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Sample records for synthesis structure properties

  1. Detonation-synthesis nanodiamonds: synthesis, structure, properties and applications

    Energy Technology Data Exchange (ETDEWEB)

    Dolmatov, Valerii Yu [Federal State Unitary Enterprise Special Design-Technology Bureau (FSUE SDTB) ' ' Tekhnolog' ' at the St Petersburg State Institute of Technology (Technical University) (Russian Federation)

    2007-04-30

    The review outlines the theoretical foundations and industrial implementations of modern detonation synthesis of nanodiamonds and chemical purification of the nanodiamonds thus obtained. The structure, key properties and promising fields of application of detonation-synthesis nanodiamonds are considered.

  2. Detonation-synthesis nanodiamonds: synthesis, structure, properties and applications

    International Nuclear Information System (INIS)

    Dolmatov, Valerii Yu

    2007-01-01

    The review outlines the theoretical foundations and industrial implementations of modern detonation synthesis of nanodiamonds and chemical purification of the nanodiamonds thus obtained. The structure, key properties and promising fields of application of detonation-synthesis nanodiamonds are considered.

  3. Synthesis, structure, and properties of azatriangulenium salts

    DEFF Research Database (Denmark)

    Laursen, B.W.; Krebs, Frederik C

    2001-01-01

    amines and, by virtue of its stepwise and irreversible nature, provides a powerful tool for the preparation of a wide variety of new heterocyclic carbenium salts. Several derivatives of the three new oxygen- and/or nitrogen-bridged triangulenium salts, azadioxa- (6), diazaoxa- (7......), and triazatriangulenium (4), have been synthesized and their physicochemical properties have been investigated. Crystal structures for compounds 2 b-PF6: 2d-PF6, 4b-BF4, 4c-BF4, 6e-BF4, and 8 are reported. The different packing modes found for the triazatriagulenium salts are discussed in relation to the electrostatic...

  4. Synthesis route and structural properties of nanoferrites

    Energy Technology Data Exchange (ETDEWEB)

    Zaharieva, Katerina; Cherkezova-Zheleva, Zara; Kunev, Boris; Shopska, Maya; Mitov, Ivan [Institute of Catalysis, Bulgarian Academy of Sciences, Sofia (Bulgaria)

    2013-07-01

    The nano dimensional magnesium ferrite materials Mg{sub 0.25}Fe{sub 2.75}O{sub 4} , Mg{sub 0.5}Fe{sub 2.5}O{sub 4} and MgFe{sub 2}O{sub 4} with different stoichiometry were prepared by co-precipitation procedure using MgCl{sub 2} •6H{sub 2}O, FeCl{sub 2} •4H{sub 2}O and FeCl{sub 3} •6H{sub 2}O and NaOH as precipitant. The physicochemical methods - X-ray diffraction analysis, Moessbauer spectroscopy and FTIR spectroscopy were performed to investigate the structural properties of obtained nano size magnesium ferrite type samples. The registered experimental data were determined the presence of spinel ferrites and additional precursor phases as iron oxihydroxides and double layered hydroxides in ferrite materials MgxFe{sub 3-x}O{sub 4} (x=0.5;1). In the case of magnesium ferrite sample Mg{sub x}Fe{sub 3-x}O{sub 4} (x=0.25) the existence of non-stoichiometric spinel ferrite and intermediate phase - iron oxihydroxides were observed only. Key words: magnesium ferrites, co-precipitation, physicochemical methods.

  5. Synthesis route and structural properties of nanoferrites

    International Nuclear Information System (INIS)

    Zaharieva, Katerina; Cherkezova-Zheleva, Zara; Kunev, Boris; Shopska, Maya; Mitov, Ivan

    2013-01-01

    The nano dimensional magnesium ferrite materials Mg 0.25 Fe 2.75 O 4 , Mg 0.5 Fe 2.5 O 4 and MgFe 2 O 4 with different stoichiometry were prepared by co-precipitation procedure using MgCl 2 •6H 2 O, FeCl 2 •4H 2 O and FeCl 3 •6H 2 O and NaOH as precipitant. The physicochemical methods - X-ray diffraction analysis, Moessbauer spectroscopy and FTIR spectroscopy were performed to investigate the structural properties of obtained nano size magnesium ferrite type samples. The registered experimental data were determined the presence of spinel ferrites and additional precursor phases as iron oxihydroxides and double layered hydroxides in ferrite materials MgxFe 3-x O 4 (x=0.5;1). In the case of magnesium ferrite sample Mg x Fe 3-x O 4 (x=0.25) the existence of non-stoichiometric spinel ferrite and intermediate phase - iron oxihydroxides were observed only. Key words: magnesium ferrites, co-precipitation, physicochemical methods

  6. Synthesis, structural and optical properties of nanoparticles (Al, V ...

    Indian Academy of Sciences (India)

    The synthesis by the sol–gel method, structural and optical properties of ZnO, Zn0.99Al0.01O (AlZ),. Zn0.9V0.1O (VZ) ... drops of the resulting suspension containing the synthesized .... ZnO films on silicon substrate, they thought that this emis-.

  7. Hydrothermal synthesis, crystal structure and luminescence property ...

    Indian Academy of Sciences (India)

    The design and construction of ... dination polymers. It is difficult to design coordination .... The first endotherm at about 180 ... graphic data for coordination polymer 1. ... Sheldrick G M 1997 SHELXS-97: Program for solution of crystal structures ...

  8. Metal Oxide Nano structures: Synthesis, Properties, and Applications

    International Nuclear Information System (INIS)

    Xu, L. H.; Patil, D. S.; Yang, J.; Xiao, J.

    2015-01-01

    In recent years, nano structured materials have attracted wide attention due to their fascinating optical and electrical properties, which make these materials potentially suitable for applications in electronics, optics, photonics, and sensors. Some metal oxides show a wide variety of morphologies such as nano wires, nano rods, nano tubes, nano rings, and nano belts. Synthesis and investigation of these metal-oxide nano structures are beneficial not only for understanding the fundamental phenomena in low dimensional systems, but also for developing new-generation nano devices with high performance.

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

    Science.gov (United States)

    Lech, Andrew Thomas

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

  10. Synthesis, crystal structures and properties of lead phosphite compounds

    International Nuclear Information System (INIS)

    Song, Jun-Ling; Hu, Chun-Li; Xu, Xiang; Kong, Fang; Mao, Jiang-Gao

    2015-01-01

    Here, we report the preparation and characterization of two lead(II) phosphites, namely, Pb_2(HPO_3)_2 and Pb_2(HPO_3)(NO_3)_2 through hydrothermal reaction or simple solution synthesis, respectively. A new lead phosphite, namely, Pb_2(HPO_3)_2, crystallizes in the noncentrosymmetric space group Cmc2_1 (no. 36), which features 3D framework formed by the interconnection of 2D layer of lead(II) phosphites and 1D chain of [Pb(HPO_3)_5]_∞. The nonlinear optical properties of Pb_2(HPO_3)(NO_3)_2 have been studied for the first time. The synergistic effect of the stereo-active lone-pairs on Pb"2"+ cations and π-conjugated NO_3 units in Pb_2(HPO_3)(NO_3)_2 produces a moderate second harmonic generation (SHG) response of ∼1.8×KDP (KH_2PO_4), which is phase matchable (type I). IR, UV–vis spectra and thermogravimetric analysis (TGA) for the two compounds were also measured. - Graphical abstract: Two lead phosphites Pb_2(HPO_3)_2 and Pb_2(HPO_3)(NO_3)_2 are studied. A new lead phosphite Pb_2(HPO_3)_2 features a unique 3D framework structure and Pb_2(HPO_3)(NO_3)_2 shows a moderate SHG response of ∼1.8×KDP (KH_2PO_4). - Highlights: • A new lead phosphite, Pb_2(HPO_3)_2 is reported. • Pb_2(HPO_3)_2 features a unique 3D framework structure. • NLO property of Pb_2(HPO_3)(NO_3)_2 is investigated. • Pb_2(HPO_3)(NO_3)_2 produces a moderate SHG response of ∼1.8×KDP (KH_2PO_4).

  11. Synthesis, structure, thermal, transport and magnetic properties of VN ceramics

    Czech Academy of Sciences Publication Activity Database

    Huber, Š.; Jankovský, O.; Sedmidubský, D.; Luxa, J.; Klimová, K.; Hejtmánek, Jiří; Sofer, Z.

    2016-01-01

    Roč. 42, č. 16 (2016), s. 18779-18784 ISSN 0272-8842 R&D Projects: GA ČR GA13-20507S Institutional support: RVO:68378271 Keywords : vanadium mononitride * phase transition * electronic structure * heat capacity * transport properties Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 2.986, year: 2016

  12. (Biodegradable Ionomeric Polyurethanes Based on Xanthan: Synthesis, Properties, and Structure

    Directory of Open Access Journals (Sweden)

    T. V. Travinskaya

    2017-01-01

    Full Text Available New (biodegradable environmentally friendly film-forming ionomeric polyurethanes (IPU based on renewable biotechnological polysaccharide xanthan (Xa have been obtained. The influence of the component composition on the colloidal-chemical and physic-mechanical properties of IPU/Xa and based films, as well as the change of their properties under the influence of environmental factors, have been studied. The results of IR-, PMS-, DMA-, and X-ray scattering study indicate that incorporation of Xa into the polyurethane chain initiates the formation of a new polymer structure different from the structure of the pure IPU (matrix: an amorphous polymer-polymer microdomain has occurred as a result of the chemical interaction of Xa and IPU. It predetermines the degradation of the IPU/Xa films as a whole, unlike the mixed polymer systems, and plays a key role in the improvement of material performance. The results of acid, alkaline hydrolysis, and incubation into the soil indicate the increase of the intensity of degradation processes occurring in the IPU/Xa in comparison with the pure IPU. It has been shown that the introduction of Xa not only imparts the biodegradability property to polyurethane, but also improves the mechanical properties.

  13. Synthesis, crystal structures and luminescence properties of two metal carboxyphosphonates

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Chaonan; Feng, Pingjing; Li, Jintang, E-mail: leejt@xmu.edu.cn; Luo, Xuetao

    2017-05-15

    Two metal carboxyphosphonates, [Co{sub 2}(OOCC{sub 5}H{sub 3}NPO{sub 3}){sub 2·}(H{sub 2}O){sub 3}] (Compound1) and Zn{sub 3}[OOCC{sub 6}H{sub 3}CH(OH)PO{sub 3}]{sub 2·}2H{sub 2}O (Compound2) were successfully synthesized under the hydrothermal reactions. In compound 1, two (Co1-NO{sub 5}) octahedra link the (CPO{sub 3}) by sharing the corner, which link the two (Co2-O{sub 6}) octahedra. From a-axis the six clusters form the layer. Each layer is linked through hydrogen bond. In compound 2, the (Zn-O{sub 4}) tetrahedron and (CPO{sub 3}) tetrahedron are corner-shared, which arrange in line. From a-axis, each line forms the columnar. The thermal and luminescence properties of these compounds were investigated. - Graphical abstract: The synthesis conditions of the two compounds and the crystal morphology. Compound 1 shows the layer and the compound 2 shows the pillared-layer. - Highlights: • Two new carboxyphosphonate ligands have been prepared. • Using the two ligands, two metal carboxyphosphonates have been synthesized. • The two MOFs may be candidates for fluorescent materials.

  14. Nanocomposites: synthesis, structure, properties and new application opportunities

    Directory of Open Access Journals (Sweden)

    Pedro Henrique Cury Camargo

    2009-03-01

    Full Text Available Nanocomposites, a high performance material exhibit unusual property combinations and unique design possibilities. With an estimated annual growth rate of about 25% and fastest demand to be in engineering plastics and elastomers, their potential is so striking that they are useful in several areas ranging from packaging to biomedical applications. In this unified overview the three types of matrix nanocomposites are presented underlining the need for these materials, their processing methods and some recent results on structure, properties and potential applications, perspectives including need for such materials in future space mission and other interesting applications together with market and safety aspects. Possible uses of natural materials such as clay based minerals, chrysotile and lignocellulosic fibers are highlighted. Being environmentally friendly, applications of nanocomposites offer new technology and business opportunities for several sectors of the aerospace, automotive, electronics and biotechnology industries.

  15. Alkyltributylphosphonium chloride ionic liquids: synthesis, physicochemical properties and crystal structure.

    Science.gov (United States)

    Adamová, Gabriela; Gardas, Ramesh L; Nieuwenhuyzen, Mark; Puga, Alberto V; Rebelo, Luís Paulo N; Robertson, Allan J; Seddon, Kenneth R

    2012-07-21

    A series of alkyltributylphosphonium chloride ionic liquids, prepared from tributylphosphine and the respective 1-chloroalkane, C(n)H(2n+1)Cl (where n = 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 12 or 14), is reported. This work is a continuation of an extended series of tetraalkylphosphonium ionic liquids, where the focus is on the variability of n and its impact on the physical properties, such as melting points/glass transitions, thermal stability, density and viscosity. Experimental density and viscosity data were interpreted using QPSR and group contribution methods and the crystal structure of propyl(tributyl)phosphonium chloride is detailed.

  16. Synthesis, structural and ferromagnetic properties of La1–x Kx ...

    Indian Academy of Sciences (India)

    2016-08-26

    Aug 26, 2016 ... Synthesis, structural and ferromagnetic properties of La1–KMnO3 (0.0≤ 0.25) phases by solution combustion method ... Structural parameters were determined by the Rietveld refinement method using powder XRD data. Parent ... The ratio of the Mn3+/Mn4+ was determined by the iodometric titration.

  17. Stacked nickelocenes: synthesis, structural characterization, and magnetic properties.

    Science.gov (United States)

    Trtica, Sabrina; Prosenc, Marc Heinrich; Schmidt, Michael; Heck, Jürgen; Albrecht, Ole; Görlitz, Detlef; Reuter, Frank; Rentschler, Eva

    2010-02-15

    The disubstitution of 1,8-diiodonaphthalene (1) with cyclopentadienyl nucleophiles reveals 1,8-(dicyclopentadienyl)-naphthalene, which rapidly undergoes Diels-Alder reaction forming 1,8-(3a',4',7',7a'-tetrahydro-4',7'-methanoindene-7a',8'-diyl)-naphthalene (2). A subsequent retro-Diels-Alder reaction in the presence of sodium hydride yields the disodium salt of 1,8-(dicyclopentadiendiyl)-naphthalene 3. The disodium salt 3 was the starting material to obtain the paramagnetic bisnickelocene derivative 4, which structure was obtained by X-ray structure analysis, revealing two nickelocenes kept together in a stacked fashion by a 1,8-naphthalene clamp. An electronic interaction between the two nickel atoms is found as a result of cyclic voltammetry, indicating five different oxidation states +4, +3, +2, +1, and 0. The magnetic properties of 4 in solution were studied by variable temperature paramagnetic (1)H NMR spectroscopy and Evans method and revealed Curie behavior between 213 and 293 K. The magnetic susceptibility of a powdered sample of 4 was measured, and an antiferromagnetic interaction with an exchange coupling of J(12) = -31.49 cm(-1) is found. In accord with experimental data, broken symmetry density functional theory (DFT) calculations revealed four antiferromagnetically coupled electrons resulting in an open shell singlet ground state.

  18. Nitrocyclopropanes: synthesis and properties

    Energy Technology Data Exchange (ETDEWEB)

    Averina, Elena B; Yashin, N V; Kuznetsova, Tamara S; Zefirov, Nikolai S [Department of Chemistry, M.V. Lomonosov Moscow State University, Moscow (Russian Federation)

    2009-10-31

    State-of-the-art data on the methods of synthesis, properties and transformations of nitro- and- dinitrocyclopropanes of different structure is generalized and described systematically. The attention is focused on stereoselective cyclopropanation methods, new approaches to the synthesis of natural products and their synthetic analogues with diversified biological activities, in particular, of aminocyclopropane acids based on nitrocyclopropanes, and the formation of structures of energetic compounds.

  19. Synthesis of arborescent model polymer structures by living carbocationic polymerization for structure-property studies

    Science.gov (United States)

    Dos Santos Freire, Lucas

    Polyisobutylene is fully saturated, therefore exhibits outstanding chemical, oxidative and thermal stability,1 which makes it ideally suitable as a model to study mechanical and viscoelastic properties of elastomers, and to correlate properties with structure. The main objective of this dissertation was to develop a fundamental understanding of the mechanism of the synthesis of arborescent (hyperbranched) polyisobutylene (arbPIB) by inimer-type (initiator-monomer) living carbocationic polymerization. The strategy for the effective synthesis of arbPIBs consists of copolymerizing the 4-(2-methoxyisopropyl)styrene (IUPAC name: p-vinylcumyl methyl ether) (IB) via controlled/living carbocationic polymerization using TiCl4 coinitiator. In situ FTIR monitoring showed that the self-condensing vinyl polymerization (SCVP) of MeOIM is possible, and that when copolymerizing MeOIM and IB, a nearly alternating structure and multiple end groups are obtained. arbPIB was synthesized and the repeatability of the polymerization was demonstrated. It was found that higher branching was obtained with increasing [MeOIM] and that branching did not further increase if additional IB was added after the MeOIM had reacted completely. No evident changes were observed when switching solvents from Hx/MeCl to a MeCHx/MeCl mixture. Branching parameters showed that arbPIBs have a behavior between polydisperse stars and polycondensates with the number of branches increasing linearly with molecular weight. Novel arbPIB-based block copolymers (TPEs) were synthesized and it was found that copolymers with low Tg short end blocks and less than 5 mol% of a second monomer exhibit thermoplastic elastomeric properties. The materials were strongly reinforced when compounded with carbon black. arbPIB-b-PS are prospective biomaterials and the establishment of reliable methods for evaluating their short and long term properties is a subject of great importance. A dynamic fatigue testing methodology was developed

  20. Synthesis, structure and luminescence properties of phosphates A1 ...

    Indian Academy of Sciences (India)

    rule and the localization of this cation in the structure, which is in agreement with the structural characterization. It appears that europium ... 1. Introduction. Atom isomorphism in complex crystalline compounds with ..... isotropic approx- imation of basis atom positions in the structures of phosphates Na0.7Eu0.1Zr2(PO4)3 and.

  1. Synthesis, structure and thermoelectric properties of La1 ...

    Indian Academy of Sciences (India)

    Structural parameters for all the compounds were confirmed by the Rietveld refinement method usingpowder X-ray diffraction (XRD) data and exhibit the rhombhohedral crystal structure with space group R-3c (No. 167). Thescanning electron microscopy study reveals that the particles are spherical in shape and sizes, in the ...

  2. Synthesis, spectral and structural properties of bis-imidazoline selones

    Indian Academy of Sciences (India)

    The solid state structures of bis-imidazoline selones were ... two biologically active selones are expected to function. ∗ .... The organic extract was washed with brine solution .... mentioned CH2 carbon and the quaternary carbon of benzene ...

  3. Structural Ceramic Nanocomposites: A Review of Properties and Powders’ Synthesis Methods

    Science.gov (United States)

    Palmero, Paola

    2015-01-01

    Ceramic nanocomposites are attracting growing interest, thanks to new processing methods enabling these materials to go from the research laboratory scale to the commercial level. Today, many different types of nanocomposite structures are proposed in the literature; however, to fully exploit their exceptional properties, a deep understanding of the materials’ behavior across length scales is necessary. In fact, knowing how the nanoscale structure influences the bulk properties enables the design of increasingly performing composite materials. A further key point is the ability of tailoring the desired nanostructured features in the sintered composites, a challenging issue requiring a careful control of all stages of manufacturing, from powder synthesis to sintering. This review is divided into four parts. In the first, classification and general issues of nanostructured ceramics are reported. The second provides basic structure–property relations, highlighting the grain-size dependence of the materials properties. The third describes the role of nanocrystalline second-phases on the mechanical properties of ordinary grain sized ceramics. Finally, the fourth part revises the mainly used synthesis routes to produce nanocomposite ceramic powders, underlining when possible the critical role of the synthesis method on the control of microstructure and properties of the sintered ceramics. PMID:28347029

  4. Carbon nanotubes on carbon fibers: Synthesis, structures and properties

    Science.gov (United States)

    Zhang, Qiuhong

    The interface between carbon fibers (CFs) and the resin matrix in traditional high performance composites is characterized by a large discontinuity in mechanical, electrical, and thermal properties which can cause inefficient energy transfer. Due to the exceptional properties of carbon nanotubes (CNTs), their growth at the surface of carbon fibers is a promising approach to controlling interfacial interactions and achieving the enhanced bulk properties. However, the reactive conditions used to grow carbon nanotubes also have the potential to introduce defects that can degrade the mechanical properties of the carbon fiber (CF) substrate. In this study, using thermal chemical vapor deposition (CVD) method, high density multi-wall carbon nanotubes have been successfully synthesized directly on PAN-based CF surface without significantly compromising tensile properties. The influence of CVD growth conditions on the single CF tensile properties and carbon nanotube (CNT) morphology was investigated. The experimental results revealed that under high temperature growth conditions, the tensile strength of CF was greatly decreased at the beginning of CNT growth process with the largest decrease observed for sized CFs. However, the tensile strength of unsized CFs with CNT was approximately the same as the initial CF at lower growth temperature. The interfacial shear strength of CNT coated CF (CNT/CF) in epoxy was studied by means of the single-fiber fragmentation test. Results of the test indicate an improvement in interfacial shear strength with the addition of a CNT coating. This improvement can most likely be attributed to an increase in the interphase yield strength as well as an improvement in interfacial adhesion due to the presence of the nanotubes. CNT/CF also offers promise as stress and strain sensors in CF reinforced composite materials. This study investigates fundamental mechanical and electrical properties of CNT/CF using nanoindentation method by designed

  5. Alkyltributylphosphonium chloride ionic liquids: synthesis, physicochemical properties and crystal structure

    OpenAIRE

    Adamova, Gabriela; Gardas, Ramesh L.; Nieuwenhuyzen, Mark; Vaca Puga, Alberto; Rebelo, Luis Paulo N.; Robertson, Allan J.; Seddon, Kenneth R.

    2012-01-01

    A series of alkyltributylphosphonium chloride ionic liquids, prepared from tributylphosphine and the respective 1-chloroalkane, CnH2n+1Cl (where n = 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 12 or 14), is reported. This work is a continuation of an extended series of tetraalkylphosphonium ionic liquids, where the focus is on the variability of n and its impact on the physical properties, such as melting points/glass transitions, thermal stability, density and viscosity. Experimental density and viscosit...

  6. Synthesis, crystal structures and properties of new quinolinium derivatives

    Science.gov (United States)

    Zhang, Xinyuan; Jiang, Xingxing; Li, Yin; Lin, Zheshuai; Zhang, Guochun; Wu, Yicheng

    2015-11-01

    Four phenyl-substituted quinolinium salts with different counter anions, C27H27NO4S, C26H25NO5S, C25H22NO5SCl, and C25H22NO5SBr, were synthesized and their single crystals were successfully grown from methanol solution by slow evaporation. Single crystal X-ray diffraction analyses showed that C27H27NO4S crystal belongs to the noncentrosymmetric orthorhombic space group Pna21, and the other three crystals belong to centrosymmetric monoclinic space group P21/n. Their first order hyperpolarization and macroscopic nonlinearity were analyzed and physical properties were characterized by UV-vis absorption spectroscopy, and differential scanning calorimetric and thermal gravimetric analysis.

  7. One dimensional coordination polymers: Synthesis, crystal structures and spectroscopic properties

    Science.gov (United States)

    Karaağaç, Dursun; Kürkçüoğlu, Güneş Süheyla; Şenyel, Mustafa; Şahin, Onur

    2016-11-01

    Two new one dimensional (1D) cyanide complexes, namely [M(4-aepy)2(H2O)2][Pt(CN)4], (4-aepy = 4-(2-aminoethyl)pyridine M = Cu(II) (1) or Zn(II) (2)), have been synthesized and characterized by vibrational (FT-IR and Raman) spectroscopy, single crystal X-ray diffraction, thermal and elemental analyses techniques. The crystallographic analyses reveal that 1 and 2 are isomorphous and isostructural, and crystallize in the monoclinic system and C2 space group. The Pt(II) ions are coordinated by four cyanide-carbon atoms in the square-planar geometry and the [Pt(CN)4]2- ions act as a counter ion. The M(II) ions display an N4O2 coordination sphere with a distorted octahedral geometry, the nitrogen donors belonging to four molecules of the organic 4-aepy that act as unidentate ligands and two oxygen atoms from aqua ligands. The crystal structures of 1 and 2 are similar each other and linked via intermolecular hydrogen bonding, Pt⋯π interactions to form 3D supramolecular network. Vibration assignments of all the observed bands are given and the spectral features also supported to the crystal structures of the complexes.

  8. Synthesis, structure, and physical properties of new rare earth ferrocenoylacetonates.

    Science.gov (United States)

    Koroteev, Pavel S; Dobrokhotova, Zhanna V; Ilyukhin, Andrey B; Efimov, Nikolay N; Rouzières, Mathieu; Kiskin, Mikhail A; Clérac, Rodolphe; Novotortsev, Vladimir M

    2016-04-21

    New ferrocenoylacetonate complexes of several rare earth elements, [Ln(fca)3(bpy)]·MeC6H5 (Ln = Pr (), Eu (), Gd (), Tb (), Dy (), Ho (), Y (); bpy - 2,2'-bipyridine; Hfca - FcCOCH2COMe) as well as scandium ferrocenoylacetonate [Sc(fca)3]·0.5MeC6H5 (), were synthesized and characterized by single crystal X-ray diffraction analysis. In the crystal lattice of the isostructural complexes , two [Ln(fca)3(bpy)] molecules form a pair due to stacking interactions between the bpy ligands. The Ln(3+) ions are coordinated in a square antiprism geometry with a coordination number of 8. The Sc(3+) ions in complex are coordinated in an octahedral geometry. Thermolysis of complexes was studied under air and argon atmospheres; in the first case, it affords perovskites LnFeO3 as one of the products. Complexes display single-molecule magnet properties, and the effective relaxation barrier for the Dy complex , was found to be Δeff/kB = 241 K, which is one of the highest values obtained for a mononuclear β-diketonate lanthanide complex.

  9. Uranium hetero-bimetallic complexes: synthesis, structure and magnetic properties

    International Nuclear Information System (INIS)

    Le Borgne, Th.

    2000-01-01

    The aim of this thesis is to synthesize molecular complexes with uranium and transition metal ions in close proximity, to determine the nature of the magnetic interaction between them. We decided to use Schiff bases as assembling ligands, which are unusual for uranium (IV). Although the simplest Schiff bases, such as H 2 Salen, lead to ligand exchange reactions, the bi-compartmental Schiff base H 4 L 6 (bis(3-hydroxy-salicylidene) - 2,2-dimethyl-propylene) allows the crystal structure determination of the complex [L 6 Cu(pyr)]U[L 6 Cu].2pyr, obtained by reaction of the metallo-ligand H 2 L 6 Cu with U(acac) 4 . In this manner, the complexes [L 6 Co(pyr)] 2 U and [L 6 Ni(pyr)] 2 U.pyr were also isolated, as well as the compounds in which the paramagnetic ions have been exchanged by the diamagnetic ions Zn II , Zr IV and Th IV ': [L 6 Zn(pyr)] 2 U, [L 6 Cu] 2 Zr and [L 6 Cu(pyr)]Th[L 6 Cu].2pyr. These complexes are the first which involve three metallic centres assembling by the means of a hexa-dentate Schiff base. The crystalline structures show, for all these complexes, the outstanding orthogonal arrangement of the two fragments L 6 M around the central atom which is in a dodecahedral environment of eight oxygen atoms of two Schiff bases. The syntheses of the isostructural complexes Cu2 II and Zn 2 U in which the uranium (IV) ion is close, in the first one, to the paramagnetic ion Cu II and, in the second one, to the diamagnetic ion Zn II , has allowed the use of the empiric method to determine the nature of the magnetic interaction between an f element and a transition metal. The comparison of the magnetic behaviour of two complexes Cu 2 U and Zn 2 U, expressed by the variation of χT vs T, reveals the ferromagnetic interaction in the heart of the triad Cu-U-Cu. The magnetic behaviour of the complexes Cu 2 Th et Cu 2 Zr which does not show any coupling between the two copper (II) ions and the weak antiferromagnetic interaction in the Ni 2 U compound, favour the

  10. 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.

  11. Green synthesis of ZnO nanoparticles by Aspalathus linearis: Structural & optical properties

    International Nuclear Information System (INIS)

    Diallo, A.; Ngom, B.D.; Park, E.; Maaza, M.

    2015-01-01

    This contribution reports for the 1st time on the synthesis and the main physical properties of ZnO nanoparticles synthesized by an entirely green physical-chemistral process using Aspalathus linearis's natural extract as an efficient reduction/oxidizing agent. Their structural and optical properties by electron microscopy, X-rays diffraction, Raman and X-rays photoemission spectroscopies as well as room temperature photoluminescence are reported. - Highlights: • 1st time report on synthesis of ZnO nanoparticles by a green process via Aspalathus linearis extract. • A. linearis's natural extract was used as an effective reduction/oxidizing agent. • Wurtzite nature of ZnO nanoparticles was confirmed via XRD, Raman, XPS and PL

  12. Green synthesis of ZnO nanoparticles by Aspalathus linearis: Structural & optical properties

    Energy Technology Data Exchange (ETDEWEB)

    Diallo, A.; Ngom, B.D. [UNESCO-UNISA Africa Chair in Nanosciences-Nanotechnology, College of Graduate Studies, University of South Africa, Muckleneuk Ridge, PO Box 392, Pretoria (South Africa); Nanosciences African Network (NANOAFNET), iThemba LABS-National Research Foundation, 1 Old Faure road, Somerset West 7129, PO Box 722, Somerset West, Western Cape (South Africa); Park, E. [UNESCO-UNISA Africa Chair in Nanosciences-Nanotechnology, College of Graduate Studies, University of South Africa, Muckleneuk Ridge, PO Box 392, Pretoria (South Africa); Nanosciences African Network (NANOAFNET), iThemba LABS-National Research Foundation, 1 Old Faure road, Somerset West 7129, PO Box 722, Somerset West, Western Cape (South Africa); Nelson Mandela African Institute for Science & Technology, Arusha (Tanzania, United Republic of); Maaza, M., E-mail: Maaza@tlabs.ac.za [UNESCO-UNISA Africa Chair in Nanosciences-Nanotechnology, College of Graduate Studies, University of South Africa, Muckleneuk Ridge, PO Box 392, Pretoria (South Africa); Nanosciences African Network (NANOAFNET), iThemba LABS-National Research Foundation, 1 Old Faure road, Somerset West 7129, PO Box 722, Somerset West, Western Cape (South Africa)

    2015-10-15

    This contribution reports for the 1st time on the synthesis and the main physical properties of ZnO nanoparticles synthesized by an entirely green physical-chemistral process using Aspalathus linearis's natural extract as an efficient reduction/oxidizing agent. Their structural and optical properties by electron microscopy, X-rays diffraction, Raman and X-rays photoemission spectroscopies as well as room temperature photoluminescence are reported. - Highlights: • 1st time report on synthesis of ZnO nanoparticles by a green process via Aspalathus linearis extract. • A. linearis's natural extract was used as an effective reduction/oxidizing agent. • Wurtzite nature of ZnO nanoparticles was confirmed via XRD, Raman, XPS and PL.

  13. Synthesis and optical properties of novel organic-inorganic hybrid nanolayer structure semiconductors

    International Nuclear Information System (INIS)

    Zhang Sanjun; Lanty, Gaetan; Lauret, Jean-Sebastien; Deleporte, Emmanuelle; Audebert, Pierre; Galmiche, Laurent

    2009-01-01

    We report on the synthesis of some novel organic-inorganic hybrid 2D perovskite semiconductors (R-(CH 2 ) n NH 3 ) 2 PbX 4 . These semiconductors are self-assembled intercalation nanolayers and have a multi-quantum-well energy level structure. We systematically vary the characteristic of organic groups (R-(CH 2 ) n NH 3 + ) to study the relationship between their structures and the optical properties of (R-(CH 2 ) n NH 3 ) 2 PbX 4 . From optical absorption and photoluminescence spectroscopy experiments performed on series of samples, we find some trends of choosing the organic groups to improve the optical performance of (R-(CH 2 ) n NH 3 ) 2 PbX 4 . A new organic group, which allows synthesis of nanolayer perovskite semiconductors with quite high photoluminescence efficiency and better long-term stability, has been found.

  14. Carbon Nanotubes Advanced Topics in the Synthesis, Structure, Properties and Applications

    CERN Document Server

    Jorio, Ado; Dresselhaus, Mildred S

    2008-01-01

    The carbon nanotubes field has evolved substantially since the publication of the bestseller "Carbon Nanotubes: Synthesis, Structure, Properties and Applications". The present volume builds on the generic aspects of the aforementioned book, which emphasizes the fundamentals, with the new volume emphasizing areas that have grown rapidly since the first volume, guiding future directions where research is needed and highlighting applications. The volume also includes an emphasis on areas like graphene, other carbon-like and other tube-like materials because these fields are likely to affect and influence developments in nanotubes in the next 5 years.

  15. Investigating the Synthesis, Structure, and Catalytic Properties of Versatile Gold-Based Nanocatalvsts

    Science.gov (United States)

    Pretzer, Lori A.

    Transition metal nanomaterials are used to catalyze many chemical reactions, including those key to environmental, medicinal, and petrochemical fields. Improving their catalytic properties and lifetime would have significant economic and environmental rewards. Potentially expedient options to make such advancements are to alter the shape, size, or composition of transition metal nanocatalysts. This work investigates the relationships between structure and catalytic properties of synthesized Au, Pd-on-Au, and Au-enzyme model transition metal nanocatalysts. Au and Pd-on-Au nanomaterials were studied due to their wide-spread application and structure-dependent electronic and geometric properties. The goal of this thesis is to contribute design procedures and synthesis methods that enable the preparation of more efficient transition metal nanocatalysts. The influence of the size and composition of Pd-on-Au nanoparticles (NPs) was systematically investigated and each was found to affect the catalyst's surface structure and catalytic properties. The catalytic hydrodechlorination of trichloroethene and reduction of 4-nitrophenol by Pd-on-Au nanoparticles were investigated as these reactions are useful for environmental and pharmaceutical synthesis applications, respectively. Structural characterization revealed that the dispersion and oxidation state of surface Pd atoms are controlled by the Au particle size and concentration of Pd. These structural changes are correlated with observed Pd-on-Au NP activities for both probe reactions, providing new insight into the structure-activity relationships of bimetallic nanocatalysts. Using the structure-dependent electronic properties of Au NPs, a new type of light-triggered biocatalyst was prepared and used to remotely control a model biochemical reaction. This biocatalyst consists of a model thermophilic glucokinase enzyme covalently attached to the surface of Au nanorods. The rod-like shape of the Au nanoparticles made the

  16. Low-temperature synthesis and structural properties of ferroelectric K 3WO 3F 3 elpasolite

    Science.gov (United States)

    Atuchin, V. V.; Gavrilova, T. A.; Kesler, V. G.; Molokeev, M. S.; Aleksandrov, K. S.

    2010-06-01

    Low-temperature ferroelectric G2 polymorph of K 3WO 3F 3 has been prepared by chemical synthesis. Structural and chemical properties of the final product have been evaluated with X-ray powder diffraction (XRD), scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS). Structure parameters of G2-K 3WO 3F 3 are refined by the Rietveld method from XRD data measured at room temperature (space group Cm, Z = 2, a = 8.7350(3) Å, b = 8.6808(5) Å, c = 6.1581(3) Å, β = 135.124(3) Å, V = 329.46(3) Å 3; RB = 2.47%). Partial ordering of oxygen and fluorine atoms has been found over anion positions. Mechanism of ferroelectric phase transition in A 2BMO 3F 3 oxyfluorides is discussed.

  17. Nitridomanganates of alkaline-earth metals. Synthesis, structure, and physical properties

    Energy Technology Data Exchange (ETDEWEB)

    Ovchinnikov, Alexander

    2016-12-02

    The main goal of the present work was the synthesis of alkaline-earth nitridomanganates (AE{sub x}Mn{sub y}N{sub z}) with extended anionic structures and the characterization of their electronic and magnetic properties. Up to now, only compounds with isolated nitridomanganate anions have been reported in the discussed ternary systems. A systematic exploratory synthesis, employing high-temperature treatment of AE nitrides and Mn under controlled N2 pressure, yielded more than ten new nitridomanganates. Their crystal structures contain anionic building blocks of different dimensionalities, ranging from isolated species to three-dimensional frameworks. In general, the formation of Mn-rich compositions was found to be driven by the emergence of Mn-Mn interactions, which creates a link between nitridometalates and transition-metal-rich binary nitrides. The obtained nitridomanganates display a plethora of interesting phenomena, such as large spin-orbit coupling, magnetic frustration, quenching of magnetism due to Mn-Mn interactions, and metal-insulator transition.

  18. Synthesis and optical properties of novel organic-inorganic hybrid nanolayer structure semiconductors

    Energy Technology Data Exchange (ETDEWEB)

    Zhang Sanjun; Lanty, Gaetan; Lauret, Jean-Sebastien [Laboratoire de Photonique Quantique et Moleculaire de l' Ecole Normale Superieure de Cachan, 61 avenue du President Wilson, 94235 Cachan (France); Deleporte, Emmanuelle, E-mail: Emmanuelle.Deleporte@lpqm.ens-cachan.fr [Laboratoire de Photonique Quantique et Moleculaire de l' Ecole Normale Superieure de Cachan, 61 avenue du President Wilson, 94235 Cachan (France); Audebert, Pierre; Galmiche, Laurent [Laboratoire de Photophysique et Photochimie Supramoleculaires et Macromoleculaires de l' Ecole Normale Superieure de Cachan, 61 avenue du President Wilson, 94235 Cachan (France)

    2009-06-15

    We report on the synthesis of some novel organic-inorganic hybrid 2D perovskite semiconductors (R-(CH{sub 2}){sub n}NH{sub 3}){sub 2}PbX{sub 4}. These semiconductors are self-assembled intercalation nanolayers and have a multi-quantum-well energy level structure. We systematically vary the characteristic of organic groups (R-(CH{sub 2}){sub n}NH{sub 3}{sup +}) to study the relationship between their structures and the optical properties of (R-(CH{sub 2}){sub n}NH{sub 3}){sub 2}PbX{sub 4}. From optical absorption and photoluminescence spectroscopy experiments performed on series of samples, we find some trends of choosing the organic groups to improve the optical performance of (R-(CH{sub 2}){sub n}NH{sub 3}){sub 2}PbX{sub 4}. A new organic group, which allows synthesis of nanolayer perovskite semiconductors with quite high photoluminescence efficiency and better long-term stability, has been found.

  19. Strontium substituted hydroxyapatites: Synthesis and determination of their structural properties, in vitro and in vivo performance

    Energy Technology Data Exchange (ETDEWEB)

    Kaygili, Omer, E-mail: okaygili@firat.edu.tr [Department of Physics, Faculty of Science, Firat University, 23119 Elazig (Turkey); Keser, Serhat [Department of Chemistry, Faculty of Science, Firat University, 23119 Elazig (Turkey); Kom, Mustafa [Department of Surgery, Faculty of Veterinary Medicine, Firat University, 23119 Elazig (Turkey); Eroksuz, Yesari [Department of Pathology, Faculty of Veterinary Medicine, Firat University, 23119 Elazig (Turkey); Dorozhkin, Sergey V. [Kudrinskaja square 1-155, Moscow 123242 (Russian Federation); Ates, Tankut [Department of Physics, Faculty of Science, Firat University, 23119 Elazig (Turkey); Ozercan, Ibrahim H. [Department of Pathology, School of Medicine, Firat University, 23119 Elazig (Turkey); Tatar, Cengiz; Yakuphanoglu, Fahrettin [Department of Physics, Faculty of Science, Firat University, 23119 Elazig (Turkey)

    2015-10-01

    The objective of this study is to present a detailed report related to the synthesis and characterization of strontium substituted hydroxyapatites. Based on this purpose, hydroxyapatite (HAp) bioceramics with different amounts of strontium (e.g., 0, 0.45, 0.90, 1.35, 1.80 and 2.25 at.%) were prepared using a sol–gel method. The effects of Sr substitution on the structural properties and biocompatibility of the samples were studied by X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy and scanning electron microscopy (SEM) techniques, in vitro and in vivo tests. All the samples composed of the nanoparticles ranging from 21 to 27 nm. The presence of Sr at low levels influenced the crystal size, crystallinity degree, lattice parameters and volume of the unit cell of the HAp. Both in vitro conditions and soaking period in simulated body fluid (SBF) significantly affected these properties. Especially, the (Ca + Sr)/P molar ratio gradually decreases with increasing soaking period in SBF. Animal experiments revealed the bone formation and osseointegration for all samples, and as compared with other groups, more reasonable, were observed for the sample with the lowest Sr content. - Highlights: • Sr content affects the structural properties of hydroxyapatite. • Bone formation and osseointegration are observed for all the samples. • In vitro conditions cause a significant change in the (Ca + Sr)/P ratio.

  20. Synthesis and properties of ZnFe2O4 replica with biological hierarchical structure

    International Nuclear Information System (INIS)

    Liu, Hongyan; Guo, Yiping; Zhang, Yangyang; Wu, Fen; Liu, Yun; Zhang, Di

    2013-01-01

    Highlights: • ZFO replica with hierarchical structure was synthesized from butterfly wings. • Biotemplate has a significant impact on the properties of ZFO material. • Our method opens up new avenues for the synthesis of spinel ferrites. -- Abstract: ZnFe 2 O 4 replica with biological hierarchical structure was synthesized from Papilio paris by a sol–gel method followed by calcination. The crystallographic structure and morphology of the obtained samples were characterized by X-ray diffraction, field-emission scanning electron microscope, and transmittance electron microscope. The results showed that the hierarchical structures were retained in the ZFO replica of spinel structure. The magnetic behavior of such novel products was measured by a vibrating sample magnetometer. A superparamagnetism-like behavior was observed due to nanostructuration size effects. In addition, the ZFO replica with “quasi-honeycomb-like structure” showed a much higher specific capacitance of 279.4 F g −1 at 10 mV s −1 in comparison with ZFO powder of 137.3 F g −1 , attributing to the significantly increased surface area. These results demonstrated that ZFO replica is a promising candidate for novel magnetic devices and supercapacitors

  1. Fused 1,2,3-Dithiazoles: Convenient Synthesis, Structural Characterization, and Electrochemical Properties

    Directory of Open Access Journals (Sweden)

    Lidia S. Konstantinova

    2016-05-01

    Full Text Available A new general protocol for synthesis of fused 1,2,3-dithiazoles by the reaction of cyclic oximes with S2Cl2 and pyridine in acetonitrile has been developed. The target 1,2,3-dithiazoles fused with various carbocycles, such as indene, naphthalenone, cyclohexadienone, cyclopentadiene, and benzoannulene, were selectively obtained in low to high yields. In most cases, the hetero ring-closure was accompanied by chlorination of the carbocyclic moieties. With naphthalenone derivatives, a novel dithiazole rearrangement (15→13 featuring unexpected movement of the dithiazole ring from α- to β-position, with respect to keto group, was discovered. Molecular structure of 4-chloro-5H-naphtho[1,2-d][1,2,3]dithiazol-5-one 13 was confirmed by single-crystal X-ray diffraction. Electrochemical properties of 13 were studied by cyclic voltammetry and a complex behavior was observed, most likely including hydrodechlorination at a low potential.

  2. Synthesis, structure, optical property, and electronic structure of Ba7AgGa5Se15

    International Nuclear Information System (INIS)

    Yin, Wenlong; He, Ran; Feng, Kai; Hao, Wenyu; Yao, Jiyong; Wu, Yicheng

    2013-01-01

    Graphical abstract: -- Highlights: •A new quaternary chalcogenide Ba 7 AgGa 5 Se 15 was synthesized. •It adopts a new structure type in the space group P31c of the trigonal system. •The structure contains a three-dimensional framework built from GaSe 4 and AgSe 4 tetrahedra. •Ba 7 AgGa 5 Se 15 is a direct semiconductor with the band gap of 2.60 (2) eV. •The electronic structure was calculated to explain the optical properties. -- Abstract: A new quaternary chalcogenide Ba 7 AgGa 5 Se 15 was synthesized by solid state reaction. It crystallizes in a new structure type in the noncentrosymmetric space group P31c of the trigonal system. In the structure, three Ga2Se 4 tetrahedra and one Ga1Se 4 tetrahedron are connected to each other by corner-sharing to form [Ga 4 Se 10 ] 8− anion clusters, which are further connected to AgSe 4 tetrahedra by corner-sharing to form a three-dimensional framework with Ba, Se7, and isolated Ga3Se 4 tetrahedra residing in the cavities. The optical band gap of 2.60 (2) eV for Ba 7 AgGa 5 Se 15 was deduced from the diffuse reflectance spectrum. From a band structure calculation, Ba 7 AgGa 5 Se 15 is a direct semiconductor and the transition between Se and Ba plays an important role in the band gap

  3. Electrospray synthesis and properties of hierarchically structured PLGA TIPS microspheres for use as controlled release technologies.

    Science.gov (United States)

    Malik, Salman A; Ng, Wing H; Bowen, James; Tang, Justin; Gomez, Alessandro; Kenyon, Anthony J; Day, Richard M

    2016-04-01

    Microsphere-based controlled release technologies have been utilized for the long-term delivery of proteins, peptides and antibiotics, although their synthesis poses substantial challenges owing to formulation complexities, lack of scalability, and cost. To address these shortcomings, we used the electrospray process as a reproducible, synthesis technique to manufacture highly porous (>94%) microspheres while maintaining control over particle structure and size. Here we report a successful formulation recipe used to generate spherical poly(lactic-co-glycolic) acid (PLGA) microspheres using the electrospray (ES) coupled with a novel thermally induced phase separation (TIPS) process with a tailored Liquid Nitrogen (LN2) collection scheme. We show how size, shape and porosity of resulting microspheres can be controlled by judiciously varying electrospray processing parameters and we demonstrate examples in which the particle size (and porosity) affect release kinetics. The effect of electrospray treatment on the particles and their physicochemical properties are characterized by scanning electron microscopy, confocal Raman microscopy, thermogravimetric analysis and mercury intrusion porosimetry. The microspheres manufactured here have successfully demonstrated long-term delivery (i.e. 1week) of an active agent, enabling sustained release of a dye with minimal physical degradation and have verified the potential of scalable electrospray technologies for an innovative TIPS-based microsphere production protocol. Copyright © 2016 The Authors. Published by Elsevier Inc. All rights reserved.

  4. Synthesis, Crystal Structure and Luminescence Property of a New Silver(I) Dimer with Isonicotinic Acid

    International Nuclear Information System (INIS)

    Yuan, Qi; Liu, Bing

    2005-01-01

    The absorption spectrum was calculated from reflection spectrum by the Kubelka.Munk function. The energy gap of the title compound determined by extrapolation from the linear portion of the absorption edge in a (α/S) versus energy plot is 1.91 eV, which suggests that the title compound behaves as semiconductor. Isonicotinic acid (Iso), namely 4.pyridinecarboxylate, a multi.functional chelating and/or bridging ligand, has proved to be very powerful for the construction of multi. dimensional metal.organic coordination networks. Furthermore, The isonicotinic acid complexes has raised many interests in fluorescence probing with numerous potential applications for studies of microsecond diffusion and dynamics of membranes. Metal centers are potential carriers of electrochemical, magnetic, catalytic, or optical properties that may be introduced into the inorganic.organic hybrid materials. d"1"0 metals with rich photophysical and photochemical character have focused attentions to synthesize polynuclear complexes. Considering the versatile coordination abilities of Iso, we employ the ligand to coordinate with silver nitrate to fabricate a coordination complex with excellent fluorescence property. Herein we report the synthesis, crystal structure and fluorescence property of a new d"1"0 coordination dimer [Ag_2(Iso)_2(NO_3)_2

  5. Synthesis, Crystal Structure and Luminescence Property of a New Silver(I) Dimer with Isonicotinic Acid

    Energy Technology Data Exchange (ETDEWEB)

    Yuan, Qi [Pharmacy College of Henan University, Kaifeng (China); Liu, Bing [Chinese Academy of Sciences, Fuzhou (China)

    2005-10-15

    The absorption spectrum was calculated from reflection spectrum by the Kubelka.Munk function. The energy gap of the title compound determined by extrapolation from the linear portion of the absorption edge in a (α/S) versus energy plot is 1.91 eV, which suggests that the title compound behaves as semiconductor. Isonicotinic acid (Iso), namely 4.pyridinecarboxylate, a multi.functional chelating and/or bridging ligand, has proved to be very powerful for the construction of multi. dimensional metal.organic coordination networks. Furthermore, The isonicotinic acid complexes has raised many interests in fluorescence probing with numerous potential applications for studies of microsecond diffusion and dynamics of membranes. Metal centers are potential carriers of electrochemical, magnetic, catalytic, or optical properties that may be introduced into the inorganic.organic hybrid materials. d{sup 10} metals with rich photophysical and photochemical character have focused attentions to synthesize polynuclear complexes. Considering the versatile coordination abilities of Iso, we employ the ligand to coordinate with silver nitrate to fabricate a coordination complex with excellent fluorescence property. Herein we report the synthesis, crystal structure and fluorescence property of a new d{sup 10} coordination dimer [Ag{sub 2}(Iso){sub 2}(NO{sub 3}){sub 2}].

  6. Influence of synthesis method on structural and magnetic properties of cobalt ferrite nanoparticles

    International Nuclear Information System (INIS)

    Gyergyek, Saso; Makovec, Darko; Kodre, Alojz; Arcon, Iztok; Jagodic, Marko; Drofenik, Miha

    2010-01-01

    properties are strongly affected by the synthesis method used.

  7. 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

  8. Microwave plasma chemical synthesis of nanocrystalline carbon film structures and study their properties

    Science.gov (United States)

    Bushuev, N.; Yafarov, R.; Timoshenkov, V.; Orlov, S.; Starykh, D.

    2015-08-01

    The self-organization effect of diamond nanocrystals in polymer-graphite and carbon films is detected. The carbon materials deposition was carried from ethanol vapors out at low pressure using a highly non-equilibrium microwave plasma. Deposition processes of carbon film structures (diamond, graphite, graphene) is defined. Deposition processes of nanocrystalline structures containing diamond and graphite phases in different volume ratios is identified. The solid film was obtained under different conditions of microwave plasma chemical synthesis. We investigated the electrical properties of the nanocrystalline carbon films and identified it's from various factors. Influence of diamond-graphite film deposition mode in non-equilibrium microwave plasma at low pressure on emission characteristics was established. This effect is justified using the cluster model of the structure of amorphous carbon. It was shown that the reduction of bound hydrogen in carbon structures leads to a decrease in the threshold electric field of emission from 20-30 V/m to 5 V/m. Reducing the operating voltage field emission can improve mechanical stability of the synthesized film diamond-graphite emitters. Current density emission at least 20 A/cm2 was obtained. Nanocrystalline carbon film materials can be used to create a variety of functional elements in micro- and nanoelectronics and photonics such as cold electron source for emission in vacuum devices, photonic devices, cathodoluminescent flat display, highly efficient white light sources. The obtained graphene carbon net structure (with a net size about 6 μm) may be used for the manufacture of large-area transparent electrode for solar cells and cathodoluminescent light sources

  9. Synthesis, Optical and Structural Properties of Copper Sulfide Nanocrystals from Single Molecule Precursors

    Directory of Open Access Journals (Sweden)

    Peter A. Ajibade

    2017-02-01

    Full Text Available We report the synthesis and structural studies of copper sulfide nanocrystals from copper (II dithiocarbamate single molecule precursors. The precursors were thermolysed in hexadecylamine (HDA to prepare HDA-capped CuS nanocrystals. The optical properties of the nanocrystals studied using UV–visible and photoluminescence spectroscopy showed absorption band edges at 287 nm that are blue shifted, and the photoluminescence spectra show emission curves that are red-shifted with respect to the absorption band edges. These shifts are as a result of the small crystallite sizes of the nanoparticles leading to quantum size effects. The structural studies were carried out using powder X-ray diffraction (XRD, transmission electron microscopy (TEM, scanning electron microscopy (SEM, energy dispersive X-ray spectroscopy (EDS, and atomic force microscopy. The XRD patterns indicates that the CuS nanocrystals are in hexagonal covellite crystalline phases with estimated particles sizes of 17.3–18.6 nm. The TEM images showed particles with almost spherical or rod shapes, with average crystallite sizes of 3–9.8 nm. SEM images showed morphology with ball-like microspheres on the surfaces, and EDS spectra confirmed the presence of CuS nanoparticles.

  10. Hydrothermal synthesis, crystal structures, and enantioselective adsorption property of bis(L-histidinato)nickel(II) monohydrate

    Science.gov (United States)

    Ramos, Christian Paul L.; Conato, Marlon T.

    2018-05-01

    Despite the numerous researches in metal-organic frameworks (MOFs), there are only few reports on biologically important amino acids, histidine in particular, on its use as bridging ligand in the construction of open-framework architectures. In this work, hydrothermal synthesis was used to prepare a compound based on Ni2+ and histidine. The coordination assembly of imidazole side chain of histidine with divalent nickel ions in aqueous condition yielded purple prismatic solids. Single crystal X-ray diffraction (XRD) analysis of the product revealed structure for Ni(C6H8N3O2)2 • H2O that has a monoclinic (C2) structure with lattice parameters, a = 29.41, b = 8.27, c = 6.31 Å, β = 90.01 ˚. Circular dichroism - optical rotatory dispersion (CD-ORD), Powder X-ray diffraction (PXRD) and Fourier transform - infrared spectroscopy (FT-IR) analyses are conducted to further characterize the crystals. Enantioselective adsorption analysis using racemic mixture of 2-butanol confirmed bis(L-histidinato)nickel(II) monohydrate MOF crystal's enantioselective property preferentially favoring the adsorption of (S)-2-butanol isomer.

  11. Constitutional Isomers of Dendrimer-like Star Polymers: Design, Synthesis and Conformational and Structural Properties; TOPICAL

    International Nuclear Information System (INIS)

    Pople, John A.

    2001-01-01

    The design, synthesis and solution properties of six constitutional isomers of dendrimer-like star polymers is described. Each of the polymers have comparable molecular weights ((approx) 80,000 g/mol), narrow polydispersities ( and lt; 1.19) and an identical number of branching junctures (45) and surface hydroxyl functionalities (48). The only difference in the six isomers is the placement of the branching junctures. The polymers are constructed from high molecular weight poly(e-caprolactone) with branching junctures derived from 2,2'-bis(hydroxylmethyl) propionic acid (bis-MPA) emanating from a central core. The use of various generations of dendritic initiators and dendrons coupled with the ring opening polymerization of e-caprolactones allowed a modular approach to the dendrimer-like star polymer isomers. The most pronounced effects on the physical properties/morphology and hydrodynamic volume was for those polymers in which the branching was distributed throughout the sample in a dendrimer-like fashion. The versatility of this approach has provided the possibility of understanding the relationship between architecture and physical properties. Dynamic light scattering and small angle X-ray scattering techniques were used to determine the hydrodynamic radius Rh and radius of gyration Rg respectively. The relationship between Rg and molecular weight was indicative of a compact star-like structure, and did not show advanced bias towards either the dense core or dense shell models. The radial density distribution of the isomers was therefore modeled according to a many arm star polymer, and good agreement was found with experimental measures of Rh/Rg

  12. Nanometric solid solutions of the fluorite and perovskite type crystal structures: Synthesis and properties

    Directory of Open Access Journals (Sweden)

    Snežana Bošković

    2012-09-01

    Full Text Available In this paper a short review of our results on the synthesis of nanosized CeO2, CaMnO3 and BaCeO3 solid solutions are presented. The nanopowders were prepared by two innovative methods: self propagating room temperature synthesis (SPRT and modified glycine/nitrate procedure (MGNP. Different types of solid solutions with rare earth dopants in concentrations ranging from 0–0.25 mol% were synthesized. The reactions forming solid solutions were studied. In addition, the characteristics of prepared nanopowders, phenomena during sintering and the properties of sintered samples are discussed.

