole-7-carboxylate (methoxy analogue of azilsartan medoxomil, 11, Methyl 1-((2’-amidobiphenyl-4-yl methyl-2-ethoxy-1H-benzo[d]imidazole-7-carboxylate (amide methyl ester, 12. The present work describes the origin, synthesis and characterization of these related substances.

  17. Synthesis and characterization of Fe{sub 3}O{sub 4} nanoparticles with perspectives in biomedical applications

    Energy Technology Data Exchange (ETDEWEB)

    Mamani, Javier Bustamante, E-mail: javierbm@einstein.br [Hospital Israelita Alberto Einstein (HIAE), Sao Paulo, SP (Brazil); Gamarra, Lionel Fernel [Universidade Federal de Sao Paulo (UNIFESP), Sao Paulo, SP (Brazil). Dept. de Neurologia e Neurocirurgia; Brito, Giancarlo Esposito de Souza [Universidade de Sao Paulo (USP), Sao Paulo, SP (Brazil). Inst. de Fisica. Dept. de Fisica Aplicada

    2014-05-15

    Nowadays the use of magnetic nanoparticles (MNP) in medical applications has exceeded expectations. In molecular imaging, MNP based on iron oxide coated with appropriated materials have several applications in vitro and in vivo studies. For applications in nanobiotechnology these MNP must present some characteristics such as size smaller than 100 nanometers, high magnetization values, among others. Therefore the MNP have physical and chemical properties that are specific to certain studies which must be characterized for quality control of the nanostructured material. This study presents the synthesis and characterization of MNP of magnetite (Fe{sub 3}O{sub 4}) dispersible in water with perspectives in a wide range of biomedical applications. The characterization of the colloidal suspension based on MNP stated that the average diameter is (12.6±0.2) nm determined by Transmission Electron Microscopy where the MNP have the crystalline phase of magnetite (Fe{sub 3}O{sub 4}) that was identified by Diffraction X-ray and confirmed by Moessbauer Spectroscopy. The blocking temperature of (89±1) K, Fe{sub 3}O{sub 4} MNP property, was determined from magnetic measurements based on the Zero Field Cooled and Field Cooled methods. The hysteresis loops were measured at different temperatures below and above blocking temperature. The magnetometry determined that the MNP showed superparamagnetic behavior confirmed by ferromagnetic resonance. (author)

  18. Green Synthesis and Characterizations of Flower Shaped CuO Nanoparticles for Biodiesel Application

    Directory of Open Access Journals (Sweden)

    Rintu Varghese

    2017-03-01

    Full Text Available Nanomaterials are primary candidates to play a key role in energy future. In this work, plant-mediated green synthesis of CuO nanoparticles was studied. The CuO nanoparticles were used as the catalysts for the production of biodiesel from coconut oil. An aqueous extract of Centella Asiatica leaves was used as a bio-reducing agent for the synthesis of CuO nanoparticles. This biocatalyst was characterized by using different techniques (FTIR, UV-Vis spectroscopy, XRD, FESEM with EDX which were confirmed the formation of CuO nanoparticles. Further, the presences of FAME (Fatty Acid Methyl Ester groups at the produced biodiesel were confirmed using both the GC-MS and FTIR analysis. From this work, it has been concluded that the plant extract mediated synthesis of CuO nanoparticles is quite simple, cost-effective and environmentally friendly. The produced biodiesel from coconut oil is considered to be a potential source for alternative conventional fuel.

  19. Synthesis of flexible magnetic nanohybrid based on bacterial cellulose under ultrasonic irradiation

    International Nuclear Information System (INIS)

    Zheng, Yi; Yang, Jingxuan; Zheng, Weili; Wang, Xiao; Xiang, Cao; Tang, Lian; Zhang, Wen; Chen, Shiyan; Wang, Huaping

    2013-01-01

    Flexible magnetic membrane based on bacterial cellulose (BC) was successfully prepared by in-situ synthesis of the Fe 3 O 4 nanoparticles under different conditions and its properties were characterized. The results demonstrated that the Fe 3 O 4 nanoparticles coated with PEG were well homogeneously dispersed in the BC matrix under ultrasonic irradiation with the saturation magnetization of 40.58 emu/g. Besides that, the membranes exhibited the striking flexibility and mechanical properties. This study provided a green and facile method to inhibit magnetic nanoparticle aggregation without compromising the mechanical properties of the nanocomposites. Magnetically responsive BC membrane would have potential applications in electronic actuators, information storage, electromagnetic shielding coating and anti-counterfeit. - Highlights: ► Flexible magnetic film is prepared by in situ synthesis on bacterial cellulose. ► Ultrasound and PEG are used together to inhibit the nanoparticle aggregation. ► The magnetic membrane demonstrates the great superparamagnetic behavior

  20. Synthesis and characterization of polycaprolactone for anterior cruciate ligament regeneration

    Energy Technology Data Exchange (ETDEWEB)

    Gurlek, Ayse Cansu; Sevinc, Burcu; Bayrak, Ece; Erisken, Cevat, E-mail: cerisken@etu.edu.tr

    2017-02-01

    Anterior cruciate ligament (ACL) is the most frequently torn ligament in the knee, and complete healing is unlikely due to lack of vascularization. Current approaches for the treatment of ACL injuries include surgical interventions and grafting, however recent reports show that surgeries have 94% recurrency, and that repaired tissues are biomechanically inferior to the native tissue. These necessitate the need for new strategies for scar-free repair/regeneration of ACL injuries. Polycaprolactone (PCL) is a biodegradable and biocompatible synthetic polymer, which has been widely used in the connective tissue repair/regeneration attempts. Here, we report on the synthesis of PCL via ring opening polymerization using ε-caprolactone as the monomer, and ammonium heptamolybdate as a catalyst. The synthesized PCL was characterized using Fourier Transform Infrared Spectroscopy (FTIR) and Nuclear Magnetic Resonance (NMR) spectroscopy. It was then processed using electrospinning to form nanofiber-based scaffolds. These scaffolds were characterized in terms of surface as well as mechanical properties, and compared to the properties of commercially available PCL, and of native ACL tissue harvested from sheep. In addition, scaffolds fabricated with synthesized PCL were evaluated regarding their cell attachment capacity using human bone marrow mesenchymal stem cells (hBMSCs). Our findings demonstrated that the synthesized PCL is similar to its commercially available counterpart in terms of surface morphology and mechanical properties. In addition, fibrous scaffolds generated with electrospinning showed weaker mechanical properties visa vis native ACL tissue in terms of ultimate stress, and elastic modulus. Also, the synthesized PCL can accommodate cell attachment when tested with hBMSCs. Putting together, these observations reveal that the PCL synthesized in this study could be a good candidate as a biomaterial for ligament repair or regeneration. - Highlights: • Synthesis of

  1. Synthesis and characterization of polycaprolactone for anterior cruciate ligament regeneration

    International Nuclear Information System (INIS)

    Gurlek, Ayse Cansu; Sevinc, Burcu; Bayrak, Ece; Erisken, Cevat

    2017-01-01

    Anterior cruciate ligament (ACL) is the most frequently torn ligament in the knee, and complete healing is unlikely due to lack of vascularization. Current approaches for the treatment of ACL injuries include surgical interventions and grafting, however recent reports show that surgeries have 94% recurrency, and that repaired tissues are biomechanically inferior to the native tissue. These necessitate the need for new strategies for scar-free repair/regeneration of ACL injuries. Polycaprolactone (PCL) is a biodegradable and biocompatible synthetic polymer, which has been widely used in the connective tissue repair/regeneration attempts. Here, we report on the synthesis of PCL via ring opening polymerization using ε-caprolactone as the monomer, and ammonium heptamolybdate as a catalyst. The synthesized PCL was characterized using Fourier Transform Infrared Spectroscopy (FTIR) and Nuclear Magnetic Resonance (NMR) spectroscopy. It was then processed using electrospinning to form nanofiber-based scaffolds. These scaffolds were characterized in terms of surface as well as mechanical properties, and compared to the properties of commercially available PCL, and of native ACL tissue harvested from sheep. In addition, scaffolds fabricated with synthesized PCL were evaluated regarding their cell attachment capacity using human bone marrow mesenchymal stem cells (hBMSCs). Our findings demonstrated that the synthesized PCL is similar to its commercially available counterpart in terms of surface morphology and mechanical properties. In addition, fibrous scaffolds generated with electrospinning showed weaker mechanical properties visa vis native ACL tissue in terms of ultimate stress, and elastic modulus. Also, the synthesized PCL can accommodate cell attachment when tested with hBMSCs. Putting together, these observations reveal that the PCL synthesized in this study could be a good candidate as a biomaterial for ligament repair or regeneration. - Highlights: • Synthesis of

  2. Synthesis and characterization of "1"3C_3-tristearin

    International Nuclear Information System (INIS)

    Wu Hangyu; Lin Lin; Li Lei; Chen Dazhou

    2011-01-01

    A highly efficient synthesis of "1"3C_3 labeled triglycerides of stearic acids from "1"3C_3-glycerol and stearic acids, by immobilized lipase-catalyzed in solvent-free medium was described. The structure of the product were characterized by fourier transform infrared spectrum (FT-IR), nuclear magnetic resonance (NMR), mass spectra (MS). The results showed that triglycerides of stearic acids contained three "1"3C atoms. The isotope abundance of "1"3C_3-tristearin was more than 99% and the yield was 80% of "1"3C_3-tristearin through calculation. Chemical purity (> 98%) was obtained by differential scanning calorimetry (DSC). (authors)

  3. Synthesis and characterization of bio-based polyurethane from ...

    Indian Academy of Sciences (India)

    Benzoylated tannin prepared by benzoylation of cashewnut husk tannin, was treated with hexame-thylenediisocyanate in the presence of 1,4-butanediol as an extender to prepare thermosetting polyurethane. The sample was characterized using FT–IR and 13C NMR spectra. Thermal, morphological, physico-chemical and ...

  4. A facile soft template synthesis and characterization of PbHAsO4 nanocrystals

    International Nuclear Information System (INIS)

    Xiu Zhiliang; Lue Mengkai; Zhou Guangjun; Gu Feng; Zhang Haiping; Xu Dong; Yuan Duorong

    2004-01-01

    Monoclinic lead hydrogen arsenate (LHA) nanocrystals with different crystallization morphologies and crystallite sizes were prepared successfully by a soft template synthesis method in the presence of sodium dodecylbenzenesulfonate (SDBS) or polyvinylpyrrolidone (PVP). The products were characterized by X-ray diffraction (XRD) and transmission electron microscopy (TEM). The possible mechanism of SDBS and PVP in the experiment was briefly illustrated

  5. Synthesis and Characterization of Fluoro- and Chlorobimetallic Alkoxides as Precursors for Luminescent Metal Oxide Materials via Sol-Gel Technique

    Institute of Scientific and Technical Information of China (English)

    ATHAR, Taimur; SEOK, Sang II; KWON, Jeong Oh

    2007-01-01

    Heterobimetallic alkoxides are broadly recognized as versatile precursors for luminescence materials, and efforts are being made to develop novel routes by applying the concept of geometrical molecular design, for their synthesis and to design a single source precursor suited to photoluminescent materials. Novel and new series of bimetallic alkoxides has been prepared by metathesis route. They exhibit a lower sensitivity towards hydrolysis and so they are easier to handle as compared to other alkoxides. All the compounds were characterized by elemental analysis, FT-IR and multinuclear NMR spectroscopies. FT-IR revealed that the molecular structure of these metal spectroscopy provided useful information about chemical shifts for better understanding the likely structure based on interactions with their coordinate metals. The mass spectra show similar types of fragmentation pattern.SEM-EDS analyses showed consistency with the formulation. XRD patterns show an enhanced homogeneity at high temperature. TGA measurements show that thermal decomposition occured in steps that depended entirely on the chemical compositions and the synthesis routes. SEM observation reveals that the morphology and particle size strongly depend on synthesis routes for their precursors.

  6. L-shaped benzimidazole fluorophores: synthesis, characterization and optical response to bases, acids and anions.

    Science.gov (United States)

    Lirag, Rio Carlo; Le, Ha T M; Miljanić, Ognjen Š

    2013-05-14

    Nine L-shaped benzimidazole fluorophores have been synthesized, computationally evaluated and spectroscopically characterized. These "half-cruciform" fluorophores respond to bases, acids and anions through changes in fluorescence that vary from moderate to dramatic.

  7. Synthesis, characterization and electrochemistry of heterobimetallic ...

    African Journals Online (AJOL)

    dimethylpyrazolyl) borate with a series of manganese(II) Schiff bases have been synthesized. Characterization by UV, IR, MS and elemental analysis support their formulations. Cyclic and differential pulse voltammograms of manganese(II) Schiff base ...

  8. Synthesis and Characterization of Hydroxyapatite/Fullerenol Nanocomposites.

    Science.gov (United States)

    Djordjevic, Aleksandar; Ignjatovic, Nenad; Seke, Mariana; Jovic, Danica; Uskokovic, Dragan; Rakocevic, Zlatko

    2015-02-01

    Fullerenols are polyhydroxylated, water soluble derivatives of fullerene C60, with potential application in medicine as diagnostic agents, antioxidants or nano drug carriers. This paper describes synthesis and physical characterization of a new nanocomposite hydroxyapatite/fullerenol. Surface of the nanocomposite hydroxyapatite/fullerenol is inhomogeneous with the diameter of the particles in the range from 100 nm to 350 nm. The ζ potential of this nanocomposite is ten times lower when compared to hydroxyapatite. Surface phosphate groups of hydroxyapatite are prone to forming hydrogen bonds, when in close contact with hydroxyl groups, which could lead to formation of hydrogen bonds between hydroxyapatite and hydroxyl groups of fullerenol. The surface of hydroxyapatite particles (-2.5 mV) was modified by fullerenol particles, as confirmed by the obtained ζ potential value of the nanocomposite biomaterial hydroxyapatite/fullerenol (-25.0 mV). Keywords: Hydroxyapatite, Fullerenol, Nanocomposite, Surface Analysis.

  9. Cu(II AND Zn(II COMPLEX COMPOUNDS WITH BIGUANIDES AROMATIC DERIVATIVES. SYNTHESIS, CHARACTERIZATION, BIOLOGICAL ACTIVITY

    Directory of Open Access Journals (Sweden)

    Ticuţa Negreanu-Pîrjol

    2011-05-01

    Full Text Available In this paper we report the synthesis, physical-chemical characterization and antimicrobial activity of some new complex compounds of hetero-aromatic biguanides ligands, chlorhexidine base (CHX and chlorhexidine diacetate (CHXac2 with metallic ions Cu(II and Zn(II, in different molar ratio. The synthesized complexes were characterized by elemental chemical analysis and differential thermal analysis. The stereochemistry of the metallic ions was determined by infrared spectra, UV-Vis, EPR spectroscopy and magnetic susceptibility in the aim to establish the complexes structures. The biological activity of the new complex compounds was identified in solid technique by measuring minimum inhibition diameter of bacterial and fungal culture, against three standard pathogen strains, Escherichia coli ATCC 25922, Staphilococcus aureus ATCC 25923 and Candida albicans ATCC 10231. The results show an increased specific antimicrobial activity for the complexes chlorhexidine:Cu(II 1:1 and 1:2 compared with the one of the Zn(II complexes.

  10. Synthesis by irradiation and mechanism and structural characterization study of high melt strength polypropylene

    International Nuclear Information System (INIS)

    Lugao, Ademar Benevolo

    2004-01-01

    Polypropylene molecular structure is made only by linear molecules interacting by weak forces. The resulting PP has very low melt strength (MS). MS is important to make feasible to process PP by all the transformation technologies based on the free expansion of the melt. The aim of this work was to develop a new process to synthesize PP with crosslinks and/or long chain branches, known as High Melt Strength Polypropylene (HMSPP) and to characterize its structure and synthesis mechanism. HMSPP was obtained by the irradiation of PP under a crosslinking (acetylene) atmosphere or inert or oxidative one, followed by thermal treatment for radical recombination and thermal treatment for annihilation of the remaining radicals under reactive or inert atmosphere. The results from rheological characterization showed that the highest levels of MS were obtained by conducting irradiation and thermal treatments under crosslinking atmospheres. The results for the elucidation of reaction mechanism by electron spin resonance (ESR) showed that acetylene irradiation is effective in promoting the creation of double bonds, based on the formation of polyenil radicals. The results of structural unraveling showed that radiation promotes predominantly the degradation of atactic molecules or molecules with atactic defects. These results support the hypothesis of formation of branched PP molecules based on the reaction of those fragments with the double bonds created in the PP molecules. (author)

  11. Performance Improvements and Congestion Reduction for Routing-based Synthesis for Digital Microfluidic Biochips

    DEFF Research Database (Denmark)

    Windh, Skyler; Phung, Calvin; Grissom, Daniel T.

    2017-01-01

    Routing-based synthesis for digital microfluidic biochips yields faster assay execution times compared to module-based synthesis. We show that routing-based synthesis can lead to deadlocks and livelocks in specific cases, and that dynamically detecting them and adjusting the probabilities...

  12. SYNTHESIS, PHYSICO-CHEMICAL AND ANTIMICROBIAL ...

    African Journals Online (AJOL)

    userpc

    -125. Byeong G. Chae D., Hae N., Hyung K. C. and. Yong K. C. (1996); Synthesis and characterization of schiff base derived 2- hydroxy napthaldehyde and aliphatic diammines. Bulletin Korean Chemical. Society 17(8): 687-693. Hassan S. W. ...

  13. Synthesis, Characterization and Applications of One-Dimensional Metal Oxide Nanostructures

    Science.gov (United States)

    Santulli, Alexander

    Nanomaterials have been of keen research interest, owing to their exciting and unique properties (e.g. optical, magnetic, electronic, and mechanical). These properties allow nanomaterials to have many applications in areas of medicine, alternative energy, catalysis, and information storage. In particular, one-dimensional (1D) nanomaterials are highly advantageous, owing to the inherent anisotropic nature, which allows for effective transport and study of properties on the nanoscale. More specifically, 1D metal oxide nanomaterials are of particular interest, owing to their high thermal and chemical stability, as well as their intriguing optical, electronic, and magnetic properties. Herein, we will investigate the synthesis and characterization of vanadium oxide, lithium niobate and chromium oxide. We will explore the methodologies utilized for the synthesis of these materials, as well as the overall properties of these unique nanomaterials. Furthermore, we will explore the application of titanium dioxide nanomaterials as the electron transport layer in dye sensitized solar cells (DSSCs), with an emphasis on the effect of the nanoscale morphology on the overall device efficiency.

  14. β-galactosidase-catalyzed synthesis of galactosyl chlorphenesin and its characterization.

    Science.gov (United States)

    Lee, Sang-Eun; Jo, Tae-Min; Lee, Hyang-Yeol; Lee, Jongsung; Jung, Kyung-Hwan

    2013-11-01

    We synthesized galactosyl chlorphenesin (CPN-G) using β-gal-containing Escherichia coli (E. coli) cells in which the conversion yield of chlorphenesin (CPN) to CPN-G reached about 64 % during 12 h. CPN-G was identified and characterized using high-performance liquid chromatography, liquid chromatography-mass spectrometry, Fourier transform-infrared spectrometry, and nuclear magnetic resonance analysis ((1)H and (13)C). We verified that a galactose was covalently bound to a CPN alcohol group during CPN-G synthesis throughout these analyses. In particular, by the hydrolysis of CPN-G using β-gal, it was confirmed that a galactose was bound to CPN. The minimal inhibitory concentration (MIC) results showed that the CPN-G MICs were fairly similar to those of CPN. HACAT cell viability was significantly higher in CPN-G-treated cells than in CPN-treated cells at concentrations of 0.0-20.0 mM. Finally, we accomplished the synthesis of less toxic CPN-G, compared with CPN, using β-gal-containing E. coli cells as whole cells without changes in the MICs against microorganisms.

  15. SYNTHESIS, CHARACTERIZATION AND ANTIBACTERIAL ...

    African Journals Online (AJOL)

    Preferred Customer

    In the present study, synthesis, and biological evaluation of some novel ... Then slowly cooled and resultant mixture was basified with aqueous sodium hydroxide ... mol), anhydrous potassium carbonate (5.52 g, 0.04 mol) in acetone (25 mL), ...

  16. Synthesis, purification and physico-chemical characterization of the deuterized chloroform

    International Nuclear Information System (INIS)

    Mihaila, V.; Olteanu-Chiper, D.

    1999-01-01

    This work refers to deuterized chloroform synthesis and purification methods. Three methods for obtaining deuterized chloroform are presented. 1. The direct chlorination of methane, in presence of light and in oxygen-free atmosphere: CH 4 + 3 Cl 2 + ℎν→ CHCl 3 + 3 HCl. The method's drawback is that the product obtained is impure, as other chlorinated compounds such as CH 3 Cl, CH 2 Cl 2 , CCl 4 also result. 2. Chlorination of acetaldehyde or acetone, in basic catalysis and in halogen excess (α substitution with direct synthesis of trihalogen compound), followed by a haloform reaction (hydrolytic splitting) in presence of chlorinated lime: CH 3 CHO (Cl 2 /HO - )/(-HCl)Cl 3 C-CHO (CaCl 2 /HOH)/(-(HCOO) 2 Ca) CHCl 3 and CH 3 -CO-CH 3 (Cl 2 /HO)/(-HCl) Cl 3 C-CO-CH 3 (NaOH)/(-CH 3 COONa) CHCl 3 . 3. Decarboxylizing of trichloroacetate acid (as sodium salt): Cl 3 C-COONa (t deg C)/(H 2 O) Cl 3 CH + NaHCO 3 . This method is the most suitable for the deuterized chloroform synthesis since the reaction takes place in absence of other hydrogen atoms (protons) and in deuterized water 99,87% purity, according to the following reaction: Cl 3 C-COONa (t deg C)/(D 2 O) Cl 3 CD + NaDCO 3 . Another advantage is that this method avoids the synthesis of secondary products which could entail additional purifications (distillations, rectifications, a.s.o.). The deuterized chloroform is separated from the deuterized sodium bicarbonate aqueous solution by washing with deuterized water, in a liquid-to-liquid separating funnel. After separation, the deuterized chloroform is dried in nitrogen atmosphere. The characterization of the final product is carried out through Nuclear Magnetic Resonance Spectrometry. (authors)

  17. Synthesis and characterization of polyglycerols dendrimers for applications in tissue engineering biological

    International Nuclear Information System (INIS)

    Passos, E.D.; Queiroz, A.A.A. de

    2014-01-01

    Full text: Introduction: Over the last twenty years is the growing development in the manufacture of synthetic scaffold in tissue engineering applications. These new materials are based on polyglycerol dendrimers (PGLD's). PGLD's are highly functional polymers with hydroxymethyl side groups, fulfill all structural prerequisites to replace poly(ethylene glycol)s in medical applications. Furthermore, since these materials are based on naturally occurring compounds that degrades over time in the body and can be safely excreted. The objective of this work was the synthesis, physicochemical, biological characterization of HPGL's with potential use as scaffolds in tissue engineering. HPGL's with oligomeric cores, of diglycerol triglycerol and tetraglycerol was used. Theoretical and Experimental Simulation Details: The synthesis of PGLD procedures involves the etherification of glycerol through anionic polymerization of glycidol. The PGLD's were characterized by chromatographic techniques (SEC and HPLC), spectroscopic (FTIR, 1H-NMR and 13C - NMR) electrochemical (zeta potential) and thermal analysis (DSC and TGA) techniques. The structure- activity relationships (SAR's) of compound prototype and its analogs were studied to determine the generation number (G) of the molecule responsible for the biological activity on the adhesion and cell proliferation process. A detailed study of the structure of PGLD's of G=0-4 was performed using the Hyperchem 7. 5 and Gromacs 4 software packages. The biocompatibility studies were studied by scanning electron microscopy (SEM) and fluorescence microscopy (EPF) technique after PGLD (G=0-4) blood contact. The overall electro-negativity/total charge density, dipole moment, frontier orbital's (HOMO - LUMO) and electrostatic potential maps (EPM) were calculated. The most stable form of the resulting compounds was determined by estimating the hydration energy and energy conformation. Results and Discussion: The techniques SEM and EPF

  18. Synthesis and characterization of breast-phantom-based gelatine-glutaraldehyde-TiO2 as a test material for the application of breast cancer diagnosis

    Science.gov (United States)

    Ukhrowiyah, Nuril; Setyaningsih, Novi; Hikmawati, Dyah; Yasin, Moh

    2017-05-01

    Synthesis of breast-phantom-based on gelatine-glutaraldehyde-TiO2 as testing material of breast cancer diagnosis using Near Infrared-Diffuse Optical Tomography (NIR-DOT) is presented. Glutaraldehyde (GA) is added to obtain optimum breast phantom which has same elasticity modulus with mammae. First, synthesis is conducted by mixing gelatine with various amounts of 1 g, 2 g and 3 g with saline solution on 40° C temperature for 30 minutes until they become homogenous. Next, GA with concentration of 0.5 and 1.0% is added. The characterization includes FTIR test, physical test, and mechanical test used to identify group of gelatine’s functions. Elasticity modulus of breast phantom of gelatine composition 2 g and 0.5% GA is obtained at 53.46 kPA which is the approximation of mammae culture elasticity. This composition is chosen to synthesise the next step. In the second step, TiO2 is added with variation of 0.01 g, 0.015 g, 0.02 g, 0.025 g, and 0,03 g. With this variation, it is aimed to get a breast phantom providing image with optimum absorption. The test of this material uses Differential Scanning Calorimetry (DSC), homogeneity test, and analysis of coefficient absorption. The result shows the sample has a good thermal property in the range of 40 - 70° C with a good homogeneity and absorption coefficient of 0.4 mm-1.

  19. Characterization of a manganese ore to define the use in the fluxes synthesis for submerged arc welding

    International Nuclear Information System (INIS)

    Cruz, A.; Quintana, R.; Perdomo, L.; Garcia, L. L.; Formoso, A.; Cores, A.

    2003-01-01

    Chemical analysis, thermal analysis (DTA and TG), phase determination by X-ray diffraction and granulometric analysis of the manganese ore from the location Margarita de Cambute in the eastern part of cuba were carried out. Based on these characterization results, a flux synthesis strategy was established, comprising the definition, as a basic condition, of the MnO/SiO 2 range of values. This strategy was confirmed experimentally by obtaining a flux prototype in an electric arc furnace connected to direct current source and the carrying out of the flux in submerged arc welding tests. (Author) 26 refs

  20. Synthesis and characterization of Al-TON zeolite using a dialkylimizadolium as structure-directing agent

    Energy Technology Data Exchange (ETDEWEB)

    Lopes, Christian Wittee; Pergher, Sibele Berenice Castella, E-mail: chriswittee@gmail.com [Universidade Federal do Rio Grande do Norte (UFRN), Natal, RN (Brazil); Villarroel-Rocha, Jhonny [Laboratorio de Solidos Porosos, Instituto de Fisica Aplicada, Universidad Nacional de San Luis, Chacabuco, San Luis (Argentina); Silva, Bernardo Araldi Da; Mignoni, Marcelo Luis [Universidade Regional Integrada, Erechim, RS (Brazil)

    2016-11-15

    In this work, the synthesis of zeolites using 1-butyl-3-methylimidazolium chloride [C{sub 4}MI]Cl as a structure-directing agent was investigated. The organic cation shows effectiveness and selectivity for the syntheses of TON zeolites under different reaction conditions compared to the traditional structure directing agent, 1,8-diaminooctane. The 1-butyl-3-methylimidazolium cation lead to highly crystalline materials and its role as OSDA in our synthesis conditions has been confirmed by characterization techniques. ICP-OES confirms the presence of Al in the samples and {sup 27}Al MAS NMR analysis indicated that aluminum atoms were incorporated in tetrahedral coordination. Scanning electron microscopy indicated that changing the crystallization condition (static or stirring), zeolites with different crystal size were obtained, which consequently affects the textural properties of the zeolites. Moreover, varying some synthesis parameters MFI zeolite can also be obtained. (author)

  1. Thermomagnetic characterization of organic-based ferrofluids prepared with Ni ferrite nanoparticles

    International Nuclear Information System (INIS)

    Arana, Mercedes; Bercoff, Paula G.; Jacobo, Silvia E.

    2017-01-01

    Highlights: • Kerosene-based ferrofluids of Ni-ferrite NPs from high energy ball milling. • Thermomagnetic characterization of organic-based ferrofluids. • Measured thermal variables enhancements of ferrofluid vs. magnetic field. • Curves successfully fitted by a gas-compression model of nanoaggregates. - Abstract: In this work, a thermomagnetic characterization of kerosene-based ferrofluids (FFs) prepared with Ni-ferrite nanoparticles (NPs) is performed by measuring their thermal conductivity and diffusivity coefficient enhancements. The particles were synthesized by high-energy ball milling, as an alternative to the most commonly chosen NPs synthesis methods for FFs. The action of an applied magnetic field on the FF increases the thermal conductivity and diffusivity due to cooperation between the NPs, as it agglomerates them favoring chain-like and clusters formations. It was found that the heat capacity of the studied FFs decreases under the application of a magnetic field. The obtained results for thermal conductivity of FFs under magnetic fields were fitted by a gas-compression model that considers NPs agglomerates in the fluid.

  2. Thermomagnetic characterization of organic-based ferrofluids prepared with Ni ferrite nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Arana, Mercedes, E-mail: mercedes.arana@labh2.coppe.ufrj.br [Facultad de Matemática, Astronomía, Física y Computación (FaMAF), Universidad Nacional de Córdoba, IFEG, CONICET, Medina Allende s/n, Ciudad Universitaria, Córdoba (Argentina); Bercoff, Paula G. [Facultad de Matemática, Astronomía, Física y Computación (FaMAF), Universidad Nacional de Córdoba, IFEG, CONICET, Medina Allende s/n, Ciudad Universitaria, Córdoba (Argentina); Jacobo, Silvia E. [DiQuiMMAI, Facultad de Ingeniería, Universidad de Buenos Aires, INTECIN, CONICET, Av. Paseo Colón 850, Buenos Aires (Argentina)

    2017-01-15

    Highlights: • Kerosene-based ferrofluids of Ni-ferrite NPs from high energy ball milling. • Thermomagnetic characterization of organic-based ferrofluids. • Measured thermal variables enhancements of ferrofluid vs. magnetic field. • Curves successfully fitted by a gas-compression model of nanoaggregates. - Abstract: In this work, a thermomagnetic characterization of kerosene-based ferrofluids (FFs) prepared with Ni-ferrite nanoparticles (NPs) is performed by measuring their thermal conductivity and diffusivity coefficient enhancements. The particles were synthesized by high-energy ball milling, as an alternative to the most commonly chosen NPs synthesis methods for FFs. The action of an applied magnetic field on the FF increases the thermal conductivity and diffusivity due to cooperation between the NPs, as it agglomerates them favoring chain-like and clusters formations. It was found that the heat capacity of the studied FFs decreases under the application of a magnetic field. The obtained results for thermal conductivity of FFs under magnetic fields were fitted by a gas-compression model that considers NPs agglomerates in the fluid.

  3. Photonic arbitrary waveform generator based on Taylor synthesis method

    DEFF Research Database (Denmark)

    Liao, Shasha; Ding, Yunhong; Dong, Jianji

    2016-01-01

    Arbitrary waveform generation has been widely used in optical communication, radar system and many other applications. We propose and experimentally demonstrate a silicon-on-insulator (SOI) on chip optical arbitrary waveform generator, which is based on Taylor synthesis method. In our scheme......, a Gaussian pulse is launched to some cascaded microrings to obtain first-, second- and third-order differentiations. By controlling amplitude and phase of the initial pulse and successive differentiations, we can realize an arbitrary waveform generator according to Taylor expansion. We obtain several typical...... waveforms such as square waveform, triangular waveform, flat-top waveform, sawtooth waveform, Gaussian waveform and so on. Unlike other schemes based on Fourier synthesis or frequency-to-time mapping, our scheme is based on Taylor synthesis method. Our scheme does not require any spectral disperser or large...

  4. Antibacterial gold nanoparticles-biomass assisted synthesis and characterization.

    Science.gov (United States)

    Badwaik, Vivek D; Willis, Chad B; Pender, Dillon S; Paripelly, Rammohan; Shah, Monic; Kherde, Yogesh A; Vangala, Lakshmisri M; Gonzalez, Matthew S; Dakshinamurthy, Rajalingam

    2013-10-01

    Xylose is a natural monosaccharide found in biomass such as straw, pecan shells, cottonseed hulls, and corncobs. Using this monosaccharide, we report the facile, green synthesis and characterization of stable xylose encapsulated gold nanoparticles (Xyl-GNPs) with potent antibacterial activity. Xyl-GNPs were synthesized using the reduction property of xylose in an aqueous solution containing choloraurate anions carried out at room temperature and atmospheric pressure. These nanoparticles were stable and near spherical in shape with an average diameter of 15 +/- 5 nm. Microbiological assay results showed the concentration dependent antibacterial activity of these particles against both Gram-negative (Escherichia coli) and Gram-positive (Staphylococcus epidermidis) bacteria. Thus the facile, environmentally friendly Xyl-GNPs have many potential applications in chemical and biomedical industries, particularly in the development of antibacterial agents in the field of biomedicine.

  5. Synthesis and characterization of waterborne polyurethane acrylate copolymers

    International Nuclear Information System (INIS)

    Sultan, Misbah; Bhatti, Haq Nawaz; Zuber, Mohammad; Barikani, Mehdi

    2013-01-01

    Polyurethane acrylate copolymers were synthesized by emulsion polymerization process. To reduce the environmental hazards, organic solvents were replaced by eco-friendly aqueous system. Concentration of polyurethane and acrylate monomer was varied to investigate the effect of chemical composition on performance properties of copolymers. FTIR spectroscopy was used as a key tool to record the chemical synthesis route. The synthesized copolymer emulsions were characterized by evaluating their particle size, viscosity, dry weight content, chemical and water resistance. Thermal decomposition was studied by thermogravimetric analysis. Scanning electron microscope was used to visualize the morphological structure of copolymers. The experimental results indicate better polyurethane acrylate compatibility till the ratio of 30/70. However, these copolymers exhibited synergistic effects between the two polymers and revealed a remarkable improvement in numerous coating properties

  6. Synthesis, Physical Characterization and Biological Activity of Some Schiff Base Complexes

    Directory of Open Access Journals (Sweden)

    R. Rajavel

    2008-01-01

    Full Text Available Structural modification of organic molecule has considerable biological relevance. Further, coordination of a biomolecules to the metal ions significantly alters the effectiveness of the biomolecules. In view of the antimicrobial activity ligand [bis-(2-aminobenzaldehyde] malonoyl dihydrazone], metal complexes with Cu(II, Ni(II, Zn(II and oxovanadium(IV have been synthesized and found to be potential antimicrobial agents. An attempt is also made to correlate the biological activities with geometry of the complexes. The complexes have been characterized by elemental analysis, molar conductance, spectra and cyclicvoltammetric measurements. The structural assessment of the complexes has been carried out based on electronic, infrared and molar conductivity values.

  7. Synthesis, characterization and behaviour to gamma radiation of the bis-L-alaninato-copper (II)

    International Nuclear Information System (INIS)

    Passos, B.F.T.

    1985-01-01

    The behaviour of coordinated compound obtained from the copper (II) and the L-(+)- alanine to gamma radiation was determined. A study of synthesis and characterization of this complex was made with elementary analysis, ultraviolet and visible electronic spectroscopy, infrared vibrational spectroscopy, proton magnetic resonance spectroscopy and thermo-gravimetric analysis. (C.G.C.)

  8. Synthesis and characterization of low-valence actinide phosphide tellurides and ternary selenium-halide iridium complexes; Synthese und Charakterisierung niedervalenter Actinoidphosphidtelluride und ternaerer Selen-Halogenid-Komplexe des Iridiums

    Energy Technology Data Exchange (ETDEWEB)

    Stolze, Karoline

    2016-04-07

    The thesis on the synthesis and characterization of low-valence actinide phosphide tellurides and ternary selenium-halide iridium complexes includes two parts: a description of the experimental synthesis of UPTe and U2PTe2O and ThPTe and the synthesis of selenium-chloride iridium complexes and selenium-bromide iridium complexes. The characterization included X-ray diffraction and phase studies.

  9. Synthesis and characterization of carboxylic acid functionalized silicon nanoparticles

    Science.gov (United States)

    Shaner, Ted V.

    Silicon nanoparticles are of great interest in a great number of fields. Silicon nanoparticles show great promise particularly in the field of bioimaging. Carboxylic acid functionalized silicon nanoparticles have the ability to covalently bond to biomolecules through the conjugation of the carboxylic acid to an amine functionalized biomolecule. This thesis explores the synthesis of silicon nanoparticles functionalized by both carboxylic acids and alkenes and their carboxylic acid functionality. Also discussed is the characterization of the silicon nanoparticles by the use of x-ray spectroscopy. Finally, the nature of the Si-H bond that is observed on the surface of the silicon nanoparticles will be investigated using photoassisted exciton mediated hydrosilation reactions. The silicon nanoparticles are synthesized from both carboxylic acids and alkenes. However, the lack of solubility of diacids is a significant barrier to carboxylic acid functionalization by a mixture of monoacids and diacids. A synthesis route to overcome this obstacle is to synthesize silicon nanoparticles with terminal vinyl group. This terminal vinyl group is distal to the surface of the silicon nanoparticle. The conversion of the vinyl group to a carboxylic acid is accomplished by oxidative cleavage using ozonolysis. The carboxylic acid functionalized silicon nanoparticles were then successfully conjugated to amine functionalized DNA strand through an n-hydroxy succinimide ester activation step, which promotes the formation of the amide bond. Conjugation was characterized by TEM and polyacrylamide gel electrophoresis (PAGE). The PAGE results show that the silicon nanoparticle conjugates move slower through the polyacrylamide gel, resulting in a significant separation from the nonconjugated DNA. The silicon nanoparticles were then characterized by the use of x-ray absorption near edge spectroscopy (Xanes) and x-ray photoelectron spectroscopy (XPS) to investigate the bonding and chemical

  10. Synthesis and Characterization of Photo-Responsive Thermotropic Liquid Crystals Based on Azobenzene

    Directory of Open Access Journals (Sweden)

    Runmiao Yang

    2018-03-01

    Full Text Available A series of new thermotropic liquid crystals (LCs containing azobenzene units was synthesized. The structures of the compounds were characterized by means of NMR and FTIR spectroscopy. Their mesomorphic behaviors were investigated via differential scanning calorimetry (DSC and polarizing optical microscopy (POM. Based on the POM and DSC measurements, the optical properties of the Razo-ester were tested using UV-vis spectroscopy. The azobenzene side chain displayed a strong ability to influence the formation of thermotropic LCs.