  13. Synthesis and properties MFe2O4 (M = Fe, Co) nanoparticles and core-shell structures

    Science.gov (United States)

    Yelenich, O. V.; Solopan, S. O.; Greneche, J. M.; Belous, A. G.

    2015-08-01

    Individual Fe3-xO4 and CoFe2O4 nanoparticles, as well as Fe3-xO4/CoFe2O4 core/shell structures were synthesized by the method of co-precipitation from diethylene glycol solutions. Core/shell structure were synthesized with CoFe2O4-shell thickness of 1.0, 2.5 and 3.5 nm. X-ray diffraction patterns of individual nanoparticles and core/shell are similar and indicate that all synthesized samples have a cubic spinel structure. Compares Mössbauer studies of CoFe2O4, Fe3-xO4 nanoparticles indicate superparamagnetic properties at 300 K. It was shown that individual magnetite nanoparticles are transformed into maghemite through oxidation during the synthesis procedure, wherein the smallest nanoparticles are completely oxidized while a magnetite core does occur in the case of the largest nanoparticles. The Mössbauer spectra of core/shell nanoparticles with increasing CoFe2O4-shell thickness show a gradual decrease in the relative intensity of the quadrupole doublet and significant decrease of the mean isomer shift value at both RT and 77 K indicating a decrease of the superparamagnetic relaxation phenomena. Specific loss power for the prepared ferrofluids was experimentally calculated and it was determined that under influence of ac-magnetic field magnetic fluid based on individual CoFe2O4 and Fe3-xO4 particles are characterized by very low heating temperature, when magnetic fluids based on core/shell nanoparticles demonstrate higher heating effect.

  14. Synthesis, electronic structure, elastic properties, and interfacial behavior of icosahedral boron-rich solids

    Energy Technology Data Exchange (ETDEWEB)

    Hunold, Oliver

    2017-08-01

    Boron-rich solids are commonly characterized by icosahedral clusters, where 12 B atoms form an icosahedron, giving rise to outstanding mechanical and transport properties. However, broader applications are limited due to the high synthesis temperature required to obtain the icosahedra-based crystalline structure. Utilizing high power pulsed magnetron sputtering (HPPMS), the deposition temperature may be lowered as compared to direct current magnetron sputtering by enhanced surface diffusion. Therefore, HPPMS was utilized to investigate the influence of the substrate temperature on the structural evolution of B-rich Al-Y-B thin films. The formation of the intended AlYB{sub 14} phase together with the (Y,Al)B{sub 6} impurity phase, containing 1.8 at.% less B than AlYB{sub 14}, was observed at a growth temperature of 800 C and hence 600 C below the bulk synthesis temperature. Based on density functional theory (DFT) calculations it is inferred that minute compositional variations may lead to formation of competing phases, such as (Y,Al)B{sub 6}. Furthermore, 800 C still limits the usage significantly. Therefore, quantum mechanical material design was applied to identify phases with even higher phase stabilities compared to AlYB{sub 14}. Phase stability of T{sub 0.75}Y{sub 0.75}B{sub 14} (T= Sc, Ti, V, Y, Zr, Nb, Si) critically depends on the exact magnitude of charge transferred by T and Y to the B icosahedra. The highest phase stabilities have been identified for Sc{sub 0.75}Y{sub 0.75}B{sub 14}, Ti{sub 0.75}Y{sub 0.75}B{sub 14}, and Zr{sub 0.75}Y{sub 0.75}B{sub 14}. ln combination with Young's modulus values up to 517 GPa these phases are very interesting from a wear-resistance point of view. Still high synthesis temperatures limit the use of such systems onto technologically relevant substrate materials. However, amorphous B-rich solids, which can be synthesized without additional heating, exhibit attractive mechanical and electrical properties. Within these

  15. Microwave-assisted hydrothermal synthesis of CePO4 nanostructures: Correlation between the structural and optical properties

    International Nuclear Information System (INIS)

    Palma-Ramírez, D.; Domínguez-Crespo, M.A.; Torres-Huerta, A.M.; Dorantes-Rosales, H.; Ramírez-Meneses, E.; Rodríguez, E.

    2015-01-01

    Highlights: • An enhancement in the hydrothermal synthesis for obtaining of CePO 4 is presented. • Microwave energy can replace the energy by convection for obtaining CePO 4 . • CePO 4 demonstrates to be an option to increase the optical properties of polymers. • Adjusting the pH, the sintering process is not necessary to obtain the desire phase. • CePO 4 morphologies undergo evolution from nanorods to semispherical nanoparticles. - Abstract: In this work, the microwave-assisted hydrothermal method is proposed as an alternative to the synthesis of cerium phosphate (CePO 4 ) nanostructures to evaluate the influence of different synthesis parameters on both the structural and optical properties. In order to reach this goal, two different sets of experiments were designed, varying the reaction temperature (130 and 180 °C), synthesis time (15 and 30 min) and sintering temperature (400 and 600 °C), maintaining a constant pH = 3. Thereafter, two experimental conditions were selected to assess changes in the properties of CePO 4 nanopowders with pH (1, 5, 9 and 11). The crystal structure and morphology of the nanostructures were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) and scanning electron microscopy (SEM), respectively. Diffuse reflectance properties of CePO 4 with different microstructures were studied. The results demonstrated that by using the microwave-assisted hydrothermal method, the shape, size and structural phase of CePO 4 can be modulated by using relatively low synthesis temperatures and short reaction times, and depending on pH, a sintering process is not needed to obtain either a desired phase or size. Under the selected experimental conditions, the materials underwent an evolution from nanorods to semispherical nanoparticles, accompanied by a phase transition from hexagonal to monoclinic

  16. Microwave-assisted hydrothermal synthesis of CePO{sub 4} nanostructures: Correlation between the structural and optical properties

    Energy Technology Data Exchange (ETDEWEB)

    Palma-Ramírez, D. [Instituto Politécnico Nacional, CICATA-Unidad Altamira, Km 14.5, Carretera Tampico-Puerto Industrial Altamira, C.P. 89600 Altamira, Tamps (Mexico); Domínguez-Crespo, M.A., E-mail: mdominguezc@ipn.mx [Instituto Politécnico Nacional, CICATA-Unidad Altamira, Km 14.5, Carretera Tampico-Puerto Industrial Altamira, C.P. 89600 Altamira, Tamps (Mexico); Torres-Huerta, A.M. [Instituto Politécnico Nacional, CICATA-Unidad Altamira, Km 14.5, Carretera Tampico-Puerto Industrial Altamira, C.P. 89600 Altamira, Tamps (Mexico); Dorantes-Rosales, H. [Instituto Politécnico Nacional, ESIQIE, Departamento de Metalurgia, C.P. 07300 México D.F. (Mexico); Ramírez-Meneses, E. [Universidad Iberoamericana, Departamento de Ingeniería y Ciencias Químicas, Prolongación Paseo de la Reforma 880, Lomas de Santa Fe, C.P. 01219 México D.F. (Mexico); Rodríguez, E. [Instituto Politécnico Nacional, CICATA-Unidad Altamira, Km 14.5, Carretera Tampico-Puerto Industrial Altamira, C.P. 89600 Altamira, Tamps (Mexico)

    2015-09-15

    Highlights: • An enhancement in the hydrothermal synthesis for obtaining of CePO{sub 4} is presented. • Microwave energy can replace the energy by convection for obtaining CePO{sub 4}. • CePO{sub 4} demonstrates to be an option to increase the optical properties of polymers. • Adjusting the pH, the sintering process is not necessary to obtain the desire phase. • CePO{sub 4} morphologies undergo evolution from nanorods to semispherical nanoparticles. - Abstract: In this work, the microwave-assisted hydrothermal method is proposed as an alternative to the synthesis of cerium phosphate (CePO{sub 4}) nanostructures to evaluate the influence of different synthesis parameters on both the structural and optical properties. In order to reach this goal, two different sets of experiments were designed, varying the reaction temperature (130 and 180 °C), synthesis time (15 and 30 min) and sintering temperature (400 and 600 °C), maintaining a constant pH = 3. Thereafter, two experimental conditions were selected to assess changes in the properties of CePO{sub 4} nanopowders with pH (1, 5, 9 and 11). The crystal structure and morphology of the nanostructures were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM) and scanning electron microscopy (SEM), respectively. Diffuse reflectance properties of CePO{sub 4} with different microstructures were studied. The results demonstrated that by using the microwave-assisted hydrothermal method, the shape, size and structural phase of CePO{sub 4} can be modulated by using relatively low synthesis temperatures and short reaction times, and depending on pH, a sintering process is not needed to obtain either a desired phase or size. Under the selected experimental conditions, the materials underwent an evolution from nanorods to semispherical nanoparticles, accompanied by a phase transition from hexagonal to monoclinic.

  17. Two-dimensional tantalum disulfide: controlling structure and properties via synthesis

    Science.gov (United States)

    Zhao, Rui; Grisafe, Benjamin; Krishna Ghosh, Ram; Holoviak, Stephen; Wang, Baoming; Wang, Ke; Briggs, Natalie; Haque, Aman; Datta, Suman; Robinson, Joshua

    2018-04-01

    Tantalum disulfide (TaS2) is a transition metal dichalcogenide (TMD) that exhibits phase transition induced electronic property modulation at low temperature. However, the appropriate phase must be grown to enable the semiconductor/metal transition that is of interest for next generation electronic applications. In this work, we demonstrate direct and controllable synthesis of ultra-thin 1T-TaS2 and 2H-TaS2 on a variety of substrates (sapphire, SiO2/Si, and graphene) via powder vapor deposition. The synthesis process leads to single crystal domains ranging from 20 to 200 nm thick and 1-10 µm on a side. The TaS2 phase (1T or 2H) is controlled by synthesis temperature, which subsequently is shown to control the electronic properties. Furthermore, this work constitutes the first demonstration of a metal-insulator phase transition in directly synthesized 1T-TaS2 films and domains by electronic means.

  18. Synthesis, crystal structure and magnetic properties of U2RuGa8

    International Nuclear Information System (INIS)

    Grin', Yu.N.; Rogl', P.; Aksel'rud, L.G.; Pecharskij, V.K.; Yarmolyuk, Ya.P.

    1988-01-01

    Synthesis of a new uranium intermetallic compound of U 2 RuGa 8 composition was conducted. The compound crystallizes in Ho 2 CoGa 8 structural type, met earlier only in compounds of rare earths. Magnetic susceptibility of the compound is rather high and is practically independent of temperature in 80-300 K range. This feature is typical for paramagnetism of electron gas and testifies to the absence of localized magnetic moments on ruthenium and uranium atoms

  19. Synthesis, thermal behavior and thermoelectric properties of disordered tellurides with structures derived from the rocksalt type

    Energy Technology Data Exchange (ETDEWEB)

    Schroeder, Thorsten

    2014-06-17

    GeBi{sub 2}Te{sub 4} is proposed as phase-change material. Nanostructures in metastable GeBi{sub 2}Te{sub 4} were obtained by high-pressure synthesis and thermal quenching, - depending on temperature and pressure different modifications were found. The differences in the electrical characteristics can be attributed to the variation of grain boundary concentration and the grain size distribution. Two synthesis approaches were used to prepare Ag{sub 3.4}In{sub 3.7}Sb{sub 76.4}Te{sub 16.5} bulk samples and studied with respect to their transport and thermal properties. A high pressure route to prepare thermoelectrics with low thermal conductivity was developed for AgIn{sub x}Sb{sub 1-x}Te{sub 2}. Disorder and and transport studies on In{sub 3}SbTe{sub 2} were performed using X-ray, neutron and electron diffraction measurements. Nanostructures in Te/Sb/Ge/Ag (TAGS) thermoelectric materials were induced by phase transitions associated with vacancy ordering. Further studies concerned solid solution series (GeTe){sub x}(LiSbTe{sub 2}){sub 2} (1 smaller or equal x smaller or equal 11) and their thermoelectric properties.

  20. Molybdenum Nitride Films: Crystal Structures, Synthesis, Mechanical, Electrical and Some Other Properties

    Directory of Open Access Journals (Sweden)

    Isabelle Jauberteau

    2015-10-01

    Full Text Available Among transition metal nitrides, molybdenum nitrides have been much less studied even though their mechanical properties as well as their electrical and catalytic properties make them very attractive for many applications. The δ-MoN phase of hexagonal structure is a potential candidate for an ultra-incompressible and hard material and can be compared with c-BN and diamond. The predicted superconducting temperature of the metastable MoN phase of NaCl-B1-type cubic structure is the highest of all refractory carbides and nitrides. The composition of molybdenum nitride films as well as the structures and properties depend on the parameters of the process used to deposit the films. They are also strongly correlated to the electronic structure and chemical bonding. An unusual mixture of metallic, covalent and ionic bonding is found in the stoichiometric compounds.

  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. Mesoporous silicas with covalently immobilized β-cyclodextrin moieties: synthesis, structure, and sorption properties

    Science.gov (United States)

    Roik, Nadiia V.; Belyakova, Lyudmila A.; Trofymchuk, Iryna M.; Dziazko, Marina O.; Oranska, Olena I.

    2017-09-01

    Mesoporous silicas with chemically attached macrocyclic moieties were successfully prepared by sol-gel condensation of tetraethyl orthosilicate and β-cyclodextrin-silane in the presence of a structure-directing agent. Introduction of β-cyclodextrin groups into the silica framework was confirmed by the results of IR spectral, thermogravimetric, and quantitative chemical analysis of surface compounds. The porous structure of the obtained materials was characterized by nitrogen adsorption-desorption measurements, powder X-ray diffraction, transmission electron microscopy, and dynamic light scattering. It was found that the composition of the reaction mixture used in β-cyclodextrin-silane synthesis significantly affects the structural parameters of the resulting silicas. The increase in (3-aminopropyl)triethoxysilane as well as the coupling agent content in relation to β-cyclodextrin leads ultimately to the lowering or complete loss of hexagonal arrangement of pore channels in the synthesized materials. Formation of hexagonally ordered mesoporous structure was observed at molar composition of the mixture 0.049 TEOS:0.001 β-CD-silane:0.007 CTMAB:0.27 NH4OH:7.2 H2O and equimolar ratio of components in β-CD-silane synthesis. The sorption of alizarin yellow on starting silica and synthesized materials with chemically attached β-cyclodextrin moieties was studied in phosphate buffer solutions with pH 7.0. Experimental results of the dye equilibrium sorption were analyzed using Langmuir, Freundlich, and Redlich-Peterson isotherm models. It was proved that the Redlich-Peterson isotherm model is the most appropriate for fitting the equilibrium sorption of alizarin yellow on parent silica with hexagonally arranged mesoporous structure as well as on modified one with chemically immobilized β-cyclodextrin groups. [Figure not available: see fulltext.

  3. Template-free synthesis of sub-micrometric cobalt fibers with controlled shape and structure. Characterization and magnetic properties

    Energy Technology Data Exchange (ETDEWEB)

    Lakhdar, Allagui [Laboratoire de Physique des Matériaux Lamellaires et Nano-Matériaux Hybrides, Faculté des Sciences de Bizerte, Université de Carthage, 7021 Bizerte (Tunisia); Borges, Joao P. [i3N/CENIMAT, Department of Materials Science, Faculty of Science and Technology, Universidade NOVA de Lisboa, Campus de Caparica, 2829-516 Caparica (Portugal); Ben Haj Amara, Abdesslam [Laboratoire de Physique des Matériaux Lamellaires et Nano-Matériaux Hybrides, Faculté des Sciences de Bizerte, Université de Carthage, 7021 Bizerte (Tunisia); Dakhlaoui-Omrani, Amel, E-mail: dakhlaoui_amel@yahoo.fr [Department of Chemistry, Faculty of Sciences and Arts-Khulais, University of Jeddah, Khulais, P. O. Box 355, Postal Code 21921 (Saudi Arabia); Laboratoire de Physico-Chimie des Matériaux Minéraux et leurs Applications, Centre National des Recherches en Sciences des Matériaux, Technopôle de Bordj Cedria, BP 73, 8027 Soliman (Tunisia)

    2017-03-01

    Sub-micrometric Co fibers were prepared via a modified polyol process at 90 °C under an external magnetic field of about 550 Oe, using ethelyne glycol as solvent and hydrazine as reducing agent. The structure, the size and the morphology of the as-elaborated products were highly controlled through properly monitoring the synthesis parameters (amount of NaOH added, the amount of the reducing agent, precursor’ concentration and precursors mixing protocol). The XRD characterization confirmed the formation of pure cobalt powders with either hexagonal compact (hcp) or face-centered-cubic (fcc) structure depending on the concentration of the metal precursor and sodium hydroxide. The scanning electron microscopy observations of the powders shows sub-micrometric fibers with about 0.4–0.6 µm in diameter and a length that could reach 15 µm. Fibers prepared at high reducing ratio were constituted of flower-like spheres that coalesce in the direction of the applied magnetic field. For their high contact surface, these fibers offer new opportunities for catalysis applications. The hysteresis loop measurements show an enhancement of the Hc of the as-obtained fibers compared to their bulk counterparts and permit to confirm the relationship between the structure and the magnetic properties of the materials. - Highlights: • Template free synthesis of cobalt sub-micrometric fibers. • High control of the structure the structure, the size and the morphology of the products through properly monitoring the synthesis parameters. • cobalt sub-micrometric fibers with enhanced magnetic properties compared to bulk cobalt.

  4. Synthesis, quantitative structure-property relationship study of novel fluorescence active 2-pyrazolines and application

    Science.gov (United States)

    Girgis, Adel S.; Basta, Altaf H.; El-Saied, Houssni; Mohamed, Mohamed A.; Bedair, Ahmad H.; Salim, Ahmad S.

    2018-03-01

    A variety of fluorescence-active fluorinated pyrazolines 13-33 was synthesized in good yields through cyclocondensation reaction of propenones 1-9 with aryl hydrazines 10-12. Some of the synthesized compounds provided promising fluorescence properties with quantum yield (Φ) higher than that of quinine sulfate (standard reference). Quantitative structure-property relationship studies were undertaken supporting the exhibited fluorescence properties and estimating the parameters governing properties. Five synthesized fluorescence-active pyrazolines (13, 15, 18, 19 and 23) with variable Φ were selected for treating two types of paper sheets (Fabriano and Bible paper). These investigated fluorescence compounds, especially compounds 19 and 23, provide improvements in strength properties of paper sheets. Based on the observed performance they can be used as markers in security documents.

  5. SnSe Nanocrystals: Synthesis, Structure, Optical Properties, and Surface Chemistry

    KAUST Repository

    Baumgardner, William J.; Choi, Joshua J.; Lim, Yee-Fun; Hanrath, Tobias

    2010-01-01

    The colloidal synthesis of SnSe nanoparticles is accomplished through the injection of bis[bis(trimethylsilyl)amino]tin(II) into hot trioctylphosphine: selenium in the presence of oleylamine. Through the manipulation of reaction temperature particles are grown with the average diameter reliably tuned to 4-10 nm. Quantum confinement is examined by establishing a relationship between particle size and band gap while the in depth growth dynamics are illuminated through UV-vis-NIR spectroscopy. Surface chemistry effects are explored, including the demonstration of useful ligand exchanges and the development of routes toward anisotropic particle growth. Finally, transient current-voltage properties of SnSe nanocrystal films in the dark and light are examined. © 2010 American Chemical Society.

  6. SnSe Nanocrystals: Synthesis, Structure, Optical Properties, and Surface Chemistry

    KAUST Repository

    Baumgardner, William J.

    2010-07-21

    The colloidal synthesis of SnSe nanoparticles is accomplished through the injection of bis[bis(trimethylsilyl)amino]tin(II) into hot trioctylphosphine: selenium in the presence of oleylamine. Through the manipulation of reaction temperature particles are grown with the average diameter reliably tuned to 4-10 nm. Quantum confinement is examined by establishing a relationship between particle size and band gap while the in depth growth dynamics are illuminated through UV-vis-NIR spectroscopy. Surface chemistry effects are explored, including the demonstration of useful ligand exchanges and the development of routes toward anisotropic particle growth. Finally, transient current-voltage properties of SnSe nanocrystal films in the dark and light are examined. © 2010 American Chemical Society.

  7. Synthesis, structural studies and biological properties of new TBA analogues containing an acyclic nucleotide.

    Science.gov (United States)

    Coppola, Teresa; Varra, Michela; Oliviero, Giorgia; Galeone, Aldo; D'Isa, Giuliana; Mayol, Luciano; Morelli, Elena; Bucci, Maria-Rosaria; Vellecco, Valentina; Cirino, Giuseppe; Borbone, Nicola

    2008-09-01

    A new modified acyclic nucleoside, namely N(1)-(3-hydroxy-2-hydroxymethyl-2-methylpropyl)-thymidine, was synthesized and transformed into a building block useful for oligonucleotide (ON) automated synthesis. A series of modified thrombin binding aptamers (TBAs) in which the new acyclic nucleoside replaces, one at the time, the thymidine residues were then synthesized and characterized by UV, CD, MS, and (1)H NMR. The biological activity of the resulting TBAs was tested by Prothrombin Time assay (PT assay) and by purified fibrinogen clotting assay. From a structural point of view, nearly all the new TBA analogues show a similar behavior as the unmodified counterpart, being able to fold into a bimolecular or monomolecular quadruplex structure depending on the nature of monovalent cations (sodium or potassium) coordinated in the quadruplex core. From the comparison of structural and biological data, some important structure-activity relationships emerged, particularly when the modification involved the TT loops. In agreement with previous studies we found that the folding ability of TBA analogues is more affected by modifications involving positions 4 and 13, rather than positions 3 and 12. On the other hand, the highest anti-thrombin activities were detected for aptamers containing the modification at T13 or T12 positions, thus indicating that the effects produced by the introduction of the acyclic nucleoside on the biological activity are not tightly connected with structure stabilities. It is noteworthy that the modification at T7 produces an ON being more stable and active than the natural TBA.

  8. Crystal Engineering: Synthesis and Structural Analysis of Coordination Polymers with Wavelike Properties

    Directory of Open Access Journals (Sweden)

    Matasebia T. Munie

    2011-10-01

    Full Text Available Supramolecular coordination polymers with wavelike structures have been synthesized by self-assembly and their structures analyzed using the sine trigonometric function. Slow evaporation of a methylene chloride-methanol solution of a 1:1 molar mixture of [M(tmhd2], where M = Co or Ni, and quinoxaline; a 1:2:1 molar mixture of [M(acac2], where M = Co or Ni, 2,2,6,6-tetramethyl-3,5-heptadione and quinoxaline; or a 1:2:1 molar mixture of [Co(acac2], dibenzoylmethane, and quinoxaline, yielded the crystalline coordination polymers. In the presence of the nitrogenous base, ligand scrambling occurs yielding the most insoluble product. The synthesis and structures of the following wavelike polymers are reported: trans-[Co(DBM2(qox]n·nH2O (2, trans-[Co(tmhd2(qox]n (3, trans-[Ni(tmhd2(qox]n (4, where DBM− = dibenzoylmethanate, tmhd− = 2,2,6,6-tetramethyl-3,5-heptadionate, and qox = quinoxaline. The wavelike structures are generated by intramolecular steric interactions and crystal packing forces between the chains. Some of the tert-butyl groups show a two-fold disorder. The sine function, φ = A sin 2πx/λ, where φ = distance (Ǻ along the polymer backbone, λ = wavelength (Ǻ, A = amplitude (Ǻ, x = distance (Ǻ along the polymer axis, provides a method to approximate and visualize the polymer structures.

  9. Synthesis, structure and photoluminescence properties of amine-templated open-framework bismuth sulfates

    International Nuclear Information System (INIS)

    Marri, Subba R.; Behera, J.N.

    2014-01-01

    Two organically-templated bismuth sulfates of the compositions, [C 6 N 2 H 14 ] [Bi(SO 4 ) 2 (NO 3 )], (1) and [C 4 N 2 H 12 ] 4 [Bi 4 (SO 4 ) 10 (H 2 O) 4 ], (2), with open architecture have been synthesized and their structures determined by single crystal X-ray diffraction. 1 has a corrugated layered structure with 8-membered aperture wherein the SO 4 tetrahedra and the BiO 8 polyhedra join together to form (4, 4) net sheets of the metal centers while 2 has a three-dimensional structure possessing 8- and 12-membered channels. Both the compounds show good fluorescence properties exhibiting blue luminescence. Time-resolved fluorescence behavior of 1 and 2 shows mean fluorescence life time of 0.9 and 1.0 ns, respectively. - Graphical abstract: Two open-framework bismuth sulfates with the layered and three-dimensional structures have been synthesized and characterized. Both the compounds show good fluorescence properties exhibiting blue luminescence. Display Omitted - Highlights: • Two organically-templated bismuth sulfates with open architecture have been synthesized and characterized. • One has a corrugated layered structure while the other one has a three-dimensional structure possessing channels. • They are novel in that open-framework three-dimensional main group metal sulfates are first to be reported. • They show good fluorescence properties exhibiting blue luminescence

  10. Novel polymeric potassium complex: Its synthesis, structural characterization, photoluminescence and electrochemical properties

    Energy Technology Data Exchange (ETDEWEB)

    Ceyhan, Goekhan [Chemistry Department, K.Maras Suetcue Imam University, 46100 K.Maras (Turkey); Tuemer, Mehmet, E-mail: mtumer@ksu.edu.tr [Chemistry Department, K.Maras Suetcue Imam University, 46100 K.Maras (Turkey); Koese, Muhammet; McKee, Vickie [Chemistry Department, Loughborough University, LE11 3TU Leicestershire (United Kingdom)

    2012-03-15

    In this paper, we obtained a novel poly(vanillinato potassium) complex (PVP) as a single crystal and characterized by analytical and spectroscopic methods. A single crystal of the PVP was obtained from the acetone solution. X-ray structural data show that crystals contain polymeric K{sup +} complex of vanillin. Each potassium ion in the polymeric structure is identical and seven-coordinate, bonded to two methoxy, two phenoxy and three aldehyde oxygen atoms from four vaniline molecules. Two aldehyde oxygen atoms are bridging between potassium ions. It crystallizes in the monoclinic system, space group P2{sub 1}/c, with lattice parameters a=9.6215(10) A, b=17.4139(19) A, c=9.6119(10) A, {beta}=100.457(2) Degree-Sign and Z=4. Thermal properties of the PVP were investigated by TGA, DTA and DSC methods. The electrochemical properties of the complex were studied in different solvents and at various scan rates. The luminescence properties of the complex in different solvents and at different pH values have been investigated. The results show that the complex exhibits more efficient luminescence property in CH{sub 3}CN and n-butanol. - Highlights: Black-Right-Pointing-Pointer Novel polymeric potassium complex was prepared and fully characterized. Black-Right-Pointing-Pointer X-ray crystal structure of complex was reported. Black-Right-Pointing-Pointer Electrochemical properties of compound were investigated. Black-Right-Pointing-Pointer Thermal and DSC measurements of complex were examined.

  11. Structure and fertilizer properties of byproducts formed in the synthesis of EDDHA.

    Science.gov (United States)

    Hernández-Apaolaza, Lourdes; García-Marco, Sonia; Nadal, Paloma; Lucena, Juan J; Sierra, Miguel A; Gómez-Gallego, Mar; Ramírez-López, Pedro; Escudero, Rosa

    2006-06-14

    The synthesis of commercial EDDHA produces o,o-EDDHA as the main reaction product, together with a mixture of regioisomers (o,p-EDDHA and p,p-EDDHA) and other unknown byproducts also able to complex Fe3+. These compounds have been obtained by direct synthesis, and their structures have been determined by ESI-MS analysis as oligomeric EDDHA-like products, formed by polysubstitution in the phenolic rings. Short-term experiments show that the iron complexes of samples enriched in these oligomeric byproducts have adequate stability in solution, but a significant amount of them is lost after interaction with soils and soil materials. Mildly chlorotic cucumber plants are able to reduce iron better from o,p-EDDHA/Fe3+ than from the iron complexes of the oligomeric byproducts. In hydroponics, the chlorotic soybean susceptible plants have a lower potential for Fe absorption from these byproducts than from o,o-EDDHA/Fe3+ and from o,p-EDDHA/Fe3+. In the studied conditions, the iron chelates of EDDHA byproducts do not have the long-lasting effect shown by o,o-EDDHA/Fe3+ and present a less efficient fast-action effect than the o,p-EDDHA/Fe3+.

  12. The effect of CNTs on structures and catalytic properties of AuPd clusters for H2O2 synthesis.

    Science.gov (United States)

    Yang, Hua-feng; Xie, Peng-yang; Yu, Hui-you; Li, Xiao-nian; Wang, Jian-guo

    2012-12-28

    The structures and catalytic properties of AuPd clusters supported on carbon nanotubes (CNTs) for H(2)O(2) synthesis have been investigated by means of density functional theory calculations. Firstly, the structures of AuPd clusters are strongly influenced by CNTs, in which the bottom layers are mainly composed of Pd and the top layers are a mix of Au and Pd due to the stronger binding of Pd than Au on CNTs. Especially, it is found that O(2) adsorption on the Pd/CNTs interfacial sites is much weaker than that on the only Pd sites, which is in contrast to transition metal oxide (for example TiO(2), Al(2)O(3), CeO(2)) supported metal clusters. Furthermore, Pd ensembles on the interfacial sites have far superior catalytic properties for H(2)O(2) formation than those away from CNT supports due to the changes in electronic structures caused by the CNTs. Therefore, our study provides a physical insight into the enhanced role of carbon supports in H(2)O(2) synthesis over supported AuPd catalysts.

  13. Ibuprofen: Synthesis, production and properties

    Directory of Open Access Journals (Sweden)

    Mijin Dušan Ž.

    2003-01-01

    Full Text Available Since its introduction in 1969, ibuprofen has become one of the most common painkillers in the world. Ibuprofen in an NSAID (non-steroidal anti-inflammatory drug and like other drugs of its class it possesses analgetic, antipyretic and anti-inflammatory properties. While ibuprofen is a relatively simple molecule, there is still sufficient structural complexity to ensure that a large number of different synthetic approaches are possible. Since the introduction of pharmaceutical products containing ibuprofen, industrial and academic scientists have developed many potential production processes. This paper describes the history, synthesis and production, as well as the properties and stability of ibuprofen.

  14. Structured mesoporous Mn, Fe, and Co oxides: Synthesis, physicochemical, and catalytic properties

    Science.gov (United States)

    Maerle, A. A.; Karakulina, A. A.; Rodionova, L. I.; Moskovskaya, I. F.; Dobryakova, I. V.; Egorov, A. V.; Romanovskii, B. V.

    2014-02-01

    Structured mesoporous Mn, Fe, and Co oxides are synthesized using "soft" and "hard" templates; the resulting materials are characterized by XRD, SEM, TEM, BET, and TG. It is shown that in the first case, the oxides have high surface areas of up to 450 m2/g that are preserved after calcination of the material up to 300°C. Even though, the surface area of the oxides prepared by the "hard-template" method does not exceed 100 m2/g; it is, however, thermally stable up to 500°C. Catalytic activity of mesoporous oxides in methanol conversion was found to depend on both the nature of the transition metal and the type of template used in synthesis.

  15. Synthesis, structure and luminescence properties of lanthanide complex with a new tetrapodal ligand featuring salicylamide arms

    International Nuclear Information System (INIS)

    Song Xueqin; Wen Xiaoguang; Liu Weisheng; Wang Daqi

    2010-01-01

    A new tetrapodal ligand 1,1,1-tetrakis{[(2'-(2-furfurylaminoformyl))phenoxyl]methyl}methane (L) has been prepared and their coordination chemistry with Ln III ions has been investigated. The structure of {[Ln 4 L 3 (NO 3 ) 12 ].H 2 O} ∞ (Ln=Nd, Eu)] shows the binodal 4,3-connected three-dimensional interpenetration coordination polymers with topology of a (8 6 ) 3 (8 3 ) 4 notation. [DyL(NO 3 ) 3 (H 2 O) 2 ].0.5CH 3 OH and [ErL(NO 3 ) 3 (H 2 O) (CH 3 OH)].CH 3 COCH 3 is a 1:1 mononuclear complex with interesting supramolecular features. The structure of [NdL(H 2 O) 6 ].3ClO 4 .3H 2 O is a 2:1 mononuclear complex which further self-assembled through hydrogen bond to form a three-dimensional supramolecular structures. The result presented here indicates that both subtle variation of the terminal group and counter anions can be applied in the modulation of the overall molecular structures of lanthanide complex of salicylamide derivatives due to the structure specialties of this type of ligand. The luminescence properties of the Eu III complex are also studied in detail. - Grapical Abstract: We present here a series of zero- to three-dimensional lanthanide coordination structures and luminescence properties of Eu(III) complex of a new tetrapodal ligand.

  16. Thorium/uranium mixed oxide nano-crystals: Synthesis, structural characterization and magnetic properties

    International Nuclear Information System (INIS)

    Hudry, Damien; Griveau, Jean-Christophe; Apostolidis, Christos; Colineau, Eric; Rasmussen, Gert; Walter, Olaf; Wang, Di; Venkata Sai Kiran Chakravadhaluna; Courtois, Eglantine; Kubel, Christian

    2014-01-01

    One of the primary aims of the actinide community within nano-science is to develop a good understanding similar to what is currently the case for stable elements. As a consequence, efficient, reliable and versatile synthesis techniques dedicated to the formation of new actinide-based nano-objects (e.g., nano-crystals) are necessary. Hence, a 'library' dedicated to the preparation of various actinide based nano-scale building blocks is currently being developed. Nano-scale building blocks with tunable sizes, shapes and compositions are of prime importance. So far, the non-aqueous synthesis method in highly coordinating organic media is the only approach which has demonstrated the capability to provide size and shape control of actinide-based nano-crystals (both for thorium and uranium, and recently extended to neptunium and plutonium). In this paper, we demonstrate that the non-aqueous approach is also well adapted to control the chemical composition of the nano-crystals obtained when mixing two different actinides. Indeed, the controlled hot co-injection of thorium acetylacetonate and uranyl acetate (together with additional capping agents) into benzyl ether can be used to synthesize thorium/uranium mixed oxide nano-crystals covering the full compositional spectrum. Additionally, we found that both size and shape are modified as a function of the thorium/uranium ratio. Finally, the magnetic properties of the different thorium/uranium mixed oxide nano-crystals were investigated. Contrary to several reports, we did not observe any ferromagnetic behavior. As a consequence, ferromagnetism cannot be described as a universal feature of nano-crystals of non-magnetic oxides as recently claimed in the literature. (authors)

  17. Synthesis, structure and photoluminescence properties of amine-templated open-framework bismuth sulfates

    Energy Technology Data Exchange (ETDEWEB)

    Marri, Subba R.; Behera, J.N., E-mail: jnbehera@niser.ac.in

    2014-02-15

    Two organically-templated bismuth sulfates of the compositions, [C{sub 6}N{sub 2}H{sub 14}] [Bi(SO{sub 4}){sub 2}(NO{sub 3})], (1) and [C{sub 4}N{sub 2}H{sub 12}]{sub 4}[Bi{sub 4}(SO{sub 4}){sub 10}(H{sub 2}O){sub 4}], (2), with open architecture have been synthesized and their structures determined by single crystal X-ray diffraction. 1 has a corrugated layered structure with 8-membered aperture wherein the SO{sub 4} tetrahedra and the BiO{sub 8} polyhedra join together to form (4, 4) net sheets of the metal centers while 2 has a three-dimensional structure possessing 8- and 12-membered channels. Both the compounds show good fluorescence properties exhibiting blue luminescence. Time-resolved fluorescence behavior of 1 and 2 shows mean fluorescence life time of 0.9 and 1.0 ns, respectively. - Graphical abstract: Two open-framework bismuth sulfates with the layered and three-dimensional structures have been synthesized and characterized. Both the compounds show good fluorescence properties exhibiting blue luminescence. Display Omitted - Highlights: • Two organically-templated bismuth sulfates with open architecture have been synthesized and characterized. • One has a corrugated layered structure while the other one has a three-dimensional structure possessing channels. • They are novel in that open-framework three-dimensional main group metal sulfates are first to be reported. • They show good fluorescence properties exhibiting blue luminescence.

  18. Fe{sub 3}C/Fe nanoparticles with urea: Synthesis, structure and magnetic properties

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Xiaobai [College of Chemistry, Jilin University, Changchun, 130012 (China); School of Chemical and Pharmaceutical Engineering, Jilin Institute of Chemical Technology, Jilin, 132022 (China); Zhang, Daguang [Department of Orthopaedic Surgery, the First Hospital of Jilin University, Changchun, 130021 China (China); Ren, Xiaozhen; Gao, Jiajia [College of Chemistry, Jilin University, Changchun, 130012 (China); Han, Yu [Department of Chemistry, College of Science, Yanbian University, Yanji, 133002 China (China); Chen, Xiaodong [College of Chemistry, Jilin University, Changchun, 130012 (China); Shi, Zhan [State Key Laboratory of Inorganic Synthesis and Preparative Chemistry, College of Chemistry, Jilin University, Changchun, 130012 (China); Yang, Hua [College of Chemistry, Jilin University, Changchun, 130012 (China)

    2016-12-15

    Fe{sub 3}C/Fe nanocomposites were synthesized by a sol–gel method. Using urea as carbon source and reduce agent in the reaction process. The CTAB works as the surfactant and the bromine contained in CTAB plays a catalytic role. Appropriate choices of the amount of urea and CTAB, reaction temperature and time are very important to obtain high-quality of products. Above 650 °C, the precursor gel turned into the nanocomposites composed of iron carbide and iron. Their structures and magnetic properties are characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), and vibrating sample magnetometry (VSM). The possible formation mechanism of as-prepared nanostructures is discussed. - Highlights: • The Fe{sub 3}C/Fe composites were synthetized by sol–gel method. • Their structure, magnetic properties are researched by XRD, VSM and TEM. • The possible formation mechanisms of the composites is discussed.

  19. Fluorinated arene, imide and unsaturated pyrrolidinone based donor acceptor conjugated polymers: Synthesis, structure-property and device studies

    Science.gov (United States)

    Liyanage, Arawwawala Don Thilanga

    After the discovery of doped polyacetylene, organic semiconductor materials are widely studied as high impending active components in consumer electronics. They have received substantial consideration due to their potential for structural tailoring, low cost, large area and mechanically flexible alternatives to common inorganic semiconductors. To acquire maximum use of these materials, it is essential to get a strong idea about their chemical and physical nature. Material chemist has an enormous role to play in this novel area, including development of efficient synthetic methodologies and control the molecular self-assembly and (opto)-electronic properties. The body of this thesis mainly focuses on the substituent effects: how different substituents affect the (opto)-electronic properties of the donor-acceptor (D-A) conjugated polymers. The main priority goes to understand, how different alkyl substituent effect to the polymer solubility, crystallinity, thermal properties (e.g.: glass transition temperature) and morphological order. Three classes of D-A systems were extensively studied in this work. The second chapter mainly focuses on the synthesis and structure-property study of fluorinated arene (TFB) base polymers. Here we used commercially available 1,4-dibromo-2,3,5,6-tetrafluorobenzene (TFB) as the acceptor material and prepare several polymers using 3,3'-dialkyl(3,3'-R2T2) or 3,3'-dialkoxy bithiophene (3,3'-RO2T2) units as electron donors. A detail study was done using 3,3'-bithiophene donor units incorporating branched alkoxy-functionalities by systematic variation of branching position and chain length. The study allowed disentangling the branching effects on (i) aggregation tendency, intermolecular arrangement, (iii) solid state optical energy gaps, and (iv) electronic properties in an overall consistent picture, which might guide future polymer synthesis towards optimized materials for opto-electronic applications. The third chapter mainly focused on

  20. Synthesis, structure and photoluminescence properties of amine-templated open-framework bismuth sulfates

    Science.gov (United States)

    Marri, Subba R.; Behera, J. N.

    2014-02-01

    Two organically-templated bismuth sulfates of the compositions, [C6N2H14] [Bi(SO4)2(NO3)], (1) and [C4N2H12]4[Bi4(SO4)10(H2O)4], (2), with open architecture have been synthesized and their structures determined by single crystal X-ray diffraction. 1 has a corrugated layered structure with 8-membered aperture wherein the SO4 tetrahedra and the BiO8 polyhedra join together to form (4, 4) net sheets of the metal centers while 2 has a three-dimensional structure possessing 8- and 12-membered channels. Both the compounds show good fluorescence properties exhibiting blue luminescence. Time-resolved fluorescence behavior of 1 and 2 shows mean fluorescence life time of 0.9 and 1.0 ns, respectively.

  1. Nest-like structures of Sr doped Bi2WO6: Synthesis and enhanced photocatalytic properties

    International Nuclear Information System (INIS)

    Liu Ying; Wang Weimin; Fu Zhengyi; Wang Hao; Wang Yucheng; Zhang Jinyong

    2011-01-01

    Highlights: → Bi 2 WO 6 with 3D nest-like structures was obtained without the presence of templates but after Sr-doping, which represents a marked improvement over previous reports. → The products showed enhanced photocatalytic properties over pure Bi 2 WO 6 . → Samples subsequently thermal treated at 500 deg. C show better photocatalytic activities. - Abstract: A series of Sr-doped Bi 2 WO 6 with three-dimensional (3D) nest-like structures were synthesized through simple hydrothermal route and characterized by XRD, FESEM, TEM, XPS, UV-vis DRS, etc. Morphology observation revealed that the as-synthesized Bi 2 WO 6 were self-assembled three-dimensional (3D) nest-like structures, which were constructed from nanoplates. UV-vis diffuse reflectance spectra indicated that the samples had absorption in both UV and visible light areas. Their photocatalytic activities were evaluated by photodegradation of rhodamine B (RhB) under UV and visible light irradiation (λ > 420 nm). The photocatalytic properties were enhanced after Sr doping. Samples subsequently thermal treated at 500 deg. C showed higher photocatalytic activities. The reasons for the differences in the photocatalytic activities of these nest-like Bi 2 WO 6 microstructures were further investigated.

  2. Synthesis, structure and magnetic properties of crystallographically aligned CuCr_2Se_4 thin films

    International Nuclear Information System (INIS)

    Esters, Marco; Liebig, Andreas; Ditto, Jeffrey J.; Falmbigl, Matthias; Albrecht, Manfred; Johnson, David C.

    2016-01-01

    We report the low temperature synthesis of highly textured CuCr_2Se_4 thin films using the modulated elemental reactant (MER) method. The structure of CuCr_2Se_4 is determined for the first time in its thin film form and exhibits cell parameters that are smaller than found in bulk CuCr_2Se_4. X-ray diffraction and precession electron diffraction show a strong degree of crystallographic alignment of the crystallites, where the axis is oriented perpendicular to the substrate surface, while being rotationally disordered within the plane. Temperature and field dependent in-plane and out-of-plane magnetization measurements show that the film is ferromagnetic with a Curie temperature of 406 K CuCr_2Se_4 synthesized utilizing the MER method shows stronger magnetic anisotropy (effective anisotropy: 1.82 × 10"6 erg cm"−"3; shape anisotropy: 1.07 × 10"6 erg cm"−"3), with the easy axis lying out of plane, and a larger magnetic moment (6 μ_B/f.u.) than bulk CuCr_2Se_4. - Highlights: • Crystallographically aligned, phase pure CuCr_2Se_4 were synthesized. • The degree of alignment decreases with annealing time. • The films are ferromagnetic with the easy axis along the direction. • The magnetization is larger than bulk CuCr_2Se_4 or other CuCr_2Se_4 films made to date.

  3. Synthesis, effect of capping agents, structural, optical and photoluminescence properties of ZnO nanoparticles

    International Nuclear Information System (INIS)

    Singh, A.K.; Viswanath, V.; Janu, V.C.

    2009-01-01

    Zinc oxide nanoparticles were synthesized using chemical method in alcohol base. During synthesis three capping agents, i.e. triethanolamine (TEA), oleic acid and thioglycerol, were used and the effect of concentrations was analyzed for their effectiveness in limiting the particle growth. Thermal stability of ZnO nanoparticles prepared using TEA, oleic acid and thioglycerol capping agents, was studied using thermogravimetric analyzer (TGA). ZnO nanoparticles capped with TEA showed maximum weight loss. X-ray diffraction (XRD) and scanning electron microscopy (SEM) were used for structural and morphological characterization of ZnO nanoparticles. Particle size was evaluated using effective mass approximation method from UV-vis spectroscopy and Scherrer's formula from XRD patterns. XRD analysis revealed single crystal ZnO nanoparticles of size 12-20 nm in case of TEA capping. TEA, oleic acid and thioglycerol capped synthesized ZnO nanoparticles were investigated at room temperature photoluminescence for three excitation wavelengths i.e. 304, 322 and 325 nm, showing strong peaks at about 471 nm when excited at 322 and 325 nm whereas strong peak was observed at 411 for 304 nm excitation.

  4. Arene-Inserted Extended Germa[n]pericyclynes: Synthesis, Structure, and Phosphorescence Properties.

    Science.gov (United States)

    Tanimoto, Hiroki; Mori, Junta; Ito, Shunichiro; Nishiyama, Yasuhiro; Morimoto, Tsumoru; Tanaka, Kazuo; Chujo, Yoshiki; Kakiuchi, Kiyomi

    2017-07-26

    This report describes the synthesis and characterization of arene-inserted extended (ArEx) germa[n]pericyclynes composed of germanium and 1,4-diethynylbenzene units. These novel cyclic germanium-π unit materials were synthesized with diethynylbenzene and germanium dichloride. X-ray crystallographic analysis revealed their structures, and the planar conformation of ArEx germa[4]pericyclyne along with the regular aromatic rings. UV/Vis absorption spectra and fluorescence emission spectra showed considerably unique and highly improved character compared to previously reported germa[n]pericyclynes. Even in the absence of transition metal components, phosphorescence emissions were observed, and the emission lifetimes were dramatically improved. ArEx germa[n]pericyclynes showed high photoluminescence quantum yields, whereas low photoluminescence quantum yields were observed for acyclic compounds. Density functional theory calculations show delocalized orbitals between skipped alkyne units through a germanium tether, and an increase in the HOMO energy level, leading to a small HOMO-LUMO energy gap. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  5. New chiral zwitterionic phosphorus heterocycles: synthesis, structure, properties and application as chiral solvating agents.

    Science.gov (United States)

    Sheshenev, Andrey E; Boltukhina, Ekaterina V; Grishina, Anastasiya A; Cisařova, Ivana; Lyapkalo, Ilya M; Hii, King Kuok Mimi

    2013-06-17

    A family of new chiral zwitterionic phosphorus-containing heterocycles (zPHC) have been derived from methylene-bridged bis(imidazolines). These structures were unambiguously determined, including single-crystal XRD analysis for two compounds. The stability, acid/base and electronic properties of these dipolar phosphorus heterocycles were subsequently investigated. zPHCs can be successfully employed as a new class of chiral solvating agents for the enantiodifferentiation of chiral carboxylic and sulfonic acids by NMR spectroscopy. The stoichiometry and binding constants for the donor-acceptor complexes formed were established by NMR titration methods. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  6. Synthesis, molecular structure and magnetic properties of a rhenium(IV) compound with catechol

    Science.gov (United States)

    Cuevas, A.; Geis, L.; Pintos, V.; Chiozzone, R.; Sanchíz, J.; Hummert, M.; Schumann, H.; Kremer, C.

    2009-03-01

    A novel Re(IV) complex containing catechol as ligand has been prepared and characterized. The crystal structure of (HNEt 3)(NBu 4)[ReCl 4(cat)]·H 2cat was determined. The rhenium ion presents a distorted octahedral geometry, being bonded to a bidentate catecholate group and four chloride anions. The magnetic properties of the complex were studied, a /2 D/ (the energy gap between ±3/2 and ±1/2 Kramers doublets) value of 190(10) cm -1. This is the largest /2 D/ value reported for Re(IV) up to now.

  7. Poly(ferrocenyldimethylsilanes) at the interface of chemistry and materials science: synthesis, structure-properties and thin film applications

    NARCIS (Netherlands)

    Lammertink, Rob G.H.

    2000-01-01

    The work described in this thesis concerns the synthesis, characterization, and properties study of ferrocenyldimethylsilane homopolymers and block copolymers. Due to the presence of iron and silicon in the polymer main chain, these macromolecules possess characteristics that are very distinctive

  8. Synthesis, optical properties and growth mechanism of MnO nano structures

    Science.gov (United States)

    Pandey, B. K.; Shahi, A. K.; Gopal, R.

    2013-10-01

    Manganese oxide (MnO) colloidal nanoparticles have been successfully synthesized by pulse laser ablation in double distilled water. Nd: YAG laser with focused output operating at different pulse energies (20, 30, 40, 50 mJ/pulse) was used for ablation. Synthesized MnO nano crystal phase and structure were confirmed by X-ray diffraction and SAED pattern. Optical properties of as synthesized MnO nano colloidal solution were studied by UV-vis absorption spectroscopy. Optical particle size and band gap of as synthesized MnO colloidal nanoparticles were calculated. Particle shape and size were determined by TEM/SEM image. It is observed that MnO nano colloidal particles assembled to make different structures after aging in the liquid media. Aspect ratio has been calculated from SEM picture. MnO nanoparticles show weak antiferromagnetic behavior at room temperature as measured by VSM. A typical mechanism has been proposed for the formation of different nanostructures.

  9. Synthesis, Structure, and Luminescent Properties of Europium-Doped Hydroxyapatite Nanocrystalline Powders

    International Nuclear Information System (INIS)

    Ciobanu, C.S.; Iconaru, S.L.; Predoi, D.; Massuyeau, F.; Constantin, L.V.; Costescu, A.

    2012-01-01

    The luminescent europium-doped hydroxyapatite (Eu:HAp, Ca 10-x Eu x (PO 4 ) 6 (OH) 2 ) with 0>x>0.2 nanocrystalline powders was synthesized by coprecipitation. The structural, morphological, and textural properties were well characterized by X-ray diffraction, scanning electron microscopy, and transmission electron microscopy. The vibrational studies were performed by Fourier transform infrared, Raman, and photoluminescence spectroscopies. The X-ray diffraction analysis revealed that hydroxyapatite is the unique crystalline constituent of all the samples, indicating that Eu has been successfully inserted into the HAp lattice. Eu doping inhibits HAp crystallization, leading to a decrease of the average crystallite size from around 20 nm in the undoped sample to around 7 nm in the sample with the highest Eu concentration. Furthermore, the samples show the characteristic 5 D 0 → 7 F 0 transition observed at 578 nm related to Eu 3+ ions distributed on Ca 2+ sites of the apatitic structure

  10. Synthesis, structure and electrochemical properties of polyaniline/MoO3 nanobelt composite for lithium battery

    International Nuclear Information System (INIS)

    Mohan, Varishetty Madhu; Chen, Wen; Murakami, Kenji

    2013-01-01

    Graphical abstract: Hydrothermal method was introduced for the synthesis of MoO 3 nanobelts and polyaniline (PANI)/MoO 3 nanobelt composites. The structure and morphology of the samples were studied by X-ray diffraction (XRD), Fourier transform infrared radiation (FTIR), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) analysis. We can see the presence of polyaniline on the MoO 3 nanobelts surface in the TEM pictures as shown in Fig. (a). The pure MoO 3 nanobelts exhibit the initial specific capacity 276 mAhg −1 , whereas PANI/MoO 3 nanobelt composite shows little low initially 228 mAhg −1 after that it has more stabilized specific capacity with increasing cycle numbers as shown in Fig. (b). The cyclic voltammograms of the PANI/MoO 3 nanobelt composite show better cyclic performance compared to pure MoO 3 nanobelts. The electrochemical impedance spectres were studied for both the pure and PANI/MoO 3 samples at 2.0 and 3.5 potentials. The role of the PANI polymeric component of the composite material seems to be the stabilization of the specific capacity due to probable homogeneous distribution of the induced stress during cycling. Display Omitted Highlights: ► Hydrothermal synthesis of MoO 3 , PANI/MoO 3 nanobelts. ► Samples were characterised by XRD, FTIR, DSC, SEM, TEM, CV and impedance. ► MoO 3 nanobelts cathode battery shows initial specific capacity 276 mAhg −1 . ► PANI/MoO 3 nanobelts show initial specific capacity 228 mAhg −1 but high stability. ► PANI/MoO 3 sample studies by impedance at the potentials of 2.0 and 3.5 V. -- Abstract: The MoO 3 nanobelts and polyaniline (PANI)/MoO 3 nanobelt composite were synthesized using hydrothermal method. The crystal structure and morphology of the samples were studied by X-ray diffraction (XRD), Fourier transform infrared radiation (FTIR), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Differential scanning calorimetric (DSC) and thermo

  11. Synthesis, structural characterization, and catalytic properties of tungsten-exchanged H-ZSM5

    International Nuclear Information System (INIS)

    Ding, Weiping; Meitzner, George D.; Marler, David O.; Iglesia, Enrique

    2001-01-01

    W-exchanged H-ZSM5 was prepared by sublimation of WCl6 at 673 K followed by hydrolysis of exchanged WClx species at 523 K. D2 exchange with residual OH groups showed that each W initially replaced about two zeolitic protons for W/Al ratios of 0.29 and 0.44, consistent with the formation of (WO2)2+ containing W6+ species bridging two cation exchange sites. As temperatures reached973 K during D2-OH exchange, these species reduced to (WO2)+ with the concurrent formation of one OD group. CH4 conversion turnover rates (per W) and C2-C1 2 selectivities are very similar to those observed on a Mo/H-ZSM5 sample with similar cation exchange level. As in the case of Mo/H-ZSM5, WOx/H-ZSM5 precursors are initially inactive in CH4 reactions, but they activate during induction with the concurrent evolution of CO, H2O, and an excess amount of H2. The reduction and carburization processes occurring during CH4 reactions and the structure of the exchanged WOx precursors was probed using in situ X-ray absorption spectroscopy (XAS). XAS studies confirmed the isolated initial nature of the exchanged WOx precursors after hydrolysis and dehydration and the formation of WCx clusters 0.6 nm in diameter during CH4 reactions at 973 K. The structural and catalytic resemblance between W- and Mo-exchanged H-ZSM5 is not unexpected, in view of chemical similarities between oxides or carbides of Mo and W. The synthesis of exchanged WOx precursors and their subsequent carburization during CH4 reactions, however, are more difficult than the corresponding processes for the MoOx counterparts. This may account for previous reports of lower CH4 reaction rates and aromatics selectivities on W/H-ZSM5 compared with those observed on Mo/H-ZSM5 and with those reported here for rigorously exchanged W/H-ZSM5

  12. Synthesis and properties of ZnFe{sub 2}O{sub 4} replica with biological hierarchical structure

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Hongyan; Guo, Yiping, E-mail: ypguo@sjtu.edu.cn; Zhang, Yangyang; Wu, Fen; Liu, Yun; Zhang, Di, E-mail: zhangdi@sjtu.edu.cn

    2013-09-20

    Highlights: • ZFO replica with hierarchical structure was synthesized from butterfly wings. • Biotemplate has a significant impact on the properties of ZFO material. • Our method opens up new avenues for the synthesis of spinel ferrites. -- Abstract: ZnFe{sub 2}O{sub 4} replica with biological hierarchical structure was synthesized from Papilio paris by a sol–gel method followed by calcination. The crystallographic structure and morphology of the obtained samples were characterized by X-ray diffraction, field-emission scanning electron microscope, and transmittance electron microscope. The results showed that the hierarchical structures were retained in the ZFO replica of spinel structure. The magnetic behavior of such novel products was measured by a vibrating sample magnetometer. A superparamagnetism-like behavior was observed due to nanostructuration size effects. In addition, the ZFO replica with “quasi-honeycomb-like structure” showed a much higher specific capacitance of 279.4 F g{sup −1} at 10 mV s{sup −1} in comparison with ZFO powder of 137.3 F g{sup −1}, attributing to the significantly increased surface area. These results demonstrated that ZFO replica is a promising candidate for novel magnetic devices and supercapacitors.