  11. Synthesis and Characterization of EDTA Complexes Useful for Trace Elements Supplementation

    Directory of Open Access Journals (Sweden)

    Baran Enrique J.

    2002-01-01

    Full Text Available The synthesis of two heterobimetallic EDTA complexes, MgCu(EDTA.6H2O and ZnCu(EDTA.6H2O, is described. They were characterized by means of vibrational (infrared and Raman and electronic (reflectance spectroscopy. Several dissolution tests in 0.1 N HCl and simulated gastric juice were also performed. The results support the potential usefulness of these complexes for copper supplementation in human and veterinary medicine and to the simultaneous reinforcement of Mg(II and Zn(II levels.

  12. Chevrel phases superconductive and ultrafine powders synthesis and characterization; Synthese et caracterisation de poudres ultrafines supraconductrices de phases de Chevrel

    Energy Technology Data Exchange (ETDEWEB)

    Even-Boudjada, S

    1994-12-01

    This work deals with the Chevrel phases superconductive and ultrafine powders synthesis and characterization. The first part of this study presents some new way of synthesis (precipitation, coprecipitation) of Chevrel phases precursors powders (PbS, SnS, MoS{sub 2}) and their characterizations (X-ray fluorescence analysis, ICP mass spectroscopy, scanning electron microscopy, transmission electron microscopy and laser granulometry). These new synthesis methods lead to quasi spherical morphology grains and very weak size grains (0.2 to 0.5 {mu}m) whereas the chemical preparation from the solid state elements gives very different morphology grains (small plates) with a size of 1 to 20 {mu}m. In the second part is shown the interest of the binary Mo{sub 6} S{sub 8} as precursor in the synthesis of ternary superconductive phases (Li, Ni, Cu, Pb). The last part presents the formation reaction of the phase PbMo{sub 6} S{sub 8} and its main chemical and physical properties. Thus some calorimetric measures associated with X-ray diffraction analysis have been realized and have allowed to understand the different reactions occurring during the PbMo{sub 6}S{sub 8} synthesis. (O.L.). 100 refs., figs., tabs.

  13. On-Surface Synthesis and Characterization of Honeycombene Oligophenylene Macrocycles.

    Science.gov (United States)

    Chen, Min; Shang, Jian; Wang, Yongfeng; Wu, Kai; Kuttner, Julian; Hilt, Gerhard; Hieringer, Wolfgang; Gottfried, J Michael

    2017-01-24

    We report the on-surface formation and characterization of [30]-honeycombene, a cyclotriacontaphenylene, which consists of 30 phenyl rings (C 180 H 120 ) and has a diameter of 4.0 nm. This shape-persistent, conjugated, and unsubstituted hexagonal hydrocarbon macrocycle was obtained by solvent-free synthesis on a silver (111) single-crystal surface, making solubility-enhancing alkyl side groups unnecessary. Side products include strained macrocycles with square, pentagonal, and heptagonal shape. The molecules were characterized by scanning tunneling microscopy and density functional theory (DFT) calculations. On the Ag(111) surface, the macrocycles act as molecular quantum corrals and lead to the confinement of surface-state electrons inside the central cavity. The energy of the confined surface state correlates with the size of the macrocycle and is well described by a particle-in-the-box model. Tunneling spectroscopy suggests conjugation within the planar rings and reveals influences of self-assembly on the electronic structure. While the adsorbed molecules appear to be approximately planar, the free molecules have nonplanar conformation, according to DFT.

  14. Synthesis and characterization of magnetite/PLGA/chitosan nanoparticles

    Science.gov (United States)

    Ibarra, Jaime; Melendres, Julio; Almada, Mario; Burboa, María G.; Taboada, Pablo; Juárez, Josué; Valdez, Miguel A.

    2015-09-01

    In this work, we report the synthesis and characterization of a new hybrid nanoparticles system performed by magnetite nanoparticles, loaded in a PLGA matrix, and stabilized by different concentrations of chitosan. Magnetite nanoparticles were hydrophobized with oleic acid and entrapped in a PLGA matrix by the emulsion solvent evaporation method, after that, magnetite/PLGA/chitosan nanoparticles were obtained by adding dropwise magnetite/PLGA nanoparticles in chitosan solutions. Magnetite/PLGA nanoparticles produced with different molar ratios did not show significant differences in size and the 3:1 molar ratio showed best spherical shapes as well as uniform particle size. Isothermal titration calorimetry studies demonstrated that the first stage of PLGA-chitosan interaction is mostly regulated by electrostatic forces. Based on a single set of identical sites model, we obtained for the average number of binding sites a value of 3.4, which can be considered as the number of chitosan chains per nanoparticle. This value was confirmed by using a model based on the DLVO theory and fitting zeta potential measurements of magnetite/PLGA/chitosan nanoparticles. From the adjusted parameters, we found that an average number of chitosan molecules of 3.6 per nanoparticle are attached onto the surface of the PLGA matrix. Finally, we evaluated the effect of surface charge of nanoparticles on a membrane model of endothelial cells performed by a mixture of three phospholipids at the air-water interface. Different isotherms and adsorption curves show that cationic surface of charged nanoparticles strongly interact with the phospholipids mixture and these results can be the basis of future experiments to understand the nanoparticles- cell membrane interaction.

  15. Synthesis and characterization of magnetite/PLGA/chitosan nanoparticles

    International Nuclear Information System (INIS)

    Ibarra, Jaime; Melendres, Julio; Almada, Mario; Juárez, Josué; Valdez, Miguel A; Burboa, María G; Taboada, Pablo

    2015-01-01

    In this work, we report the synthesis and characterization of a new hybrid nanoparticles system performed by magnetite nanoparticles, loaded in a PLGA matrix, and stabilized by different concentrations of chitosan. Magnetite nanoparticles were hydrophobized with oleic acid and entrapped in a PLGA matrix by the emulsion solvent evaporation method, after that, magnetite/PLGA/chitosan nanoparticles were obtained by adding dropwise magnetite/PLGA nanoparticles in chitosan solutions. Magnetite/PLGA nanoparticles produced with different molar ratios did not show significant differences in size and the 3:1 molar ratio showed best spherical shapes as well as uniform particle size. Isothermal titration calorimetry studies demonstrated that the first stage of PLGA-chitosan interaction is mostly regulated by electrostatic forces. Based on a single set of identical sites model, we obtained for the average number of binding sites a value of 3.4, which can be considered as the number of chitosan chains per nanoparticle. This value was confirmed by using a model based on the DLVO theory and fitting zeta potential measurements of magnetite/PLGA/chitosan nanoparticles. From the adjusted parameters, we found that an average number of chitosan molecules of 3.6 per nanoparticle are attached onto the surface of the PLGA matrix. Finally, we evaluated the effect of surface charge of nanoparticles on a membrane model of endothelial cells performed by a mixture of three phospholipids at the air–water interface. Different isotherms and adsorption curves show that cationic surface of charged nanoparticles strongly interact with the phospholipids mixture and these results can be the basis of future experiments to understand the nanoparticles- cell membrane interaction. (paper)

  16. Design, synthesis, and characterization of 0-D, 1-D, and 2-D Zinc–Adeninate coordination assemblies

    Energy Technology Data Exchange (ETDEWEB)

    An, Ji Hyun [Dept. of Chemistry Education, Seoul National University, Seoul (Korea, Republic of); Geib, Steven J. [Dept. of Chemistry, University of Pittsburgh, Pittsburgh (United States); Kim, Myung Gil [Dept. of Chemistry, Chungang University, Seoul (Korea, Republic of)

    2015-08-15

    In this study, we demonstrate the synthesis and characterization of zinc– adeninate coordination polymers with 0-D, 1-D, and 2-D structures. We describe methods for controlling the structure of these materials by applying different synthetic conditions and discuss their structural relationships. 0-D, 1-D, and 2-D zinc–adeninate coordination polymers with the same metal–adeninate coordination mode were synthesized and characterized. By controlling the temperature, a material with 0-D macrocycle or 1-D chain coordination polymer was prepared. A replacement of pyridine with bipyridine formed 2-D sheet structure by connecting 1-D chains with each other. They exhibited an interesting relationship between synthetic methods and structures. Further study of metal–adeninate coordination chemistry will render a precise control of the structure in synthesis and will open a new venue to new materials with fascinating properties.

  17. Graphitic carbon nitride: Synthesis, characterization and photocatalytic decomposition of nitrous oxide

    International Nuclear Information System (INIS)

    Praus, Petr; Svoboda, Ladislav; Ritz, Michal; Troppová, Ivana; Šihor, Marcel; Kočí, Kamila

    2017-01-01

    Graphitic carbon nitride (g-C_3N_4) was synthetized by condensation of melamine at the temperatures of 400–700 °C in air for 2 h and resulting products were characterized and finally tested for the photocatalytic decomposition of nitrous oxide. The characterization methods were elemental analysis, UV–Vis diffuse reflectance spectroscopy (DRS), photoluminescence (PL), Fourier transform infrared (FTIR) and Raman spectroscopy, measurement of specific surface area (SSA), X-ray powder diffraction (XRD), scanning (SEM) and transmission (TEM) electron microscopy. The XRD patterns, FTIR and Raman spectra proved the presence of g-C_3N_4 at above 550 °C but the optimal synthesis temperature of 600–650 °C was found. Under these conditions graphitic carbon nitride of the overall empirical composition of C_6N_9H_2 was formed. At lower temperatures g-C_3N_4 with a higher content of hydrogen was formed but at higher temperatures g-C_3N_4 was decomposed. At the temperatures above 650 °C, its exfoliation was observed. The photocatalytic experiments showed that the activity of all the samples synthetized at 400–700 °C was very similar, that is, within the range of experimental error (5 %). The total conversion of N_2O reached about 43 % after 14 h. - Highlights: • Graphitic carbon nitride (g-C_3N_4) was thermally synthetized from melamine in the range of 400–700 °C. • The optimal temperature was determined at 600–650 °C. • All synthesis products were properly characterized by physico-chemical methods. • Exfoliation of g-C_3N_4 at above 600 °C was observed. • g-C_3N_4 was used for the photocatalytic decomposition of N_2O.

  18. Synthesis and Characterization of Birnessite and Cryptomelane Nanostructures in Presence of Hoffmeister Anions

    Directory of Open Access Journals (Sweden)

    Marcos A. Cheney

    2009-01-01

    Full Text Available The effect of Hoffmeister anions Cl−, SO42−, and ClO4− on the structure and morphology of birnessite and cryptomelane-type manganese dioxide nanostructures, produced by the reduction reaction of KMnO4 and MnSO4 in aqueous acidic media, was studied. The syntheses were based on the decomposition of aqueous KMnO4 in presence of HCl for birnessite-type and acidified MnSO4 for cryptomelane-type manganese dioxide under soft hydrothermal conditions. They were characterized using X-ray diffraction (XRD, transmission electron microscopy (TEM, and high-resolution transmission electron microscopy (HRTEM techniques. XRD patterns show the formation of birnessite for the first synthesis and a mixture of cryptomelane and birnessite-types MnO2 for the second synthesis. XRD data revealed that the Hoffmeister anions have a significant effect on the nanostructures of birnessite. The sulphate ion-treated birnessite has the smallest crystals, whereas the chloride ion-treated birnessite has the largest crystals. Their TEM and HRTEM studies revealed a transformation from nanoplatelet morphology for chloride-treated samples to nanofibrous morphology for sulphate-treated birnessite. For the cryptomelane nanostructures, Hoffmeister anions also show a profound effect on their crystalline structures as determined by XRD analyses revealing a transformation of the cryptomelane phase to birnessite phase of MnO2. This transformation is also supported by TEM and HRTEM studies.

  19. Synthesis and characterization of arsenic-doped cysteine-capped thoria-based nanoparticles

    International Nuclear Information System (INIS)

    Pereira, F. J.; Díez, M. T.; Aller, A. J.

    2013-01-01

    Thoria materials have been largely used in the nuclear industry. Nonetheless, fluorescent thoria-based nanoparticles provide additional properties to be applied in other fields. Thoria-based nanoparticles, with and without arsenic and cysteine, were prepared in 1,2-ethanediol aqueous solutions by a simple precipitation procedure. The synthesized thoria-based nanoparticles were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM), energy dispersive X-ray spectrometry (ED-XRS), Raman spectroscopy, Fourier transform infrared (FT-IR) spectroscopy and fluorescence microscopy. The presence of arsenic and cysteine, as well as the use of a thermal treatment facilitated fluorescence emission of the thoria-based nanoparticles. Arsenic-doped and cysteine-capped thoria-based nanoparticles prepared in 2.5 M 1,2-ethanediol solutions and treated at 348 K showed small crystallite sizes and strong fluorescence. However, thoria nanoparticles subjected to a thermal treatment at 873 K also produced strong fluorescence with a very narrow size distribution and much smaller crystallite sizes, 5 nm being the average size as shown by XRD and TEM. The XRD data indicated that, even after doping of arsenic in the crystal lattice of ThO 2 , the samples treated at 873 K were phase pure with the fluorite cubic structure. The Raman and FT-IR spectra shown the most characteristics vibrational peaks of cysteine together with other peaks related to the bonds of this molecule to thoria and arsenic when present

  20. Synthesis and characterization of reactions by nanoferrites Co2Fe2O4 combustion

    International Nuclear Information System (INIS)

    Santos, P.T.A.; Dantas, B.B.; Costa, A.C.F.M.; Araujo, P.M.A.G.

    2012-01-01

    In this work CoFe 2 O 4 of magnetic nanoparticles were synthesized by combustion reaction and the structural and morphological characteristics of the synthesized samples as well as the parameters of synthesis temperature and reaction time were investigated in order to assess the reproducibility of the synthesis. The maximum temperature and time of the combustion flame were obtained with pyrometer coupled to a computer with online measurement and a stopwatch. The resulting samples were characterized by X-ray diffraction (XRD), infrared spectroscopy (FTIR) and scanning electron microscopy (SEM). The maximum temperature achieved during synthesis for all reactions ranged from 623 deg C and 755 deg C. The combustion flame time varied between 18 and 23 seconds. The XRD showed the formation of only CoFe 2 O 4 inverse spinel phase, with crystallite size 28 nm and crystallinity 78%, with typical morphology of the formation of agglomerates of uniform size, brittle and comprising nanoparticles together by weak forces. (author)

  1. Synthesis, characterization, and application of two Al(OR(F))3 Lewis superacids.

    Science.gov (United States)

    Kraft, Anne; Trapp, Nils; Himmel, Daniel; Böhrer, Hannes; Schlüter, Peter; Scherer, Harald; Krossing, Ingo

    2012-07-23

    We report herein the synthesis and full characterization of the donor-free Lewis superacids Al(OR(F))(3) with OR(F) = OC(CF(3))(3) (1) and OC(C(5)F(10))C(6)F(5) (2), the stabilization of 1 as adducts with the very weak Lewis bases PhF, 1,2-F(2)C(6)H(4), and SO(2), as well as the internal C-F activation pathway of 1 leading to Al(2)(F)(OR(F))(5) (4) and trimeric [FAl(OR(F))(2)](3) (5, OR(F) = OC(CF(3))(3)). Insights have been gained from NMR studies, single-crystal structure determinations, and DFT calculations. The usefulness of these Lewis acids for halide abstractions has been demonstrated by reactions with trityl chloride (NMR; crystal structures). The trityl salts allow the introduction of new, heteroleptic weakly coordinating [Cl-Al(OR(F))(3)](-) anions, for example, by hydride or alkyl abstraction reactions. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  2. Synthesis and characterization of new oxalate ester-polymer composites for practical applications

    Energy Technology Data Exchange (ETDEWEB)

    Petre, Razvan [Scientific Research Centre for CBRN Defense and Ecology, 225 Sos. Oltenitei, Bucharest 041309 (Romania); University POLITEHNICA of Bucharest, 149 Calea Victoriei, Bucharest 010072 (Romania); Zecheru, Teodora, E-mail: teodora.zecheru@yahoo.com [Scientific Research Centre for CBRN Defense and Ecology, 225 Sos. Oltenitei, Bucharest 041309 (Romania)

    2013-03-15

    The present study focused on the synthesis of high purity oxalate esters: bis(2,4,6-trichlorophenyl) oxalate (TCPO) and bis(2,4,5-trichloro-6-carbobutoxyphenyl) oxalate (TCCBPO), and further on their incorporation into potentially applicative polymer composites. The organic compounds were characterized through NMR and the composites obtained were evaluated for light capacity availability at room temperature and low temperatures. The concentrations of the peroxide, fluorescer, catalyst, and polymer additives were optimized. The chemiluminescent composites' performances were evaluated after 360 days and returned satisfactory results. - Highlights: Black-Right-Pointing-Pointer bis(2,4,6-Trichlorophenyl)-oxalate (TCPO) was synthesized. Black-Right-Pointing-Pointer bis(2,4,5-Trichloro-6-carbobutoxiphenyl)-oxalate (TCCBPO) was synthesized. Black-Right-Pointing-Pointer TCPO and TCCBPO-based composites were obtained. Black-Right-Pointing-Pointer The composites light emission was evaluated versus scotopic visual sensitivity. Black-Right-Pointing-Pointer The new compositions present superior performances within extensive emission time.

  3. Synthesis, Characterization, and Electrochemical Properties of Polyaniline Thin Films

    Science.gov (United States)

    Rami, Soukaina

    Conjugated polymers have been used in various applications (battery, supercapacitor, electromagnetic shielding, chemical sensor, biosensor, nanocomposite, light-emitting-diode, electrochromic display etc.) due to their excellent conductivity, electrochemical and optical properties, and low cost. Polyaniline has attracted the researchers from all disciplines of science, engineering, and industry due to its redox properties, environmental stability, conductivity, and optical properties. Moreover, it is a polymer with fast electroactive switching and reversible properties displayed at low potential, which is an important feature in many applications. The thin oriented polyaniline films have been fabricated using self-assembly, Langmuir-Blodgett, in-situ self-assembly, layer-by-layer, and electrochemical technique. The focus of this thesis is to synthesize and characterize polyaniline thin films with and without dyes. Also, the purpose of this thesis is to find the fastest electroactive switching PANI electrode in different electrolytic medium by studying their electrochemical properties. These films were fabricated using two deposition techniques: in-situ self-assembly and electrochemical deposition. The characterization of these films was done using techniques such as Fourier Transform Infrared Spectroscopy (FTIR), UV-spectroscopy, Scanning Electron Microscope (SEM), and X-Ray Diffraction (XRD). FTIR and UV-spectroscopy showed similar results in the structure of the polyaniline films. However, for the dye incorporated films, since there was an addition in the synthesis of the material, peak locations shifted, and new peaks corresponding to these materials appeared. The 1 layer PANI showed compact film morphology, comparing to other PANI films, which displayed a fiber-like structure. Finally, the electrochemical properties of these thin films were studied using cyclic voltammetry (CV), chronoamperometry (CA), and electrochemical impedance spectroscopy (EIS) in

  4. Synthesis and characterization of nanostructured powders of hydroxyapatite and β-calcium phosphate

    Energy Technology Data Exchange (ETDEWEB)

    Prants, W.T.; Muller, D.T.; Orzechowski, L.G.; Feit, G.; Delima, S.A.; Camargo, N.H.A.; Gemelli, E., E-mail: w_prants@hotmail.com, E-mail: danielt_muller@yahoo.com.br, E-mail: sarahamindelima@hotmail.com, E-mail: dem2nhac@joinville.udesc.br, E-mail: gemelli@joinville.udesc.br [Universidade do Estado de Santa Catarina (UDESC), Joinville, SC (Brazil). Campus Universitario Prof. Avelino Marcante

    2009-07-01

    Biphasic calcium phosphate (BCP) bioceramics are composed in a general manner from a mixture between hydroxyapatite (HA), and β-calcium phosphate. In the recent years, the BCP bioceramics are pointed out in researches from regeneration and reconstitution in osseous tissue, in reason of their similar mineralogical characteristics of the human bone structure, as great biodegradation, absorption and formation of precocious osseous tissue. The biphasic materials (BCP) are detached for use in medical and dental application, as filling bone cavities, maxillofacial treatment, medicaments discharge for treatment cancerous osteomyelitis and antibiotics discharge related with orthopedic injuries reparation. The aim of this work focused in synthesis and characterization of hydroxyapatite and β-calcium phosphate. The presented results are related with the mineralogical characterization with X-ray diffraction, thermal behavior with Differential Scanning Calorimetry and Dilatometer. The Scanning Electronic Microscopy (SEM) was used to help in the morphological characterization of the nanostructured powders. (author)

  5. Synthesis and characterization of nanostructured powders of hydroxyapatite and β-calcium phosphate

    International Nuclear Information System (INIS)

    Prants, W.T.; Muller, D.T.; Orzechowski, L.G.; Feit, G.; Delima, S.A.; Camargo, N.H.A.; Gemelli, E.

    2009-01-01

    Biphasic calcium phosphate (BCP) bioceramics are composed in a general manner from a mixture between hydroxyapatite (HA), and β-calcium phosphate. In the recent years, the BCP bioceramics are pointed out in researches from regeneration and reconstitution in osseous tissue, in reason of their similar mineralogical characteristics of the human bone structure, as great biodegradation, absorption and formation of precocious osseous tissue. The biphasic materials (BCP) are detached for use in medical and dental application, as filling bone cavities, maxillofacial treatment, medicaments discharge for treatment cancerous osteomyelitis and antibiotics discharge related with orthopedic injuries reparation. The aim of this work focused in synthesis and characterization of hydroxyapatite and β-calcium phosphate. The presented results are related with the mineralogical characterization with X-ray diffraction, thermal behavior with Differential Scanning Calorimetry and Dilatometer. The Scanning Electronic Microscopy (SEM) was used to help in the morphological characterization of the nanostructured powders. (author)

  6. Polypyrrole-silver Nanocomposite: Synthesis and Characterization

    Directory of Open Access Journals (Sweden)

    D. M. Nerkar

    2016-07-01

    Full Text Available Polypyrrole-Silver (PPy-Ag nanocomposite has been successfully synthesized by the chemical oxidative polymerization of pyrrole with iron (III chloride as an oxidant, in the presence of a colloidal suspension of silver nanoparticles. Turkevich method (Citrate reduction method was used for the synthesis of silver nanoparticles (Ag NPs. The silver nanoparticles were characterized by UV-Visible spectroscopy which showed an absorption band at 423 nm confirming the formation of nanoparticles. PPy-Ag nanocomposite was characterized by Transmission Electron Microscopy (TEM, Scanning Electron Microscopy (SEM, Fourier Transform Infrared Spectroscopy (FTIR and X-ray diffraction (XRD techniques for morphological and structural confirmations. TEM and SEM images revealed that the silver nanoparticles were well dispersed in the PPy matrix. XRD pattern showed that PPy is amorphous but the presence of the peaks at 2q values of 38.24°, 44.57°, 64.51° and 78.45° corresponding to a cubic phase of silver, revealed the incorporation of silver nanoparticles in the PPy matrix. A possible formation mechanism of PPy-Ag nanocomposite was also proposed. The electrical conductivity of PPy-Ag nanocomposite was studied using two probe method. The electrical conductivity of the PPy-Ag nanocomposite prepared was found to be 4.657´10- 2 S/cm, whereas that of pure PPy was found to be 9.85´10-3 S/cm at room temperature (303 K. The value of activation energy (Ea for pure PPy was 0.045 eV while it decreased to 0.034 eV for PPy-Ag nanocomposite. The synthesized nanocomposite powder can be utilized as a potential material for fabrication of gas sensors operating at room temperature.

  7. Synthesis and characterization of titanium oxide/bismuth sulfide nanorods for solar cells applications

    International Nuclear Information System (INIS)

    Solis, M.; Rincon, M. E.

    2008-01-01

    In the present work is showed the synthesis and characterization of titanium oxide/bismuth sulfide nanowires hetero-junctions for solar cells applications. Conductive glass substrates (Corning 25 x 75 mm) were coated with a thin layer of sol-gel TiO2 and used as substrates for the subsequent deposition of bismuth sulfide nanorods (BN). TiO2 films (∼400 nm) were deposited with a semiautomatic immersion system with controlled immersion/withdraw velocity, using titanium isopropoxide as the titania precursor [1]. For BN synthesis and deposition, the solvo-thermal method was used, introducing air annealed TiO2-substrates in the autoclave. The typical bilayer TiO2/BN hetero-junction was 600 nm thick. The synthesized materials (powders and films) were characterized by X-Ray Diffraction, Scanning Electron Microscopy, and UV-Visible Spectroscopy. Anatase was the crystalline phase of TiO2, while bismuth sulfide nanotubes show a diffraction pattern characteristic of bismuthinite distorted by the preferential growth of some planes [2-4]. The optoelectronic characterization of TiO2/NB hetero-junctions was compared with hetero-junctions obtained by sensitizing TiO2 with chemically deposited bismuth sulfide films. Bismuth sulfide nanowires are 2µm long and 70nm wide (aspect ratio L/D = 43), while chemically deposited bismuth sulfide have L/D = 1, therefore the effect of particle size evaluation and geometry in the photosensitization phenomena will be discussed in the context of new materials for solar-cells applications. (Full text)

  8. Synthesis and Characterization of Polyfunctional Polyhedral Silsesquioxane Cages

    Science.gov (United States)

    Sulaiman, Santy

    Recent studies on octameric polyhedral silsesquioxanes, (RSiO1.5 )8, indicate that the silsesquioxane cage is not just a passive component but appears to be involved in electron delocalization with conjugated organic tethers in the excited state. This dissertation presents the synthesis and characterization of (RSiO1.5)8 molecules with unique photophysical properties that provide support for the existence of conjugation that involves the (RSiO1.5)8 cage. The dissertation first discusses the elaboration of octavinylsilsesquioxane via cross-metathesis to form styrenyl-functionalized octasilsesquioxane molecules. Subsequent Heck coupling reactions of p-bromostyrenyl derivative provides vinylstilbene-functionalized octasilsesquioxane. The amino derivative, NH2VinylStilbeneOS, show highly red-shifted emission spectrum (100 nm from the simple organic analog p-vinylstilbene) and high two-photon absorption (TPA) cross-section value (100 GM/moiety), indicating charge-transfer processes involving the silsesquioxane cage as the electron acceptor. The unique photophysical properties of polyfunctional luminescent cubic silsesquioxanes synthesized from ortho-8-, (2,5)-16-, and 24-brominated octaphenylsilsesquioxane (OPS) via Heck coupling show how the steric interactions of the organic tethers at the silsesquioxane cage corner affect conjugation with the silsesquioxane cage. Furthermore, the high TPA cross-section (10 GM/moiety) and photoluminescence quantum yield (20%) of OPS functionalized with 24 acetoxystyrenyl groups suggest that the existence excited states in these molecules with similar energies and decay rates: normal radiative pi- pi* transition and charge transfer involving the silsesquioxane cage. The fluoride ion-catalyzed rearrangement reactions of cage and polymeric silsesquioxanes provide a convenient route to a mixture of deca- and dodecameric silsesquioxane molecules in high yields, giving us the opportunity to investigate the effect of silsesquioxane cage

  9. Synthesis, characterization, and photocatalytic properties of core/shell mesoporous silica nanospheres supporting nanocrystalline titania

    International Nuclear Information System (INIS)

    Cendrowski, K.; Chen, X.; Zielinska, B.; Kalenczuk, R. J.; Rümmeli, M. H.; Büchner, B.; Klingeler, R.; Borowiak-Palen, E.

    2011-01-01

    The facile bulk synthesis of silica nanospheres makes them an attractive support for the transport of chemical compounds such as nanocrystalline titanium dioxide. In this contribution we present a promising route for the synthesis of mesoporous silica nanospheres (m-SiO 2 ) with diameter in range 200 nm, which are ideal supports for nanocrystalline titanium dioxide (TiO 2 ). The detailed microscopic and spectroscopic characterizations of core/shell structure (m-SiO 2 /TiO 2 ) were conducted. Moreover, the photocatalytic potential of the nanostructures was investigated via phenol decomposition and hydrogen generation. A clear enhancement of photoactivity in both reactions as compared to commercial TiO 2 -Degussa P25 catalyst is detected.

  10. Synthesis, characterization, and photocatalytic properties of core/shell mesoporous silica nanospheres supporting nanocrystalline titania

    Science.gov (United States)

    Cendrowski, K.; Chen, X.; Zielinska, B.; Kalenczuk, R. J.; Rümmeli, M. H.; Büchner, B.; Klingeler, R.; Borowiak-Palen, E.

    2011-11-01

    The facile bulk synthesis of silica nanospheres makes them an attractive support for the transport of chemical compounds such as nanocrystalline titanium dioxide. In this contribution we present a promising route for the synthesis of mesoporous silica nanospheres (m-SiO2) with diameter in range 200 nm, which are ideal supports for nanocrystalline titanium dioxide (TiO2). The detailed microscopic and spectroscopic characterizations of core/shell structure (m-SiO2/TiO2) were conducted. Moreover, the photocatalytic potential of the nanostructures was investigated via phenol decomposition and hydrogen generation. A clear enhancement of photoactivity in both reactions as compared to commercial TiO2-Degussa P25 catalyst is detected.

  11. Synthesis and characterization of rhodium sulfide nanoparticles and thin films

    International Nuclear Information System (INIS)

    Sosibo, Ndabenhle M.; Revaprasadu, Neerish

    2008-01-01

    The synthesis and characterization of a rhodium complex, [Rh(S 2 CNEt 2 ) 2 ] is described. The complex was thermolysed at a high temperature (280 deg. C) in the presence of capping agent, hexadecylamine (HDA) to form Rh 2 S 3 nanoparticles. Rod-shaped Rh 2 S 3 nanoparticles with an average length of 26.7 nm and an average breadth of 7.8 nm were synthesized. The complex was also used as a single molecule precursor for the deposition of Rh 2 S 3 thin films on a glass substrate at 350 deg. C and 450 deg. C using the Aerosol Assisted Chemical Vapour Deposition (AACVD) technique. The resultant thin films showed temperature dependent morphologies and showed (0 2 2), (4 1 1) and (6 1 1) lattice planes characteristic of to the orthorhombic Rh 2 S 3 phase. X-ray diffraction and scanning electron microscopy techniques were used to characterize the films

  12. Synthesis and characterization of rhodium sulfide nanoparticles and thin films

    Energy Technology Data Exchange (ETDEWEB)

    Sosibo, Ndabenhle M. [Department of Chemistry, University of Zululand, Private Bag X1001, KwaDlangezwa 3886 (South Africa); Revaprasadu, Neerish [Department of Chemistry, University of Zululand, Private Bag X1001, KwaDlangezwa 3886 (South Africa)], E-mail: nrevapra@pan.uzulula.za

    2008-05-15

    The synthesis and characterization of a rhodium complex, [Rh(S{sub 2}CNEt{sub 2}){sub 2}] is described. The complex was thermolysed at a high temperature (280 deg. C) in the presence of capping agent, hexadecylamine (HDA) to form Rh{sub 2}S{sub 3} nanoparticles. Rod-shaped Rh{sub 2}S{sub 3} nanoparticles with an average length of 26.7 nm and an average breadth of 7.8 nm were synthesized. The complex was also used as a single molecule precursor for the deposition of Rh{sub 2}S{sub 3} thin films on a glass substrate at 350 deg. C and 450 deg. C using the Aerosol Assisted Chemical Vapour Deposition (AACVD) technique. The resultant thin films showed temperature dependent morphologies and showed (0 2 2), (4 1 1) and (6 1 1) lattice planes characteristic of to the orthorhombic Rh{sub 2}S{sub 3} phase. X-ray diffraction and scanning electron microscopy techniques were used to characterize the films.

  13. Nanoscale Synthesis and Characterization Laboratory Annual Report 2005

    Energy Technology Data Exchange (ETDEWEB)

    Hamza, A V; Lesuer, D R

    2006-01-03

    The Nanoscale Synthesis and Characterization Laboratory's (NSCL) primary mission is to create and advance interdisciplinary research and development opportunities in nanoscience and technology. The initial emphasis of the NSCL has been on development of scientific solutions in support of target fabrication for the NIF laser and other stockpile stewardship experimental platforms. Particular emphasis has been placed on the design and development of innovative new materials and structures for use in these targets. Projects range from the development of new high strength nanocrystalline alloys to graded density materials to high Z nanoporous structures. The NSCL also has a mission to recruit and train personnel for Lab programs such as the National Ignition Facility (NIF), Defense and Nuclear Technologies (DNT), and Nonproliferation, Arms control and International security (NAI). The NSCL continues to attract talented scientists to the Laboratory.

  14. Synthesis of Well-Defined Polyethylene-Based 3-Miktoarm Star Copolymers and Terpolymers

    KAUST Repository

    Zhang, Zhen

    2016-03-25

    Novel polyethylene (PE)-based 3-miktoarm star copolymers A2B, (AB)2B and terpolymers (AC)2(BC) [A: PE; B, C: polystyrene (PS) or poly(methyl methacrylate) (PMMA)] were synthesized by combining boron chemistry, polyhomologation, and atom transfer radical polymerization (ATRP). 1,4-Pentadiene-3-yl 2-bromo-2-methylpropanoate was first synthesized followed by hydroboration with thexylborane to afford B-thexylboracyclanes, a multi-heterofunctional initiator with two initiating sites for polyhomologation and one for ATRP. After polyhomologation of dimethylsulfoxonium methylide the α,ω-dihydroxyl polyethylene (PE-OH)2-Br produced served as macroinitiator for the ATRP of styrene to afford (PE-OH)2-(PS-Br). Both (PE-OH)2-Br and (PE-OH)2-(PS-Br) were transformed to two new trifunctional macroinitiators (PE-Br)2-Br and (PE-Br)2-(PS-Br) through esterification reactions and used for the synthesis of (AB)2B and (AC)2(BC) 3-miktoarm star co/terpolymers. All intermediates and final products were characterized by 1H NMR, high temperature gel permeation chromatography (HT-GPC), and differential scanning calorimetry (DSC). The synthetic method is a general one and can be used for the synthesis of complex PE-based architectures by combination with other living/living-controlled polymerization techniques. © 2016 American Chemical Society.

  15. Synthesis, characterization, and reactivity of furan- and thiophene-functionalized bis(n-heterocyclic carbene) complexes of iron(II)

    KAUST Repository

    Rieb, Julia; Raba, Andreas; Haslinger, Stefan; Kaspar, Manuel; Pö thig, Alexander; Cokoja, Mirza; Basset, Jean-Marie; Kü hn, Fritz

    2014-01-01

    The synthesis of iron(II) complexes bearing new heteroatom-functionalized methylene-bridged bis(N-heterocyclic carbene) ligands is reported. All complexes are characterized by single-crystal X-ray diffraction (SC-XRD), nuclear magnetic resonance

  16. Synthesis, characterization and properties

    Indian Academy of Sciences (India)

    Unknown

    work, we report herein the synthesis, structural cha- racterization and properties of a chiral Mn(IV) mononuclear ... atmosphere with a platinum disc working electrode, a platinum wire auxiliary electrode and a Ag/AgCl ... SMART APEX CCD area detector system [λ(Mo-. Kα) = 0⋅71073 Å], graphite monochromator, 2400.

  17. Synthesis And Characterization Of Mebrofenin For Hepatobiliary Imaging

    International Nuclear Information System (INIS)

    Purwoko; Tamat, Swasono R.; Yunita, Fitri; Kristanti, Eti

    2003-01-01

    Mebrofenin labeled with Technetium-99m is a new radiopharmaceutical having superior and ideal characteristic as a hepatobiliary-imaging agent. The synthesis and characterization of Mebrofenin (3-Bromo-2,4,6-trimethyl acetanilido iminodiacetic acid) as IDA derivative has been carried out involving three steps of reaction i.e. : acetyllization of 2,4,6-Trimethyl aniline to get 2,4,6-trimethyl chloro acetanilide which upon bromination gives the intermediate bromotrimethyl derivative and [mally by nucleophilic substitution this intermediate product with iminodiacetic acid (IDA) gives mebrofenin. The acetylation and bromination reactions were carried out in acetic acid condition while the substitution was carried out by reflux for 5 hours in ethanol and water adjusted at pH 11. The ethanol was then removed under low pressure, and the unreacted compound was removed by filtration. The filtrate was adjusted to pH 2 - 2.5, and the resulting mebrofenin was isolated by filtration and recrystallized 3 times in ethanol. Characterization of the mebrofenin product was performed by observing its melting point (197-l99 o C), ultra violet and infra red spectra as well as mass spectrometric and high performance liquid chromatographic analysis. The results showed that the product was highly pure and the yield was around 20%

  18. New porphyrin-polyoxometalate hybrid materials: synthesis, characterization and investigation of catalytic activity in acetylation reactions.

    Science.gov (United States)

    Araghi, Mehdi; Mirkhani, Valiollah; Moghadam, Majid; Tangestaninejad, Shahram; Mohammdpoor-Baltork, Iraj

    2012-10-14

    New hybrid complexes based on covalent interaction between 5,10,15,20-tetrakis(4-aminophenyl)porphyrinatozinc(II) and 5,10,15,20-tetrakis(4-aminophenyl)porphyrinatotin(IV) chloride, and a Lindqvist-type polyoxometalate, Mo(6)O(19)(2-), were prepared. These new porphyrin-polyoxometalate hybrid materials were characterized by (1)H NMR, FT IR and UV-Vis spectroscopic methods and cyclic voltammetry. These spectro- and electrochemical studies provided several spectral data for synthesis of these compounds. Cyclic voltammetry showed the influence of the polyoxometalate on the redox process of the porphyrin ring. The catalytic activity of tin(IV)porphyrin-hexamolybdate hybrid material was investigated in the acetylation of alcohols and phenols with acetic anhydride. The reusability of this catalyst was also investigated.

  19. Microwave-assisted synthesis and micellization behavior of soy-based copoly(2-oxazoline)s.

    Science.gov (United States)

    Hoogenboom, Richard; Leenen, Mark A M; Huang, Haiying; Fustin, Charles-André; Gohy, Jean-François; Schubert, Ulrich S

    2006-01-01

    Polymers based on renewable resources are promising candidates for replacing common organic polymers, and thus, for reducing oil consumption. In this contribution we report the microwave-assisted synthesis of block and statistical copolymers from 2-ethyl-2-oxazoline and 2-"soy alkyl"-2-oxazoline via a cationic ring-opening polymerization mechanism. The synthesized copolymers were characterized by gel permeation chromatography and 1 H-NMR spectroscopy. The micellization of these amphiphilic copolymers was investigated by dynamic light scattering and atomic force microscopy to examine the effect of hydrophobic block length and monomer distribution on the resulting micellar characteristics.

  20. TUNG OIL BASED MONOMER FOR THERMOSETTING POLYMERS: SYNTHESIS, CHARACTERIZATION AND COPOLYMERIZATION WITH STYRENE

    Directory of Open Access Journals (Sweden)

    Chengguo Liu,

    2011-11-01

    Full Text Available A tung oil (TO based monomer for rigid thermosetting polymer was synthesized, characterized, and copolymerized with styrene in this study. Tung oil was alcoholyzed with pentaerythritol (PER to get tung oil pentaerythritol alcoholysis products (TOPER, and the optimized conditions were explored according to the yields of TOPER analyzed by gas chromatography-mass spectrometry (GC-MS. The resulting alcoholysis products were maleinated to form tung oil maleate half ester (TOPERMA, and the reaction conditions were determined by monitoring the reaction extents of TOPER and maleic anhydride (MA with 1HNMR spectroscopy. The TO alcoholysis and maleinization reaction products were characterized by IR, 1HNMR, and electrospray ionization-mass spectrometry (ESI-MS techniques. At last, the TOPERMA mixture was cured with styrene (St, and the initiator tert-butyl peroxy benzoate (TPB. Differential scanning calorimetry (DSC was employed to characterize the curing process. Mechanical properties of the cured TOPERMA/St resin further confirmed the best procedure for the maleinization reaction. The loading of TO reached about 30% weight of the resulting thermosetting polymer. This promising material from renewable resources can be a potential substitution for petroleum products when used as sheet molding compounds.

  1. Synthesis and characterization of poly aniline/wood and poly aniline/carbon composites

    International Nuclear Information System (INIS)

    Kanwal, F.; Siddiqi, S.A.; Tasleem, S.

    2009-01-01

    Conducting polymers have shown many applications in the field of nano science, nano technology and nuclear science. Poly aniline (PAN I) is the most studied conducting polymer due to its environmental stability, easy availability of its raw materials, and simple synthesis. We have synthesized poly aniline and two of its conducting composites i.e., poly aniline-carbon and poly aniline-wood in acidic medium (HCI) using K/sub 2/Cr/sub 2/O/sub 7/ as oxidizing agent. All samples were characterized by FTIR and four-probe d.c. conductivity methods The synthesis was carried out at two different temperatures (0 degree C and -5 degree C) and it was found that the yield and conductivity were maximum at lower temperature (-5 degree C). The poly aniline-carbon composites showed enhanced conductivity whereas poly aniline-wood composites showed reduced conductivity when compared with the conductivity of pure poly aniline. (author)

  2. Synthesis, structure characterization and catalytic activity of nickel tungstate nanoparticles

    Science.gov (United States)

    Pourmortazavi, Seied Mahdi; Rahimi-Nasrabadi, Mehdi; Khalilian-Shalamzari, Morteza; Zahedi, Mir Mahdi; Hajimirsadeghi, Seiedeh Somayyeh; Omrani, Ismail

    2012-12-01

    Taguchi robust design was applied to optimize experimental parameters for controllable, simple and fast synthesis of nickel tungstate nanoparticles. NiWO4 nanoparticles were synthesized by precipitation reaction involving addition of nickel ion solution to the tungstate aqueous reagent and then formation of nickel tungstate nucleolus which are insoluble in aqueous media. Effects of various parameters such as nickel and tungstate concentrations, flow rate of reagent addition and reactor temperature on diameter of synthesized nickel tungstate nanoparticles were investigated experimentally by the aid of orthogonal array design. The results for analysis of variance (ANOVA) showed that particle size of nickel tungstate can be effectively tuned by controlling significant variables involving nickel and tungstate concentrations and flow rate; while, temperature of the reactor has a no considerable effect on the size of NiWO4 particles. The ANOVA results proposed the optimum conditions for synthesis of nickel tungstate nanoparticles via this technique. Also, under optimum condition nanoparticles of NiWO4 were prepared and their structure and chemical composition were characterized by means of EDAX, XRD, SEM, FT-IR spectroscopy, UV-vis spectroscopy, and photoluminescence. Finally, catalytic activity of the nanoparticles in a cycloaddition reaction was examined.

  3. Synthesis and characterization of iron nano particles for the arsenic removal in water

    International Nuclear Information System (INIS)

    Gutierrez M, O. E.

    2011-01-01

    The synthesis of iron nanoparticles for the removal of metallic ions in polluted waters has been during the last years study topic for different world organizations. This work presents a synthesis method of conditioned coal with iron nanoparticles starting from the use of leaves of pineapple crown, with the purpose of using it in arsenic removal processes in aqueous phase. For the synthesis of this material, the leaves of the pineapple crown were used like supports structure of the iron nanoparticles. First, the pyrolysis appropriate temperature was determined. For the preparation of the support material, this had contact with a ferric nitrate and hexamine solution, because the preparation of the material and the coal synthesis were realized during the pyrolysis process, where the hexamine molecules and the ferric nitrate react, causing the reduction of the iron particles and their dispersion on the support material, obtaining as product a conditioned coal with iron nanoparticles. For the characterization of the materials were used techniques as: Scanning electron microscopy, Transmission electron microscopy, X-Rays Diffraction), X-Ray photoelectron spectroscopy and Moessbauer spectroscopy; moreover was determined the isoelectric point and the density of surface sites. The arsenic sorption capacity of the materials was evaluated by means of the methodology type lots where was determined the sorption kinetics and isotherms in terms of arsenic concentration and mass. (Author)

  4. A cell-based fluorescent assay to detect the activity of AB toxins that inhibit protein synthesis

    Science.gov (United States)

    AB-type protein toxins, produced by numerous bacterial pathogens and some plants, elicit a cytotoxic effect involving the inhibition of protein synthesis. To develop an improved method to detect the inhibition of protein synthesis by AB-type toxins, the present study characterized a Vero cell line t...

  5. Synthesis and characterization of the natural and burned hydrotalcite

    International Nuclear Information System (INIS)

    Granados C, F.

    2006-01-01

    The synthesis and the structural and surface properties of the natural and burned hydrotalcite using salts of AlCl 3 and MgCl 2 .6H 2 O its were studied. Its were used those analysis of BET, IR, XRD, TGA and SEM to characterize these materials. The obtained product was identified as the natural or carbonated hydrotalcite of chemical formula Mg 6 Al 2 (OH) 16 CO 3 .4H 2 O. The hydrotalcite was roasted at 500 C during 5 h and the was obtained roasted hydrotalcite (HTC) that is a material of high selectivity toward the anions that it can be efficiently used as adsorbent material in studies of adsorption for the treatment of anionic radioactive waste present in watery solution. (Author)

  6. SYNTHESIS, CHARACTERIZATION AND BIO-ACTIVITY OF SOME ...

    African Journals Online (AJOL)

    Preferred Customer

    Organophosphorus compounds have wide range of applications in the industrial, agricultural and medicinal chemistry owing to their unique physicochemical and biological properties. Their utility as reagents and potential synthons in organic synthesis is gaining increased attention [1]. Synthesis of a-aminophosphonates, ...

  7. Synthesis and structural characterization of piperazino-modified DNA that favours hybridization towards DNA over RNA

    DEFF Research Database (Denmark)

    Skov, Joan; Bryld, Torsten; Lindegaard, Dorthe

    2011-01-01

    We report the synthesis of two C4'-modified DNA analogues and characterize their structural impact on dsDNA duplexes. The 4'-C-piperazinomethyl modification stabilizes dsDNA by up to 5°C per incorporation. Extension of the modification with a butanoyl-linked pyrene increases the dsDNA stabilizati...

  8. Synthesis and characterization of iron based nanoparticles for novel applications

    Science.gov (United States)

    Khurshid, Hafsa

    The work in this thesis has been focused on the fabrication and characterization of iron based nanoparticles with controlled size and morphology with the aim: (i) to investigate their properties for potential applications in MICR toners and biomedical field and (ii) to study finite size effects on the magnetic properties of the nanoparticles. For the biomedical applications, core/shell structured iron/iron-oxide and hollow shell nanoparticles were synthesized by thermal decomposition of iron organometallic compounds [Fe(CO)5] at high temperature. Core/shell structured iron/iron-oxide nanoparticles have been prepared in the presence of oleic acid and oleylamine. Particle size and composition was controlled by varying the reaction parameters during synthesis. The as-made particles are hydrophobic and not dispersible in water. Water dispersibility was achieved by ligand exchange a with double hydrophilic diblock copolymer. Relaxometery measurements of the transverse relaxation time T2 of the nanoparticles solution at 3 Tesla confirm that the core/shell nanoparticles are an excellent MRI contrast agent using T2 weighted imaging sequences. In comparison to conventionally used iron oxide nanoparticles, iron/iron-oxide core/shell nanoparticles offer four times stronger T2 shortening effect at comparable core size due to their higher magnetization. The magnetic properties were studied as a function of particle size, composition and morphology. Hollow nanostructures are composed of randomly oriented grains arranged together to make a shell layer and make an interesting class of materials. The hollow morphology can be used as an extra degree of freedom to control the magnetic properties. Owing to their hollow morphology, they can be used for the targeted drug delivery applications by filling the drug inside their cavity. For the magnetic toners applications, particles were synthesized by chemically reducing iron salt using sodium borohydride and then coated with polyethylene

  9. Synthesis, Spectral, and In Vitro Antibacterial Studies of Organosilicon(IV) Complexes with Schiff Bases Derived from Amino Acids.

    Science.gov (United States)

    Singh, Har Lal; Singh, Jangbhadur; Mukherjee, A

    2013-01-01

    The present work stems from our interest in the synthesis, characterization, and antibacterial evaluation of organosilicon(IV) complexes of a class of amino-acid-based Schiff base which have been prepared by the interaction of ethoxytrimethylsilane with the Schiff bases (N OH) in 1 : 1 molar ratio. These complexes have been characterized by elemental analysis, molar conductance, and spectroscopic studies including electronic IR and NMR ((1)H, (13)C, and (29)Si) spectroscopy. The analytical and spectral data suggest trigonal bipyramidal geometry around the silicon atom in the resulting complexes. The ligands and their organosilicon complexes have also been evaluated for in vitro antimicrobial activity against bacteria (Bacillus cereus, Nocardia spp., E. aerogenes, Escherichia coli, Klebsiella spp., and Staphylococcus spp.). The complexes were found to be more potent as compared to the ligands.

  10. Creating wavelet-based models for real-time synthesis of perceptually convincing environmental sounds

    Science.gov (United States)

    Miner, Nadine Elizabeth

    1998-09-01

    This dissertation presents a new wavelet-based method for synthesizing perceptually convincing, dynamic sounds using parameterized sound models. The sound synthesis method is applicable to a variety of applications including Virtual Reality (VR), multi-media, entertainment, and the World Wide Web (WWW). A unique contribution of this research is the modeling of the stochastic, or non-pitched, sound components. This stochastic-based modeling approach leads to perceptually compelling sound synthesis. Two preliminary studies conducted provide data on multi-sensory interaction and audio-visual synchronization timing. These results contributed to the design of the new sound synthesis method. The method uses a four-phase development process, including analysis, parameterization, synthesis and validation, to create the wavelet-based sound models. A patent is pending for this dynamic sound synthesis method, which provides perceptually-realistic, real-time sound generation. This dissertation also presents a battery of perceptual experiments developed to verify the sound synthesis results. These experiments are applicable for validation of any sound synthesis technique.

  11. Synthesis and characterization of zeolite from coal fly ash

    Science.gov (United States)

    Liu, Yong; Luo, Qiong; Wang, Guodong; Li, Xianlong; Na, Ping

    2018-05-01

    Fly ash (FA) from coal-based thermal power plant was used to synthesize zeolite in NaOH solution with hydrothermal method in this work. Firstly, the effects of calcination and acid treatment on the removal of impurities in fly ash were studied. Then based on the pretreated FA, the effects of alkali concentration, reaction temperature and Si/Al ratio on the synthesis of zeolite were studied in detail. The mineralogy, morphology, thermal behavior, infrared spectrum and specific surface for the synthetic sample were investigated. The results indicated that calcination at 750 °C for 1.5 h can basically remove unburned carbon from FA, and 4 M hydrochloric acid treatment of calcined FA at 90 °C for 2 h will reduce the quality of about 34.3%wt, which are mainly iron, calcium and sulfur elements. The concentration of NaOH, reaction temperature and Si/Al ratio have important effect on the synthesis of zeolite. In this study, 0.5 M NaOH cannot obtain any zeolite. High temperature is beneficial to zeolite synthesis from FA, but easily lead to a variety of zeolites. The synthetic sample contains three kinds of zeolites such as zeolite P, sodalite and zeolite X, when the reaction conditions are 2 M NaOH and 120 °C for 24 h. In this research, quartz always exists in the synthetic sample, but will reduce with the increase of temperature. The synthetic zeolite has the specific surface area of about 42 m2 g‑1 and better thermal stability.

  12. Synthesis and characterization of palm oil fuel ash (POFA) and metakaolin based geopolymer for possible application in nanocoating

    Science.gov (United States)

    Khan, Ihsan Ullah; Bhat, A. H.; Masset, Patrick J.; Khan, Farman Ullah; Rehman, Wajid Ur

    2016-11-01

    The main aim of this study was to synthesize and characterize highly amorphous geopolymer from palm oil fuel ash (POFA) and metakaolin, to be used as nanocoating. Geopolymers are man-made aluminosilicate materials that are amorphous analogues of zeolites. The geopolymers were made by condensing a mixture of raw materials metakaolin and palm oil fuel ash (POFA) with alkaline activator at a fixed ratio at room temperature. The kaolin type clay was calcined at 700 °C for 4hrs to transform it into amorphous metakaolin which is more reactive precursor for geopolymer formation. The characteristics of metakaolin and geopolymers (metakaolin and palm oil fuel ash based geopolymers) were analyzed by using x-ray fluorescence (XRF), Fourier transform infra-red spectrometry (FTIR), Thermogravimetric analysis (TG/DTA) and scanning electron microscopy with energy dispersive x-ray analysis (SEM-EDX). FTIR revealed the presence of Al-O and Si-O stretching vibrations of amorphous alumino-silicate structure for metakaolin, palm oil fuel ash and geopolymers. SEM-EDX images showed the presence of reaction product complementary to NASH (N = Na2O, A = Al2O3, S = SiO2, H = H2O) solid. The resulting geopolymers that were synthesized with NaOH/Na2SiO3 solution cured at 60 °C for 3 days. The results demonstrated the suitability of metakaolin and palm oil fuel ash (POFA) for synthesis of geopolymer at room temperatures.

  13. Copper nanoparticles mediated by chitosan: synthesis and characterization via chemical methods.

    Science.gov (United States)

    Usman, Muhammad Sani; Ibrahim, Nor Azowa; Shameli, Kamyar; Zainuddin, Norhazlin; Yunus, Wan Md Zin Wan

    2012-12-14

    Herein we report a synthesis of copper nanoparticles (Cu-NPs) in chitosan (Cts) media via a chemical reaction method. The nanoparticles were synthesized in an aqueous solution in the presence of Cts as stabilizer and CuSO(4)·5H(2)O precursor. The synthesis proceeded with addition of NaOH as pH moderator, ascorbic acid as antioxidant and hydrazine( )as the reducing agent. The characterization of the prepared NPs was done using ultraviolet-visible spectroscopy, which showed a 593 nm copper band. The Field Emission Scanning Electron Microscope (FESEM) images were also observed, and found to be in agreement with the UV-Vis result, confirming the formation of metallic Cu-NPs. The mean size of the Cu-NPs was estimated to be in the range of 35-75 nm using X-ray diffraction. XRD was also used in analysis of the crystal structure of the NPs. The interaction between the chitosan and the synthesized NPs was studied using Fourier transform infrared (FT-IR) spectroscopy, which showed the capping of the NPs by Cts.

  14. Synthesis and characterization of polyglycerols dendrimers for applications in tissue engineering biological

    Energy Technology Data Exchange (ETDEWEB)

    Passos, E.D.; Queiroz, A.A.A. de [Universidade Federal de Itajuba (UNIFEI), MG (Brazil)

    2014-07-01

    Full text: Introduction: Over the last twenty years is the growing development in the manufacture of synthetic scaffold in tissue engineering applications. These new materials are based on polyglycerol dendrimers (PGLD's). PGLD's are highly functional polymers with hydroxymethyl side groups, fulfill all structural prerequisites to replace poly(ethylene glycol)s in medical applications. Furthermore, since these materials are based on naturally occurring compounds that degrades over time in the body and can be safely excreted. The objective of this work was the synthesis, physicochemical, biological characterization of HPGL's with potential use as scaffolds in tissue engineering. HPGL's with oligomeric cores, of diglycerol triglycerol and tetraglycerol was used. Theoretical and Experimental Simulation Details: The synthesis of PGLD procedures involves the etherification of glycerol through anionic polymerization of glycidol. The PGLD's were characterized by chromatographic techniques (SEC and HPLC), spectroscopic (FTIR, 1H-NMR and 13C - NMR) electrochemical (zeta potential) and thermal analysis (DSC and TGA) techniques. The structure- activity relationships (SAR's) of compound prototype and its analogs were studied to determine the generation number (G) of the molecule responsible for the biological activity on the adhesion and cell proliferation process. A detailed study of the structure of PGLD's of G=0-4 was performed using the Hyperchem 7. 5 and Gromacs 4 software packages. The biocompatibility studies were studied by scanning electron microscopy (SEM) and fluorescence microscopy (EPF) technique after PGLD (G=0-4) blood contact. The overall electro-negativity/total charge density, dipole moment, frontier orbital's (HOMO - LUMO) and electrostatic potential maps (EPM) were calculated. The most stable form of the resulting compounds was determined by estimating the hydration energy and energy conformation. Results and

  15. Tunable synthesis of copper nanotubes

    International Nuclear Information System (INIS)

    Kaniukov, E; Yakimchuk, D; Kozlovsky, A; Shlimas, D; Zdorovets, M; Kadyrzhanov, K

    2016-01-01

    Simple method of tunable synthesis of copper nanotubes based on template synthesis was developed. A comprehensive study of the structural, morphological and electrical characteristics of the obtained nanostructures was carried out. Characterization of structural features was made by methods of scanning electron microscopy, energy dispersive spectroscopy and X-ray diffractometry analysis. Evaluation of wall thickness is made by methods of gas permeability. Electrical conductivity of nanotubes was define in the study of their current-voltage characteristics. The possibility to control of copper nanotubes physical properties by variation of the deposition parameters was shown. (paper)

  16. Novel Green Synthesis and Characterization of Nanopolymer ...

    African Journals Online (AJOL)

    Purpose: To develop a novel approach to green synthesis of nano-polymer porous gold oxide nanoparticles, and examine the effects of the temperatures on their surface. Methods: Green synthesis of nano-polymer porous gold oxide nanoparticles (GONPs) using cetyle trimethylammonium bromide (CTAB) surfactant with a ...

  17. Size control synthesis and characterization of ZnO nanoparticles and its application as ZnO-water based nanofluid in heat transfer enhancement in light water nuclear reactor

    Energy Technology Data Exchange (ETDEWEB)

    Sharma, Deepak; Pandey, Krishna Murari [National Institute of Technology Silchar, Assam (India). Dept. of Mechanical Engineering

    2017-03-15

    A novel and facile approach for size-tunable synthesis of ZnO nanoparticle (NPs) is reported. Size-tuning was attained by using PEG (polyethylene glycol) of molecular weights 400 and 4000. ZnO NPs was synthesized using homogeneous chemical precipitation followed by hydrothermal. Here triethylamine (TEA) was used as a hydroxylating agent. As-synthesized ZnO NPs were characterized by powder X-ray diffraction (XRD), transmission electron microscopy (TEM) and Energy Dispersive Spectroscopy (EDS) analysis. Synthesized ZnO nanoparticle was used for the preparation of ZnO-water based nanofluid and its application in heat transfer enhancement in light water nuclear reactor. In this work, ZnO-water based nanofluid of different volume concentration (1%, 2% and 3%) and particle size of 10 nm and 20 nm is used for enhancement in heat transfer in annular channel by using two phase approach. The particle size of 10 nm gives better result for enhancing the heat transfer rate in comparison to 20 nm particle size in nuclear reactor.

  18. Synthesis and antibacterial characterization of sustainable nanosilver using naturally-derived macromolecules

    Energy Technology Data Exchange (ETDEWEB)

    Osonga, Francis J.; Kariuki, Victor M.; Yazgan, Idris; Jimenez, Apryl; Luther, David; Schulte, Jürgen; Sadik, Omowunmi A., E-mail: osadik@binghamton.edu

    2016-09-01

    Greener nanosynthesis utilizes fewer amounts of materials, water, and energy; while reducing or replacing the need for organic solvents. A novel approach is presented using naturally-derived flavonoids including Quercetin pentaphosphate (QPP), Quercetin sulfonic acid (QSA) and Apigenin Triphosphate (ATRP). These water soluble, phosphorylated flavonoids were utilized both as reducing agent and stabilizer. The synthesis was achieved at room temperature using water as a solvent and it requires no capping agents. The efficiency of the resulting silver nanoparticle synthesis was compared with naturally-occurring flavonoid such as Quercetin (QCR). Results show that QCR reduced Ag{sup +} faster followed by QPP, QSA and ATRP respectively. This is the first evidence of direct utilization of QCR for synthesis of silver nanoparticles (AgNPs) in water. The percentage conversion of Ag{sup +} to Ag{sup 0} was determined to be 96% after 35 min. The synthesized nanoparticles were characterized using Transmission electron microscopy (TEM), Energy dispersive absorption spectroscopy (EDS), UV–vis spectroscopy, High resolution TEM (HR-TEM) with selected area electron diffraction (SAED). The particle sizes ranged from 2 to 80 nm with an average size of 22 nm and in the case of ATRP, the nanoparticle shapes varied from spherical to hexagonal with dispersed particle size ranging from 2 to 30 nm. Crystallinity was confirmed by XRD and the SAED of (111), (200), and the fringes observed in HRTEM images. Results were in agreement with the UV resonance peaks of 369–440 nm. The particles also exhibit excellent antibacterial activity against Staphylococcus epidermidis, Escherichia coli and Citrobacter freundii in water. - Highlights: • Greener nanosilver prepared using flavonoid derivatives • Synthesized nanosilver exhibits exhibit antibacterial activity. • Approach suitable for industrial synthesis.

  19. SYNTHESIS, CHARACTERIZATION AND DENSITY FUNCTIONAL ...

    African Journals Online (AJOL)

    Preferred Customer

    We synthesized a number of aniline derivatives containing acyl groups to compare their barriers of rotation around ... KEY WORDS: Monoacyl aniline, Synthesis, Density functional theory, Rotation barrier. INTRODUCTION. Developments in ...

  20. Synthesis of new Schiff bases as materials for the design of ...

    African Journals Online (AJOL)

    Synthesis of new Schiff bases as materials for the design of photovoltaics cells. ... We describe the synthesis of new organic Schiff bases chromophores 5 containing a rhodanine-3- acetic as electron accepteur moiety. Imines 3 were obtained by a condensation reaction from a lead molecule, the aminothiazolinethione 1 with ...

  1. Synthesis and study of nano-structured cellulose acetate based materials for energy applications

    International Nuclear Information System (INIS)

    Fischer, F.

    2006-12-01

    Nano-structured materials have unique properties (high exchange areas, containment effect) because of their very low characteristic dimensions. The elaboration way set up in this PhD work consists in applying the classical processes for the preparation of aerogel-like materials (combining sol-gel synthesis and CO 2 supercritical extraction) to cellulosic polymers. This work is divided in four parts: a literature review, the presentation and the study of the chemical synthesis that leads to cellulose acetate-based aerogel, the characterizations (chemical, structural and thermal) of the elaborated nano-materials, and finally the study of the first carbons that were obtained after pyrolysis of the organic matrix. The formulations and the sol-gel protocol lead to chemical gels by crosslinking cellulose acetate using a poly-functional iso-cyanate. The dry materials obtained after solvent extraction with supercritical CO 2 are nano-structured and mainly meso-porous. Correlations between chemical synthesis parameters (reagent concentrations, crosslinking rate and degree of polymerisation) and porous properties (density, porosity, pore size distribution) were highlighted thanks to structural characterizations. An ultra-porous reference aerogel, with a density equals to 0,245 g.cm -3 together with a meso-porous volume of 3,40 cm 3 .g -1 was elaborated. Once in granular shape, this material has a thermal conductivity of 0,029 W.m -1 .K -1 . In addition, carbon materials produced after pyrolysis of the organic matrix and after grinding are nano-structured and nano-porous, even if important structural modifications have occurred during the carbonization process. The elaborated materials are evaluated for applications in relation with energy such as thermal insulation (organic aerogels) but also for energy conversion and storage through electrochemical way (carbon aerogels). (author)

  2. Tuned apatitic materials: Synthesis, characterization and potential antimicrobial applications

    Science.gov (United States)

    Fierascu, Irina; Fierascu, Radu Claudiu; Somoghi, Raluca; Ion, Rodica Mariana; Moanta, Adriana; Avramescu, Sorin Marius; Damian, Celina Maria; Ditu, Lia Mara

    2018-04-01

    Inorganic antimicrobial materials can be viable for multiple applications (related to its use for new buildings with special requirements related to microbiological loading, such as hospital buildings and for consolidation of cultural heritage constructions); also the use of substituted hydroxyapatites for protection of stone artefacts against environmental factors (acidic rain) and biodeterioration it's an option to no longer use of toxic substances. This paper presents methods of synthesis and characterization of the material from the point of view of the obtained structures and final applications. The materials were characterized in terms of composition and morphology (using X-ray Diffraction, X-ray Fluorescence, Inductively coupled plasma-atomic emission spectrometry, Fourier Transform Infrared Spectroscopy, X-ray Photoelectron Spectroscopy, Surface area and pore size determination). Antimicrobial activity was tested against filamentous fungi strains and pathogenic bacteria strains, using both spot on lawn qualitative method (on agar medium) and serial microdilution quantitative method (in broth medium). Further, it was evaluated the anti-biofilm activity of the tested samples toward the most important microbial strains implicated in biofilm development, using crystal violet stained biofilms microtiter assay, followed by spectrophotometric quantitative evaluation.

  3. SYNTHESIS AND CHARACTERIZATION OF FUNCTIONALIZED ...

    African Journals Online (AJOL)

    In addition, these compounds have emerged as potential calcium ... As a consequence, the synthesis of dihydropyrimidinone derivatives has ..... Ramazani, A.; Shaghaghi,Z.; Aghahosseini, H.; Asiabi, P.A.; Joo, S.W. Silica nanoparticles.

  4. Synthesis and characterization of functional magnetic nanocomposites

    Science.gov (United States)

    Gass, J.; Sanders, J.; Srinath, S.; Srikanth, H.

    2006-03-01

    Magnetic nanoparticles and carbon nanotubes have been excellent functional materials that could be dispersed in polymer matrices for various applications. However, uniform dispersion of particles in polymers without agglomeration is quite challenging. We have fabricated PMMA/polypyrrole bilayer structures embedded with Fe3O4 magnetite nanoparticles synthesized using wet chemical synthesis. Agglomeration-free dispersion of nanoparticles was achieved by coating the particles with surfactants and by dissolving both the particles and PMMA in chlorobenzene. Structural characterization was done using XRD and TEM. Magnetic properties of the bilayer structures indicated superparamagnetic behavior that is desirable for RF applications as the magnetic losses are reduced. Our polymer nanocomposite bilayer films with conducting polymer coatings are potential candidates for tunable RF applications with integrated EMI suppression. We will also report on our studies of pumped ferrofluids flowing past carbon nanotubes that are arranged in microchannel arrays. Magnetization under various flow conditions is investigated and correlated with the hydrodynamic properties. This scheme provides a novel method of energy conversion and storage using nanocomposite materials.

  5. Synthesis, spectroscopic characterization and catalytic oxidation ...

    Indian Academy of Sciences (India)

    were characterized by infrared, electronic, electron paramagnetic resonance ... The catalytic oxidation property of ruthenium(III) complexes were also ... cies at room temperature. ..... aldehyde part of Schiff base ligands, catalytic activ- ity of new ...

  6. Boron-doped diamond electrode: synthesis, characterization, functionalization and analytical applications.

    Science.gov (United States)

    Luong, John H T; Male, Keith B; Glennon, Jeremy D

    2009-10-01

    In recent years, conductive diamond electrodes for electrochemical applications have been a major focus of research and development. The impetus behind such endeavors could be attributed to their wide potential window, low background current, chemical inertness, and mechanical durability. Several analytes can be oxidized by conducting diamond compared to other carbon-based materials before the breakdown of water in aqueous electrolytes. This is important for detecting and/or identifying species in solution since oxygen and hydrogen evolution do not interfere with the analysis. Thus, conductive diamond electrodes take electrochemical detection into new areas and extend their usefulness to analytes which are not feasible with conventional electrode materials. Different types of diamond electrodes, polycrystalline, microcrystalline, nanocrystalline and ultrananocrystalline, have been synthesized and characterized. Of particular interest is the synthesis of boron-doped diamond (BDD) films by chemical vapor deposition on various substrates. In the tetrahedral diamond lattice, each carbon atom is covalently bonded to its neighbors forming an extremely robust crystalline structure. Some carbon atoms in the lattice are substituted with boron to provide electrical conductivity. Modification strategies of doped diamond electrodes with metallic nanoparticles and/or electropolymerized films are of importance to impart novel characteristics or to improve the performance of diamond electrodes. Biofunctionalization of diamond films is also feasible to foster several useful bioanalytical applications. A plethora of opportunities for nanoscale analytical devices based on conducting diamond is anticipated in the very near future.

  7. Synthesis and characterization of an additive type super plasticizers obtained from plastics cups of polystyrene

    International Nuclear Information System (INIS)

    Araujo, Carolina G.L.; Freire, Carolina B.; Tello, Cledola C. de O.

    2013-01-01

    This paper aims to describe the synthesis of an additive type superplasticizer from alternative material - plastic cups used of polystyrene - and characterize it physically and chemically in order to verify their efficiency and compare it with a commercial use superplasticizer. Following the search, the synthesized superplasticizer is used in mortars to assess their efficiency

  8. Synthesis, Characterization and Utility of Carbon Nanotube Based Hybrid Sensors in Bioanalytical Applications

    Science.gov (United States)

    Badhulika, Sushmee

    The detection of gaseous analytes and biological molecules is of prime importance in the fields of environmental pollution control, food and water - safety and analysis; and medical diagnostics. This necessitates the development of advanced and improved technology that is reliable, inexpensive and suitable for high volume production. The conventional sensors are often thin film based which lack sensitivity due to the phenomena of current shunting across the charge depleted region when an analyte binds with them. One dimensional (1-D) nanostructures provide a better alternative for sensing applications by eliminating the issue of current shunting due to their 1-D geometries and facilitating device miniaturization and low power operations. Carbon nanotubes (CNTs) are 1-D nanostructures that possess small size, high mechanical strength, high electrical and thermal conductivity and high specific area that have resulted in their wide spread applications in sensor technology. To overcome the issue of low sensitivity of pristine CNTs and to widen their scope, hybrid devices have been fabricated that combine the synergistic properties of CNTs along with materials like metals and conducting polymers (CPs). CPs exhibit electronic, magnetic and optical properties of metals and semiconductors while retaining the processing advantages of polymers. Their high chemical sensitivity, room temperature operation and tunable charge transport properties has made them ideal for use as transducing elements in chemical sensors. In this dissertation, various CNT based hybrid devices such as CNT-conducting polymer and graphene-CNT-metal nanoparticles based sensors have been developed and demonstrated towards bioanalytical applications such as detection of volatile organic compounds (VOCs) and saccharides. Electrochemical polymerization enabled the synthesis of CPs and metal nanoparticles in a simple, cost effective and controlled way on the surface of CNT based platforms thus resulting in

  9. Synthesis, characterization of novel chitosan based water dispersible polyurethanes and their potential deployment as antibacterial textile finish.

    Science.gov (United States)

    Arshad, Noureen; Zia, Khalid Mahmood; Jabeen, Farukh; Anjum, Muhammad Naveed; Akram, Nadia; Zuber, Mohammad

    2018-05-01

    Our current research work comprised of synthesis of a series of novel chitosan based water dispersible polyurethanes. The synthesis was carried out in three steps, in first step, the NCO end capped PU-prepolymer was formed through the reaction between Polyethylene glycol (PEG) (Mn = 600), Dimethylolpropionic acid (DMPA) and Isophorone diisocyanate (IPDI). In second step, the neutralization step was carried out by using Triethylamine (TEA) which resulted the formation of neutralized NCO terminated PU-prepolymer, after that the last step chain extension was performed by the addition of chitosan and followed the formation of dispersion by adding calculated amount of water. The proposed structure of CS-WDPUs was confirmed by using FTIR technique. The antimicrobial activities of the plain weave poly-cotton printed and dyed textile swatches after application of CS-WDPUs were also evaluated. The results showed that the chitosan incorporation in to PU backbone has markedly enhanced the antibacterial activity of WDPUs. These synthesized CS-WDPUs are eco-friendly antimicrobial finishes (using natural bioactive agents such as chitosan) with potential applications on polyester/cotton textiles. Copyright © 2018 Elsevier B.V. All rights reserved.

  10. Synthesis and characterization of surfactant assisted Mn2+ doped ZnO nanocrystals

    Directory of Open Access Journals (Sweden)

    N. Shanmugam

    2016-09-01

    Full Text Available We report the synthesis and characterization of Mn doped ZnO nanocrystals, both in the free standing and PVP capped particle forms. The nanocrystals size could be controlled by capping them with polyvinylpyrollidone and was estimated by X-ray diffraction and transmission electron microscopy. The chemical compositions of the products were characterized by FT-IR spectroscopy. UV–Vis absorption spectroscopy measurements reveal that the capping of ZnO leads to blue shift due to quantum confinement effect. The morphology of the particles was evaluated by Scanning Electron Microscopy (SEM and Transmission Electron Microscopy (TEM. Both the Thermo Gravimetric Analysis (TGA and Differential Thermal Analysis (DTA curves of the ZnO show no further weight loss and thermal effect at a temperature above 510 °C.

  11. Synthesis and characterization of multicolour fluorescent ...

    Indian Academy of Sciences (India)

    ... of latent fingerprints. The optical and structural characterization of the nanoparticles was carried .... by absorption of phonons from the host matrix [13], the exchange of energy in ... impressions based on the fluorescent properties exhibited by.