  13. Synthesis, structure and solvatochromic properties of some novel 5-arylazo-6-hydroxy-4-phenyl-3-cyano-2-pyridone dyes

    Directory of Open Access Journals (Sweden)

    Alimmari Adel

    2012-07-01

    Full Text Available Abstract Background A series of some novel arylazo pyridone dyes was synthesized from the corresponding diazonium salt and 6-hydroxy-4-phenyl-3-cyano-2-pyridone using a classical reaction for the synthesis of the azo compounds. Results The structure of the dyes was confirmed by UV-vis, FT-IR, 1H NMR and 13C NMR spectroscopic techniques and elemental analysis. The solvatochromic behavior of the dyes was evaluated with respect to their visible absorption properties in various solvents. Conclusions The azo-hydrazone tautomeric equilibration was found to depend on the substituents as well as on the solvent. The geometry data of the investigated dyes were obtained using DFT quantum-chemical calculations. The obtained calculational results are in very good agreement with the experimental data.

  14. Synthesis, structure and properties of novel epoxy and rubber-modified epoxy impregnated Y-Ba-Cu-O superconductors

    International Nuclear Information System (INIS)

    Low, I.M.; Lim, F.W.; Chisholm, W.

    1992-01-01

    This paper reports the synthesis, structure and properties of novel YBa 2 Cu 3 O 6+x (123) - polymer composites. The polymers used were epoxy and rubber-modified epoxy resins. Superconducting composites with good strength, toughness, hardness and chemical resistance have been successfully fabricated. The presence of polymer(s) does not appear to affect the superconducting (T c ) of about 90 K. Levitation experiments show that the height (z) of the levitating magnet depends on sample thickness, and mass and pole strength of the magnet. A simple image force model best describes the observed dependence of z on the mass and pole strength. Atomic absorption and pH measurements in the corrosion study show that the polymer coating provides an impermeable barrier to the ingress of solvents and a concomitant resistance to phase decomposition. 12 refs., 2 tabs., 5 figs

  15. A Novel Coordination Polymer Based on Trinuclear Cobalt Building Blocks Cluster: Synthesis, Crystal Structure, and Properties

    Science.gov (United States)

    Lu, J. F.; Tang, Z. H.; Shi, J.; Ge, H. G.; Jiang, M.; Song, J.; Jin, L. X.

    2017-12-01

    The title compound {[Co3(μ3-OH)(μ2-H2O)2(H2O)5(BTC)2] · 6H2O} n (H3BTC is a 1,3,5-benzenetricarboxylic acid) was prepared and characterized by single crystal and powder X-ray diffraction, Fourier transform infrared spectroscopy, thermogravimetric and elemental analyses. The single crystal X-ray diffraction reveals that the title compound consists of 1D infinite zigzag chains which were constructed by trinuclear cobalt cluster and BTC3- ligand. Neighbouring above-mentioned 1D infinite zigzag chains are further linked by intermolecular hydrogen bonding to form a 3D supermolecular structure. In addition, the luminescent properties of the title compound were investigated.

  16. Synthesis and structural, optical and thermal properties of CdS:Zn2+ nanoparticles

    Science.gov (United States)

    Muruganandam, S.; Anbalagan, G.; Murugadoss, G.

    2014-12-01

    Undoped and Zn (1-5, 10 %) -doped CdS nanoparticles were successfully synthesized by chemical method and polyvinylpyrrolidone was used as capping agent. The morphology and crystalline structure of the samples were studied by transmission electron microscopy and X-ray diffraction. The average particle size of the spherical nanoparticles determined by these techniques was of the order of 2.5-6 nm. The functional groups of the capping agent on CdS:Zn2+ surface were identified by FT-IR study. The band gap of the nanoparticles was calculated using UV-visible absorption spectra and the result showed that the band gap values were dramatically blue shifted from the bulk CdS. The optimum concentration of the doping ions was selected through absorption study. Photoluminescence of the CdS:Zn2+ nanoparticle showed strong blue and green emission. The thermal properties of the nanoparticles were analyzed by thermogravimetric-differential thermal analysis.

  17. Synthesis, Crystal Structure and Water Vapor Adsorption Properties of a Porous Supramolecular Architecture

    Directory of Open Access Journals (Sweden)

    Rui Qiao

    2017-10-01

    Full Text Available A new complex, [Cu4(HL4(H2O14] (1, H3L·HCl = 5-((4-carboxypiperidin-1-ylmethylisophthalic acid hydrochloride, has been prepared and characterized by single-crystal X-ray diffraction, elemental analysis, IR spectroscopy and powder X-ray diffraction (PXRD. The result of the X-ray diffraction analysis reveals that the complex crystallizes in monoclinic, space group C2/c and three unique Cu(II atoms that are connected by partially deprotonated HL2− anion to form a cyclic structure. The rich hydrogen bonding and π-π non-covalent packing interactions extend cyclic units into a three-dimensional (3D supramolecular polymer. Moreover, the thermogravimetric (TG analysis and water vapor adsorption property of 1 were also discussed.

  18. Solid-state synthesis, structural and magnetic properties of CoPd films

    Science.gov (United States)

    Myagkov, V. G.; Bykova, L. E.; Zhigalov, V. S.; Tambasov, I. A.; Bondarenko, G. N.; Matsynin, A. A.; Rybakova, A. N.

    2015-05-01

    The results of the investigation of the structural and magnetic properties of CoPd films with equiatomic composition have been presented. The films have been synthesized by vacuum annealing of polycrystalline Pd/Co and epitaxial Pd/α-Co(110) and Pd/β-Co(001) bilayer samples. It has been shown that, for all samples, the annealing to 400°C does not lead to the mixing of layers and the formation of compounds. A further increase in the annealing temperature results in the formation of a disordered CoPd phase at the Pd/Co interface, which is fully completed after annealing at 650°C. The epitaxial relationships between the disordered CoPd phase and the MgO(001) substrate are determined as follows: CoPd(110)<

  19. SYNTHESIS, STRUCTURE AND SPECTRAL PROPERTIES OF POTASSIUMALUMINA- BORATE GLASS WITH NANOCRYSTALS OF MANGANESE FERRITE

    Directory of Open Access Journals (Sweden)

    D. I. Sobolev

    2016-07-01

    Full Text Available Subject of Research.The paper presents research results of optical properties of potassium-alumina-borate glass, activated with ions of iron and manganese. The formation process of nanocrystals of manganese ferrite MnFe2O4 in potassium-alumina-borate glass host was studied. Magneto-optical characteristics were analyzed. Method. The studied glasses were synthesized by the method of charge melting in the crucible. Potassium-alumina-borate glass system was used (K2O-Al2O3-B2O3 proposed by S.A. Stepanov (Vavilov State Institute. Glass system was doped by 3 wt% of Fe2O3 and 2 wt% MnO by weight (composition 1 and 2 wt% Fe2O3 and 1 wt% MnO by weight (composition 2. The glass transition temperature was 430 °C. Segregating of the crystal phase of manganese ferrite MnFe2O4 occurred during heat treatment at 550 °C for 2 hours in a programmable muffle furnace. The absorption spectrum in the wavelength range 200-2000 nm was recorded with Perkin Elmer Lambda 650 and Varian Cary 500 spectrophotometers. The XRD patterns were obtained on Rigaku Ultima IV X-ray diffractometer by copper anode with a wavelength λ (Cu = 0.15418 nm. Magneto-optical Verde constant was measured by the angle of polarization plane rotation of the passing light through the sample when the sample is placed in magnetic field. Main Results. New technological modes of potassium-alumina-borate glass synthesis doped with ions of iron and manganese were developed and studied. It is established that during heat treatment nanocrystals of manganese ferrites are evolved with an average size of 18 nm. These glasses have a Verde constant equal to 0.9 arc.min/(cm·Oe. It is shown that obtained glasses possess high absorbance in ultra-violet and visible light spectrum. Practical Relevance. Proposed and analyzed nanoglass-ceramics could be accepted as a basis for creation of sensing environments for sensors current and magnetic field and for creation of optical isolators based on the Faraday effect.

  20. Synthesis, structure and photochromic properties of a novel 1,6-hexanediamine trimolybdate supramolecular compound

    International Nuclear Information System (INIS)

    Sun Dehui; Zhang Hongjie; Zhang Jilin; Zheng Guoli; Yu Jiangbo; Gao Shuyan

    2007-01-01

    A novel supramolecular compound 1,6-hexanediamine trimolybdate ((C 6 H 18 N 2 )[Mo 3 O 10 ], denoted as HDAMo) has been synthesized by a hydrothermal method and its structure has been characterized by elemental analyses, Fourier transform infrared (FT-IR) spectra, single-crystal X-ray diffraction (XRD) technique. This single crystal compound consists of protonated 1,6-hexanediamine (HDA) cations and polyoxometalate [Mo 3 O 10 ] 2- anions. Its crystal structure belongs to monoclinic system (space group P2 1 /n) with a=7.7508(14), b=11.467(2), c=16.167(3) A, β=92.689(3) o , V=1435.3(5) A 3 , Z=4 and D calc =2.619 g cm -3 . The final statistics based on F 2 are GOF=0.980, R 1 =0.0261 and wR 2 =0.0506 for I>2σ(I). XRD analysis revealed that in the crystal structure of HDAMo, novel infinite [Mo 3 O 10 ] 2- chains parallel to a axis are made up of distorted MoO 6 octahedra connected by corners and edges. The protonated HDA cations occupy channels formed by [Mo 3 O 10 ] 2- chains and exhibit strong hydrogen bond interactions to terminal and bridging oxo groups of the chains. The [Mo 3 O 10 ] 2- chains linked through protonated HAD cations formed a one-dimensional network. The HDAMo compound shows novel photochromic properties, i.e., its color changes from white to reddish brown gradually under UV irradiation. XRD, FT-IR, ESR spectra and XPS are used to investigate the photochromic behavior of the compound. - Graphical abstract: Crystal structure of 1,6-hexanediamine trimolybdate (C 6 H 18 N 2 )[Mo 3 O 10 ] along c-axis. It consists of protonated 1,6-hexanediamine (HDA) and novel infinite chains [Mo 3 O 10 ] 2- . Infinite chains [Mo 3 O 10 ] 2- are made up of distorted MoO 6 octahedron connected by edges and corners and are linked through protonated HDA cations into a one-dimensional network. What is more, the compound displays photochromic properties and may be applied to the field of photosensitive materials

  1. Synthesis, structures and properties of a series of manganese coordination complexes constructed from dicarboxylic fluorene derivatives

    Energy Technology Data Exchange (ETDEWEB)

    Li Xing, E-mail: lixing@nbu.edu.cn [State Key Laboratory Base of Novel Functional Materials and Preparation Science, Faculty of Materials Science and Chemical Engineering, Ningbo University, Ningbo, Zhejiang, 315211 (China); Zhao Xiuhua; Bing Yue; Zha Meiqin; Xie Hongzhen; Guo Zhiyong [State Key Laboratory Base of Novel Functional Materials and Preparation Science, Faculty of Materials Science and Chemical Engineering, Ningbo University, Ningbo, Zhejiang, 315211 (China)

    2013-01-15

    Assembly reactions of 9,9-diethylfluorene-2,7-dicarboxylic acid (H{sub 2}DFDC) and Mn(CH{sub 3}COO){sub 2}{center_dot}4H{sub 2}O or MnCl{sub 2}{center_dot}4H{sub 2}O by tuning of various secondary ligands such as 2,2 Prime -bipyridine (2,2 Prime -bpy), 4,4 Prime -bipyridine (4,4 Prime -bpy) or 1,3-bis(4-pyridyl)propane) (bpp), gave rise to four complexes {l_brace} [Mn{sub 2}(DFDC){sub 2}(DMF){sub 2}]{center_dot}H{sub 2}O{r_brace} {sub n} (1), [Mn(DFDC)(2,2 Prime -bpy)]{sub n} (2), {l_brace} [Mn{sub 2}(DFDC){sub 2}(4,4 Prime -bpy){sub 2}]{center_dot}2CH{sub 3}OH{r_brace} {sub n} (3), and {l_brace} [Mn{sub 4}(DFDC){sub 4}(bpp){sub 2}(CH{sub 3}OH){sub 3} (H{sub 2}O){sub 3}]{center_dot}3(CH{sub 3}OH){center_dot}3(H{sub 2}O){r_brace} {sub n} (4). Single crystal X-ray diffraction analysis reveal that complex 1 is three dimensional structure with rhombic channels filled by guest water molecules; 2 presents a close-packed structure with high thermal stability; 3 exhibits a three dimensional framework with micro-porous channels filled by guest methanol molecules and 4 is a two-dimensional structure. The photoluminescent properties of 1-4 have been studied, respectively, showing that the Mn(II) ions, accessorial organic ligands or crystal structures exert important influences on the photoluminescence emissions of H{sub 2}DFDC ligands. Thermogravimetric analysis show that the complexes have remarkably high thermal stability. Magnetic susceptibility measurements have been finished and discussed for the complexes. - Graphical abstract: Assembly of 9,9-diethylfluorene-2,7-dicarboxylic acid and Mn(II) salts by tuning of various accessorial ligands resulted in four manganese complexes with different topological frameworks. Highlights: Black-Right-Pointing-Pointer Four manganese complexes based on 9,9-diethylfluorene-2,7-dicarboxylic acid were obtained. Black-Right-Pointing-Pointer The complexes were structurally characterized by single-crystal X-ray diffraction. Black

  2. Synthesis and structural, magnetic, thermal, and transport properties of several transition metal oxides and aresnides

    Energy Technology Data Exchange (ETDEWEB)

    Das, Supriyo [Iowa State Univ., Ames, IA (United States)

    2010-01-01

    Oxide compounds containing the transition metal vanadium (V) have attracted a lot of attention in the field of condensed matter physics owing to their exhibition of interesting properties including metal-insulator transitons, structural transitions, ferromagnetic and an- tiferromagnetic orderings, and heavy fermion behavior. Binary vanadium oxides VnO2n-1 where 2 ≤ n ≤ 9 have triclinic structures and exhibit metal-insulator and antiferromagnetic transitions.[1–6] The only exception is V7O13 which remains metallic down to 4 K.[7] The ternary vanadium oxide LiV2O4 has the normal spinel structure, is metallic, does not un- dergo magnetic ordering and exhibits heavy fermion behavior below 10 K.[8] CaV2O4 has an orthorhombic structure[9, 10] with the vanadium spins forming zigzag chains and has been suggested to be a model system to study the gapless chiral phase.[11, 12] These provide great motivation for further investigation of some known vanadium compounds as well as to ex- plore new vanadium compounds in search of new physics. This thesis consists, in part, of experimental studies involving sample preparation and magnetic, transport, thermal, and x- ray measurements on some strongly correlated eletron systems containing the transition metal vanadium. The compounds studied are LiV2O4, YV4O8, and YbV4O8. The recent discovery of superconductivity in RFeAsO1-xFx (R = La, Ce, Pr, Gd, Tb, Dy, Sm, and Nd), and AFe2As2 (A = Ba, Sr, Ca, and Eu) doped with K, Na, or Cs at the A site with relatively high Tc has sparked tremendous activities in the condensed matter physics community and a renewed interest in the area of superconductivity as occurred following the discovery of the layered cuprate high Tc superconductors in 1986. To discover more supercon- ductors

  3. Synthesis, electrochemistry, STM investigation of oligothiophene self-assemblies with superior structural order and electronic properties

    Energy Technology Data Exchange (ETDEWEB)

    Kuo, Cheng-Yu [C-PCS, Chemistry Division, Los Alamos National Laboratory, Los Alamos, NM 87545 (United States); Liu, Yinghao; Yarotski, Dmitry [Center of Integrated Nanotechnologies, Materials Physics and Application Division, Los Alamos National Laboratory, Los Alamos, NM 87545 (United States); Li, Hao [Theory Division, Los Alamos National Laboratory, Los Alamos, NM 87545 (United States); Xu, Ping; Yen, Hung-Ju [C-PCS, Chemistry Division, Los Alamos National Laboratory, Los Alamos, NM 87545 (United States); Tretiak, Sergei, E-mail: serg@lanl.gov [Theory Division, Los Alamos National Laboratory, Los Alamos, NM 87545 (United States); Wang, Hsing-Lin, E-mail: hwang@lanl.gov [C-PCS, Chemistry Division, Los Alamos National Laboratory, Los Alamos, NM 87545 (United States)

    2016-12-20

    validated by our computational results suggesting different interaction patterns of oligothiophenes with odd numbered and even numbered thiophene repeat units placed in a dimer configuration. Observed correlations between oligomer geometry and structural order of monolayer assembly elucidate important structure–property relationships and have implications for these molecular structures in organic optoelectronic devices and energy devices.

  4. Synthesis and ferroelectric properties of rare earth compounds with tungsten bronze-type structure

    Energy Technology Data Exchange (ETDEWEB)

    Bouziane, M., E-mail: bouzianemeryem@yahoo.fr [Laboratoire de Chimie du Solide Appliquee, Faculte des Sciences, Avenue Ibn Batouta, BP 1014, Rabat (Morocco); Taibi, M. [Laboratoire de Physico-Chimie des Materiaux, LAF 502, Ecole Normale Superieure, BP 5118, Rabat (Morocco); Boukhari, A. [Laboratoire de Chimie du Solide Appliquee, Faculte des Sciences, Avenue Ibn Batouta, BP 1014, Rabat (Morocco)

    2011-10-03

    Highlights: {center_dot} Polycrystalline materials with the tungsten bronze-type structure have been synthesized and characterized. {center_dot} Effect of the incorporation of rare earth ions and paramagnetic cations (Fe{sup 3+}) into a matrix ferroelectrically active was studied. {center_dot} Ferroelectric transition is pronounced by a large thermal hysteresis during the heating and cooling cycles. {center_dot} Phase transitions around T{sub c} were confirmed by differential scanning calorimetry (DSC) measurements. - Abstract: Polycrystalline materials with a general formula Pb{sub 2}Na{sub 0.8}R{sub 0.2}Nb{sub 4.8}Fe{sub 0.2}O{sub 15} (R = Dy, Eu, Sm, Nd, La) have been synthesized, in air by a high temperature solid state reaction method. X-ray diffraction study, at room temperature, revealed that they crystallize in the tungsten bronze-type structure. Dielectric properties were performed, in the temperature range 25-500 deg. C, at three different frequencies 10, 100 and 1000 kHz. The ferroelectric transition is pronounced by a large thermal hysteresis during the heating and cooling cycles. The determined Curie temperature values T{sub c} were discussed as a function of rare earth size. Phase transitions around T{sub c} for the investigated compounds were confirmed by differential scanning calorimetry (DSC) measurements.

  5. Synthesis, structure and some properties of a manganese(II) benzoate containing diimine

    Science.gov (United States)

    Paul, Pranajit; Roy, Subhadip; Sarkar, Sanjoy; Chowdhury, Shubhamoy; Purkayastha, R. N. Dutta; Raghavaiah, Pallepogu; McArdle, Patrick; Deb, Lokesh; Devi, Sarangthem Indira

    2015-12-01

    A new monomeric manganese(II) benzoate complex containing nitrogen donor 2,2‧-bipyridine, [Mn(OBz)2(bipy)(H2O)] (OBz = benzoate, bipy = 2,2‧-bipyridine) has been synthesized from aqueous methanol medium and characterized by analytical, spectroscopic and single crystal X-ray diffraction studies. The compound exhibits moderate to appreciable antimicrobial activity. The complex crystallizes in space group P21/n. Mn(II) atom is ligated by two N atoms of bipyridine, three O atoms from a monodentate and a bidentate benzoate ligand and a water molecule forming distorted octahedral structure. The coordinated water molecule forms intramolecular hydrogen bonds and links the monomer molecules into hydrogen bonded dimer. The hydrogen bonded dimers are involved in intermolecular C-H···O and π-π stacking interactions. Density functional theory (DFT) computation was carried out to compute the frequencies of relevant vibrational modes and electronic properties, the results are in compliance with the experimentally obtained structural and spectral data.

  6. Synthesis, Structure, and Luminescent Properties of Europium-Doped Hydroxyapatite Nanocrystalline Powders

    Directory of Open Access Journals (Sweden)

    Carmen Steluta Ciobanu

    2012-01-01

    Full Text Available The luminescent europium-doped hydroxyapatite (Eu:HAp, Ca10−xEux(PO46(OH2 with 0≤x≤0.2 nanocrystalline powders was synthesized by coprecipitation. The structural, morphological, and textural properties were well characterized by X-ray diffraction, scanning electron microscopy, and transmission electron microscopy. The vibrational studies were performed by Fourier transform infrared, Raman, and photoluminescence spectroscopies. The X-ray diffraction analysis revealed that hydroxyapatite is the unique crystalline constituent of all the samples, indicating that Eu has been successfully inserted into the HAp lattice. Eu doping inhibits HAp crystallization, leading to a decrease of the average crystallite size from around 20 nm in the undoped sample to around 7 nm in the sample with the highest Eu concentration. Furthermore, the samples show the characteristic 5D0→7F0 transition observed at 578 nm related to Eu3+ ions distributed on Ca2+ sites of the apatitic structure.

  7. New metal-organic complexes based on bis(tetrazole) ligands: Synthesis, structures and properties

    Science.gov (United States)

    Du, Ceng-Ceng; Fan, Jian-Zhong; Wang, Xin-Fang; Zhou, Sheng-Bin; Wang, Duo-Zhi

    2017-04-01

    In this paper, a series of new complexes, [Zn2(HL1)2(H2O)4]·H2O (1), [Co2(HL1)2]·TEA (2), [Co3(HL1)2(H2L1)2(H2O)4]n (3), [Cu(HL1)(H2O)2]n (4), {[Cu5(HL2)2(OH)4(ClO4)2]·4H2O}n (5) and [Cu2(L3)]n (6) were successfully prepared by utilizing three bis(tetrazole) ligands [bis-(1H-tetrazol-5-ylmethyl)-amine (H3L1), bis-(1H-tetrazol-5-ylethyl)-amine (H3L2) and 1,5-bis(5-tetrazolo)-3-thiapentane (H2L3)], all of which have been characterized by elemental analyses, FT-IR spectroscopy, powder X-ray diffraction (PXRD), thermogravimetric analyses as well as single-crystal X-ray diffraction analyses showing different dimensionalities (0D, 1D and 3D). Complexes 1 and 2 are 0D structures, 1 shows a dinuclear structure, 2 displays two crystallographically different mononuclear structures, 1 and 2 are further assembled to form 3D supramolecular framework and 2D supramolecular network by hydrogen-bonding interactions, respectively. Complexes 3, 4 and 5 are 1D structures, 3 features a mononuclear unit and a 1D chain, which are arranged into 3D supramolecular architecture by hydrogen-bonding interactions, 4 presents a zigzag chain, 5 shows an infinite chain structure constructed from pentanuclear Cu(II) subunits and ClO4- anions. Complex 6 exhibits a 3D coordination framework based on cyclic [Cu4(L3)2] dimmer subunits as nodes possessing an 8-connected network topology with the point symbol {424·64}. Further, semiconductor behaviors, the solid-state luminescent properties of the complexes 1-3 and 6 were measured and studied seriously at room temperature.

  8. Synthesis, structure and thermoelectric properties of La1-xNaxCoO3 ...

    Indian Academy of Sciences (India)

    29

    system. Here we report the synthesis of Na+-ions doped LaCoO3 samples by the nitrate-citrate ... product retains uniform cation distribution even at low concentrations. .... through the clamping blocks and the voltage drop is measured by the Pt ...

  9. Synthesis, structure and optical properties of single-crystalline In{sub 2}O{sub 3} nanowires

    Energy Technology Data Exchange (ETDEWEB)

    Hadia, N.M.A., E-mail: nomery_abass@yahoo.com [Physics Department, Faculty of Science, Sohag University, 82524 Sohag (Egypt); Mohamed, H.A. [Physics Department, Faculty of Science, Sohag University, 82524 Sohag (Egypt); King Saud University, Teachers College, Science Department (Physics), 11148 Riyadh (Saudi Arabia)

    2013-01-15

    Highlights: Black-Right-Pointing-Pointer Metal and metal oxide one dimensional (1D) nanostructured materials are of crucial importance. Black-Right-Pointing-Pointer The paper deals with the synthesis of In{sub 2}O{sub 3} nanowires without the use of catalysts. Black-Right-Pointing-Pointer The optical constants and Photoluminescence (PL) of In{sub 2}O{sub 3} nanowires were evaluated. - Abstract: Indium oxide In{sub 2}O{sub 3} nanowires have been recently synthesized revealing interesting properties and used in various applications. In order to reduce as much as possible the influence of undesired dopants and/or impurities on the observed properties, In{sub 2}O{sub 3} nanowires have been grown without the use of catalysts, directly from metallic indium by a vapor transport technique and a controlled oxidation with oxygen-argon mixtures. Depending on the growth conditions (temperature, vapor pressure, oxygen concentration, etc.) different results have been achieved and it has been observed that a 'proper' In condensation on the substrates may enhance the nanowires growth. Detailed structural analysis showed that the In{sub 2}O{sub 3} nanostructures are single crystalline with a cubic crystal structure. The grown In{sub 2}O{sub 3} nanowires were optically characterized in order to evaluate the absorption coefficient, optical band gap, refractive index and extinction coefficient. Room temperature Photoluminescence (PL) spectrum showed broad and intense blue emission at 375 nm.

  10. Synthesis and structural property of Si nanosheets connected to Si nanowires using MnCl{sub 2}/Si powder source

    Energy Technology Data Exchange (ETDEWEB)

    Meng, Erchao [Graduate School of Science and Technology, Shizuoka University, 3-5-1 Johuku, Naka-ku, Hamamatsu, Shizuoka 432-8561 (Japan); Ueki, Akiko [Toyota Central R& D Labs., Inc., 41-1 Yokomichi, Nagakute, Aichi 480-1192 (Japan); Meng, Xiang [Graduate School of Science and Technology, Shizuoka University, 3-5-1 Johuku, Naka-ku, Hamamatsu, Shizuoka 432-8561 (Japan); Suzuki, Hiroaki [Graduate School of Engineering, Shizuoka University, 3-5-1 Johuku, Naka-ku, Hamamatsu, Shizuoka 432-8561 (Japan); Itahara, Hiroshi [Toyota Central R& D Labs., Inc., 41-1 Yokomichi, Nagakute, Aichi 480-1192 (Japan); Tatsuoka, Hirokazu, E-mail: tatsuoka.hirokazu@shizuoka.ac.jp [Graduate School of Integrated Science and Technology, Shizuoka University, 3-5-1 Johuku, Naka-ku, Hamamatsu, Shizuoka 432-8561 (Japan)

    2016-08-15

    Graphical abstract: Si nanosheets connected to Si nanowires synthesized using a MnCl{sub 2}/Si powder source with an Au catalyst avoid the use of air-sensitive SiH{sub 4} or SiCl{sub 4}. It was evident from these structural features of the nanosheets (leaf blade) with nanowires (petiole) that the nanosheets were formed by the twin-plane reentrant-edge mechanism. The feature of the observed lattice fringes of the Si(111) nanosheets was clearly explained by the interference with the extra diffraction spots that arose due to the reciprocal lattice streaking effect. - Highlights: • New Si nanosheets connected to Si nanowires were synthesized using MnCl{sub 2}/Si powders. • The synthesis method has benefits in terms of avoiding air sensitive SiH{sub 4} or SiCl{sub 4}. • Structural property and electron diffraction of the Si nanosheets were clarified. • Odd lattice fringes of the Si nanosheets observed by HRTEM were clearly explained. - Abstract: Si nanosheets connected to Si nanowires were synthesized using a MnCl{sub 2}/Si powder source with an Au catalyst. The synthesis method has benefits in terms of avoiding conventionally used air-sensitive SiH{sub 4} or SiCl{sub 4}. The existence of the Si nanosheets connected to the Si<111> nanowires, like sprouts or leaves with petioles, was observed, and the surface of the nanosheets was Si{111}. The nanosheets were grown in the growth direction of <211> perpendicular to that of the Si nanowires. It was evident from these structural features of the nanosheets that the nanosheets were formed by the twin-plane reentrant-edge mechanism. The feature of the observed lattice fringes, which do not appear for Si bulk crystals, of the Si(111) nanosheets obtained by high resolution transmission electron microscopy was clearly explained due to the extra diffraction spots that arose by the reciprocal lattice streaking effect.

  11. Hydrothermal synthesis of mixed zinc–cobalt ferrite nanoparticles: structural and magnetic properties

    Energy Technology Data Exchange (ETDEWEB)

    Coppola, P. [Univ. de Brasília, Complex Fluids Group, Instituto de Química (Brazil); Silva, F. G. da [Univ. de Brasília, Laboratório de Nanociência Ambiental e Aplicada - LNAA, Faculdade UnB Planaltina (Brazil); Gomide, G.; Paula, F. L. O. [Univ. de Brasília, Complex Fluids Group, Instituto de Física (Brazil); Campos, A. F. C. [Univ. de Brasília, Laboratório de Nanociência Ambiental e Aplicada - LNAA, Faculdade UnB Planaltina (Brazil); Perzynski, R. [Sorbonne Universités, UPMC Univ. Paris 06, CNRS, Laboratoire PHENIX (France); Kern, C. [Univ. de Brasília, Complex Fluids Group, Instituto de Química (Brazil); Depeyrot, J. [Univ. de Brasília, Complex Fluids Group, Instituto de Física (Brazil); Aquino, R., E-mail: reaquino@unb.br [Univ. de Brasília, Laboratório de Nanociência Ambiental e Aplicada - LNAA, Faculdade UnB Planaltina (Brazil)

    2016-05-15

    We synthesize Zn-substituted cobalt ferrite (Zn{sub x}Co{sub 1−x}Fe{sub 2}O{sub 4}, with 0 ≤ x ≤ 1) magnetic nanoparticles by a hydrothermal co-precipitation method in alkaline medium. The chemical composition is evaluated by atomic absorption spectroscopy and energy-dispersive X-ray spectroscopy techniques. The structure and morphology of the nanopaticles are investigated by X-ray diffraction (XRD) and transmission electron microscopy (TEM), respectively. XRD Rietveld refinements reveal the cation distribution among the tetrahedral (A) and octahedral (B) sites. It shows that up to x ~0.5 zinc ions occupy preferably A-sites, above which Zn ions begin also a gradual occupancy of B-sites. TEM images show nanoparticles with different shapes varying from spheres, cubes, to octahedrons. Hysteresis loop properties are studied at 300 and 5 K. These properties are strongly influenced by the Zn and Co proportion in the nanoparticle composition. At 300 K, only samples with high Co content present hysteresis. At 5 K, the reduced remanent magnetization ratio (M{sub R}/M{sub S}) and the coercivity (H{sub C}) suggest that nanoparticles with x < 0.5 have cubic anisotropy. A kink on the hysteresis loop, close to the remanence, is observed at low temperature. This feature is presumably associated to interplay between hard and soft anisotropy regimes in the powder samples.Graphical Abstract.

  12. Mesoporous TiO2 Micro-Nanometer Composite Structure: Synthesis, Optoelectric Properties, and Photocatalytic Selectivity

    Directory of Open Access Journals (Sweden)

    Kun Liu

    2012-01-01

    Full Text Available Mesoporous anatase TiO2 micro-nanometer composite structure was synthesized by solvothermal method at 180°C, followed by calcination at 400°C for 2 h. The as-prepared TiO2 was characterized by X-ray diffraction (XRD, scanning electron microscope (SEM, transmission electron microscope (TEM, and Fourier transform infrared spectrum (FT-IR. The specific surface area and pore size distribution were obtained from N2 adsorption-desorption isotherm, and the optoelectric property of the mesoporous TiO2 was studied by UV-Vis absorption spectrum and surface photovoltage spectra (SPS. The photocatalytic activity was evaluated by photodegradation of sole rhodamine B (RhB and sole phenol aqueous solutions under simulated sunlight irradiation and compared with that of Degussa P-25 (P25 under the same conditions. The photodegradation preference of this mesoporous TiO2 was also investigated for an RhB-phenol mixed solution. The results show that the TiO2 composite structure consists of microspheres (∼0.5–2 μm in diameter and irregular aggregates (several hundred nanometers with rough surfaces and the average primary particle size is 10.2 nm. The photodegradation activities of this mesoporous TiO2 on both RhB and phenol solutions are higher than those of P25. Moreover, this as-prepared TiO2 exhibits photodegradation preference on RhB in the RhB-phenol mixture solution.

  13. Synthesis, Structural, and Adsorption Properties and Thermal Stability of Nanohydroxyapatite/Polysaccharide Composites.

    Science.gov (United States)

    Skwarek, Ewa; Goncharuk, Olena; Sternik, Dariusz; Janusz, Wladyslaw; Gdula, Karolina; Gun'ko, Vladimir M

    2017-12-01

    A series of composites based on nanohydroxyapatite (nHAp) and natural polysaccharides (PS) (nHAp/agar, nHAp/chitosan, nHAp/pectin FB300, nHAp/pectin APA103, nHAp/sodium alginate) was synthesized by liquid-phase two-step method and characterized using nitrogen adsorption-desorption, DSC, TG, FTIR spectroscopy, and SEM. The analysis of nitrogen adsorption-desorption data shows that composites with a nHAp: PS ratio of 4:1 exhibit a sufficiently high specific surface area from 49 to 82 m 2 /g. The incremental pore size distributions indicate mainly mesoporosity. The composites with the component ratio 1:1 preferably form a film-like structure, and the value of S BET varies from 0.3 to 43 m 2 /g depending on the nature of a polysaccharide. Adsorption of Sr(II) on the composites from the aqueous solutions has been studied. The thermal properties of polysaccharides alone and in nHAp/PS show the influence of nHAp, since there is a shift of characteristic DSC and DTG peaks. FTIR spectroscopy data confirm the presence of functional groups typical for nHAp as well as polysaccharides in composites. Structure and morphological characteristics of the composites are strongly dependent on the ratio of components, since nHAp/PS at 4:1 have relatively large S BET values and a good ability to adsorb metal ions. The comparison of the adsorption capacity with respect to Sr(II) of nHAp, polysaccharides, and composites shows that it of the latter is higher than that of nHAp (per 1 m 2 of surface).

  14. Synthesis, crystal structure, spectroscopic characterization and nonlinear optical properties of Co(II)- picolinate complex

    Energy Technology Data Exchange (ETDEWEB)

    Tamer, Ömer, E-mail: omertamer@sakarya.edu.tr; Avcı, Davut; Atalay, Yusuf

    2015-11-15

    A cobalt(II) complex of picolinate was synthesized, and its structure was fully characterized by the applying of X-ray diffraction method as well as FT-IR, FT-Raman and UV–vis spectroscopies. In order to both support the experimental results and convert study to more advanced level, density functional theory calculations were performed by using B3LYP level. Single crystal X-ray structural analysis shows that cobalt(II) ion was located to the center of distorted octahedral geometry. The C=O, C=C and C=N stretching vibrations were found as highly active and strong peaks, inducing the molecular charge transfer within Co(II) complex. The small energy gap between frontier molecular orbital energies was another indicator of molecular charge transfer interactions within Co(II) complex. The nonlinear optical properties of Co(II) complex were investigated at DFT/B3LYP level, and the hypepolarizability parameter was found to be decreased due to the presence of inversion symmetry. The natural bond orbital (NBO) analysis was performed to investigate molecular stability, hyperconjugative interactions, intramolecular charge transfer (ICT) and bond strength for Co(II) complex. Finally, molecular electrostatic potential (MEP) and spin density distributions for Co(II) complex were evaluated. - Highlights: • Co(II) complex of picolinate was prepared. • Its FT-IR, FT-Raman and UV–vis spectra were measured. • DFT calculations were performed to support experimental results. • Small HOMO-LUMO energy gap is an indicator of molecular charge transfer. • Spin density localized on Co(II) as well as O and N atoms.

  15. Synthesis for Structure Rewriting Systems

    Science.gov (United States)

    Kaiser, Łukasz

    The description of a single state of a modelled system is often complex in practice, but few procedures for synthesis address this problem in depth. We study systems in which a state is described by an arbitrary finite structure, and changes of the state are represented by structure rewriting rules, a generalisation of term and graph rewriting. Both the environment and the controller are allowed to change the structure in this way, and the question we ask is how a strategy for the controller that ensures a given property can be synthesised.

  16. Synthesis, structure, and photoluminescence properties of an organically-templated uranyl selenite

    Energy Technology Data Exchange (ETDEWEB)

    Liu, Dong-Sheng; Kuang, Han-Mao; Chen, Wen-Tong; Luo, Qiu-Yan; Sui, Yan [Institute of Applied Chemistry, School of Chemistry and Chemical Engineering, Jinggangshan University, Ji' an, Jiangxi 343009 (China)

    2015-09-15

    The organically-templated uranyl selenite, (H{sub 2}en)[(UO{sub 2})(SeO{sub 3})(HSeO{sub 3})](NO{sub 3}).0.5H{sub 2}O (1) (en = 1,2-ethylenediamine) was synthesized and characterized by elemental analyses, IR spectroscopy, TG, and single-crystal X-ray diffraction. Compound 1 crystallizes in the orthorhombic system, space group Pbca, with a = 13.170(3) Aa, b = 11.055(2) Aa, c = 18.009(4) Aa, V = 2621.8(9) Aa{sup 3}, M = 1316.19, Z = 4, D{sub cal} = 3.334 g.cm{sup -3}, μ(Mo-K{sub α}) = 17.998 mm{sup -1}, GOF = 1.059, R{sub 1} = 0.0263, wR{sub 2} = 0.0532 [I>2σ(I)]. The X-ray diffraction analysis reveals that compound 1 has a three-dimensional (3D) supramolecular structure. It contains negatively charged [UO{sub 2}(HSeO{sub 3})(SeO{sub 3})]{sup -} inorganic anion layers and is balanced by [H{sub 2}en]{sup 2+} cations and NO{sub 3}{sup -} anions located in the interlayers. Furthermore, the photoluminescence properties of 1 were investigated. (Copyright copyright 2015 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  17. Synthesis, structure and physical properties of YbNi3Al9.23

    International Nuclear Information System (INIS)

    Tobash, P H; Ronning, F; Thompson, J D; Scott, B L; Bauer, E D; Jiang, Yu; Booth, C H

    2011-01-01

    The physical properties of YbNi 3 Al 9.23(1) , including the crystal structure, magnetization, specific heat, valence, and electrical resistivity, are reported. Single crystal x-ray diffraction reveals that the compound crystallizes with the rhombohedral space group R32 and has unit cell parameters a = 7.2443(3) A and c = 27.251(3) A with some crystallographic disorder at Al sites. The compound orders antiferromagnetically at T N = 3 K despite the presence of strong ferromagnetic correlations, accompanied by a spin-flop-like transition to a moment-aligned state above 0.1 T. X-ray absorption spectroscopy and magnetic susceptibility measurements indicate a localized Yb 3+ electronic configuration, while the Sommerfeld coefficient for the magnetically ordered state was determined as approximately 135 mJ mol -1 K -2 , suggesting moderately heavy fermion behavior. Therefore, these data indicate a balance between competing Ruderman-Kittel-Kasuya-Yosida (RKKY) and Kondo interactions in YbNi 3 Al 9.23(1) with a somewhat dominant RKKY interaction that leads to a relatively high ordering temperature.

  18. Synthesis of Polydimethylsiloxane-Modified Polyurethane and the Structure and Properties of Its Antifouling Coatings

    Directory of Open Access Journals (Sweden)

    Zhan-Ping Zhang

    2018-04-01

    Full Text Available Polydimethylsiloxane (PDMS could be used to improve the antifouling properties of the fouling release coatings based on polyurethane (PU. A series of polydimethylsiloxane-modified polyurethane coatings were synthesized with various PDMS contents, using the solvent-free method. The effects of PDMS content and seawater immersion on the chain structure and surface morphology were investigated by confocal laser scanning microscopy (CLSM, atomic force microscopy (AFM, Fourier transform infrared spectroscopy (FTIR, differential scanning calorimetry (DSC, thermogravimetric analysis (TGA and X-ray diffraction (XRD. Based on the measurements of contact angles of deionized water and diiodomethane, surface free energies of the coatings were estimated according to the Owens two-liquid method. The PDMS-modified polyurethane exhibited lower surface free energy and a lower glass transition temperature than polyurethane. The presence of PDMS increased the degree of microphase separation, and enhanced the water resistance of the coatings. The optimum amount of PDMS reduced the elastic modulus and increased the ductility of the coating. The presence of PDMS benefited the removal of weakly attached organisms. Panel tests in the Yellow Sea demonstrated the antifouling activity of the PDMS-modified polyurethane.

  19. A New 1D Chained Coordination Polymer: Synthesis, Crystal Structure, Antitumor Activity and Luminescent Property

    Directory of Open Access Journals (Sweden)

    Xi-Shi Tai

    2015-11-01

    Full Text Available A new 1D chained coordination polymer of Zn(II, {[Zn(L2(4,4′-bipy]·(H2O}n(1 (HL = N-acetyl-l-phenylalanine; 4,4′-bipy = 4,4′-bipyridine has been synthesized and characterized by elemental analysis, IR and X-ray single crystal diffraction analysis. Theresults show that each asymmetric unit of Zn(II complex belongs to monoclinic, space group P21 with a = 11.421(2 Å, b = 9.2213(17 Å, c = 15.188(3 Å,β = 106.112(3°, V = 1536.7(5 Å3, Z = 2, Dc = 1.444 g·cm−3, µ = 0.857 mm−1, F(000 = 696, and final R1 = 0.0439, ωR2 = 0.1013. The molecules form one-dimensional chained structure by its the bridging 4,4′-bipyridine ligands. The antitumor activities and luminescent properties of Zn(II coordination polymer have also been investigated.

  20. Synthesis, structure and magnetic properties of DyAl2 nanoparticles

    International Nuclear Information System (INIS)

    Zhang, W.S.; Brueck, E.; Zhang, Z.D.; Tegus, O.; Li, W.F.; Si, P.Z.; Geng, D.Y.; Klaasse, J.C.P.; Buschow, K.H.J.

    2006-01-01

    DyAl 2 nanoparticles have been prepared by means of arc discharge in a mixture of argon and hydrogen gas. The structure of DyAl 2 nanoparticles is studied by means of X-ray diffraction, X-ray photoelectron spectroscopy, and high-resolution transmission electron microscopy. X-ray photoelectron spectroscopy shows that the as-prepared DyAl 2 nanoparticles are coated with a layer of Al 2 O 3 phase on the surface, and their sizes vary from 20 nm to about 100 nm. The DyAl 2 nanoparticles exhibit ferromagnetic properties that are different from bulk DyAl 2 compound. The gradual decrease of the magnetization with increasing temperature in a wide temperature range reveals the size distribution of the DyAl 2 nanoparticles. The magnetic-entropy changes are derived from the isothermal magnetization curves measured at different temperatures. The magnetic-entropy change of the DyAl 2 nanoparticles is lower than that of the bulk DyAl 2 material but has a broadened peak

  1. Synthesis, structures and electroluminescence properties of CdS:In/Si nanoheterostructure array

    Energy Technology Data Exchange (ETDEWEB)

    Yan, Ling Ling; Cai, Hong Xin; Chen, Liang [Henan Polytechnic University, School of Physics and Electronic Information Engineering, Jiaozuo (China)

    2017-10-15

    An In-doped CdS/Si nanoheterojunction (CdS:In/Si-NPA) is prepared by depositing an In-doped CdS thin film onto a Si nanoporous pillar array (Si-NPA) via a successive ionic layer adsorption and reaction method. Based on the measured J-V characteristic curve, the nanoheterojunction exhibits a good rectifying behavior with a low forward turn-on voltage (2.2 V), a small leakage current density (0.5 mA/cm{sup 2} at - 3 V) and a high reverse breakdown voltage (> 8 V). The electroluminescence (EL) measurements reveal that a broadband emerges between 400 and 700 nm, and this band is confirmed as a white light emission based on the value of the chromaticity coordinate. The EL properties, including the CIE chromaticity coordinates, Colour Rendering Index and correlated color temperature, can be tuned by the applied voltage. The generation mechanism of the EL can be well interpreted depending on the energy band structure of CdS:In/Si-NPA. The green band should be attributed to the band-edge emission of CdS and the yellow emission may be related to Cd interstitial. These results highlight the potential of CdS:In/Si-NPA as a light source for future white light emitting devices. (orig.)

  2. Synthesis, structure and luminescence properties of zinc (II) complexes with terpyridine derivatives as ligands

    International Nuclear Information System (INIS)

    Chen Xuegang; Zhou Quanguo; Cheng Yanxiang; Geng Yanhou; Ma Dongge; Xie Zhiyuan; Wang Lixiang

    2007-01-01

    Five zinc (II) complexes (1-5) with 4'-phenyl-2,2':6',2''-terpyridine (ptpy) derivatives as ligands have been synthesized and fully characterized. The para-position of phenyl in ptpy is substituted by the group (R), i.e. tert-butyl (t-Bu), hexyloxy (OHex), carbazole-9-yl (Cz), naphthalen-1-yl-phenyl-amine-N-yl (NPA) and diphenyl amine-N-yl (DPA), with different electron-donating ability. With increasing donor ability of the R, the emission color of the complexes in film was modulated from violet (392 nm) to reddish orange (604 nm). The photoexcited luminescence exhibits significant solvatochromism because the emission of the complexes involves the intra-ligand charge transfer (ILCT) excited state. The electrochemical investigations show that the complexes with stronger electro-donating substituent have lower oxidation potential and then higher HOMO level. The electroluminescence (EL) properties of these zinc (II) complexes were studied with the device structure of ITO/PEDOT/Zn (II) complex: PBD:PMMA/BCP/AlQ/LiF/Al. Complexes 3, 4 and 5 exhibit EL wavelength at 552, 600 and 609 nm with maximum current efficiency of 5.28, 2.83 and 2.00 cd/A, respectively

  3. Enhancement of structural and magnetic properties of M-type hexaferrite permanent magnet based on synthesis temperature

    Science.gov (United States)

    Anjum, Safia; Sehar, Fatima; Mustafa, Zeeshan; Awan, M. S.

    2018-01-01

    The main purpose of this research work is to develop the single domain magnetic particles of M-type barium hexaferrite (BaFe12O19) using oxide precursors employing conventional powder metallurgy technique. The phase formation and magnetic performance of the powders and magnets will be optimized by adjusting calcination and sintering temperatures. The synthesis of M-type barium hexaferrite was carried out in two sections. A series of four samples have been prepared by initial wet mixed powders calcined at different temperatures, i.e., 750, 850, 950 and 1050 °C. On the basis of structural analysis, the sample calcined at 950 °C has been selected and further divided into four parts to sintered them at 1100, 1150, 1200 and 1250 °C. The structural measurements depict the confirmation of M-type barium hexaferrite structure. SEM micrographs show the hexagonal-shaped grains. The abrupt decrease in coercivity for the sample sintered at 1250 °C has been seen which may be due to high sintering temperature, at which the particles have multi-domain properties.

  4. Synthesis, structural, dielectric and magnetic properties of polyol assisted copper ferrite nano particles

    Energy Technology Data Exchange (ETDEWEB)

    Pavithradevi, S. [Assistant Professor, Department of Physics, Park College of Engineering and Technology, Coimbatore (India); Suriyanarayanan, N., E-mail: madurasuri2210@yahoo.com [Prof & Head, Department of Physics, Government College of Technology, Coimbatore (India); Boobalan, T. [Lecturer, Department of Physics, PSG Polytechnic College, Coimbatore (India)

    2017-03-15

    Nanocrystalline copper ferrite CuFe{sub 2}O{sub 4} is synthesized by co-precipitation method in ethylene glycol as chelating agent, using sodium Hydroxide as precipitator at pH 8. The as synthesized CuFe{sub 2}O{sub 4} is annealed at temperatures of 350 °C, 700 °C, and 1050 °C for 2 h respectively. The thermal analysis of the synthesized sample is done by TG technique. It is shown that at 260 °C ethylene glycol has evaporated completely and after 715 °C, spinel ferrite is formed with a cubic structure. The calculated lattice parameters are in agreement with the reported values. FTIR spectra of CuFe{sub 2}O{sub 4} nano particles are as synthesized and annealed at 1050 °C and recorded between 400 cm{sup −1} and 4000 cm{sup −1}. It shows that when the temperature increases ethylene glycol gradually evaporates. Finally, nano crystalline single phase spinel ferrite is obtained. X-ray diffraction (XRD) and electron diffraction (EDS) studies show that the sample is indexed as the face centered cubic spinel structure. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) indicated that the particles are flaky and spherical with the crystallite size in the range of 25–34 nm. From the dielectric studies, the dielectric constant decreases as the frequency increases. Low value of dielectric loss at higher frequencies suggests that the material is suitable for high frequency applications. AC conductivity increases with frequency. The magnetic properties of the samples are measured using a vibrating sample magnetometer (VSM) at room temperature, which shows that the sample exhibited a typical super paramagnetic behavior at low temperature. The saturation magnetization, remanant magnetism, and coercivity increases with applied field. - Highlights: • Complete removal of hematite phase along with ethylene glycol at 1050 °C. • Large decrease in particle sizes noticed along with ethylene glycol. • Ethylene glycol improves purity of the

  5. Effect of Synthesis Parameters on the Structure and Magnetic Properties of Magnetic Manganese Ferrite/Silver Composite Nanoparticles Synthesized by Wet Chemistry Method

    DEFF Research Database (Denmark)

    Huy, L.T.; Tam, L.T.; Phan, V.N.

    2016-01-01

    In the present work, magnetic manganese ferrite/silver (MnFe2O4-Ag) composite nanoparticles were synthesized by wet chemistry method. This synthesis process consists of two steps: first, the seed of manganese ferrite nanoparticles (MnFe2O4 NPs) was prepared by a coprecipitationmethod; second......, growth of silver nanoparticles (AgNPs) on the MnFe2O4 seed by modified photochemical reaction. We have conducted systematically the effects of synthesis parameters such as pH value, synthesis time, precursor salts concentration, mass ratio and stabilizing agents on the structure and magnetic properties......-prepared MnFe2O4-Ag magnetic nanocomposites display excellent properties of high crystallinity, long-term aggregation stability in aqueous medium, large saturation magnetization in the range of 15-20 emu/g, and small sizes of Ag-NPs similar to 20 nm. These exhibited properties made the MnFe2O4-Ag...

  6. The assembly and properties of protobiological structures - The beginnings of cellular peptide synthesis

    Science.gov (United States)

    Fox, S. W.; Nakashima, T.

    1980-01-01

    New data indicate that lysine-rich proteinoids have the ability to catalyze the synthesis of peptide bonds from a variety of amino acids and ATP. This capacity is evident in aqueous solution, in suspension of phase-separated complexes of lysine-rich proteinoid with acidic proteinoids, and in suspension of phase-separated particles composed of lysine-rich proteinoids with polynucleotides. Since the proteinoid complexes can contain other catalytic activities, including ability to catalyze internucleotide bond formation, it is inferred that the first protocells on earth already had a number of biological types of activity.

  7. Synthesis, structure and magnetic properties of the one-dimensional bimetallic oxide [Cu(terpy)Mo2O7

    International Nuclear Information System (INIS)

    Burkholder, Eric; Gabriel Armatas, N.; Golub, Vladimir; O'Connor, Charles J.; Zubieta, Jon

    2005-01-01

    The hydrothermal reaction of Cu(CH 3 CO 2 ) 2 .H 2 O, Na 2 MoO 4 and terpyridine at 140 deg. C for 48 h yields [Cu(terpy)Mo 2 O 7 ] (1), a bimetallic one-dimensional oxide. The structure consists of ruffled chains of edge- and corner-sharing {MoO 5 } square pyramids, decorated with {CuN 3 O 2 } '4+1' axially distorted square pyramids. The Cu(II) polyhedra are disposed so as to produce an alternating pattern of Cu-Cu distances across the {Mo 2 O 2 } rhombi of the chain of 6.25 and 6.82 A. This structural feature is reflected in the magnetic properties which are characteristic of a dimer rather than a linear chain, consistent with an alternating antiferromagnetic Heisenberg chain. -- Graphical abstract: Hydrothermal synthesis provided the one-dimensional bimetallic oxide [Cu(terpy)Mo 2 O 7 ], a material consisting of a zig-zag {Mo 2 O 7 } n 2 n - chain, decorated with {Cu(terpy)} 2+ groups exhibiting alternating short-long Cu-Cu distances between copper sites

  8. Synthesis of carbide fuels from nano-structured precursors: impact on carbo-reduction and physico-chemical properties

    International Nuclear Information System (INIS)

    Saravia, Alvaro

    2015-01-01

    The classical way classically used for manufacturing carbide fuels consists of carbo-reducing at high temperature (1600 C) and under primary vacuum a mixture of AnO 2 and graphite powders. These conditions are disadvantageous for the synthesis of mixed (U,Pu)C carbides on account of plutonium volatilization. Therefore, one of the main aims of these studies is to decrease the carbo-reduction temperature. The experiments focused mainly on the lowering of the uranium oxide temperature. This result has been obtained with the use of uranium oxide and carbon nano-structured precursors. To achieve this goal colloidal suspensions of uranium oxide have been prepared and stabilized by cellulosic ethers. Cellulosic ethers are both stabiliser for uranium oxide nanoparticles and carbon source for carbo-reduction. It has been shown that these precursors are more efficient for carbo-reduction than the standard precursors: a reduction of 300 C of carbo-reduction temperature has been obtained. The impact of these precursors on carbo-reduction and on physico-chemical properties as well as the structural and microstructural characterizations of the obtained carbides have been carried out. (author) [fr

  9. Effect of estrogen on tendon collagen synthesis, tendon structural characteristics, and biomechanical properties in postmenopausal women

    DEFF Research Database (Denmark)

    Hansen, Mette; Kongsgaard, Mads; Holm, Lars

    2009-01-01

    and fibril characteristics were determined by MRI and transmission electron microscopy, whereas tendon biomechanical properties were measured during isometric maximal voluntary contraction by ultrasound recording. Tendon FSR was markedly higher in ERT-users (P

  10. A series of novel lanthanide carboxyphosphonates with a 3D framework structure: synthesis, structure, and luminescent and magnetic properties.

    Science.gov (United States)

    Chen, Kai; Dong, Da-Peng; Sun, Zhen-Gang; Jiao, Cheng-Qi; Li, Chao; Wang, Cheng-Lin; Zhu, Yan-Yu; Zhao, Yan; Zhu, Jiang; Sun, Shou-Hui; Zheng, Ming-Jing; Tian, Hui; Chu, Wei

    2012-08-28

    By introduction of 1,4-benzenedicarboxylic acid as the second organic ligand, a series of novel lanthanide carboxyphosphonates with a 3D framework structure, namely, [Ln(3)(H(2)L)(HL)(2)(bdc)(2)(H(2)O)]·7H(2)O (Ln = La (1), Ce (2), Pr (3), Nd (4), Sm (5), Eu (6), Gd (7), Tb (8); H(3)L = H(2)O(3)PCH(2)NC(5)H(9)COOH; H(2)bdc = HOOCC(6)H(4)COOH) have been synthesized under hydrothermal conditions. Compounds are isostructural and feature a 3D framework in which Ln(III) polyhedra are interconnected by bridging {CPO(3)} tetrahedra into 2D inorganic layers parallel to the ab plane. The organic groups of H(2)L(-) are grafted on the two sides of the layer. These layers are further cross-linked by the bdc(2-) ligands from one layer to the Ln atoms from the other into a pillared-layered architecture with one-dimensional channel system along the a axis. The thermal stability of compounds has been investigated. Luminescent properties of compounds , and the magnetic properties of compound have also been studied.

  11. Synthesis, structural, and optical properties of type-II ZnO–ZnS core–shell nanostructure

    Energy Technology Data Exchange (ETDEWEB)

    Sookhakian, M., E-mail: m.sokhakian@gmail.com [Department of Physics, University of Malaya, Kuala Lumpur 50603 (Malaysia); Amin, Y.M. [Department of Physics, University of Malaya, Kuala Lumpur 50603 (Malaysia); Basirun, W.J. [Department of Chemistry, University of Malaya, Kuala Lumpur 50603 (Malaysia); Nanotechnology and Catalysis Research Centre (NanoCat), Institute of Postgraduate Studies, University Malaya, 50603 Kuala Lumpur (Malaysia); Tajabadi, M.T. [Department of Chemistry, University of Malaya, Kuala Lumpur 50603 (Malaysia); Kamarulzaman, N. [Centre for Nanomaterials Research Institute of Science, Level 3 Block C (Old Engineering Building), Universiti Teknologi MARA (UiTM), 40450 Shah Alam, Selangor (Malaysia)

    2014-01-15

    We demonstrate a facile one-step method for the preparation of ZnO–ZnS core–shell type-II nanostructures, pure ZnS quantum dots and pure ZnO nanoparticles with different experimental conditions. Treatment with sodium hydroxide as a capping agent is investigated systematically during the synthesis of ZnS quantum dots (QDs). The thickness of the ZnS shell is controlled by the concentration of the sodium sulphide during the synthesis of ZnO–ZnS core–shell nanostructures. The morphology and structure of samples are verified by X-ray diffraction (XRD), high resolution transmission electron microscopy (HRTEM) and energy dispersive X-ray analysis (EDX). The UV–vis absorption spectra of the pure ZnS QDs exhibit a blue shift in the absorption edge due to the quantum confinement effect. The PL emission spectra of the ZnO–ZnS core–shell nanostructure are compared with the ZnO nanoparticles. The ZnO–ZnS core–shell nanostructures show decrease in the UV and green emissions with the appearance of a blue emission, which are not found in the ZnO nanoparticles. -- Highlights: • It has synthesised ZnO–ZnS core–shell type II in one-step for the first time. • The as-synthesised samples were characterised by using XRD, UV–vis. • The photoluminescence properties of ZnO–ZnS core–shell was compared with ZnO. • The UV and green emission in the PL spectrum of ZnO–ZnS core–shell decreased. • The blue emission in the PL spectrum of ZnO–ZnS core–shell appeared.

  12. Synthesis, structural, and optical properties of type-II ZnO–ZnS core–shell nanostructure

    International Nuclear Information System (INIS)

    Sookhakian, M.; Amin, Y.M.; Basirun, W.J.; Tajabadi, M.T.; Kamarulzaman, N.

    2014-01-01

    We demonstrate a facile one-step method for the preparation of ZnO–ZnS core–shell type-II nanostructures, pure ZnS quantum dots and pure ZnO nanoparticles with different experimental conditions. Treatment with sodium hydroxide as a capping agent is investigated systematically during the synthesis of ZnS quantum dots (QDs). The thickness of the ZnS shell is controlled by the concentration of the sodium sulphide during the synthesis of ZnO–ZnS core–shell nanostructures. The morphology and structure of samples are verified by X-ray diffraction (XRD), high resolution transmission electron microscopy (HRTEM) and energy dispersive X-ray analysis (EDX). The UV–vis absorption spectra of the pure ZnS QDs exhibit a blue shift in the absorption edge due to the quantum confinement effect. The PL emission spectra of the ZnO–ZnS core–shell nanostructure are compared with the ZnO nanoparticles. The ZnO–ZnS core–shell nanostructures show decrease in the UV and green emissions with the appearance of a blue emission, which are not found in the ZnO nanoparticles. -- Highlights: • It has synthesised ZnO–ZnS core–shell type II in one-step for the first time. • The as-synthesised samples were characterised by using XRD, UV–vis. • The photoluminescence properties of ZnO–ZnS core–shell was compared with ZnO. • The UV and green emission in the PL spectrum of ZnO–ZnS core–shell decreased. • The blue emission in the PL spectrum of ZnO–ZnS core–shell appeared

  13. Synthesis and structural, magnetic and magnetotransport properties of permalloy powders containing nanoparticles prepared by arc discharge

    International Nuclear Information System (INIS)

    Prakash, Tushara; Williams, Grant V.M.; Kennedy, John; Murmu, Peter P.; Leveneur, Jérôme; Chong, Shen V.; Rubanov, Sergey

    2014-01-01

    Highlights: • New method of arc discharge used to synthesise permalloy containing nanoparticles. • The highest quality powders were made using a 78% Ni permalloy rod in N 2 . • The Saturation moment was slightly less and the coercive field was low (3 mT). • MR contributions from the spin-dependent tunneling between the particles. - Abstract: We report the synthesis of permalloy powders that were made using an arc-discharge method and with 78% or 45% Ni concentrations in N 2 or Ar. Our research was motivated by the fact that magnetic nanoparticles displaying large magnetoresistances are useful for magnetic field sensors applications. The permalloy powders contained some nanoparticles and the particle sizes ranged from 10 nm to ∼20 μm. The highest quality powders were made using a 78% Ni permalloy rod in N 2 where the coercivity was low (0.3 mT) and the saturation moment per formula unit was slightly less than that expected for the bulk compound. Magnetoresistance was observed in a cold pressed pellet where it is likely to be dominated by the ordinary magnetoresistance and spin-dependent tunneling between the particles

  14. Facile synthesis, structure, and properties of Ag{sub 2}S/Ag heteronanostructure

    Energy Technology Data Exchange (ETDEWEB)

    Sadovnikov, S. I., E-mail: sadovnikov@ihim.uran.ru; Gusev, A. I. [Ural Branch of the Russian Academy of Sciences, Institute of Solid State Chemistry (Russian Federation)

    2016-09-15

    Ag{sub 2}S/Ag heteronanostructure has been produced by a simple one-stage chemical deposition from aqueous solutions of silver nitrate, sodium sulfide, and sodium citrate with the use of monochromatic light irradiation. For simultaneous synthesis of Ag{sub 2}S and Ag nanoparticles, deposition has been performed from reaction mixtures with reduced sodium sulfide concentration. The size of Ag{sub 2}S and Ag nanoparticles is 45–50 and 15–20 nm, respectively. It is established that in the contact layer between silver sulfide and silver, nonconducting α-Ag{sub 2}S acanthite transforms into superionic β-Ag{sub 2}S argentite under the action of external electric field. The scheme of the operation of a resistive switch based on an Ag{sub 2}S/Ag heteronanostructure is proposed. The UV–Vis optical absorption spectra of colloidal solutions of Ag{sub 2}S/Ag heteronanostructures have been studied.Graphical Abstract.

  15. Synthesis of Zn{sup 2+} substituted maghemite nanoparticles and investigation of their structural and magnetic properties

    Energy Technology Data Exchange (ETDEWEB)

    Mozaffari, M. [Department of Physics, Faculty of Science, University of Isfahan, Isfahan 81746-73441 (Iran, Islamic Republic of); Shatooti, S. [Department of Physics, Razi University, Kermanshah 67149-67346 (Iran, Islamic Republic of); Jafarzadeh, M., E-mail: mjafarzadeh1027@yahoo.com [Faculty of Chemistry, Razi University, Kermanshah 67149-67346 (Iran, Islamic Republic of); Niyaifar, M. [Department of Physics, Ahvaz Branch, Islamic Azad University, Ahvaz (Iran, Islamic Republic of); Aftabi, A. [Department of Physics, University of Kurdistan, Sanandaj 66177-15175 (Iran, Islamic Republic of); Mohammadpour, H. [Department of Physics, Ahvaz Branch, Islamic Azad University, Ahvaz (Iran, Islamic Republic of); Amiri, Sh. [Department of Physics, Razi University, Kermanshah 67149-67346 (Iran, Islamic Republic of)

    2015-05-15

    Maghemite and Zn{sup 2+} substituted maghemite (γ-Fe{sub 2−y} Zn{sub 3y/2}O{sub 3}, y=0.0, 0.11, 0.24, 0.36, 0.50 and 0.66) nanoparticles were prepared by coprecipitation method. The effect of Zn{sup 2+} substitution on the structural, morphological and magnetic properties of the nanoparitcles were studied by different techniques such as X-ray diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy, field emission scanning electron microscopy (FESEM), magnetometry, magnetic thermogravimetry and Mössbauer spectroscopy. The results of XRD showed that all samples have spinel structure with an increase in lattice parameter by increasing the content of Zn{sup 2+}. FTIR spectra were proved the synthesis of maghemite and Zn{sup 2+} substituted maghemite with appearance of the related absorption bands and band shift upon Zn{sup 2+} substitution. Morphological studies by FESEM demonstrated that the nanoparticles were uniform and spherical with average particle size in range of 20–24 nm. Room temperature magnetic measurements showed that as Zn{sup 2+} content increases, saturation magnetization initially increase up to 75.34 emu/g for y=0.11 and then decrease to 3.65 emu/g for y=0.66, due to substitution of magnetic Fe{sup 3+} by non-magnetic Zn{sup 2+}. Decrease in Curie temperature of the samples, from 510 for maghemite to 250 °C for y=0.36, by increasing the Zn{sup 2+} substitution was a result of reduction of superexchange interactions between different sites. Then, the Curie temperature increased up to 680 °C for y=0.66 which was due to migration of some Zn{sup 2+} ions from A to B sites in the structure of spinel. Room temperature Mössbauer spectra exhibited that the sample with y=0.0 was superparamagnetic, while by increasing the content of Zn{sup 2+}, relaxation effect increased by weakening of A–B exchange interaction. - Highlights: • Synthesis of Zn{sup 2+}-substituted maghemite via co-precipitation/oxidation method. • Increase in lattice

  16. A novel rhombohedron-like nickel ferrite nanostructure: Microwave combustion synthesis, structural characterization and magnetic properties

    Directory of Open Access Journals (Sweden)

    G. Suresh Kumar

    2016-09-01

    Full Text Available Research on nickel ferrite nanostructures has drawn a great interest because of its inherent chemical, physical and electronic properties. In this study, we have synthesized rhombohedron – like nickel ferrite nanostructure by a rapid microwave assisted combustion method using ethylenediamminetetraacetic acid as a chelating agent. X-ray diffraction, Fourier transform infrared spectrometer, transmission electron microscope and energy dispersive X-ray microanalyser were used to characterize the prepared sample. The magnetic behaviour was analysed by means of field dependent magnetization measurement which indicates that the prepared sample exhibits a soft ferromagnetic nature with saturation magnetization of 63.034 emu/g. This technique can be a potential method to synthesize novel nickel ferrite nanostructure with improved magnetic properties.

  17. Synthesis, structural properties and thermal stability of Mn-doped hydroxyapatite

    Science.gov (United States)

    Paluszkiewicz, Czesława; Ślósarczyk, Anna; Pijocha, Dawid; Sitarz, Maciej; Bućko, Mirosław; Zima, Aneta; Chróścicka, Anna; Lewandowska-Szumieł, Małgorzata

    2010-07-01

    Hydroxyapatite (HA) - Ca 10(PO 4) 6(OH) 2 is a basic inorganic model component of hard biological tissues, such as bones and teeth. The significant property of HA is its ability to exchange Ca 2+ ions, which influences crystallinity, physico-chemical and biological properties of modified hydroxyapatite materials. In this work, FTIR, Raman spectroscopy, XRD, SEM and EDS techniques were used to determine thermal stability, chemical and phase composition of Mn containing hydroxyapatite (MnHA). Described methods confirmed thermal decomposition and phase transformation of MnHA to αTCP, βTCP and formation of Mn 3O 4 depending on sintering temperature and manganese content. In vitro biological evaluation of Mn-modified HA ceramics was also performed using human osteoblast cells.

  18. Anthracene-Based Lanthanide Metal-Organic Frameworks: Synthesis, Structure, Photoluminescence, and Radioluminescence Properties

    Directory of Open Access Journals (Sweden)

    Stephan R. Mathis

    2018-01-01

    Full Text Available Four anthracene-based lanthanide metal-organic framework structures (MOFs were synthesized from the combination of the lanthanide ions, Eu3+, Tb3+, Er3+, and Tm3+, with 9,10-anthracenedicarboxylic acid (H2ADC in dimethylformamide (DMF under hydrothermal conditions. The 3-D networks crystalize in the triclinic system with P-1 space group with the following compositions: (i {{[Ln2(ADC3(DMF4·DMF]}n, Ln = Eu (1 and Tb (2} and (ii {{[Ln2(ADC3(DMF2(OH22·2DMF·H2O]}n, Ln = Er (3 and Tm (4}. The metal centers exist in various coordination environments; nine coordinate in (i, while seven and eight coordinate in (ii. The deprotonated ligand, ADC, assumes multiple coordination modes, with its carboxylate functional groups severely twisted away from the plane of the anthracene moiety. The structures show ligand-based photoluminescence, which appears to be significantly quenched when compared with that of the parent H2ADC solid powder. Structure 2 is the least quenched and showed an average photoluminescence lifetime from bi-exponential decay of 0.3 ns. On exposure to ionizing radiation, the structures show radioluminescence spectral features that are consistent with the isolation of the ligand units in its 3-D network. The spectral features vary among the 3-D networks and appear to suggest that the latter undergo significant changes in their molecular and/or electronic structure in the presence of the ionizing radiation.

  19. η6-Cycloparaphenylene transition metal complexes: synthesis, structure, photophysical properties, and application to the selective monofunctionalization of cycloparaphenylenes.

    Science.gov (United States)

    Kubota, Natsumi; Segawa, Yasutomo; Itami, Kenichiro

    2015-01-28

    The synthesis, structure, photophysical properties, and reactivity of cycloparaphenylenes (CPPs) coordinated to group 6 transition metal fragments are described. The η(6)-coordination of [9]CPP or [12]CPP with M(CO)6 (M = Cr, Mo, W) afforded the corresponding [n]CPP-M(CO)3 complexes (n = 9, 12; M = Cr, Mo, W). In the (1)H NMR spectra of these complexes, characteristic upfield-shifted singlet signals corresponding to the four hydrogen atoms attached to the coordinated C6H4 ring of the CPPs were observed at 5.4-5.9 ppm. The complex [9]CPP-Cr(CO)3 could be successfully isolated in spite of its instability. X-ray crystallographic analysis and computational studies of [9]CPP-Cr(CO)3 revealed that chromium-CPP coordination occurs at the convex surface of [9]CPP both in the solid state and in solution. TD-DFT calculations suggested that the emerging high-wavenumber absorption peak upon coordination of [9]CPP to Cr(CO)3 should be assigned to a weak HOMO-LUMO transition. Moreover, by using the complex [9]CPP-Cr(CO)3, a rapid and highly monoselective CPP functionalization has been achieved. The established one-pot method, consisting of complexation, deprotonation, nucleophilic substitution, and decomplexation steps, yielded silyl-, boryl-, and methoxycarbonyl-substituted CPPs in up to 93% yield relative to reacted starting material.

  20. Synthesis, Structural Characterization and Up-Conversion Luminescence Properties of NaYF4:Er3+,Yb3+@MOFs Nanocomposites

    Science.gov (United States)

    Giang, Lam Thi Kieu; Marciniak, Lukasz; Huy, Tran Quang; Vu, Nguyen; Le, Ngo Thi Hong; Binh, Nguyen Thanh; Lam, Tran Dai; Minh, Le Quoc

    2017-10-01

    This paper describes a facile synthesis of NaYF4:Er3+,Yb3+ nanoparticles embraced in metal-organic frameworks (MOFs), known as NaYF4:Er3+, Yb3+@MOFs core/shell nanostructures, by using iron(III) carboxylate (MIL-100) and zeolitic imidazolate frameworks (ZIF-8). Morphological, structural and optical characterization of these nanostructures were investigated by field emission-scanning electron microscopy, Fourier transform infrared spectroscopy, x-ray diffraction, and up-conversion luminescence measurements. Results showed that spherical-shaped NaYF4:Er3+,Yb3+@MIL-100 nanocomposites with diameters of 150-250 nm, and rod-shaped NaYF4:Er3+,Yb3+@ZIF-8 nanocomposites with lengths of 300-550 nm, were successfully synthesized. Under a 980-nm laser excitation at room temperature, the NaYF4:Er3+,Yb3+@MOFs nanocomposites exhibited strong up-conversion luminescence with two emission bands in the green part of spectrum at 520 nm and 540 nm corresponding to the 2H11/2 → 4I15/2 and 4S3/2 → 4I15/2 transitions of Er3+ ions, respectively, and a red emission band at 655 nm corresponding to the 4F9/2 → 4I15/2 transition of Er3+ ions. The above properties of NaYF4:Er3+,Yb3+@MOFs make them promising candidates for applications in biotechnology.

  1. Two novel metal–organic coordination polymers based on diphosphonate and oxalate: Synthesis, structures and properties

    International Nuclear Information System (INIS)

    Niu, Qing-Jun; Zheng, Yue-Qing; Zhou, Lin-Xia; Zhu, Hong-Lin

    2015-01-01

    Two 2-(1-imidazole)-1-hydroxyl-1,1'-ethylidenediphosphonato and oxalic acid bridged coordination polymers (H 2 en)[Co 3 (H 2 zdn) 2 (ox)(H 2 O) 2 ] (1) and Cd 2 (H 2 zdn)(ox) 0.5 (H 2 O) (2) (2-(1-imidazole)-1-hydroxyl-1,1'-ethylidenediphosphonic acid=H 5 zdn; oxalic acid=H 2 ox) were synthesized under hydrothermal conditions and characterized by the infrared (IR), thermogravimetric analyses (TGA), elemental analyses (EA) and X-ray diffraction (XRD). Compound 1 is bridged by phosphonate anions to 1D chain, and further linked by oxalate anions to 2D layer. Compound 2 is bridged by O–P–O units of H 5 zdn to the layer, and then pillared by oxalate anions to generate 3D frameworks. Compound 1 shows anti-ferromagnetic behaviors analyzed with the temperature-dependent zero-field ac magnetic susceptibilities, while compound 2 exhibits an influence on the luminescent property. - Graphical abstract: Linked by oxalate, two zoledronate-based metal–organic frameworks are synthesized, which exhibits the different frameworks. Magnetism and luminescent properties have been studied. The weak antiferromagnetic coupling is conducted in 1. - Highlights: • Compound 1 and 2 are first linked by oxalate anion based on zoledronic acid. • Compound 1 generates a classic “dia Diamond” (6 6 ) topology. • Compound 2 exhibits a (4 4 ·6 2 )(4 4 ·6 6 ) topology. • Magnetism and luminescent properties of 1 and 2 have been studied, respectively

  2. Synthesis, properties, and molecular structure of a trivalent organouranium diphosphine hydride

    International Nuclear Information System (INIS)

    Duttera, M.R.; Fagan, P.J.; Marks, T.J.; Day, V.W.

    1982-01-01

    Hydrogenolysis of U[(CH 3 ) 5 C 5 ] 2 R 2 , [R = CH 3 Ch 2 Si(CH 3 ) 3 ], proceeds at -20 0 C in the presence of excess bis(2 dimethylphosphino)ethane(dmpe) according to this reaction: U[(CH 3 ) 3 C 5 ] 2 R 2 + 1.5H 2 + dmpe → (toluene, 18h) U[(CH 3 ) 5 C 5 ] 2 (dmpe) H + 2RH. Black microcrystals can be purified by vacuum Soxhlet extraction with toluene. All processes involving this compound must be performed under argon or helium atmospheres, since it reacts with nitrogen. The structure was studied by NMR, ir spectra. The molar magnetic suceptibility was measured at 295 K, 5120 x 10 -4 emu and is consistent with a U (III) formulation. Crystals are orthorhombic. X-ray diffraction data were collected. Structural parameters were refined to convergence. X-ray structural analysis reveals monocrystals of discrete mononuclear U[eta 5 -(CH 3 ) 5 C 5 ] 2 (dmpe)H molecules. The molecular structure is evaluated. 1 figure

  3. Synthesis, crystal structure and photo luminescent property of a 3D ...

    Indian Academy of Sciences (India)

    isonicotinate)2(suc)2]n. Empirical formula. C20H16Cd3N2O12. Formula weight. 813.58 ..... SMART and SAINT, Bruker AXS Inc, Madison, WI. 1998. 47. Sheldrick G M 1997 SHELXS-97 Program for solution of crystal structures, University of Gottingen, ...

  4. Synthesis, structural and ferromagnetic properties of La1–x Kx ...

    Indian Academy of Sciences (India)

    MnO3 (0.0 ≤ ≤ 0.25) perovskite phases, which is a low temperature initiated, rapid route to prepare metal oxides. As-synthesized compounds are amorphous in nature; crystallinity was observed on heating at 800°C for 5 min. Structural ...

  5. Synthesis, structural and ferromagnetic properties of La1–x Kx MnO3

    Indian Academy of Sciences (India)

    Administrator

    2009-09-05

    Sep 5, 2009 ... Solid State and Structural Chemistry Unit, Indian Institute of Science, Bangalore 560 012, India .... equation for the formation of samples can be proposed as follows ..... for La-site in LaMnO3 system by the rapid solution com-.

  6. A porous cadmium(II) framework. Synthesis, crystal structure, gas adsorption, and fluorescence sensing properties

    Energy Technology Data Exchange (ETDEWEB)

    Zhou, Pingping [College of Sciences, Agricultural University of Hebei, Baoding (China)

    2017-05-18

    The Cd{sup II} compound, namely [Cd(Tppa)(SO{sub 4})(H{sub 2}O)]{sub n} (1) [Tppa = tris(4-(pyridyl)phenyl) amine], was synthesized by the reaction of CdSO{sub 4}.8H{sub 2}O and Tppa under solvothermal conditions. Single crystal X-ray diffraction analysis revealed that compound 1 features a 3D porous framework based on 1D inorganic -[Cd-SO{sub 4}-Cd]{sub n}- chains. Topological analysis reveals that compound 1 represents a trinodal (3,4,6)-connected topological network with the point symbol of {6.7"2}{sub 2}{6"4.7.10}{6"4.7"5.8"4.10"2}. Gas adsorption properties investigations indicate that compound 1 exhibits moderate adsorption capacities for light hydrocarbons at room temperature. Luminescence property studies revealed that this Cd{sup II} compound exhibits high fluorescence sensitivity for sensing of CS{sub 2} molecule. (copyright 2017 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  7. Synthesis, crystal structure and optical properties of BiMgVO 5

    Science.gov (United States)

    Benmokhtar, S.; El Jazouli, A.; Chaminade, J. P.; Gravereau, P.; Guillen, F.; de Waal, D.

    2004-11-01

    The new vanadate BiMgVO 5 has been prepared and its structure has been determined by single crystal X-ray diffraction: space group P21/n, a=7.542(6) Å, b=11.615(5) Å, c=5.305(3) Å, β=107.38(5)°, wR2=0.0447, R=0.0255. The structure consists of [Mg 2O 10] and [Bi 2O 10] dimers sharing their corners with [VO 4] tetrahedra. The ranges of bond lengths are 2.129-2.814 Å for Bi-O; 2.035-2.167 Å for Mg-O and 1.684-1.745 Å for V-O. V-O bond lengths determined from Raman band wavenumbers are between 1.679 and 1.747 Å. An emission band overlapping the entire visible region with a maximum around 650 nm is observed.

  8. Na3Tb(PO4)2: Synthesis, crystal structure and greenish emitting properties

    Science.gov (United States)

    Zhao, Dan; Ma, Zhao; Liu, Bao-Zhong; Zhang, Rui-Juan; Wu, Zhi-Qiang; Wang, Jian; Duan, Pei-Gao

    2018-03-01

    A anhydrous orthoborate Na3Tb(PO4)2 has been prepared and its crystal structure was determined by X-Ray diffraction of a non-merohedral twinned single crystal. The results show that the compound crystallizes in monoclinic space group C2/c and the structure features a 3D framework containing PO4, NaO6, NaO7, NaO8 and TbO8 polyhedra. Under near-UV excitation (370 nm), Na3Tb(PO4)2 shows intense characteristic emission bands of Tb3+ (490 nm, 543 nm, 585 nm and 620 nm) with the CIE coordinate of (0.3062, 0.5901), corresponding to greenish color. The excitation spectrum covers a wide range from 340 nm to 390 nm, which indicates that phosphor Na3Tb(PO4)2 can be efficiently activated by near-UV LED ship.

  9. Synthesis, structure and fluorescence properties of a novel 3D Sr(II) coordination polymer

    Science.gov (United States)

    Tan, Yu-Hui; Xu, Qing; Gu, Zhi-Feng; Gao, Ji-Xing; Wang, Bin; Liu, Yi; Yang, Chang-Shan; Tang, Yun-Zhi

    2016-09-01

    Solvothermal reaction of 2,2‧-bipyridine-5,5‧-dicarboxylic acid (H2bpdc) and SrCl2 affords a novel coordination polymer [Sr(Hbpdc)2]n1. X-ray structure determination shows that 1 exhibits a novel three-dimensional network. The unique Sr II cation sits on a two-fold axis and coordinated by four O-atom donors from four Hbptc- ligands and four N-atom donors from two Hbptc- ligands in distorted dodecahedral geometry. In 1 each Sr II cation connects to six different Hbptc- ligands and each Hbptc- ligand bridges three different Sr II cations which results in the formation of a three-dimensional polymeric structure. Corresponding to the free ligand, the fluorescent emission of complex 1 display remarkable "Einstain" shifts, which may be attributed to the coordination interaction of Sr atoms, thus reduce the rigidity of pyridyl rings.

  10. Synthesis and Properties of Layered-Structured Mn5O8 Nanorods

    DEFF Research Database (Denmark)

    Gao, Tao; Norby, Poul; Krumeich, Frank

    2010-01-01

    Mn5O8 nanorods were prepared by a topotactic conversion of γ-MnOOH nanorod precursors in nitrogen at 400 °C. The as-prepared Mn5O8 nanorods crystallized in a monoclinic structure (space group C2/m) with unit cell dimensions a = 10.3784(2) Å, b = 5.7337(7) Å, c = 4.8668(6) Å, and β = 109.491(6)°, ...

  11. A monomeric copper-phosphoramide complex: synthesis, structure, and electronic properties

    Czech Academy of Sciences Publication Activity Database

    Henriques, Margarida Isabel Sousa; Gorbunov, D.I.; Ponomaryov, A.Y.; Saneei, A.; Pourayoubi, M.; Dušek, Michal; Zvyagin, S.; Uhlarz, M.; Wosnitza, J.

    2016-01-01

    Roč. 118, Nov (2016), s. 154-158 ISSN 0277-5387 R&D Projects: GA ČR(CZ) GA14-03276S; GA MŠk LO1603 EU Projects: European Commission(XE) CZ.2.16/3.1.00/24510 Institutional support: RVO:68378271 Keywords : phosphoramide * magnetization * EPR * mononuclear copper complex * crystal structure Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 1.926, year: 2016

  12. Synthesis, structure and physical properties of a new TTF derivative containing a PPD part

    International Nuclear Information System (INIS)

    Fujiwara, H; Sugishima, Y; Tsujimoto, K

    2008-01-01

    To develop new photo-conducting multi-functional materials, a new tetrathiafulvalene (TTF) derivative containing a 2,5-diphenyl-1,3,4-oxadiazole (PPD) moiety, in which the PPD part is connected directly to the TTF part with a single bond, was synthesized by the Pd(PPh 3 ) 4 -catalyzed Stille coupling reaction. X-Ray crystal structure analysis of the t-Butyl derivative (1) indicated the high planarity of the molecular skeleton and possible conduction pathways along the side-by-side direction of the TTF parts. Fluorescence from the PPD part of 1 was almost quenched by the intramolecular electron transfer from the electron-donating TTF part to the PPD part even when the PPD was irradiated by the excitation light of 315 nm. The single crystalline sample of the TCNQ complex of 1 (1-TCNQ) was prepared by a mixing method in CH 3 CN. The X-ray crystal structure analysis of 1-TCNQ revealed that there is PPD - TCNQ - TTF -type mixed stacking structure along the stacking direction, resulting in insulating behaviour of this complex.

  13. Synthesis, structures, and luminescent properties of lanthanide complexes with triphenylphospine oxide

    Energy Technology Data Exchange (ETDEWEB)

    Ma, Yan; Xu, Shan; Wang, Xin; Li, Yue-Xue; Jin, Qiong-Hua [Department of Chemistry, Capital Normal University, Beijing (China); Liu, Min [The College of Materials Science and Engineering, Beijing University of Technology (China); Xin, Xiu-Lan [School of Food and Chemical Engineering, Beijing Technology and Business University (China)

    2017-07-03

    Seven lanthanide complexes [Ln(OPPh{sub 3}){sub 3}(NO{sub 3}){sub 3}] (1-3) (OPPh{sub 3} = triphenylphosphine oxide, Ln = Nd, Sm, Gd), [Dy(OPPh{sub 3}){sub 4}(NO{sub 3}){sub 2}](NO{sub 3}) (4), [Ln(OPPh{sub 3}){sub 3}(NO{sub 3}){sub 3}]{sub 2} (5-7) (Ln = Pr, Eu, Gd) were synthesized by the reactions of different lanthanide salts and OPPh{sub 3} ligand in the air. These complexes were characterized by single-crystal X-ray diffraction analysis, elemental analysis, IR and fluorescence spectra. Structure analysis shows that complexes 1-4 are mononuclear complexes formed by OPPh{sub 3} ligands and nitrates. The asymmetric units of complexes 5-7 consist of two crystallographic-separate molecules. Complex 1 is self-assembled to construct a 2D layer-structure of (4,4) net topology by hydrogen bond interactions. The other complexes show a 1D chain-like structure that was assembled by OPPh{sub 3} ligands and nitrate ions through C-H..O interactions. Solid emission spectra of compounds 4 and 6 are assigned to the characteristic fluorescence of Tb{sup 3+} (λ{sub em} = 480, 574 nm) and Eu{sup 3+} (λ{sub em} = 552, 593, 619, 668 nm). (copyright 2017 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  14. Synthesis, structure and photoelectrochemical properties of single crystalline silicon nanowire arrays

    International Nuclear Information System (INIS)

    Dalchiele, E.A.; Martin, F.; Leinen, D.; Marotti, R.E.; Ramos-Barrado, J.R.

    2010-01-01

    In the present work, n-type silicon nanowire (n-SiNW) arrays have been synthesized by self-assembly electroless metal deposition (EMD) nanoelectrochemistry. The synthesized n-SiNW arrays have been submitted to scanning electron microscopy (SEM), transmission electron microscopy (TEM), high-resolution transmission electron microscopy (HRTEM), X-ray photoelectron spectroscopy (XPS), and optical studies. Initial probes of the solar device conversion properties and the photovoltaic parameters such as short-circuit current, open-circuit potential, and fill factor of the n-SiNW arrays have been explored using a liquid-junction in a photoelectrochemical (PEC) system under white light. Moreover, a direct comparison between the PEC performance of a polished n-Si(100) and the synthesized n-SiNW array photoelectrodes has been done. The PEC performance was significantly enhanced on the n-SiNWs photoelectrodes compared with that on polished n-Si(100).

  15. Hydrothermal synthesis, crystal structures and photoluminescence properties of mixed europium–yttrium organic frameworks

    International Nuclear Information System (INIS)

    Han Yinfeng; Fu Lianshe; Mafra, Luís; Shi, Fa-Nian

    2012-01-01

    Three mixed europium–yttrium organic frameworks: Eu 2−x Y x (Mel)(H 2 O) 6 (Mel=mellitic acid or benzene-1,2,3,4,5,6-hexacarboxylic acid, x=0.38 1, 0.74 2, and 0.86 3) have been synthesized and characterized. All the compounds contain a 3-D net with (4, 8)-flu topology. The study indicates that the photoluminescence properties are effectively affected by the different ratios of europium and yttrium ions, the quantum efficiency is increased and the Eu 3+ lifetime becomes longer in these MOFs than those of the Eu analog. - Graphical abstract: Three mixed europium and yttrium organic frameworks: Eu 2−x Y x (Mel)(H 2 O) 6 (Mel=mellitic acid) have been synthesized and characterized. All the compounds contain a 3-D net with (4, 8)-flu topology. The study indicates that the photoluminescence properties are effectively affected by the different ratios of europium and yttrium ions, the quantum efficiency is increased and the Eu 3+ lifetime becomes longer in these MOFs than those of the Eu analog. Highlights: ► Three (4, 8)-flu topological mixed Eu and Y MOFs were synthesized under mild conditions. ► Metal ratios were refined by the single crystal data consistent with the EDS analysis. ► Mixed Eu and Y MOFs show longer lifetime and higher quantum efficiency than the Eu analog. ► Adding inert lanthanide into luminescent MOFs enlarges the field of luminescent MOFs.

  16. Synthesis, growth, structural modeling and physio-chemical properties of a charge transfer molecule: Guanidinium tosylate

    Science.gov (United States)

    Era, Paavai; Jauhar, RO. MU.; Vinitha, G.; Murugakoothan, P.

    2018-05-01

    An organic nonlinear optical material, guanidinium tosylate was synthesized adopting slow evaporation method and the crystals were harvested from aqueous methanolic medium with dimensions 13 × 9 × 3 mm3. Constitution of crystalline material was confirmed by single crystal X-ray diffraction study. The title compound crystallizes in the monoclinic crystal system with space group P21/c. The UV-vis-NIR spectral study of the grown crystal exhibits high transparency of 80% in the entire visible region with lower cut-off wavelength at 282 nm. Optimized molecular geometry of the grown crystal was obtained using density functional theory (DFT) and the frontier energy gaps calculated from the DFT aids to understand the charge transfer taking place in the molecule. The dielectric properties were studied as a function of temperature and frequency to find the charge distribution within the crystal. The titular compound is thermally stable up to 230 °C assessed by thermogravimetric and differential thermal analysis. Anisotropy in the mechanical behavior was observed while measuring for individual planes. The laser induced surface damage threshold of the grown crystal was measured to be 0.344 GW/cm2 for 1064 nm Nd:YAG laser radiation. Z-scan technique confirms the third-order nonlinear optical property with the ascertained nonlinear refractive index (n2), nonlinear absorption coefficient (β) and third order nonlinear susceptibility (χ(3)). Optical limiting study divulges that the transmitted output power step-up linearly with the increase of the input power at lower power realms and saturates from the threshold 24.95 mW/cm2 and amplitude 0.23 mW/cm2.

  17. Hexagonal nanorods of tungsten trioxide: Synthesis, structure, electrochemical properties and activity as supporting material in electrocatalysis

    Energy Technology Data Exchange (ETDEWEB)

    Salmaoui, Samiha; Sediri, Faouzi; Gharbi, Neji [Laboratoire de Chimie de la Matiere Condensee, Institut Preparatoire aux Etudes d' Ingenieurs, Universite de Tunis (Tunisia); Perruchot, Christian; Aeiyach, Salah [Interfaces, Traitements, Organisation et DYnamique des Systemes (ITODYS), UMR 7086, Universite Paris Diderot Paris 7, 15, rue Jean de Baif, 75205 Paris Cedex 13 (France); Rutkowska, Iwona A.; Kulesza, Pawel J. [Department of Chemistry, University of Warsaw, Pasteura 1, PL-02-093 Warsaw (Poland); Jouini, Mohamed, E-mail: jouini@univ-paris-diderot.fr [Interfaces, Traitements, Organisation et DYnamique des Systemes (ITODYS), UMR 7086, Universite Paris Diderot Paris 7, 15, rue Jean de Baif, 75205 Paris Cedex 13 (France)

    2011-07-15

    Tungsten trioxide, unhydrated with hexagonal structure (h-WO{sub 3}), has been prepared by hydrothermal method at a temperature of 180 {sup o}C in acidified sodium tungstate solution. Thus prepared h-WO{sub 3} has been characterized by X-ray diffraction (XRD) method and using electrochemical techniques. The morphology has been examined by scanning and transmission electron microscopies (SEM and TEM) and it is consistent with existence of nanorods of 50-70 nm diameter and up to 5 {mu}m length. Cyclic voltammetric characterization of thin films of h-WO{sub 3} nanorods has revealed reversible redox behaviour with charge-discharge cycling corresponding to the reversible lithium intercalation/deintercalation into the crystal lattice of the h-WO{sub 3} nanorods. In propylene carbonate containing LiClO{sub 4}, two successive redox processes of hexagonal WO{sub 3} nanorods are observed at the scan rate of 50 mV/s. Such behaviour shall be attributed to the presence of at least two W atoms of different surroundings in the lattice structure of h-WO{sub 3} nanorods. On the other hand, in aqueous LiClO{sub 4} solution, only one redox process is observed at the scan rate of 10 mV/s. The above observations can be explained in terms of differences in the diffusion of ions inside two types of channel cavities existing in the structure of the h-WO{sub 3} nanorods. Moreover, the material can be applied as active support for the catalytic bi-metallic Pt-Ru nanoparticles during electrooxidation of ethanol in acid medium (0.5 mol dm{sup -3} H{sub 2}SO{sub 4}).

  18. Hexagonal nanorods of tungsten trioxide: Synthesis, structure, electrochemical properties and activity as supporting material in electrocatalysis

    International Nuclear Information System (INIS)

    Salmaoui, Samiha; Sediri, Faouzi; Gharbi, Neji; Perruchot, Christian; Aeiyach, Salah; Rutkowska, Iwona A.; Kulesza, Pawel J.; Jouini, Mohamed

    2011-01-01

    Tungsten trioxide, unhydrated with hexagonal structure (h-WO 3 ), has been prepared by hydrothermal method at a temperature of 180 o C in acidified sodium tungstate solution. Thus prepared h-WO 3 has been characterized by X-ray diffraction (XRD) method and using electrochemical techniques. The morphology has been examined by scanning and transmission electron microscopies (SEM and TEM) and it is consistent with existence of nanorods of 50-70 nm diameter and up to 5 μm length. Cyclic voltammetric characterization of thin films of h-WO 3 nanorods has revealed reversible redox behaviour with charge-discharge cycling corresponding to the reversible lithium intercalation/deintercalation into the crystal lattice of the h-WO 3 nanorods. In propylene carbonate containing LiClO 4 , two successive redox processes of hexagonal WO 3 nanorods are observed at the scan rate of 50 mV/s. Such behaviour shall be attributed to the presence of at least two W atoms of different surroundings in the lattice structure of h-WO 3 nanorods. On the other hand, in aqueous LiClO 4 solution, only one redox process is observed at the scan rate of 10 mV/s. The above observations can be explained in terms of differences in the diffusion of ions inside two types of channel cavities existing in the structure of the h-WO 3 nanorods. Moreover, the material can be applied as active support for the catalytic bi-metallic Pt-Ru nanoparticles during electrooxidation of ethanol in acid medium (0.5 mol dm -3 H 2 SO 4 ).

  19. Hexagonal nanorods of tungsten trioxide: Synthesis, structure, electrochemical properties and activity as supporting material in electrocatalysis

    Science.gov (United States)

    Salmaoui, Samiha; Sediri, Faouzi; Gharbi, Néji; Perruchot, Christian; Aeiyach, Salah; Rutkowska, Iwona A.; Kulesza, Pawel J.; Jouini, Mohamed

    2011-07-01

    Tungsten trioxide, unhydrated with hexagonal structure (h-WO 3), has been prepared by hydrothermal method at a temperature of 180 °C in acidified sodium tungstate solution. Thus prepared h-WO 3 has been characterized by X-ray diffraction (XRD) method and using electrochemical techniques. The morphology has been examined by scanning and transmission electron microscopies (SEM and TEM) and it is consistent with existence of nanorods of 50-70 nm diameter and up to 5 μm length. Cyclic voltammetric characterization of thin films of h-WO 3 nanorods has revealed reversible redox behaviour with charge-discharge cycling corresponding to the reversible lithium intercalation/deintercalation into the crystal lattice of the h-WO 3 nanorods. In propylene carbonate containing LiClO 4, two successive redox processes of hexagonal WO 3 nanorods are observed at the scan rate of 50 mV/s. Such behaviour shall be attributed to the presence of at least two W atoms of different surroundings in the lattice structure of h-WO 3 nanorods. On the other hand, in aqueous LiClO 4 solution, only one redox process is observed at the scan rate of 10 mV/s. The above observations can be explained in terms of differences in the diffusion of ions inside two types of channel cavities existing in the structure of the h-WO 3 nanorods. Moreover, the material can be applied as active support for the catalytic bi-metallic Pt-Ru nanoparticles during electrooxidation of ethanol in acid medium (0.5 mol dm -3 H 2SO 4).

  20. Synthesis, crystal structure and magnetic properties of an alternating manganese chain

    International Nuclear Information System (INIS)

    Ramos Silva, Manuela; Matos Beja, Ana; Antonio Paixao, Jose; Martin-Gil, Jesus

    2006-01-01

    A new 1D complex has been prepared and characterized. X-ray single crystal structure confirms that the Mn(II) ions assemble in alternating chains with Mn-Mn distances of 3.8432(13) and 4.4428(14) A. A 3D network of hydrogen bonds links the chains together. The temperature dependence of the magnetic susceptibility reveals that this compound undergoes a magnetic transition and exhibits an antiferromagnetic interaction in the low-temperature phase with two alternating exchange interactions of -2.32(1) and -5.55(1) cm -1 . - Graphical abstract: Portion of the dimeric manganese chain showing the two alternating exchange interactions paths

  1. Synthesis, structure and magnetic properties of CoFe_2O_4 nanomaterial by coprecipitation method

    International Nuclear Information System (INIS)

    Nguyen Anh Tien; Hoang Thi Tuyet

    2015-01-01

    CoFe_2O_4 spinel nanomaterial has been synthesized by coprecipitation method through the hydrolysis of Co(II) and Fe(III) cations in boiling water. The results of DTA/TGA/DrTGA, XRD, TEM methods showed that CoFe_2O_4 crystals formed after a calcination at 700 °C exhibited structure of cubic with the particles size of 30-50 nm, H_c = 1526.89 Oe, M_s = 41.703 emu/g, M_r = 19.545 emu/g. (author)

  2. Synthesis, properties, and crystal structure of complex Cp2Yb(DAD)

    International Nuclear Information System (INIS)

    Trifonov, A.A.; Kirillov, E.N.; Bochkarev, M.N.; Shumani, G.; Myule, S.

    1999-01-01

    Diazadiene complex of trivalent ytterbium Cp 2 Yb(DAD) (1) (DAD = Bu 1 -N CH-CH = N-Bu 1 ) was obtained by three routes: the oxidation of Cp 2 Yb(THF) 2 by diazadiene in tetrahydrofuran (THF), the reaction of Cp 2 YbCl with DAD 2- Na 2 + (2:1), and the reaction of Cp 2 YbCl(THF) with DAD - K + in the 1:1 ratio. Complex 1 was characterized by microanalysis, IR spectroscopy, magnetochemistry, and X-ray structural analysis [ru

  3. Synthesis, structure and electrical properties of a new tin vanadium selenide

    Energy Technology Data Exchange (ETDEWEB)

    Atkins, Ryan, E-mail: atkins@uoregon.edu [Department of Chemistry and Materials Science Institute, University of Oregon, Eugene, OR 97403 (United States); Disch, Sabrina, E-mail: disch@ill.fr [Institut Laue-Langevin (ILL), F-38042 Grenoble (France); Jones, Zachary, E-mail: zjones@chem.ucsb.edu [Department of Chemistry and Materials Science Institute, University of Oregon, Eugene, OR 97403 (United States); Haeusler, Ines, E-mail: haeusler@physik.hu-berlin.de [Novel Materials, Humboldt-Universität zu Berlin, Newtonstr. 15, 12489 Berlin (Germany); Grosse, Corinna, E-mail: Corinna.Grosse@physik.hu-berlin.de [Novel Materials, Humboldt-Universität zu Berlin, Newtonstr. 15, 12489 Berlin (Germany); Fischer, Saskia F., E-mail: Saskia.Fischer@physik.hu-berlin.de [Novel Materials, Humboldt-Universität zu Berlin, Newtonstr. 15, 12489 Berlin (Germany); Neumann, Wolfgang, E-mail: wsn@uoregon.edu [Department of Chemistry and Materials Science Institute, University of Oregon, Eugene, OR 97403 (United States); Zschack, Paul, E-mail: zschack@bnl.gov [Advanced Photon Source, Argonne National Laboratory, Argonne, IL 60439 (United States); Johnson, David C., E-mail: davej@uoregon.edu [Department of Chemistry and Materials Science Institute, University of Oregon, Eugene, OR 97403 (United States)

    2013-06-15

    The turbostratically disordered misfit layer compound (SnSe){sub 1.15}VSe{sub 2} was synthesized and structurally characterized. Electrical transport measurements suggest this compound undergoes a charge or spin density wave (CDW or SDW) transition, which has not been observed in previous misfit layer compounds. The (SnSe){sub 1.15}VSe{sub 2} compound, created through the modulated elemental reactants technique, contains highly oriented intergrowths of SnSe bilayers and VSe{sub 2} structured Se–V–Se trilayers with abrupt interfaces between them perpendicular to the c-axis. X-ray diffraction data and transmission electron microscope images show that each constituent has in-plane crystallinity but that there is a random rotational disorder between the constituent layers. Temperature-dependent electrical resistivity data and Hall measurements are consistent with (SnSe){sub 1.15}VSe{sub 2} being a metal, however an abrupt increase in the resistivity occurs between 30 and 100 K. The carrier concentration decreases by approximately 1 carrier per vanadium atom during this temperature interval. - Graphical abstract: Turbostratically disordered (SnSe){sub 1.15}VSe{sub 2}. - Highlights: • New compound (SnSe){sub 1.15}VSe{sub 2}. • Turbostratic disorder. • Charge density wave at 100 K.

  4. Facile synthesis of Zn doped CuO hierarchical nanostructures: Structural, optical and antibacterial properties

    Directory of Open Access Journals (Sweden)

    Javed Iqbal

    2015-12-01

    Full Text Available ZnxCu1−xO (where x= 0, 0.01, 0.03, 0.05, 0.07 and 0.1 mol% hierarchical nanostructures have been prepared via soft chemical route. X-ray diffraction (XRD results of the synthesized samples reveal the monoclinic structure of CuO without any impurity related phases. The micro-structural parameters such as crystallite size and microstrain have been strongly influenced by Zn doping. Scanning electron microscope (SEM analyses depict the formation of hierarchical nanostructures having average particle size in the range of 26-43 nm. The surface area of CuO nanostructures has been reduced systematically with the increase in Zn content which is linked with the variations in particle size. An obvious decrease in the optical band gap energy of the synthesized CuO hierarchical nanostructures has been observed with Zn doping which is assigned to the formation of shallow levels in the band gap of CuO and combined transition from oxygen 2p states to d sates of Cu and Zn ions. The bactericidal potency of the CuO hierarchical nanostructures have been found to be enhanced remarkably with Zn doping.

  5. Synthesis, crystal structure, and nonlinear optical properties of Bi2Cu5B4O14

    International Nuclear Information System (INIS)

    Pan Shilie; Smit, Jared P.; Marvel, Michael R.; Stampler, Evan S.; Haag, Jacob M.; Baek, Jaewook; Halasyamani, P. Shiv; Poeppelmeier, Kenneth R.

    2008-01-01

    Bi 2 Cu 5 B 4 O 14 crystallizes in the noncentrosymmetric triclinic space group P1 (No. 1) with cell parameters a=10.1381(11) A, b=9.3917(11) A, c=3.4566(4) A, α=105.570(2) o , β=92.275(2) o , γ=107.783(2) o , Z=1 and R 1 =0.0401 and wR 2 =0.0980. It is a layered structure that is built up from sheets of rectangular CuO 4 and trigonal BO 3 groups. The sheets are connected by infinite chains of edge shared BiO 6 polyhedra that intersect the bc plane at an angle slightly greater than 90 o . The second-harmonic generation efficiency of Bi 2 Cu 5 B 4 O 14 , using 1064 nm radiation, is about one half times that of KH 2 PO 4 . - Graphical abstract: The figure shows a layered structure that is built up from sheets of distorted rectangular CuO 4 and trigonal BO 3 groups. The sheets are connected by infinite chains of edge shared BiO 6 polyhedra that intersect the bc plane. These distortions lead to the second-harmonic generation efficiency of Bi 2 Cu 5 B 4 O 14 about one half times that of KH 2 PO 4 Display Omitted

  6. Synthesis, structural and paramagnetic properties of SnO{sub 2} doped NiO nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Islam, I., E-mail: ishtihadahislam@gmail.com; Dwivedi, Sonam; Dar, Hilal A.; Dar, M. A.; Varshney, Dinesh, E-mail: vdinesh33@rediffmail.com [School of Physics, Vigyan Bhawan, Devi Ahilya University, Khandwa Road Campus, Indore 452001 (India)

    2016-05-06

    In this work, Sn doped NiO nanoparticles were synthesized by co-precipitation route to explore the impact of doping on lattice structure, dielectric constant and magnetization. X-ray diffraction analysis confirmed cubic (Fd-3m) structure of Sn doped NiO. Average crystallite size decreases from 78.2 nm (Ni{sub 0.95}Sn{sub 0.05}O) to 64.23 nm (Ni{sub 0.8}Sn{sub 0.2}O). Scanning electron microscopy images confirm that nanocrystals have agglomerated spherical morphology. The Raman spectrum exhibits a strong, broad peak at 410 cm{sup -1} and is attributed to the Ni-O stretching mode and doped samples show a blue shift. The dielectric constants at about 1 Hz are measured to be about 1.795, 1.030, 0.442, and 0.302 × 10{sup 3} Ni{sub 1-x}Sn{sub x}O (x = 0.05, 0.1, 0.15, 0.2), respectively. The dielectric constant in nanoparticles of doped Ni{sub 1-x}Sn{sub x}O is three orders of magnitude higher as compared to pure NiO ceramics. The nature of magnetization - applied field (M-H) infers paramagnetic behaviour for Sn doped NiO nanoparticles.

  7. Synthesis, structure and electrical properties of a new tin vanadium selenide

    International Nuclear Information System (INIS)

    Atkins, Ryan; Disch, Sabrina; Jones, Zachary; Haeusler, Ines; Grosse, Corinna; Fischer, Saskia F.; Neumann, Wolfgang; Zschack, Paul; Johnson, David C.

    2013-01-01

    The turbostratically disordered misfit layer compound (SnSe) 1.15 VSe 2 was synthesized and structurally characterized. Electrical transport measurements suggest this compound undergoes a charge or spin density wave (CDW or SDW) transition, which has not been observed in previous misfit layer compounds. The (SnSe) 1.15 VSe 2 compound, created through the modulated elemental reactants technique, contains highly oriented intergrowths of SnSe bilayers and VSe 2 structured Se–V–Se trilayers with abrupt interfaces between them perpendicular to the c-axis. X-ray diffraction data and transmission electron microscope images show that each constituent has in-plane crystallinity but that there is a random rotational disorder between the constituent layers. Temperature-dependent electrical resistivity data and Hall measurements are consistent with (SnSe) 1.15 VSe 2 being a metal, however an abrupt increase in the resistivity occurs between 30 and 100 K. The carrier concentration decreases by approximately 1 carrier per vanadium atom during this temperature interval. - Graphical abstract: Turbostratically disordered (SnSe) 1.15 VSe 2 . - Highlights: • New compound (SnSe) 1.15 VSe 2 . • Turbostratic disorder. • Charge density wave at 100 K

  8. Synthesis, growth, structural, optical and thermal properties of a new organic salt crystal: 3-nitroanilinium trichloroacetate

    Science.gov (United States)

    Selvakumar, E.; Chandramohan, A.; Anandha Babu, G.; Ramasamy, P.

    2014-09-01

    A new organic non-linear optical salt 3-nitroanilinium trichloroacetate has been synthesized and single crystals grown by slow solvent evaporation solution growth technique at room temperature using methanol as the solvent. The 1H and 13C Nuclear magnetic resonance spectra were recorded to establish the molecular structure of the title salt. The crystal structure of the title crystal has been determined by single crystal X-ray diffraction analysis and it belongs to monoclinic crystal system with non-centrosymmetric space group P21. Fourier transform infrared spectral study has been carried out to confirm the presence of various functional groups. The optical transmittance spectrum was recorded in the range 200-2500 nm, to find the optical transmittance window and lower cut off wavelength. The thermo gravimetric and differential thermal analyses were carried out to establish the thermal stability of the title crystal. The second harmonic generation in the title crystal was confirmed by the modified Kurtz-Perry powder test employing the Nd: YAG laser as the source for infrared radiation.

  9. Facile synthesis of Zn doped CuO hierarchical nanostructures: Structural, optical and antibacterial properties

    Energy Technology Data Exchange (ETDEWEB)

    Iqbal, Javed, E-mail: tariqjan84@gmail.com, E-mail: javed.suggau@iiu.edu.pk; Jan, Tariq, E-mail: tariqjan84@gmail.com, E-mail: javed.suggau@iiu.edu.pk; Ul-Hassan, Sibt; Umair Ali, M.; Abbas, Fazal [Laboratory of Nanoscience and Technology, Department of Physics, International Islamic University, H-10, Islamabad (Pakistan); Ahmed, Ishaq [Experimental Physics Labs, National Center for Physics, Islamabad (Pakistan); Mansoor, Qaisar; Ismail, Muhammad [Institute of Biomedical and Genetic Engineering (IBGE), Islamabad (Pakistan)

    2015-12-15

    Zn{sub x}Cu{sub 1−x}O (where x= 0, 0.01, 0.03, 0.05, 0.07 and 0.1 mol%) hierarchical nanostructures have been prepared via soft chemical route. X-ray diffraction (XRD) results of the synthesized samples reveal the monoclinic structure of CuO without any impurity related phases. The micro-structural parameters such as crystallite size and microstrain have been strongly influenced by Zn doping. Scanning electron microscope (SEM) analyses depict the formation of hierarchical nanostructures having average particle size in the range of 26-43 nm. The surface area of CuO nanostructures has been reduced systematically with the increase in Zn content which is linked with the variations in particle size. An obvious decrease in the optical band gap energy of the synthesized CuO hierarchical nanostructures has been observed with Zn doping which is assigned to the formation of shallow levels in the band gap of CuO and combined transition from oxygen 2p states to d sates of Cu and Zn ions. The bactericidal potency of the CuO hierarchical nanostructures have been found to be enhanced remarkably with Zn doping.

  10. Synthesis, X-ray Structure, Spectroscopic Properties and DFT Studies of a Novel Schiff Base

    Directory of Open Access Journals (Sweden)

    Kew-Yu Chen

    2014-10-01

    Full Text Available A series of Schiff bases, salicylideneaniline derivatives 1–4, was synthesized under mild conditions and characterized by 1H NMR, HRMS, UV-Vis and fluorescence spectra, and single-crystal X-ray diffraction. In solid and aprotic solvents 1–4 exist mainly as E conformers that possess an intramolecular six-membered-ring hydrogen bond. A weak intramolecular C–H×××F hydrogen bond is also observed in fluoro-functionalized Schiff base 4, which generates another S(6 ring motif. The C–H×××F hydrogen bond further stabilizes its structure and leads it to form a planar configuration. Compounds 1–3 exhibit solely a long-wavelength proton-transfer tautomer emission, while dipole-functionalized Schiff base 4 shows remarkable dual emission originated from the excited-state intramolecular charge transfer (ESICT and excited-state intramolecular proton transfer (ESIPT states. Furthermore, the geometric structures, frontier molecular orbitals (MOs and the potential energy curves for 1–4 in the ground and the first singlet excited state were fully rationalized by density functional theory (DFT and time-dependent DFT calculations.

  11. Two novel metal-organic coordination polymers based on diphosphonate and oxalate: Synthesis, structures and properties

    Science.gov (United States)

    Niu, Qing-Jun; Zheng, Yue-Qing; Zhou, Lin-Xia; Zhu, Hong-Lin

    2015-07-01

    Two 2-(1-imidazole)-1-hydroxyl-1,1'-ethylidenediphosphonato and oxalic acid bridged coordination polymers (H2en)[Co3(H2zdn)2(ox)(H2O)2] (1) and Cd2(H2zdn)(ox)0.5(H2O) (2) (2-(1-imidazole)-1-hydroxyl-1,1'-ethylidenediphosphonic acid=H5zdn; oxalic acid=H2ox) were synthesized under hydrothermal conditions and characterized by the infrared (IR), thermogravimetric analyses (TGA), elemental analyses (EA) and X-ray diffraction (XRD). Compound 1 is bridged by phosphonate anions to 1D chain, and further linked by oxalate anions to 2D layer. Compound 2 is bridged by O-P-O units of H5zdn to the layer, and then pillared by oxalate anions to generate 3D frameworks. Compound 1 shows anti-ferromagnetic behaviors analyzed with the temperature-dependent zero-field ac magnetic susceptibilities, while compound 2 exhibits an influence on the luminescent property.