  12. Synthesis and characterization of oxovanadium (IV) dithiocarbamates with pyridine

    Energy Technology Data Exchange (ETDEWEB)

    Doadrio, Antonio L.; Sotelo, Jose; Fernandez-Ruano, Ana [Universidad Complutense, Madrid (Spain). Facultad de Farmacia. Dept. de Quimica Inorganica y Bioinorganica]. E-mail: antoniov@farm.ucm.es

    2002-07-01

    We report the synthesis and study of a new series of oxovanadium (IV) dithiocarbamate adducts and derivatives with pyridine and cyclohexyl, di-iso-butyl, di-n-propyl, aniline, morpholine, piperidine and di-iso-propyl amines. The complexes have been characterized by analytical, magneto chemical, IR, visible-UV spectral and thermal studies, and are assigned the formulas [VO(L){sub 2}].py, where L=cyclohexyl, di-iso-butyl, di-n-propyl, aniline dithiocarbamate and [VO(OH)(L)(py){sub 2}] OH.H{sub 2}O (L=morpholine, piperidine and di-iso-propyl dithiocarbamate). The effect of the adduct formation on the p{sub V=0} bound is discussed in terms of the IR (V=O, V-S and V-N stretching frequencies) and electronic spectra (d-d transitions). (author)

  13. Synthesis and characterization of monodispersed orthorhombic manganese oxide nanoparticles produced by Bacillus sp. cells simultaneous to its bioremediation

    Energy Technology Data Exchange (ETDEWEB)

    Sinha, Arvind [Enzyme and Microbial Biochemistry Laboratory, Department of Chemistry, Indian Institute of Technology, Delhi, Hauz Khas, New Delhi 110 016 (India); Singh, Vidya Nand; Mehta, Bodh Raj [Thin Film Laboratory, Department of Physics, Indian Institute of Technology, Delhi Hauz Khas, New Delhi 110016 (India); Khare, Sunil Kumar, E-mail: skhare@rocketmail.com [Enzyme and Microbial Biochemistry Laboratory, Department of Chemistry, Indian Institute of Technology, Delhi, Hauz Khas, New Delhi 110 016 (India)

    2011-08-30

    Highlights: {yields} An efficient process wherein remediated manganese is synthesized into nanoparticles. {yields} A microbial process for manganese nanoparticle synthesis from metal waste streams. {yields} Nanoparticles characterized as monodispersed, spherical and 4.62 {+-} 0.14 nm sized MnO{sub 2}. -- Abstract: A heavy metal resistant strain of Bacillus sp. (MTCC10650) is reported. The strain exhibited the property of bioaccumulating manganese, simultaneous to its remediation. The nanoparticles thus formed were characterized and identified using energy dispersive X-ray analysis (EDAX), high resolution transmission electron microscopy (HRTEM), X-ray photoelectron spectroscopy (XPS), powder X-ray diffraction (PXRD) and atomic force microscopy (AFM). When the cells were challenged with manganese, the cells effectively synthesized nanoparticles of average size 4.62 {+-} 0.14 nm. These were mostly spherical and monodispersed. The ex situ enzymatically synthesized nanoparticles exhibited an absorbance maximum at 329 nm. These were more discrete, small and uniform, than the manganese oxide nanoparticles recovered after cell sonication. The use of Bacillus sp. cells seems promising and advantageous approach. Since, it serves dual purposes of (i) remediation and (ii) nanoparticle synthesis. Considering the increasing demand of developing environmental friendly and cost effective technologies for nanoparticle synthesis, these cells can be exploited for the remediation of manganese from the environment in conjunction with development of a greener process for the controlled synthesis of manganese oxide nanoparticles.

  14. Synthesis and characterization of monodispersed orthorhombic manganese oxide nanoparticles produced by Bacillus sp. cells simultaneous to its bioremediation

    International Nuclear Information System (INIS)

    Sinha, Arvind; Singh, Vidya Nand; Mehta, Bodh Raj; Khare, Sunil Kumar

    2011-01-01

    Highlights: → An efficient process wherein remediated manganese is synthesized into nanoparticles. → A microbial process for manganese nanoparticle synthesis from metal waste streams. → Nanoparticles characterized as monodispersed, spherical and 4.62 ± 0.14 nm sized MnO 2 . -- Abstract: A heavy metal resistant strain of Bacillus sp. (MTCC10650) is reported. The strain exhibited the property of bioaccumulating manganese, simultaneous to its remediation. The nanoparticles thus formed were characterized and identified using energy dispersive X-ray analysis (EDAX), high resolution transmission electron microscopy (HRTEM), X-ray photoelectron spectroscopy (XPS), powder X-ray diffraction (PXRD) and atomic force microscopy (AFM). When the cells were challenged with manganese, the cells effectively synthesized nanoparticles of average size 4.62 ± 0.14 nm. These were mostly spherical and monodispersed. The ex situ enzymatically synthesized nanoparticles exhibited an absorbance maximum at 329 nm. These were more discrete, small and uniform, than the manganese oxide nanoparticles recovered after cell sonication. The use of Bacillus sp. cells seems promising and advantageous approach. Since, it serves dual purposes of (i) remediation and (ii) nanoparticle synthesis. Considering the increasing demand of developing environmental friendly and cost effective technologies for nanoparticle synthesis, these cells can be exploited for the remediation of manganese from the environment in conjunction with development of a greener process for the controlled synthesis of manganese oxide nanoparticles.

  15. Synthesis and transport characterization of electrochemically deposited CdTe nanowires

    Science.gov (United States)

    Kaur, Jaskiran; Kaur, Harmanmeet; Singh, R. C.

    2018-04-01

    This paper reports the synthesis and characterization of CdTe nanowires. A thin polymeric films were irradiated with 80MeV Ag ions at a fluence of 8E7 ions/cm2, followed by UV irradiation and chemically etching in aqueous NaOH. Nanosizes go-through pores so formed were filled using a specially designed cell via electrodeposition. Nanowires so formed were further studied using SEM, I-V, UV and XRD analysis. SEM images show very smooth and uniform CdTe nanowires freely standing on the substrate. The in-situ I-V characteristics of nano-/micro structures was carried out at room temperature by leaving the structures embedded in the insulating template membrane itself.

  16. Synthesis of new radiotracers based on aniline

    International Nuclear Information System (INIS)

    Ayari, Issra

    2008-01-01

    There are several possible applications of radioactivity, we cite: the study of the functional and neurochirnical aspects related to the brain. This study requires the synthesis of specific radiotracers able to cross their target tissue. The synthesis methods need to be constantly updated to respond to the big demand of this domain. The development of the chemistry of metal complexes helped us to find a stable radiotracer based on aniline and marked with technetium. This stability aI 10wed us to realize a possible biodistribution and to envisage to count the radioactivity and to valid the radiopharmaceutical. (Author)

  17. Synthesis and characterization of PMMA/clay nanocomposites prepared by in situ polymerization assisted by sonication

    International Nuclear Information System (INIS)

    Prado, Bruna R.; Bartoli, Julio R.; Ito, Edson N.

    2015-01-01

    In this work is presented the synthesis of nanocomposites of poly(methyl methacrylate), PMMA, with organically montmorillonite (OMMT) modified clays by in situ polymerization assisted by sonication. A statistically designed experiment was used, central composing design (CCD), to study the effect of synthesis variables on the dispersion of nanoparticles in PMMA matrix. The processing and formulation factors studied were: energy of sonication and Flory-Huggins interaction parameter between PMMA and organoclay. The structural (XRD) and morphological (TEM) characterizations of the PMMA/OMMT nanocomposites are compared with the literature. It was observed significant exfoliation of OMMT modified with hydroxyl groups in the nanocomposites of PMMA, mainly at the low ultrasonic energy level (90 and 105 kJ) studied. (author)

  18. Hyperbranched Polyethylenebased Macromolecular Architectures: Synthesis, Characterization, and Selfassembly

    KAUST Repository

    Al-Sulami, Ahlam

    2018-05-01

    "Chain walking” catalytic polymerization CWCP is a powerful tool for the one-pot synthesis of a unique class of hyperbranched polyethylene HBPE-based macromolecules with a controllable molecular weight, topology, and composition. This dissertation focuses on new synthetic routes to prepare HBPE-based macromolecular architectures by combining the CWCP technique with ring opening polymerization ROP, atom–transfer radical polymerization ATRP, and “click” chemistry. Taking advantage of end-functionalized HBPE, and a new ethynyl-soketal star-shape agent, we were able to synthesize different types of the HBPE-based architectures including hyperbranched-on-hyperbranched core-shell nanostructure, and miktoarm-star-HBPE-based block copolymers. The first part of the dissertation provides a general introduction to the synthesis of polyethylene types with controllable structures. Well-defined polyethylene with different macromolecule architectures were synthesized either for academic or industrial purposes. In the second part, the HBPE with different topologies was synthesized by CWCP, using a α-diimine Pd (II) catalyst. The effect of the temperature and pressure on the catalyst activity and polymer properties, including branch content, molecular weight, distribution, and thermal properties were studied. Two series of samples were synthesized: a) serial samples (A) under pressures of 1, 5, and 27 atm at 5˚C, and b) serial samples (B) at temperatures of 5, 15, and 35 ˚C under 5 atm. Proton nuclear magnetic resonance spectroscopy, 1H NMR, and gel permeation chromatography, GPC, analysis were used to calculate the branching content, molecular weight, and distribution, whereas differential scanning calorimetry, DSC, was used to record the melting and glass transition temperatures as well as the degree of the crystallinity. Well-defined HBPE-based core diblock copolymers with predictable amphiphilic properties are studied in the third part of the project. Hyperbranched

  19. Synthesis and characterization of transition-metal-doped zinc oxide nanocrystals for spintronics

    Science.gov (United States)

    Wang, Xuefeng

    Spintronics (spin transport electr onics), in which both spin and charge of carriers are utilized for information processing, is believed to challenge the current microelectronics and to become the next-generation electronics. Nanostructured spintronic materials and their synthetic methodologies are of paramount importance for manufacturing future nanoscale spintronic devices. This thesis aims at studying synthesis, characterization, and magnetism of transition-metal-doped zinc oxide (ZnO) nanocrystals---a diluted magnetic semiconductor (DMS)---for potential applications in future nano-spintronics. A simple bottom-up-based synthetic strategy named a solvothermal technique is introduced as the primary synthetic approach and its crystal growth mechanism is scrutinized. N-type cobalt-doped ZnO-based DMS nanocrystals are employed as a model system, and characterized by a broad spectrum of advanced microscopic and spectroscopic techniques. It is found that the self-orientation growth mechanism, imperfect oriented attachment, is intimately correlated with the high-temperature ferromagnetism via defects. The influence of processing on the magnetic properties, such as compositional variations, reaction conditions, and post-growth treatment, is also studied. In this way, an in-depth understanding of processing-structure-property interrelationships and origins of magnetism in DMS nanocrystals are obtained in light of the theoretical framework of a spin-split impurity band model. In addition, a nanoscale spinodal decomposition phase model is also briefly discussed. Following the similar synthetic route, copper- and manganese-doped ZnO nanocrystals have been synthesized and characterized. They both show high-temperature ferromagnetism in line with the aforementioned theoretical model(s). Moreover, they display interesting exchange biasing phenomena at low temperatures, revealing the complexity of magnetic phases therein. The crystal growth strategy demonstrated in this work

  20. Graphitic carbon nitride: Synthesis, characterization and photocatalytic decomposition of nitrous oxide

    Energy Technology Data Exchange (ETDEWEB)

    Praus, Petr, E-mail: petr.praus@vsb.cz [Institute of Environmental Technology, VŠB-Technical University of Ostrava, 17. Listopadu 15/2172, Ostrava 708 33 (Czech Republic); Department of Chemistry, Faculty of Metallurgy and Materials Engineering, VŠB-Technical University of Ostrava, 17. Listopadu 15/2172, Ostrava 708 33 (Czech Republic); Svoboda, Ladislav [Institute of Environmental Technology, VŠB-Technical University of Ostrava, 17. Listopadu 15/2172, Ostrava 708 33 (Czech Republic); Department of Chemistry, Faculty of Metallurgy and Materials Engineering, VŠB-Technical University of Ostrava, 17. Listopadu 15/2172, Ostrava 708 33 (Czech Republic); Ritz, Michal [Department of Chemistry, Faculty of Metallurgy and Materials Engineering, VŠB-Technical University of Ostrava, 17. Listopadu 15/2172, Ostrava 708 33 (Czech Republic); Troppová, Ivana; Šihor, Marcel; Kočí, Kamila [Institute of Environmental Technology, VŠB-Technical University of Ostrava, 17. Listopadu 15/2172, Ostrava 708 33 (Czech Republic)

    2017-06-01

    Graphitic carbon nitride (g-C{sub 3}N{sub 4}) was synthetized by condensation of melamine at the temperatures of 400–700 °C in air for 2 h and resulting products were characterized and finally tested for the photocatalytic decomposition of nitrous oxide. The characterization methods were elemental analysis, UV–Vis diffuse reflectance spectroscopy (DRS), photoluminescence (PL), Fourier transform infrared (FTIR) and Raman spectroscopy, measurement of specific surface area (SSA), X-ray powder diffraction (XRD), scanning (SEM) and transmission (TEM) electron microscopy. The XRD patterns, FTIR and Raman spectra proved the presence of g-C{sub 3}N{sub 4} at above 550 °C but the optimal synthesis temperature of 600–650 °C was found. Under these conditions graphitic carbon nitride of the overall empirical composition of C{sub 6}N{sub 9}H{sub 2} was formed. At lower temperatures g-C{sub 3}N{sub 4} with a higher content of hydrogen was formed but at higher temperatures g-C{sub 3}N{sub 4} was decomposed. At the temperatures above 650 °C, its exfoliation was observed. The photocatalytic experiments showed that the activity of all the samples synthetized at 400–700 °C was very similar, that is, within the range of experimental error (5 %). The total conversion of N{sub 2}O reached about 43 % after 14 h. - Highlights: • Graphitic carbon nitride (g-C{sub 3}N{sub 4}) was thermally synthetized from melamine in the range of 400–700 °C. • The optimal temperature was determined at 600–650 °C. • All synthesis products were properly characterized by physico-chemical methods. • Exfoliation of g-C{sub 3}N{sub 4} at above 600 °C was observed. • g-C{sub 3}N{sub 4} was used for the photocatalytic decomposition of N{sub 2}O.

  1. Synthesis and characterization of MgO nanocrystals for biosensing applications

    Energy Technology Data Exchange (ETDEWEB)

    Li, Hongji [Tianjin Key Laboratory of Organic Solar Cells and Photochemical Conversion, School of Chemistry & Chemical Engineering, Tianjin University of Technology, Tianjin 300384 (China); Li, Mingji, E-mail: limingji@163.com [Tianjin Key Laboratory of Film Electronic and Communication Devices, School of Electronics Information Engineering, Tianjin University of Technology, Tianjin 300384 (China); Qiu, Guojun [Tianjin Key Laboratory of Organic Solar Cells and Photochemical Conversion, School of Chemistry & Chemical Engineering, Tianjin University of Technology, Tianjin 300384 (China); Li, Cuiping; Qu, Changqing; Yang, Baohe [Tianjin Key Laboratory of Film Electronic and Communication Devices, School of Electronics Information Engineering, Tianjin University of Technology, Tianjin 300384 (China)

    2015-05-25

    Highlights: • MgO nanocrystals were prepared using DC arc plasma jet CVD method. • The growth time does not exceed 10 min in process of the synthesis. • The samples were found to consist of cubic MgO nanobelts and nanosheets. • Nanocrystals contain contacts, rough edges, vacancies, and doping defects. • The samples exhibited excellent electrochemical biosensing properties. - Abstract: MgO nanocrystals were prepared using a simple direct current arc plasma jet chemical vapor deposition method. Magnesium nitrate was used as source material and Mo film was used as a substrate and catalyst. The high-temperature plasma produced ensured rapid synthesis of the MgO nanocrystals. The as-prepared nanocrystals were characterized by field-emission scanning electron microscopy, high-resolution transmission electron microscopy, X-ray diffraction, energy-dispersive spectroscopy, Fourier transform infrared spectrometry, ultraviolet–visible spectrophotometry, and photoluminescence measurements. The as-synthesized samples were found to consist of cubic MgO nanobelts and nanosheets with large surface areas and low coordination oxide ions, and contained numerous contacts, rough edges, vacancies, and doping defects. The nanostructures exhibited excellent electrochemical sensing properties with high-sensing sensitivity toward ascorbic acid. Their high electrocatalytic activity was attributed to the effect of defects and the surface electron transfer ability of the one-dimensional MgO nanobelts.

  2. Synthesis, characterization, spectroscopic properties and DFT study of a new pyridazinone family

    Science.gov (United States)

    Arrue, Lily; Rey, Marina; Rubilar-Hernandez, Carlos; Correa, Sebastian; Molins, Elies; Norambuena, Lorena; Zarate, Ximena; Schott, Eduardo

    2017-11-01

    Nitrogen compounds are widely investigated due to their pharmacological properties such as antihypertensive, antinociceptive, antibacterial, antifungal, analgesic, anticancer and inhibition activities and lately even as pesticide. In this context, we present the synthesis of new compounds: (E)-6-(3,4-dimethoxyphenyl)-3-(3-(3,4-dimethoxyphenyl)acryloyl)-1-(4-R-phenyl)- 5,6-dihydropyridazin-4(1H)-one (with R = sbnd H(1), -Cl(2), -Br(3), sbnd I(4) and sbnd COOH(5)) that was carried out by reaction of (1E, 6E)-1,7-bis(3,4-dimethoxyphenyl)hepta-1,6-diene-3,5-dione with a substituted phenylamine with general formula p-R-C6H4sbnd NH2 (R = sbnd H (1), sbnd Cl (2), -Br(3), sbnd I(4) and sbnd COOH(5)). This is the first synthesis report of a pyridazinone using as precursors a curcuminoid derivative and a diazonium salt formed in situ. All compounds were characterized by EA, FT-IR, UV-Vis, Emission,1H- and13C-NMR spectroscopy and the crystalline and molecular structure of 4 was solved by X-rays diffraction method. DFT and TD-DFT quantum chemical calculations were also employed to characterize the compounds and provide a rational explanation to the spectroscopic properties. To assess the biological activity of the systems, we focused on pesticide tests on compound 2, which showed an inhibitory effect in plant growth of Agrostis tenuis Higland.

  3. Synthesis and characterization of cotton fiber-based nanocellulose.

    Science.gov (United States)

    Theivasanthi, T; Anne Christma, F L; Toyin, Adeleke Joshua; Gopinath, Subash C B; Ravichandran, Ramanibai

    2018-04-01

    Nanocellulose prepared from the natural material has a promising wide range of opportunities to obtain the superior material properties towards various end-products. In this research, commercially available natural cotton was treated with aqueous sodium hydroxide solution to eliminate the hemicellulose and lignin, then cellulose was collected. The collected cellulose was subjected to acid hydrolysis using sulfuric acid to obtain nanocellulose. The prepared nanocellulose was further characterized with the aid of Fourier transform infrared spectroscopy, X-ray diffraction and Scanning Electron Microscopy to elucidate the chemical structure, crystallinity and the morphology. Copyright © 2017 Elsevier B.V. All rights reserved.

  4. Model-Based Synthesis of Visual Speech Movements from 3D Video

    Directory of Open Access Journals (Sweden)

    Edge JamesD

    2009-01-01

    Full Text Available We describe a method for the synthesis of visual speech movements using a hybrid unit selection/model-based approach. Speech lip movements are captured using a 3D stereo face capture system and split up into phonetic units. A dynamic parameterisation of this data is constructed which maintains the relationship between lip shapes and velocities; within this parameterisation a model of how lips move is built and is used in the animation of visual speech movements from speech audio input. The mapping from audio parameters to lip movements is disambiguated by selecting only the most similar stored phonetic units to the target utterance during synthesis. By combining properties of model-based synthesis (e.g., HMMs, neural nets with unit selection we improve the quality of our speech synthesis.

  5. Synthesis, spectroscopic characterization and acoustic, volumetric, transport and thermal properties of hydroxyl ammonium based ionic liquids

    International Nuclear Information System (INIS)

    Losetty, Venkatramana; Chennuri, Bharath Kumar; Gardas, Ramesh L.

    2016-01-01

    Graphical abstract: Density, ρ (■) in kg · m"−"3, speed of sound, u (●) in m · s"−"1, dynamic viscosity, η (▴) in mPa · s, electrical conductivity, σ (♦) in S · cm"−"1of [BHEA][TFA] as the function of temperature and at 0.1 MPa pressure. - Highlights: • N-butyl-(N-hydroxyethyl) ammonium based protic ionic liquids (PILs) were synthesized. • Density, speed of sound, electrical conductivity and viscosity were measured for studied PILs. • Transport property data were fitted to Vogel–Tammann–Fulcher (VTF) equation. • FT-IR spectrum was helpful to explain the hydrogen bonding between ions. • Measured and derived properties were analyzed in terms of chemical structure of PILs. - Abstract: In the present work, solvent-free synthesis of two hydroxyethyl ammonium-based ionic liquids (ILs) at room temperature was carried out namely, N-butyl-(N-hydroxyethyl) ammonium trifluoroacetate ([BHEA][TFA]) and N-butyl-(N-hydroxyethyl) ammonium nitrate ([BHEA][NO_3]). The synthesized ionic liquids were characterized by various spectroscopic techniques such as "1H-NMR, "1"3C-NMR and FTIR. Furthermore, density (ρ), speed of sound (u), electrical conductivity (σ) and viscosity (η) have been measured within the temperature range from T = (303.15 to 343.15) K and at 0.1 MPa pressure. The measured density and viscosity values were fitted to the linear and Vogel–Tammann–Fulcher (VTF) equation, respectively. The temperature dependence conductivity of the measured ILs was fitted to a similar equation type of viscosity (VTF). Furthermore, the refractive index was measured at T = 303.15 K, in turn molar refraction (R_m) and free volume (f_V) were calculated using the Lorentz–Lorenz equation. The thermodynamic properties such as thermal expansion coefficient (α), isentropic compressibility (β_S) and intermolecular free length (L_f) were calculated by using the experimental values of density and speed of sound. The thermal decomposition temperature (T

  6. Synthesis and characterization of new ionic liquids; Sintese e caracterizacao de novos liquidos ionicos

    Energy Technology Data Exchange (ETDEWEB)

    Oliveira, L.M.C. de; Mattedi, S.; Boaventura, J.S., E-mail: luanaufrn@hotmail.co [Universidade Federal da Bahia (UFBA), Salvador, BA (Brazil). Escola Politecnica. Programa de Pos-Graduacao em Engenharia Quimica; Iglesias, M. [Universidade Federal da Bahia (UFBA), Salvador, BA (Brazil). Escola Politecnica. Programa de Pos-Graduacao em Engenharia Quimica; Universidad de Santiago de Compostela (Spain). Escuela Tecnica Superior de Ingenieria. Dept. de Ingenieria Quimica

    2010-07-01

    In recent years, ionic liquids have been highlighted for its potential in various industrial applications. Among them, the salts of Broensted has a promising profile for the low toxicity, low cost and simple synthesis. This paper presents the synthesis and characterization of new salts of Bronsted with branched (lactate) or large chain anions (oleate) for future use as additives promoters of proton conductivity in fuel cells of ethanol. Experimental data were measured for density, sound velocity and conductivity of pure ionic liquids and mixtures. The density decreases linearly with increasing temperature, and sound velocity shows a similar trend, but not linear. The conductivity increases according to the Arrhenius model with activation energy less than 10 J/mol. Tests NMR, FTIR and TGA confirm ionic structure and thermal stability up to 165 deg C. (author)

  7. Synthesis, characterization and electrospinning of corn cob cellulose-graft-polyacrylonitrile and their clay nanocomposites.

    Science.gov (United States)

    Kalaoğlu, Özlem I; Ünlü, Cüneyt H; Galioğlu Atıcı, Oya

    2016-08-20

    This study aims at evaluation of cellulose recovered from agricultural waste (corn cob) in terms of synthesis of graft copolymers, polymer/clay nanocomposites, and nanofibers. The copolymers and nanocomposites were synthesized in aqueous solution using Ce(4+) initiator. Conditions (concentrations of the components, reaction temperature, and period) were determined first for copolymer synthesis to obtain the highest conversion ratio. Then found parameters were used to synthesize nanocomposites adding clay mineral to reaction medium. Although there was a decrease in conversion in nanocomposites syntheses, thermal and rheologic measurements indicated enhancements compared to pristine copolymer. Obtained polymeric materials have been successfully electrospun into nanofibers and characterized. Average diameter of the nanofibers was about 650nm and was strongly influenced by NaMMT amount in the nanocomposite sample. Copyright © 2016 Elsevier Ltd. All rights reserved.

  8. Synthesis and characterization of platinum supported on alumina doped with cerium catalyst

    International Nuclear Information System (INIS)

    Yusof Abdullah; Abd Fatah Awang Mat; Mohd Ali Sufi; Sarimah Mahat; Razali Kassim; Nurhaslinda Abdullah.

    1996-03-01

    The synthesis and characterization of gamma-alumina doped with cerium as platinum support for the automobile exhaust catalyst are described. Platinum/alumina/ceria catalyst were prepared by impregnation of hexachloroplatinic acid and sintered at 500 degree Celsius to obtain metal dispersions of 1.0 wt%. Catalyst distribution inside the powder and the effects of the addition of cerium to alumina were analyzed by the scanning electron microscopy (SEM) and x-ray fluorescence spectroscopy (XRF). The results showed that the alumina - supported catalysts contained well dispersion of the noble metal

  9. SYNTHESIS AND CHARACTERIZATION OF CANNABIS INDICA FIBER REINFORCED COMPOSITES

    Directory of Open Access Journals (Sweden)

    Amar Singh Singha

    2011-04-01

    Full Text Available This paper reports on the synthesis of Cannabis indica fiber-reinforced composites using Urea-Resorcinol-Formaldehyde (URF as a novel matrix through compression molding technique. The polycondensation between urea, resorcinol, and formaldehyde in different molar ratios was applied to the synthesis of the URF polymer matrix. A thermosetting matrix based composite, reinforced with lignocellulose from Cannabis indica with different fiber loadings 10, 20, 30, 40, and 50% by weight, was obtained. The mechanical properties of randomly oriented intimately mixed fiber particle reinforced composites were determined. Effects of fiber loadings on mechanical properties such as tensile, compressive, flexural strength, and wear resistance were evaluated. Results showed that mechanical properties of URF resin matrix increased considerably when reinforced with particles of Cannabis indica fiber. Thermal (TGA/DTA/DTG and morphological studies (SEM of the resin, fiber and polymer composite thus synthesized were carried out.

  10. Synthesis of Cyclic Polymers and Characterization of Their Diffusive Motion in the Melt State at the Single Molecule Level

    KAUST Repository

    Habuchi, Satoshi

    2016-09-26

    We demonstrate a method for the synthesis of cyclic polymers and a protocol for characterizing their diffusive motion in a melt state at the single molecule level. An electrostatic self-assembly and covalent fixation (ESA-CF) process is used for the synthesis of the cyclic poly(tetrahydrofuran) (poly(THF)). The diffusive motion of individual cyclic polymer chains in a melt state is visualized using single molecule fluorescence imaging by incorporating a fluorophore unit in the cyclic chains. The diffusive motion of the chains is quantitatively characterized by means of a combination of mean-squared displacement (MSD) analysis and a cumulative distribution function (CDF) analysis. The cyclic polymer exhibits multiple-mode diffusion which is distinct from its linear counterpart. The results demonstrate that the diffusional heterogeneity of polymers that is often hidden behind ensemble averaging can be revealed by the efficient synthesis of the cyclic polymers using the ESA-CF process and the quantitative analysis of the diffusive motion at the single molecule level using the MSD and CDF analyses.

  11. Carbazole Containing Copolymers: Synthesis, Characterization, and Applications in Reversible Holographic Recording

    Directory of Open Access Journals (Sweden)

    Bénédicte Mailhot-Jensen

    2010-01-01

    Full Text Available Carbazolic copolymers have been developed to be used in reversible holographic recording. This paper describes a complete analysis, from synthesis of the material to its applications, together with the corresponding characterizations. The investigated materials were photosensitive copolymers obtained from carbazolylalkylmethacrylates (CEM and octylmethacrylate (OMA. A detailed investigation was undertaken involving infrared spectroscopy and NMR techniques, 1H, 13C, COSY, and HSQC, in order to establish the chemical structure and the composition of the copolymers. Holographic recording characteristics were investigated with one- and two-layer photothermoplastic carriers. The two-layer carrier contains separate photosensitive and thermoplastic layers and gives the best holographic response. The surface of microstructured samples has been characterized by atomic force microscopy analysis. It is shown that via a photothermoplastic recording process, it is possible to record and read holograms practically in real time (~3 s with a diffraction efficiency of 10% and a spatial resolution higher than 1000 mm−1.

  12. Synthesis and spectral characterization of 2,2-diphenylethyl glucosinolate and HPLC-based reaction progress curve data for the enzymatic hydrolysis of glucosinolates by Sinapis alba myrosinase

    Directory of Open Access Journals (Sweden)

    Chase A. Klingaman

    2017-02-01

    Full Text Available The data presented in this article are related to the research article, “HPLC-based enzyme kinetics assay for glucosinolate hydrolysis facilitate analysis of systems with both multiple reaction products and thermal enzyme denaturation” (C.K. Klingaman, M.J. Wagner, J.R. Brown, J.B. Klecker, E.H. Pauley, C.J. Noldner, J.R. Mays, [1]. This data article describes (1 the synthesis and spectral characterization data of a non-natural glucosinolate analogue, 2,2-diphenylethyl glucosinolate, (2 HPLC standardization data for glucosinolate, isothiocyanate, nitrile, and amine analytes, (3 reaction progress curve data for enzymatic hydrolysis reactions with variable substrate concentration, enzyme concentration, buffer pH, and temperature, and (4 normalized initial velocities of hydrolysis/formation for analytes. These data provide a comprehensive description of the enzyme-catalyzed hydrolysis of 2,2-diphenylethyl glucosinolate (5 and glucotropaeolin (6 under widely varied conditions.

  13. Carbon-based nanomaterial synthesis using nanosecond electrical discharges in immiscible layered liquids: n-heptane and water

    KAUST Repository

    Hamdan, Ahmad

    2018-05-14

    Plasmas in- or in-contact with liquids have been extensively investigated due to their high potential for a wide range of applications including but not limited to, water treatment, material synthesis and functionalization, bio-medical applications, and liquid fuel reformation. Recently, we successfully developed a discharge using two immiscible liquids, having very different electrical permittivities, which could significantly intensify the electric field intensity. Here, we establish nanosecond discharges at the interface n-heptane-water (with respective relative dielectric permittivities of 2 and 80) to enable the synthesis of carbon-based nanomaterials. A characterization of the as-synthesized material and the annealed (500 °C) material, using various techniques (Fourier-Transform, Infra-Red, Scanning and Transmission electron microscopes, etc.), shows that the as-synthesized material is a mixture of two carbon-based phases: a crystalline phase (graphite like) embedded into a phase of hydrogenated amorphous carbon. The existence of two-phases may be explained by the non-homogeneity of the discharge that induces various chemical reactions in the plasma channel.

  14. Carbon-based nanomaterial synthesis using nanosecond electrical discharges in immiscible layered liquids: n-heptane and water

    Science.gov (United States)

    Hamdan, Ahmad; Cha, Min Suk

    2018-06-01

    Plasmas in- or in-contact with liquids have been extensively investigated due to their high potential for a wide range of applications including, but not limited to, water treatment, material synthesis and functionalization, bio-medical applications, and liquid fuel reformation. Recently, we successfully developed a discharge using two immiscible liquids, having very different electrical permittivities, which could significantly intensify the electric field intensity. Here, we establish nanosecond discharges at the interface n-heptane-water (with respective relative dielectric permittivities of 2 and 80) to enable the synthesis of carbon-based nanomaterials. A characterization of the as-synthesized material and the annealed (500 °C) material, using various techniques (Fourier-transform, infra-red, scanning and transmission electron microscopes, etc), shows that the as-synthesized material is a mixture of two carbon-based phases: a crystalline phase (graphite like) embedded into a phase of hydrogenated amorphous carbon. The existence of two-phases may be explained by the non-homogeneity of the discharge that induces various chemical reactions in the plasma channel.

  15. Ion beams provided by small accelerators for material synthesis and characterization

    Science.gov (United States)

    Mackova, Anna; Havranek, Vladimir

    2017-06-01

    The compact, multipurpose electrostatic tandem accelerators are extensively used for production of ion beams with energies in the range from 400 keV to 24 MeV of almost all elements of the periodic system for the trace element analysis by means of nuclear analytical methods. The ion beams produced by small accelerators have a broad application, mainly for material characterization (Rutherford Back-Scattering spectrometry, Particle Induced X ray Emission analysis, Nuclear Reaction Analysis and Ion-Microprobe with 1 μm lateral resolution among others) and for high-energy implantation. Material research belongs to traditionally progressive fields of technology. Due to the continuous miniaturization, the underlying structures are far beyond the analytical limits of the most conventional methods. Ion Beam Analysis (IBA) techniques provide this possibility as they use probes of similar or much smaller dimensions (particles, radiation). Ion beams can be used for the synthesis of new progressive functional nanomaterials for optics, electronics and other applications. Ion beams are extensively used in studies of the fundamental energetic ion interaction with matter as well as in the novel nanostructure synthesis using ion beam irradiation in various amorphous and crystalline materials in order to get structures with extraordinary functional properties. IBA methods serve for investigation of materials coming from material research, industry, micro- and nano-technology, electronics, optics and laser technology, chemical, biological and environmental investigation in general. Main research directions in laboratories employing small accelerators are also the preparation and characterization of micro- and nano-structured materials which are of interest for basic and oriented research in material science, and various studies of biological, geological, environmental and cultural heritage artefacts are provided too.

  16. Synthesis and characterization of iron based superconductor Nd-1111

    Science.gov (United States)

    Alborzi, Z.; Daadmehr, V.

    2018-06-01

    Polycrystalline sample of NdFeAsO0.8F0.2 was prepared by one-step solid-state reaction method. The structural and electrical properties of sample were characterized through XRD pattern and the 4-probe method. The critical temperature was obtained at 56 K. The crystal structure was tetragonal with P4/nmm:2 symmetry group.

  17. Synthesis, characterization and application of nanozeolite NaX from Vietnamese kaolin

    International Nuclear Information System (INIS)

    Ngoc, Don Ta; Pham, Thanh Huyen; Hong Nguyen, Khanh Dieu

    2013-01-01

    This paper presents the results of synthesis of nanozeolite NaX from Vietnamese kaolin. Influence factors on the control of crystal sizes and application of synthesized materials as adsorbent for organic compound are discussed. The results show that there are several factors that influence the synthesis. When water content in gel increases, crystal size of NaX increases sharply. The increase of alkaline and silica contents increases the crystallinity and decreases the particle size of nano NaX, and the particle size reaches the minimum at Na 2 O/Al 2 O 3 = 5.0 and SiO 2 /Al 2 O 3 = 4.0. Crystal sizes formed at low crystallizing temperature are smaller than those formed at higher temperature. Ageing time and crystallizing time strongly influence the crystallinity and crystal size, which is related to the number of crystal seeds formed during ageing period, the growth of seed and the partial solubility of crystal at maximum formation. Nano NaX was characterized by x-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), Brunauer–Emmett–Teller (BET) adsorption, Fourier transform infrared (FTIR) and simultaneous thermogravimetry–differential scanning calorimetry (TG/DSC). At optimized synthesis conditions, nano NaX has surface area of 573 m 2 g −1 with external surface area of 92 m 2 g −1 , pore size distribution at 0.81 and 10.8 nm, average crystal size of 25 nm and thermal stability up to 789 °C. This material can adsorb cumene rapidly with high adsorption capacity and stability. (paper)

  18. Synthesis and thermoluminescent characterization of LiF doped with Ag; Sintesis y caracterizacion termoluminiscente de LiF dopado con Ag

    Energy Technology Data Exchange (ETDEWEB)

    Encarnacion, E. K.; Reyes, J.; Guerrero, Z. [Universidad Autonoma de Santo Domingo, Facultad de Ciencias, Ciudad Universitaria, Santo Domingo (Dominican Republic); Sosa, M. A.; Vallejo, M. A.; Rivera P, E., E-mail: emma.kee@gmail.com [Universidad de Guanajuato, Campus Leon, Division de Ciencias e Ingenierias, Loma del Bosque 103, Col. Lomas del Campestre, 37150 Leon, Guanajuato (Mexico)

    2015-10-15

    Full text: In this paper the synthesis and characterization of lithium fluoride (LiF) crystals pure and activated with silver (Ag) is reported. The synthesis was carried out by the method of co-precipitation; three samples were obtained one of pure LiF and two were activated with 0.02 and 0.04% of Ag. All samples were subjected to X-ray emission and the results were analyzed. The synthesized samples were characterized by X-ray diffraction, thermoluminescence and X-ray fluorescence. The XRD results show complete crystal structures. The radiation dosimetry responses are discussed. These are the first results of a research conducted at the Universidad Autonoma de Santo Domingo in collaboration with the Universidad de Guanajuato. (Author)

  19. Natural precursor based hydrothermal synthesis of sodium carbide for reactor applications

    Science.gov (United States)

    Swapna, M. S.; Saritha Devi, H. V.; Sebastian, Riya; Ambadas, G.; Sankararaman, S.

    2017-12-01

    Carbides are a class of materials with high mechanical strength and refractory nature which finds a wide range of applications in industries and nuclear reactors. The existing synthesis methods of all types of carbides have problems in terms of use of toxic chemical precursors, high-cost, etc. Sodium carbide (Na2C2) which is an alkali metal carbide is the least explored one and also that there is no report of low-cost and low-temperature synthesis of sodium carbide using the eco-friendly, easily available natural precursors. In the present work, we report a simple low-cost, non-toxic hydrothermal synthesis of refractory sodium carbide using the natural precursor—Pandanus. The formation of sodium carbide along with boron carbide is evidenced by the structural and morphological characterizations. The sample thus synthesized is subjected to field emission scanning electron microscopy (FESEM), x-ray powder diffraction (XRD), ultraviolet (UV)—visible spectroscopy, Fourier transform infrared spectroscopy (FTIR), Raman, and photoluminescent (PL) spectroscopic techniques.

  20. Synthesis and characterization of TiO2 nanoparticles by the method Pechini

    International Nuclear Information System (INIS)

    Zoccal, Joao Victor Marques; Arouca, Fabio de Oliveira; Goncalves, Jose Antonio Silveira

    2009-01-01

    In recent years, scientific research showed an increasing interest in the field of nanotechnology, resulting in several techniques for the production of nanoparticles, such as methods of chemical synthesis. Among the various existing methods, the Pechini method has been used to obtain nanoparticles of titanium dioxide (TiO 2 ). Thus, this work aims to synthesize and characterize nanoparticles of TiO 2 obtained by this method. The technique constitutes in the reaction between citric acid with titanium isopropoxide, resulting as the product the titanium citrate. With the addition of the ethylene glycol polymerization occurs, resulting in a polymeric resin. At the end of the process, the resin is calcined to remove organic matter, creating nanoparticles of TiO 2 . The resulting powders were characterized by thermogravimetric analysis (TGA) and thermal differential analysis (DTA), X-ray diffraction, absorption spectrophotometry in the infrared, method of adsorption nitrogen / helium (BET method) and scanning electron microscopy. The results obtained in the characterization techniques showed that the Pechini method is promising in obtaining nanosized TiO 2 . (author)

  1. Synthesis and characterization of ceramic powders of pure and doped with trivalent erbium barium tungstate

    International Nuclear Information System (INIS)

    Sousa, R.B. de; Nascimento, V.A. do; Matos, J. M.E. de; Santos, M.R.M.C.