  12. Conventional hydrothermal synthesis of titanate nanotubes: Systematic discussions on structural, optical, thermal and morphological properties

    Directory of Open Access Journals (Sweden)

    S. Muniyappan

    2017-12-01

    Full Text Available Titanate nanotubes were successfully synthesized by hydrothermal technique under acidic-base medium. The anatase and titanate phase of the starting TiO2 and tubular titanate was confirmed by powder XRD technique. The UV–vis-NIR spectroscopy was used to study the absorption nature of titanate nanotubes and the band gap was calculated as 3.3 eV. Infrared technique was employed to detect the presence of all the functional groups in the synthesized titanate nanotube material. Thermal properties of the title material were studied by TG-DTA analyses. The shrinkage of interlayer distance of TiO2 network confirms the nanotube formation. Morphology and size information about the synthesized material were carried out using FESEM and TEM analysis. Titanate nanotubes are having the maximum length of 2.24 µm and the average diameter of 169.73 nm. EDX analysis gives out the elemental composition of the as synthesized product. This report may fetch an efficient way to synthesize TiO2 nanotubes using TiO2 nanoparticles.

  13. Synthesis, structure and electromagnetic properties of Mn-Zn ferrite by sol-gel combustion technique

    Science.gov (United States)

    Wang, Wenjie; Zang, Chongguang; Jiao, Qingjie

    2014-01-01

    The electromagnetic absorbing behaviors of a thin coating fabricated by mixing Mn-Zn ferrite with epoxy resin (EP) were studied. The spinel ferrites Mn1-xZnxFe2O4 (x=0.2, 0.5 and 0.8) were synthesized with citrate acid as complex agent by sol-gel combustion method. The microstructure and surface morphology of Mn-Zn ferrite powders were characterized by X-ray diffraction (XRD) and scanning electron microscope (SEM). The complex permittivity and complex permeability of the fabricated ferrite/EP composites were investigated in terms of their contributions to the absorbing properties in the low frequency (10 MHz to 1 GHz). The microwave absorption of the prepared ferrite/EP composites could be tailored by matching the dielectric loss and magnetic loss and by controlling the doped metal ratio. The composites with the ferrite composition x=0.2 are found to show higher reflection loss compared with the composites with other compositions. It is proposed that the prepared composites can potentially be applied in electromagnetic microwave absorbing field.

  14. Synthesis, structure, and magnetic properties of two 1-D helical coordination polymeric Cu(II) complexes

    Science.gov (United States)

    Bian, He-Dong; Yang, Xiao-E.; Yu, Qing; Chen, Zi-Lu; Liang, Hong; Yan, Shi-Ping; Liao, Dai-Zheng

    2008-01-01

    Two helical coordination polymeric copper(II) complexes bearing amino acid Schiff bases HL or HL', which are condensed from 2-hydroxy-1-naphthaldehyde with 2-aminobenzoic acid or L-valine, respectively, have been prepared and characterised by X-ray crystallography. In [CuL] n ( 1) the copper(II) atoms are bridged by syn- anti carboxylate groups giving infinite 1-D right-handed helical chains which are further connected by weak C-H⋯Cu interactions to build a 2-D network. While in [CuL'] n ( 2) the carboxylate group acts as a rare monatomic bridge to connect the adjacent copper(II) atoms leading to the formation of a left-handed helical chain. Magnetic susceptibility measurements indicate that 1 exhibits weak ferromagnetic interactions whereas an antiferromagnetic coupling is established for 2. The magnetic behavior can be satisfactorily explained on the basis of the structural data.

  15. Synthesis, band structure, and optical properties of Ba2ZnV2O8

    International Nuclear Information System (INIS)

    Chen, D.-G.; Cheng, W.-D.; Wu, D.-S.; Zhang, H.; Zhang, Y.-C.; Gong, Y.-J.; Kan, Z.-G.

    2004-01-01

    A novel compound Ba 2 ZnV 2 O 8 has been synthesized in high temperature solution reaction and its crystal structure has been characterized by means of single crystal X-ray diffraction analysis. It crystallizes in monoclinic system and belongs to space group P2 1 /c with a=7.9050(16), b=16.149(3), c=6.1580(12)A, β=90.49(3). It builds up from 1-D branchy chains of [ZnV 2 O 8 4- ] ∞ , and the Ba 2+ cations are located in the space among these chains. The IR spectrum, ultraviolet-visible diffuse reflection integral spectrum and fluorescent spectra of this compound have been investigated. The calculated results of energy band structure by the density functional theory method show that the solid-state compound of Ba 2 ZnV 2 O 8 is an insulator with direct band gap of 3.48eV. The calculated total and partial density of states indicate that the top valence bands are contributions from the mixings of O-2p, V-3d, and Zn-3d states and low conduction bands mostly originate from unoccupied antibonding states between the V-3d and O-2p states. The V-O bonds are mostly covalence characters and Zn-O bonds are mostly ionic interactions, and the ionic interaction strength is stronger between the Ba-O than between the Zn-O. The refractive index of n x , n y , and n z is estimated to be 1.7453, 1.7469, and 1.7126, respectively, at wavelength of 1060nm for Ba 2 ZnV 2 O 8 crystal

  16. Ionothermal synthesis, structures, properties of cobalt-1,4-benzenedicarboxylate metal–organic frameworks

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Zong-Hui [Key Laboratory of Macromolecular Science of Shaanxi Province, School of Chemistry & Chemical Engineering, Shaanxi Normal University, Xi’an 710062, Shaanxi Province (China); State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences, Fsuzhou, Fujian 350002 (China); Xu, Ling, E-mail: xuling@snnu.edu.cn [Key Laboratory of Macromolecular Science of Shaanxi Province, School of Chemistry & Chemical Engineering, Shaanxi Normal University, Xi’an 710062, Shaanxi Province (China); Jiao, Huan, E-mail: jiaohuan@snnu.edu.cn [Key Laboratory of Macromolecular Science of Shaanxi Province, School of Chemistry & Chemical Engineering, Shaanxi Normal University, Xi’an 710062, Shaanxi Province (China)

    2016-06-15

    Eight kinds of 1-methyl-3-alkylimidazolium halide [RMI]X (R=ethyl (E), propyl (P), butyl (B) and amyl (A); MI = imidazolium; X= Cl{sup −}, I{sup −}) ionic liquids (ILs) were used as reaction media and obtained a series of 2D [RMI]{sub 2}[Co{sub 3}(BDC){sub 3}X{sub 2}] frameworks through the ionothermal reactions of 1,4-benzenedicarboxylic acid (H{sub 2}BDC) with Co(NO{sub 3}){sub 2}·6H{sub 2}O. The 2D [RMI]{sub 2}[Co{sub 3}(BDC){sub 3}X{sub 2}] frameworks exhibit a same (3,6) topology network with [RMI]{sup +} cations locating in the interlayer space. [RMI]{sup +} cations play a template role in the structure constructions, whose influence combining with the effect of X{sup −} anions pass to the TG behaviors. The decomposition temperatures of the [RMI]{sub 2}[Co{sub 3}(BDC){sub 3}X{sub 2}] frameworks decrease with the alkyl chains in [RMI]{sup +} cations, and the compounds containing Cl{sup −} show higher thermal stabilities than those with I{sup −}. However, compounds 1–8 exhibit two similar broad emissions at ca. 380 and 390 nm, assigned to ILCT. The RMI{sup +} templates and the X{sup −} anions do not exert their influence on the fluorescence. - Graphical abstract: Eight 2D [RMI]{sub 2}[Co{sub 3}(BDC){sub 3}X{sub 2}] compounds were synthesized through ionothermal reactions. [RMI]{sup +} cations play a template role in the structure constructions, and tune the TG behaviors combining with the effect of X{sup −} anions. Display Omitted.

  17. Synthesis, Structural, Optical and Dielectric Properties of Nanostructured 0-3 PZT/PVDF Composite Films.

    Science.gov (United States)

    Revathi, S; Kennedy, L John; Basha, S K Khadheer; Padmanabhan, R

    2018-07-01

    Nanostructured PbZr0.52Ti0.48O3 (PZT) powder was synthesized at 500 °C-800 °C using sol-gel route. X-ray diffraction and Rietveld analysis confirmed the formation of perovskite structure. The sample heat treated at 800 °C alone showed the formation of morphotropic phase boundary with coexistence of tetragonal and rhombohedral phase. The PZT powder and PVDF were used in 0-3 connectivity to form the PZT/PVDF composite film using solvent casting method. The composite films containing 10%, 50%, 70% and 80% volume fraction of PZT in PVDF were fabricated. The XRD spectra validated that the PZT structure remains unaltered in the composites and was not affected by the presence of PVDF. The scanning electron microscopy images show good degree of dispersion of PZT in PVDF matrix and the formation of pores at higher PZT loading. The quantitative analysis of elements and their composition were confirmed from energy dispersive X-ray analysis. The optical band gap of the PVDF film is 3.3 eV and the band gap decreased with increase in volume fraction of PZT fillers. The FTIR spectra showed the bands corresponding to different phases of PVDF (α, β, γ) and perovskite phase of PZT. The thermogravimetric analysis showed that PZT/PVDF composite films showed better thermal stability than the pure PVDF film and hydrophobicity. The dielectric constant was measured at frequency ranging from 1 Hz to 6 MHz and for temperature ranging from room temperature to 150 °C. The composite with 50% PZT filler loading shows the maximum dielectric constant at the studied frequency and temperature range with flexibility.

  18. Synthesis, crystal structure and optical property of three coordination polymer constructed from m-phenylenediacrylate acid

    Energy Technology Data Exchange (ETDEWEB)

    Xiao, YiFan; Wang, TingTing; Zeng, HePing, E-mail: hpzeng@scut.edu.cn

    2015-01-15

    Three new complexes of the wholly deprotonated flexible ligand m-phenylenediacrylate acid (H{sub 2}mpda), namely, [Zn (mpda) (H{sub 2}O)] [1], [Pr{sub 2}(mpda){sub 2}(H{sub 2}O){sub 2}(CHOO){sub 2}] [2], and [Mn{sub 2}(mpda){sub 2} (H{sub 2}O){sub 4}] [3], were synthesized by the solvothermal reaction. The complexes were characterized by IR spectroscopy, thermogravimetric analysis, and X-ray single-crystal diffraction. A mixed sample [Nd(mpda)(H{sub 2}O)(CHOO)·Pr(mpda)(H{sub 2}O)(CHOO)] [2{sup ]} was also synthesized and studied. Compounds [1] and [2] exhibit a selective sensing function with respect to acetone, and they are a potential luminescent sensory material for the selective detection of Zn{sup 2+} and Ni{sup 2+} ions, respectively. Furthermore, the fluorescent changes of compound [1] upon the addition of cations (Fe{sup 3+} and Zn{sup 2+}, Bi{sup 2+} and Zn{sup 2+}) are utilized to construct two logic gates at the molecular level. - Graphical abstract: Three new complexes of flexible ligand m-phenylenedicarboxylic acid were synthesized by solvothermal reaction. Three metal−organic frameworks exhibiting 1D, 2D, 3D structures, respectively. - Highlights: • Three new complexes of m-phenylenedicarboxylic acid were synthesized. • Three metal−organic frameworks exhibiting 1D, 2D, 3D structures, respectively. • [1] and [2] exhibits a very high quenching effect with acetone. • [1] and [2] are a potential luminescent sensory material for Zn{sup 2+}, Ni{sup 2+} ions. • Two logic gates have been constructed using compound [1].

  19. Synthesis, structure and electromagnetic properties of Mn–Zn ferrite by sol–gel combustion technique

    International Nuclear Information System (INIS)

    Wang, Wenjie; Zang, Chongguang; Jiao, Qingjie

    2014-01-01

    The electromagnetic absorbing behaviors of a thin coating fabricated by mixing Mn–Zn ferrite with epoxy resin (EP) were studied. The spinel ferrites Mn 1−x Zn x Fe 2 O 4 (x=0.2, 0.5 and 0.8) were synthesized with citrate acid as complex agent by sol–gel combustion method. The microstructure and surface morphology of Mn–Zn ferrite powders were characterized by X-ray diffraction (XRD) and scanning electron microscope (SEM). The complex permittivity and complex permeability of the fabricated ferrite/EP composites were investigated in terms of their contributions to the absorbing properties in the low frequency (10 MHz to 1 GHz). The microwave absorption of the prepared ferrite/EP composites could be tailored by matching the dielectric loss and magnetic loss and by controlling the doped metal ratio. The composites with the ferrite composition x=0.2 are found to show higher reflection loss compared with the composites with other compositions. It is proposed that the prepared composites can potentially be applied in electromagnetic microwave absorbing field. - Highlights: • We designed and synthesized Mn 1−x Zn x Fe 2 O 4 (x=0.2, 0.5 and 0.8), with citrate acid as complex agent by the sol–gel combustion method. • Citrate acid as the complex agent overcomes the aggregation of ferrite resulting in high purity and homogeneous particles. • We investigated the electromagnetic absorbing performance of a fabricated thin coating by introducing Mn–Zn ferrite into epoxy resin (EP). • The Mn 0.8 Zn 0.2 Fe 2 O 4 composite coatings could achieve the satisfactory absorbing value of −17 dB at 800 MHz. • The prepared composites can potentially be used for the application in electromagnetic microwave absorbing field

  20. 1D cyanide complexes with 2-pyridinemethanol: Synthesis, crystal structures and spectroscopic properties

    Science.gov (United States)

    Sayın, Elvan; Kürkçüoğlu, Güneş Süheyla; Yeşilel, Okan Zafer; Hökelek, Tuncer

    2015-12-01

    Two new one-dimensional coordination polymers, [Cu(hmpH)2Pd(μ-CN)2(CN)2]n (1) and [Cu(hmpH)2Pt(μ-CN)2(CN)2]n (2), (hmpH = 2-pyridinemethanol), have been synthesized and characterized by vibrational (FT-IR and Raman) spectroscopy, single crystal X-ray diffraction, thermal and elemental analyses techniques. Single crystal X-ray diffraction analysis indicates that complexes 1 and 2 are isomorphous and isostructural, and crystallize in the triclinic system and P-1 space group. The Pd(II) or Pt(II) ions are four coordinated with four cyanide-carbon atoms in a square planar geometry. Cu(II) ion displays a distorted octahedral coordination by two N-atoms and two O-atoms of hmpH ligands, two bridging cyanide groups. In one dimensional structure of the complexes, [M(CN)4]2- (M = Pd(II) or Pt(II)) anions and [Cu(hmpH)2]2+ cations are linked via bridging cyanide ligands. In the complexes, the presence of intramolecular C-H⋯M (M = Pd(II) or Pt(II)) interactions with distance values of 3.00-2.95 Å are established, respectively.

  1. Hydrothermal synthesis, structure, and catalytic properties of UO2Sb2O4

    International Nuclear Information System (INIS)

    Sykora, Richard E.; King, Joseph E.; Illies, Andreas J.; Albrecht-Schmitt, Thomas E.

    2004-01-01

    A new uranyl antimonite, UO 2 Sb 2 O 4 (1), has been prepared from the hydrothermal reaction of UO 3 with Sb 2 O 3 and KCl. The structure of 1 consists of neutral two-dimensional ∞ 2 [UO 2 Sb 2 O 4 ] layers. The U(VI) centers are ligated by two trans oxo ligands and four square pyramidal antimonite anions. In addition, the U(VI) also forms long contacts with two additional oxygen atoms that are distorted by 12.7(2) degree sign out of the equatorial plane perpendicular to the uranyl unit. These long interactions are significant owing to evidence supplied by bond valence sum calculations. The two-dimensional layers found in 1 are built from one-dimensional chains formed from edge-sharing UO 6 octahedra that run along the b-axis, and are linked together by [Sb 2 O 4 ] 2- chains. A flow microreactor system has been used to study the catalytic activity of 1, and these results show that it can be used as a catalyst in the conversion of propene and O 2 to acrolein. Crystallographic data: 1, monoclinic, space group C2/m, a=13.490(2) A, b=4.0034(6) A, c=5.1419(8) A, β=104.165(3) deg., Z=2, MoKα, λ=0.71073, R(F)=1.74% for 30 parameters with 365 reflections with I>2σ(I)

  2. Synthesis, X-ray Structure, Optical, and Electrochemical Properties of a White-Light-Emitting Molecule

    Directory of Open Access Journals (Sweden)

    Jiun-Wei Hu

    2016-01-01

    Full Text Available A new white-light-emitting molecule (1 was synthesized and characterized by NMR spectroscopy, high resolution mass spectrometry, and single-crystal X-ray diffraction. Compound 1 crystallizes in the orthorhombic space group Pnma, with a = 12.6814(6, b = 7.0824(4, c = 17.4628(9 Å, α = 90°, β = 90°, γ = 90°. In the crystal, molecules are linked by weak intermolecular C-H···O hydrogen bonds, forming an infinite chain along [100], generating a C(10 motif. Compound 1 possesses an intramolecular six-membered-ring hydrogen bond, from which excited-state intramolecular proton transfer (ESIPT takes place from the phenolic proton to the carbonyl oxygen, resulting in a tautomer that is in equilibrium with the normal species, exhibiting a dual emission that covers almost all of the visible spectrum and consequently generates white light. It exhibits one irreversible one-electron oxidation and two irreversible one-electron reductions in dichloromethane at modest potentials. Furthermore, the geometric structures, frontier molecular orbitals (MOs, and the potential energy curves (PECs for 1 in the ground and the first singlet excited state were fully rationalized by density functional theory (DFT and time-dependent DFT calculations. The results demonstrate that the forward and backward ESIPT may happen on a similar timescale, enabling the excited-state equilibrium to be established.

  3. Synthesis Structural and Optical Properties Of (Co, Al) co-doped ZnO Nano Particles

    Science.gov (United States)

    Swapna, P.; Venkatramana Reddy, S.

    2018-02-01

    We prepared (Co, Al) co-doped ZnO nanostructures using the method chemical co-precipitation successfully, at room temperature using PEG (Poly ethylene glycol) as stabilizing agent. Samples are prepared with different concentrations by keeping aluminium at 5 mol percent constant and varying the concentration of cobalt from 1 to 5 mol percent. After the preparation all the samples are carefully subjected to characterizations such as XRD, SEM with EDS, TEM, PL and UV-VIS-NIR. XRD pattern shows that all the samples possess hexagonal wurtzite crystal structure having no secondary phases pertaining to Al or cobalt, which shows successful dissolution of the dopents. TEM results shows the accurate size of particles and is confirmed the XRD data. SEM images of all the samples shows that particles are in nearly spherical shape, EDS spectrum reveals that incorporation of cobalt and aluminum in host lattice. PL spectrum shows that all the samples containing two prominent peaks centered at 420 nm and 446 nm. UV-VIS-NIR spectra has shown three absorptions peaks in the range of wavelength 550 nm to 700 nm, which are ascribed as typical d-d transitions of cobalt ions.

  4. Synthesis, optical, structural, and electrical properties of single-crystalline CdS nanobelts

    Energy Technology Data Exchange (ETDEWEB)

    Alqahtani, Mohammed S. [King Saud University, Department of Physics and Astronomy, Riyadh (Saudi Arabia); Hadia, N.M.A.; Mohamed, S.H. [Sohag University, Physics Department, Faculty of Science, Sohag (Egypt)

    2017-04-15

    CdS nanobelts (NBs) were synthesized by vapor transport of CdS powders. The growth was carried out without any catalyst on quartz and Si (100) substrates. The synthesized CdS NBs were examined by transmission electron microscopy (TEM), field emission scanning electron microscopy (FE-SEM) and selected area electron diffraction (SAED), high-resolution transmission electron microscopy (HR-TEM), X-ray powder diffraction (XRD), energy dispersion analysis of X-ray (EDAX), spectrophotometer, and photoluminescence spectroscopy. CdS NBs were indexed as hexagonal wurtzite structure. The growth was via vapor-solid growth mechanism and along the [100] direction. The refractive index was evaluated in the transparent region, as suggested by Swanepoel, using the envelope method. The refractive index values and the extinction coefficient were decreased by increasing the wavelength. The calculated optical band gap was 2.50 eV. The photoluminescence (PL) spectrum of the synthesized CdS NBs exhibited a green emission peak at 510 nm and a broad red emission peak at 696 nm. The conductivity measurements were achieved, in the temperature range from 300 to 600 K, using the conventional two-probe technique. Two different slopes with different activation energies of 0.618 and 0.215 eV were obtained. The CdS NBs are likely being novel functional materials. Thus, they can be used in the manufacture of innovative optoelectronic nanodevices. (orig.)

  5. Halide/pseudohalide complexes of cadmium(II) with benzimidazole: Synthesis, crystal structures and fluorescence properties

    Science.gov (United States)

    Zhao, Hai-Yan; Yang, Fu-Li; Li, Na; Wang, Xiao-Jing

    2017-11-01

    Two new dinuclear Cd(II) complexes, [CdL1Cl2]2·H2O (1) and [CdL1(N3)2]2·CH3OH (2) and one dicyanamide bridged one-dimensional polynuclear network [CdL1(μ1,5-dca)dca]n (3) of the potentially tridentate NNN-donor Schiff base 2-((1H-benzimidazol-2-yl-ethylimino)-methyl)pyridine (L1) and another dinucler Cd(II) complex [CdL2Cl(dca)]2 (4) of a similar NNN-donor Schiff base ligand 2-((1H-benzimidazol-2-yl-propylimino)-methyl)pyridine (L2), have been synthesized and characterized by elemental analyses, IR and single crystal X-ray crystallography. The ligands L1 and L2 are [1 + 1] condensation products of pyridine-2-carbaldehyde with 2-aminoethyl-1H-benzimidazole and 2-aminopropyl-1H-benzimidazole, respectively. In the complexes 1 and 4 the two Cd(II) centers are held together by the bridged chloride ligands, while in 2 the two Cd(II) centers are bridged by μ1,1-azide ions. Complex 3 has a one-dimensional infinite chain structure in which Cd(II) ions are bridged by single dicyanamide groups in end-to-end fashion. All the metal centers have a distorted octahedral geometry and H-bonding or π⋯π interactions are operative to bind the complex units in the solid state. Furthermore, these complexes have been investigated by thermogravimetric analyses and fluorescence spectra.

  6. Synthesis, Crystal Structural Characterization and Biological Properties of Thiosemicarbazones of Schiff Bases Derived from 4-Acyl-2-pyrazoline-5-one

    Directory of Open Access Journals (Sweden)

    Arjunsinh Rana

    2011-01-01

    Full Text Available A novel synthesis, single crystal and biological activity of 4-acylthiosemicarbazone-3-methyl-1-(4`-methylphenyl-2-pyrazolin-5-one by condensation of 4-acyl-3-methyl-1-(4`-methylphenyl-2-pyrazolin-5-one with thiosemicarbazide was carried out. The compounds were characterized on the basis of elemental analysis, IR, 1H NMR, Mass, DSC and 13C NMR spectral data. The compounds were tested for their antibacterial activity against various gram +ve and -ve bacteria. The results were compared with the marketed drugs. The crystal structure was determined by single x-ray diffraction. 4-Acetyl thiosemicarbazone-3-methyl-1-(4`-methylphenyl-2-pyrazolin-5-one(AcPTMP-ths crystallizes in the monoclinic system, space group P21/n with a=6.0828(7Å, b=29.547(4Å, c=7.9101(15Å, α=90°, γ=95.602(15°, γ=90°, V=1414.9(4 Å3, Z=4, Dc=1.429 mg/m3 and 4-Propionylthiosemicarbazone-3-methyl-1-(4`-methylphenyl-2-pyrazolin-5-one (PropPTMP-ths crystallizes in the monoclinic system, space group P21/c with a=13.5622(10Å, b=13.3671(12Å, c=22.151(2Å, α=90°, β=93.13(7°, γ=90°, V=4010.1(6 Å3, Z=8, Dc=1.310 mg/m3. The compounds were screened for antibacterial properties and exhibited potential activity.

  7. Synthesis of Ag2O nanocrystals with systematic shape evolution from cubic to hexapod structures and their surface properties.

    Science.gov (United States)

    Lyu, Lian-Ming; Wang, Wei-Ching; Huang, Michael H

    2010-12-17

    We report the development of a facile method for the synthesis of Ag(2)O crystals with systematic shape evolution from cubic to edge- and corner-truncated cubic, rhombicuboctahedral, edge- and corner-truncated octahedral, octahedral, and hexapod structures by mixing AgNO(3), NH(4)NO(3), and NaOH at molar ratios of 1:2:11.8. A sufficient volume of NaOH solution was first added to a mixture of AgNO(3) and NH(4)NO(3) solution to promote the formation of Ag(NH(3))(2)(+) complex ions and the growth of Ag(2)O nanocrystals with good morphological control. The crystals are mostly submicrometer-sized. X-ray diffraction, scanning electron microscopy, and transmission electron microscopy characterization has been performed to determine the crystalline surface facets. A band gap value of approximately 1.45 eV has been found for the octahedral Ag(2)O crystals. By changing the molar ratios of AgNO(3)/NH(4)NO(3)/NaOH to 1:2:41.8, corner-depressed rhombicuboctahedra and elongated hexapods were obtained as a result of enhanced crystal growth along the [100] directions. Smaller nanocubes with average sizes of approximately 200 and 300 nm and octapods can also be prepared by adjusting the reagent molar ratios and their added volumes. Both the octahedra and hexapods with largely silver atom-terminated {111} surface facets responded repulsively and moved to the surface of the solution when dispersing in a solution of positively charged methylene blue, but can be suspended in a negatively charged methyl orange solution. The cubes and octapods, bounded by the {100} faces, were insensitive to the molecular charges in solution. The dramatic facet-dependent surface properties of Ag(2)O crystals have been demonstrated.

  8. Synthesis, properties, structure and thermochemistry of hexa-aqua-tris (N,N-dimethylformamide) lanthanide tri fluoro methane sulfonates

    International Nuclear Information System (INIS)

    Araujo Melo, D.M. de.

    1989-01-01

    Addition compounds between several lanthanide salts and dimethylformamide (DMF) have been described in the literature. This thesis reports the synthesis and characterization of the compounds of general composition Ln (C H 3 SO 3 ) 3 . 3 DMF.6 H 3 O) (Ln = La - Ho) and Ln (C H 3 SO 3 ) 3 DMF.6 H 2 O (Ln = Er - Lu). The structure of the neodymium compound, isomorphous with the series, is also described. The enthalpy variations were determined by solution calorimetry. (author)

  9. Synthesis, crystal structure, and transport properties of Fe substituted rhombohedral skutterudite derivatives Co4−xFexGe6Se6

    KAUST Repository

    Wei, Kaya

    2014-11-01

    We report on the synthesis and low temperature transport properties of rhombohedral derivatives of the cubic skutterudite CoSb3, namely Co4-xFexGe6Se6 with x = 0, 1, 1.5. Rietveld refinement and elemental analyses were used to identify the structure and stoichiometry of the compositions. The thermal conductivity was investigated by employing the Debye model with different phonon-scattering parameters. This investigation demonstrates that Fe substitution is feasible in these skutterudite derivatives and can significantly affect the transport properties as compared with Co4Ge6Se6. © 2014 Elsevier B.V. All rights reserved.

  10. Synthesis, crystal structure, and transport properties of Fe substituted rhombohedral skutterudite derivatives Co4−xFexGe6Se6

    KAUST Repository

    Wei, Kaya; Dong, Yongkwan; Puneet, Pooja; Tritt, Terry M.; Nolas, George S.

    2014-01-01

    We report on the synthesis and low temperature transport properties of rhombohedral derivatives of the cubic skutterudite CoSb3, namely Co4-xFexGe6Se6 with x = 0, 1, 1.5. Rietveld refinement and elemental analyses were used to identify the structure and stoichiometry of the compositions. The thermal conductivity was investigated by employing the Debye model with different phonon-scattering parameters. This investigation demonstrates that Fe substitution is feasible in these skutterudite derivatives and can significantly affect the transport properties as compared with Co4Ge6Se6. © 2014 Elsevier B.V. All rights reserved.

  11. Synthesis of C-di-saccharidic compounds by radical cyclisation. Study of biological, structural and dynamic properties

    International Nuclear Information System (INIS)

    Rubinstenn, Gilles

    1996-01-01

    The synthesis of carbohydrate mimics and particularly of C-disaccharides, molecules in which the inter-glycosidic oxygen atom has been replaced by a methylene group, has become, this past two decades, an important challenge in organic chemistry. In the first chapter we present the synthesis of C-disaccharides from the neutral series by a silaketal tethering. The key step of this C-glycosylation is a radical macro-cyclisation. This strategy is applied to the synthesis of two analogues of natural, biologically active, products, the lactose and the Lewis x tri-saccharide. The biological activity of this mimetics is then evaluated. A new tethering strategy, based on the use of phosphorus III compounds, is applied, in the second chapter, to the building of C-disaccharides of the 2'-amino 2'- deoxy series. The third chapter deals with the structural and dynamics study of the C-glycosides prepared in chapter 1 by Nuclear Magnetic Resonance. A new methodology, studying the dipolar relaxation along an effective field, generated through an off-resonance RF field, allowed the precise measurement of longitudinal and transverse cross-relaxation rates. Structural and dynamics parameter thus derived are used as restraints for molecular modeling. The results of this study are then compared to those of the biological tests. (author) [fr

  12. One dimensional CuO nanocrystals synthesis by electrical explosion: A study on structural, optical and electronic properties

    Energy Technology Data Exchange (ETDEWEB)

    Krishnan, Shutesh, E-mail: shutesh.k@onsemi.com [Department of Mechanical Engineering University of Malaya, 50603 Kuala Lumpur (Malaysia); ON Semiconductor Package Innovation and Development Center, 70450 Seremban (Malaysia); Haseeb, A.S.M.A.; Johan, Mohd Rafie [Department of Mechanical Engineering University of Malaya, 50603 Kuala Lumpur (Malaysia)

    2014-02-15

    Highlights: • One-dimensional CuO nanoflakes were synthesized by novel wire explosion technique. • A physical synthesis method capable of producing high aspect ratio (1:16) nanocrystals. • Most energy efficient and eco-friendly synthesis of low-dimensional transition metal oxide nanocrystals. -- Abstract: One-dimensional (1D) copper oxide (CuO) nanocrystals were synthesized using a novel wire explosion in de-ionized (DI) water without any chemical additives. Highly crystalline 1D CuO nanocrystals with 1:16 aspect ratio were successfully synthesized using this technique. The chemical nature and physical structure of the nanocrystals were controlled by simply modulating the exploding medium temperature. The results showed that nanocrystals produced at explosion temperatures 65 °C and 95 °C are pure CuO with optical band-gap energy of 2.38 eV. High Resolution Transmission Electron Microscope analysis (HRTEM) indicates that the CuO nanocrystals are with growth in [1{sup ¯}11] and [1 1 1] directions. The epitaxial crystal growth kinetics of the 1D nanostructure by aggregation was discussed. The incorporation of microstructural features like edge dislocations and porosity in the growth mechanism was examined. X-ray photoelectron spectroscopy (XPS) characterization indicates the formation of high purity CuO nanocrystals with valence state +2. This study provides an energy efficient and eco-friendly synthesis method of 1D transition metal oxide nanocrystals for electronic applications.

  13. One dimensional CuO nanocrystals synthesis by electrical explosion: A study on structural, optical and electronic properties

    International Nuclear Information System (INIS)

    Krishnan, Shutesh; Haseeb, A.S.M.A.; Johan, Mohd Rafie

    2014-01-01

    Highlights: • One-dimensional CuO nanoflakes were synthesized by novel wire explosion technique. • A physical synthesis method capable of producing high aspect ratio (1:16) nanocrystals. • Most energy efficient and eco-friendly synthesis of low-dimensional transition metal oxide nanocrystals. -- Abstract: One-dimensional (1D) copper oxide (CuO) nanocrystals were synthesized using a novel wire explosion in de-ionized (DI) water without any chemical additives. Highly crystalline 1D CuO nanocrystals with 1:16 aspect ratio were successfully synthesized using this technique. The chemical nature and physical structure of the nanocrystals were controlled by simply modulating the exploding medium temperature. The results showed that nanocrystals produced at explosion temperatures 65 °C and 95 °C are pure CuO with optical band-gap energy of 2.38 eV. High Resolution Transmission Electron Microscope analysis (HRTEM) indicates that the CuO nanocrystals are with growth in [1 ¯ 11] and [1 1 1] directions. The epitaxial crystal growth kinetics of the 1D nanostructure by aggregation was discussed. The incorporation of microstructural features like edge dislocations and porosity in the growth mechanism was examined. X-ray photoelectron spectroscopy (XPS) characterization indicates the formation of high purity CuO nanocrystals with valence state +2. This study provides an energy efficient and eco-friendly synthesis method of 1D transition metal oxide nanocrystals for electronic applications

  14. Synthesis,crystal structure and properties of inorganic-organic hybrid polymers based on 8-hydroxylquinoline-5-sulfonic acid

    Institute of Scientific and Technical Information of China (English)

    2009-01-01

    Two new inorganic-organic hybrid polymers, Mn(QS)(H2O) (1) and Co(QS)(H2O)2 (2) (H2QS=8-hydroxyl-quinoline-5-sulfonic acid), based on 8-hydroxylquinoline-5-sulfonate ligand, have been synthesized under solvothermal conditions and their structures were solved by single-crystal X-ray diffraction analysis. Compound 1 is a three-dimensional open framework with rutile topology structure, and compound 2 is a three-dimensional supramolecular structure. These compounds were characterized by powder XRD, infrared spectroscopy, thermogravimetric analysis, fluorescence properties and magnetism properties.

  15. Synthesis, Structure, and Film Properties of Novel low-k UV-active Polycarbosilanes with Embedded Disilacyclobutanes

    Science.gov (United States)

    LeFevre, Scott W.

    The phenylene-bridged cyclolinear polycarbosilane (PBCLPCS) was synthesized via Grignard coupling from 1,4-bis(bromomagnesio)benzene with 1,3-dichloro-, and 1,3-diethoxy-1,3-disilacyclobutanes (DCDSCB, and DEDSCB respectively). Investigation of the resulting chemical structures by nuclear magnetic resonance spectroscopy (NMR) revealed a wide array of possible end groups and thus termination mechanisms. Temperature-gradient interaction chromatography (TGIC) was employed as an effective separation tool to achieve a predominantly monomer-by-monomer separation of the low molecular weight reaction products. Further analysis of the TGIC fractions by matrix-assisted laser desorption ionization mass spectrometry with time of flight detection (MALDI-ToF) allowed for a much more detailed study of chemical structure, revealing very different primary modes of termination for the two synthesis schemes. While the slightly more reactive Si-Cl groups from DCDSCB are more sensitive to multiple side reactions including hydrolysis, it was shown that the primary end groups were phenyl rings, indicating a possible imbalance in stoichiometry favoring the aryl-Grignard reagent. The DEDSCB-based synthesis has fewer side reactions, as indicated by few groupings of MALDI peaks at regular intervals equal to the repeat unit molecular weight; however the primary end groups were unreacted ethoxy moieties, and a bromine terminated phenyl ring. This indicates that the primary modes of termination were either limited chain growth from the less reactive ethoxy groups, or incomplete formation of the di-Grignard. The optical, UV-curing and thin film characteristics of PBCLPCS were investigated to gain an understanding of the unique film properties of this new class of material. Upon UV-curing PBCLPCS, the chromophore blue shifts 11nm but still absorbs appreciably at 254nm, leading to UV attenuation at greater depths within a film. The thickness dependent UV-curing characteristics were investigated

  16. Polyfuran Conducting Polymers: Synthesis, Properties, and Applications.

    OpenAIRE

    González-Tejera, M.J.; Sánchez de la Blanca, Emilia; Carrillo Ramiro, Isabel

    2008-01-01

    In this review, polyfuran (PFu) synthesis methods and the nucleation mechanism; the electrochemical, structural, morphological, and magnetic properties of PFu; thermal behavior; theoretical calculations on PFu, as well as its applications reported to date, have been compiled. Not only PFu homopolymers have been reviewed, but also PFu co-polymers, PFu bipolymers, and PFu composites. The results are listed, discussed, and compared. It is hoped that this assembly of all the relevant data might e...

  17. Bismuth-, Tin-, and Lead-Containing Metal-Organic Materials: Synthesis, Structure, Photoluminescence, Second Harmonic Generation, and Ferroelectric Properties

    Science.gov (United States)

    Wibowo, Arief Cahyo

    Metal-Organic Materials (MOMs) contain metal moieties and organic ligands that combine to form discrete (e.g. metal-organic polyhedra, spheres or nanoballs, metal-organic polygons) or polymeric structures with one-, two-, or three-dimensional periodicities that can exhibit a variety of properties resulting from the presence of the metal moieties and/or ligand connectors in the structure. To date, MOMs with a range of functional attributes have been prepared, including record-breaking porosity, catalytic properties, molecular magnetism, chemical separations and sensing ability, luminescence and NLO properties, multiferroic, ferroelectric, and switchable molecular dielectric properties. We are interested in synthesizing non-centrosymmetric MOM single crystals possessing one of the ten polar space groups required for non-linear optical properties (such as second harmonic generation) and ferroelectric applications. This thesis is divided into two main parts: materials with optical properties, such as photoluminescence and materials for targeted applications such as second harmonic generation and ferroelectric properties. This thesis starts with an introduction describing material having centrosymmetric, non-polar space groups, single crystals structures and their photoluminescence properties. These crystals exhibit very interesting and rare structures as well as interesting photoluminescence properties. Chapters 2-5 of this thesis focus on photoluminescent properties of new MOMs, and detail the exploratory research involving the comparatively rare bismuth, lead, and tin coordination polymers. Specifically, the formation of single white-light emitting phosphors based on the combination of bismuth or lead with pyridine-2,5-dicarboxylate is discussed (Chapter 2). The observation of a new Bi2O2 layer and a new Bi4O 3 chain in bismuth terephthalate-based coordination polymers is presented in Chapter 3, while the formation of diverse structures of tin-based coordination

  18. Photoluminescent Copper(I) Complex Based on 3-(2-(Cyclohexylthio) ethoxy)pyridine: Synthesis, Structure, and Physical Properties

    Energy Technology Data Exchange (ETDEWEB)

    Park, Hyunjin; Kwon, Eunjin; Kang, Gihaeng; Kim, Jieun; Kim, Tae Ho [Gyeongsang National University, Jinju (Korea, Republic of)

    2016-07-15

    In recent years, the Cu(I) complexes, with d 10 electronic configuration, have been attracting interest due to their diverse structures and photophysical properties. A copper(I) coordination polymer 1 based on a sulfur-containing pyridyl ligand L was synthesized and identified by X-ray crystallography. Photophysical and thermal properties of 1 have been investigated. More Cu(I) coordination polymers based on mixed donor ligands are under investigation in order to discover factors governing luminescence wavelength, such as Cu[BOND]Cu distances, intermolecular interactions, structures of ligands, and so on.

  19. Hybrid nanostructures: synthesis, morphology and functional properties

    International Nuclear Information System (INIS)

    Povolotskaya, A V; Povolotskiy, A V; Manshina, A A

    2015-01-01

    Hybrid nanostructures representing combinations of different materials and possessing properties that are absent in separate components forming the hybrid are discussed. Particular attention is given to hybrid structures containing plasmonic and magnetic nanoparticles, methods of their synthesis and the relationship between the composition, structure and properties. The functional features of the hybrid nanomaterials of various morphology (with core–shell structures, with encapsulated metal nanoparticles and with metal nanoparticles on the surface) are considered. The unique properties of these hybrid materials are demonstrated, which are of interest for solving problems of catalysis and photocatalysis, detecting impurities in various media, in vivo visualization, bioanalysis, as well as for the design of optical labels and multifunctional diagnostic nanoplatforms. The bibliography includes 182 references

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

    Directory of Open Access Journals (Sweden)

    Lkhamsuren Bayarjargal

    2011-09-01

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

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

    Science.gov (United States)

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

    2011-01-01

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

  2. Modeling of alkynes: synthesis and theoretical properties

    Directory of Open Access Journals (Sweden)

    Renato Rosseto

    2003-06-01

    Full Text Available In this paper we present the synthesis and simulation of alkynes derivatives. Semiempirical calculations were carried out for the ground and first excited states, including the spectroscopic properties of the absorption and emission (fluorescence and phosphorescence spectra by INDO/S-CI and DNdM-INDO/S-CI methods with geometries fully optimized by PM3/CI. The fact that the theoretical spectra are in accord with the experimental absorption spectra gives us a new possible approach on how structure modifications could affect the non-linear optical properties of alkynes.

  3. Iron(iii) bis(pyrazol-1-yl)acetate based decanuclear metallacycles: synthesis, structure, magnetic properties and DFT calculations.

    Science.gov (United States)

    Gajewska, Małgorzata J; Bieńko, Alina; Herchel, Radovan; Haukka, Matti; Jerzykiewicz, Maria; Ożarowski, Andrzej; Drabent, Krzysztof; Hung, Chen-Hsiung

    2016-09-27

    The synthesis, structural aspects, magnetic interpretation and theoretical rationalizations for a new member of the ferric wheel family, a decanuclear iron(iii) complex with the formula [Fe 10 (bdtbpza) 10 (μ 2 -OCH 3 ) 20 ] (1), featuring the N,N,O tridentate bis(3,5-di-tert-butylpyrazol-1-yl)acetate ligand, are reported. The influence of the steric effect on both the core geometry and coordination mode is observed. Temperature dependent (2.0-300 K range) magnetic susceptibility studies carried out on complexes 1 established unequivocally antiferromagnetic (AF) interactions between high-spin iron(iii) centers (S = 5/2), leading to a ground state S = 0. The mechanism of AF intramolecular coupling was proved using a broken-symmetry approach within the density functional method at the B3LYP/def2-TZVP(-f)/def2-SVP level of theory.

  4. Microwave combustion synthesis of hexagonal prism shaped ZnO nanoparticles and effect of Cr on structural, optical and electrical properties of ZnO nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Yathisha, R.O. [Department of Chemistry, School of Chemical Sciences, Kuvempu University, Jnanasahyadri, Shankaraghatta 577 451, Karnataka (India); Nayaka, Y. Arthoba, E-mail: drarthoba@yahoo.co.in [Department of Chemistry, School of Chemical Sciences, Kuvempu University, Jnanasahyadri, Shankaraghatta 577 451, Karnataka (India); Vidyasagar, C.C. [Department of Chemistry, School of Basic Sciences, Ranichannamma University, Belgaum 591156, Karnataka (India)

    2016-09-15

    The synthesis and study of semiconducting nanostructure materials have become a considerable interdisciplinary area of research over the past few decades. The control of morphologies and effective doping by right dopant are the two tasks for the synthesis of semiconducting nanoparticles. The present work outlines the synthesis of ZnO and Cr-ZnO nanoparticles via microwave combustion method without using any fuel. The crystal morphology, optical and electrical properties were characterized by X-ray diffraction study (XRD), UV–Visible spectroscopy (UV–Vis), Scanning electron microscopy (SEM), Energy-dispersive analysis using X-rays (EDAX), Transmission electron microscopy (TEM) and Keithley source meter. The crystal size was determined from XRD, whose values were found to be decreased with increase in the concentration of Cr up to 2 wt% and further increase in the dopant concentration resulted the formation secondary phase (ZnCr{sub 2}O{sub 4}). Scanning electron micrographs shows the hexagonal prism structure of ZnO and Cr-ZnO nanoparticles. EDAX shows the existence of Cr ion in the Cr-ZnO. The optical properties and bandgap studies were undertaken by UV–Visible spectroscopy. I-V characterization study was performed to determine the electrical property of ZnO and Cr-ZnO films. - Highlights: • The prism shaped Zn{sub 1−x}Cr{sub x}O (0 ≤ x ≤ 0.15) was prepared by microwave combustion method. • Effect of Cr on the properties of ZnO was reported. • Change in crystal size was explained by lattice strain and Zener-Pinning effect. • The optical measurements shows up to 8 wt% of Cr doping had more efficient. • Compared to ZnO, Cr doped ZnO enhance the photo voltaic activity.

  5. Actinide tris(hydrocarbyls). Synthesis, properties, structure, and molecular dynamics of thorium and uranium pentamethylcyclopentadienyl tris(eta/sup n/-benzyls)

    International Nuclear Information System (INIS)

    Mintz, E.A.; Moloy, K.G.; Marks, T.J.; Day, V.W.

    1982-01-01

    This report focuses on the synthesis, unusual molecular structure(s), and other interesting properties of ligands within a metal coordination sphere (cf. M(eta 5 -C 5 H 5 ) 3 R vs. M[eta 5 -(CH 3 ) 5 ] 2 R 2 chemistry, where M=Th or U). This report represents a continuing effort to ''tune'' the actinide ligation environment with respect to such factors as the chemical characteristics of actinide-to-carbon sigma bonds. These bonds are a sensitive function of the number and nature of the other ligands within the metal coordination sphere. Structural analysis is reported that examines the nature and arrangement of the bonds in Th[eta 5 -(CH 3 ) 5 C 5 ](CH 2 C 6 H 5 ) 3 and U[eta 5 -(CH 3 ) 5 C 5 ](CH 2 C 6 H 5 ) 3 complexes

  6. Synthesis, structural investigation and magnetic properties of Zn2+ substituted cobalt ferrite nanoparticles prepared by the sol–gel auto-combustion technique

    International Nuclear Information System (INIS)

    Raut, A.V.; Barkule, R.S.; Shengule, D.R.; Jadhav, K.M.

    2014-01-01

    Structural morphology and magnetic properties of the Co 1−x Zn x Fe 2 O 4 (0.0≤x≥1.0) spinel ferrite system synthesized by the sol–gel auto-combustion technique using nitrates of respective metal ions have been studied. The ratio of metal nitrates to citric acid was taken at 1:3. The as prepared powder of cobalt zinc ferrite was sintered at 600 °C for 12 h after TG/DTA thermal studies. Compositional stoichiometry was confirmed by energy dispersive analysis of the X-ray (EDAX) technique. Single phase cubic spinel structure of Co–Zn nanoparticles was confirmed by XRD data. The average crystallite size (t), lattice constant (a) and other structural parameters of zinc substituted cobalt ferrite nanoparticles were calculated from XRD followed by SEM and FTIR. It is observed that the sol–gel auto-combustion technique has many advantages for the synthesis of technologically applicable Co–Zn ferrite nanoparticles. The present investigation clearly shows the effect of the synthesis method and possible relation between magnetic properties and microstructure of the prepared samples. Increase in nonmagnetic Zn 2+ content in cobalt ferrite nanoparticles is followed by decrease in n B , M s and other magnetic parameters. Squareness ratio for the Co-ferrite was 1.096 at room temperature. - Highlights: • Co–Zn nanoparticles are prepared by sol–gel auto-combustion method. • Structural properties were characterized by XRD, SEM, and FTIR. • Compositional stoichiometry was confirmed by EDAX analysis. • Magnetic parameters were measured by the pulse field hysteresis loop technique

  7. Synthesis, structural investigation and magnetic properties of Zn{sup 2+} substituted cobalt ferrite nanoparticles prepared by the sol–gel auto-combustion technique

    Energy Technology Data Exchange (ETDEWEB)

    Raut, A.V., E-mail: nano9993@gmail.com [Vivekanand Arts and Sardar Dalipsingh Commerce and Science College, Aurangabad, 431004 Maharastra (India); Barkule, R.S.; Shengule, D.R. [Vivekanand Arts and Sardar Dalipsingh Commerce and Science College, Aurangabad, 431004 Maharastra (India); Jadhav, K.M., E-mail: drjadhavkm@gmail.com [Department of Physics, Dr. Babasaheb Ambedkar Marathwada University, Aurangabad, 431004 Maharastra (India)

    2014-05-01

    Structural morphology and magnetic properties of the Co{sub 1−x}Zn{sub x}Fe{sub 2}O{sub 4} (0.0≤x≥1.0) spinel ferrite system synthesized by the sol–gel auto-combustion technique using nitrates of respective metal ions have been studied. The ratio of metal nitrates to citric acid was taken at 1:3. The as prepared powder of cobalt zinc ferrite was sintered at 600 °C for 12 h after TG/DTA thermal studies. Compositional stoichiometry was confirmed by energy dispersive analysis of the X-ray (EDAX) technique. Single phase cubic spinel structure of Co–Zn nanoparticles was confirmed by XRD data. The average crystallite size (t), lattice constant (a) and other structural parameters of zinc substituted cobalt ferrite nanoparticles were calculated from XRD followed by SEM and FTIR. It is observed that the sol–gel auto-combustion technique has many advantages for the synthesis of technologically applicable Co–Zn ferrite nanoparticles. The present investigation clearly shows the effect of the synthesis method and possible relation between magnetic properties and microstructure of the prepared samples. Increase in nonmagnetic Zn{sup 2+} content in cobalt ferrite nanoparticles is followed by decrease in n{sub B}, M{sub s} and other magnetic parameters. Squareness ratio for the Co-ferrite was 1.096 at room temperature. - Highlights: • Co–Zn nanoparticles are prepared by sol–gel auto-combustion method. • Structural properties were characterized by XRD, SEM, and FTIR. • Compositional stoichiometry was confirmed by EDAX analysis. • Magnetic parameters were measured by the pulse field hysteresis loop technique.

  8. Synthesis, growth, structure, mechanical and optical properties of a new semi-organic 2-methyl imidazolium dihydrogen phosphate single crystal

    Energy Technology Data Exchange (ETDEWEB)

    Nagapandiselvi, P., E-mail: nagapandiselvip@ssn.edu.in [Department of Physics, SSN College of Engineering, Kalavakkam (India); Baby, C. [Sophisticated Analytical Instrument Facility, Indian Institute of Technology Madras, Chennai (India); Gopalakrishnan, R. [Crystal Research Lab, Department of Physics, Anna University, Chennai (India)

    2016-09-15

    Highlights: • 2MIDP crystals were grown by slow evaporation solution growth technique. • Single crystal XRD revealed self-assembled supramolecular framework. • Z scan technique is employed for third order nonlinear optical susceptibility. • Structure-property correlation is established. - Abstract: A new semi-organic compound, 2-methyl imidazolium dihydrogen phosphate (2MIDP), was prepared and good quality single crystals of 2MIDP were grown by slow evaporation solution growth technique. Crystal structure elucidated using Single crystal XRD showed that 2MIDP crystallizes in monoclinic system with P2{sub 1}/c space group. FT-IR, UV-Vis-NIR, Fluorescence and FT-NMR spectra confirm the molecular structure of 2MIDP. The UV-Vis-NIR spectra established the suitability of the compound for NLO applications. TG-DSC showed that 2MIDP is thermally stable up to 200 °C. Mechanical characteristics like hardness number (H{sub v}), stiffness constant (C{sub 11}), yield strength (σ{sub v}), fracture toughness (K{sub c}) and brittleness index (B{sub i}) were assessed using Vicker’s microhardness tester. Third order nonlinear optical properties determined from Z-scan measurement using femto and picosecond lasers showed two photon reverse saturable absorption. The enhancement of nonlinear optical properties in femto second laser, revealed the suitability of 2MIDP for optical limiting applications.

  9. Properties and synthesis of milrinone

    Directory of Open Access Journals (Sweden)

    Mirković Jelena M.

    2013-01-01

    Full Text Available Milrinone, 1,6-dihydro-2-methyl-6-oxo-[3,4’-bipyridine]-5-carbonitrile, is a positive inotropic cardiotonic agent with vasodilator properties that acts as selective phosphodiesterase 3 inhibitor in cardiac and vascular smooth muscle. Trade names of milrinone are Primacor, Corotrop, Corotrope, and Milrila. Milrinone, an amrinone derivative, is 20 to 50 times more active than amrinone and possesses reduced propensity to side effects. The use of milrinone has created controversy in the medical as the result of increased mortality rate among patients that received high amounts of milrinone in oral form. Reaserch show that it can be benifitial for patients with severe congestive heart failure when used as short-time intravenous therapy. Milrinone properties, stability, as well as mechanism of action and synthesis under laboratory and industry conditions have been described in this paper. For industrial purposes milrinone is synthesized by condensation of cyanoacetamide with 4-(dimethylamino-3-(4-pyridinyl-3-buten-2-one and 4-ethoxy-3-(4-pyridinyl-3-buten-2-one in presence of a base, or by the reaction of 1-(4-pyridinyl- 2-propanone with ethoxymethylenmalononitrile or 4-alkoxy-3-(4-pyridinyl-3-buten-2-one with malononitrile without the use of external base. The starting compound for these syntheses is 4-picoline. Alternative synthesis of milrinone starts from 2-methyl-3-(4-pyridylidiene-1,1,5-tricyano-1,4-pentadiene-5-carboxamide and 2-methyl-6-oxo-1,6-dihydro-3,4’-bipyridine-5-carboxamide. Lastly, methods for milrinone synthesis in laboratory, injection preparation and purification have been summarized.

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-06-15

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

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

    International Nuclear Information System (INIS)

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

    2015-01-01

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

  12. Synthesis from zinc oxalate, growth mechanism and optical properties of ZnO nano/micro structures

    Energy Technology Data Exchange (ETDEWEB)

    Raj, C. Justin; Varma, K.B.R. [Materials Research Centre, Indian Institute of Science, Bangalore 560 012 (India); Joshi, R.K. [Special Center for Nano Sciences, Jawaharlal Nehru University, New Delhi 110067 (India)

    2011-11-15

    We report the synthesis of various morphological micro to nano structured zinc oxide crystals via simple precipitation technique. The growth mechanisms of the zinc oxide nanostructures such as snowflake, rose, platelets, porous pyramid and rectangular shapes were studied in detail under various growth conditions. The precursor powders were prepared using several zinc counter ions such as chloride, nitrate and sulphate along with oxalic acid as a precipitating agent. The precursors were decomposed by heating in air resulting in the formation of different shapes of zinc oxide crystals. Variations in ZnO nanostructural shapes were possibly due to the counter ion effect. Sulphate counter ion led to unusual rose-shape morphology. Strong ultrasonic treatment on ZnO rose shows that it was formed by irregular arrangement of micro to nano size hexagonal zinc oxide platelets. The X-ray diffraction studies confirmed the wurzite structure of all zinc oxide samples synthesized using different zinc counter ions. Functional groups of the zinc oxalate precursor and zinc oxide were identified using micro Raman studies. The blue light emission spectra of the various morphologies were recorded using luminescence spectrometer. (copyright 2011 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim) (orig.)

  13. Nitrides and carbides of molybdenum and tungsten with high specific-surface area: their synthesis, structure, and catalytic properties

    International Nuclear Information System (INIS)

    Volpe, L.

    1985-01-01

    Temperature-programmed reactions between trioxides of molybdenum or tungsten and ammonia provide a new method to synthesize dimolybdenum and ditungsten nitrides with specific surface areas to two-hundred-and-twenty and ninety-one square meters per gram, respectively. These are the highest values on record for any unsupported metallic powders. They correspond to three-four nonometer particles. The reaction of molybdenum trioxide with ammonia is topotactic in the sense that one-zero-zero planes of dimolybdenum nitride are parallel to zero-one-zero planes of molybdenum trioxide. As the trioxide transforms, it passes through an oxynitride intermediate with changing bulk structure and increasing surface area and extent of reduction. The nitride product consists of platelets, pseudomorphous with the original trioxide, which can be regarded as highly porous defect single crystals. By treating small particles of dimolybdenum or ditungsten nitride with methane-dihydrogen mixtures it is possible to replace interstitial nitrogen atoms by carbon atoms, without sintering, and thus to prepare carbides of molybdenum and tungsten with very high specific surface areas. Molybdenum nitride powders catalyze ammonia synthesis. A pronounced increase in the catalytic activity with increasing particle size confirms the structure-sensitive character of this reaction

  14. Synthesis, structure and optical properties of two isotypic crystals, Na3MO4Cl (M=W, Mo)

    International Nuclear Information System (INIS)

    Han, Shujuan; Bai, Chunyan; Zhang, Bingbing; Yang, Zhihua; Pan, Shilie

    2016-01-01

    Two isotypic compounds, Na 3 MO 4 Cl (M = W, Mo) have been obtained from the high temperature solution, and their structures were determined by single-crystal X-ray diffraction. Both of them crystallize in the space group P4/nmm of tetragonal system with the unit cells: a=7.5181(15), c=5.360(2) for Na 3 WO 4 Cl and a=7.4942(12), c=5.3409(18) for Na 3 MoO 4 Cl. The structure exhibits a 3D network built up by the ClNa 6 groups, and the MO 4 groups reside in the tunnels of the 3D network. The structural similarities and differences between Na 3 MO 4 Cl (M=W, Mo) and Sr 3 MO 4 F (M=Al, Ga) have been discussed. Meanwhile, detailed structure comparison analyses between Na 3 MO 4 Cl (M=W, Mo) and Na 3 MO 4 F (M=W, Mo) indicate that the different connection modes of ClNa 6 and FNa 6 make Na 3 MO 4 Cl and Na 3 MO 4 F crystallize in different structures. The IR spectra were used to verify the validity of the structure. The diffuse reflectance spectra show that the UV absorption edges are about 249 nm (4.99 eV) and 265 nm (4.69 eV) for Na 3 WO 4 Cl and Na 3 MoO 4 Cl, respectively. In addition, the first-principles theoretical studies are also carried out to aid the understanding of electronic structures and linear optical properties. - Graphical abstract: Two isotypic compounds, Na 3 MO 4 Cl (M=W, Mo) have been obtained from the high temperature solution. Both of them crystallize in the space group P4/nmm of tetragonal system. The structure exhibits a 3D network built up by the ClNa 6 groups, and the MO 4 groups reside in the tunnels of the 3D network. - Highlights: • Structure and properties of Na 3 MO 4 Cl (M=W, Mo) are reported for the first time. • They show a 3D network built by ClNa 6 , and WO 4 lies in the tunnels of the network. • IR spectra were used to verify the validity of the structure. • Band structures and density of states have been calculated.