    2014-01-01

    This research proposes the synthesis and characterization of pure and doped with Er"3"+ (1 and 2 %) barium tungstate powders prepared by the coprecipitation method. In order to characterize the obtained powders were used X-Ray Diffractometry, Raman Spectroscopy and Fourier Transform Infrared Spectroscopy. According to the standard XRD spectra, the crystals exhibited the presence of tetragonal scheelite structure without the presence of secondary phases. Raman spectra showed the presence of eleven vibrational modes and two modes were observed in the infrared spectra. The synthesized oxides showed good crystallinity and structurally ordered at short and long-range. (author)

  2. Synthesis and characterization of organic-inorganic hybrids formed between conducting polymers and crystalline antimonic acid

    Directory of Open Access Journals (Sweden)

    Beleze Fábio A.

    2001-01-01

    Full Text Available In this paper we report the synthesis and characterization of novel organic-inorganic hybrid materials between the crystalline antimonic acid (CAA and two conductive polymers: polypyrrole and polyaniline. The hybrids were obtained by in situ oxidative polymerization of monomers by the Sb(V present in the pyrochlore-like CAA structure. The materials were characterized by infrared and Raman spectroscopy, X-ray diffraction, cyclic voltammetry, CHN elemental analysis and electronic paramagnetic resonance spectroscopy. The results showed that both polymers were formed in their oxidized form, with the CAA structure acting as a counter anion.

  3. Ruthenium(III) Complexes of Heterocyclic Tridentate (ONN) Schiff Base: Synthesis, Characterization and its Biological Properties as an Antiradical and Antiproliferative Agent

    Science.gov (United States)

    Ejidike, Ikechukwu P.; Ajibade, Peter A.

    2016-01-01

    The current work reports the synthesis, spectroscopic studies, antiradical and antiproliferative properties of four ruthenium(III) complexes of heterocyclic tridentate Schiff base bearing a simple 2′,4′-dihydroxyacetophenone functionality and ethylenediamine as the bridging ligand with RCHO moiety. The reaction of the tridentate ligands with RuCl3·3H2O lead to the formation of neutral complexes of the type [Ru(L)Cl2(H2O)] (where L = tridentate NNO ligands). The compounds were characterized by elemental analysis, UV-vis, conductivity measurements, FTIR spectroscopy and confirmed the proposed octahedral geometry around the Ru ion. The Ru(III) compounds showed antiradical potentials against 2,2-Diphenyl-1-Picrylhydrazyl (DPPH) and 2,2′-azinobis-(3-ethylbenzothiazoline-6-sulfonic acid) (ABTS) radicals, with DPPH scavenging capability in the order: [(PAEBOD)RuCl2] > [(BZEBOD)RuCl2] > [(MOABOD)RuCl2] > [Vit. C] > [rutin] > [(METBOD)RuCl2], and ABTS radical in the order: [(PAEBOD)RuCl2] < [(MOABOD)RuCl2] < [(BZEBOD)RuCl2] < [(METBOD)RuCl2]. Furthermore, in vitro anti-proliferative activity was investigated against three human cancer cell lines: renal cancer cell (TK-10), melanoma cancer cell (UACC-62) and breast cancer cell (MCF-7) by SRB assay. PMID:26742030

  4. Ruthenium(III Complexes of Heterocyclic Tridentate (ONN Schiff Base: Synthesis, Characterization and its Biological Properties as an Antiradical and Antiproliferative Agent

    Directory of Open Access Journals (Sweden)

    Ikechukwu P. Ejidike

    2016-01-01

    Full Text Available The current work reports the synthesis, spectroscopic studies, antiradical and antiproliferative properties of four ruthenium(III complexes of heterocyclic tridentate Schiff base bearing a simple 2′,4′-dihydroxyacetophenone functionality and ethylenediamine as the bridging ligand with RCHO moiety. The reaction of the tridentate ligands with RuCl3·3H2O lead to the formation of neutral complexes of the type [Ru(LCl2(H2O] (where L = tridentate NNO ligands. The compounds were characterized by elemental analysis, UV-vis, conductivity measurements, FTIR spectroscopy and confirmed the proposed octahedral geometry around the Ru ion. The Ru(III compounds showed antiradical potentials against 2,2-Diphenyl-1-Picrylhydrazyl (DPPH and 2,2′-azinobis-(3-ethylbenzothiazoline-6-sulfonic acid (ABTS radicals, with DPPH scavenging capability in the order: [(PAEBODRuCl2] > [(BZEBODRuCl2] > [(MOABODRuCl2] > [Vit. C] > [rutin] > [(METBODRuCl2], and ABTS radical in the order: [(PAEBODRuCl2] < [(MOABODRuCl2] < [(BZEBODRuCl2] < [(METBODRuCl2]. Furthermore, in vitro anti-proliferative activity was investigated against three human cancer cell lines: renal cancer cell (TK-10, melanoma cancer cell (UACC-62 and breast cancer cell (MCF-7 by SRB assay.

  5. Synthesis, characterization and wound healing imitation of Fe3O4 magnetic nanoparticle grafted by natural products

    Science.gov (United States)

    Pala, Sravan Kumar

    This research focused on the study of the core-shelled magnetic nanomaterials derived from a colloidal chemistry. The goals are four-fold: (1) synthesis of Fe3O4MNMs using colloidal chemistry. The Fe 3O4 MNMs were then grafted with extracts derived from natural products, namely Olecraceavar italica (broccoli), Boletus edulis (mushroom)and Solanum lycopersicum (tomato);(2)characterization of natural products by chromatography and mass spectrometry;(3) characterization of MNMs to determine their crystallinity, morphological and elemental composition by the state-of-the-art instruments; and (4) biological evaluation using Gram-negative and Gram-positive bacteria. The approach provides advantages to precisely control the composition and homogeneity. The second advantage of the colloidal chemistry is its user friendliness and feasibility. Due to the nature of the natural products, the compatibility of MNM is anticipated to be enhanced.In this chapter, the nanomaterials will be discussed from four perspectives,§1.1 Nanotechnology (§1.1), §1.2 Synthesis of nanomaterials; §1.3 The natural product extract,; §1.4 Characterization of nanomaterials; and §1.5Biological application of nanomaterials.Fig. 1 summarized the overarching goals of this study.

  6. Bio-assisted synthesis and characterization of nanostructured bismuth (III) sulphide using Clostridium acetobutylicum

    International Nuclear Information System (INIS)

    Kamaraj, Sathish Kumar; Venkatachalam, Ganesh; Arumugam, Palaniappan; Berchmans, Sheela

    2014-01-01

    Nanostructured bismuth (III) sulphide is synthesized at room temperature using a hydrogen sulphide producing microorganism namely Clostridium acetobutylicum. On contrary to chemical routes involving both the high and room temperature methods, the present experimental procedure involves a bio-assisted approach. This method is free from the usage of toxic and hazardous chemicals making it an environment friendly route. The synthesized bismuth sulphide is characterized using transmission electron microscope (TEM), powder X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and cyclic voltammetry (CV). From our experiments we find that bismuth sulphide produced using this bio-assisted approach exhibits a hexagonal shaped plate-like structures and is stabilized by the extracellular proteins present in the culture medium. - Graphical abstract: A green chemistry approach towards the synthesis of bismuth (III) sulphide nanostructures at room temperature using a hydrogen sulphide producing microorganism namely, Clostridium acetobutylicum is demonstrated. - Highlights: • Environmentally benign (greener) route towards synthesis of Bi 2 S 3 nanostructures. • Bio-assisted synthesis of Bi 2 S 3 at room temperature using Clostridium acetobutylicum. • Extracellular proteins in H 2 S producing microorganism as stabilizer for Bi 2 S 3 NPs. • Hexagonal platelets of Bi 2 S 3 possessing an orthorhombic crystalline structure

  7. Selective synthesis and characterization of chlorins as sensitizers for photodynamic therapy

    Science.gov (United States)

    Montforts, Franz-Peter; Kusch, Dirk; Hoper, Frank; Braun, Stefan; Gerlach, Benjamin; Brauer, Hans-Dieter; Schermann, Guido; Moser, Joerg G.

    1996-04-01

    Chlorin type sensitizers have ideal photophysical properties for an application in PDT. The basic chlorin framework of these sensitizers has to be modified by attachment of lipophilic and hydrophilic residues to achieve a good cell uptake and tumor enrichment. In the present study we describe the selective synthesis of amphiphilic chlorins starting from the readily accessible red blood pigment heme. The photophysical properties of the well defined synthetic chlorins are characterized by photophysical investigations. The kinetic of cell uptake, the localization in the cell and the photodynamic behavior of the amphiphilic sensitizers are demonstrated by incubation of A 375 cancer cell lines with structurally different chlorins.

  8. Synthesis, characterization and applications of graphene architectures

    Science.gov (United States)

    Thomas, Abhay Varghese

    Graphene, a two--dimensional sheet of sp2 hybridized carbon atoms arranged in a honeycomb lattice structure, has garnered tremendous interest from the scientific community for its unique combination of properties. It has interesting electrical, thermal, optical and mechanical properties that scientists and engineers are trying to understand and harness to improve current products as well as focus on disruptive technologies that can be made possible by this next generation material. In this thesis the synthesis, characterization and applications of various graphene architectures were explored from the context of a bottom--up and top--down synthesis approach. The work is divided into three main chapters and each one deals with a unique architecture of graphene as well as its properties and an application to a real world problem. In Chapter 2, we focus on bottom--up synthesis of graphene sheets by chemical vapor deposition. We then studied the wetting properties of graphene coated surfaces. More specifically the wetting properties of single and multilayer graphene films on flat and nanoscale rough surfaces are explored and the insights gained are used in improving heat transfer performance of copper surfaces. Single layer graphene, on certain flat surfaces, was shown to exhibit `wetting transparency' as a result of its sheer thinness and this property is of interest in various wetting related applications. Surface protection from corrosion and/or oxidation without change in wetting properties is tremendously useful in multiple fields and we looked to apply this property to dehumidification of copper surfaces. The short time scales results demonstrated that graphene indeed served to prevent oxidation of the surface which in turn promoted increased heat transfer co--efficients with respect to the oxidized copper surfaces. Closer inspection of the surface over long time scales however revealed that the oxide layer changed the wetting properties and this was detrimental

  9. SYNTHESIS AND CHARACTERIZATION OF NEW STABILIZERS WITH OPTIMAL MOLECULAR WEIGHT

    Institute of Scientific and Technical Information of China (English)

    Jiang-qing Pan

    2001-01-01

    Over 2 × l08 tons of polymers are produced every year, and a large portion of polymers faces the degradation problem. There are many effective methods to protect polymers against degradation and the addition of stabilizers to polymer remains the most convenient and effective way of enhancing polymer life and performance. In this article, a series of effective stabilizers with optimal molecular weight (MW), including common, monomeric and polymeric stabilizers (antioxidant and light stabilizer) were synthesized using isocyanation, controlled isocyanation, hydrosilylation, epoxide addition, macroreaction of stabilizing functional compounds and polymerization of monomeric stabilizers. The sructure and performance of these new stabilizers were characterized by using IR, NMR, MS, UV-spectra, XPS and elemental analysis. The current development of stabilizer synthesis was also reviewed.``

  10. Synthesis and Characterization of High-Dielectric-Constant Nanographite-Polyurethane Composite

    Science.gov (United States)

    Mishra, Praveen; Bhat, Badekai Ramachandra; Bhattacharya, B.; Mehra, R. M.

    2018-05-01

    In the face of ever-growing demand for capacitors and energy storage devices, development of high-dielectric-constant materials is of paramount importance. Among various dielectric materials available, polymer dielectrics are preferred for their good processability. We report herein synthesis and characterization of nanographite-polyurethane composite with high dielectric constant. Nanographite showed good dispersibility in the polyurethane matrix. The thermosetting nature of polyurethane gives the composite the ability to withstand higher temperature without melting. The resultant composite was studied for its dielectric constant (ɛ) as a function of frequency. The composite exhibited logarithmic variation of ɛ from 3000 at 100 Hz to 225 at 60 kHz. The material also exhibited stable dissipation factor (tan δ) across the applied frequencies, suggesting its ability to resist current leakage.

  11. Novel polymer anchored Cr(III) Schiff base complexes: Synthesis, characterization and antimicrobial properties

    Science.gov (United States)

    Selvi, Canan; Nartop, Dilek

    2012-09-01

    New polymer-bound Schiff bases and Cr(III) complexes have been synthesized by the reaction of 4-benzyloxybenzaldehyde, polymer-bound with 2-aminophenol, 2-amino-4-chlorophenol and 2-amino-4-methylphenol. The structure of polymeric-Schiff bases and their Cr(III) complexes have been characterized by elemental analyses, magnetic measurements, IR, UV-Vis, TG-DTA and 1H-NMR. All these compounds have also been investigated for antibacterial activity by the well-diffusion method against Staphylococcus aureus (RSKK-07035), Shigella dysenteria type 10 (RSKK 1036), Listeria monocytogenes 4b(ATCC 19115, Escherichia coli (ATCC 1230), Salmonella typhi H (NCTC 901.8394), Staphylococcus epidermis (ATCC 12228), Brucella abortus (RSKK-03026), Micrococcs luteus (ATCC 93419, Bacillus cereus sp., Pseudomonas putida sp. and for antifungal activity against Candida albicans (Y-1200-NIH).

  12. Property Based Process and Product Synthesis and Design

    DEFF Research Database (Denmark)

    Eden, Mario Richard

    2003-01-01

    in terms of the constitutive (synthesis/design) variables instead of the process variables, thus providing the synthesis/design targets. The second reverse problem (reverse property prediction) solves the constitutive equations to identify unit operations, operating conditions and/or products by matching......This thesis describes the development of a general framework for solving process and product design problems. Targeting the desired performance of the system in a systematic manner relieves the iterative nature of conventional design techniques. Furthermore, conventional component based methods...... are not capable of handling problems, where the process or product objectives are driven by functionalities or properties rather than chemical constituency. The framework is meant to complement existing composition based methods by being able to handle property driven problems. By investigating the different...

  13. Synthesis and characterization of tunable coumarin- linked glasses as new class of organic/inorganic phosphors

    Energy Technology Data Exchange (ETDEWEB)

    Luridiana, Alberto; Pretta, Gianluca; Secci, Francesco; Frongia, Angelo [Dipartimento di Scienze Chimiche e Geologiche, Università degli Studi di Cagliari, Complesso universitario di Monserrato, SS 554, bivio per Sestu, Monserrato (Canada) (Italy); Chiriu, Daniele; Carbonaro, Carlo Maria; Corpino, Riccardo [Dipartimento di Fisica, Università degli Studi di Cagliari, Complesso universitario di Monserrato, SS 554, bivio per Sestu, Monserrato (Canada) (Italy); Ricci, Pier Carlo, E-mail: carlo.ricci@dsf.unica.it [Dipartimento di Fisica, Universitá degli Studi di Cagliari, S.P. Monserrato-Sestu Km 0,700, 09042 Monserrato (Canada) (Italy)

    2014-10-21

    It is well known that stilbene with a trans conformation is highly fluorescent. From the viewpoint of molecular structure, coumarins bear a carbon-carbon double bond which is fixed as trans conformation as in trans-stilbene through a lactone structure. This can help to avoid the trans-cis transformation of the double bond under ultraviolet (UV) irradiation as observed in stilbene compounds and results in strong fluorescence and high fluorescence quantum yield and photostability in most of coumarin derivatives. Herein we report some preliminary results about the synthesis and spectroscopic characterization of tunable coumarins and the development of a new linkage protocol for the obtainment of monolayer coumarin-covalently linked glasses. The resulting organic/inorganic coumarin/silica based Self-Assembled Monolayer (SMA) film is proposed as new phosphors for the substituting of critical raw materials, like rare earths, in photonics applications.

  14. Synthesis, stability range and characterization of Pr2Cu2O5

    Science.gov (United States)

    Fernández-Sanjulián, Javier; Morán, Emilio; Ángel Alario-Franco, Miguel

    2010-03-01

    A novel Pr2Cu2O5 phase has been prepared under high-pressure and high-temperature conditions (P ∼6 GPa and T ∼1673 K) in a Belt-type apparatus and characterized by X-ray diffraction and electron microscopy. The crystal structure appears to be an orthorhombic "oxygen-deficient perovskite" (M.T. Anderson, J.T. Vaughey, and K.R. Poeppelmeier, Structural similarities among oxygen-deficient perovskites, Chem. Mater. 5 (1993), pp. 151-165) isostructural with La2Cu2O5 (J.F. Bringley, B.A. Scott, S.J. La Placa, R.F. Boheme, T.M. Shaw, M.W. McElfresh, S.S. Trail, and D.E. Cox, Synthesis of the defect perovskite series LaCuO 3-δ with copper valence varying from 2+to 3+, Nature 347 (1990), pp. 263-265) and Nd2Cu2O5 (B.-H. Chen, D. Walker, E. Suard, B.A. Scott, B. Mercey, M. Hervieu, and B. Raveau, High pressure synthesis of NdCuO3-δ perovskites (0≤δ≤0.5). Inorg. Chem. 34 (1995), pp. 2077-2083).

  15. Synthesis and characterization of poly iodine anilines by plasma

    International Nuclear Information System (INIS)

    Enriquez P, M.A.

    2003-01-01

    The polymers and organic materials present a numberless quantity of applications. However, it has not been but until recent times that it has been found that some of these materials can possess semiconductor properties. This has generated a great interest for the investigation in the area of semiconductor polymers. The poly aniline (Pan) it is one of the main semiconductor polymers because their electric properties change depending on the doping and of the state of oxidation to the one the molecules are subjected. The synthesis of this material has been carried out by means of chemical oxidation or electrochemistry. In this work a study is presented on the formation of poly aniline polymers with halogens chemically united to the aniline ring, poly(m-iodine aniline) (m-PAnI) and poly(m-chloroaniline) (m-PAnCI) for plasma. The plasma is generated by means of discharges of splendor with an r f amplifier to 13.5 MHz to drops pressures (10 -2 mbar). The synthesized polymers were obtained in form of thin film in the walls of the reactor and in the substrate introduced in the one. The electric properties of the polymers were evaluated in function of the time of reaction. Also, the conductivity of the polymers was compared synthesized in this work with reported data of synthesized poly aniline and doped with iodine for plasma. The highest values in conductivity are obtained in the poly aniline where the halogens are chemically connected to the ring that if it is doped with iodine. The atomic proportion in the surface of the polymers was analyzed by dispersive energy spectroscopy with which is deduced that the halogens come off of the molecules of the monomers or of the polymer in formation and that the atoms of iodine get lost more easily than those of chlorine. Other techniques that were used to characterize to the poly aniline were scanning electron microscopy, infrared spectroscopy, thermal gravimetric analysis and X-ray diffraction. The results are presented in

  16. Using framework-based synthesis for conducting reviews of qualitative studies.

    Science.gov (United States)

    Dixon-Woods, Mary

    2011-04-14

    Framework analysis is a technique used for data analysis in primary qualitative research. Recent years have seen its being adapted to conduct syntheses of qualitative studies. Framework-based synthesis shows considerable promise in addressing applied policy questions. An innovation in the approach, known as 'best fit' framework synthesis, has been published in BMC Medical Research Methodology this month. It involves reviewers in choosing a conceptual model likely to be suitable for the question of the review, and using it as the basis of their initial coding framework. This framework is then modified in response to the evidence reported in the studies in the reviews, so that the final product is a revised framework that may include both modified factors and new factors that were not anticipated in the original model. 'Best fit' framework-based synthesis may be especially suitable in addressing urgent policy questions where the need for a more fully developed synthesis is balanced by the need for a quick answer. Please see related article: http://www.biomedcentral.com/1471-2288/11/29.

  17. Synthesis, characterization and biological studies of copper oxide nanostructures

    Science.gov (United States)

    Jillani, Saquf; Jelani, Mohsan; Hassan, Najam Ul; Ahmad, Shahbaz; Hafeez, Muhammad

    2018-04-01

    The development of synthetic methods has been broadly accepted as an area of fundamental importance to the understanding and application of nanoscale materials. It allows the individual to modulate basic parameters such as morphology, particle size, size distributions, and composition. Several methods have been developed to synthesize CuO nanostructures with diverse morphologies, sizes, and dimensions using different chemical and physical based approaches. In this work, CuO nanostructures have been synthesized by aqueous precipitation method and simple chemical deposition method. The characterization of these products has been carried out by the x-ray Diffraction (XRD), Scanning Electron Microscope (SEM), Fourier Transform Infrared (FTIR) and UV–vis spectroscopy. Biological activity such as antibacterial nature of synthesized CuO is also explored. XRD peaks analysis revealed the monoclinic crystalline phase of copper oxide nanostructures. While the rod-like and particle-like morphologies have been observed in SEM results. FTIR spectra have confirmed the formation of CuO nanoparticles by exhibiting its characteristic peaks corresponding to 494 cm‑1 and 604 cm‑1. The energy band gap of the as-prepared CuO nanostructures determined from UV–vis spectra is found to be 2.18 eV and 2.0 eV for precipitation and chemically deposited samples respectively. The antibacterial activity results described that the synthesized CuO nanoparticles showed better activity against Staphylococcus aureus. The investigated results suggested the synthesis of highly stable CuO nanoparticles with significant antibacterial activities.

  18. Synthesis and characterization of novel nanothermometers

    Energy Technology Data Exchange (ETDEWEB)

    Baumert, Delphine [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL); Larsen, George [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL); Coopersmith, Kaitlin [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL); Schyck, Sarah [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL); Murph, Simona [Savannah River Site (SRS), Aiken, SC (United States). Savannah River National Lab. (SRNL)

    2016-03-23

    A straightforward approach was developed for the synthesis of Pd, Pd-Fe2O3, Au-Fe2O3, and Au-Pd-Fe2O3 nanothermometers, using a single SL DNA. These NP-DNA conjugates were characterized using techniques including EDX measurements, ζ-potential of NPs before and after DNA functionalization, electron microscopy studies and fluorescence spectroscopy. The fluorescence studies of the NP-DNA demonstrate the interaction between the NP and the fluorophore, which is quenched in the case of Au-Pd-Fe2O3 NPs and is perhaps enhanced (when compared to AuNPs) in the case of Pd and Pd-Fe2O3 NPs. In order to achieve more accurate and reproducible measurements, designing a system that is able to hold the NP-DNA conjugates at a temperature for a longer period of time to allow them to 12 equilibrate is currently underway. Our studies show that Au-Pd-Fe2O3 NPs are the best candidate material to serve as nanothermometers when compared to Pd, Pd-Fe2O3, and Au-Fe2O3 materials.

  19. Synthesis and characterization of a new composite based on copper (II) and octa (aminopropil)silsesquioxane; Sintese e caracterizacao de novos compositos a base de cobre (II) e octa(aminopropil)silsesquioxano

    Energy Technology Data Exchange (ETDEWEB)

    Magossi, M.S. de; Carmo, D.R. do, E-mail: marymagossi@gmail.com [Universidade Estadual Paulista Julio de Mesquita Filho (UNESP), Ilha Solteira, SP (Brazil). Faculdade de Engenharia

    2014-07-01

    In this work, a new compound based silsesquioxane and nitroprusside of copper was prepared starting from octa (aminopropyl)silsesquioxane following a new route of synthesis. The composite prepared as described ACCuN was preliminarily characterized by spectroscopic techniques, such as Infrared Spectroscopy in the Region of the Fourier transform (FTIR), Energy Dispersive X-ray (EDX), Scanning Electron Microscopy (SEM) and cyclic voltammetry (VC). The FTIR spectra showed absorption bands at 1106 cm{sup -1} due to stretching Si-O-Si{sub (νSi-O-Si)} characteristic of the structure of octa(aminopropylsilsesquioxane and absorption bands at 2063 cm{sup -1} ascribed to the stretching NO{sub (νN-O}) and 2192 cm{sup -1} attributed to the stretching C≡N{sub (ν≡}N{sub )}. SEM and EDX observed cluster of cubic particles with an average size of approximately 241 nm, containing Si, O, N, Cu and Fe. Cyclic voltammogram of the material (ACCuN) showed a redox couple with average potential Eθ '= 0.73 V. (author)

  20. Synthesis and characterization of nano hydroxyapatite using reverse micro emulsions as nano reactors

    International Nuclear Information System (INIS)

    Amin, S.; Siddique, T.

    2015-01-01

    In the present work reverse micro emulsion has been employed as nano reactors to synthesize nano crystalline Hydroxyapatite (HA). Two precursors; calcium and phosphate with different counter ions of each were used for the synthesis of HA at two different temperatures. To maintain the emulsified nano reactor, cyclohexane, TX-100 and 1-butanol including phosphate precursor was the continuous phase while aqueous Ca precursor solution was taken as the dispersed phase. Nano crystalline particles thus produced were evaluated on the basis of synthesis route, counter ions and temperature. It has been shown that emulsified nano reactors control the morphology, particle size and minimize phase transformation of HA. Characterizations of nano powder of HA are carried out using x-ray diffraction (XRD), Fourier transform infra-red spectroscopy (FTIR), and scanning electron microscopy (SEM). HA crystallite size was found to be in the range of 20-25 nm whereas the morphology of nano particles changed from spheres to rods. (author)

  1. Synthesis and Photophysical Characterizations of Thermal -Stable Naphthalene Benzimidazoles

    OpenAIRE

    Erten Ela, Şule; Özçelik, Serdar; Eren, Ersin

    2011-01-01

    Microwave-assisted synthesis, photophysical and electrochemical properties of thermal-stable naphthalene benzimidazoles and naphthalimides are studied in this paper. Microwave-assisted synthesis of naphthalene benzimidazoles provide higher yields than the conventional thermal synthesis. Comparative photophysical properties of naphthalene benzimidazoles and naphthalimides are revealed that conjugation of electron-donating group onto naphthalimide moiety increases fluorescence ...

  2. Synthesis and Characterization of a Magnetically Active 19F Molecular Beacon.

    Science.gov (United States)

    Dempsey, Megan E; Marble, Hetal D; Shen, Tun-Li; Fawzi, Nicolas L; Darling, Eric M

    2018-02-21

    Gene expression is used extensively to describe cellular characteristics and behaviors; however, most methods of assessing gene expression are unsuitable for living samples, requiring destructive processes such as fixation or lysis. Recently, molecular beacons have become a viable tool for live-cell imaging of mRNA molecules in situ. Historically, beacon-mediated imaging has been limited to fluorescence-based approaches. We propose the design and synthesis of a novel molecular beacon for magnetic resonance detection of any desired target nucleotide sequence. The biologically compatible synthesis incorporates commonly used bioconjugation reactions in aqueous conditions and is accessible for laboratories without extensive synthesis capabilities. The resulting beacon uses fluorine ( 19 F) as a reporter, which is broadened, or turned "off", via paramagnetic relaxation enhancement from a stabilized nitroxide radical spin label when the beacon is not bound to its nucleic acid target. Therefore, the 19 F NMR signal of the beacon is quenched in its hairpin conformation when the spin label and the 19 F substituent are held in proximity, but the signal is recovered upon beacon hybridization to its specific complementary nucleotide sequence by physical separation of the radical from the 19 F reporter. This study establishes a path for magnetic resonance-based assessment of specific mRNA expression, providing new possibilities for applying molecular beacon technology in living systems.

  3. Quantitative phase analysis and microstructure characterization of magnetite nanocrystals obtained by microwave assisted non-hydrolytic sol–gel synthesis

    Energy Technology Data Exchange (ETDEWEB)

    Sciancalepore, Corrado, E-mail: corrado.sciancalepore@unimore.it [Department of Engineering “Enzo Ferrari”, University of Modena and Reggio Emilia, Via Pietro Vivarelli 10, 41100 Modena (Italy); Bondioli, Federica [Department of Industrial Engineering, University of Parma, Parco Area delle Scienze, 181/A, 43124 Parma (Italy); INSTM Consortium, Via G. Giusti 9, 51121 Firenze (Italy); Manfredini, Tiziano [Department of Engineering “Enzo Ferrari”, University of Modena and Reggio Emilia, Via Pietro Vivarelli 10, 41100 Modena (Italy); INSTM Consortium, Via G. Giusti 9, 51121 Firenze (Italy); Gualtieri, Alessandro [Department of Chemical and Geological Science, University of Modena and Reggio Emilia, Via S. Eufemia 19, 41121 Modena Italy (Italy)

    2015-02-15

    An innovative preparation procedure, based on microwave assisted non-hydrolytic sol–gel synthesis, to obtain spherical magnetite nanoparticles was reported together with a detailed quantitative phase analysis and microstructure characterization of the synthetic products. The nanoparticle growth was analyzed as a function of the synthesis time and was described in terms of crystallization degree employing the Rietveld method on the magnetic nanostructured system for the determination of the amorphous content using hematite as internal standard. Product crystallinity increases as the microwave thermal treatment is increased and reaches very high percentages for synthesis times longer than 1 h. Microstructural evolution of nanocrystals was followed by the integral breadth methods to obtain information on the crystallite size-strain distribution. The results of diffraction line profile analysis were compared with nanoparticle grain distribution estimated by dimensional analysis of the transmission electron microscopy (TEM) images. A variation both in the average grain size and in the distribution of the coherently diffraction domains is evidenced, allowing to suppose a relationship between the two quantities. The traditional integral breadth methods have proven to be valid for a rapid assessment of the diffraction line broadening effects in the above-mentioned nanostructured systems and the basic assumption for the correct use of these methods are discussed as well. - Highlights: • Fe{sub 3}O{sub 4} nanocrystals were obtained by MW-assisted non-hydrolytic sol–gel synthesis. • Quantitative phase analysis revealed that crystallinity up to 95% was reached. • The strategy of Rietveld refinements was discussed in details. • Dimensional analysis showed nanoparticles ranging from 4 to 8 nm. • Results of integral breadth methods were compared with microscopic analysis.

  4. Quantitative phase analysis and microstructure characterization of magnetite nanocrystals obtained by microwave assisted non-hydrolytic sol–gel synthesis

    International Nuclear Information System (INIS)

    Sciancalepore, Corrado; Bondioli, Federica; Manfredini, Tiziano; Gualtieri, Alessandro

    2015-01-01

    An innovative preparation procedure, based on microwave assisted non-hydrolytic sol–gel synthesis, to obtain spherical magnetite nanoparticles was reported together with a detailed quantitative phase analysis and microstructure characterization of the synthetic products. The nanoparticle growth was analyzed as a function of the synthesis time and was described in terms of crystallization degree employing the Rietveld method on the magnetic nanostructured system for the determination of the amorphous content using hematite as internal standard. Product crystallinity increases as the microwave thermal treatment is increased and reaches very high percentages for synthesis times longer than 1 h. Microstructural evolution of nanocrystals was followed by the integral breadth methods to obtain information on the crystallite size-strain distribution. The results of diffraction line profile analysis were compared with nanoparticle grain distribution estimated by dimensional analysis of the transmission electron microscopy (TEM) images. A variation both in the average grain size and in the distribution of the coherently diffraction domains is evidenced, allowing to suppose a relationship between the two quantities. The traditional integral breadth methods have proven to be valid for a rapid assessment of the diffraction line broadening effects in the above-mentioned nanostructured systems and the basic assumption for the correct use of these methods are discussed as well. - Highlights: • Fe 3 O 4 nanocrystals were obtained by MW-assisted non-hydrolytic sol–gel synthesis. • Quantitative phase analysis revealed that crystallinity up to 95% was reached. • The strategy of Rietveld refinements was discussed in details. • Dimensional analysis showed nanoparticles ranging from 4 to 8 nm. • Results of integral breadth methods were compared with microscopic analysis

  5. Synthesis and Characterization of a Micelle-Based pH Nanosensor with an Unprecedented Broad Measurement Range

    DEFF Research Database (Denmark)

    Ek, Pramod Kumar; Feldborg, Lise N.; Almdal, Kristoffer

    2013-01-01

    A new cross-linked micelle pH nanosensor design was investigated. The nanosensor synthesis was based on self-assembly of an amphiphilic triblock copolymer, poly(ethylene glycol)-b-poly(2-amino ethyl methacrylate)-b-poly(coumarin methacrylate) (PEG-b-PAEMA-b-PCMA), which was synthesized by isolated...... irradiation (320 nm pH nanosensors by binding the pH-sensitive fluorophores oregon green 488 and 2′,7′-bis-(2-carboxyethyl)-5-(and-6......) carboxyfluorescein and a reference fluorophore Alexa 633 to the PAEMA shell region of the micelles. Fluorescence measurements show that these pH nanosensors are sensitive in a surprisingly broad pH range of 3.4–8.0, which is hypothesized to be due to small differences in the individual fluorophores’ local...

  6. Synthesis, structural characterization and antitumor activity of a Ca(II) coordination polymer based on 4-formyl-1,3-benzenedisulfonate-2-furoic acid hydrazide ligands

    Energy Technology Data Exchange (ETDEWEB)

    Tai, Xi-Shi, E-mail: taixs@wfu.edu.cn [Weifang University, College of Chemistry and Chemical Engineering (China); Wang, Xin [Qinghai Normal University, Department of Chemistry (China)

    2017-03-15

    A new Ca(II) coordination polymer, ([CaL(H{sub 2}O){sub 4}] · (H{sub 2}O){sub 4}){sub n} (L = 4-formyl-1,3-benzenedisulfonate-2-furoic acid hydrazide) has been prepared by one-pot synthesis method. And it was characterized by elemental analysis, IR and thermal analysis. The result of X-ray single-crystal diffraction analysis shows that the Ca(II) complex molecules form one-dimensional chain structure by the bridging oxygen atoms. The anti-tumor activity of L ligand and the Ca(II) coordination polymer has also been studied.

  7. Synthesis and Spectral Characterization of Antifungal Sensitive Schiff Base Transition Metal Complexes

    Science.gov (United States)

    Sakthivel, A.; Rajasekaran, K.

    2007-01-01

    New N2O2 donor type Schiff base has been designed and synthesized by condensing acetoacetanilido-4-aminoantipyrine with 2-aminobenzoic acid in ethanol. Solid metal complexes of the Schiff base with Cu(II), Ni(II), Co(II), Mn(II), Zn(II), VO(IV), Hg(II) and Cd(II) metal ions were synthesized and characterized by elemental analyses, magnetic susceptibility, molar conduction, fast atom bombardment (FAB) mass, IR, UV-Vis, and 1H NMR spectral studies. The data show that the complexes have the composition of ML type. The UV-Vis. and magnetic susceptibility data of the complexes suggest a square-planar geometry around the central metal ion except VO(IV) complex which has square-pyramidal geometry. The in vitro antifungal activities of the compounds were tested against fungi such as Aspergillus niger, Aspergillus flavus, Rhizopus stolonifer, Candida albicans, Rhizoctonia bataicola and Trichoderma harizanum. All the metal complexes showed stronger antifungal activities than the free ligand. The minimum inhibitory concentrations (MIC) of the metal complexes were found in the range of 10~31 µg/ml. PMID:24015086

  8. New Homologues Series of Heterocyclic Schiff Base Ester: Synthesis and Characterization

    Directory of Open Access Journals (Sweden)

    Yee-Ting Chong

    2016-01-01

    Full Text Available A homologous series of liquid crystal bearing with heterocyclic thiophene Schiff base ester with alkanoyloxy chain (CH3(CH2nCOO–, where n=4, 6, 8, 10, 12, 14, 16 was successfully synthesized through the modification of some reported methods. The structural information of these compounds was isolated and characterized through some spectroscopic techniques, such as FTIR, 1H, and 13C NMR and elemental analysis. Textural observation was carried out using a polarizing optical microscope (POM over heating and cooling cycles. It was found that all synthesized compounds (3a–g exhibited an enantiotropic nematic phase upon the heating and cooling cycle with high thermal stability. Moreover, a characteristic bar transition texture was observed for compounds 3f and 3g which have shown transition of nematic-to-smectic C phase. This has been further confirmed by obtaining relative phase transition temperature using the differential scanning calorimetry (DSC.

  9. Synthesis, Structure, Stability and Redispersion of Gold-based Nanoparticles

    Science.gov (United States)

    Tiruvalam, Ram Chandra

    Nanoscale gold has been shown to possess an intriguing combination of unexpected optical, photochemical and catalytic properties. The ability to control the size, shape, morphology, composition and dispersion of gold-based nanostructures is key to optimizing their performance for nanotechnology applications. The advanced electron microscopy studies described in this thesis analyze three important aspects of gold and gold-palladium alloy nanoparticles: namely, (i) the ability to synthesize gold nanoparticles of controlled size and shape in an aqueous medium; (ii) the colloidal preparation of designer gold-palladium alloys for selective oxidation catalysis; and (iii) the ability to disperse gold as finely and homogeneously as possible on a metal oxide or carbon support. The ability to exploit the nanoscale properties of gold for various engineering applications often depends on our ability to control size and shape of the nanoscale entity by careful manipulation of the synthesis parameters. We have explored an aqueous based synthesis route, using oleylamine as both a reductant and surfactant, for preparing gold nanostructures. By systematically varying synthesis parameters such as oleylamine concentration, reaction temperature, and aging time it is possible to identify processing regimens that generate Au nanostructures having either pseudo-spherical, faceted polyhedral, nanostar or wire shaped morphologies. Furthermore, by quenching the reaction partway through it is possible to create a class of metastable Au-containing structures such as nanocubes, nanoboxes and nanowires. Possible formation mechanisms for these gold based nano-objects are discussed. There is a growing interest in using supported bimetallic AuPd alloy nanoparticles for selective oxidation reactions. In this study, a systematic series of size controlled AuPd bimetallic particles have been prepared by colloidal synthesis methods. Particles having random alloy structures, as well as `designer

  10. Synthesis and characterization of inorganic ion exchangers based on mixed oxide tin-titanium to be used in recovery of cadmium and nickel and photoluminescent studies

    International Nuclear Information System (INIS)

    Paganini, Paula Pinheiro

    2007-01-01

    This work presents the synthesis, characterization and adsorption studies of inorganic ion exchangers based on mixed tin-titanium oxide for recovery of cadmium and nickel metals from aqueous effluents, discarded in the environment mainly through Ni-Cd battery. The exchangers were synthesized by sol-gel modified method using a mixture of tin(IV) chloride and titanium(III) chloride and ammonium hydroxide, as precursors reagents. The materials obtained: SnO 2 /TiO 2 and SnO 2 /TiO 2 :Eu 3+ were characterized by infrared spectroscopy, thermal analysis, scattering electronic microscopy (SEM), X-ray powder diffraction (XRD) (powder method) and electronic spectroscopy (excitation and emission) for the europium doped exchanger. The same materials also were synthesized in polymeric matrix too and can be used in column, because the synthesized materials showed crystals size in nano metric scale. It was determined by the distribution ratios for metals taking as parameters the influence of pH, the concentration of metals (by adsorption isotherms) and the contact time (by adsorption kinetic). The inorganic ion exchanger presented high exchange capacity with adsorption percent above 90 por cent for the studied conditions, quickly kinetic, heterogeneous exchange surfaces, physic adsorption and spontaneous process of exchange. To the doped exchanger spectroscopy properties were studied and also it was calculated the intensity parameters and it was found a satisfactory quantum yield. (author)

  11. Synthesis and characterization of a new complex binuclear of binuclear of Pd(II) containing the antibiotic oxy tetracycline

    International Nuclear Information System (INIS)

    Guerra, Wendell; Fontes, Ana Paula Soares; Pereira-Maia, Elene Cristina

    2010-01-01

    This article reports the synthesis and characterization of a new binuclear complex of palladium (II) containing the antibiotic oxytetracycline. The complex was characterized by the usual techniques of analysis. With respect to sites of coordination, the IR spectral data suggests the involvement the oxygen of the amide group and the oxygen of the neighbor hydroxyl group at ring A and to the carbonyl oxygen at C11 and the hydroxyl group at C12. (author)

  12. Reduce synthesis temperature and improve dispersion of YAG nanopowders based on the co-crystallization method

    Energy Technology Data Exchange (ETDEWEB)

    Fan, G.F.; Tang, Y.Q.; Lu, W.Z., E-mail: lwz@mail.hust.edu.cn; Zhang, X.R.; Xu, X.

    2015-01-05

    Highlights: • YAG nanopowders were synthesized through a co-crystallization method. • A three-layer core–shell structure was made to lower the synthesis temperature. • PAA again reduced the synthesis temperature based on the core–shell structure. • YAG nanopowders were synthesized at 700 °C in normal apparatus. • Agglomeration was greatly improved by PAA. - Abstract: Pure yttrium aluminum garnet (YAG) nanopowders were synthesized at 950 °C from the co-crystallization precursor of Y(NO{sub 3}){sub 3}⋅6H{sub 2}O and Al(NO{sub 3}){sub 3}⋅9H{sub 2}O (nitrate process). When 17 wt.% of Y(NO{sub 3}){sub 3}⋅6H{sub 2}O was replaced by Y{sub 2}O{sub 3} nanopowders, so as to make up a three-layer core–shell structure of the precursor, the synthesis temperature was reduced to 850 °C (Y{sub 2}O{sub 3} process). Based on Y{sub 2}O{sub 3} process, further reducing the synthesis temperature to 700 °C was realized by adding polyacrylic acid (PAA, 50% M), which was used to shorten the distance of the metal ions and provide combustion heat (PAA process). TEM characterizations indicated that the powders produced through nitrate and Y{sub 2}O{sub 3} processes agglomerated, while the powders produced through PAA process were dispersed much better. The agglomerate size analysis results demonstrated that the powders produced through PAA process were with smaller agglomerate size and wider agglomerate size distribution than those through nitrate process or Y{sub 2}O{sub 3} process. And they were more likely to be sintered to YAG transparent ceramics.

  13. Ecosystem health pattern analysis of urban clusters based on emergy synthesis: Results and implication for management

    International Nuclear Information System (INIS)

    Su, Meirong; Fath, Brian D.; Yang, Zhifeng; Chen, Bin; Liu, Gengyuan

    2013-01-01

    The evaluation of ecosystem health in urban clusters will help establish effective management that promotes sustainable regional development. To standardize the application of emergy synthesis and set pair analysis (EM–SPA) in ecosystem health assessment, a procedure for using EM–SPA models was established in this paper by combining the ability of emergy synthesis to reflect health status from a biophysical perspective with the ability of set pair analysis to describe extensive relationships among different variables. Based on the EM–SPA model, the relative health levels of selected urban clusters and their related ecosystem health patterns were characterized. The health states of three typical Chinese urban clusters – Jing-Jin-Tang, Yangtze River Delta, and Pearl River Delta – were investigated using the model. The results showed that the health status of the Pearl River Delta was relatively good; the health for the Yangtze River Delta was poor. As for the specific health characteristics, the Pearl River Delta and Yangtze River Delta urban clusters were relatively strong in Vigor, Resilience, and Urban ecosystem service function maintenance, while the Jing-Jin-Tang was relatively strong in organizational structure and environmental impact. Guidelines for managing these different urban clusters were put forward based on the analysis of the results of this study. - Highlights: • The use of integrated emergy synthesis and set pair analysis model was standardized. • The integrated model was applied on the scale of an urban cluster. • Health patterns of different urban clusters were compared. • Policy suggestions were provided based on the health pattern analysis

  14. Synthesis-on” and “synthesis-off” modes of carbon arc operation during synthesis of carbon nanotubes

    International Nuclear Information System (INIS)

    Yatom, Shurik; Selinsky, Rachel S.

    2017-01-01

    Arc discharge synthesis of single-walled carbon nanotubes (SWCNTs) remains largely uncontrollable, due to incomplete understanding of the synthetic process itself. Here, we show that synthesis of SWCNTs by a carbon arc may not constitute a single continuous process, but may instead consist of two distinct modes. One of these, a “synthesis-on” mode, produces the majority of the nanomaterials. During the synthesis-on mode, proportionally more carbon nanotubes are collected than in another mode, a “synthesis-off” mode. Both synthesis-on and synthesis-off modes for a typical arc configuration, employing a hollow anode filled with a mixture of powdered metal catalyst and graphite, were characterized by using in situ electrical, imaging, and spectroscopic diagnostics, along with ex situ imaging and spectroscopy. The synthesis-on mode duration is rare compared to the total arc run-time, helping to explain the poor selectivity found in the final collected products, a known inadequacy of arc synthesis. Finally, the rarity of the synthesis on mode occurence may be due to the synthesis off mode being more favorable energetically.

  15. Incorporation of the zosteric sodium salt in silica nanocapsules: synthesis and characterization of new fillers for antifouling coatings

    Science.gov (United States)

    Ruggiero, Ludovica; Crociani, Laura; Zendri, Elisabetta; El Habra, Naida; Guerriero, Paolo

    2018-05-01

    In the last decade many commercial biocides were gradually banned for toxicity. This work reports, for the first time, the synthesis and characterization of silica nanocontainers loaded with a natural product antifoulant (NPA), the zosteric sodium salt which is a non-commercial and environmentally friendly product with natural origin. The synthesis approach is a single step dynamic self-assembly with tetraethoxysilane (TEOS) as silica precursor. Unlike conventional mesoporous silica nanoparticles, the structure of these silica nanocontainers provides loading capacity and allows prolonged release of biocide species. The obtained nanocapsules have been characterized morphologically by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The encapsulation was checked by FTIR ATR spectroscopy and thermogravimetric analyses. The results of the release studies show the great potential of the here presented newly developed nanofillers in all applications where a controlled release of non-toxic and environmentally friendly biocides is required.

  16. Synthesis, Characterization, and Catalytic Ability of U3O8/SiO2 Nocomposite Materials

    Science.gov (United States)

    Green, Fatima

    Applications of uranium oxide nanoparticles as oxidative catalysts is a field uncommonly studied. In the past, little research has been done to study the potential of this material for room temperature, catalytic breakdown of organic pollutants. Due to an increase in the presence of these pollutants in surface water, an effort to study these reactions in aqueous solution has been a high priority. To further enhance the properties of the nanoparticles, synthesis was performed using the sol-gel method. Characterization of the material was carried out using, Fourier transform infrared spectroscopy (FTIR), powder X-ray diffraction, (XRD) and transmission electron microscopy (TEM). This material has proven to be pure, crystalline alpha-phase U3O8 with an average particle size of 27 nm. Based on previous studies, we hypothesized that under ambient conditions our synthesized material will be able to effectively breakdown organic molecules in aqueous solution. Catalytic studies were monitored using titration techniques with oxalic acid as a model system. The decomposition percentages varied based on amounts of nanocomposite used and temperature controls.

  17. Synthesis and test of sorbents based on calcium aluminates for SE-SR

    International Nuclear Information System (INIS)

    Barelli, L.; Bidini, G.; Di Michele, A.; Gallorini, F.; Petrillo, C.; Sacchetti, F.

    2014-01-01

    Highlights: • Synthesis strategy of CaO incorporation into calcium aluminates was approached. • Three innovative sorbents (M1, M2, M3) were synthesized and characterized. • Sorption capacity of developed sorbents was evaluated in multi-cycle processes. • M3 sorbent showed best performance, much higher than conventional CaO ones. • M3 sorbent functionality in SE-SR process was verified. - Abstract: Greenhouse gases emission of power generation plants will be continuously tightened to achieve European targets in terms of CO 2 emissions. In particular, the switching to a sustainable power generation using fossil fuels will be strongly encouraged in the future. In this context, sorption-enhanced steam reforming (SE-SR) is a promising process because it can be implemented as a CCS pre-combustion methodology. The purpose of this study is to develop and test innovative materials in order to overcome main limitations of standard CaO sorbent, usually used in the SE-SR process. The investigated innovative sorbents are based on incorporation of CaO particles into inert materials which significantly reduce the performance degradation. In particular, sorbent materials based on calcium aluminates were considered, investigating different techniques of synthesis. All synthesized materials were packed, together with the catalyst, in a fixed bed reactor and tested in sorption/regeneration cycles. Significant improvements were obtained respect to standard CaO regarding sorption capacity stability exhibited by the sorbent

  18. Synthesis and characterization of composites HoMn_1_-_x(Ni,Co)_xO_3

    International Nuclear Information System (INIS)

    Santos, Cassio Morilla dos

    2011-01-01

    In this work was accomplished the synthesis process and structural and magnetic characterization of HoMn_1_-_X(Ni,Co)_XO_3 compounds of perovskite structure. The samples synthesis were performed through modified polymeric precursor method. After synthesis and solvent removal, the polymer resin formed was treated at 350 deg C/4h for organic constituents removal, followed by heating treatment at 500 deg C/4h and 900 deg C/20h to obtain the crystalline phase. For structural characterization, it was used D10B-XPD beam line of Laboratorio Nacional de Luz Sincrotron (LNLS), where X-rays wavelengths below cobalt, manganese and nickel absorption edge, were used. The formation of HoNi_0_._5_0Mn_0_._5_0O_3, HoCo_0_._5_0Mn_0_._5_0O_3 and HoNi_0_._2_5Co_0_._2_5Mn_0_._5_0O_3 phases were observed by X-ray diffraction technique. By Rietveld refinement method for sample HoNi_0_._2_5Co_0_._2_5Mn_0_._5_0O_3, it was determined that cobalt and nickel had similar occupations at the top and bottom of unit cell, while the manganese preferentially occupied plan 002. The magnetic response of samples was studied through magnetization curves according to the temperature function and the applied magnetic field. The ZFC curves showed a paramagnetic response associated to holmium magnetic moment, and ferromagnetism, antiferromagnetism and ferrimagnetism coexistence, due to sublattices formed by transition metals. The FC curves evidenced the spin reversal phenomenon, associated to the interaction between the sublattice formed by transition metals with sublattices formed by rare-earth, considering a mechanism of antiferromagnetic exchange interaction. (author)

  19. SYNTHESIS AND CHARACTERIZATION OF NOVEL M(II) (M = Mn(II ...

    African Journals Online (AJOL)

    The coordination chemistry towards the M(II) metal centre (M = Mn, Ni, Cu or ... On continuing our work in the field of the synthesis of hydrazide ligand and the studies of ... The 1H and 13C NMR spectra of the Schiff base were recorded in CDCl3 on a ..... The octahedral geometry can be supported by the d–d transition bands ...

  20. Synthesis of Hydrocarbons from H2-Deficient Syngas in Fischer-Tropsch Synthesis over Co-Based Catalyst Coupled with Fe-Based Catalyst as Water-Gas Shift Reaction

    Directory of Open Access Journals (Sweden)

    Ting Ma

    2015-01-01

    Full Text Available The effects of metal species in an Fe-based catalyst on structural properties were investigated through the synthesis of Fe-based catalysts containing various metal species such, as Mn, Zr, and Ce. The addition of the metal species to the Fe-based catalyst resulted in high dispersions of the Fe species and high surface areas due to the formation of mesoporous voids about 2–4 nm surrounded by the catalyst particles. The metal-added Fe-based catalysts were employed together with Co-loaded beta zeolite for the synthesis of hydrocarbons from syngas with a lower H2/CO ratio of 1 than the stoichiometric H2/CO ratio of 2 for the Fischer-Tropsch synthesis (FTS. Among the catalysts, the Mn-added Fe-based catalyst exhibited a high activity for the water-gas shift (WGS reaction with a comparative durability, leading to the enhancement of the CO hydrogenation in the FTS in comparison with Co-loaded beta zeolite alone. Furthermore, the loading of Pd on the Mn-added Fe-based catalyst enhanced the catalytic durability due to the hydrogenation of carbonaceous species by the hydrogen activated over Pd.

  1. Spectroscopic characterization of metal complexes of novel Schiff base. Synthesis, thermal and biological activity studies

    Science.gov (United States)

    Omar, M. M.; Mohamed, Gehad G.; Ibrahim, Amr A.

    2009-07-01

    Novel Schiff base (HL) ligand is prepared via condensation of 4-aminoantipyrine and 2-aminobenzoic acid. The ligand is characterized based on elemental analysis, mass, IR and 1H NMR spectra. Metal complexes are reported and characterized based on elemental analyses, IR, 1H NMR, solid reflectance, magnetic moment, molar conductance and thermal analyses (TGA, DrTGA and DTA). The molar conductance data reveal that all the metal chelates are non-electrolytes. IR spectra show that HL is coordinated to the metal ions in a uninegatively tridentate manner with NNO donor sites of the azomethine N, amino N and deprotonated caroxylic-O. From the magnetic and solid reflectance spectra, it is found that the geometrical structures of these complexes are octahedral. The thermal behaviour of these chelates shows that the hydrated complexes losses water molecules of hydration in the first step followed immediately by decomposition of the anions and ligand molecules in the subsequent steps. The activation thermodynamic parameters, such as, E*, ΔH*, ΔS* and ΔG* are calculated from the DrTG curves using Coats-Redfern method. The synthesized ligands, in comparison to their metal complexes also were screened for their antibacterial activity against bacterial species, Escherichia Coli, Pseudomonas aeruginosa, Staphylococcus Pyogones and Fungi (Candida). The activity data show that the metal complexes to be more potent/antibacterial than the parent Shciff base ligand against one or more bacterial species.

  2. Synthesis and characterization of nanostructured titanium carbide for fuel cell applications

    Energy Technology Data Exchange (ETDEWEB)

    Singh, Paviter; Singh, Harwinder; Singh, Bikramjeet; Kaur, Manpreet; Kaur, Gurpreet; Kumar, Akshay, E-mail: akshaykumar.tiet@gmail.com [Advanced Functional Material Laboratory, Department of Nanotechnology,, Sri Guru Granth Sahib World University, Fatehgarh Sahib-140 406 Punjab (India); Kumar, Manjeet [Department of Materials Engineering, Defense Institute of Advanced Technology (DU), Pune-411 025 (India); Bala, Rajni [Department of Mathematics Punjabi University Patiala-147 002 Punjab (India)

    2016-04-13

    Titanium carbide (TiC) nanoparticles have been successfully synthesized by carbo-thermic reaction of titanium and acetone at 800 °C. This method is relatively low temperature synthesis route. It can be used for large scale production of TiC. The synthesized nanoparticles have been characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and differential thermal analyzer (DTA) techniques. XRD analysis confirmed the formation of single phase TiC. XRD analysis confirmed that the particles are spherical in shape with an average particle size of 13 nm. DTA analysis shows that the phase is stable upto 900 °C and the material can be used for high temperature applications.

  3. CsPb2Br5 Single Crystals: Synthesis and Characterization

    KAUST Repository

    Dursun, Ibrahim

    2017-08-02

    CsPb2Br5 is a ternary halogen-plumbate material with close characteristics to well-reported halide perovskites. Due to its unconventional two-dimensional structure, CsPb2Br5 is being looked at broadly for potential applications in optoelectronics. CsPb2Br5 investigations are currently limited to nanostructures and powder forms of the material, which present unclear and conflicting optical properties. In this study, we present the synthesis and characterization of CsPb2Br5 bulk single crystals, which enabled us to finally clarify the material\\'s optical features. Our CsPb2Br5 crystal has a two-dimensional structure with Pb2Br5- layers spaced by Cs+ cations, and exhibits a ~3.1 eV indirect bandgap with no emission in the visible spectrum.

  4. Synthesis, characterization and antibacterial property of ZnO:Mg nanoparticles

    Science.gov (United States)

    Kompany, A.; Madahi, P.; Shahtahmasbi, N.; Mashreghi, M.

    2012-09-01

    Sol-gel method was successfully used for the synthesis of ZnO nanoparticles (NPs) doped with different concentrations of Mg and the structural, optical and antibacterial properties of the nanoparticles were studied. The synthesized ZnO:Mg powders were characterized using x-ray diffraction (XRD), transmission electron microscopy (TEM), Fourier transformation Infrared (FTIR) and UV-Vis spectroscopy. It was revealed that the samples have hexagonal Wurtzite structure, and the phase segregation takes place for 15% Mg content. TEM images show that the average size of the particles is about 50 nm. Also, the antibacterial activities of the nanoparticles were tested against Escherichia coli (Gram negative) cultures. ZnO:Mg nanofluid showed good antibacterial activity which increases with the increase of NPs concentration, and decreases slightly with the amount of Mg.

  5. Synthesis and Characterization of Novel Polymethylene-Based 3-Miktoarm Star Copolymers by Combining Polyhomologation with Other Living Polymerizations

    KAUST Repository

    Altaher, Maryam

    2015-01-01

    Polyethylene (PE) is produced in a huge scale globally and has plenty of desirable properties. It is used in coating, packaging, and artificial joint replacements. The growing need for high performance polyethylene led to the development of new catalysts, monomers and polymerizations. The synthesis of polymethylene (equivalent to polyethylene) by living polyhomologation opened the way to well-defined polymethylenes-based polymeric materials with controlled structure, molecular weight and narrow polydispersity. Such model polymers are substantial to study the structure-properties relationships. This research presents a new strategy based on the in situ formation of B-thexyl-silaboracyclic serving as initiating sites for the polyhomologation of dimethylsulfoxonium methylide. Combination with metal-free ring-opening polymerization (ROP) of ɛ-caprolactone (CL) and atom transfer radical polymerization (ATRP) of styrene led to three polymethylene-based 3-miktoarm stars copolymers PCL(PM-OH)2, Br-PCL(PM-OH)2 and PS(PM-OH)2.

  6. Synthesis and Characterization of Novel Polymethylene-Based 3-Miktoarm Star Copolymers by Combining Polyhomologation with Other Living Polymerizations

    KAUST Repository

    Altaher, Maryam

    2015-05-01

    Polyethylene (PE) is produced in a huge scale globally and has plenty of desirable properties. It is used in coating, packaging, and artificial joint replacements. The growing need for high performance polyethylene led to the development of new catalysts, monomers and polymerizations. The synthesis of polymethylene (equivalent to polyethylene) by living polyhomologation opened the way to well-defined polymethylenes-based polymeric materials with controlled structure, molecular weight and narrow polydispersity. Such model polymers are substantial to study the structure-properties relationships. This research presents a new strategy based on the in situ formation of B-thexyl-silaboracyclic serving as initiating sites for the polyhomologation of dimethylsulfoxonium methylide. Combination with metal-free ring-opening polymerization (ROP) of ɛ-caprolactone (CL) and atom transfer radical polymerization (ATRP) of styrene led to three polymethylene-based 3-miktoarm stars copolymers PCL(PM-OH)2, Br-PCL(PM-OH)2 and PS(PM-OH)2.

  7. Supporting Information Synthesis of fatty monoester lubricant base ...

    Indian Academy of Sciences (India)

    Synthesis of fatty monoester lubricant base oil catalyzed by Fe-Zn ... Physical properties of fatty acid monoesters viz., kinematic viscosity, viscosity index, density ... The analysis method involves titration of the diluted sample with ethanolic alkali ...

  8. Synthesis and characterization of hydroxyapatite (HAp) for binder tungstate in 188W/188Re generator system

    International Nuclear Information System (INIS)

    Eni Hartati; Yati B Yuliyati; Duyeh Setiawan

    2014-01-01

    In this study, the synthesis of hydroxyapatite has been carried out through a process of precipitation of calcium hydroxide (Ca(OH) 2 ) with phosphoric acid (H 3 PO 4 ) based on acid base reaction process that produce crystalline solid and then it will be used for binder tungstate in 188 W/ 188 Re generator system. The purpose of this study were to characterize the results of synthesized hydroxyapatite and to determine the optimum conditions on generator 188 W/ 188 Re performance such as activation of the heating hydroxyapatite, pH of Na 2 WO 4 , reaction temperature, distribution coefficient and the adsorption capacity (adsorption coefficient) of hydroxyapatite. The characterization of synthesized hydroxyapatite was done using FTIR, XRD and SEM-EDAX, while the determination of the optimum condition of each parameters based on distribution coefficient and adsorption capacity hydroxyapatite using spectrophotometric method. The FTIR results of hydroxyapatite (Ca 10 (PO 4 ) 6 (OH) 2 ) showed the appearance of peaks in the O-H stretching wave number (υ) and 3434.9 cm -1 and 563.8 cm -1 , while the group PO 4 -3 is shown by the P-O bond in (υ) 1033.8 cm -1 . The XRD results indicate that hydroxyapatite had three peaks at 2θ region is 31,875° , 32,205° and 33,080°. Characterization by SEM showed columnar morphology with a particle size of 200 nm. The optimum conditions of each parameter obtained at hydroxyapatite heating temperature 100 °C, Na 2 WO 4 solution pH 3, and the reaction temperature of 60 °C, which gave result on distribution coefficients of 193.74 mL/g and adsorption capacity (adsorption coefficient) of 5.20 mg W/g HAp. (author)

  9. Ultrafiltration membranes from waste polyethylene terephthalate and additives: synthesis and characterization

    Directory of Open Access Journals (Sweden)

    Smitha Rajesh

    2014-01-01

    Full Text Available The synthesis and characterization of asymmetric ultrafiltration membranes from recycled polyethylene terephthalate (PET and polyvinylpyrrolidone (PVP is reported. PET is currently used in many applications, including the manufacture of bottles and tableware. Monomer extraction from waste PET is expensive, and this process has not yet been successfully demonstrated on a viable scale. Hence, any method to recycle or regenerate PET once it has been used is of significant importance from scientific and environmental research viewpoints. Such a process would be a green alternative due to reduced raw monomer consumption and the additional benefit of reduced manufacturing costs. The membranes described here were prepared by a phase-inversion process, which involved casting a solution containing PET, m-cresol as solvent, and polyethylene glycol (PEG of different molecular weights as additives. The membranes were characterized in terms of pure water permeability (PWP, molecular weight cut-off (MWCO, and flux and membrane morphology. The results show that the addition of PEG with high molecular weights leads to membranes with higher PWP. The presence of additives affects surface roughness and membrane morphology.

  10. Low Temperature Solid-State Synthesis and Characterization of LaBO3

    Directory of Open Access Journals (Sweden)

    Azmi Seyhun KIPÇAK

    2016-11-01

    Full Text Available Rare earth (lanthanide series borates, possess high vacuum ultraviolet (VUV transparency, large electronic band gaps, chemical and environmental stability and exceptionally large optical damage thresholds and used in the development of plasma display panels (PDPs. In this study the synthesis of lanthanum borates via solid-state method is studied. For this purpose, lanthanum oxide (La2O3 and boric acid (H3BO3 are used for as lanthanum and boron sources, respectively. Different elemental molar ratios of La to B (between 3:1 to 1:6 as La2O3:H3BO3 were reacted by solid-state method at the reaction temperatures between 500°C - 700°C with the constant reaction time of 4 h. Following the synthesis, characterizations of the synthesized products are conducted by X-ray diffraction (XRD, Fourier transform infrared spectroscopy (FT-IR, Raman spectroscopy and scanning electron microscope (SEM. From the results of the experiments, three types of lanthanum borates of; La3BO6, LaBO3 and La(BO23 were observed at different reaction parameters. Among these three types of lanthanum borates LaBO3 phase were obtained as a major phase.

  11. Synthesis, characterization and antibacterial study on the chitosan-functionalized Ag nanoparticles.

    Science.gov (United States)

    Biao, Linhai; Tan, Shengnan; Wang, Yuanlin; Guo, Ximin; Fu, Yujie; Xu, Fengjie; Zu, Yuangang; Liu, Zhiguo

    2017-07-01

    This study provided a facile, one-step hydrothermal method to synthesize stable Ag colloid in aqueous solution by utilizing chitosan as both reductant and stabilizer. The formation of chitosan-functionalized Ag nanoparticles was verified by UV-Vis, FTIR, TEM, AFM and XRD measurements. FTIR results revealed that the primary amine groups and amide groups of chitosan have specific interactions with the surface of Ag nanoparticles. The average diameter of the Ag nanoparticles is 10.0±5.4nm as determined by TEM. Ag nanoparticles are highly crystalline as revealed by HR-TEM and XRD measurements. The size and shape of Ag nanoparticles are also found to depend on the pH condition in the synthesis. Ag nanoparticles were the main products at pH5.0 whereas large Ag nanotriangle and truncated triangular nanoplate were dominant at pH4.0 in the synthesis. Due to its monodispersity and good stability, the chitosan-functionalized Ag colloid synthesized at pH5.0 was further tested for its antibacterial activities against gram-positive bacteria, gram-negative bacteria and fungus. The results of zone of inhibition, inhibition ratio and SEM characterization revealed that chitosan-functionalized Ag nanoparticles have great bactericidal efficiency against both bacteria and fungus. Copyright © 2017 Elsevier B.V. All rights reserved.

  12. Synthesis and characterization of maltose-based amphiphiles as supramolecular hydrogelators.

    Science.gov (United States)

    Clemente, María J; Fitremann, Juliette; Mauzac, Monique; Serrano, José L; Oriol, Luis

    2011-12-20

    Low molecular mass amphiphilic glycolipids have been prepared by linking a maltose polar head and a hydrophobic linear chain either by amidation or copper(I)-catalyzed azide-alkyne [3 + 2] cycloaddition. The liquid crystalline properties of these amphiphilic materials have been characterized. The influence of the chemical structure of these glycolipids on the gelation properties in water has also been studied. Glycolipids obtained by the click coupling of the two components give rise to stable hydrogels at room temperature. The fibrillar structure of supramolecular hydrogels obtained by the self-assembly of these gelators have been characterized by electron microscopy. Fibers showed some torsion, which could be related with a chiral supramolecular arrangement of amphiphiles, as confirmed by circular dichroism (CD). The sol-gel transition temperature was also determined by differential scanning calorimetry (DSC) and NMR. © 2011 American Chemical Society

  13. Synthesis and characterization of zirconium molybdates of 99 Mo/99m Tc generators

    International Nuclear Information System (INIS)

    Contreras R, A.; Monroy G, F.; Diaz A, L.V.

    2002-01-01

    The zirconium molybdates are gels which are used as cation exchangers in the production of 99 Mo/ 99m Tc generators. The synthesis method and the characterization of these gels by thermogravimetry, infrared spectroscopy and X-ray diffraction is presented with the purpose of finding which the factors are that influence in the efficiency of the 99m Tc production. The results show that the quantity of molecular water contained in gel, is possibly the cause of variations of the efficiencies of the 99 Mo/ 99m Tc generator. (Author)

  14. Design, synthesis, and characterization of new phosphazene related materials, and study the structure property correlations

    Science.gov (United States)

    Tian, Zhicheng

    The work described in this thesis is divided into three major parts, and all of which involve the exploration of the chemistry of polyphosphazenes. The first part (chapters 2 and 3) of my research is synthesis and study polyphoshazenes for biomedical applications, including polymer drug conjugates and injectable hydrogels for drug or biomolecule delivery. The second part (chapters 4 and 5) focuses on the synthesis of several organic/inorganic hybrid polymeric structures, such as diblock, star, brush and palm tree copolymers using living cationic polymerization and atom transfer radical polymerization techniques. The last part (chapters 6 and 7) is about exploratory synthesis of new polymeric structures with fluorinated side groups or cycloaliphatic side groups, and the study of new structure property relationships. Chapter 1 is an outline of the fundamental concepts for polymeric materials, as such the history, important definitions, and some introductory material for to polymer chemistry and physics. The chemistry and applications of phopshazenes is also briefly described. Chapter 2 is a description of the design, synthesis, and characterization of development of a new class of polymer drug conjugate materials based on biodegradable polyphosphazenes and antibiotics. Poly(dichlorophosphazene), synthesized by a thermal ring opening polymerization, was reacted with up to 25 mol% of ciprofloxacin or norfloxacin and three different amino acid esters (glycine, alanine, or phenylalanine) as cosubstituents via macromolecular substitutions. Nano/microfibers of several selected polymers were prepared by an electrospinning technique. Chapter 3 is concerned with the development of a class of injectable and biodegradable hydrogels based on water-soluble poly(organophosphazenes) containing oligo(ethylene glycol) methyl ethers and glycine ethyl esters. The hydrogels can be obtained by mixing alpha-cyclodextrin aqueous solution and poly(organophosphazenes) aqueous solution in

  15. Synthesis of Cyclic Polymers and Characterization of Their Diffusive Motion in the Melt State at the Single Molecule Level

    KAUST Repository

    Habuchi, Satoshi; Yamamoto, Takuya; Tezuka, Yasuyuki

    2016-01-01

    We demonstrate a method for the synthesis of cyclic polymers and a protocol for characterizing their diffusive motion in a melt state at the single molecule level. An electrostatic self-assembly and covalent fixation (ESA-CF) process is used

  16. Synthesis and electrochemical characterization of palladium-based cathode catalysts, resistant to the presence of methanol; Sintesis y caracterizacion electroquimica de catalizadores catodicos base paladio, resistentes a la presencia de metanol

    Energy Technology Data Exchange (ETDEWEB)

    Salvador, Jose J. [Centro de Investigacion y de Estudios Avanzados del IPN, Mexico D.F. (Mexico)] e-mail: jsalvador@cinvestav.mx; Collins, Virginia H. [Centro de Investigacion en Materiales Avanzados, Chihuahua, Chihuahua (Mexico); Solorza Feria, Omar [Centro de Investigacion y de Estudios Avanzados del IPN, Mexico D.F. (Mexico)

    2009-09-15

    This work presents the synthesis and characterization of palladium-based electrocatalysts (PdSn and PdPtSn) prepared with the salt-reduction method for oxygen reduction reaction (ORR). The compounds obtained are characterized by sweep electron microscopy, electron transmission microscopy and x-ray diffraction of powder. The electrocatalysts obtained had particle sizes less than 10 nm. The evaluation of the catalytic activity of the catalysts was performed using cyclic voltametry and rotating disc electrode. These experiments were conducted in an H{sub 2}SO{sub 4} 0.5 M solution with different methanol concentrations. The presence of methanol improved the catalytic activity of PdSn, but did not show any effect on the PdPtSn alloy. The performance of the DMFC mono cell using PdPtSn as a cathode showed a potential of 10 mW cm{sup -2} at 50 degrees Celsius. [Spanish] En este trabajo se presenta la sintesis y caracterizacion de electrocatalizadores de base Paladio (PdSn y PdPtSn) preparados mediante el metodo de reduccion de sales, para la reaccion de reduccion de oxigeno (RRO). Los compuestos obtenidos se caracterizaron por microscopia electronica de barrido, microscopia electronica de transmision y difraccion de rayos X de polvos. Los electrocatalizadores obtenidos presentaron un tamano de particula menores a 10 nm. La evaluacion de la actividad catalitica de los catalizadores se llevo a cabo mediante voltametria Ciclica y electrodo de disco rotatorio, estos experimentos fueron realizados en una solucion de H{sub 2}SO{sub 4} 0.5 M con diferentes concentraciones de metanol. La presencia de metanol mejoro la actividad catalitica de PdSn, pero no mostro ningun efecto sobre la aleacion PdPtSn. El desempeno de la monocelda de DMFC usando como catodo PdPtSn, mostro una potencia de 10 mW cm{sup -2} a 50 grados centigrados.

  17. MnWO{sub 4} nanocapsules: Synthesis, characterization and its electrochemical sensing property

    Energy Technology Data Exchange (ETDEWEB)

    Muthamizh, Selvamani; Suresh, Ranganathan; Giribabu, Krishnamoorthy; Manigandan, Ramadoss; Praveen Kumar, Sivakumar; Munusamy, Settu; Narayanan, Vengidusamy, E-mail: vnnara@yahoo.co.in

    2015-01-15

    Highlights: • Synthesis of MnWO{sub 4} nanocapsules without use of any other external reagent. • High crystalline MnWO{sub 4} was obtained with phase purity. • Electrochemical sensing platform based on MnWO{sub 4} for sensing quercetin. • Micromolar detection ability of MnWO{sub 4} modified GCE. - Abstract: Manganese tungstate (MnWO{sub 4}) was synthesized by surfactant free precipitation method. MnWO{sub 4} was characterized by using various spectroscopic techniques. The phase, crystalline nature and the morphological analysis were carried out using XRD, scanning electron microscopy (SEM), and high resolution transmission electron microscopy (HR-TEM). Further, FT-IR, Raman, and DRS-UV–Vis spectral analysis were carried out in order to ascertain the optical property and the presence of functional groups. From the analysis, the morphology of the MnWO{sub 4} was observed to be in capsules with breadth and thickness were in nm range. The oxidation state of tungsten (W), and manganese (Mn) were investigated using X-ray photo electron spectroscopy (XPS) and electron paramagnetic resonance spectroscopy (EPR). The synthesized MnWO{sub 4} nanocapsules were used to modify glassy carbon electrode (GCE) to detect quercetin.

  18. Adsorption and Deactivation Characteristics of Cu/ZnO-Based Catalysts for Methanol Synthesis from Carbon Dioxide

    Energy Technology Data Exchange (ETDEWEB)

    Natesakhawat, Sittichai; Ohodnicki, Paul R; Howard, Bret H; Lekse, Jonathan W; Baltrus, John P; Matranga, Christopher

    2013-07-09

    The adsorption and deactivation characteristics of coprecipitated Cu/ZnO-based catalysts were examined and correlated to their performance in methanol synthesis from CO₂ hydrogenation. The addition of Ga₂O₃ and Y₂O₃ promoters is shown to increase the Cu surface area and CO₂/H₂ adsorption capacities of the catalysts and enhance methanol synthesis activity. Infrared studies showed that CO₂ adsorbs spontaneously on these catalysts at room temperature as both monoand bi-dentate carbonate species. These weakly bound species desorb completely from the catalyst surface by 200 °C while other carbonate species persist up to 500 °C. Characterization using N₂O decomposition, X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), and transmission electron microscopy (TEM) with energy-dispersive X-ray spectroscopy (EDX) analysis clearly indicated that Cu sintering is the main cause of catalyst deactivation. Ga and Y promotion improves the catalyst stability by suppressing the agglomeration of Cu and ZnO particles under pretreatment and reaction conditions.

  19. Synthesis and characterization of optical and electrical composite hybrid PVAl/CdS

    International Nuclear Information System (INIS)

    Oliveira, M.S.; Aquino, H.A.