  15. Synthesis, Structural and Optical Properties of TOPO and HDA Capped Cadmium Sulphide Nanocrystals, and the Effect of Capping Ligand Concentration

    Directory of Open Access Journals (Sweden)

    Damian C. Onwudiwe

    2015-01-01

    Full Text Available The thermal decomposition of bis(N,N-diallyldithiocarbamatoCd(II in a “one-pot” synthesis in tri-n-octylphosphine oxide (TOPO and hexadecylamine (HDA afforded CdS (TOPO-CdS and HDA-CdS of varying optical properties and morphologies. The influence of the ratio of the precursor concentration to the capping molecule, as a factor affecting the morphology and size of the nanoparticles, was investigated. The particles varied in shape from spheres to rods and show quantum size effects in their optical spectra with clear differences in the photoluminescence (PL spectra. The PL spectrum of the HDA capped CdS nanoparticles has an emission maximum centred at 468, 472, and 484 nm for the precursor to HDA concentration ratio of 1 : 10, 1 : 15, and 1 : 20, respectively, while the TOPO capped nanoparticles show emission peaks at 483, 494, and 498 nm at the same concentration ratio. Powdered X-ray diffraction (p-XRD shows the nanoparticles to be hexagonal. The crystallinity of the nanoparticles was evident from high resolution transmission electron microscopy (HRTEM which gave well-defined images of particles with clear lattice fringes.

  16. synthesis and structures

    Indian Academy of Sciences (India)

    Priya Saxena

    2017-08-29

    Aug 29, 2017 ... to a single crystal X-ray diffraction study for 1, 2 and 4-7. Keywords. Sterically .... 2.2b Mono-Schiff base 2: A suspension of I (1.00 g,. 2.27 mmol) and ...... bridge Crystallographic Data Centre, CCDC, 12 Union. Road, Cambridge .... H-C 2014 Rational design and synthesis of porous poly- mer networks: ...

  17. Structural synthesis of parallel robots

    CERN Document Server

    Gogu, Grigore

    This book represents the fifth part of a larger work dedicated to the structural synthesis of parallel robots. The originality of this work resides in the fact that it combines new formulae for mobility, connectivity, redundancy and overconstraints with evolutionary morphology in a unified structural synthesis approach that yields interesting and innovative solutions for parallel robotic manipulators.  This is the first book on robotics that presents solutions for coupled, decoupled, uncoupled, fully-isotropic and maximally regular robotic manipulators with Schönflies motions systematically generated by using the structural synthesis approach proposed in Part 1.  Overconstrained non-redundant/overactuated/redundantly actuated solutions with simple/complex limbs are proposed. Many solutions are presented here for the first time in the literature. The author had to make a difficult and challenging choice between protecting these solutions through patents and releasing them directly into the public domain. T...

  18. Synthesis, structural and semiconducting properties of Ba(Cu1/3 Sb2/3)O3-PbTiO3 solid solutions

    Science.gov (United States)

    Singh, Chandra Bhal; Kumar, Dinesh; Prashant, Verma, Narendra Kumar; Singh, Akhilesh Kumar

    2018-05-01

    We report the synthesis and properties of a new solid solution 0.05Ba(Cu1/3Sb2/3)O3-0.95PbTiO3 (BCS-PT) which shows the semiconducting properties. In this study, we have designed new perovskite-type (ABO3) solid solution of BCS-PT that have tunable optical band gap. BCS-PT compounds were prepared by conventional solid-state reaction method and their structural, micro-structural and optical properties were analyzed. The calcination temperature for BCS-PT solid solutions has been optimized to obtain a phase pure system. The Reitveld analysis of X-ray data show that all samples crystallize in tetragonal crystal structure with space group P4mm. X-ray investigation revealed that increase in calcination temperature led to increase of lattice parameter `a' while `c' parameter value lowered. The band gap of PbTiO3 is reduced from 3.2 eV to 2.8 eV with BCS doping and with increasing calcination temperature it further reduces to 2.56 eV. The reduced band gap indicated that the compounds are semiconducting and can be used for photovoltaic device applications.

  19. Nonlinear optical and G-Quadruplex DNA stabilization properties of novel mixed ligand copper(II) complexes and coordination polymers: Synthesis, structural characterization and computational studies

    Science.gov (United States)

    Rajasekhar, Bathula; Bodavarapu, Navya; Sridevi, M.; Thamizhselvi, G.; RizhaNazar, K.; Padmanaban, R.; Swu, Toka

    2018-03-01

    The present study reports the synthesis and evaluation of nonlinear optical property and G-Quadruplex DNA Stabilization of five novel copper(II) mixed ligand complexes. They were synthesized from copper(II) salt, 2,5- and 2,3- pyridinedicarboxylic acid, diethylenetriamine and amide based ligand (AL). The crystal structure of these complexes were determined through X-ray diffraction and supported by ESI-MAS, NMR, UV-Vis and FT-IR spectroscopic methods. Their nonlinear optical property was studied using Gaussian09 computer program. For structural optimization and nonlinear optical property, density functional theory (DFT) based B3LYP method was used with LANL2DZ basis set for metal ion and 6-31G∗ for C,H,N,O and Cl atoms. The present work reveals that pre-polarized Complex-2 showed higher β value (29.59 × 10-30e.s.u) as compared to that of neutral complex-1 (β = 0.276 × 10-30e.s.u.) which may be due to greater advantage of polarizability. Complex-2 is expected to be a potential material for optoelectronic and photonic technologies. Docking studies using AutodockVina revealed that complex-2 has higher binding energy for both G-Quadruplex DNA (-8.7 kcal/mol) and duplex DNA (-10.1 kcal/mol). It was also observed that structure plays an important role in binding efficiency.

  20. Synthesis, structural and microwave dielectric properties of Al2W3-xMoxO12 (x = 0-3) ceramics

    International Nuclear Information System (INIS)

    Surjith, A.; James, Nijesh K.; Ratheesh, R.

    2011-01-01

    Highlights: → Solid state synthesis of phase pure Al 2 W 3-x Mo x O 12 (x = 0-3) compositions. → Sintering studies of Al 2 W 3-x Mo x O 12 (x = 0-3) ceramics. → Structural and microstructural evaluation using powder X-ray diffraction and SEM studies. → Microwave dielectric property evaluation of Al 2 W 3-x Mo x O 12 (x = 0-3) ceramics through Hakki and Coleman post resonator and cavity perturbation techniques. → Structure-property correlation through Laser Raman studies. - Abstract: Low dielectric ceramics in the Al 2 W 3-x Mo x O 12 (x = 0-3) system have been prepared through solid state ceramic route. The phase purity of the ceramic compositions has been studied using powder X-ray diffraction (XRD) studies. The microstructure of the sintered ceramics was evaluated by Scanning Electron Microscopy (SEM). The crystal structure of the ceramic compositions as a result of Mo substitution has been studied using Laser Raman spectroscopy. The microwave dielectric properties of the ceramics were studied by Hakki and Coleman post resonator and cavity perturbation techniques. Al 2 Mo x W 3-x O 12 (x = 0-3) ceramics exhibited low dielectric constant and relatively high unloaded quality factor. The temperature coefficient of resonant frequency of the compositions is found to be in the range -41 to -72 ppm/deg. C.

  1. Hydrothermal synthesis, crystal structures, and luminescent properties of a series of new lanthanide oxalatophosphonates with a layer architecture.

    Science.gov (United States)

    Zhu, Yan-Yu; Sun, Zhen-Gang; Tong, Fei; Liu, Zhong-Min; Huang, Cui-Ying; Wang, Wei-Nan; Jiao, Cheng-Qi; Wang, Cheng-Lin; Li, Chao; Chen, Kai

    2011-05-28

    Eleven new lanthanide oxalatophosphonate hybrids with a 2D layered structures, namely, [Ln(H(3)L)(C(2)O(4))]·2H(2)O (Ln = La-Dy, Er and Y, H(4)L = C(6)H(5)CH(2)N(CH(2)PO(3)H(2))(2)), have been synthesized under hydrothermal conditions and structurally characterized by X-ray single-crystal diffraction, X-ray powder diffraction, infrared spectroscopy, elemental analysis and thermogravimetric analysis. Compounds 1-11 are isomorphous and they exhibit a 2D framework structure. Two {LnO(8)} polyhedra and four {CPO(3)} tetrahedra are interconnected into a unit via corner-sharing, and the so-built units are bridged by the oxalate anions into a layer. The result of connections in this manner is the formation of a 24-atom window. The thermal stabilities and guest desorption-sorption properties of compounds 1-11 have been investigated. The luminescent properties of compounds 5, 6, 8 and 9 have also been studied.

  2. Synthesis, crystal structure and luminescence properties of lanthanide coordination polymers with a new semirigid bridging thenylsalicylamide ligand

    International Nuclear Information System (INIS)

    Song, Xue-Qin; Wang, Li; Zhao, Meng-Meng; Wang, Xiao-Run; Peng, Yun-Qiao; Cheng, Guo-Quan

    2013-01-01

    Two new lanthanide coordination polymers based on a semirigid bridging thenylsalicylamide ligand ([Ln 2 L 3 (NO 3 ) 6 ]·(C 4 H 8 O 2 ) 2 ) ∞ were obtained and characterized by elemental analysis, X-ray diffraction, IR and TGA measurements. The two compounds are isostructure and possess one dimensional trapezoid ladder-like chain built up from the connection of isolated LnO 3 (NO 3 ) 3 polyhedra (distorted monocapped antisquare prism) through the ligand. The photoluminescence analysis suggest that there is an efficient ligand-to-Ln(III) energy transfer in Tb(III) complex and the ligand is an efficient “antenna” for Tb(III). From a more general perspective, the results demonstrated herein provide the possibility of controlling the formation of the desired lanthanide coordination structure to enrich the crystal engineering strategy and enlarge the arsenal for developing excellent luminescent lanthanide coordination polymers. - Graphical abstract: We present herein one dimensional lanthanide coordination polymers of a new semirigid exo-bidentate ligand which not only display interesting structures but also possess strong luminescence properties. Display Omitted - Highlights: • We present lanthanide coordination polymers of a new semirigid exo-bidentate ligand. • The lanthanide coordination polymers exhibit interesting structures. • The luminescent properties of Tb(III) complexes are discussed in detail

  3. Structure and Optical Properties of Titania-PDMS Hybrid Nanocomposites Prepared by In Situ Non-Aqueous Synthesis

    Directory of Open Access Journals (Sweden)

    Antoine R. M. Dalod

    2017-12-01

    Full Text Available Organic-inorganic hybrid materials are attractive due to the combination of properties from the two distinct types of materials. In this work, transparent titania-polydimethylsiloxane hybrid materials with up to 15.5 vol. % TiO2 content were prepared by an in situ non-aqueous method using titanium (IV isopropoxide and hydroxy-terminated polydimethylsiloxane as precursors. Spectroscopy (Fourier transform infrared, Raman, Ultraviolet-visible, ellipsometry and small-angle X-ray scattering analysis allowed to describe in detail the structure and the optical properties of the nanocomposites. Titanium alkoxide was successfully used as a cross-linker and titania-like nanodomains with an average size of approximately 4 nm were shown to form during the process. The resulting hybrid nanocomposites exhibit high transparency and tunable refractive index from 1.42 up to 1.56, depending on the titania content.

  4. Low pressure bottom-up synthesis of metal@oxide and oxide nanoparticles: control of structure and functional properties

    Science.gov (United States)

    D'Addato, Sergio; Chiara Spadaro, Maria

    2018-03-01

    Experimental activity on core@shell, metal@oxide, and oxide nanoparticles (NPs) grown with physical synthesis, and more specifically by low pressure gas aggregation sources (LPGAS) is reviewed, through a selection of examples encompassing some potential applications in nanotechnology. After an introduction to the applications of NPs, a brief description of the main characteristics of the growth process of clusters and NPs in LPGAS is given. Thereafter, some relevant case studies are reported: • Formation of native oxide shells around the metal cores in core@shell NPs. • Experimental efforts to obtain magnetic stabilization in magnetic core@shell NPs by controlling their structure and morphology. • Recent advancements in NP source design and new techniques of co-deposition, with relevant results in the realization of NPs with a greater variety of functionalities. • Recent results on reducible oxide NPs, with potentialities in nanocatalysis, energy storage, and other applications. Although this list is far from being exhaustive, the aim of the authors is to provide the reader a descriptive glimpse into the physics behind the growth and studies of low pressure gas-phase synthesized NPs, with their ever-growing potentialities for the rational design of new functional materials.

  5. A novel asymmetric chair-like hydroxyl-bridged tetra-copper compound: Synthesis, supramolecular structure and magnetic property

    Science.gov (United States)

    Wang, Xiao-Feng; Du, Ke-Jie; Wang, Hong-Qing; Zhang, Xue-Li; Nie, Chang-Ming

    2017-06-01

    A new polynuclear Cu(II) compound, [Cu4(bpy)4(OH)4(H2O)(BTC)]NO3·8H2O (1), was prepared by self-assembly from the solution of copper(II) nitrate and two kinds of ligands, 2,2‧-bipyridine (bpy) and benzene-tricarboxylic acid (H3BTC). Single crystal structure analysis reveals that 1 features a rare asymmetric chair-like hydroxyl-bridged tetra-copper cluster: [Cu4(OH)4] core along with one H2O and one BTC3- occupied each terminal coordinated site. In addition, the magnetic property has been investigated.

  6. Modulation of surface structure and catalytic properties of cerium oxide nanoparticles by thermal and microwave synthesis techniques

    Energy Technology Data Exchange (ETDEWEB)

    He, Jian [College of Pharmacy, Third Military Medical University, Chongqing 400038 (China); Zhou, Lan; Liu, Jie; Yang, Lu; Zou, Ling; Xiang, Junyu; Dong, Shiwu [School of Biomedical Engineering, Third Military Medical University, Chongqing 400038 (China); Yang, Xiaochao, E-mail: xcyang@tmmu.edu.cn [School of Biomedical Engineering, Third Military Medical University, Chongqing 400038 (China)

    2017-04-30

    Highlights: • The CNPs synthesized by microwave irradiation have more reactive hot spots than that synthesized by convective heating. • The CNPs synthesized by microwave irradiation exhibited higher SOD activity than that synthesized by convective heating. • The CNPs synthesized by microwave irradiation heating could better protect cells from oxidative stress. - Abstract: Cerium oxide nanoparticles (CNPs) have been intensively explored for biomedical applications in recent few years due to the versatile enzyme mimetic activities of the nanoparticles. However, the control of CNPs quality through the optimization of synthesis conditions remains largely unexplored as most of the previous studies only focus on utilizing the catalytic activities of the nanoparticles. In the present study, CNPs with size about 5 nm were synthesized by thermal decomposition method using traditional convective heating and recently developed microwave irradiation as heating source. The quality of CNPs synthesized by the two heating manner was evaluated. The CNPs synthesized by convective heating were slightly smaller than that synthesized by microwave irradiation heating. The cores of the CNPs synthesized by the two heating manner have similar crystal structure. While the surface subtle structures of the CNPs synthesized by two heating manner were different. The CNPs synthesized by microwave irradiation have more surface reactive hot spot than that synthesized by convective heating as the nanoparticles responded more actively to the redox environment variation. This difference resulted in the higher superoxide dismutase (SOD) mimetic activity of CNPs synthesized by microwave irradiation heating than that of the convective heating. Preliminary experiments indicated that the CNPs synthesized by microwave irradiation heating could better protect cells from oxidative stress due to the higher SOD mimetic activity of the nanoparticles.

  7. Modulation of surface structure and catalytic properties of cerium oxide nanoparticles by thermal and microwave synthesis techniques

    International Nuclear Information System (INIS)

    He, Jian; Zhou, Lan; Liu, Jie; Yang, Lu; Zou, Ling; Xiang, Junyu; Dong, Shiwu; Yang, Xiaochao

    2017-01-01

    Highlights: • The CNPs synthesized by microwave irradiation have more reactive hot spots than that synthesized by convective heating. • The CNPs synthesized by microwave irradiation exhibited higher SOD activity than that synthesized by convective heating. • The CNPs synthesized by microwave irradiation heating could better protect cells from oxidative stress. - Abstract: Cerium oxide nanoparticles (CNPs) have been intensively explored for biomedical applications in recent few years due to the versatile enzyme mimetic activities of the nanoparticles. However, the control of CNPs quality through the optimization of synthesis conditions remains largely unexplored as most of the previous studies only focus on utilizing the catalytic activities of the nanoparticles. In the present study, CNPs with size about 5 nm were synthesized by thermal decomposition method using traditional convective heating and recently developed microwave irradiation as heating source. The quality of CNPs synthesized by the two heating manner was evaluated. The CNPs synthesized by convective heating were slightly smaller than that synthesized by microwave irradiation heating. The cores of the CNPs synthesized by the two heating manner have similar crystal structure. While the surface subtle structures of the CNPs synthesized by two heating manner were different. The CNPs synthesized by microwave irradiation have more surface reactive hot spot than that synthesized by convective heating as the nanoparticles responded more actively to the redox environment variation. This difference resulted in the higher superoxide dismutase (SOD) mimetic activity of CNPs synthesized by microwave irradiation heating than that of the convective heating. Preliminary experiments indicated that the CNPs synthesized by microwave irradiation heating could better protect cells from oxidative stress due to the higher SOD mimetic activity of the nanoparticles.

  8. Synthesis, Crystal Structure and Luminescent Property of A Novel Cd(II) Coordination Polymer with Bis-imidazole Ligand

    International Nuclear Information System (INIS)

    Zhou, Yong Hong

    2013-01-01

    The key to the successful design of metal-organic coordination polymers is the judicious selection of organic ligand. Recently, polydentate aromatic nitrogen heterocyclic ligands with five-membered rings have been well-studied in the construction of supramolecular structure for their N-coordinated sites apt to coordinating to transition metals. Similar to six-membered N-heterocyclic ligands, the azole-based five-membered N-heterocyclic ligands, such as imidazoles, triazoles and tetrazoles have been extensively employed in the construction of various coordination polymers with diverse topologies and interesting properties. The bis(azole) ligands in which N-donor azole rings (imidazole, triazole, or tetrazole) are separated by alkyl, (CH 2 ) n , spacers are good choices for flexible bridging ligands. The conformational flexibility of the spacers makes the ligands adaptable to various coordination networks with one-, two-, and three dimensional structures

  9. Synthesis, Crystal Structure, and Luminescence Properties of a New Calcium(II Coordination Polymer Based on L-Malic Acid

    Directory of Open Access Journals (Sweden)

    Duraisamy Senthil Raja

    2013-01-01

    Full Text Available A new calcium coordination polymer [Ca(HL-MA]n (H3L-MA = L-malic acid has been solvothermally synthesized. The structure of the newly synthesized complex has been determined by single-crystal X-ray diffraction analysis and further characterized by elemental analysis, reflectance UV-Vis & IR spectra, powder X-ray diffraction (PXRD, and thermogravimetric analysis (TGA. The single crystal structure analysis showed that the complex forms three-dimensional framework. The new Ca(II complex has displayed very high thermal stability which was inferred from TGA and PXRD results. As far as the optical property of the new complex is concerned, the complex emitted its own characteristic sensitized luminescence.

  10. Synthesis, crystal structure and electrochemical properties of the manganese-doped LiNaFe[PO{sub 4}]F materials

    Energy Technology Data Exchange (ETDEWEB)

    Ben Yahia, Hamdi, E-mail: benyahia.hamdi@aist.go.jp; Shikano, Masahiro, E-mail: shikano.masahiro@aist.go.jp; Sakaebe, Hikari; Kobayashi, Hironori

    2013-08-15

    The new compounds LiNaFe{sub 1−x}Mn{sub x}[PO{sub 4}]F (x ≤ 1/4) were synthesized by a solid state reaction route. The crystal structure of LiNaFe{sub 3/4}Mn{sub 1/4}[PO{sub 4}]F was determined from single crystal X-ray diffraction data. LiNaFe{sub 3/4}Mn{sub 1/4}[PO{sub 4}]F crystallizes with the Li{sub 2}Ni[PO{sub 4}]F-type structure, space group Pnma, a = 10.9719(13), b = 6.3528(7), c = 11.4532(13) Å, V = 798.31(16) Å{sup 3}, and Z = 8. The structure consists of edge-sharing (Fe{sub 3/4}Mn{sub 1/4})O{sub 4}F{sub 2} octahedra forming (Fe{sub 3/4}Mn{sub 1/4})FO{sub 3} chains running along the b-axis. These chains are interlinked by PO{sub 4} tetrahedra forming a three-dimensional framework with the tunnels and the cavities filled by the well-ordered sodium and lithium atoms, respectively. The manganese-doped phases show poor electrochemical behavior comparing to the iron pure phase LiNaFe[PO{sub 4}]F. - Highlights: • We investigated the synthesis of LiNaFe{sub 1−x}Mn{sub x}[PO{sub 4}]F by solid state reaction. • We demonstrated that a solid solution exist only for x ≤ 1/4. • We solved the crystal structure of LiNaFe{sub 3/4}Mn{sub 1/4}[PO{sub 4}]F using single crystal data. • We studied the electrochemical performances of LiNaFe{sub 1−x}Mn{sub x}[PO{sub 4}]F. • The Mn-doped phases have poor electrochemical performances comparing to LiNaFe[PO{sub 4}]F.

  11. Structural and surface properties of highly ordered mesoporous magnesium-aluminium composite oxides derived from facile synthesis

    Energy Technology Data Exchange (ETDEWEB)

    Pan, Dahai, E-mail: pandahai@foxmail.com; Dong, Zhaoyang; He, Min; Chen, Wei; Chen, Shuwei; Yu, Feng; Fan, Binbin; Cui, Xingyu; Li, Ruifeng, E-mail: rfli@tyut.edu.cn

    2017-01-15

    Highly ordered mesoporous magnesium-aluminium composite oxides (denoted as OMMA-x) with a variety of n{sub Al}/n{sub Mg} ratios have been successfully synthesized via a facile strategy, and a salt effect was proposed to explain the formation mechanism. The incorporation of Mg can significantly improve the structural and surface properties of ordered mesoporous alumina (OMA) material. The resultant OMMA-x exhibited a much more ordered 2-D hexagonal mesostructure, a narrower pore size distribution, a higher specific surface area and pore volume, and a stronger basicity than those of OMA. More importantly, the highly homogeneous incorporation of Mg at the atomic level and the formation of framework Mg−O−Al bonds could effectively suppress the formation of crystalline alumina during the calcination process. As a result, OMMA-x demonstrated a superior thermal stability. For example, the ordered mesostructure of OMMA-8 could be well maintained with a high surface area of 182 m{sup 2}/g even after thermal treatment at 1000 °C. - Graphical abstract: A schematic procedure to illustrate the preparation of highly ordered mesoporous Mg-Al composite oxides (OMMA-x) with highly homogeneously dispersed Mg species and enhanced structural stability. - Highlights: • Mesoporous Mg-Al composite oxides with excellent structural and surface properties. • A highly homogeneous incorporation of Mg into the mesoporous framework of alumina. • A superior structural stability up to 1000 °C coupled with a large surface area. • A salt effect from the addition of Mg(NO{sub 3}){sub 2}·6H{sub 2}O to explain the formation mechanism.

  12. Hydrothermal synthesis, crystal structure, luminescent and magnetic properties of a new mononuclear GdIII coordination complex

    Science.gov (United States)

    Coban, Mustafa Burak

    2018-06-01

    A new GdIII coordination complex, {[Gd(2-stp)2(H2O)6].2(4,4'-bipy).4(H2O)}, complex 1, (2-stp = 2-sulfoterephthalate anion and 4,4'-bipy = 4,4'-bipyridine), has been synthesized by hydrothermal method and characterized by elemental analysis, solid state UV-Vis and FT-IR spectroscopy, single-crystal X-ray diffraction, solid state photoluminescence and variable-temperature magnetic measurements. The crystal structure determination shows that GdIII ions are eight coordinated and adopt a distorted square-antiprismatic geometry. Molecules interacting through intra- and intermolecular (O-H⋯O, O-H⋯N) hydrogen bonds in complex 1, give rise to 3D hydrogen bonded structure and the discrete lattice 4,4'-bipy molecules occupy the channel of the 3D structure. π-π stacking interactions also exist 4,4'-bipy-4,4'-bipy and 4,4'-bipy-2-stp molecule rings in 3D structures. Additionally, solid state photoluminescence properties of complex 1 at room temperature have been investigated. Under the excitation of UV light (at 349 nm), the complex 1 exhibited green emissions (at 505 nm) of GdIII ion in the visible region. Furthermore, Variable-temperature magnetic susceptibility and isothermal magnetization as function of external magnetic field studies reveal that complex 1 displays possible antiferromagnetic interaction.

  13. Synthesis and Visible-Light Photocatalytic Property of Bi2WO6Hierarchical Octahedron-Like Structures

    Directory of Open Access Journals (Sweden)

    Li Yuanyuan

    2008-01-01

    Full Text Available Abstract A novel octahedron-like hierarchical structure of Bi2WO6has been fabricated by a facile hydrothermal method in high quantity. XRD, SEM, TEM, and HRTEM were used to characterize the product. The results indicated that this kind of Bi2WO6crystals had an average size of ~4 μm, constructed by quasi-square single-crystal nanosheets assembled in a special fashion. The formation of octahedron-like hierarchical structure of Bi2WO6depended crucially on the pH value of the precursor suspensions. The photocatalytic activity of the hierarchical Bi2WO6structures toward RhB degradation under visible light was investigated, and it was found to be significantly better than that of the sample fabricated by SSR. The better photocatalytic property should be strongly associated with the high specific surface area and the abundant pore structure of the hierarchical octahedron-like Bi2WO6.

  14. Synthesis and mechanical properties of radiation-cured acrylo-urethane elastomers and their structural and morphological features

    International Nuclear Information System (INIS)

    Khamis, M.A.

    1984-01-01

    Polyacrylo-urethane elastomers were synthesized using a polyethylene adipate diol capped with toluene diisocyanate and hydroxyethylacrylate, to characterize the morphology of these elastomers and correlate their properties with both morphological and structural features. The one shot polymerization technique was used, where the prepolymer, the 2-hydroxyethylacrylate and the chain extender were mixed in the desired stoichiometric ratios and then reacted at various times and temperatures. The reaction progress was monitored by the isocyanate consumption. Acrylo-urethane mono-oligomers showed low elongation at break when compared with others in the literature at equivalent degrees of cross-linking in agreement with earlier work. It was postulated that the cause of low elongation was the high functionality of the cross-link in the polymerized network. Moisture-curing of the polymer films improved the mechanical properties of the partially reacted films, which was attributed to the formation of cross-linking by allophanate formation. Catalysts used (such as tertiary amines and metal catalysts) increase the rate so that even at lower temperatures the reaction is completed in a relatively short time, with no great influence on the film properties

  15. Three coordination polymers constructed from 5-(4-(tetrazol-5-yl)phenyl)isophthalic acid: Synthesis, crystal structure and properties

    Science.gov (United States)

    Zhai, Dandan; Sun, Wujuan; Fan, Fei; Liao, Xuzhao; Chen, Sanping; Yang, Xuwu

    2017-04-01

    Three new coordination polymers, namely, {[Co2(TPA)(μ3-O)3]·0.5DMA}n (1), {[Co(H2TPA)(bibp)(H2O)3]·H2O}n (2) and {[Cd3(TPA)2(phen)4]·4H2O}n (3), (H3TPA = 5-(4-(tetrazol-5-yl)phenyl)isophthalic acid, bibp = 4,4'-bis(imidazolyl)biphenyl, phen = 1,10-phenanthroline and DMA = N,N-dimethylacetamide), have been synthesized under solvothermal conditions and structurally characterized by elemental analysis, IR spectroscopy, powder X-ray diffraction (PXRD) and single-crystal X-ray diffraction analysis. Polymer 1 exhibits a three-dimensional (3D) structure constructed from 5-connected secondary building units (SBUs) [Co3(μ3-O)] and 3-connected H3TPA ligands. Polymer 2 has a 1D zigzag polymer chain connected by H3TPA and bibp ligands. Polymer 3 features an unusual 3D framework with a (3,4,2)-connected {4; 6;8}{4; 62;83} topology. Moreover, the thermal stabilities of 1-3 and photoluminescence properties of 3 have been investigated. Magnetic susceptibility measurements indicate that polymers 1-2 display antiferromagnetic exchange properties.

  16. Synthesis, crystal and band structures, and properties of a new supramolecular complex (Hg2As)2(CdI4)

    International Nuclear Information System (INIS)

    Zou Jianping; Wu Dongsheng; Huang Shuping; Zhu Jing; Guo Guocong; Huang Jinshun

    2007-01-01

    A new quaternary supramolecular complex (Hg 2 As) 2 (CdI 4 ) (1) has been prepared by the solid-state reaction and structurally characterized by single crystal X-ray diffraction analysis. Compound 1 crystallizes in the space group P2 1 of the monoclinic system with two formula units in a cell: a=7.945(4), b=12.934(6), c=8.094(4) A, β=116.898 o (1), V=741.7(6) A 3 . The structure of 1 is characterized by a tridymite-like three-dimensional cationic framework, which is composed of mercury and arsenic atoms, with the channels being occupied by discrete CdI 4 2- tetrahedral guest-anions. The optical properties were investigated in terms of the diffuse reflectance and Fourier transform infrared spectra. The electronic band structure along with density of states (DOS) calculated by DFT method indicates that the present compound is a semiconductor with a direct band gap, and that the optical absorption is mainly originated from the charge transitions from I-5p and As-4p to Cd-5s and Hg-6s states. - Graphical abstract: A new quaternary supramolecular complex (Hg 2 As) 2 (CdI 4 ) (1) has been prepared by the solid-state reaction, and structurally characterized by single crystal X-ray diffraction analysis. The structure of 1 is characterized by a 3-D tridymite-like cationic framework with the channels being occupied by discrete CdI 4 2- tetrahedral guest-anions

  17. Synthesis of cerium oxide nanoparticles using Gloriosa superba L. leaf extract and their structural, optical and antibacterial properties

    Energy Technology Data Exchange (ETDEWEB)

    Arumugam, Ayyakannu, E-mail: sixmuga@yahoo.com [Department of Nanoscience and Technology, Alagappa University, Karaikudi 630 004, Tamil Nadu (India); Karthikeyan, Chandrasekaran; Haja Hameed, Abdulrahman Syedahamed [PG and Research Department of Physics, Jamal Mohamed College, Tiruchirappalli 620 020, Tamil Nadu (India); Gopinath, Kasi; Gowri, Shanmugam; Karthika, Viswanathan [Department of Nanoscience and Technology, Alagappa University, Karaikudi 630 004, Tamil Nadu (India)

    2015-04-01

    CeO{sub 2} nanoparticles (NPs) were green synthesized using Gloriosa superba L. leaf extract. The synthesized nanoparticles retained the cubic structure, which was confirmed by X-ray diffraction studies. The oxidation states of the elements (C (1s), O (1s) and Ce (3d)) were confirmed by XPS studies. TEM images showed that the NPs possessed spherical shape and particle size of 5 nm. The Ce–O stretching bands were observed at 451 cm{sup −1} and 457 cm{sup −1} from the FT-IR and Raman spectra respectively. The band gap of the CeO{sub 2} NPs was estimated as 3.78 eV from the UV–visible spectrum. From the photoluminescence measurements, the broad emission composed of eight different bands were found. The antibacterial studies performed against a set of bacterial strains showed that Gram positive (G +) bacteria were relatively more susceptible to the NPs than Gram negative (G −) bacteria. The toxicological behavior of CeO{sub 2} NPs was found due to the synthesized NPs with uneven ridges and oxygen defects in CeO{sub 2} NPs. - Highlights: • Phytosynthesis of CeO{sub 2} NPs using Gloriosa superba leaf extract • Single step synthesis • Characterized by XRD, XPS, TEM, FTIR, Raman, UV–vis, PL and TG/DTA analyses • CeO{sub 2} NPs were of spherical shape with an average size of 5 nm. • CeO{sub 2} NPs showed highly potent antibacterial activity.

  18. Synthesis, structure and magnetic properties of crystallographically aligned CuCr{sub 2}Se{sub 4} thin films

    Energy Technology Data Exchange (ETDEWEB)

    Esters, Marco [Department of Chemistry, University of Oregon, Eugene, OR 97403 (United States); Liebig, Andreas [Institut für Physik, Universität Augsburg, 86159 Augsburg (Germany); Ditto, Jeffrey J.; Falmbigl, Matthias [Department of Chemistry, University of Oregon, Eugene, OR 97403 (United States); Albrecht, Manfred [Institut für Physik, Universität Augsburg, 86159 Augsburg (Germany); Johnson, David C., E-mail: davej@uoregon.edu [Department of Chemistry, University of Oregon, Eugene, OR 97403 (United States)

    2016-06-25

    We report the low temperature synthesis of highly textured CuCr{sub 2}Se{sub 4} thin films using the modulated elemental reactant (MER) method. The structure of CuCr{sub 2}Se{sub 4} is determined for the first time in its thin film form and exhibits cell parameters that are smaller than found in bulk CuCr{sub 2}Se{sub 4}. X-ray diffraction and precession electron diffraction show a strong degree of crystallographic alignment of the crystallites, where the <111> axis is oriented perpendicular to the substrate surface, while being rotationally disordered within the plane. Temperature and field dependent in-plane and out-of-plane magnetization measurements show that the film is ferromagnetic with a Curie temperature of 406 K CuCr{sub 2}Se{sub 4} synthesized utilizing the MER method shows stronger magnetic anisotropy (effective anisotropy: 1.82 × 10{sup 6} erg cm{sup −3}; shape anisotropy: 1.07 × 10{sup 6} erg cm{sup −3}), with the easy axis lying out of plane, and a larger magnetic moment (6 μ{sub B}/f.u.) than bulk CuCr{sub 2}Se{sub 4}. - Highlights: • Crystallographically aligned, phase pure CuCr{sub 2}Se{sub 4} were synthesized. • The degree of alignment decreases with annealing time. • The films are ferromagnetic with the easy axis along the <111> direction. • The magnetization is larger than bulk CuCr{sub 2}Se{sub 4} or other CuCr{sub 2}Se{sub 4} films made to date.

  19. Nanosilicon properties, synthesis, applications, methods of analysis and control

    CERN Document Server

    Ischenko, Anatoly A; Aslalnov, Leonid A

    2015-01-01

    Nanosilicon: Properties, Synthesis, Applications, Methods of Analysis and Control examines the latest developments on the physics and chemistry of nanosilicon. The book focuses on methods for producing nanosilicon, its electronic and optical properties, research methods to characterize its spectral and structural properties, and its possible applications. The first part of the book covers the basic properties of semiconductors, including causes of the size dependence of the properties, structural and electronic properties, and physical characteristics of the various forms of silicon. It presents theoretical and experimental research results as well as examples of porous silicon and quantum dots. The second part discusses the synthesis of nanosilicon, modification of the surface of nanoparticles, and properties of the resulting particles. The authors give special attention to the photoluminescence of silicon nanoparticles. The third part describes methods used for studying and controlling the structure and pro...

  20. Facile one-step synthesis and photoluminescence properties of Ag–ZnO core–shell structure

    International Nuclear Information System (INIS)

    Zhai, HongJu; Wang, LiJing; Han, DongLai; Wang, Huan; Wang, Jian; Liu, XiaoYan; Lin, Xue; Li, XiuYan; Gao, Ming; Yang, JingHai

    2014-01-01

    Graphical abstract: The PL of the Ag–ZnO core-shell nanostructure showed obvious increase of UV emission and slight decrease of visible light emission compared to that of the pure ZnO. With the calcination temperature increasing from 300 to 600 °C, the primary peak located at 380 nm became stronger and sharper, indicating that the increasing calcination temperature made the samples crystallize better. - Highlights: • Ag-ZnO core-shell structure was obtained via a simple one-step solvothermal process. • The approach was simple, mild, low cost, reproducible and easy-to-handle. • The obvious enhancement of UV luminescent has been observed. • Effects of the calcining temperature to luminescence were investigated in detail. - Abstract: Ag–ZnO core–shell structures were gained via one-step solvothermal process. The products were characterized by means of X-ray diffraction (XRD), transmission electron microscopy (TEM), Raman spectroscopy, photoluminescence (PL) and UV–vis spectroscopy, respectively. It was shown that the properties were greatly changed compared to pure ZnO from the PL and Raman spectra, which indicated the strong interfacial interaction between ZnO and Ag. The work provides a feasible method to synthesize Ag–ZnO core–shell structure photocatalyst, which is promising in the further practical application of ZnO-based photocatalytic materials

  1. Synthesis, crystal structures and luminescent properties of zinc(II) metal–organic frameworks constructed from terpyridyl derivative ligand

    International Nuclear Information System (INIS)

    Yang, Xiao-Le; Shangguan, Yi-Qing; Hu, Huai-Ming; Xu, Bing; Wang, Bao-Cheng; Xie, Juan; Yuan, Fei; Yang, Meng-Lin; Dong, Fa-Xin; Xue, Gang-Lin

    2014-01-01

    Five zinc(II) metal–organic frameworks, [Zn 3 (344-pytpy) 2 Cl 6 ] n ·n(H 2 O) (1), [Zn(344-pytpy)(ox)] n (2), [Zn 2 (344-pytpy)(bdc) 2 ] n ·1.5n(H 2 O) (3), [Zn 2 (344-pytpy) 2 (sfdb) 2 ] n ·1.5n(H 2 O) (4) and [Zn 3 (344-pytpy) 2 (btc) 2 ] n ·2n(H 2 O) (5), (344-pytpy=4′-(3-pyridyl)-4,2′:6′,4″-terpyridine, H 2 ox=oxalic acid, H 2 bdc=1,4-benzenedi-carboxylic acid, H 2 sfdb=4,4′-sulfonyldibenzoic acid and H 3 btc=1,3,5-benzene-tricarboxylic acid) have been prepared by hydrothermal reactions. Compound 1 is a 1D chain structure, in which 344-pytpy ligand links three Zn II centers through three of terminal N-donors. Compound 2 is a 4-connected 3D framework with the dia topological net and the Schläfli symbol of 6 6 . Compound 3 displays a unusual 3-fold interpenetrating 3D coordination network which exhibits a new intriguing (3,3,4)-connected topological net with the Schläfli symbol of (4.8 2 )(4.8 5 )(8 3 ). Compound 4 features a two-fold interpenetrating 4-connected 2D framework with the sql topological net and the Schläfli symbol of (4 4 .6 2 ). Compound 5 is a new self-interpenetrating (3,3,4,4)-connected topological net with the Schläfli symbol of (6.8 2 ) 2 (6 2 .8 2 .10.12)(6 2 .8 3 .10) 2 (6 2 .8) 2 . The luminescence properties of 1–5 have been investigated by emission spectra and they possess great thermal stabilities which can be stable up to around 400 °C. - Graphical abstract: Five new Zn(II) metal–organic frameworks based on dicarboxylate and terpyridyl derivative ligands have been synthesized by hydrothermal reactions, giving networks from 1D to 3D structures. The thermal stability and luminescent property have been investigated. - Highlights: • Five zinc(II) metal–organic frameworks have been prepared under hydrothermal conditions. • Their crystal and topological structures have been investigated. • The luminescent properties have been investigated. • They possess great thermal stabilities which can be stable up to

  2. Synthesis, structure and solvatochromic properties of 3-cyano-4,6-diphenyl-5-(3- and 4-substituted phenylazo-2-pyridones

    Directory of Open Access Journals (Sweden)

    NINA TODOROVIĆ

    2010-08-01

    Full Text Available A series of some new pyridone arylazo dyes was synthesized from the corresponding diazonium salts and 3-cyano-4,6-diphenyl-2-pyridone using the classical reaction for the synthesis of the azo compounds. The structures of these dyes were confirmed by UV–Vis, FT-IR and 1H-NMR spectroscopic techniques. The solvatochromism of the dyes was evaluated with respect to visible absorption properties in various solvents. The effects of solvent dipolarity/polarizability and solvent/solute hydrogen bonding interactions were analyzed by means of the linear solvation energy relationship concept proposed by Kamlet and Taft. The 2-pyridone/2-hydroxypiridine tautomeric equilibration was found to depend on the substituents as well as on the solvents.

  3. The synthesis, structure, and properties of 5,6,11,12-tetraarylindeno[1,2-b]fluorenes and their applications as donors for organic photovoltaic devices

    KAUST Repository

    Lo, Yuan-Chih; Ting, Hao-Chun; Li, Ya-Ze; Li, Yi-Hua; Liu, Shun-Wei; Huang, Kuo-Wei; Wong, Ken-Tsung

    2016-01-01

    The synthesis, structure, and properties of three new 5,6,11,12-tetraarylindeno[1,2-b]fluorenes are reported. The highly twisted conformations between an indeno[1,2-b]fluorene core and peripheral aryl substitutions endow these indeno[1,2-b]fluorene derivatives with good photostability for use as electron donors for vacuum-deposited photovoltaic devices. The optimized device based on a TAInF2 donor blended with C70 as an electron acceptor produces a high open-circuit voltage (>0.9 V) and a power conversion efficiency of 2.91%. This work demonstrates the first application of an indenofluorene derivative as an electron donor in organic solar cells.

  4. The synthesis, structure, and properties of 5,6,11,12-tetraarylindeno[1,2-b]fluorenes and their applications as donors for organic photovoltaic devices

    KAUST Repository

    Lo, Yuan-Chih

    2016-12-01

    The synthesis, structure, and properties of three new 5,6,11,12-tetraarylindeno[1,2-b]fluorenes are reported. The highly twisted conformations between an indeno[1,2-b]fluorene core and peripheral aryl substitutions endow these indeno[1,2-b]fluorene derivatives with good photostability for use as electron donors for vacuum-deposited photovoltaic devices. The optimized device based on a TAInF2 donor blended with C70 as an electron acceptor produces a high open-circuit voltage (>0.9 V) and a power conversion efficiency of 2.91%. This work demonstrates the first application of an indenofluorene derivative as an electron donor in organic solar cells.

  5. Unprecedented Hexanuclear Cobalt(II Nonsymmetrical Salamo-Based Coordination Compound: Synthesis, Crystal Structure, and Photophysical Properties

    Directory of Open Access Journals (Sweden)

    Zong-Li Ren

    2018-03-01

    Full Text Available A novel hexanuclear Co(II coordination compound with a nonsymmetrical Salamo-type bisoxime ligandH4L, namely [{Co3(HL(MeO(MeOH2(OAc2}2]·2MeOH, was prepared and characterized by elemental analyses, UV–vis, IR and fluorescence spectra, and X-ray single-crystal diffraction analysis. Each Co(II is hexacoordinated, and possesses a distorted CoO6 or CoO4N2 octahedrons. The Co(II coordination compound possesses a self-assembled infinite 2D supramolecular structure with the help of the intermolecular C–H···O interactions. Meanwhile, the photophysical properties of the Co(II coordination compound were studied.

  6. Synthesis and characterization of structural and magnetic properties of polyaniline-cobalt ferrite (PA-CoFe) nanocomposites

    Science.gov (United States)

    Thakur, Sonika; Kaur, Parminder; Singh, Lakhwant

    2018-05-01

    The growing interest in the investigation of the properties of modified conducting polymers stems from their potential applications in various fields such as in sensing and catalytic devices. The present work reports the modification of conducting polymer polyaniline with cobalt ferrite (CoFe) nanoparticles, where CoFe nanoparticles are added in different successive weight percents. The composite samples were synthesized by in-situ chemical oxidative polymerization technique. The density of the samples has been found to increase with an increase in the CoFe content. Structural analysis of the synthesized sample has been done using X-ray diffraction studies. Perusal of the hysteresis curves of the prepared samples depicts that the introduction of CoFe into the polymer matrix leads to enhancement in the ferromagnetic behavior of the synthesized samples, suggesting that these nanocomposites have excellent microwave absorbing capacity.

  7. Synthesis, growth, structural, optical, thermal, electrical and mechanical properties of hydrogen bonded organic salt crystal: Triethylammonium-3, 5-dinitrosalicylate

    Science.gov (United States)

    Rajkumar, Madhu; Chandramohan, Angannan

    2017-04-01

    Triethylammonium-3, 5-dinitrosalicylate, an organic salt was synthesized and single crystals grown by slow solvent evaporation solution growth technique using methanol as a solvent. The presence of various functional groups and mode of vibrations has been confirmed by FT-IR spectroscopic technique. The UV-vis-NIR Spectrum was recorded in the range 200-1200 nm to find optical transmittance window and lower cut off wavelength of the title crystal. The formation of the salt and the molecular structure was confirmed by NMR spectroscopic technique. Crystal system, crystalline nature, cell parameters and hydrogen bonding interactions of the grown crystal were determined by single crystal x-ray diffraction analysis. The thermal characteristics of grown crystal were analyzed by thermo gravimetric and differential thermal analyses. Dielectric studies were carried out to study the distribution of charges within the crystal. The mechanical properties of the title crystal were studied by Vicker's microhardness technique.

  8. Synthesis, crystal structure and electrical properties of A-site cation ordered BaErMn2O5 and BaErMn2O6

    International Nuclear Information System (INIS)

    Świerczek, Konrad; Klimkowicz, Alicja; Zheng, Kun; Dabrowski, Bogdan

    2013-01-01

    In this paper, we report on a synthesis procedure, structural and electrical properties of BaErMn 2 O 5 and BaErMn 2 O 6 , A-site double perovskites having layered arrangement of Ba and Er cations. These materials belong to a family of BaLnMn 2 O 5+δ oxides, which up to now were successfully synthesized for Ln=Y and La–Ho lanthanides. Up to our knowledge, this is the first report on the successful synthesis of BaErMn 2 O 5 and BaErMn 2 O 6 , yielding>95 wt% of the considered compounds. Structural characterization of the materials is given at room temperature, together with in situ XRD studies, performed during oxidation of BaErMn 2 O 5 in air, at elevated temperatures up to 500 °C. A complex structural behavior was observed, with oxidation process of BaErMn 2 O 5 occurring at around 300 °C. The oxidized BaErMn 2 O 6 shows a structural phase transition at about 225 °C. Results of structural studies are supported by thermogravimetric measurements of the oxidation process, performed in air, as well as reduction process, preformed in 5 vol% of H 2 in Ar. Additionally, isothermal oxidation/reduction cycles were measured at 500 °C, showing interesting properties of BaErMn 2 O 5+δ , from a point of view of oxygen storage technology. Electrical conductivity of BaErMn 2 O 5 is of the order of 10 −4 S cm −1 at room temperature and shows activated character on temperature with activation energy E a =0.30(1) eV. Positive sign of Seebeck coefficient for this material indicates holes as dominant charge carriers. Oxidized BaErMn 2 O 6 possesses much higher electrical conductivity, almost 0.2 S cm −1 at room temperature. Additional, about 10-fold increase of electrical conductivity, occurring in the vicinity of 225 °C for this material, can be associated with phase transition from charge/orbital-ordered insulator COI(CE) to paramagnetic metal PM phase. The highest conductivity for BaErMn 2 O 6 was measured near 500 °C and is almost equal to 40 S cm −1 , while

  9. Synthesis of polycarbonate urethane elastomers and effects of the chemical structures on their thermal, mechanical and biocompatibility properties.

    Science.gov (United States)

    Zhu, Rong; Wang, Yiyu; Zhang, Zongrui; Ma, Daiwei; Wang, Xinyu

    2016-06-01

    In this study, to obtain biomedical polyurethane elastomers with good mechanical properties and biocompatibility, a series of polycarbonate urethanes were synthesized via a two-step solution of polymerization method using the poly(1,6-hexanediol)carbonate diols (PCDL) as the soft segment, 4,4'-methylenebis(cyclohexyl isocyanate) (H12MDI), 1,6-hexamethylene diisocyanate (HDI) and 1,4-butanediol (BDO) as the hard segment with dibutyltin dilaurate as the catalyst. In this article, we illustrated the physical behaviors were obviously influenced by synthetic routes. And their chemical and physical structures were investigated by gel permeation chromatograph (GPC), differential scanning calorimeter (DSC), fourier transform infrared spectrography (FT-IR) and mechanical properties tests. The surface wettability were studied by contact angle measurement (CA). As a kind of short-term implant biomaterial, the results of the hemolysis and platelet adhesive tests were recorded by spectrophotometer and scanning electron microscopy (SEM), indicating the materials have a great potential for developments and applications in biomedical field.

  10. Synthesis of polycarbonate urethane elastomers and effects of the chemical structures on their thermal, mechanical and biocompatibility properties

    Directory of Open Access Journals (Sweden)

    Rong Zhu

    2016-06-01

    Full Text Available In this study, to obtain biomedical polyurethane elastomers with good mechanical properties and biocompatibility, a series of polycarbonate urethanes were synthesized via a two-step solution of polymerization method using the poly(1,6-hexanediolcarbonate diols (PCDL as the soft segment, 4,4′-methylenebis(cyclohexyl isocyanate (H12MDI, 1,6-hexamethylene diisocyanate (HDI and 1,4-butanediol (BDO as the hard segment with dibutyltin dilaurate as the catalyst. In this article, we illustrated the physical behaviors were obviously influenced by synthetic routes. And their chemical and physical structures were investigated by gel permeation chromatograph (GPC, differential scanning calorimeter (DSC, fourier transform infrared spectrography (FT-IR and mechanical properties tests. The surface wettability were studied by contact angle measurement (CA. As a kind of short-term implant biomaterial, the results of the hemolysis and platelet adhesive tests were recorded by spectrophotometer and scanning electron microscopy (SEM, indicating the materials have a great potential for developments and applications in biomedical field.

  11. Synthesis, growth, crystal structure, optical and third order nonlinear optical properties of quinolinium derivative single crystal: PNQI

    Science.gov (United States)

    Karthigha, S.; Krishnamoorthi, C.

    2018-03-01

    An organic quinolinium derivative nonlinear optical (NLO) crystal, 1-ethyl-2-[2-(4-nitro-phenyl)-vinyl]-quinolinium iodide (PNQI) was synthesized and successfully grown by slow evaporation solution growth technique. Formation of a crystalline compound was confirmed by single crystal X-ray diffraction. The quinolinium compound PNQI crystallizes in the triclinic crystal system with a centrosymmetric space group of P-1 symmetry. The molecular structure of PNQI was confirmed by 1H NMR and 13C NMR spectral studies. The thermal properties of the crystal have been investigated by thermogravimetric (TG) and differential scanning calorimetry (DSC) studies. The optical characteristics obtained from UV-Vis-NIR spectral data were described and the cut-off wavelength observed at 506 nm. The etching study was performed to analyse the growth features of PNQI single crystal. The third order NLO properties such as nonlinear refractive index (n2), nonlinear absorption coefficient (β) and nonlinear susceptibility (χ (3)) of the crystal were investigated using Z-scan technique at 632.8 nm of Hesbnd Ne laser.

  12. Core@shell@shell structured carbon-based magnetic ternary nanohybrids: Synthesis and their enhanced microwave absorption properties

    Science.gov (United States)

    Yang, Erqi; Qi, Xiaosi; Xie, Ren; Bai, Zhongchen; Jiang, Yang; Qin, Shuijie; Zhong, Wei; Du, Youwei

    2018-05-01

    High encapsulation efficiency of core@shell@shell structured carbon-based magnetic ternary nanohybrids have been synthesized in high yield by chemical vapor deposition of acetylene directly over octahedral-shaped Fe2O3 nanoparticles. By controlling the pyrolysis temperature, Fe3O4@Fe3C@carbon nanotubes (CNTs) and Fe@Fe3C@CNTs ternary nanohybrids could be selectively produced. The optimal RL values for the as-prepared ternary nanohybrids could reach up to ca. -46.7, -52.7 and -29.5 dB, respectively. The excellent microwave absorption properties of the obtaiend ternary nanohybrids were proved to ascribe to the quarter-wavelength matching model. Moreover, the as-prepared Fe@Fe3C@CNTs ternary nanohybrids displayed remarkably enhanced EM wave absorption capabilities compared to Fe3O4@Fe3C@CNTs due to their excellent dielectric loss abilities, good complementarities between the dielectric loss and the magnetic loss, and high attenuation constant. Generally, this strategy can be extended to explore other categories of core@shell or core@shell@shell structured carbon-based nanohybrids, which is very beneficial to accelerate the advancements of high performance MAMs.

  13. Sol-gel synthesis, structure and photoluminescence properties of nanocrystalline Lu{sub 2}MoO{sub 6}:Eu

    Energy Technology Data Exchange (ETDEWEB)

    Li, Huaiyong; Yang, Hyun Kyoung [Department of Physics, Pukyong National University, 599-1 Nam-Gu, Daeyeon 3 Dong, Busan 608-737 (Korea, Republic of); Jeong, Jung Hyun, E-mail: jhjeong@pknu.ac.kr [Department of Physics, Pukyong National University, 599-1 Nam-Gu, Daeyeon 3 Dong, Busan 608-737 (Korea, Republic of); Jang, Kiwan; Lee, Ho Sueb [Department of Physics, Changwon National University, Changwon 641-773 (Korea, Republic of); Yi, Soung Soo [Department of Electronic Material Engineering, Silla University, Busan 617-736 (Korea, Republic of)

    2011-09-15

    Highlights: {yields} Monoclinic-structural Lu{sub 2}MoO{sub 6} has strong absorption of near-UV light. {yields} The absorbed energy can be transferred from MoO{sub 5} groups to doped Eu{sup 3+} and luminescence. {yields} The absorption edge and the peak of the MoO{sub 5} excitation band shift in reverse ways. {yields} The decline of the crystallinity and the introduced defect respond for the variation. -- Abstract: In this paper, we reported the obtention of Eu{sup 3+} ion doped Lu{sub 2}MoO{sub 6} powders synthesized by a sol-gel method, and followed by annealing at different temperatures. The structure and photoluminescence properties of these powders were investigated. The X-ray diffraction pattern suggests that Lu{sub 2}MoO{sub 6} powder has a monoclinic structure. It was observed that the UV-visible and photoluminescence spectra of Lu{sub 2}MoO{sub 6}:Eu nanocrystallines varied systematically with the calcination temperature. The near-UV absorption edge shifts to long wavelength direction with the decreasing of the calcination temperature, while the peak of MoO{sub 5} excitation band shifts in an opposite way. The decline of the crystallinity and the introduced lattice defect were considered to respond for these variations. Additionally, due to the efficient red light emission under near-UV light excitation, the powder can be a candidate as red phosphor for white-light-emitting diodes.