    2010-01-01

    Aiming to develop new hybrid nanocomposite materials that present the physical properties of both components which allows to be applied in a variety of areas of nanotechnology among them in photonics, optoelectronics and sensor. The hybrid organic / inorganic PVAl / CdS is compound of a polymer matrix the polyvinyl alcohol (PVAl) and phase second cadmium sulfide (CdS), the synthesis was to did using the 'hydrothermal method' with five different concentrations of CdS between 0.05 and 0.7% (w/w). The hybrid solution obtained is to put sth down on glass substrate by the method 'Casting' so we get films with thicknesses ranging from 20 and 150 μm. The morphology of the films was characterized by X ray diffraction (DRX) and ultraviolet-visible spectroscopy (UV-vis). And the influence of CdS on the dielectric behavior in the films of PVAl / CdS, as dielectric relaxation (relaxation frequencies) were characterized by impedance spectroscopy. (author)

  20. Synthesis and Characterization of a Chondroitin Sulfate Based Hybrid Bio/Synthetic Biomimetic Aggrecan Macromolecule

    Science.gov (United States)

    Sarkar, Sumona

    Lower back pain resulting from intervertebral disc degeneration is one of the leading musculoskeletal disorders confronting our health system. In order to mechanically stabilize the disc early in the degenerative cascade and prevent the need for spinal fusion surgeries, we have proposed the development of a hybrid-bio/synthetic biomimetic proteoglycan macromolecule for injection into the disc in the early stages of degeneration. The goal of this thesis was to incorporate natural chondroitin sulfate (CS) chains into bottle brush polymer synthesis strategies for the fabrication of CS-macromolecules which mimic the proteoglycan structure and function while resisting enzymatic degradation. Both the "grafting-to" and "grafting-through" techniques of bottle brush synthesis were explored. CS was immobilized via a terminal primary amine onto a model polymeric backbone (polyacrylic acid) for investigation of the "grafting-to" strategy and an epoxy-amine step-growth polymerization technique was utilized for the "grafting-through" synthesis of CS-macromolecules with polyethylene glycol backbone segments. Incorporation of a synthetic polymeric backbone at the terminal amine of CS was confirmed via biochemical assays, 1H-NMR and FTIR spectroscopy, and CS-macromolecule size was demonstrated to be higher than that of natural CS via gel permeation chromatography, transmission electron microscopy and viscosity measurements. Further analysis of CS-macromolecule functionality indicated maintenance of natural CS properties such as high fixed charge density, high osmotic potential and low cytotoxicity with nucleus pulposus cells. These studies are the first attempt at the incorporation of natural CS into biomimetic bottle brush structures. CS-macromolecules synthesized via the methods developed in these studies may be utilized in the treatment and prevention of debilitating back pain as well as act as mimetics for other proteoglycans implicated in cartilage, heart valve, and nervous

  1. Synthesis and characterization of cationic lipid coated magnetic nanoparticles using multiple emulsions as microreactors

    Energy Technology Data Exchange (ETDEWEB)

    Akbaba, Hasan; Karagöz, Uğur [Ege University, Faculty of Pharmacy, Department of Pharmaceutical Biotechnology, 35100 Izmir (Turkey); Selamet, Yusuf [Izmir Institute of Technology, Faculty of Science, Department of Physics, 35433 Izmir (Turkey); Kantarcı, A. Gülten, E-mail: gulten.kantarci@ege.edu.tr [Ege University, Faculty of Pharmacy, Department of Pharmaceutical Biotechnology, 35100 Izmir (Turkey)

    2017-03-15

    The aim of this study was to develop a novel iron oxide nanoparticle synthesis method with in-situ surface coating. For this purpose multiple emulsions were used as microreactors for the first time and magnetic iron oxide particles synthesized in the core of cationic solid lipid nanoparticles. DLS, SEM, TEM, VSM, Raman Spectrometer, XRD, and XPS techniques were performed for characterization of the magnetic nanoparticles. Obtained magnetic nanoparticles are superparamagnetic and no additional process was needed for surface adjustments. They are positively charged as a result of cationic lipid coating and has appropriate particle size (<30 nm) for drug or nucleic acid delivery. Structure analysis showed that magnetic core material is in the form of magnetite. Saturation magnetization value was measured as 15–17 emu g{sup −1} for lipid coated magnetic nanoparticles obtained by multiple emulsion method which is reasonably sufficient for magnetic targeting. - Highlights: • A novel iron oxide nanoparticle synthesis method with in-situ surface coating. • Combining advantages of microemulsions and multiple emulsion methods. • Multiple emulsions were used as microreactors for magnetic nanoparticle synthesis. • Superparamagnetic iron oxide particles synthesized in the core of cationic lipids. • Possible delivery systems for nucleic acids, oil soluble compounds or drugs.

  2. Chemistry of the Colloidal Group II-VI Nanocrystal Synthesis

    International Nuclear Information System (INIS)

    Liu, Haitao

    2007-01-01

    In the last two decades, the field of nanoscience and nanotechnology has witnessed tremendous advancement in the synthesis and application of group II-VI colloidal nanocrystals. The synthesis based on high temperature decomposition of organometallic precursors has become one of the most successful methods of making group II-VI colloidal nanocrystals. This method is first demonstrated by Bawendi and coworkers in 1993 to prepare cadmium chalcogenide colloidal quantum dots and later extended by others to prepare other group II-VI quantum dots as well as anisotropic shaped colloidal nanocrystals, such as nanorod and tetrapod. This dissertation focuses on the chemistry of this type of nanocrystal synthesis. The synthesis of group II-VI nanocrystals was studied by characterizing the molecular structures of the precursors and products and following their time evolution in the synthesis. Based on these results, a mechanism was proposed to account for the 2 reaction between the precursors that presumably produces monomer for the growth of nanocrystals. Theoretical study based on density functional theory calculations revealed the detailed free energy landscape of the precursor decomposition and monomer formation pathway. Based on the proposed reaction mechanism, a new synthetic method was designed that uses water as a novel reagent to control the diameter and the aspect ratio of CdSe and CdS nanorods

  3. Synthesis and Characterization of Processable Polyaniline Salts

    International Nuclear Information System (INIS)

    Gul, Salma; Bilal, Salma; Shah, Anwar-ul-Haq Ali

    2013-01-01

    Polyaniline (PANI) is one of the most promising candidates for possible technological applications. PANI has potential applications in batteries, anion exchanger, tissue engineering, inhibition of steel corrosion, fuel cell, sensors and so on. However, its insolubility in common organic solvents limits its range of applications. In the present study an attempt has been made to synthesize soluble polyaniline salt via inverse polymerization pathway using benzoyl peroxide as oxidant and dodecylbenzenesulfonic acid (DBSA) as dopant as well as a surfactant. A mixture of chloroform and 2-butanol was used as dispersion medium for the first time. The influence of synthesis parameters such as concentration of aniline, benzoyl peroxide and DBSA on the yield and other properties of the resulting PANI salt was studied. The synthesized PANI salt was found to be completely soluble in DMSO, DMF, chloroform and in a mixture of toluene and 2-propanol. The synthesized polymer salt was also characterized with cyclic voltam-metry, SEM, XRD, UV-Vis spectroscopy and viscosity measurements. TGA was used to analyze the thermal properties of synthesized polymer. The extent of doping of the PANI salt was determined from UV-Vis spectra and TGA analysis. The activation energy for the degradation of the polymer was calculated with the help of TGA.

  4. Solution based synthesis of perovskite-type oxide films and powders

    International Nuclear Information System (INIS)

    McHale, J.M. Jr.

    1995-01-01

    Conventional solid state reactions are diffusion limited processes that require high temperatures and long reaction times to reach completion. In this work, several solution based methods were utilized to circumvent this diffusion limited reaction and achieve product formation at lower temperatures. The solution methods studied all have the common goal of trapping the homogeneity inherent in a solution and transferring this homogeneity to the solid state, thereby creating a solid atomic mixture of reactants. These atomic mixtures can yield solid state products through diffusionless mechanisms. The effectiveness of atomic mixtures in solid state synthesis was tested on three classes of materials, varying in complexity. A procedure was invented for obtaining the highly water soluble salt, titanyl nitrate, TiO(NO 3 ) 2 , in crystalline form, which allowed the production of titanate materials by freeze drying. The freeze drying procedures yielded phase pure, nanocrystalline BaTiO 3 and the complete SYNROC-B phase assemblage after ten minute heat treatments at 600 C and 1,100 C, respectively. Two novel methods were developed for the solution based synthesis of Ba 2 YCu 3 O 7-x and Bi 2 Sr 2 Ca 2 Cu 3 O 10 . Thin and thick films of Ba 2 YCu 3 O 7-x and Bi 2 Sr 2 Ca 2 Cu 3 O 10 were synthesized by an atmospheric pressure, chemical vapor deposition technique. Liquid ammonia solutions of metal nitrates were atomized with a stream of N 2 O and ignited with a hydrogen/oxygen torch. The resulting flame was used to coat a substrate with superconducting material. Bulk powders of Ba 2 YCu 3 O 7-x and Bi 2 Sr 2 Ca 2 Cu 3 O 10 were synthesized through a novel acetate glass method. The materials prepared were characterized by XRD, TEM, SEM, TGA, DTA, magnetic susceptibility and electrical resistivity measurements

  5. Synthesis and characterization of magnetite nanoparticles encapsulated in a bovine hemoglobin microgel

    Science.gov (United States)

    Mody, Puja J.

    This study shows the successful synthesis and characterization of a novel material that is composed of iron oxide particles within a protein gel. During the synthesis, bovine hemoglobin surrounds the forming Fe 3O4 nanoparticles, resulting in a biocompatible hydrogel, which has the potential to be used as a targeted drug delivery vehicle and as an MRI contrast agent. The structure, size, and thermal stability of these hydrogel complexes were analyzed using a range of techniques. Powder x-ray diffraction and infrared spectroscopy indicated the presence of Fe3O 4 and hemoglobin without significant interactions between particles in the solid state. Microscopy analysis determined the average size of these microgel complexes to be 4-9 mum2 in area (˜2-3 mum in diameter), and DSC analysis indicated that none of the microgels exhibited a denaturing or unfolding transition below 54°C regardless of the iron: hemoglobin ratio. Initial testing has been performed on the ability of these materials to act as magnetically activated drug delivery vehicles. Other pertinent tests (for magnetic properties and MRI applicability) are currently proceeding at external labs.

  6. Synthesis and characterization ligand tris-(2-thiosalicylamidoethyl)amine and its iron complexes and indium

    International Nuclear Information System (INIS)

    Guerra-Garcia, Pedro Pablo; Valle Bourrouet, Grettel

    2006-01-01

    The synthesis of coordination chemistry ligand tris-(2-tiosalicilamidoetil)amine is presented within the framework of study of tripod ligands, the corresponding complexes of iron and indium. Also, its spectroscopic characterization by proton magnetic resonance is showed; so the influence of ligand on a redox active metal and an inactive is compared. Electrochemical methods have been used. The presence of sulfur atoms modifies the redox and magnetic behavior of iron ion (III), as has been found in other similar ligands [es

  7. Synthesis and characterization of CdS/PVA nanocomposite films

    Science.gov (United States)

    Wang, Hongmei; Fang, Pengfei; Chen, Zhe; Wang, Shaojie

    2007-08-01

    A series CdS/PVA nanocomposite films with different amount of Cd salt have been prepared by means of the in situ synthesis method via the reaction of Cd 2+-dispersed poly vinyl-alcohol (PVA) with H 2S. The as-prepared films were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), ultraviolet-visible (UV-vis) absorption, photoluminescence (PL) spectra, Fourier transform infrared spectroscope (FTIR) and thermogravimetric analysis (TGA). The XRD results indicated the formation of CdS nanoparticles with hexagonal phase in the PVA matrix. The primary FTIR spectra of CdS/PVA nanocomposite in different processing stages have been discussed. The vibrational absorption peak of Cd sbnd S bond at 405 cm -1 was observed, which further testified the generation of CdS nanoparticles. The TGA results showed incorporation of CdS nanoparticles significantly altered the thermal properties of PVA matrix. The photoluminescence and UV-vis spectroscopy revealed that the CdS/PVA films showed quantum confinement effect.

  8. Synthesis and characterization of CdS/PVA nanocomposite films

    International Nuclear Information System (INIS)

    Wang Hongmei; Fang Pengfei; Chen Zhe; Wang Shaojie

    2007-01-01

    A series CdS/PVA nanocomposite films with different amount of Cd salt have been prepared by means of the in situ synthesis method via the reaction of Cd 2+ -dispersed poly vinyl-alcohol (PVA) with H 2 S. The as-prepared films were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), ultraviolet-visible (UV-vis) absorption, photoluminescence (PL) spectra, Fourier transform infrared spectroscope (FTIR) and thermogravimetric analysis (TGA). The XRD results indicated the formation of CdS nanoparticles with hexagonal phase in the PVA matrix. The primary FTIR spectra of CdS/PVA nanocomposite in different processing stages have been discussed. The vibrational absorption peak of Cd-S bond at 405 cm -1 was observed, which further testified the generation of CdS nanoparticles. The TGA results showed incorporation of CdS nanoparticles significantly altered the thermal properties of PVA matrix. The photoluminescence and UV-vis spectroscopy revealed that the CdS/PVA films showed quantum confinement effect

  9. Synthesis, spectroscopic characterization and pH dependent photometric and electrochemical fate of Schiff bases.

    Science.gov (United States)

    Rauf, Abdur; Shah, Afzal; Abbas, Saghir; Rana, Usman Ali; Khan, Salah Ud-Din; Ali, Saqib; Zia-Ur-Rehman; Qureshi, Rumana; Kraatz, Heinz-Bernhard; Belanger-Gariepy, Francine

    2015-03-05

    A new Schiff base, 1-((4-bromophenylimino) methyl) naphthalen-2-ol (BPIMN) was successfully synthesized and characterized by (1)H NMR, (13)C NMR, FTIR and UV-Vis spectroscopy. The results were compared with a structurally related Schiff base, 1-((4-chlorophenylimino) methyl) naphthalen-2-ol (CPIMN). The photometric and electrochemical fate of BPIMN and CPIMN was investigated in a wide pH range. The experimental findings were supported by quantum mechanical approach. The redox mechanistic pathways were proposed on the basis of results obtained electrochemical techniques. Moreover, pH dependent UV-Vis spectroscopy of BPIMN and CPIMN was carried out and the appearance of isosbestic points indicated the existence of these compounds in different tautomeric forms. Copyright © 2014 Elsevier B.V. All rights reserved.

  10. Nanoparticle synthesis of zinc peroxide: structural and morphological characterization for bactericidal applications

    International Nuclear Information System (INIS)

    Colonia, Roberto; Martinez, Vanessa C.; Solis, Jose L.; Gomez, Monica M.

    2013-01-01

    Zinc peroxide (ZnO 2 ) nanoparticles were synthesized by sol-gel technique. The chemicals used for the synthesis were zinc acetate di-hydrate (Zn(CH 3 COO) 2. 2H 2 O) and hydrogen peroxide (H 2 O 2 ) at 30 % in an aqueous solution with sonication. The structure of the ZnO 2 nanoparticles was characterized by X-ray diffraction. While the morphology and the cluster size were determined using scanning and transmission electron microscopy. For a preliminary evaluation of the bactericidal properties of the ZnO 2 , the material was exposed to Staphylococcus aureus, Escherichia coli y Bacillus subtili, and the nanoparticles presented good bactericidal properties. (author)

  11. Synthesis, Characterization, and Computational Modeling of N-(1-Ethoxyvinylpyridinium Triflates, an Unusual Class of Pyridinium Salts

    Directory of Open Access Journals (Sweden)

    Jonathan D. Shapiro

    2018-02-01

    Full Text Available N-Substituted pyridinium salts constitute one of the most valuable reagent classes in organic synthesis, due to their versatility and ease of use. Herein we report a preliminary synthesis and detailed structural analysis of several N-(1-ethoxyvinylpyridinium triflates, an unusual class of pyridinium salts with potentially broad use as a reagent in organic synthesis. Treatment of pyridines with trifluoromethane sulfonic acid and ethoxyacetylene generates stable, isolable adducts which have been extensively characterized, due to their novelty. Three-dimensional structural stability is perpetuated by an array of C–H•••O hydrogen bonds involving oxygen atoms from the –SO3 groups of the triflate anion, and hydrogen atoms from the aromatic ring and vinyl group of the pyridinium cation. Predictions from density functional theory calculations of the energy landscape for rotation about the exocyclic C–N bond of 2-chloro-1-(1-ethoxyvinylpyridine-1-ium trifluoromethanesulfonate (7 and 1-(1-ethoxyvinylpyridine-1-ium trifluoromethanesulfonate (16 are also reported. Notably, the predicted global energy minimum of 7 was nearly identical to that found within the crystal structure.

  12. Combinatorial Strategies for Synthesis and Characterization of Alloy Microstructures over Large Compositional Ranges.

    Science.gov (United States)

    Li, Yanglin; Jensen, Katharine E; Liu, Yanhui; Liu, Jingbei; Gong, Pan; Scanley, B Ellen; Broadbridge, Christine C; Schroers, Jan

    2016-10-10

    The exploration of new alloys with desirable properties has been a long-standing challenge in materials science because of the complex relationship between composition and microstructure. In this Research Article, we demonstrate a combinatorial strategy for the exploration of composition dependence of microstructure. This strategy is comprised of alloy library synthesis followed by high-throughput microstructure characterization. As an example, we synthesized a ternary Au-Cu-Si composition library containing over 1000 individual alloys using combinatorial sputtering. We subsequently melted and resolidified the entire library at controlled cooling rates. We used scanning optical microscopy and X-ray diffraction mapping to explore trends in phase formation and microstructural length scale with composition across the library. The integration of combinatorial synthesis with parallelizable analysis methods provides a efficient method for examining vast compositional ranges. The availability of microstructures from this vast composition space not only facilitates design of new alloys by controlling effects of composition on phase selection, phase sequence, length scale, and overall morphology, but also will be instrumental in understanding the complex process of microstructure formation in alloys.

  13. Enzymatic preparation and characterization of soybean lecithin-based emulsifiers

    OpenAIRE

    R. C. Reddy Jala; B. Chen; H. Li; Y. Zhang; L-Z Cheong; T. Yang; X. Xu

    2016-01-01

    Simple enzymatic methods were developed for the synthesis of lysolecithin, glycerolyzed lecithin and hydrolyzed lecithin. The products were characterized in terms of their acetone insoluble matter, hexane insoluble matter, moisture, phospholipid distribution and fatty acid composition. The HLB value ranges of different products with different acid values were detected. The efficiency of optimally hydrolyzed lecithin was examined at high calcium ion, low pH, and aqueous solutions and compared ...

  14. Synthesis and electrochemical characterization of nano-sized Ag_4Sn particles as anode material for lithium-ion batteries

    International Nuclear Information System (INIS)

    Schmuelling, Guido; Oehl, Nikolas; Fromm, Olga; Knipper, Martin; Kolny-Olesiak, Joanna; Plaggenborg, Thorsten; Parisi, Jürgen; Winter, Martin; Placke, Tobias

    2016-01-01

    For the first time, sub 10 nm sized intermetallic Ag_4Sn particles are prepared via an aqueous synthesis route in order to improve the electrochemical performance of pure Sn nanoparticles. High-resolution transmission electron microscopy, X-ray diffraction and thermogravimetric analysis are used to investigate the morphology, crystal structure and particle surface of the as prepared Ag_4Sn nanoparticles. In addition, galvanostatic cycling and cyclic voltammetry measurements are carried out to characterize the electrochemical behavior of the particles. Upon lithiation and de-lithiation a phase transformation from Ag_4Sn to Ag_3Sn is observed, which has not been reported so far. The intermetallic nanoparticle-based anode delivers a specific de-lithiation capacity of 460 mAhg"−"1 for more than 150 cycles.

  15. Synthesis and characterization of carbon cryogel microspheres from lignin-furfural mixtures for biodiesel production.

    Science.gov (United States)

    Zainol, Muzakkir Mohammad; Amin, Nor Aishah Saidina; Asmadi, Mohd

    2015-08-01

    The aim of this work was to study the potential of biofuel and biomass processing industry side-products as acid catalyst. The synthesis of carbon cryogel from lignin-furfural mixture, prepared via sol-gel polycondensation at 90°C for 0.5h, has been investigated for biodiesel production. The effect of lignin to furfural (L/F) ratios, lignin to water (L/W) ratios and acid concentration on carbon cryogel synthesis was studied. The carbon cryogels were characterized and tested for oleic acid conversion. The thermally stable amorphous spherical carbon cryogel has a large total surface area with high acidity. Experimental results revealed the optimum FAME yield and oleic acid conversion of 91.3wt.% and 98.1wt.%, respectively were attained at 65°C for 5h with 5wt.% catalyst loading and 20:1 methanol to oleic acid molar ratio. Therefore, carbon cryogel is highly potential for heterogeneous esterification of free fatty acid to biodiesel. Copyright © 2015 Elsevier Ltd. All rights reserved.

  16. 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.

  17. Synthesis and Characterization of Monometallic (Ag, Cu and Bimetallic Ag-Cu Particles for Antibacterial and Antifungal Applications

    Directory of Open Access Journals (Sweden)

    Marta Paszkiewicz

    2016-01-01

    Full Text Available In this paper, the experimental studies are concerned with the effect of the synthesis parameters on the formation of monometallic Ag and Cu nanoparticles (NPs. We consider the synthesis strategies verification for the bimetallic core-shell and alloy particles preparation. It was successfully obtained by chemical reduction method. The obtained colloidal solution is characterized by the transmission electron microscopy (TEM with energy-dispersive X-ray spectroscopy (EDX data, UV-Vis spectra, particle size distribution, and zeta potential. This work presents a comprehensive overview of experimental studies of the most stable colloidal solutions to impregnate fabrics that will exhibit a bactericidal and fungicidal activity against Candida albicans, Escherichia coli, and Staphylococcus aureus.

  18. Synthesis, Characterization and Biological Activities of Creatinine Amides and Creatinine Schiff Bases.

    Science.gov (United States)

    Mumtaz, Amara; Zahoor, Fareeha; Zaib, Sumera; Nawaz, Muhammad Azhar H; Saeed, Aamer; Waseem, Amir; Khan, Afsar; Hussain, Izhar; Iqbal, Jamshed

    2017-01-30

    In spite of substantial progress in scientific cognizance and medical technology, still infectious diseases are among the leading cause of morbidity and mortality. Creatinine and Schiff bases are well known for their diverse range of biological activities and thought to be emerging and useful therapeutic target for the treatment of several diseases. The present work was aimed to illustrate the influence of substitution of amides and Schiff bases on creatinine and their antimicrobial, antioxidant and anti-urease effectiveness was determined. Creatinine substituted amides (1-2) and creatinine Schiff bases (3-7) were synthesized and characterized by NMR and IR spectral data in combination with elemental analysis. All the compounds (1-7) were investigated on Jack bean urease for their urease inhibitory potential. Investigation of antimicrobial activity of the compounds was made by the agar dilution method. Moreover, 1,1-diphenyl-2- picrylhydrazyl (DPPH) method was used to determine their antioxidant potential. Molecular docking studies were also carried out to elucidate their relationship with the binding pockets of the enzyme. The compounds were found to be potent inhibitors of urease. The synthesized derivatives exhibited significant inhibition against Gram-positive and Gram-negative bacterial strains, as compared to standard, ciprofloxacin. Creatinine based derivatives exhibited potential antifungal activity when tested on infectious and pathogenic fungal strains. Similarly, most of the compounds exhibited good antioxidant activity. These derivatives may serve as a source of potential antioxidants and also help to retard microbial growth in food industry. Similarly, the studies provide a basis for further research to develop more potent urease inhibitory compounds of medicinal /agricultural interest. Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.

  19. Hydrothermal Synthesis and Characterization of a Metal-Organic Framework by Thermogravimetric Analysis, Powder X-Ray Diffraction, and Infrared Spectroscopy: An Integrative Inorganic Chemistry Experiment

    Science.gov (United States)

    Crane, Johanna L.; Anderson, Kelly E.; Conway, Samantha G.

    2015-01-01

    This advanced undergraduate laboratory experiment involves the synthesis and characterization of a metal-organic framework with microporous channels that are held intact via hydrogen bonding of the coordinated water molecules. The hydrothermal synthesis of Co[subscript 3](BTC)[subscript 2]·12H[subscript 2]O (BTC = 1,3,5-benzene tricarboxylic acid)…

  20. Synthesis and characterization of zeolite P using technical-grade materials

    CERN Document Server

    Aghabozorg, H R; Aghabozorg, H R; Sharif, M

    2001-01-01

    Research attempts on zeolites show structural and industrial importance of these inorganic compounds. In this regard, the synthesis of zeolites is of great importance, because their natural occurring counterparts are often impure. Zeolite Na-P with a silicon to aluminium ratio of one has a better ion exchange capacity than Na-A and can be used as a detergent builder. In this work, zeolite Na-P of high purity was successfully synthesized using commercial silica and alumina sources. parameters such as H sub 2 O:A1 sub 2 O sub 3 and SiO sub 2 :A1 sub 2 O sub 3 molar ratios and crystallization temperature and time were investigated. So that the optimum condition was obtained. X-ray powder diffraction, infrared, scanning electron microscopy and elemental analysis were utilized for the characterization of the product.

  1. Metal-organic frameworks: structure, properties, methods of synthesis and characterization

    International Nuclear Information System (INIS)

    Butova, V V; Soldatov, M A; Guda, A A; Lomachenko, K A; Lamberti, C

    2016-01-01

    This review deals with key methods of synthesis and characterization of metal-organic frameworks (MOFs). The modular structure affords a wide variety of MOFs with different active metal sites and organic linkers. These compounds represent a new stage of development of porous materials in which the pore size and the active site structure can be modified within wide limits. The set of experimental methods considered in this review is sufficient for studying the short-range and long-range order of the MOF crystal structure, determining the morphology of samples and elucidating the processes that occur at the active metal site in the course of chemical reactions. The interest in metal-organic frameworks results, first of all, from their numerous possible applications, ranging from gas separation and storage to chemical reactions within the pores. The bibliography includes 362 references

  2. Synthesis and characterization of NiO nanoparticles by Pechini method

    International Nuclear Information System (INIS)

    Nascimento, A.; Ribeiro, M.A.; Costa, A.C.F.M.; Gama, L.; Bernardi, M.I.B.

    2009-01-01

    In recent years, ultrafine magnetic particles of NiO have attracting the attention because of its unknown behavior, enormous scientific potential and technological application. Some of its more important properties are accented magnetic moments, double dynamic exchange, quantization of wave of spin and etc. In this context, this work has for objective to synthesize and to characterize nanoparticles of NiO for the Pechini method. The powder was analyzed by X-rays diffraction. The results of scanning electron microscopy, adsorption of nitrogen. The analysis of X-rays diffraction of the sample showed single-phase peaks of NiO, with crystallite size close to 38 nm. The surface area was 6.44 m 2 /g. The image from scanning electron microscopy shows soft homogeneous agglomerates. The Pechini synthesis was efficient in the production of powders of NiO nano metrics and single-phase. (author)

  3. Design, Synthesis, and Mechanistic Evaluation of Iron-Based Catalysis for Synthesis Gas Conversion to Fuels and Chemicals. Technical Progress Report

    International Nuclear Information System (INIS)

    Akio Ishikawa; Manuel Ojeda; Nan Yao; Enrique Iglesia

    2006-01-01

    This project extends previously discovered Fe-based catalysts to hydrogen-poor synthesis gas streams derived from coal and biomass sources. These catalysts have shown unprecedented Fischer-Tropsch synthesis rate, selectivity for feedstocks consisting of synthesis gas derived from methane. During the first reporting period, we certified a microreactor, installed required analytical equipment, and reproduced synthetic protocols and catalytic results previously reported. During the second reporting period, we prepared several Fe-based compositions for Fischer-Tropsch synthesis and tested the effects of product recycle under both subcritical and supercritical conditions. During the third and fourth reporting periods, we improved the catalysts preparation method, which led to Fe-based FT catalysts with the highest FTS reaction rates and selectivities so far reported, a finding that allowed their operation at lower temperatures and pressures with high selectivity to desired products (C 5+ , olefins). During this fifth reporting period, we have studied the effects of different promoters on catalytic performance, specifically how their sequence of addition dramatically influences the performance of these materials in the Fischer-Tropsch synthesis. The resulting procedures have been optimized to improve further upon the already unprecedented rates and C 5+ selectivities of the Fe-based catalysts that we have developed as part of this project. During this fifth reporting period, we have also continued our studies of optimal activation procedures, involving reduction and carburization of oxide precursors during the early stages of contact with synthesis gas. We have completed the analysis of the evolution of oxide, carbide, and metal phases of the active iron components during initial contact with synthesis gas using advanced synchrotron techniques based on X-ray absorption spectroscopy. We have confirmed that the Cu or Ru compensates for inhibitory effects of Zn, a surface

  4. Synthesis and characterization of recombinant abductin-based proteins.

    Science.gov (United States)

    Su, Renay S-C; Renner, Julie N; Liu, Julie C

    2013-12-09

    Recombinant proteins are promising tools for tissue engineering and drug delivery applications. Protein-based biomaterials have several advantages over natural and synthetic polymers, including precise control over amino acid composition and molecular weight, modular swapping of functional domains, and tunable mechanical and physical properties. In this work, we describe recombinant proteins based on abductin, an elastomeric protein that is found in the inner hinge of bivalves and functions as a coil spring to keep shells open. We illustrate, for the first time, the design, cloning, expression, and purification of a recombinant protein based on consensus abductin sequences derived from Argopecten irradians . The molecular weight of the protein was confirmed by mass spectrometry, and the protein was 94% pure. Circular dichroism studies showed that the dominant structures of abductin-based proteins were polyproline II helix structures in aqueous solution and type II β-turns in trifluoroethanol. Dynamic light scattering studies illustrated that the abductin-based proteins exhibit reversible upper critical solution temperature behavior and irreversible aggregation behavior at high temperatures. A LIVE/DEAD assay revealed that human umbilical vein endothelial cells had a viability of 98 ± 4% after being cultured for two days on the abductin-based protein. Initial cell spreading on the abductin-based protein was similar to that on bovine serum albumin. These studies thus demonstrate the potential of abductin-based proteins in tissue engineering and drug delivery applications due to the cytocompatibility and its response to temperature.

  5. Video Texture Synthesis Based on Flow-Like Stylization Painting

    Directory of Open Access Journals (Sweden)

    Qian Wenhua

    2014-01-01

    Full Text Available The paper presents an NP-video rendering system based on natural phenomena. It provides a simple nonphotorealistic video synthesis system in which user can obtain a flow-like stylization painting and infinite video scene. Firstly, based on anisotropic Kuwahara filtering in conjunction with line integral convolution, the phenomena video scene can be rendered to flow-like stylization painting. Secondly, the methods of frame division, patches synthesis, will be used to synthesize infinite playing video. According to selection examples from different natural video texture, our system can generate stylized of flow-like and infinite video scenes. The visual discontinuities between neighbor frames are decreased, and we also preserve feature and details of frames. This rendering system is easy and simple to implement.

  6. Synthesis and characterization of SiC based composite materials for immobilizing radioactive graphite

    Science.gov (United States)

    Wang, Qing; Teng, Yuancheng; Wu, Lang; Zhang, Kuibao; Zhao, Xiaofeng; Hu, Zhuang

    2018-06-01

    In order to immobilize high-level radioactive graphite, silicon carbide based composite materials{ (1-x) SiC· x MgAl2O4 (0.1 ≤ x≤0.4) } were fabricated by solid-state reaction at 1370 °C for 2 h in vacuum. Residual graphite and precipitated corundum were observed in the as-synthesized product, which attributed to the interface reaction of element silicon and magnesium compounds. To further understand the reasons for the presence of graphite and corundum, the effects of mole ratio of Si/C, MgAl2O4 content and non-stoichiometry of MgAl2O4 on the synthesis were investigated. To immobilize graphite better, residual graphite should be eliminated. The target product was obtained when the mole ratio of Si/C was 1.3:1, MgAl2O4 content was x = 0.2, and the mole ratio of Al to Mg in non-stoichiometric MgAl2O4 was 1.7:1. In addition, the interface reaction between magnesium compounds and silicon not graphite was displayed by conducting a series of comparative experiments. The key factor for the occurrence of interface reaction is that oxygen atom is transferred from magnesium compound to SiO gas. Infrared and Raman spectrum revealed the increased disorders of graphite after being synthesized.

  7. Synthesis, Transfer, and Characterization of Nanoscale 2-Dimensional Materials

    Science.gov (United States)

    2015-09-01

    Shi Y, Hamsen C, Jia X, Kim KK, Reina A, Hofmann M, Kong J. Synthesis of few-layer hexagonal boron nitride thin film by chemical vapor deposition...hexagonal boron nitride layers. Nano Letters. 2010;10(8):3209–3215. 12. Kim KK, Hsu A, Jia X, Kim SM, Shi Y, Hofmann M, Kong J. Synthesis of...microscopy. Physical Review B. 2009;80(15):155425. 33. Kim KK, Hsu A, Jia X, Kim SM, Shi Y, Hofmann M, Kong J. Synthesis of monolayer hexagonal boron

  8. Issues involved in a knowledge-based approach to procedure synthesis

    International Nuclear Information System (INIS)

    Hajek, B.K.; Khartabil, L.F.; Miller, D.W.

    1992-01-01

    Many knowledge-based systems (KBSs) have been built to assist human operators in managing nuclear power plant operating functions, such as monitoring, fault diagnosis, alarm filtering, and procedure management. For procedure management, KBSs have been built to display and track existing written procedures or to dynamically follow procedure execution by monitoring plant data and action execution and suggesting recovery steps. More recent works build KBSs able to synthesize procedures. This paper addresses and examines the main issues related to the implementation of on-line procedure synthesis using KBSs. A KBS for procedure synthesis can provide a more robust and effective procedural plan during accidents. Currently existing procedures for abnormal plant conditions, written as precompiled step sets based on the event and symptom approaches, are inherently not robust because anticipation of all potential plant states and associated plant responses is not possible. Thus, their failure recovery capability is limited to the precompiled set. Procedure synthesis has the potential to overcome these two problems because it does not require such precompilation of large sets of plant states and associated recovery procedures. Other benefits obtained from a complete procedure synthesis system are providing (a) a methodology for off-line procedure verification and (b) a methodology for the eventual automation of plant operations

  9. Nanoparticle-Assisted Diffusion Brazing of Metal Microchannel Arrays: Nanoparticle Synthesis, Deposition, and Characterization

    Science.gov (United States)

    Eluri, Ravindranadh T.

    sputtering a 1 microm thick layer of Cu before depositing a 5 nm thick film of AgNPs resulting in a lap shear strength of 45.3 +/- 0.2 MPa. In the middle section of this thesis, several techniques are investigated for the synthesis of sub 10 nm diameter nickel nanoparticles (NiNPs) to be used in the diffusion brazing of 316L stainless steel. The average NiNP size was varied from 9.2 nm to 3.9 nm based on the synthesis technique, solvent and reducing agent used. Conventional wet-chemical synthesis using NiCl2.6H2O in ethylene glycol (solvent) and N2 H4.H2O (reducing agent) resulted in the formation of 5.4 +/- 0.9 nm NiNPs. Continuous flow synthesis using a microchannel T-mixer (barrel diameter of 521microm) and a 10 second residence time of reactants in a bath temperature of 130ºC resulted in a particle size of with 5.3 +/- 1 nm. To make the synthesis safer and less energy intense, microwave heating was used along with less toxic Ni(CH3CO 2)2·4H2O (nickel salt), propylene glycol (solvent) and NaPH2O2 (reducing agent) yielding 3.9 +/- 0.8 nm diameter NiNPs. For the final section, nickel nanoparticles were synthesized using NiCl2.6H2O (nickel salt), de-ionized water (solvent), NaBH4 (co-reducing agent), N2H4.H 2O (reducing agent) and polyvinylpyrolidone (capping agent) yielding 4.2 +/- 0.6 nm NiNP. Several deposition techniques were investigated for controlling film thickness and uniformity in the diffusion brazing of 316L stainless steel (SS). Using in-house prepared NiNP and automated dispensing, a hermetic joint up to 70 psi (tested pressure) was obtained in 316L SS substrates under brazing conditions of 800ºC, 2 MPa and 30 min. Throughout the course of this thesis, techniques used for characterizing nanoparticles, films and joints included FT-IR, XRD, SEM, TEM, HRTEM, EDS, EPMA, DSC, mass spectrometry, and lap-shear testing.

  10. Synthesis and Characterization of Highly Intercalated Graphite Bisulfate

    OpenAIRE

    Salvatore, Marcella; Carotenuto, Gianfranco; De Nicola, Sergio; Camerlingo, Carlo; Ambrogi, Veronica; Carfagna, Cosimo

    2017-01-01

    Different chemical formulations for the synthesis of highly intercalated graphite bisulfate have been tested. In particular, nitric acid, potassium nitrate, potassium dichromate, potassium permanganate, sodium periodate, sodium chlorate, and hydrogen peroxide have been used in this synthesis scheme as the auxiliary reagent (oxidizing agent). In order to evaluate the presence of delamination, and pre-expansion phenomena, and the achieved intercalation degree in the prepared samples, the obtain...

  11. Synthesis and characterization of dioxouranium (VI) complexes of Schiff bases derived from isatin, isovanillin and o-vanillin

    International Nuclear Information System (INIS)

    Singh, Kavita; Agarwala, B.V.; Naganagowda, G.A.

    1996-01-01

    Three Schiff bases viz. isatin semicarbazone, isovanillin thiosemicarbazone, o-vanillin para-anisidine and their dioxouranium (VI) complexes have been synthesised and characterized by elemental analysis, IR and NMR spectral studies. (author). 19 refs., 1 tab

  12. Synthesis and characterization of carbon nano fibers for its application in the adsorption of toxic gases

    International Nuclear Information System (INIS)

    Juanico L, J.A.