  14. Four Mixed-Ligand Zn(II Three-Dimensional Metal-Organic Frameworks: Synthesis, Structural Diversity, and Photoluminescent Property

    Directory of Open Access Journals (Sweden)

    Chih-Chieh Wang

    2017-11-01

    Full Text Available Assemblies of four three-dimensional (3D mixed-ligand coordination polymers (CPs having formulas, {[Zn2(bdc2(4-bpdh]·C2H5OH·2H2O}n (1, [Zn(bdc(4-bpdh]n (2, {[Zn2(bdc2(4-bpdh2]·(4-bpdh}n (3, and {[Zn(bdc(4-bpdh]·C2H5OH}n (4 (bdc2− = dianion of 1,4-benzenedicarboxylic acid, 4-bpdh = 2,5-bis(4-pyridyl-3,4-diaza-2,4-hexadiene have been synthesized and structurally characterized by single-crystal X-ray diffraction method. Structural determination reveals that the coordination numbers (geometry of Zn(II ions in 1, 2, 3, and 4 are five (distorted square-pyramidal (SP, six (distorted octahedral (Oh, five (trigonal-bipyramidal (TBP, and four (tetrahedral (Td, respectively, and are bridged by 4-bpdh with bis-monodentate coordination mode and bdc2− ligands with bis-bidentate in 1, chelating/bidentate in 2, bis-monodentate and bis-bidentate in 3, and bis-monodentate in 4, to generate two-fold interpenetrating 3D cube-like metal-organic framework (MOF with pcu topology, non-interpenetrating 3D MOF, two-fold interpenetrating 3D rectangular-box-like MOF with pcu topology and five-fold interpenetrating diamondoid-like MOF with dia topology, respectively. These different intriguing architectures indicate that the coordination numbers and geometries of Zn(II ions, coordination modes of bdc2− ligand, and guest molecules play important roles in the construction of MOFs and the formation of the structural topologies and interpenetrations. Thermal stabilities, and photoluminescence study of 1–4 were also studied in detail. The complexes exhibit ligands based photoluminescence properties at room temperature.

  15. Synthesis, structural and luminescence properties of Bi3+ co-doped Y2Sn2O7:Tb nanoparticles

    International Nuclear Information System (INIS)

    Nigam, S.; Sudarsan, V.; Vatsa, R.K.

    2010-01-01

    Full text: In recent years, advanced materials derived from Pyrochlore-type oxides (A 2 B 2 O 7 ) have been of extensive scientific and technological interest. Chemical substitution of A or B sites of pyrochlore oxide by rare earth ions is a widely used approach to prepare thermally stable, lanthanide ion doped luminescent materials. Due to the higher symmetry around the A and B sites in the lattice lanthanide ions like Eu 3+ and Tb 3+ when incorporated at the A or B sites give very poor luminescence. This problem can be avoided by incorporating other ions like Bi 3+ in the lattice so that the lattice gets distorted and luminescent intensity from the lanthanide ions increases. The present study deals with the synthesis and characterization of Bi 3+ co-doped Y 2 Sn 2 O 7 :Tb nanoparticles. For the preparation of Tb 3+ and Bi 3+ doped Y 2 Sn 2 O 7 nano-materials, Sn metal, Bi(NO 3 ) 3 , Tb 4 O 7 , Y 2 CO 3 , were used as starting materials. The solution containing Y 3+ , Sn 4+ ,and Bi 3+ -Tb 3+ in ethylene glycol medium was slowly heated up to 120 deg C and then subjected to urea hydrolysis. The obtained precipitate after washing was heated to 700 deg C. As prepared samples are amorphous in nature and 700 deg C heated sample showed well crystalline pyrochlore structure as revealed by the XRD studies. Average particles size is calculated from the width of the X-ray diffraction peaks and found to be ∼ 5 nm. TEM images of the nanoparticles obtained at 700 deg C shows very fine spherical particles having a diameter in the range of 2-5 nm. Luminescence measurements were carried out for as prepared and 700 deg C heated samples of 2.5%Tb doped Y 2 Sn 2 O 7 nanoparticles. Green emission characteristic 5 D 4 7 F 5 transition of Tb 3+ has been observed from as prepared sample but on heating to 700 deg C the emission characteristic of Tb 3+ ions got completely removed . However, there is a significant improvement in Tb 3+ emission from 2.5% Bi 3+ co-doped Y 2 Sn 2 O 7 :Tb 3

  16. Synthesis, structure and magnetic properties of distorted Y{sub x}La{sub 1-x}FeO{sub 3}: Effects of mechanochemical activation and composition

    Energy Technology Data Exchange (ETDEWEB)

    Cristobal, A.A. [Instituto de Investigaciones en Ciencia y Tecnologia de Materiales, INTEMA (CONICET-UNMdP), J.B. Justo 4302 B7608FDQ, Mar del Plata (Argentina); Botta, P.M., E-mail: pbotta@fi.mdp.edu.ar [Instituto de Investigaciones en Ciencia y Tecnologia de Materiales, INTEMA (CONICET-UNMdP), J.B. Justo 4302 B7608FDQ, Mar del Plata (Argentina); Aglietti, E.F.; Conconi, M.S. [Centro de Tecnologia de Recursos Minerales y Ceramica, CETMIC (CIC-CONICET), Camino P. Centenario y 506 B1897ZCA, Gonnet (Argentina); Bercoff, P.G. [Facultad de Matematica, Astronomia y Fisica, FaMAF UNC and IFEG (CONICET), Ciudad Universitaria (5000), Cordoba (Argentina); Porto Lopez, J.M. [Instituto de Investigaciones en Ciencia y Tecnologia de Materiales, INTEMA (CONICET-UNMdP), J.B. Justo 4302 B7608FDQ, Mar del Plata (Argentina)

    2011-11-01

    Highlights: {yields} Y{sub x}La{sub 1-x}FeO{sub 3} phases (0 {<=} x {<=} 1) were prepared at RT by mechanochemical treatment. {yields} The obtained materials showed an anisotropic distortion of its crystal structure. {yields} Combination of Y-doping and mechanochemistry produced weak ferromagnetic materials. {yields} Thermal treatments improved the structural order, leading to antiferromagnetic solids. {yields} Neel temperature decreased with x due to less stable magnetic structures. - Abstract: The influence of mechanochemical treatment on the synthesis and properties of Y{sub x}La{sub 1-x}FeO{sub 3} (0 {<=} x {<=} 1) orthoferrites is studied. Solid mixtures of the corresponding metal oxides were treated in a high-energy ball-mill. X-ray diffraction revealed that during the milling the disappearance of the reactants and a fast conversion to orthoferrite phase take place. Magnetic measurements showed a weak ferromagnetic behavior of the obtained materials, observing higher magnetization for larger x. The activated powders heated at 600 and 800 deg. C showed a progressive crystalline ordering together with a significant drop of magnetization. Thermal treatments at 1000 deg. C produced the formation of the phase Y{sub 3}Fe{sub 5}O{sub 12} for the samples richer in yttrium, increasing the magnetization. Rietveld refinements of the diffraction patterns and dynamical scanning calorimetry were used respectively to determine the lattice parameters and Neel temperatures for the formed orthoferrites. The effect of the composition on the structure and magnetic behavior is discussed.

  17. Superconducting selenides intercalated with organic molecules: synthesis, crystal structure, electric and magnetic properties, superconducting properties, and phase separation in iron based-chalcogenides and hybrid organic-inorganic superconductors

    Science.gov (United States)

    Krzton-Maziopa, Anna; Pesko, Edyta; Puzniak, Roman

    2018-06-01

    Layered iron-based superconducting chalcogenides intercalated with molecular species are the subject of intensive studies, especially in the field of solid state chemistry and condensed matter physics, because of their intriguing chemistry and tunable electric and magnetic properties. Considerable progress in the research, revealing superconducting inorganic–organic hybrid materials with transition temperatures to superconducting state, T c, up to 46 K, has been brought in recent years. These novel materials are synthesized by low-temperature intercalation of molecular species, such as solvates of alkali metals and nitrogen-containing donor compounds, into layered FeSe-type structure. Both the chemical nature as well as orientation of organic molecules between the layers of inorganic host, play an important role in structural modifications and may be used for fine tuning of superconducting properties. Furthermore, a variety of donor species compatible with alkali metals, as well as the possibility of doping also in the host structure (either on Fe or Se sites), makes this system quite flexible and gives a vast array of new materials with tunable electric and magnetic properties. In this review, the main aspects of intercalation chemistry are discussed with a particular attention paid to the influence of the unique nature of intercalating species on the crystal structure and physical properties of the hybrid inorganic–organic materials. To get a full picture of these materials, a comprehensive description of the most effective chemical and electrochemical methods, utilized for synthesis of intercalated species, with critical evaluation of their strong and weak points, related to feasibility of synthesis, phase purity, crystal size and morphology of final products, is included as well.

  18. Facile synthesis of flower like FePt@ZnO core–shell structure and its bifunctional properties

    Energy Technology Data Exchange (ETDEWEB)

    Majeed, Jerina [Chemistry Division, Bhabha Atomic Research Centre, Trombay, Mumbai 400085 (India); Jayakumar, O.D., E-mail: ddjaya@barc.gov.in [Chemistry Division, Bhabha Atomic Research Centre, Trombay, Mumbai 400085 (India); Mandal, B.P. [Chemistry Division, Bhabha Atomic Research Centre, Trombay, Mumbai 400085 (India); Salunke, H.G. [Technical Physics Division, Bhabha Atomic Research Centre, Trombay, Mumbai 400085 (India); Naik, R. [Department of Physics, Wayne State University, Detroit, MI 48202 (United States); Tyagi, A.K., E-mail: aktyagi@barc.gov.in [Chemistry Division, Bhabha Atomic Research Centre, Trombay, Mumbai 400085 (India)

    2014-06-01

    Graphical abstract: Flower shaped FePt and ZnO coated FePt with core–shell nanostructures are synthesized by a facile solvothermal procedure. Shell thickness of ZnO over FePt core was tuned by varying FePt concentration with respect to ZnO. Hybrid structure with lower FePt concentration exhibited bifunctionality such as near room temperature ferromagnetism and photoluminescence. Pristine FePt crystallize in the fct (L1{sub 0}) phase whereas it converts into fcc phase in presence of ZnO. - Highlights: • FePt@ZnO hybrid core–shell particles, with unique flower shape morphology have been prepared by solvothermal method. • Phase transition of fct-FePt to fcc-FePt has been found in presence of ZnO nanoparticles. • Plausible mechanism for growth of flowershaped nanoparticle is in accordance with energy minimization principle. • The core shell structure (FePt@ZnO) exhibits bi-functional properties. - Abstract: Flower shaped FePt and ZnO coated FePt (FePt@ZnO) core–shell nanostructures are synthesized by a facile solvothermal procedure. Two different compositions (molar ratio) of FePt and ZnO (FePt:ZnO = 1:3 and FePt:ZnO = 1:6) core–shells with different thicknesses of ZnO shells were synthesized. Hybrid FePt@ZnO core–shell flower structure with lower FePt concentration (FePt:ZnO = 1:6) exhibited bifunctionality including near room temperature ferromagnetism and photoluminescence at ambient conditions. X-ray diffraction patterns of pristine FePt showed partially ordered face centred tetragonal (fct) L1{sub 0} phase whereas ZnO coated FePt (FePt@ZnO) nanostructures showed hexagonal ZnO and disordered phase of FePt with fcc structure. The phase transition of fct FePt to fcc phase occurring in presence of ZnO is further confirmed by transmission electron microscopy and magnetic measurement studies. The formation of the nanoflowers was possibly due to growth along the [0 1 1] or [0 0 1] direction, keeping the core nearly spherical in accordance with the

  19. Reverse micellar synthesis, structural characterization and dielectric properties of Sr-doped BaZrO_3 nanoparticles

    International Nuclear Information System (INIS)

    Ahmad, Tokeer; Ubaidullah, Mohd; Shahazad, Mohd; Kumar, Dinesh; Al-Hartomy, Omar A.

    2017-01-01

    Sr-doped BaZrO_3 nanoparticles with strontium content varying from 5 to 20 mol % were successfully synthesized by reverse micellar method at 900 °C for the first time. Systematic studies have been carried out to establish the structural and electrical properties of the as prepared nanoparticles. These nanoparticles were characterized using powder X-ray diffraction, transmission electron microscopy, BET surface area and dielectric measurements. X-ray diffraction analysis showed the formation of monophasic and highly crystalline nanoparticles which could be indexed in cubic BaZrO_3 with contraction of lattice on strontium substitution. A monotonic shift of diffraction pattern towards higher angel confirms the formation of solid solutions of Ba_1_−_xSr_xZrO_3 (0.05 ≤ x ≤ 0.20) which was corroborating well with lattice parameter studies. Transmission electron microscopic studies showed the formation of cubic, spherical and hexagonal nanoparticles with an average grain size of 40–65 nm. Energy dispersive X-ray spectroscopic studies confirmed the presence of dopant (Sr"2"+) in the BaZrO_3 matrix and estimated chemical species corroborate well with the loaded composition. Specific surface area of the solid solution comes out to be in the range of 104–244 m"2 g"-"1. Smallest particle of size 40 nm shows highest surface area 244 m"2 g"-"1 for 20 mol% Sr-doped BaZrO_3. Dielectric and impedance studies were also carried out as a function of frequency and temperature to explore the electrical properties of Sr-doped BaZrO_3. The dielectric constant of Ba_1_−_xSr_xZrO_3 (0.05 ≤ x ≤ 0.20) was found to be in the range of 13–25 for x = 0.05 to x = 0.20 with nearly similar dielectric loss of the order of 0.02. The conductance increases linearly with increase in frequency at room temperature, however the impedance has an inverse effect. - Highlights: • Monophasic nanocrystalline Ba_1_−_xSr_xZrO_3 at low dopant concentration using reverse micelles for the first

  20. Reverse micellar synthesis, structural characterization and dielectric properties of Sr-doped BaZrO{sub 3} nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Ahmad, Tokeer, E-mail: tahmad3@jmi.ac.in [Nanochemistry Laboratory, Department of Chemistry, Jamia Millia Islamia, New Delhi, 110025 (India); Ubaidullah, Mohd [Nanochemistry Laboratory, Department of Chemistry, Jamia Millia Islamia, New Delhi, 110025 (India); Department of Chemistry, Banasthali University, Tonk, Rajasthan, 304022 (India); School of Science and Technology, Glocal University, Mirzapur, Saharanpur, 247121, Uttar Pradesh (India); Shahazad, Mohd [Nanochemistry Laboratory, Department of Chemistry, Jamia Millia Islamia, New Delhi, 110025 (India); Kumar, Dinesh [Department of Chemistry, Banasthali University, Tonk, Rajasthan, 304022 (India); Al-Hartomy, Omar A. [Department of Physics, Faculty of Science, King Abdulaziz University, Jeddah, 21589 (Saudi Arabia)

    2017-01-01

    Sr-doped BaZrO{sub 3} nanoparticles with strontium content varying from 5 to 20 mol % were successfully synthesized by reverse micellar method at 900 °C for the first time. Systematic studies have been carried out to establish the structural and electrical properties of the as prepared nanoparticles. These nanoparticles were characterized using powder X-ray diffraction, transmission electron microscopy, BET surface area and dielectric measurements. X-ray diffraction analysis showed the formation of monophasic and highly crystalline nanoparticles which could be indexed in cubic BaZrO{sub 3} with contraction of lattice on strontium substitution. A monotonic shift of diffraction pattern towards higher angel confirms the formation of solid solutions of Ba{sub 1−x}Sr{sub x}ZrO{sub 3} (0.05 ≤ x ≤ 0.20) which was corroborating well with lattice parameter studies. Transmission electron microscopic studies showed the formation of cubic, spherical and hexagonal nanoparticles with an average grain size of 40–65 nm. Energy dispersive X-ray spectroscopic studies confirmed the presence of dopant (Sr{sup 2+}) in the BaZrO{sub 3} matrix and estimated chemical species corroborate well with the loaded composition. Specific surface area of the solid solution comes out to be in the range of 104–244 m{sup 2} g{sup -1}. Smallest particle of size 40 nm shows highest surface area 244 m{sup 2} g{sup -1} for 20 mol% Sr-doped BaZrO{sub 3}. Dielectric and impedance studies were also carried out as a function of frequency and temperature to explore the electrical properties of Sr-doped BaZrO{sub 3}. The dielectric constant of Ba{sub 1−x}Sr{sub x}ZrO{sub 3} (0.05 ≤ x ≤ 0.20) was found to be in the range of 13–25 for x = 0.05 to x = 0.20 with nearly similar dielectric loss of the order of 0.02. The conductance increases linearly with increase in frequency at room temperature, however the impedance has an inverse effect. - Highlights: • Monophasic nanocrystalline Ba{sub 1

  1. Synthesis, structures and properties of a family of four two-dimensional coordination polymers constructed from 5-hydroxyisophthalate

    International Nuclear Information System (INIS)

    Zhang, Kou-Lin; Zhang, Jing-Bo; Jing, Chu-Yue; Zhang, Lei; Walton, Richard I.; Zhu, Peizhi; Ng, Seik Weng

    2014-01-01

    Four 2D coordination polymers (CPs) with different structures containing the multifunctional ligand 5-hydroxyisophthalate (5-OH-BDC 2− ), [Zn(5-OH-BDC)(btb)]·2H 2 O (1), [Cd(5-OH-BDC)(btp)(H 2 O)]·3H 2 O (2), [Cd(5-OH-BDC)(bth) 2 (H 2 O)]·H 2 O (3) and [Pb(5-OH-BDC)]·H 2 O (4) [btp=1, 3-bis(1,2,4-triazol-1-yl)propane, btb=1,4-bis(1,2,4-triazol-1-yl)butane, bth=1, 6-bis(1,2,4-triazol-1-yl)hexane] were obtained. 1–3 were synthesised hydrothermally, while 4 was obtained under ambient condition. The adjacent (2D→2D) polycatenated 2D layers of 1 polythread in a parallel manner to form an unusual 2D→3D polythreaded framework. 2 contains an undulated 2D (4, 4) network and further extends into an “embracing” double-layer structure through the C–H···π and π···π stacking interactions. 3 exhibits a non-interpenetrating 2D (4, 4)-network. 4 exhibits a 2D double-layered binodal (4, 4)-net containing oblong nanochannels with symbol (4 3 6 3 ) 2 . Reversible dehydration–rehydration is observed in 1, 2 and 4, which fall within the category of “recoverable collapsing” and “guest-induced re-formation” frameworks, while 3 exhibits irreversible dehydration–rehydration behaviour. The solid state fluorescent properties of 1–4 have been investigated. -- Graphical abstract: Among four 2D CPs reported, 1 is an unusual 2D→3D polythreaded framework. 4 exhibits 2D double-layered binodal (4, 4)-net containing nanochannels. Reversible dehydration–rehydration is observed in 1, 2 and 4. Highlights: • Four 2D CPs based on 5-hydroxyisophthalate with d 10 and Pb(II) ions were reported. • 1 is an unusual 2D→3D polythreaded framework. • 4 shows a binodal (4, 4)-connected 2D double-layer network with nanochannels. • The materials 1, 2 and 4 show reversible dehydration–rehydration behaviours. • Solid state fluorescent properties were investigated

  2. Synthesis, structures and properties of a family of four two-dimensional coordination polymers constructed from 5-hydroxyisophthalate

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Kou-Lin, E-mail: klzhang@yzu.edu.cn [Key Laboratory of Environmental Material and Environmental Engineering of Jiangsu Province, College of Chemistry and Chemical Engineering, Yangzhou University, Yangzhou 225002 (China); Zhang, Jing-Bo; Jing, Chu-Yue; Zhang, Lei [Key Laboratory of Environmental Material and Environmental Engineering of Jiangsu Province, College of Chemistry and Chemical Engineering, Yangzhou University, Yangzhou 225002 (China); Walton, Richard I. [Department of Chemistry, University of Warwick, Coventry CV4 7AL (United Kingdom); Zhu, Peizhi, E-mail: pzzhu@yzu.edu.cn [Key Laboratory of Environmental Material and Environmental Engineering of Jiangsu Province, College of Chemistry and Chemical Engineering, Yangzhou University, Yangzhou 225002 (China); Ng, Seik Weng [Department of Chemistry, University of Malaya, 50603 Kuala Lumpur (Malaysia)

    2014-03-15

    Four 2D coordination polymers (CPs) with different structures containing the multifunctional ligand 5-hydroxyisophthalate (5-OH-BDC{sup 2−}), [Zn(5-OH-BDC)(btb)]·2H{sub 2}O (1), [Cd(5-OH-BDC)(btp)(H{sub 2}O)]·3H{sub 2}O (2), [Cd(5-OH-BDC)(bth){sub 2}(H{sub 2}O)]·H{sub 2}O (3) and [Pb(5-OH-BDC)]·H{sub 2}O (4) [btp=1, 3-bis(1,2,4-triazol-1-yl)propane, btb=1,4-bis(1,2,4-triazol-1-yl)butane, bth=1, 6-bis(1,2,4-triazol-1-yl)hexane] were obtained. 1–3 were synthesised hydrothermally, while 4 was obtained under ambient condition. The adjacent (2D→2D) polycatenated 2D layers of 1 polythread in a parallel manner to form an unusual 2D→3D polythreaded framework. 2 contains an undulated 2D (4, 4) network and further extends into an “embracing” double-layer structure through the C–H···π and π···π stacking interactions. 3 exhibits a non-interpenetrating 2D (4, 4)-network. 4 exhibits a 2D double-layered binodal (4, 4)-net containing oblong nanochannels with symbol (4{sup 3}6{sup 3}){sub 2}. Reversible dehydration–rehydration is observed in 1, 2 and 4, which fall within the category of “recoverable collapsing” and “guest-induced re-formation” frameworks, while 3 exhibits irreversible dehydration–rehydration behaviour. The solid state fluorescent properties of 1–4 have been investigated. -- Graphical abstract: Among four 2D CPs reported, 1 is an unusual 2D→3D polythreaded framework. 4 exhibits 2D double-layered binodal (4, 4)-net containing nanochannels. Reversible dehydration–rehydration is observed in 1, 2 and 4. Highlights: • Four 2D CPs based on 5-hydroxyisophthalate with d{sup 10} and Pb(II) ions were reported. • 1 is an unusual 2D→3D polythreaded framework. • 4 shows a binodal (4, 4)-connected 2D double-layer network with nanochannels. • The materials 1, 2 and 4 show reversible dehydration–rehydration behaviours. • Solid state fluorescent properties were investigated.

  3. Synthesis, crystal structures and properties of new homoleptic Ni(II)/Pd(II) β-oxodithioester chelates

    Science.gov (United States)

    Yadav, Chote L.; Manar, Krishna K.; Yadav, Manoj K.; Tiwari, Neeraj; Singh, Rakesh K.; Drew, Michael G. B.; Singh, Nanhai

    2018-05-01

    Six new cis-chelate complexes, [M(L)2] (L = methyl-3-hydroxy-3-(furyl)-2-propenedithioate L1, M = Ni(II) 1, Pd(II) 4; methyl-3-hydroxy-3-(thiophenyl)-2-propenedithioate L2, M = Ni(II) 2, Pd(II) 5 and methyl-3-hydroxy-3-(phenyl)-2-propenedithioate L3, M = Ni(II) 3, Pd(II) 6 have been prepared and characterized by elemental analyses, spectroscopy (IR, UV-Vis., 1H and 13C{1H} NMR). The structures of 2-6 have been revealed by X-ray crystallography. In all the crystal structures, the metal has four-coordinate slightly distorted square planar geometry with a cis-configuration of the ligands. Anti-leishmanial properties of the complexes have been studied; 2, 3 and 6 showed potential anti-promastigote and anti-amastigote activities with IC50 values of 1.70 ± 0.50, 1.62 ± 0.19, 9.20 ± 2.16 μg/mL and IC50 2.50 ± 0.10, 2.05 ± 0.40, 12.84 ± 3.46 μg/mL respectively. Cytotoxicity assays on these complexes showed toxicity on the promastigotes but less toxicity against RAW 264.7 cell lines at different concentrations. Palladium complexes 4, 5 and 6 show luminescent characteristics in CH2Cl2 solution at room temperature. Complexes 1-6 are weakly conducting (σrt = 10-4-10-6 S cm-1, Ea = 0.19-1.13 eV) but show semiconducting behavior in the solid phase.

  4. Controllable synthesis, crystal structure and magnetic properties of Monomer-Dimer Cocrystallized MnIII Salen-type composite material

    Science.gov (United States)

    Wu, Qiong; Wu, Wei; Wu, Yongmei; Li, Weili; Qiao, Yongfeng; Wang, Ying; Wang, Baoling

    2018-04-01

    By the reaction of manganese-Schiff-base complexes with penta-anionic Anderson heteropolyanion, a new supramolecular architecture [Mn2(Salen)2(H2O)2][Mn(Salen)(H2O)2]2Na[IMo6O24]·8H2O (1) (salen = N,N‧-ethylene-bis (salicylideneiminate) has been isolated. Compound 1 was characterized by the single-crystal X-ray diffraction, elemental, IR and thermal gravimetric analyses. Structural analysis reveals that the unit cell simultaneously contains MnIII-Salen dimer and monomer cation fragments, for which the Anderson-type polyanions serve as counter anions. In the packing arrangement, all the MnIII dimers are well separated by polyoxometalate units and form tertiary structure together with MnIII monomers. Interestingly, different from the previous work, in the exact same reaction conditions, we are able to template MnIII-Salen complexes into different configurations by varying the charge state of polyanions. Besides, the magnetic properties of 1 were also examined by using both dc and ac magnetic field of the superconducting quantum interference devices. Most importantly, our fitting of the experimental data to a Heisenberg-type spin model shows that there exists a ferromagnetic exchange interaction ∼5 K between the spins (S = 2) on MnIII in the dimer, while antiferromagnetic ones exist among monomers and dimer (∼2 K). This meta-magnetic state could induce a slight spin frustration at low temperature, which would in turn affect the magnetic behavior. In addition, our ac field measurement of the susceptibilities suggests a typical signature for a single-molecule magnet.

  5. Synthesis of ferrofluids based on cobalt ferrite nanoparticles: Influence of reaction time on structural, morphological and magnetic properties

    Energy Technology Data Exchange (ETDEWEB)

    Amirabadizadeh, Ahmad; Salighe, Zohre; Sarhaddi, Reza, E-mail: reza.sarhaddi@birjand.ac.ir; Lotfollahi, Zahra

    2017-07-15

    Highlights: • Ferrofluids based on cobalt ferrite nanoparticles were synthesized by co-precipitation method. • The crystallite and particle size of cobalt ferrite can be controlled effectively by reaction time. • The ferrofluids have lower values of saturation magnetization and coercivity as compared to nanoparticles. • By increasing the size of nanoparticles, the narrower and sharper spikes of ferrofluids are formed. - Abstract: In this work, for first time the ferrofluids based on the cobalt ferrite (CoFe{sub 2}O{sub 4}) nanoparticles were prepared by the co-precipitation method at different reaction times (0.5–6.5 h). Crystal structure, morphology and magnetic properties of the cobalt ferrite nanoparticles and the ferrofluids based on the nanoparticles were studied by X-ray diffraction (XRD), field emission scanning electron microscope (FESEM) and vibrating sample magnetometer (VSM). The XRD patterns of CoFe{sub 2}O{sub 4} nanoparticles synthesized at different reaction times indicated that all samples are single phase in accordance with inverse cubic spinel structure with space group Fd-3m, and no impurity phase was observed. By increasing the reaction time to 3.5 h, the lattice parameter and the average crystallites size increased and then afterwards decreased by increasing the reaction time. The microscopic studies indicated the formation of nanosized particles with nearly spherical in shape, whereas the average particle size for all samples is found to be less than 50 nm. The results of VSM also showed that the saturation magnetization and coercivity field of the cobalt ferrite nanoparticles and the ferrofluids were influenced by reaction time, whereas the ferrofluids have lower values of magnetic parameters than that of nanoparticles.

  6. Synthesis, surface structure and optical properties of double perovskite Sr{sub 2}NiMoO{sub 6} nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Xu, Lei; Wan, Yingpeng [State and Local Joint Engineering Laboratory for Novel Functional Polymeric Materials, College of Chemistry, Chemical Engineering and Materials Science, Soochow University, Suzhou, 215123 (China); Xie, Hongde, E-mail: xiehongde@suda.edu.cn [State and Local Joint Engineering Laboratory for Novel Functional Polymeric Materials, College of Chemistry, Chemical Engineering and Materials Science, Soochow University, Suzhou, 215123 (China); Huang, Yanlin; Yang, Li [State and Local Joint Engineering Laboratory for Novel Functional Polymeric Materials, College of Chemistry, Chemical Engineering and Materials Science, Soochow University, Suzhou, 215123 (China); Qin, Lin [Department of Physics and Interdisciplinary Program of Biomedical, Mechanical & Electrical Engineering, Pukyong National University, Busan, 608-737 (Korea, Republic of); Seo, Hyo Jin, E-mail: hjseo@pknu.ac.kr [Department of Physics and Interdisciplinary Program of Biomedical, Mechanical & Electrical Engineering, Pukyong National University, Busan, 608-737 (Korea, Republic of)

    2016-12-15

    Highlights: • Double perovskite Sr{sub 2}NiMoO{sub 6} nanoparticles were prepared via sol-gel route. • The nanoparticles have efficient optical absorption in visible light. • The band structure and energy positions were determined. • The perovskite has efficient photocatalytic on RhB photodegradation. • Multivalent Mo and Ni-ions on the surfaces were investigated. - Abstract: Double perovskite Sr{sub 2}NiMoO{sub 6} nanoparticles were synthesized via the chemical sol-gel route. The phase formation was investigated through X-ray polycrystalline diffraction (XRD) and Rietveld refinements. The perovskite crystallized in worm-like nano-grains with the diameter of 20–50 nm. The optical properties were measured by the optical absorption spectra. The nanoparticles present an indirect allowed transition with a narrow band gap of 2.1 eV. Sr{sub 2}NiMoO{sub 6} nanoparticles have obvious photocatalytic ability on the degradation of Rhodamine B (RhB) solutions under the irradiation of visible light. The transport behaviors of the excitons were investigated from the photoluminescence spectra and the corresponding decay lifetimes. Sr{sub 2}NiMoO{sub 6} nanoparticles present several advantages for photocatalysis such as the appropriate band energy positions, the quenched luminescence, and the coexistence of multivalent ions in the lattices.

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

    Science.gov (United States)

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

    2012-05-07

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

  8. Synthesis, X-ray crystal structure and optical properties research of novel diphenyl sulfone-based bis-pyrazoline derivatives

    International Nuclear Information System (INIS)

    Gong Zhongliang; Zheng Liangwen; Zhao Baoxiang

    2012-01-01

    A series of novel bis-pyrazoline derivatives were synthesized by the reaction of chalcone and (sulfonylbis(3,1-phenylene))bis(hydrazine) in 20–34% yields. The structures of the compounds were determined by IR, 1 H NMR, HRMS spectra, and a representative compound 3b was confirmed based on the X-ray crystallographic analysis. Absorption and fluorescence spectra of these compounds in dichloromethane solution were investigated. The results showed that the emission maxima varied from 415 to 444 nm mainly depending on C3 substituents of pyrazoline moiety. The compounds had higher quantum yields, when C3 substituent was an electron-withdrawing p-chlorophenyl group. Moreover, absorption spectra and emission spectra exhibited a blue-shift and a red-shift with increasing the polarity of solvents, respectively. Fluorescent molecules happened to collide with each other and resulted in quench of the fluorescence when the concentration increased over to 10 −5 M. - Highlights: ► A series of novel diphenyl sulfone-based bis-pyrazoline derivatives were designed and synthesized. ► Their UV–vis absorption and fluorescence emission spectra were investigated. ► The relationship of substituents and the optical properties were discussed. ► With increasing the solvent polarity, fluorescence emission displayed a red-shift and fluorescence quantum yields decreased. ► Fluorescence was quenched when the concentration increased over to 10 −5 M.

  9. Synthesis and effect of copper incorporation on the thermoluminescence and structural properties of SiO{sub 2} particles

    Energy Technology Data Exchange (ETDEWEB)

    Burruel I, S. E.; Cruz V, C.; Salas J, Ch. J. [Universidad de Sonora, Departamento de Investigacion en Polimeros y Materiales, Apdo. Postal 130, 83000 Hermosillo, Sonora (Mexico); Bernal, R. [Universidad de Sonora, Centro de Investigacion en Fisica, Apdo. Postal 5-088, 83190 Hermosillo, Sonora (Mexico); Garcia H, A. R. [Universidad de Sonora, Departamento de Ciencias Quimico Biologicas, 83000 Hermosillo, Sonora (Mexico); Castano, V. M., E-mail: silvia@gimmunison.com [UNAM, Instituto de Fisica, Departamento de Fisica Aplicada y Tecnologia Avanzada, Apdo. Postal 1-1010, 76000 Queretaro, Qro. (Mexico)

    2015-10-15

    Full text: In this work, we evaluated the effect of Cu-dopant concentration in SiO{sub 2} particles on structural and thermoluminescence (Tl) properties, prepared by the sol-gel technique. Tl studies in silica samples containing Cu show an important enhancement of their Tl response when compared with pure silica samples. In the copper doped silica a prominent Tl peak is observed, the glow curve was observed between 70 and 450 degrees C after exposure to beta irradiation. The maximum temperature of the glow peak centered at around 140 degrees C shifts to higher values and the intensity enhancement with increasing Cu content, this glow curve is surely composed of several overlapped individual Tl peaks. Also, the particle size is affected by the concentration of Cu dopant. In the case SiO{sub 2}, only is observed a glow peak centered to 95 degrees C, which is interesting for non-Tl dosimetry of ionizing radiation, which is based in detecting the afterglow response following exposure to radiation. The dose response of SiO{sub 2}:Cu showed a linear behaviour in the interval studied with no saturation evidence until 6.4 kGy, which makes this material suitable and promising for medical, industrial and also space dosimetry applications. (Author)

  10. Synthesis, crystal structure, physicochemical properties of hydrogen bonded supramolecular assembly of N,N-diethylanilinium-3, 5-dinitrosalicylate crystal

    Science.gov (United States)

    Rajkumar, M.; Chandramohan, A.

    2017-12-01

    An organic salt, N,N-diethylanilinium 3,5-dinitrosalicylate was synthesized and single crystals grown by employing the slow solvent evaporation solution growth technique in methanol-acetone (1:1) mixture. The electronic transitions of the salt crystal were studied by UV-Visible spectrum. The optical transmittance window and lower wavelength cut-off of grown crystal have been identified by UV-Vis-NIR studies. The FT-IR spectrum was recorded to confirm the presence of various functional groups in the grown crystal. 1H and 13C NMR spectrum were recorded to establish the molecular structure of the title crystal. Single crystal X-ray diffraction data indicated that the crystal belongs to monoclinic crystal system with P21/n space group. The thermal stability of the crystal was established by TG/DTA studies. The mechanical properties of the grown crystal were studied by Vickers' microhardness technique. The dielectric studies indicated that the dielectric constant and dielectric loss decrease exponentially with frequency at different temperatures.

  11. Synthesis and effect of copper incorporation on the thermoluminescence and structural properties of SiO2 particles

    International Nuclear Information System (INIS)

    Burruel I, S. E.; Cruz V, C.; Salas J, Ch. J.; Bernal, R.; Garcia H, A. R.; Castano, V. M.

    2015-10-01

    Full text: In this work, we evaluated the effect of Cu-dopant concentration in SiO 2 particles on structural and thermoluminescence (Tl) properties, prepared by the sol-gel technique. Tl studies in silica samples containing Cu show an important enhancement of their Tl response when compared with pure silica samples. In the copper doped silica a prominent Tl peak is observed, the glow curve was observed between 70 and 450 degrees C after exposure to beta irradiation. The maximum temperature of the glow peak centered at around 140 degrees C shifts to higher values and the intensity enhancement with increasing Cu content, this glow curve is surely composed of several overlapped individual Tl peaks. Also, the particle size is affected by the concentration of Cu dopant. In the case SiO 2 , only is observed a glow peak centered to 95 degrees C, which is interesting for non-Tl dosimetry of ionizing radiation, which is based in detecting the afterglow response following exposure to radiation. The dose response of SiO 2 :Cu showed a linear behaviour in the interval studied with no saturation evidence until 6.4 kGy, which makes this material suitable and promising for medical, industrial and also space dosimetry applications. (Author)

  12. Synthesis, molecular structure, spectroscopic properties and stability of (Z)-N-methyl-C-2,4,6-trimethylphenylnitrone

    Science.gov (United States)

    Lasri, Jamal; Ismail, Ali I.; Haukka, Matti; Soliman, Saied M.

    2015-02-01

    New N-methyl-C-2,4,6-trimethylphenylnitrone 1 has been synthesized starting from N-methylhydroxylamine and mesitaldehyde. The product was fully characterized using different spectroscopic techniques; FTIR, NMR, UV-Vis, high resolution mass spectrometry and X-ray diffraction. The relative stability and percent of population of its two possible isomers (E and Z) were calculated using the B3LYP/6-311++G(d,p) method in gas phase and in solution. In agreement with the X-ray results, it was found that Z-isomer is the most stable one in both gas phase and solution. The molecular geometry, vibrational frequencies, gauge-including atomic orbital (GIAO), and chemical shift values were also calculated using the same level of theory. The TD-DFT results of the studied nitrone predicted a π-π∗ transition band at 285.1 nm (fosc = 0.3543) in the gas phase. The rest of the spectral bands undergo either hyperchromic or hypsochromic shifts in the presence of solvent. Polarizability and HOMO-LUMO gap values were used to predict the nonlinear optical properties (NLO) of the studied compound. NBO analysis has been used to determine the most accurate Lewis structure of the studied molecule.

  13. Structure-Processing-Property Relationship of Poly(Glycolic Acid for Drug Delivery Systems 1: Synthesis and Catalysis

    Directory of Open Access Journals (Sweden)

    Vineet Singh

    2010-01-01

    Full Text Available Till date, market is augmented with a huge number of improved drug delivery systems. The success in this area is basically due to biodegradable polymers. Although conventional systems of drug delivery utilizing the natural and semisynthetic polymers so long but synthetic polymer gains success in the controlled drug delivery area due to better degradation profile and controlled network and functionality. The polyesters are the most studied class group due the susceptible ester linkage in their backbone. The Poly(glycolic Acid (PGA, Poly(lactic acid (PLA, and Polylactide-co-glycolide (PLGA are the best profiled polyesters and are most widely used in marketed products. These polymers, however, still are having drawbacks which failed them to be used in platform technologies like matrix systems, microspheres, and nanospheres in some cases. The common problems arose with these polymers are entrapment inefficiency, inability to degrade and release drugs with required profile, and drug instability in the microenvironment of the polymers. These problems are forcing us to develop new polymers with improved physicochemical properties. The present review gave us an insight in the various structural elements of Poly(glycolic acid, polyester, with in depth study. The first part of the review focuses on the result of studies related to synthetic methodologies and catalysts being utilized to synthesize the polyesters. However the author will also focus on the effect of processing methodologies but due some constraints those are not included in the preview of this part of review.

  14. Synthesis, Structures and Luminescence Properties of Metal-Organic Frameworks Based on Lithium-Lanthanide and Terephthalate

    Directory of Open Access Journals (Sweden)

    Mohammed S. M. Abdelbaky

    2016-03-01

    Full Text Available Metal-organic frameworks assembled from Ln(III, Li(I and rigid dicarboxylate ligand, formulated as [LiLn(BDC2(H2O·2(H2O] (MS1-6,7a and [LiTb(BDC2] (MS7b (Ln = Tb, Dy, Ho, Er, Yb, Y0.96Eu0.04, Y0.93Tb0.07, and H2BDC = terephthalic acid, were obtained under hydrothermal conditions. The isostructural MS1-6 crystallize in monoclinic P21/c space group. While, in the case of Tb3+ a mixture of at least two phases was obtained, the former one (MS7a and a new monoclinic C2/c phase (MS7b. All compounds have been studied by single-crystal and powder X-ray diffraction, thermal analyses (TGA, vibrational spectroscopy (FTIR, and scanning electron microscopy (SEM-EDX. The structures of MS1-6 and MS7a are built up of inorganic-organic hybrid chains. These chains constructed from unusual four-membered rings, are formed by edge- and vertex-shared {LnO8} and {LiO4} polyhedra through oxygen atoms O3 (vertex and O6-O7 (edge. Each chain is cross-linked to six neighboring chains through six terephthalate bridges. While, the structure of MS7b is constructed from double inorganic chains, and each chain is, in turn, related symmetrically to the adjacent one through the c glide plane. These chains are formed by infinitely alternating {LiO4} and {TbO8} polyhedra through (O2-O3 edges to create Tb–O–Li connectivity along the c-axis. Both MS1-6,7a and MS7b structures possess a 3D framework with 1D trigonal channels running along the a and c axes, containing water molecules and anhydrous, respectively. Topological studies revealed that MS1-6 and MS7a have a new 2-nodal 3,10-c net, while MS7b generates a 3D net with unusual β-Sn topology. The photoluminescence properties Eu- and Tb-doped compounds (MS5-6 are also investigated, exhibiting strong red and green light emissions, respectively, which are attributed to the efficient energy transfer process from the BDC ligand to Eu3+ and Tb3+.

  15. Synthesis and properties of bimetallic aluminium alkoxides

    International Nuclear Information System (INIS)

    Vyshinskaya, K.I.; Vasil'ev, G.A.; Vishnyakova, T.A.

    1997-01-01

    A single stage method of aluminium bimetallic alkoxide synthesis, which consists in activated aluminium reaction with metal salts in the relevant alcohols, has been developed. Properties of the compounds prepared are described

  16. Synthesis, structure, and electronic properties of a dimer of Ru(bpy)2 doubly bridged by methoxide and pyrazolate.

    Science.gov (United States)

    Jude, Hershel; Rein, Francisca N; White, Peter S; Dattelbaum, Dana M; Rocha, Reginaldo C

    2008-09-01

    The heterobridged dinuclear complex cis,cis-[(bpy) 2Ru(mu-OCH 3)(mu-pyz)Ru(bpy) 2] (2+) ( 1; bpy = 2,2'-bipyridine; pyz = pyrazolate) was synthesized and isolated as a hexafluorophosphate salt. Its molecular structure was fully characterized by X-ray crystallography, (1)H NMR spectroscopy, and ESI mass spectrometry. The compound 1.(PF 6) 2 (C 44H 38F 12N 10OP 2Ru 2) crystallizes in the monoclinic space group P2 1/ c with a = 13.3312(4) A, b = 22.5379(6) A, c = 17.2818(4) A, beta = 99.497(2) degrees , V = 5121.3(2) A (3), and Z = 4. The meso diastereoisomeric form was exclusively found in the crystal structure, although the NMR spectra clearly demonstrated the presence of two stereoisomers in solution (rac and meso forms at approximately 1:1 ratio). The electronic properties of the complex in acetonitrile were investigated by cyclic voltammetry and UV-vis and NIR-IR spectroelectrochemistries. The stepwise oxidation of the Ru (II)-Ru (II) complex into the mixed-valent Ru (II)-Ru (III) and fully oxidized Ru (III)-Ru (III) states is fully reversible on the time scale of the in situ (spectro)electrochemical measurements. The mixed-valent species displays strong electronic coupling, as evidenced by the large splitting between the redox potentials for the Ru(III)/Ru(II) couples (Delta E 1/2 = 0.62 V; K c = 3 x 10 (10)) and the appearance of an intervalence transfer (IT) band at 1490 nm that is intense, narrow, and independent of solvent. Whereas this salient band in the NIR region originates primarily from highest-energy of the three IT transitions predicted for Ru(II)-Ru(III) systems, a weaker absorption band corresponding to the lowest-energy IT transition was clearly evidenced in the IR region ( approximately 3200 cm (-1)). The observation of totally coalesced vibrational peaks in the 1400-1650 cm (-1) range for a set of five bpy spectator vibrations in Ru (II)-Ru (III) relative to Ru (II)-Ru (II) and Ru (III)-Ru (III) provided evidence for rapid electron transfer and

  17. Synthesis, crystal structures, and luminescent properties of two series' of new lanthanide (III) amino-carboxylate-phosphonates.

    Science.gov (United States)

    Zhou, Tian-Hua; Yi, Fei-Yan; Li, Pei-Xin; Mao, Jiang-Gao

    2010-02-01

    Hydrothermal reactions of lanthanide(III) chlorides with 4-HOOC-C(6)H(4)-CH(2)NHCH(2)PO(3)H(2) (H(3)L) at different ligand-to-metal (L/M) ratios afforded nine new lanthanide(III) carboxylate-phosphonates with two types of 3D network structures, namely, LnCl(HL)(H(2)O)(2) (Ln = Sm, 1; Eu, 2; Gd, 3; Tb, 4; Dy, 5; Er, 6) and [Ln(2)(HL)(H(2)L)(L)(H(2)O)(2)].4H(2)O (Ln = Nd, 7; Sm, 8; Eu, 9). Compounds 1-6 are isostructural and feature a 3D network in which the LnO(7)Cl polyhedra are interconnected by bridging CPO(3) tetrahedra into 2D inorganic layers parallel to the bc plane. These layers are further cross-linked by organic groups of the carboxylate-phosphonate ligands via the coordination of the carboxylate groups into a pillared-layered architecture. Compounds 7-9 are also isostructural and feature a 3D open-framework composed of 1D lanthanide(III) phosphonate inorganic slabs which are further bridged by organic groups of the carboxylate-phosphonate liagnds via the coordination of the carboxylate groups, forming large 1D tunnels along the b-axis which are filled by lattice water molecules. Luminescent measurements indicate that compounds 2, 4, and 5 show strong emission bands in red, green, and yellow light region, respectively. Magnetic properties of 2, 3, 5, and 7 have also been studied.

  18. Synthesis, structural characterization and photoluminescence properties of rhenium(I) complexes based on bipyridine derivatives with carbazole moieties.

    Science.gov (United States)

    Li, Hong-Yan; Wu, Jing; Zhou, Xin-Hui; Kang, Ling-Chen; Li, Dong-Ping; Sui, Yan; Zhou, Yong-Hui; Zheng, You-Xuan; Zuo, Jing-Lin; You, Xiao-Zeng

    2009-12-21

    Three N,N-bidentate ligands, 5,5'-dibromo-2,2-bipyridine (L1) and two carbazole containing ligands of 5-bromo-5'-carbazolyl-2,2-bipyridine (L2), 5,5'-dicarbazolyl-2,2'-bipyridine (L3), and their corresponding rhenium Re(CO)3Cl(L) complexes (ReL1-ReL3) have been successfully synthesized and characterized by elemental analysis, 1H NMR and IR spectra. Their photophysical properties and thermal analysis, along with the X-ray crystal structure analysis of L3 and complexes ReL1 and ReL3 are also described. In CH2Cl2 solution at room temperature, all complexes display intense absorption bands at ca. 220-350 nm, which can be assigned to spin-allowed intraligand (pi-->pi*) transitions, and the low energy broad bands in the 360-480 nm region are attributed to the metal to ligand charge-transfer d(Re)-->pi* (diimine) (MLCT). The introduction of carbazole moieties improves the MLCT absorption and molar extinction coefficient of these complexes. Upon excitation at the peak maxima, all complexes show strong emissions around 620 nm, which are assigned to d(Re)-->pi* (diimine) MLCT phosphorescence. The photoluminescence lifetime decay of Re(I) complexes were measured and the quantum efficiencies of the rhenium(I) complexes were calculated by using air-equilibrated [Ru(bpy)3]2+ x 2 Cl- aqueous solution as standard (phi(std) = 0.028). The complexes with appended carbazole moieties exhibit enhanced luminescence performances relative to ReL1.

  19. Synthesis, Crystal Structure and Luminescent Property of Cd (II Complex with N-Benzenesulphonyl-L-leucine

    Directory of Open Access Journals (Sweden)

    Xishi Tai

    2012-09-01

    Full Text Available A new trinuclear Cd (II complex [Cd3(L6(2,2-bipyridine3] [L = N-phenylsulfonyl-L-leucinato] has been synthesized and characterized by elemental analysis, IR and X-ray single crystal diffraction analysis. The results show that the complex belongs to the orthorhombic, space group P212121 with a = 16.877(3 Å, b = 22.875(5 Å, c = 29.495(6 Å, α = β = γ = 90°, V = 11387(4 Å3, Z = 4, Dc= 1.416 μg·m−3, μ = 0.737 mm−1, F (000 = 4992, and final R1 = 0.0390, ωR2 = 0.0989. The complex comprises two seven-coordinated Cd (II atoms, with a N2O5 distorted pengonal bipyramidal coordination environment and a six-coordinated Cd (II atom, with a N2O4 distorted octahedral coordination environment. The molecules form one dimensional chain structure by the interaction of bridged carboxylato groups, hydrogen bonds and p-p interaction of 2,2-bipyridine. The luminescent properties of the Cd (II complex and N-Benzenesulphonyl-L-leucine in solid and in CH3OH solution also have been investigated.

  20. Effect of Synthesis Temperature on Structure and Magnetic Properties of (La,Nd)0.7Sr0.3MnO3 Nanoparticles.

    Science.gov (United States)

    Shlapa, Yulia; Solopan, Sergii; Bodnaruk, Andrii; Kulyk, Mykola; Kalita, Viktor; Tykhonenko-Polishchuk, Yulia; Tovstolytkin, Alexandr; Belous, Anatolii

    2017-12-01

    Two sets of Nd-doped La 0.7 Sr 0.3 MnO 3 nanoparticles were synthesized via sol-gel method with further heat treatment at 1073 and 1573 K, respectively. Crystallographic and magnetic properties of obtained nanoparticles were studied, and the effect of synthesis conditions on these properties was investigated. According to X-ray data, all particles crystallized in the distorted perovskite structure. Magnetic parameters, such as saturation magnetization, coercivity, Curie temperature, and specific loss power, which is released on the exposure of an ensemble of nanoparticles to AC magnetic field, were determined for both sets of samples. The correlation between the values of Curie temperature and maximal heating temperature under AC magnetic field was found. It was revealed that for the samples synthesized at 1573 K, the dependences of crystallographic and magnetic parameters on Nd content were monotonous, while for the samples synthesized at 1073 K, they were non-monotonous. It was concluded that Nd-doped La 0.7 Sr 0.3 MnO 3 nanoparticles are promising materials for self-controlled magnetic hyperthermia applications, but the researchers should be aware of the unusual behavior of the particles synthesized at relatively low temperatures.

  1. 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.

  2. A novel zinc(II) metal–organic framework with a diamond-like structure: synthesis, study of thermal robustness and gas adsorption properties

    Czech Academy of Sciences Publication Activity Database

    Almáši, M.; Zeleňák, V.; Zukal, Arnošt; Kuchár, J.; Čejka, Jiří

    2016-01-01

    Roč. 45, č. 3 (2016), s. 1233-1242 ISSN 1477-9226 R&D Projects: GA ČR GA14-07101S Institutional support: RVO:61388955 Keywords : synthesis * gas adsorption properties * physical chemistry Subject RIV: CF - Physical ; Theoretical Chemistry Impact factor: 4.029, year: 2016

  3. CTAB-Assisted Hydrothermal Synthesis of WO3 Hierarchical Porous Structures and Investigation of Their Sensing Properties

    Directory of Open Access Journals (Sweden)

    Dan Meng

    2015-01-01

    Full Text Available WO3 hierarchical porous structures were successfully synthesized via cetyltrimethylammonium bromide- (CTAB- assisted hydrothermal method. The structure and morphology were investigated using scanning electron microscope, X-ray diffractometer, transmission electron microscopy, X-ray photoelectron spectra, Brunauer-Emmett-Teller nitrogen adsorption-desorption, and thermogravimetry and differential thermal analysis. The result demonstrated that WO3 hierarchical porous structures with an orthorhombic structure were constructed by a number of nanoparticles about 50–100 nm in diameters. The H2 gas sensing measurements showed that well-defined WO3 hierarchical porous structures with a large specific surface area exhibited the higher sensitivity compared with products without CTAB at all operating temperatures. Moreover, the reversible and fast response to H2 gas and good selectivity were obtained. The results indicated that the WO3 hierarchical porous structures are promising materials for gas sensors.

  4. CoFe2O4 nanocrystalline powders prepared by citrate-gel methods: Synthesis, structure and magnetic properties

    International Nuclear Information System (INIS)

    Cannas, C.; Falqui, A.; Musinu, A.; Peddis, D.; Piccaluga, G.

    2006-01-01

    Nanocrystalline CoFe 2 O 4 powders were prepared by decomposition of metal ion citrate precursors. Four samples were synthesized from precursor solutions having different pH values in the range 2 physisorption and Transmission Electron Microscopy. Magnetic properties were explored by a SQUID magnetometer. Three out of the four samples, coming from solutions of pH 2, 4 and 7, were produced by an autocombustion reaction and are very similar as regards average size of the nanoparticles (about 20 nm), their morphology and the magnetic properties, while the fourth sample was produced by a slower thermal decomposition and is composed of smaller nanoparticles (about 10 nm)

  5. Structure and magnetic properties of Co and Ni nano-ferrites prepared by a two step direct microemulsions synthesis

    Czech Academy of Sciences Publication Activity Database

    Pulišová, Petra; Kováč, J.; Voigt, A.; Raschman, P.

    2013-01-01

    Roč. 341, september (2013), s. 93-99 ISSN 0304-8853 Institutional support: RVO:61388980 Keywords : Precipitation in microemulsion s * Ferrite nano-powder * Magnetic properties * ZFC * FC measurements Subject RIV: CA - Inorganic Chemistry Impact factor: 2.002, year: 2013

  6. Hydrothermal synthesis, crystal structure and properties of a novel chain coordination polymer constructed by tetrafunctional phosphonate anions and cobalt ions

    International Nuclear Information System (INIS)

    Guan, Lei; Wang, Ying

    2015-01-01

    A novel cobalt phosphonate, [Co(HL)(H 2 O) 3 ] n (1) (L=N(CH 2 PO 3 H) 3 3− ) has been synthesized by hydrothermal reaction at 150 °C and structurally characterized by X-ray diffraction, infrared spectroscopy, elemental and thermogravimetric analysis. Complex 1 features a 1D chain structure with double-channel built from CoO 6 octahedra bridged together by the phosphonate groups. Each cobalt ion is octahedrally coordinated by three phosphonate oxygen atoms and three water molecules. The coordinated water molecules can form the hydrogen bonds with the phosphonate oxygen atoms to link the 1D chains, building a 2D layered structure, further resulting in a 3D network. The luminescence spectrum indicates an emission maximum at 435 nm. The magnetic susceptibility curve exhibits a dominant antiferromagnetic behavior with a weakly ferromagnetic component at low temperatures. - Graphical abstract: The connectivity between cobalt ions and the ligands results in a chain structure with a 1D double-channel structure, which is constructed by A-type subrings and B-type subrings. - Highlights: • The tetrafunctional phosphonate ligand was used as the ligand. • A novel chain structure can be formed by A-type rings and B-type rings. • Two types of rings can form a 1D double-channel structure, along the c-axis

  7. Template Synthesis, Crystal Structure, and Magnetic Properties of a Dinuclear Copper(II) Complex with Cooperative Hydrogen Bonding

    International Nuclear Information System (INIS)

    Kang, Shin Geol; Nam, Kwang Hee; Min, Kil Sik; Lee, Uk

    2011-01-01

    The dinuclear complex with cooperative hydrogen bonds can be prepared by the metal-directed reaction of Eq. This work shows that the coordinated hydroxyl group trans to the secondary amino group is deprotonated more readily than that trans to the tertiary amino group and acts as the hydrogen-bond accepter. The lattice water molecules in act as bridges between the two mononuclear units through hydrogen bonds. The complex is quite stable as the dimeric form even in various polar solvents. The complex exhibits a weak antiferromagnetic interaction between the metal ions in spite of relatively long Cu···Cu distance. This strongly supports the suggestion that the antiferromagnetic behavior is closely related to the cooperative hydrogen bonds. The design and synthesis of polynuclear transition metal complexes have received much attention because of their potential applications in various fields, such as catalysis, supramolecular chemistry, and materials chemistry. Until now, various types of dinuclear copper(II) complexes have been prepared and investigated. Some dinuclear copper(II) complexes resulting from cooperative hydrogen bonding, such as containing two N_2O_2 donor sets, are also reported

  8. Controllable synthesis and electrochemical hydrogen storage properties of Sb₂Se₃ ultralong nanobelts with urchin-like structures.