    2004-01-01

    The production of carbon nano fibers (CNF's) by diverse techniques as the electric arc, laser ablation, or chemical deposition in vapor phase, among other, they have been so far used from final of the 90's. However, the synthesis method by discharge Glow arc of alternating current and high frequency developed by Pacheco and collaborators, is a once alternative for its obtaining. In the plasma Application Laboratory (LAP) of the National Institute of Nuclear Research (INlN) it was designed and manufactured a reactor of alternating current and high frequency that produces a Glow arc able to synthesize carbon nano fibers. Its were carried out nano fibers synthesis with different catalysts to different proportions and with distinct conditions of vacuum pressure and methane flow until obtaining the best nano fibers samples and for it, this nano structures were characterized by Scanning and Transmission Electron Microscopy, X-ray Diffraction, Raman spectrometry and EDS spectrometry. Once found the optimal conditions for the nano fibers production its were contaminated with NO 2 toxic gas and it was determined if they present adsorption, for it was used the thermal gravimetric analysis technique. This work is divided in three parts, in the first one, conformed by the chapters 1, at the 3, they are considered the foundations of the carbon nano fibers, their history, their characteristics, growth mechanisms, synthesis techniques, the thermal gravimetric analysis principles and the adsorption properties of the nano fibers. In the second part, consistent of the chapters 4 and 5, the methodology of synthesis and characterization of the nano fibers is provided. Finally, in third part its were carried out the activation energy calculation, the adsorption of the CNF's is analyzed and the conclusions are carried out. The present study evaluates the adsorption of environmental gas pollutants as the nitrogen oxides on carbon nano fibers at environmental or near conditions. Also

  13. Synthesis and characterization of a push-pull terpolymer based on anthracene, fluorene and benzothiadiazole

    Energy Technology Data Exchange (ETDEWEB)

    Floriano, Ana Carolina; Silveira, Daiana Santos; Cristovan, Fernando Henrique, E-mail: carolina.floriano@unifesp.br [Universidade Federal de Sao Paulo (UNIFESP), Sao Jose dos Campos, SP (Brazil); Rosa, Gabriel Marques; Liao, Luciano Morais [Universidade Federal de Goias (UFG), Goiania, GO (Brazil); Piovessan, Erick [Universidade Federal de Uberlandia (UFU), MG (Brazil)

    2016-07-01

    Full text: The development of organic optoelectronic devices with higher efficiency required new forms of polymers with strong donor-acceptor character (D-A), called a push-pull polymers. Most studies of organic polymers used in optoelectronic applications are centered on poly(3-hexylthiophene) with high regioregularity. However, there are other polymers synthesized with monomers that enables the possibility to adapt its electrical and optical properties. Polyfluorene derivatives show interesting chemical and physical properties due to a rigid planar biphenyl unit that are easily substituted at the remote C-9 position, improving the its processability in relation to polyfluorene, so it can be can be processed by spin-coating and many others deposition techniques. Fluorene derivatives copolymers prepared with anthracene unit improve electrochemical properties and present good photo and electroluminescence properties, due to an enhancement of the system conjugation. The benzothiadiazole, known by their environmental stability, planarity and electron-withdrawing nature, are a promising molecule in push−pull type semiconducting polymers. In this study proceed with the terpolymer synthesis containing 9,9-Dihexylfluorene and anthracene as pushing unit and benzothiadiazole as pushing unit. Also we synthesized the poly(9,9-dihexylfluorene)-co-(anthracene) and poly(9,9- dihexylfluorene)-co-(benzothiadiazole) copolymers. The polymers were synthesized using Suzuki coupling and characterized by FT-IR spectroscopy that shows the characteristic monomer bands and the polymer formation were confirmed by {sup 1}H-NMR. Polymerization yield of three polymers were about 50-70%. Polymers present good solubility in common organic solvent such as chloroform. Terpolymer UV-Vis spectra revealed broadband absorbance from 300 to 680nm and absorption maximum at 441 nm. Finally, the preliminary results indicate that the push-pull terpolymer is a promising broadband absorbing polymer for

  14. Synthesis and characterization of a push-pull terpolymer based on anthracene, fluorene and benzothiadiazole

    International Nuclear Information System (INIS)

    Floriano, Ana Carolina; Silveira, Daiana Santos; Cristovan, Fernando Henrique; Rosa, Gabriel Marques; Liao, Luciano Morais; Piovessan, Erick

    2016-01-01

    Full text: The development of organic optoelectronic devices with higher efficiency required new forms of polymers with strong donor-acceptor character (D-A), called a push-pull polymers. Most studies of organic polymers used in optoelectronic applications are centered on poly(3-hexylthiophene) with high regioregularity. However, there are other polymers synthesized with monomers that enables the possibility to adapt its electrical and optical properties. Polyfluorene derivatives show interesting chemical and physical properties due to a rigid planar biphenyl unit that are easily substituted at the remote C-9 position, improving the its processability in relation to polyfluorene, so it can be can be processed by spin-coating and many others deposition techniques. Fluorene derivatives copolymers prepared with anthracene unit improve electrochemical properties and present good photo and electroluminescence properties, due to an enhancement of the system conjugation. The benzothiadiazole, known by their environmental stability, planarity and electron-withdrawing nature, are a promising molecule in push−pull type semiconducting polymers. In this study proceed with the terpolymer synthesis containing 9,9-Dihexylfluorene and anthracene as pushing unit and benzothiadiazole as pushing unit. Also we synthesized the poly(9,9-dihexylfluorene)-co-(anthracene) and poly(9,9- dihexylfluorene)-co-(benzothiadiazole) copolymers. The polymers were synthesized using Suzuki coupling and characterized by FT-IR spectroscopy that shows the characteristic monomer bands and the polymer formation were confirmed by 1 H-NMR. Polymerization yield of three polymers were about 50-70%. Polymers present good solubility in common organic solvent such as chloroform. Terpolymer UV-Vis spectra revealed broadband absorbance from 300 to 680nm and absorption maximum at 441 nm. Finally, the preliminary results indicate that the push-pull terpolymer is a promising broadband absorbing polymer for

  15. Synthesis and characterization of CuO flower-nanostructure processing by a domestic hydrothermal microwave

    International Nuclear Information System (INIS)

    Volanti, D.P.; Keyson, D.; Cavalcante, L.S.; Simoes, A.Z.; Joya, M.R.; Longo, E.; Varela, J.A.; Pizani, P.S.; Souza, A.G.

    2008-01-01

    The synthesis and characterization of CuO flower-nanostructure processed in domestic hydrothermal microwave oven was presented. Phase analysis was carried out using X-ray diffraction (XRD) and micro-Raman scattering (MRS) and the results confirmed the CuO flower-nanostructure as a single-phase. The field-emission scanning electron microscopy (FEG-SEM) was used to estimate the average spheres diameter while transmission electron microscope (TEM) to observe the thorn of the flower-nanostructures. The mechanism of CuO flower-nanostructures formation is proposed and explained

  16. Synthesis and characterization of CuO flower-nanostructure processing by a domestic hydrothermal microwave

    Energy Technology Data Exchange (ETDEWEB)

    Volanti, D.P. [Laboratorio Interdisciplinar em Ceramica, Departamento de Fisico-Quimica, Instituto de Quimica, Universidade Estadual Paulista, P.O. Box 355, 14801-907 Araraquara, SP (Brazil); Keyson, D. [Laboratorio de Ensino de Ciencias e Laboratorio de Combustiveis e Materiais, Departamento de Quimica, Universidade Federal da Paraiba, 58051-900 Joao Pessoa, PB (Brazil); Cavalcante, L.S. [Laboratorio Interdisciplinar de Eletroquimica e Ceramica, Departamento de Quimica, Universidade Federal de Sao Carlos, P.O. Box 676, 13565-905 Sao Carlos, SP (Brazil)], E-mail: laeciosc@bol.com.br; Simoes, A.Z. [Laboratorio Interdisciplinar em Ceramica, Departamento de Fisico-Quimica, Instituto de Quimica, Universidade Estadual Paulista, P.O. Box 355, 14801-907 Araraquara, SP (Brazil); Joya, M.R. [Departamento de Fisica, Universidade Federal de Sao Carlos, P.O. Box 676, 13565-905 Sao Carlos, SP (Brazil); Longo, E.; Varela, J.A. [Laboratorio Interdisciplinar em Ceramica, Departamento de Fisico-Quimica, Instituto de Quimica, Universidade Estadual Paulista, P.O. Box 355, 14801-907 Araraquara, SP (Brazil); Pizani, P.S. [Departamento de Fisica, Universidade Federal de Sao Carlos, P.O. Box 676, 13565-905 Sao Carlos, SP (Brazil); Souza, A.G. [Laboratorio de Ensino de Ciencias e Laboratorio de Combustiveis e Materiais, Departamento de Quimica, Universidade Federal da Paraiba, 58051-900 Joao Pessoa, PB (Brazil)

    2008-07-14

    The synthesis and characterization of CuO flower-nanostructure processed in domestic hydrothermal microwave oven was presented. Phase analysis was carried out using X-ray diffraction (XRD) and micro-Raman scattering (MRS) and the results confirmed the CuO flower-nanostructure as a single-phase. The field-emission scanning electron microscopy (FEG-SEM) was used to estimate the average spheres diameter while transmission electron microscope (TEM) to observe the thorn of the flower-nanostructures. The mechanism of CuO flower-nanostructures formation is proposed and explained.

  17. Auto-combustion Synthesis, Characterization and Photovoltaic

    African Journals Online (AJOL)

    NICOLAAS

    Ag-NiTiO3, sol-gel method, semiconductor, photovoltaic, doping. 1. Introduction ... convenient for synthesis of pure mixed metal oxides nanoparticles. Furthermore .... current density voltage (I-V) curve for Ag-NiTiO3 was carried out under the ...

  18. [Synthesis and characterization of polylactide-based thermosetting polyurethanes with shape memory properties].

    Science.gov (United States)

    Shi, Shuo; Gu, Lin; Yang, Yihu; Yu, Haibin; Chen, Rui; Xiao, Xianglian; Qiu, Jun

    2016-06-25

    A series of bio-based thermosetting polyurethanes (Bio-PUs) were synthesized by the crosslinking reaction of polylactide and its copolymers diols with hexamethylene diisocyanate (HDI) trimer. The obtained Bio-PUs were characterized by Fourier Transform Infrared Spectroscopy (FTIR), Differential Scanning Calorimetry (DSC), Thermal Gravimetric Analysis (TGA), universal tensile testing machine and cytotoxicity test. Results indicate that the PLA copolymer (P(LA-co-CL)) diols reduced the glass transition temperature (Tg) of Bio-PUs and improved their thermal stability, compared with PLA diols. The Bio-PUs synthesized from P (LA-co-CL) diols exhibit better mechanical performance and shape memory properties. Especially, Young modulus and elongation at break of the obtained Bio-PUs were 277.7 MPa and 230% respectively; the shape recovery time of the obtained Bio-PUs at body temperature was only 93 s. Furthermore, alamar blue assay results showed that the obtained Bio-PUs had no cell toxicity.

  19. Synthesis, Characterization and in Vitro Antibacterial Activities of CdO Nanoparticle and Nano-sheet Mixed-ligand of Cadmium(ІІ Complex

    Directory of Open Access Journals (Sweden)

    Zohreh Rashidi Ranjbar

    2016-07-01

    Full Text Available Here, we report the synthesis of a Schiff-base mixed-ligand complex of cadmium(ІІ in bulk and nano-scales via the precipitation and sonochemical methods, respectively. The complex formula is [Cd(3-bpdh(3-bpdbCl2]n (1, where the ligands are 3-bpdh = 2,5-bis(3-pyridyl-3,4-diaza-2,4-hexadiene and 3-bpdb = 1,4-bis(3-pyridyl-2,3-diaza-1,3-butadiene. The structure of mixed-ligand complex (1 was characterized by IR, 1H NMR and elemental analyses. Cadmium(ІІ oxide nanoparticles were prepared by direct thermolysis from nanosheet of complex (1. The cadmium(ІІ oxide structure was characterized by X-ray Diffraction (XRD and Energy Dispersive X-ray  analyses (EDAX. Size, morphology and structural dispersion of all obtained nanostructures were characterized by Scanning Electron Microscopy (SEM. The Schiff-base ligands, bulk and nano-scales of complex (1 and cadmium(ІІ oxide nanoparticles were analyzed for antibacterial activities against Bacillus alvei (bacteria causing the honey bee European foulbrood disease. The Minimum Inhibitory Concentrations (MIC has been shown moderate antibacterial activities compared with some other standard drugs. Known antibiotics like penicillin and SXT (Trimethoprim/sulfamethoxazole were used as positive control.

  20. Synthesis and X-ray crystal structure of the first tetrathiafulvalene-based acceptor-donor-acceptor sandwich

    DEFF Research Database (Denmark)

    Simonsen, Klaus B.; Thorup, Niels; Cava, Michael P.

    1998-01-01

    The synthesis and characterization of a bis-macrocyclic A-D-A sandwich produced in a simple one-pot reaction is reported. Only one acceptor unit participates in charge-transfer interactions with the TTF unit in the solid state....

  1. Green synthesis of novel quinoline based imidazole derivatives and evaluation of their antimicrobial activity

    Directory of Open Access Journals (Sweden)

    N.C. Desai

    2014-12-01

    Full Text Available We have described the conventional and microwave method for the synthesis of N-(4-((2-chloroquinolin-3-ylmethylene-5-oxo-2-phenyl-4,5-dihydro-1H-imidazol-1-yl(arylamides 3a–l. It is observed that the solvent-free microwave thermolysis is a convenient, rapid, high-yielding, and environmental friendly protocol for the synthesis of quinoline based imidazole derivatives when compared with conventional reaction in a solution phase. Antimicrobial activity of the newly synthesized compounds is screened in vitro on the following microbial cultures: Escherichia coli (MTCC 443, Pseudomonas aeruginosa (MTCC 1688, Staphylococcus aureus (MTCC 96, Streptococcus pyogenes (MTCC 442, Candida albicans (MTCC 227, Aspergillus niger (MTCC 282, Aspergillus clavatus (MTCC 1323. All the synthesized bio-active molecules are tested for their in vitro antimicrobial activity by bioassay namely serial broth dilution. Among these compounds 3c, 3d, 3f, 3h and 3j show significant potency against different microbial strains. All the compounds have been characterized by IR, 1H NMR, 13C NMR and mass spectral data. On the basis of statistical analysis, it is observed that these compounds give significant co-relation.

  2. Solid-phase synthesis and structural characterization of highly substituted hydroxyproline-based 2,5-diketopiperazines

    DEFF Research Database (Denmark)

    Bianco; Sonksen; Roepstorff

    2000-01-01

    . The synthesis procedures were conceived to enable a sequence of Hyp alkylation, Hyp N-acylation, cyclization, and amide bond alkylation. Up to three different centers of molecular diversity were introduced around the DKP scaffold. Highly functionalized bicyclic compounds were obtained in good yield and purity...... with multidimensional NMR experiments. The described reaction pathways can be applied to the identification of heterocyclic molecule inhibitors to diverse enzyme targets....

  3. Synthesis and thermal characterization of xylan-graft-polyacrylonitrile.

    Science.gov (United States)

    Ünlü, Cüneyt H; Öztekin, N Simge; Atıcı, Oya Galioğlu

    2012-10-01

    In this study emulsion polymerization of acrylonitrile using xylan from agricultural waste material (corn cob) and cerium ammonium nitrate was investigated in terms of catalyst acid. Stock ceric solutions were prepared using either nitric or perchloric acid as catalyst. Optimum conditions were determined using different parameters such as reaction time, temperature, and component concentrations. Nitric acid catalyzed reactions resulted in maximum conversion ratio (96%) at 50°C, 1 h where ceric ion, acrylonitrile, xylan, and catalyst concentrations were 21.7 mmol l(-1), 0.5 mol l(-1), 0.2% (w/v), and 0.1 mol l(-1), respectively. However, 83% conversion was obtained with perchloric acid catalysis at 27 °C, 1 h where concentrations were 5.4 mmol l(-1), 0.8 mol l(-1), 0.5% (w/v), and 0.2 mol l(-1), respectively. Copolymer synthesis using perchloric acid was realized at milder conditions than using nitric acid. Thermal analyses of obtained polymers were conducted to characterize copolymers. Results showed that calculated activation energy, maximum degradation temperature, and heat of thermal decomposition changed relying mainly on molecular weight. Copyright © 2012 Elsevier Ltd. All rights reserved.

  4. Biomimetic synthesis and characterization of semiconducting hybrid

    Indian Academy of Sciences (India)

    Triple hybrid materials based on polyaniline-polyethylene glycol and cadmium sulphide have been prepared by the duffusion–limited biomimetic route and characterized by a number of spectroscopic, XRD, SEM, thermal and electrical measurements. These hybrid materials have been prepared by controlled precipitation of ...

  5. New Titanium-Based Catalysts for the Synthesis of Poly(ethylene terephthalate)

    International Nuclear Information System (INIS)

    Yang, Youngkeun; Yoon, Seungwoong; Hwang, Yongtaek; Song, Bogeun

    2012-01-01

    Poly(ethylene terephthalate) (PET) is a polymer with relatively low cost and high performance, which is widely used in various applications such as bottles, textile fibers, films and engineering plastics for automobiles and electric industries. Commercial catalysts used for synthesis of PET are in general antimony (Sb) compounds. Antimony(III) oxide, antimony(III) acetate and antimony(III) glycolate are used as a catalyst in 95% of PET manufacturing industries worldwide. The few organoantimony compounds that have been identified in environmental and biological samples are all in the form of methylated Sb-species. The Sb trace element is extremely toxic to mammals, and interferes with embryonic and fetal development, also, carcinogenic to humans. In addition to being found in drinking water, food packaging and soft-drink bottles. According to the World Health Organization (WHO), Sb species concentration lower than 20 ppb are acceptable for drinking water. According to a recent study, in 14 brands of bottled water from Canada, Sb concentrations increased on average 19% during 6 months storage at room temperature, but 48 brands of water from 11 European countries increased on average 90% under identical conditions. Therefore, a very important challenge for polyester catalysis is to come-up with a new Sb-free catalysts with low environmental impact. Intensive efforts have been made to find other stable and more environmental friendly non-antimony catalysts, such as those based on titanium. Titanium-based catalysts have been known for many years and actually are used for polybutylene terephthalate (PBT) and polypropylene terephthalate (PPT) production, however, polycondensation (PC) of PET manufacture is not well studied in literature. To date, only few esterification processes have been applied for the synthesis of PET by titanium catalysts. Herein, we report an efficient synthesis characterization and polymerization of PET for a series of new nontoxic organotitanium

  6. Hydrothermal synthesis of a photovoltaic material based on CuIn0.5Ga0.5Se2

    Science.gov (United States)

    Castellanos Báez, Y. T.; Fuquen Peña, D. A.; Gómez-Cuaspud, J. A.; Vera-López, E.; Pineda-Triana, Y.

    2017-12-01

    The present work report, the synthesis and characterization of the CuIn0.5Ga0.5Se2 system (abbreviated CIGS), by the implementation of a hydrothermal route, in order to obtain a solid with appropriate properties in terms of surface, morphological and texture properties for potential applications in the design of photovoltaic cells. The synthesis was carried out using the corresponding stoichiometric quantities (Cu:In:Ga:Se 1:0.5:0.5:2), which were mixed in a Teflon vessel under stirring conditions. The homogeneous solution was treated in a steel autoclave at 300°C for 72 hours at the end of which the resulting material was characterized by X-Ray Diffraction (XRD) and Rietveld refinement. The results of the structural characterization allowed to confirm the obtaining of a chalcopyrite type structure, with a I-42 d (122) structure and cell parameters a=0.570, b=0.570, c=1.140nm, α=90, β=90, γ=90° oriented along (1 0 4) facet, detecting the presence of a secondary phases, related with CuInSe and CuIn metallic selenides, derived from synthesis process. The structural refinement allowing to validate the obtaining of a nanometric crystalline material (10-20nm) for potential applications in field of photovoltaic technology.

  7. Ultrafast Hydro-Micromechanical Synthesis of Calcium Zincate: Structural and Morphological Characterizations

    Directory of Open Access Journals (Sweden)

    Vincent Caldeira

    2017-01-01

    Full Text Available Calcium zincate is a compound with a large panel of application: mainly known as an advantageous replacement of zinc oxide in negative electrodes for air-zinc or nickel-zinc batteries, it is also used as precursor catalyst in biodiesel synthesis and as antifungal compound for the protection of limestone monuments. However, its synthesis is not optimized yet. In this study, it was elaborated using an ultrafast synthesis protocol: Hydro-Micromechanical Synthesis. Two other synthesis methods, Hydrochemical Synthesis and Hydrothermal Synthesis, were used for comparison. In all cases, the as-synthesized samples were analyzed by X-ray diffraction, scanning electron microscopy, and LASER diffraction particle size analysis. Rietveld method was used to refine various structural parameters and obtain an average crystallite size, on a Hydro-Micromechanical submicronic sample. X-ray single crystal structure determination was performed on a crystal obtained by Hydrochemical Synthesis. It has been shown that regardless of the synthesis protocol, the prepared samples always crystallize in the same crystal lattice, with P21/c space group and only differ from their macroscopic textural parameters. Nevertheless, only the Hydro-Micromechanical method is industrially scalable and enables a precise control of the textural parameters of the obtained calcium zincate.

  8. Synthesis of Fe–Ni bimetallic nanoparticles from pixel target ablation: plume dynamics and surface characterization

    International Nuclear Information System (INIS)

    Niu Xiaoxu; Murray, Paul T.; Sarangan, Andrew

    2012-01-01

    A novel Fe–Ni bimetallic nanoparticle synthesis technique, denoted pixel target ablation, is reported. The technique entails ablating a thin film target consisting of patterned Fe and Ni pixels with a selected ratio using a KrF excimer laser. The laser energy breaks a known amount of target materials into metal atoms, which then form nanoparticles by recombination in the gas phase. Due to the nature of thin-film ablation, splashing of large particles was eliminated with the added benefit of minimizing nanoparticle agglomeration. Plume dynamics and surface characterizations were carried out to exploit the formation of Fe–Ni nanoparticles more fully. The composition was readily controlled by varying the initial relative amount of Fe and Ni target pixels. Synthesis of multi-element nanoparticles by pixel target ablation should be possible with any element combination that can be prepared as a thin-film target.

  9. Synthesis and characterization of hexagonal nano-sized nickel selenide by simple hydrothermal method assisted by CTAB

    Energy Technology Data Exchange (ETDEWEB)

    Sobhani, Azam [Department of Inorganic Chemistry, Faculty of Chemistry, University of Kashan, Kashan, P.O. Box 87317-51167 (Iran, Islamic Republic of); Davar, Fatemeh [Institute of Nano Science and Nano Technology, University of Kashan, Kashan, P.O. Box 87317-51167 (Iran, Islamic Republic of); Salavati-Niasari, Masoud, E-mail: salavati@kashanu.ac.ir [Department of Inorganic Chemistry, Faculty of Chemistry, University of Kashan, Kashan, P.O. Box 87317-51167 (Iran, Islamic Republic of); Institute of Nano Science and Nano Technology, University of Kashan, Kashan, P.O. Box 87317-51167 (Iran, Islamic Republic of)

    2011-07-01

    Nano-sized nickel selenide powders have been successfully synthesized via an improved hydrothermal route based on the reaction between NiCl{sub 2}.6H{sub 2}O, SeCl{sub 4} and hydrazine (N{sub 2}H{sub 4}.H{sub 2}O) in water, in present of cetyltrimethyl ammonium bromide (CTAB) as surfactant, at various conditions. The products were characterized by X-ray diffraction, scanning electron microscopy, transmission electron microscopy and X-ray energy dispersive spectroscopy analysis. Effects of temperature, reaction time and reductant agent on the morphology, the particle sizes and the phase of the final products have been investigated. It was found that the phase and morphology of the products could be greatly influenced by these parameters. The synthesis procedure is simple and uses less toxic reagents than the previously reported methods. Photoluminescence (PL) was used to study the optical properties of NiSe samples.

  10. Conductive polymer-based nanoparticles for laser-mediated photothermal ablation of cancer: synthesis, characterization, and in vitro evaluation

    Directory of Open Access Journals (Sweden)

    Cantu T

    2017-01-01

    Full Text Available Travis Cantu,1 Kyle Walsh,2 Varun P Pattani,3 Austin J Moy,3 James W Tunnell,3 Jennifer A Irvin,1,2 Tania Betancourt1,2 1Materials Science, Engineering, and Commercialization Program, Texas State University, San Marcos, TX, USA; 2Department of Chemistry and Biochemistry, Texas State University, San Marcos, TX, USA; 3Department of Biomedical Engineering, The University of Texas at Austin, Austin, TX, USA Abstract: Laser-mediated photothermal ablation of cancer cells aided by photothermal agents is a promising strategy for localized, externally controlled cancer treatment. We report the synthesis, characterization, and in vitro evaluation of conductive polymeric nanoparticles (CPNPs of poly(diethyl-4,4'-{[2,5-bis(2,3-dihydrothieno[3,4-b][1,4]dioxin-5-yl-1,4-phenylene]bis(oxy}dibutanoate (P1 and poly(3,4-ethylenedioxythiophene (PEDOT stabilized with 4-dodecylbenzenesulfonic acid and poly(4-styrenesulfonic acid-co-maleic acid as photothermal ablation agents. The nanoparticles were prepared by oxidative-emulsion polymerization, yielding stable aqueous suspensions of spherical particles of <100 nm diameter as determined by dynamic light scattering and electron microscopy. Both types of nanoparticles show strong absorption of light in the near infrared region, with absorption peaks at 780 nm for P1 and 750 nm for PEDOT, as well as high photothermal conversion efficiencies (~50%, that is higher than commercially available gold-based photothermal ablation agents. The nanoparticles show significant photostability as determined by their ability to achieve consistent temperatures and to maintain their morphology upon repeated cycles of laser irradiation. In vitro studies in MDA-MB-231 breast cancer cells demonstrate the cytocompatibility of the CPNPs and their ability to mediate complete cancer cell ablation upon irradiation with an 808-nm laser, thereby establishing the potential of these systems as agents for laser-induced photothermal therapy. Keywords

  11. Efficient synthesis and physicochemical characterization of natural danshensu, its S isomer and intermediates thereof

    Science.gov (United States)

    Sidoryk, Katarzyna; Filip, Katarzyna; Cmoch, Piotr; Łaszcz, Marta; Cybulski, Marcin

    2018-02-01

    The synthesis and molecular structure details of R- 3,4-dihydroxyphenyl lactic acid (danshensu) and related compounds, i.e. S isomer and the key intermediates have been described. Danshensu is an important water soluble phenolic acid of Salvia miltiorrhiza herb (danshen or red sag) with numerous applications in traditional Chinese medicine (TCM). Our synthetic approach was based on the Knoevenagel condensation of the protected 3,4-dihydroxybenzaldehyd and Meldrum acid derivative, followed by asymmetric Sharples dihydroxylation, reductive mono dehydroxylation and final deprotection. All compounds were characterized by various spectroscopic techniques: 1H-, 13C- magnetic resonance (NMR); Fourier-transformed infrared (FTIR); Raman, HR mass spectroscopy. For the determination of compound optical purities original HPLC methods were developed which allowed for the efficient resolution of danshensu R and S enantiomers as well as its intermediate enantiomers, using commercially available chiral stationary phases. Furthermore, in order to better understand danshensu specificity as a potential API in drug formulation, the physicochemical properties of the compounds were studied by thermal analysis, including differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA).

  12. Python based high-level synthesis compiler

    Science.gov (United States)

    Cieszewski, Radosław; Pozniak, Krzysztof; Romaniuk, Ryszard

    2014-11-01

    This paper presents a python based High-Level synthesis (HLS) compiler. The compiler interprets an algorithmic description of a desired behavior written in Python and map it to VHDL. FPGA combines many benefits of both software and ASIC implementations. Like software, the mapped circuit is flexible, and can be reconfigured over the lifetime of the system. FPGAs therefore have the potential to achieve far greater performance than software as a result of bypassing the fetch-decode-execute operations of traditional processors, and possibly exploiting a greater level of parallelism. Creating parallel programs implemented in FPGAs is not trivial. This article describes design, implementation and first results of created Python based compiler.

  13. Synthesis of polyetherimide / halloysite nanotubes (PEI/HNTs) based nanocomposite membrane towards hydrogen storage

    Science.gov (United States)

    Muthu, R. Naresh; Rajashabala, S.; Kannan, R.

    2018-04-01

    Even though hydrogen is considered as green and clean energy sources of future, the blooming of hydrogen economy mainly relies on the development of safe and efficient hydrogen storage medium. The present work is aimed at the synthesis and characterization of polyetherimide/acid treated halloysite nanotubes (PEI/A-HNTs) nanocomposite membranes for solid state hydrogen storage medium, where phase inversion technique was adopted for the synthesis of nanocomposite membrane. The synthesized PEI/A-HNTs nanocomposite membranes were characterized by XRD, FTIR, SEM, EDX, CHNS elemental analysis and TGA. Hydrogenation studies were performed using a Sievert's-like hydrogenation setup. The important conclusions arrived from the present work are the PEI/A-HNTs nanocomposite membranes have better performance with a maximum hydrogen storage capacity of 3.6 wt% at 100 °C than pristine PEI. The adsorbed hydrogen possesses the average binding energy of 0.31 eV which lies in the recommended range of US- DOE 2020 targets. Hence it is expected that the PEI/A-HNTs nanocomposite membranes may have bright extent in the scenario of hydrogen fuel cell applications.

  14. Synthesis, characterization and catalytic application of silica supported tin oxide nanoparticles for synthesis of 2,4,5-tri and 1,2,4,5-tetrasubstituted imidazoles under solvent-free conditions

    Directory of Open Access Journals (Sweden)

    Ashok V. Borhade

    2017-02-01

    Full Text Available Highly efficient and eco-friendly, one pot synthesis of 1,2,4,5-tetra substituted imidazoles and 2,4,5-trisubstituted imidazoles was reported under solvent free conditions using nanocrystalline silica supported tin oxide (SiO2:SnO2 as a catalyst with excellent yield. The present methodology offers several advantages such as mild reaction conditions, short reaction time, good yield, high purity of product, recyclable catalyst without a noticeable decrease in catalytic activity and can be used for large scale synthesis. The synthesized SiO2:SnO2 nanocrystalline catalyst was characterized by XRD, BET surface area and TEM techniques.

  15. Synthesis, characterization and TG-DSC study of cadmium halides adducts with caffeine

    Energy Technology Data Exchange (ETDEWEB)

    Farias, Robson F. de; Silva, Ademir O. da; Silva, Umberto G. da

    2003-11-28

    The synthesis, characterization and TG-DSC study of the compounds CdX{sub 2}{center_dot}ncaff, for which X: Cl, Br and I; n=1 and 2 and caff: caffeine is reported. It is verified that caffeine is coordinated through more than one coordination site, despite the fact that the nitrogen of the imidazole ring is the main coordination site. The following thermal stability trend is observed: Cl>Br>I and monoadducts are more stable than bisadducts. The thermal degradation (td) enthalpies have the values (kJ mol{sup -1}): 58.2 and 71.5; 74.9 and 91.4; 31.1 and 47.5 for Cl, Br and I mono and bisadducts, respectively.

  16. Synthesis of Siloxanes Directly from Amorphous Silica

    International Nuclear Information System (INIS)

    Myint Sandar Win

    2011-12-01

    A direct synthesis of oligomeric-siloxanes from amorphous silica has been achieved. The compound prepared was caedonal-siloxane. Cardonal is a mono hydroxyphenolic compound with a bulky group in the meta position. It was derived as a by-product from the renewable resources cashew nut shell liquid (CNSL). In the synthesis, one pot synthesis was carried out by using ethylene glycol (EG) as solvent. In the reaction ethylene glycol served as a primary precursor chelating ligand in the synthesised product. The one pot synthesis was enhanced by the strong base, triethylenetetramine (TETA) which served as the promoter catalyst. In the synthesis, optimal conditions were established on the basic of the yield percent of organo-siloxane compounds with respect to the variation of the weight fraction of TETA and to the variation of reaction time. Experimental runs were carried out at (ca 210 2c) which was nearly above the boiling point of the solvent. The substituted organo-silicon compounds obtained were characterized by FT- ir, Thermal analysis, XRD and SEM.

  17. Niobium-Doped Hydroxyapatite Bioceramics: Synthesis, Characterization and In Vitro Cytocompatibility

    Directory of Open Access Journals (Sweden)

    Nádia S. V. Capanema

    2015-07-01

    Full Text Available Doping calcium phosphates with ionic species can play an important role in biological responses promoting alkaline phosphatase activity, and, therefore inducing the generation of new bone. Thus, in this study, the synthesis of niobium-doped hydroxyapatite (Nb-HA nanosize particles obtained by the precipitation process in aqueous media followed by thermal treatment is presented. The bioceramics were extensively characterized by X-ray diffraction, wavelength dispersive X-ray fluorescence spectrometry, Fourier transform infrared spectroscopy, scanning electron microscopy/energy dispersive X-ray spectroscopy analysis, transmission electron microscopy, atomic force microscopy and thermal analysis regarding their chemical composition, structure and morphology. The results showed that the precipitate dried at 110 °C was composed of amorphous calcium phosphate and HA, with polidisperse particles ranging from micro to nano dimensions. After the thermal treatment at 900 °C, the bioceramic system evolved predominantly to HA crystalline phase, with evident features of particle sintering and reduction of surface area. Moreover, the addition of 10 mol% of niobium salt precursor during the synthesis indicated the complete incorporation of the Nb(V species in the HA crystals with detectable changes in the original lattice parameters. Furthermore, the incorporation of Nb ions caused a significant refinement on the average particle size of HA. Finally, the preliminary cytocompatibility response of the biomaterials was accessed by human osteoblast cell culture using MTT and resazurin assays, which demonstrated no cytotoxicity of the Nb-alloyed hydroxyapatite. Thus, these findings seem promising for developing innovative Nb-doped calcium phosphates as artificial biomaterials for potential use in bone replacements and repair.

  18. Rule-Based Storytelling Text-to-Speech (TTS Synthesis

    Directory of Open Access Journals (Sweden)

    Ramli Izzad

    2016-01-01

    Full Text Available In recent years, various real life applications such as talking books, gadgets and humanoid robots have drawn the attention to pursue research in the area of expressive speech synthesis. Speech synthesis is widely used in various applications. However, there is a growing need for an expressive speech synthesis especially for communication and robotic. In this paper, global and local rule are developed to convert neutral to storytelling style speech for the Malay language. In order to generate rules, modification of prosodic parameters such as pitch, intensity, duration, tempo and pauses are considered. Modification of prosodic parameters is examined by performing prosodic analysis on a story collected from an experienced female and male storyteller. The global and local rule is applied in sentence level and synthesized using HNM. Subjective tests are conducted to evaluate the synthesized storytelling speech quality of both rules based on naturalness, intelligibility, and similarity to the original storytelling speech. The results showed that global rule give a better result than local rule

  19. V2O5 xerogel-poly(ethylene oxide) hybrid material: Synthesis, characterization, and electrochemical properties

    International Nuclear Information System (INIS)

    Guerra, Elidia M.; Ciuffi, Katia J.; Oliveira, Herenilton P.

    2006-01-01

    In this work, we report the synthesis, characterization, and electrochemical properties of vanadium pentoxide xerogel-poly(ethylene oxide) (PEO) hybrid materials obtained by varying the average molecular weight of the organic component as well as the components' ratios. The materials were characterized by X-ray diffraction, ultraviolet/visible and infrared spectroscopies, thermogravimetric analysis, scanning electron microscopy, electron paramagnetic resonance, and cyclic voltammetry. Despite the presence of broad and low intensity peaks, the X-ray diffractograms indicate that the lamellar structure of the vanadium pentoxide xerogel is preserved, with increase in the interplanar spacing, giving evidence of a low-crystalline structure. We found that the electrochemical behaviour of the hybrid materials is quite similar to that found for the V 2 O 5 xerogel alone, and we verified that PEO leads to stabilization and reproducibility of the Li + electrochemical insertion/de-insertion into the V 2 O 5 xerogel structure, which makes these materials potential components of lithium ion batteries. - Graphical abstract: The synthesis, structural and electrochemical properties of vanadium pentoxide xerogel-poly(ethylene oxide) hybrid materials have been described. Despite the presence of broad and low intensity peaks, the X-ray diffractograms indicate that the lamellar structure of the vanadium pentoxide xerogel is preserved. The cyclic voltammetry technique demonstrated that PEO intercalation provides an improvement in the electrochemical properties, mainly with respect to the lithium electroinsertion process into the oxide matrix

  20. Synthesis and characterization of hematite pigment obtained from a steel waste industry

    Energy Technology Data Exchange (ETDEWEB)

    Prim, S.R. [Department of Mechanical Engineering, University of the State of Santa Catarina, Santa Catarina (Brazil); Folgueras, M.V., E-mail: dem2mvf@joinville.udesc.br [Department of Mechanical Engineering, University of the State of Santa Catarina, Santa Catarina (Brazil); Lima, M.A. de [Department of Mechanical Engineering, University of the State of Santa Catarina, Santa Catarina (Brazil); Hotza, D. [Departamento de Engenharia Quimica, Federal University of Santa Catarina, Santa Catarina (Brazil)

    2011-09-15

    Highlights: {yields} The study of using of a industrial waste for the synthesis of hematite pigments. {yields} The nanometer dimension this waste and your behavior as chromophore. {yields} The effect of process variables on the mechanisms of encapsulation sintered pigments. - Abstract: Pigments that meet environmental and technology requirements are the focus of the research in the ceramic sector. This study focuses on the synthesis of ceramic pigment by encapsulation of hematite in crystalline and amorphous silica matrix. Iron oxide from a metal sheet rolling process was used as chromophore. A different content of hematite and silica was homogenized by conventional and high energy milling. The powders obtained after calcinations between 1050 and 1200 {sup o}C for 2 h were characterized by X-ray diffraction and SEM analysis. The pigments were applied to ceramic enamel and porcelain body. The effect of pigment was measured by comparing L*a*b* values of the heated samples. Results showed that the color developed is influenced by variables such as oxide content employed, conditions of milling and processing temperature. The results showed that the use of pigment developed does not interfere in microstructural characteristics of pigmented material. The best hue was obtained from samples with 15 wt% of chromophore, heated at 1200 {sup o}C in amorphous silica matrix.