    Science.gov (United States)

    Jin, Rencheng; Chen, Gang; Pei, Jian; Sun, Jingxue; Wang, Yang

    2011-09-01

    The controlled synthesis of one-dimensional and three-dimensional Sb(2)Se(3) nanostructures has been achieved by a facile solvothermal process in the presence of citric acid. By simply controlling the concentration of citric acid, the nucleation, growth direction and exposed facet can be readily tuned, which brings the different morphologies and nanostructures to the final products. The as-prepared products have been characterized by means of X-ray diffraction, field-emission scanning electron microscopy, transmission electron microscopy (TEM), high-resolution TEM and selected area electron diffraction. Based on the electron microscope observations, a possible growth mechanism of Sb(2)Se(3) with distinctive morphologies including ultralong nanobelts, hierarchical urchin-like nanostructures is proposed and discussed in detail. The electrochemical hydrogen storage measurements reveal that the morphology plays a key role on the hydrogen storage capacity of Sb(2)Se(3) nanostructures. The Sb(2)Se(3) ultralong nanobelts with high percentage of {-111} facets exhibit higher hydrogen storage capacity (228.5 mA h g(-1)) and better cycle stability at room temperature.

  9. Optical and structural properties of undoped and Mn{sup 2+} doped Ca–Li hydroxyapatite nanopowders using mechanochemical synthesis

    Energy Technology Data Exchange (ETDEWEB)

    Ravindranadh, K. [Department of Physics, Andhra Loyola College, Vijayawada 520008 (India); Department of Physics, Acharya Nagarjuna University, Guntur 522510 (India); Babu, B.; Pushpa Manjari, V.; Thirumala Rao, G. [Department of Physics, Acharya Nagarjuna University, Guntur 522510 (India); Rao, M.C. [Department of Physics, Andhra Loyola College, Vijayawada 520008 (India); Ravikumar, R.V.S.S.N., E-mail: rvssn@yahoo.co.in [Department of Physics, Acharya Nagarjuna University, Guntur 522510 (India)

    2015-03-15

    Undoped and Mn{sup 2+} doped calcium–lithium hydroxyapatite (CLHA) nanopowders were prepared by mechanochemical synthesis. The prepared samples were characterized by powder X-ray diffraction, scanning electron microscope, transmission electron microscope, optical absorption, photoluminescence, electron paramagnetic resonance and FT-IR spectroscopy techniques. From powder XRD pattern, lattice cell parameters and average crystallite sizes were evaluated. The morphologies of prepared samples were analyzed by using SEM and TEM studies. Optical and EPR data confirmed that the doped Mn{sup 2+} enter into the host material as distorted octahedral site. Photoluminescence spectra of undoped and Mn{sup 2+} doped CLHA nanopowders exhibited blue, blue-green emission bands at 425, 443, 468 nm and green, strong orange emission bands at 534, 577 nm respectively under the excitation wavelength of 365 nm. The CIE chromaticity coordinates were also calculated from emission spectra for undoped and Mn{sup 2+} doped CLHA nanopowders. Vibrational bands related to phosphate molecules, P–O–H and hydroxyl ions are observed in FT-IR spectra. - Highlights: • PXRD pattern of prepared undoped and Mn{sup 2+} doped CLHA nanopowders are in nanosize. • Optical and EPR studies reveal site symmetry of Mn{sup 2+} doped CLHA nanopowders are distorted octahedral symmetry. • FT-IR spectra exhibits the various vibrational modes of phosphate ions, P–O–H and water molecules.

  10. Optical and structural properties of undoped and Mn2+ doped Ca–Li hydroxyapatite nanopowders using mechanochemical synthesis

    International Nuclear Information System (INIS)

    Ravindranadh, K.; Babu, B.; Pushpa Manjari, V.; Thirumala Rao, G.; Rao, M.C.; Ravikumar, R.V.S.S.N.

    2015-01-01

    Undoped and Mn 2+ doped calcium–lithium hydroxyapatite (CLHA) nanopowders were prepared by mechanochemical synthesis. The prepared samples were characterized by powder X-ray diffraction, scanning electron microscope, transmission electron microscope, optical absorption, photoluminescence, electron paramagnetic resonance and FT-IR spectroscopy techniques. From powder XRD pattern, lattice cell parameters and average crystallite sizes were evaluated. The morphologies of prepared samples were analyzed by using SEM and TEM studies. Optical and EPR data confirmed that the doped Mn 2+ enter into the host material as distorted octahedral site. Photoluminescence spectra of undoped and Mn 2+ doped CLHA nanopowders exhibited blue, blue-green emission bands at 425, 443, 468 nm and green, strong orange emission bands at 534, 577 nm respectively under the excitation wavelength of 365 nm. The CIE chromaticity coordinates were also calculated from emission spectra for undoped and Mn 2+ doped CLHA nanopowders. Vibrational bands related to phosphate molecules, P–O–H and hydroxyl ions are observed in FT-IR spectra. - Highlights: • PXRD pattern of prepared undoped and Mn 2+ doped CLHA nanopowders are in nanosize. • Optical and EPR studies reveal site symmetry of Mn 2+ doped CLHA nanopowders are distorted octahedral symmetry. • FT-IR spectra exhibits the various vibrational modes of phosphate ions, P–O–H and water molecules

  11. Structural, optical, thermal and Photocatalytic properties of ZnO nanoparticles of Betel Leave by using Green synthesis method

    Directory of Open Access Journals (Sweden)

    S. Rajesh

    2016-07-01

    Full Text Available In this present study reports the green synthesis of zinc oxide nanoparticles using Betel leaf extracts and zinc acetate. The functionalization of ZnO particles through Betel leaf extract mediated bio reduction of ZnO was investigated through X-ray diffraction, Field emission scanning electron microscopy, photoluminescence, thermal gravimetric-differential thermal analysis, hexagonal shaped ZnO-nanoparticles  with  size  about  50 nm  were synthesized and characterized using X-ray diffraction analysis. The diameter of the nanoparticles in the range of 50 nm was found from scanning electron microscopy study. Photo luminescence study reveals the blue emission at 463nm respectively. hermal gravimetric-differential thermal analysis show that the observed at 480oC, indicating that no decomposition occurs above this temperature. The photocatalytic degradation of methylene blue dye was examined using ZnO nanoparticles under solar as well as ultra violet light irradiation of the MB dye. The  method  stands out primarily due to the fact that it is eco-friendly and shuts down the demerits of conventional  physical  and  chemical  methods. These particles are anticipated to have extensive applications in various industries.

  12. Synthesis, crystal structure, and properties of the ordered double perovskite Sr_2CoOsO_6

    International Nuclear Information System (INIS)

    Kumar Paul, Avijit; Reehuis, Manfred; Felser, Claudia; Abdala, Paula M.; Jansen, Martin

    2013-01-01

    Sr_2CoOsO_6, a new osmium based ordered semiconductor double perovskite was prepared by solid state synthesis from the respective binary oxides. Room temperature PXRD analysis shows the compound to be tetragonal [I4/m; a = 5.5503(1) Aa and c = 7.9320(1) Aa], whereas low temperature synchrotron data refinement has revealed a second monoclinic polymorph [I2/m; a = 5.4969(2) Aa, b = 5.4979(2) Aa, c = 8.0090(1) Aa and γ = 90.527(1) ] with a fully ordered rocksalt arrangement of cobalt and osmium atoms over the perovskite B-sites. Heat capacity and magnetic measurements indicate that Sr_2CoOsO_6 shows antiferromagnetic ordering below T_N = 108 K followed by a second magnetic transition at T_2 = 65 K. It was shown that the change from the tetragonal to the monoclinic phase occurs at T_N. (Copyright copyright 2013 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  13. Synthesis, structures, and properties of alkali and alkaline earth coordination polymers based on V-shaped ligand

    Czech Academy of Sciences Publication Activity Database

    Cheng, P. C.; Tseng, F. S.; Yeh, C. T.; Chang, T. G.; Kao, C. C.; Lin, C. H.; Liu, W. R.; Chen, J. S.; Zima, Vítězslav

    2012-01-01

    Roč. 14, č. 20 (2012), s. 6812-6822 ISSN 1466-8033 Institutional support: RVO:61389013 Keywords : metal organic frameworks * structure * carboxylates Subject RIV: CA - Inorganic Chemistry Impact factor: 3.879, year: 2012

  14. Surface active monomers synthesis, properties, and application

    CERN Document Server

    Borzenkov, Mykola

    2014-01-01

    This brief includes information on the background?of and development of synthesis of various types of surface active monomers. The authors explain the importance of utilization of surface active monomers for creation of surface active polymers? and the various biomedical applications of such compounds . This brief introduces techniques for the synthesis of novel types of surface active monomers, their colloidal and polymerizable properties and application for needs of medicine and biology.

  15. Synthesis, structural and electrical properties of [C{sub 2}H{sub 10}N{sub 2}][(SnCl(NCS){sub 2}]{sub 2}

    Energy Technology Data Exchange (ETDEWEB)

    Karoui, Sahel [Laboratoire genie de materiaux et environnement, ENIS, BP.1173,3038- Sfax, Universite de Sfax (Tunisia); Kamoun, Slaheddine, E-mail: slah.kamoun@gmail.com [Laboratoire genie de materiaux et environnement, ENIS, BP.1173,3038- Sfax, Universite de Sfax (Tunisia); Jouini, Amor [Laboratoire de Chimie du Solide, Departement de Chimie, Faculte des Sciences de Monastir, 5019 Monastir (Tunisia)

    2013-01-15

    Synthesis, structural and electrical properties are given for a new organic stannous pseudo halide material. The structure of the [C{sub 2}H{sub 10}N{sub 2}][(SnCl(NCS){sub 2}]{sub 2} reveals that the adjacent Sn(II) centres are bridged by a pair of SCN{sup -} anions to form a 1-D array giving rise to the anionic chains (SnCl(NCS){sub 2}){sub n}{sup n-}. These chains are themselves interconnected by means of N-H Horizontal-Ellipsis Cl(S) hydrogen bonds originating from the organic cation [(NH{sub 3}){sub 2}(CH{sub 2}){sub 2}]{sup 2+}. The AC impedance measurements were performed as a function of both frequency and temperature. The electrical conduction and dielectric relaxation have been studied. The activation energy associated with the electrical relaxation determined from the electric modulus spectra was found close to that of the activation energy obtained for DC conductivity. The conduction mechanisms are attributed to the quantum mechanical tunneling model in phase I and to the proton hopping among hydrogen vacancies in phase II. - Graphical abstract: Atomic coordination in [C2H10N2][SnCl(NCS)2)2]. Highlights: Black-Right-Pointing-Pointer X-ray diffraction analysis shows the 1D network character of the structure. Black-Right-Pointing-Pointer DSC experiments show a phase transition at 336 K. Black-Right-Pointing-Pointer The AC conductivity is interpreted in terms of Jonsher's law. Black-Right-Pointing-Pointer Two conduction mechanisms are proposed for phase I and II.

  16. Nd(III) and Dy(III) coordination compounds based on 1H-tetrazolate-5-acetic acid ligands: Synthesis, crystal structures and catalytic properties

    Energy Technology Data Exchange (ETDEWEB)

    Li Qiaoyun; Chen Dianyu; He Minghua [Jiangsu Laboratory of Advanced Functional Materials, Department of Chemistry and Materials Engineering, Changshu Institute of Technology, Changshu 215500, Jiangsu (China); Yang Gaowen, E-mail: ygwsx@126.com [Jiangsu Laboratory of Advanced Functional Materials, Department of Chemistry and Materials Engineering, Changshu Institute of Technology, Changshu 215500, Jiangsu (China); Shen Lei; Zhai Chun; Shen Wei; Gu Kun; Zhao Jingjing [Jiangsu Laboratory of Advanced Functional Materials, Department of Chemistry and Materials Engineering, Changshu Institute of Technology, Changshu 215500, Jiangsu (China)

    2012-06-15

    Reactions of 1H-tetrazolate-5-acetic acid(H{sub 2}tza) with Nd(NO{sub 3}){sub 3}{center_dot}6H{sub 2}O or Dy(NO{sub 3}){sub 3}{center_dot}6H{sub 2}O with the presence of KOH under solvothermal conditions, produced two new coordination compounds, [M{sub 2}(tza){sub 3}(H{sub 2}O){sub 6}]{center_dot}2H{sub 2}O [M=Nd(1), Dy(2)]. Both compounds were structurally characterized by elemental analysis, IR spectroscopy and single-crystal X-ray diffraction. Compounds 1 and 2 reveal 1D structures via bridging tza as linker. Furthermore, the compounds 1 and 2 showed a specific and good catalytic behavior for the polymerization of styrene, and the polymerization showed controlled characteristics. - Graphical Abstract: Two new coordination compounds, [M{sub 2}(tza){sub 3}(H{sub 2}O){sub 6}]{center_dot}2H{sub 2}O [M=Nd(1), Dy(2)] have been synthesis. 1 and 2 reveal 1D structures via bridging tza as linker, and showed a specific and good catalytic behavior for the polymerization of styrene. Highlights: Black-Right-Pointing-Pointer we have reported two novel compounds formed by H{sub 2}tza and Nd(III) or Dy(III). Black-Right-Pointing-Pointer Compounds 1 and 2 were found to have catalysis property for the photo-polymerization of styrene. Black-Right-Pointing-Pointer The high molecular weight polymers with narrow molecular weight distributions were obtained.

  17. Carbon Domains on MoS2/TiO2 System via Catalytic Acetylene Oligomerization: Synthesis, Structure, and Surface Properties

    Directory of Open Access Journals (Sweden)

    Sara Cravanzola

    2017-11-01

    Full Text Available Carbon domains have been obtained at the surface of a MoS2/TiO2 (Evonik, P25 system via oligomerization and cyclotrimerization reactions involved in the interaction of the photoactive material with acetylene. Firstly, MoS2 nanosheets have been synthesized at the surface of TiO2, via sulfidation of a molybdenum oxide precursor with H2S (bottom-up method. Secondly, the morphology and the structure, the optical and the vibrational properties of the obtained materials, for each step of the synthesis procedure, have been investigated by microscopy and spectroscopy methods. In particular, transmission electron microscopy images provide a simple tool to highlight the effectiveness of the sulfidation process, thus showing 1L, 2L, and stacked MoS2 nanosheets anchored to the surface of TiO2 nanoparticles. Lastly, in-situ FTIR spectroscopy investigation gives insights into the nature of the oligomerized species, showing that the formation of both polyenic and aromatic systems can be taken into account, being their formation promoted by both Ti and Mo catalytic sites. This finding gives an opportunity for the assembly of extended polyenic, polyaromatic, or mixed domains firmly attached at the surface of photoactive materials. The presented approach, somehow different from the carbon adding or doping processes of TiO2, is of potential interest for the advanced green chemistry and energy conversion/transport applications.

  18. The green hydrothermal synthesis of nanostructured Cu2ZnSnSe4 as solar cell material and study of their structural, optical and morphological properties

    Science.gov (United States)

    Vanalakar, S. A.; Agawane, G. L.; Kamble, A. S.; Patil, P. S.; Kim, J. H.

    2017-12-01

    Cu2ZnSnSe4 (CZTSe) has attracted intensive attention as an absorber material for the thin-film solar cells due to its high absorption coefficient, direct band gap, low toxicity, and abundance of its constituent elements. In this study nanostructured CZTSe nanoparticles are prepared via green hydrothermal synthesis without using toxic solvents, organic amines, catalysts or noxious chemicals. The structural, optical, and morphological properties of CZTSe nanostructured powder were studied using X-ray diffraction (XRD), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), UV-vis absorption spectroscopy, and transmission electron microscope (TEM) techniques. Raman peaks at 170, 195, and 232 cm-1 confirm the formation of pure phase CZTSe nanostructured particles. In addition, the EDS and XPS results confirm the appropriate chemical purity of the annealed CZTSe nanoparticles. Meanwhile, the TEM analysis showed the presence of phase pure oval like CZTSe particle with size of about 80-140 nm. The UV-Vis-NIR absorption spectra analysis showed that the optical band gap of CZTSe nanostructured particles is about 1.14 eV. This band gap energy is close to the optimum value of a photovoltaic solar cell absorber material.

  19. Structure and morphology controllable synthesis of Ag/carbon hybrid with ionic liquid as soft-template and their catalytic properties

    International Nuclear Information System (INIS)

    Wu Shuying; Ding Yunsheng; Zhang Xiaomin; Tang Haiou; Chen Long; Li Boxuan

    2008-01-01

    Ag/carbon hybrids were fabricated by the redox of glucose and silver nitrate (AgNO 3 ) in the presence of imidazolium ionic liquid ([C 14 mim]BF 4 ) under hydrothermal condition. Monodisperse carbon hollow sub-microspheres encapsulating Ag nanoparticles and Ag/carbon cables were selectively prepared by varying the concentration of ionic liquid. Other reaction parameters, such as reaction temperature, reaction time and the mole ratio of silver nitrate to glucose, play important roles in controlling the structures of the products. The products were characterized by XRD, TEM (HRTEM), SEM, energy-dispersive X-ray spectroscopy (EDX), FTIR spectroscopy and a Raman spectrometer. The possible formation mechanism was proposed. The catalytic property of the hybrid in the oxidation of 1-butanol by H 2 O 2 was also investigated. - Graphical abstract: Monodisperse carbon hollow nanospheres encapsulating Ag nanoparticles and Ag/carbon nanocables were selectively prepared with ionic liquids as the soft-template. The controllable synthesis of Ag/C nano-hybrids was realized by varying the concentration of ionic liquids, reaction temperature, reaction time and the mole ratio of silver nitrate to glucose. The catalysis of Ag/C nano-hybrid in the oxidation of 1-butanol by H 2 O 2 was also investigated

  20. Impact of High-Temperature, High-Pressure Synthesis Conditions on the Formation of the Grain Structure and Strength Properties of Intermetallic Ni3Al

    Science.gov (United States)

    Ovcharenko, V. E.; Ivanov, K. V.; Boyangin, E. N.; Krylova, T. A.; Pshenichnikov, A. P.

    2018-01-01

    The impact of the preliminary load on 3Ni+Al powder mixture and the impact of the duration of the delay in application of compacting pressure to synthesis product under the conditions of continuous heating of the mixture up to its self-ignition on the grain size and strength properties of the synthesized Ni3Al intermetallide material have been studied. The grain structure of the intermetallide synthesized under pressure was studied by means of metallography, transmission electron microscopy and EBSD analysis, with the dependence of ultimate tensile strength on the grain size in the synthesized intermetallide having been investigated at room temperature and at temperatures up to 1000°C. It is shown that an increase in the pressure preliminarily applied to the initial mixture compact results in reduced grain size of the final intermetallide, whereas an increase in pre-compaction time makes the grain size increased. A decrease in the grain size increases the ultimate tensile strength of the intermetallide. The maximum value of the ultimate tensile strength in the observed anomalous temperature dependence of this strength exhibits a shift by 200°C toward higher temperatures, and the ultimate strength of the synthesized intermetallide at 1000°C increases roughly two-fold.

  1. Synthesis, structural, thermal and optical properties of TeO2-Bi2O3-GeO2-Li2O glasses

    Science.gov (United States)

    Dimowa, Louiza; Piroeva, Iskra; Atanasova-Vladimirova, S.; Petrova, Nadia; Ganev, Valentin; Titorenkova, Rositsa; Yankov, Georgi; Petrov, Todor; Shivachev, Boris L.

    2016-10-01

    In this study, synthesis and characterization of novel quaternary tellurite glass system TeO2-Bi2O3-GeO2-Li2O is presented. The compositions include TeO2 and GeO2 as glass formers while different proportion of Bi2O3 and Li2O act as network modifiers. Differential thermal analysis, X-ray diffraction, scanning electron microscopy energy dispersive X-ray spectroscopy, laser ablation inductively coupled plasma mass spectrometry, UV-Vis and Raman spectroscopy are applied to study the structural, thermal and optical properties of the studied glasses. Obtained glasses possess a relatively low glass transition temperature (around 300 °C) if compared to other tellurite glasses, show good thermal transparency in the visible and near infra-red (from 2.4 to 0.4 μm) and can double the frequency of laser light from its original wavelength of 1064 nm to its second-harmonic at 532 nm (i.e. second harmonic generation).

  2. Two coordination polymers based on semicarbazone Schiff base and azide: synthesis, crystal structure, electrochemistry, magnetic properties and biological activity

    Czech Academy of Sciences Publication Activity Database

    Shaabani, B.; Khandar, A.A.; Dušek, Michal; Pojarová, Michaela; Mahmoudi, F.; Feher, A.; Kajňaková, M.

    2013-01-01

    Roč. 66, č. 5 (2013), s. 748-762 ISSN 0095-8972 Grant - others:AV ČR(CZ) AP0701 Program:Akademická prémie - Praemium Academiae Institutional support: RVO:68378271 Keywords : Schiff bases * semicarbazone * coordination polymer * structure analyses Subject RIV: CB - Analytical Chemistry, Separation Impact factor: 2.224, year: 2013

  3. Composites prepared from the waterborne polyurethane cationomers-modified graphene. Part I. Synthesis, structure, and physicochemical properties

    Czech Academy of Sciences Publication Activity Database

    Król, P.; Król, B.; Pielichowska, K.; Špírková, Milena

    2015-01-01

    Roč. 293, č. 2 (2015), s. 421-431 ISSN 0303-402X R&D Projects: GA ČR(CZ) GA13-06700S Institutional support: RVO:61389013 Keywords : polyurethane films * surface structure * AFM microscopy Subject RIV: CD - Macromolecular Chemistry Impact factor: 1.890, year: 2015

  4. Synthesis, structure and properties of heavily Mn-doped perovskite-type SrTiO.sub.3./sub. nanoparticles

    Czech Academy of Sciences Publication Activity Database

    Trepakov, Vladimír; Makarova, Marina; Stupakov, Oleksandr; Tereshina, Evgeniya; Drahokoupil, Jan; Čerňanský, Marian; Potůček, Zdeněk; Borodavka, Fedir; Valvoda, V.; Lynnyková, Anna; Jäger, Aleš; Jastrabík, Lubomír; Dejneka, Alexandr

    2014-01-01

    Roč. 143, č. 2 (2014), s. 570-577 ISSN 0254-0584 R&D Projects: GA TA ČR TA01010517; GA ČR GAP108/12/1941; GA ČR GBP108/12/G043; GA MŠk(CZ) LM2011026 Institutional support: RVO:68378271 Keywords : nanostructures * oxides * ferroelectricity * magnetic properties Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 2.259, year: 2014 http://www.sciencedirect.com/science/article/pii/S0254058413007141

  5. Synthesis, structural, optical and electrical properties of metal nanoparticle-rare earth ion dispersed in polymer film

    Science.gov (United States)

    Kumar, Brijesh; Kaur, Gagandeep; Singh, P.; Rai, S. B.

    2013-03-01

    Cu-nanoparticles have been prepared by ablating a copper target submerged in benzene with laser pulses of Nd:YAG (wavelength: 355, 532 nm and 1,064 nm). Colloidal nanoparticles have been characterized by UV-Vis spectroscopy and transmission electron microscopy. The obtained radius for the nanoparticles prepared using 1,064 nm irradiation lies in the range 15-30 nm, with absorption peak at 572 nm. Luminescence properties of Tb3+ ions in the presence and absence of Cu-nanoparticles have been investigated using 355 nm excitation. An enhancement in luminescence of Tb3+ by local field effect causing increase in lifetime of 5D4 level of Tb3+ ion has been observed. Frequency and temperature-dependent conductivity of Tb3+ doped PVA thin films with and without Cu-nanoparticles have been measured in the frequency range 20 Hz-1 MHz and in the temperature range 318-338 K (well below its melting temperature). Real part of the conductivity spectra has been explained in terms of power law. The electrical properties of the thin films show a decrease in dc conductivity on incorporation of the Cu-nanoparticles.

  6. Synthesis, crystal structures, spectral, thermal and antimicrobial properties of new Zn(II) 5-iodo- and 5-bromosalicylates

    Science.gov (United States)

    Košická, Petra; Győryová, Katarína; Smolko, Lukáš; Gyepes, Róbert; Hudecová, Daniela

    2018-03-01

    Two new analogous zinc(II) complexes containing 5-iodo- and 5-bromosalicylate ligands, respectively, were prepared in single-crystal form and characterized by IR spectroscopy, thermal analysis and elemental analysis. The solid-state structures of prepared complexes were determined by single crystal X-ray crystallography. Both complexes are isostructural and their crystal structures composed of neutral molecules [Zn(5-Xsal)2(H2O)2] (where X = Br, I, sal = salicylato). Central Zn(II) atom is in both complexes coordinated by six oxygen atoms, four of which are from two chelate bonded 5-halosalicylates and remaining two from coordinated water molecules. The found chelate binding mode is in line with the Δ values calculated from IR spectral data. Antimicrobial activity of prepared complexes was studied against selected bacteria, yeast and filamentous fungi. Obtained results indicate that 5-iodosalicylate complex is more antimicrobially active than its 5-bromo substituted analogue.

  7. Synthesis, structures and properties of the new lithium cobalt(II) phosphate Li4Co(PO4)2

    International Nuclear Information System (INIS)

    Glaum, R.; Gerber, K.; Schulz-Dobrick, M.; Herklotz, M.; Scheiba, F.; Ehrenberg, H.

    2012-01-01

    α-Li 4 Co(PO 4 ) 2 has been synthesized and crystallized by solid-state reactions. The new phosphate crystallizes in the monoclinic system (P2 1 /a, Z=4, a=8.117(3) Å, b=10.303(8) Å, c=8.118(8) Å, β=104.36(8) Å) and is isotypic to α-Li 4 Zn(PO 4 ) 2 . The structure of α-Li 4 Co(PO 4 ) 2 has been determined from single-crystal X-ray diffraction data {R 1 =0.040, wR 2 =0.135, 2278 unique reflections with F o >4σ(F o )}. The crystal structure, which might be regarded as a superstructure of the wurtzite structure type, is build of layers of regular CoO 4 , PO 4 and Li1O 4 tetrahedra. Lithium atoms Li2, Li3 and Li4 are located between these layers. Thermal investigations by in-situ XRPD, DTA/TG and quenching experiments suggest decomposition followed by formation and phase transformation of Li 4 Co(PO 4 ) 2 : α-Li 4 Co(PO 4 ) 2 ⟹ 442°C β-Li 3 PO 4 +LiCoPO 4 ⇌ 773°C β-Li 4 Co(PO 4 ) 2 ⟹ quenchingto25°C α-Li 4 Co(PO 4 ) 2 According to HT-XRPD at θ=850°Cβ-Li 4 Co(PO 4 ) 2 (Pnma, Z=2, 10.3341(8) Å, b=6.5829(5) Å, c=5.0428(3) Å) is isostructural to γ-Li 3 PO 4 . The powder reflectance spectrum of α-Li 4 Co(PO 4 ) 2 shows the typical absorption bands for the tetrahedral chromophore [Co II O 4 ]. - Graphical abstract: The complex formation and decomposition behavior of Li 4 Co(PO 4 ) 2 with temperature has been elucidated. The crystal structure of its α-phase was determined from single crystal data, HT-XRPD allowed derivation of a structure model for the β-phase. Both modifications belong to the Li 3 PO 4 structure family. Highlights: ► Li 4 Co(PO 4 ) 2 exhibits complex thermal behavior. ► The new phosphate belongs to the Li 3 PO 4 structure family. ► A single-crystal structure analysis is provided for the metastable α-Li 4 Co(PO 4 ) 2 . ► From HT-XRPD data a cation distribution model is developed for β-Li 4 Co(PO 4 ) 2 . ► No electrochemical delithiation is observed up to 5 V.

  8. Two Organic Cation Salts Containing Tetra(isothiocyanatecobaltate(II: Synthesis, Crystal Structures, Spectroscopic, Optical and Magnetic Properties

    Directory of Open Access Journals (Sweden)

    Zheng Zhang

    2017-03-01

    Full Text Available Single crystals of two hybrid organic-inorganic molecular solids, benzyl pyridinium tetra(isothiocyanatecobalt ([BzPy]2[Co(NCS4] (1 and benzyl quinolinium tetra(isothiocyanatecobalt ([BzQl]2[Co(NCS4] (2, were grown using a slow evaporation growth technique at room temperature and their IR, UV-Vis, X-ray crystal structures, luminescence, and magnetism were reported. The crystal structural analysis revealed that two molecular solids crystallize in the monoclinic space group P21/c of 1 and P21/n of 2. The cations form a dimer through weak C–H···π/π···π interactions in 1 and 2, and the adjacent cation (containing N(6 atom in 2 forms a columnar structure through π···π weak interactions between the quinoline and benzene rings, while the anions in 1 form a layer structure via short S···Co interactions. The anions (A and cations (C are arranged alternatively into a column in the sequence of ···A–CC–A–CC–A··· for 1, while the two anions and cationic dimer in 2 form an alliance by the C–H···π, C–H···S and C–H···N hydrogen bonds. A weak S···π interaction was found in 1 and 2. The two molecular solids show a broad fluorescence emission around 400 nm in the solid state at room temperature, and weak antiferromagnetic coupling behavior when the temperature is lowered.

  9. Synthesis, structure and properties of oxo- and dioxochloride complexes of molybdenum(VI) and tungsten(VI) with 8-oxyquinoline

    International Nuclear Information System (INIS)

    Abramenko, V.L.; Sergienko, V.S.; Egorova, O.A.

    2005-01-01

    Complexes of oxo- and dioxochlorides of molybdenum(VI) and tungsten(VI) with 8-oxyquinoline of molecular and intracomplex type are synthesized and studied by the method of IR spectroscopy. The complexes have octahedral structure. It is proposed that 8-oxyquinoline in molecular complexes is coordinated by central atom through nitrogen atom of heterocycle, but in intracomplex compounds - through heterocyclic nitrogen atom and oxygen atom of deprotonated OH-group. Thermal stability of the complexes is studied [ru

  10. Synthesis, structure, spectral properties and theoretical studies of two half-sandwich titanium-complexes with adamantoxy ligands

    Czech Academy of Sciences Publication Activity Database

    Varga, Vojtěch; Mach, Karel; Pinkas, Jiří; Kubišta, Jiří; Szarka, K.; Gyepes, R.

    2017-01-01

    Roč. 1142, AUG 2017 (2017), s. 248-254 ISSN 0022-2860 R&D Projects: GA ČR(CZ) GAP207/12/2368; GA ČR(CZ) GA14-08531S Institutional support: RVO:61388955 Keywords : half-sandwich complex * ionic complex * solid-state structure Subject RIV: CF - Physical ; Theoretical Chemistry OBOR OECD: Inorganic and nuclear chemistry Impact factor: 1.753, year: 2016

  11. Effects of size reduction on the structure and magnetic properties of core-shell Ni3Si/silica nanoparticles prepared by electrochemical synthesis

    Czech Academy of Sciences Publication Activity Database

    Pigozzi, G.; Mukherji, D.; Elerman, Y.; Strunz, Pavel; Gilles, R.; Hoelzel, M.; Barbier, B.; Schmutz, P.

    2014-01-01

    Roč. 584, JAN (2014), s. 119-127 ISSN 0925-8388 Institutional support: RVO:61389005 Keywords : intermetallics * nanostructured materials * transition metal alloys and compounds * electrochemical synthesis * crystal structure * magnetic measurements Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 2.999, year: 2014

  12. Zinc(II) halide complexes with 2-methoxyaniline ligand: Synthesis, characterization, thermal analyses, crystal structure determination and luminescent properties

    Science.gov (United States)

    Amani, Vahid

    2018-03-01

    Three new mononuclear zinc(II) complexes, [Zn(2-MeO-C6H4NH2)2X2] (X is Cl in 1, Br in 2 and I in 3), were prepared from the reactions of ZnX2 with 2-methoxyaniline (2-MeO-C6H4NH2) ligand in methanol. Suitable crystals of these complexes were obtained for X-ray diffraction measurements by slow evaporation of methanol solution at room temperature. The three complexes were thoroughly characterized by thermogravimetric analysis, elemental analysis (CHNO), spectral methods (IR, UV-Vis, 13C{1H}NMR, 1H NMR and luminescence), and single crystal X-ray diffraction. The X-ray structural analysis indicated that in the structures of these complexes, the zinc(II) cation is four-coordinated in a distorted tetrahedral configuration by two N atoms from two 2-methoxyanyline ligands and two halide anions. Also, in these complexes intermolecular interactions, for example Nsbnd H⋯X hydrogen bonds (in 1-3), Csbnd H⋯X hydrogen bonds (in 3), Csbnd H⋯π interactions (in 1 and 2) and π⋯π interactions (in 3), are effective in the stabilization of the crystal structures. In addition, the luminescence spectra of all complexes in methanolic solution show that the intensity of their emission bands is stronger than that for free 2-methoxyaniline ligand.

  13. Synthesis, crystal structure, and properties of a perovskite-related bismuth phase, (NH43Bi2I9

    Directory of Open Access Journals (Sweden)

    Shijing Sun

    2016-03-01

    Full Text Available Organic-inorganic halide perovskites, especially methylammonium lead halide, have recently led to remarkable advances in photovoltaic devices. However, due to environmental and stability concerns around the use of lead, research into lead-free perovskite structures has been attracting increasing attention. In this study, a layered perovskite-like architecture, (NH43Bi2I9, is prepared from solution and the structure solved by single crystal X-ray diffraction. The band gap, which is estimated to be 2.04 eV using UV-visible spectroscopy, is lower than that of CH3NH3PbBr3. The energy-minimized structure obtained from first principles calculations is in excellent agreement with the X-ray results and establishes the locations of the hydrogen atoms. The calculations also point to a significant lone pair effect on the bismuth ion. Single crystal and powder conductivity measurements are performed to examine the potential application of (NH43Bi2I9 as an alternative to the lead containing perovskites.

  14. Synthesis and anion exchange properties of a Zn/Ni double hydroxide salt with a guarinoite structure

    Science.gov (United States)

    Delorme, F.; Seron, A.; Licheron, M.; Veron, E.; Giovannelli, F.; Beny, C.; Jean-Prost, V.; Martineau, D.

    2009-09-01

    In this study, the first route to synthesize a compound with the guarinoite structure (Zn,Co,Ni) 6(SO 4)(OH,Cl) 10·5H 2O is reported. Zn/Ni guarinoite is obtained from the reaction of NiSO 4·7H 2O with solid ZnO in aqueous solution. The resulting green Zn/Ni guarinoite ((Zn 3.52Ni 1.63)(SO 4) 1.33(OH 7.64)·4.67H 2O) was characterized by X-ray diffraction, infrared spectrometry, UV-Visible spectrometry and thermal analysis. It is shown that its structure is similar to the one described for the layered Zn sulfate hydroxide hydrate, i.e. brucite layers with {1}/{4} empty octahedra presenting tetrahedrally coordinated divalent atoms above and below the empty octahedra. Ni atoms are located in the octahedra and zinc atoms in tetrahedra and octahedra. In this structure the exchangeable anions are located at the apex of tetrahedra. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) observations show that the Zn/Ni guarinoite is composed of aggregates of hexagonal plates of several hundreds of nanometers. Due to its interest for industrial or environmental applications, the exchange of sulfate groups by carbonates has been investigated. Results show a limited exchange and a higher affinity of the Zn/Ni guarinoite for sulfates compared to carbonates.

  15. Mononuclear mercury(II) complexes containing bipyridine derivatives and thiocyanate ligands: Synthesis, characterization, crystal structure determination, and luminescent properties

    Science.gov (United States)

    Amani, Vahid; Alizadeh, Robabeh; Alavije, Hanieh Soleimani; Heydari, Samira Fadaei; Abafat, Marzieh

    2017-08-01

    A series of mercury(II) complexes, [Hg(Nsbnd N)(SCN)2] (Nsbnd N is 4,4‧-dimethyl-2,2‧-bipyridine in 1, 5,5‧-dimethyl-2,2‧-bipyridine in 2, 6,6‧-dimethyl-2,2‧-bipyridine in 3 and 6-methyl-2,2‧-bipyridine in 4), were prepared from the reactions of Hg(SCN)2 with mentioned ligands in methanol. Suitable crystals of these complexes were obtained for X-ray diffraction measurement by methanol diffusion into a DMSO solution. The four complexes were thoroughly characterized by spectral methods (IR, UV-Vis, 13C{1H}NMR, 1H NMR and luminescence), elemental analysis (CHNS) and single crystal X-ray diffraction. The X-ray structural analysis indicated that in the structures of these complexes, the mercury(II) cation is four-coordinated in a distorted tetrahedral configuration by two S atoms from two thiocyanate anions and two N atoms from one chelating 2,2‧-bipyridine derivative ligand. Also, in these complexes intermolecular interactions, for example Csbnd H⋯N hydrogen bonds (in 1-4), Csbnd H⋯S hydrogen bonds (in 1, 2 and 4), π … π interactions (in 2-4), Hg⋯N interactions (in 2) and S⋯S interactions (in 4), are effective in the stabilization of the crystal structures and the formation of the 3D supramolecular complexes. Furthermore, the luminescence spectra of the title complexes show that the intensity of their emission bands are stronger than the emission bands for the free bipyridine derivative ligands.

  16. Flux synthesis, modulated crystal structures, and physical properties of REMn0.5SeO (RE = La, Ce)

    International Nuclear Information System (INIS)

    Peschke, Simon; Johrendt, Dirk; Nitsche, Fabian

    2015-01-01

    The selenide oxides REMn 0.5 SeO (RE = La, Ce) were synthesized by heating RE 2 O 3 , RE, Mn, and Se in a NaI/KI flux at 800 C, and their modulated crystal structures determined by X-ray single crystal and powder diffraction {P 1 1 2/n(αβ1/2)0s, Z = 2, LaMn 0.5 SeO: a = 405.7(1), b = 405.7(1), c = 915.2(1) pm, γ = 90 , q = [1/10, -1/10, 1/2]; CeMn 0.5 SeO: a = 402.0(1), b = 401.8(1), c = 910.7(1) pm, γ = 90.000(4) , q = [0.0789(2), -0.0783(2), 1/2]}. The structures are related to the ZrCuSiAs-type structure with ordered vacancies at the manganese sites. The resulting modulations of the checkerboard pattern in the [Mn 0.5 Se] layers can be approximated by 10a x 10b x 2c and 51a x 51b x 2c supercells in LaMn 0.5 SeO and CeMn 0.5 SeO, respectively. Both compounds are insulators. The optical bandgap of LaMn 0.5 SeO was determined to 2.13 eV from the Kubelka-Munk function. Magnetic measurements indicate antiferromagnetic ordering of the Mn 2+ moments with Neel points well above room temperature, as known from related manganese compounds. (Copyright copyright 2015 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  17. Synthesis and anion exchange properties of a Zn/Ni double hydroxide salt with a guarinoite structure

    International Nuclear Information System (INIS)

    Delorme, F.; Seron, A.; Licheron, M.; Veron, E.; Giovannelli, F.; Beny, C.; Jean-Prost, V.; Martineau, D.

    2009-01-01

    In this study, the first route to synthesize a compound with the guarinoite structure (Zn,Co,Ni) 6 (SO 4 )(OH,Cl) 10 .5H 2 O is reported. Zn/Ni guarinoite is obtained from the reaction of NiSO 4 .7H 2 O with solid ZnO in aqueous solution. The resulting green Zn/Ni guarinoite ((Zn 3.52 Ni 1.63 )(SO 4 ) 1.33 (OH 7.64 ).4.67H 2 O) was characterized by X-ray diffraction, infrared spectrometry, UV-Visible spectrometry and thermal analysis. It is shown that its structure is similar to the one described for the layered Zn sulfate hydroxide hydrate, i.e. brucite layers with 1/4 empty octahedra presenting tetrahedrally coordinated divalent atoms above and below the empty octahedra. Ni atoms are located in the octahedra and zinc atoms in tetrahedra and octahedra. In this structure the exchangeable anions are located at the apex of tetrahedra. Scanning electron microscopy (SEM) and transmission electron microscopy (TEM) observations show that the Zn/Ni guarinoite is composed of aggregates of hexagonal plates of several hundreds of nanometers. Due to its interest for industrial or environmental applications, the exchange of sulfate groups by carbonates has been investigated. Results show a limited exchange and a higher affinity of the Zn/Ni guarinoite for sulfates compared to carbonates. - Graphical abstract: SEM micrograph (secondary electrons) of the synthesized Zn/Ni guarinoite showing that aggregates are composed of small plate-like particles.

  18. Synthesis, Crystal Structures and Properties of Ferrocenyl Bis-Amide Derivatives Yielded via the Ugi Four-Component Reaction.

    Science.gov (United States)

    Zhao, Mei; Shao, Guang-Kui; Huang, Dan-Dan; Lv, Xue-Xin; Guo, Dian-Shun

    2017-05-04

    Ten ferrocenyl bis-amide derivatives were successfully synthesized via the Ugi four-component reaction by treating ferrocenecarboxylic acid with diverse aldehydes, amines, and isocyanides in methanol solution. Their chemical structures were fully characterized by IR, NMR, HR-MS, and X-ray diffraction analyses. They feature unique molecular morphologies and create a 14-membered ring motif in the centro-symmetric dimers generated in the solid state. Moreover, the electrochemical behavior of these ferrocenyl bis-amides was assessed by cyclic voltammetry.

  19. Solvent induced synthesis, structure and properties of coordination polymers based on 5-hydroxyisophthalic acid as linker and 1,10-phenanthroline as auxiliary ligand

    International Nuclear Information System (INIS)

    Kariem, Mukaddus; Yawer, Mohd; Sheikh, Haq Nawaz

    2015-01-01

    Three new coordination polymers [Mn(hip)(phen) (H_2O)]_n (1), [Co(hip)(phen) (H_2O)]_n (2), and [Cd(hip) (phen) (H_2O)]_n (3) (H_2hip=5-hydroxyisophthalic acid; phen=1,10-phenanthroline) have been synthesized by solvo-hydrothermal method using diethyl formamide-water (DEF-H_2O) as solvent system. Single-crystal X-ray diffraction analysis reveals that all three coordination polymers 1, 2 and 3 crystallize in monoclinic space group P2/n. Metal ions are inter-connected by hydroxyisophthalate anions forming zig-zag 1D chain. 1D chains are further inter-connected by hydrogen bonding and π–π stacking interactions leading to 3D supramolecular architecture. Hydrogen-bonding and π–π stacking provide thermal stability to polymers. Compounds 1 and 2 are paramagnetic at room temperature and variable temperature magnetic moment measurements revealed weak ferromagnetic interactions between metal ions at low temperature. Compound 3 exhibits excellent photoluminescence with large Stokes shift. - Graphical abstract: 1D helical chains of coordination polymers were synthesized by solvo-hydrothermal reaction of 5-hydroxyisopthalic acid and 1,10-phenanthroline with MnCl_2·4H_2O / CoCl_2·6H_2O / Cd(NO_3)_2·6H_2O. - Highlights: • Solvent induced synthesis of three coordination polymers with 1D zig-zag structure. • Crystal structures of coordination polymers are reported and discussed. • 1,10-Phenanthroline influences magnetic and luminescent properties of polymers. • Coordination polymer of Cd is luminescent exhibiting large Stokes shift.

  20. Solvent induced synthesis, structure and properties of coordination polymers based on 5-hydroxyisophthalic acid as linker and 1,10-phenanthroline as auxiliary ligand

    Energy Technology Data Exchange (ETDEWEB)

    Kariem, Mukaddus; Yawer, Mohd; Sheikh, Haq Nawaz, E-mail: hnsheikh@rediffmail.com

    2015-11-15

    Three new coordination polymers [Mn(hip)(phen) (H{sub 2}O)]{sub n} (1), [Co(hip)(phen) (H{sub 2}O)]{sub n} (2), and [Cd(hip) (phen) (H{sub 2}O)]{sub n} (3) (H{sub 2}hip=5-hydroxyisophthalic acid; phen=1,10-phenanthroline) have been synthesized by solvo-hydrothermal method using diethyl formamide-water (DEF-H{sub 2}O) as solvent system. Single-crystal X-ray diffraction analysis reveals that all three coordination polymers 1, 2 and 3 crystallize in monoclinic space group P2/n. Metal ions are inter-connected by hydroxyisophthalate anions forming zig-zag 1D chain. 1D chains are further inter-connected by hydrogen bonding and π–π stacking interactions leading to 3D supramolecular architecture. Hydrogen-bonding and π–π stacking provide thermal stability to polymers. Compounds 1 and 2 are paramagnetic at room temperature and variable temperature magnetic moment measurements revealed weak ferromagnetic interactions between metal ions at low temperature. Compound 3 exhibits excellent photoluminescence with large Stokes shift. - Graphical abstract: 1D helical chains of coordination polymers were synthesized by solvo-hydrothermal reaction of 5-hydroxyisopthalic acid and 1,10-phenanthroline with MnCl{sub 2}·4H{sub 2}O / CoCl{sub 2}·6H{sub 2}O / Cd(NO{sub 3}){sub 2}·6H{sub 2}O. - Highlights: • Solvent induced synthesis of three coordination polymers with 1D zig-zag structure. • Crystal structures of coordination polymers are reported and discussed. • 1,10-Phenanthroline influences magnetic and luminescent properties of polymers. • Coordination polymer of Cd is luminescent exhibiting large Stokes shift.

  1. Temperature effects during Ostwald ripening on structural and bandgap properties of TiO2 nanoparticles prepared by sonochemical synthesis

    International Nuclear Information System (INIS)

    Gonzalez-Reyes, L.; Hernandez-Perez, I.; Diaz-Barriga Arceo, L.; Dorantes-Rosales, H.; Arce-Estrada, E.; Suarez-Parra, R.; Cruz-Rivera, J.J.

    2010-01-01

    Anatase TiO 2 nanocrystalline (6 nm) with BET specific surface area of 300 m 2 /g and direct bandgap of 3.31 eV were prepared sonochemically and then it was subjected to thermal treatment from 400 to 900 deg. C for 2 h, in order to produce variable anatase-rutile ratio. Three stages were considered in the samples thermally treated: (i) anatase grains coarsening as a result of heat treatment temperature increasing the structural homogeneity and crystallinity and both phenomena produce a reduction in the specific surface area, (ii) coexistence of two phases (anatase and rutile) separated by a transition region, called an interface, and (iii) process where the rutile grains evolve into a new equilibrium shape without the presence of anatase phase, minimizing the total surface and the grain boundary energies, by mass transport diffusion. In this last stage the rutile phase has the sole function of growth and densification. The structure evolution, morphology and microstructure characteristics were obtained by X-ray diffraction (XRD) and transmission electron microscopy (TEM). All the stages of phase transformation are subject to thermal effects that stem from the redistribution of energy in the system. The UV-vis absorption spectra show that direct and indirect transitions can take place in the same sample simultaneously. This is attributed to the combined effect of samples with variable anatase-rutile ratio and particle size effect.

  2. Hybrid compounds of Keggin polyoxotungstate with transition metal ion as the central atom. Synthesis, structure and properties

    Science.gov (United States)

    Li, Xiao-Min; Chen, Ya-Guang; Shi, Tian

    2016-02-01

    The compounds (Hbipy)2[Co(bipy)2(H2O)4]2(CoW12O40)·2bipy·7H2O (1) and [Ni2(Hbipy)2(bipy)(H2O)4(H2W12O40)]·5H2O (2) (bipy = 4,4-bipyridine) were synthesized hydrothermally and characterized by elemental analysis, IR spectroscopy, TG analyses, solid ultraviolet diffuse spectroscopy and single crystal X-ray diffraction method. In 1 the complex ions, [Co(bipy)2(H2O)4]2+, construct a supramolecular layer through π-π stacking interaction. The heteropolyanions with central Co atom and supramolecular layers are linked by hydrogen bonds. In 2 a 2D structure is formed from metatungstate anions and binuclear Ni-bipy complexes through the coordination of metatungstate anions and bipy to Ni ions. Between the layers and bipyridine molecules are the hydrogen bond interactions. The formation of 1 and 2 shows that the solution acidity and metal ions influence greatly the structure of the compounds. Solid ultraviolet diffusion results indicate that the compounds 1 and 2 are potential semiconductor materials. In 1 and 2 there exists a weak antiferromagnetic interaction.

  3. Synthesis, physical properties and band structure of non-magnetic Y{sub 3}AlC

    Energy Technology Data Exchange (ETDEWEB)

    Ghule, S.S. [Bharati Vidyapeeth Deemed University College of Engineering, Pune-Satara Road, Pune 411043 (India); Garde, C.S., E-mail: gardecs@gmail.com [Vishwakarma Institute of Information Technology, S. no. 2/3/4, Kondhwa(Bk), Pune 411048 (India); Ramakrishnan, S. [Tata Institute of Fundamental Research, Navynagar, Mumbai 400005 (India); Singh, S. [Indian Institute of Science Education and Research, Dr Homi Bhabha Road, Pashan, Pune 411008 (India); Rajarajan, A.K. [Bhabha Atomic Research Centre, Trombay, Mumbai 400085 (India); Laad, Meena [Symbiosis Institute of Technology (SIT), Symbiosis International University (SIU), Lavale, Pune 412115 (India)

    2016-10-01

    Y{sub 3}AlC has been synthesized by arc melting and subsequent annealing. Rietveld analysis of the powder x-ray diffraction (XRD) data confirms cubic Pm-3m structure. Electrical resistivity (ρ) of Y{sub 3}AlC exhibits metallic behaviour. No sign of superconductivity is observed down to the lowest measurement temperatures of 4.2 K in ρ, and 2 K in magnetic susceptibility (χ) and specific heat (C{sub p}) measurements. The value of the electronic specific heat coefficient γ is 1.36 mJ/K{sup 2} mol from which the density of states (DOS) at the Fermi energy (E{sub F}) is obtained as 0.57 states/eV.unit cell. The value of Debye temperature θ{sub D} is estimated to be 315 K. Electronic band structure calculations of Y{sub 3}AlC reveal a pseudo-gap in the DOS at E{sub F} leading to a small value of 0.5 states/eV unit cell which matches quite well with that obtained from γ. Non-zero value of the DOS indicates metallic behaviour as confirmed by our ρ data. Covalent and ionic bonding seem to co-exist with metallic bonding in Y{sub 3}AlC as indicated by van Arkel- Ketelaar triangle for Zintl-like systems.

  4. Synthesis, Crystal Structure, Luminescence, Electrochemical and Antimicrobial Properties of Bis(salamo-Based Co(II Complex

    Directory of Open Access Journals (Sweden)

    Li Wang

    2017-09-01

    Full Text Available A newly designed Co(II complex, [Co3(L(OAc2(CH3OH2]·CH3OH, by the reaction of a bis(salamo-type tetraoxime ligand (H4L with Co(II acetate tetrahydrate was synthesized and characterized by elemental analyses, IR, UV-vis spectra and single-crystal X-ray crystallography. The UV-vis titration experiment manifested that a trinuclear (L:M = 1:3 complex was formed. It is worth noting that the two terminal Co(II (Co1 and Co3 atoms of the Co(II complex have different coordination modes and geometries unreported earlier. Furthermore, through intermolecular interactions (C–H···O, C–H···π and O–H···O, a 2D layer-like network is constructed. In addition, the fluorescence behaviors, antimicrobial activities and electrochemical properties of H4L and its Co(II complex were investigated.

  5. A pair of novel Cd(II) enantiomers based on lactate derivatives: Synthesis, crystal structures and properties

    International Nuclear Information System (INIS)

    Xu, Zhong-Xuan; Ao, Ke-Hou; Zhang, Jian

    2016-01-01

    A pair of novel 3D homochiral metal−organic frameworks (HMOFs), namely [Cd 2.5 ((R)-CIA) 6 (1,4-DIB)(H 2 O) 2 ]·((CH 3 ) 2 NH 2 )·H 2 O (1-D), [Cd 2.5 ((S)-CIA) 6 (1,4-DIB)(H 2 O) 2 ]·((CH 3 ) 2 NH 2 )·H 2 O (1-L), have been synthesized using lactic acid derivative ligands ((R)-H 3 CIA and (S)-H 3 CIA) and 1,4-DIB. Crystallographic analyses indicate that the complexes 1-D and 1-L are packed by cage substructures. Some physical characteristics, such as solid-state circular dichroism (CD), thermal stabilities and photoluminescent properties are also investigated. Our results highlight the effective method to apply lactic acid derivative ligands to form interesting HMOFs. - Graphical abstract: Using lactic acid derivative ligands ((R)-H 3 CIA and (S)-H 3 CIA) and 1,4-DIB to assemble with Cd 2+ ions, a pair of novel 3D homochiral metal-organic frameworks (HMOFs) with cage substructures have been synthesized. Display Omitted - Highlights: • Lactic acid derivative ligands • Cage substructure • Enantiomers

  6. A pair of novel Cd(II) enantiomers based on lactate derivatives: Synthesis, crystal structures and properties

    Energy Technology Data Exchange (ETDEWEB)

    Xu, Zhong-Xuan, E-mail: xuzhongxuan1974@163.com [Department of Chemistry, Zunyi Normal College, Zunyi, Guizhou 563002 (China); State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, the Chinese Academy of Sciences, Fuzhou, Fujian 350002 (China); Ao, Ke-Hou [Department of Chemistry, Zunyi Normal College, Zunyi, Guizhou 563002 (China); Zhang, Jian [State Key Laboratory of Structural Chemistry, Fujian Institute of Research on the Structure of Matter, the Chinese Academy of Sciences, Fuzhou, Fujian 350002 (China)

    2016-09-15

    A pair of novel 3D homochiral metal−organic frameworks (HMOFs), namely [Cd{sub 2.5}((R)-CIA){sub 6}(1,4-DIB)(H{sub 2}O){sub 2}]·((CH{sub 3}){sub 2}NH{sub 2})·H{sub 2}O (1-D), [Cd{sub 2.5}((S)-CIA){sub 6}(1,4-DIB)(H{sub 2}O){sub 2}]·((CH{sub 3}){sub 2}NH{sub 2})·H{sub 2}O (1-L), have been synthesized using lactic acid derivative ligands ((R)-H{sub 3}CIA and (S)-H{sub 3}CIA) and 1,4-DIB. Crystallographic analyses indicate that the complexes 1-D and 1-L are packed by cage substructures. Some physical characteristics, such as solid-state circular dichroism (CD), thermal stabilities and photoluminescent properties are also investigated. Our results highlight the effective method to apply lactic acid derivative ligands to form interesting HMOFs. - Graphical abstract: Using lactic acid derivative ligands ((R)-H{sub 3}CIA and (S)-H{sub 3}CIA) and 1,4-DIB to assemble with Cd{sup 2+} ions, a pair of novel 3D homochiral metal-organic frameworks (HMOFs) with cage substructures have been synthesized. Display Omitted - Highlights: • Lactic acid derivative ligands • Cage substructure • Enantiomers.

  7. Synthesis, crystal structure and photo physical properties of isomeric fluorinated s-shaped polyaromatic dibenzo[c,l]chrysene derivatives

    Science.gov (United States)

    Moriguchi, Tetsuji; Tabuchi, Daichi; Yakeya, Daisuke; Tsuge, Akihiko; Jalli, Venkataprasad; Yoza, Kenji

    2018-01-01

    Two s-shaped fluorinated isomeric polyaromatic dibenzo[c,l]chrysene derivatives have been synthesized by a two step process using the Wittig, Heck and iodine promoted cyclization reactions. These cyclized compounds were characterized by 1H NMR and EI-MS. Further, absolute configurations of isomeric 4a and 4b were determined by X-ray diffraction analysis. Compound 4a crystallized under monoclinic system with space group P21/c and compound 4b crystallized under monoclinic system with space group Cc. They have good solubility in common organic solvents such as dichloromethane, chloroform and THF. Photophysical properties of 4a and 4b were evaluated by using UV-Visible and Fluorescence spectrophotometer. Compounds 4a and 4b showed strong absorption maximum wavelength at 317 nm. The emission spectra of 4a and 4b displayed sharp peaks in the visible region from 417 to 441 nm. The shape of the UV-Visible and Fluorescence spectra of 4a and 4b looks almost identical. But compound 4a exhibited better fluorescence intensity than compound 4b. This difference may be due to the difference in the configuration of compounds 4a and 4b.

  8. Synthesis, crystal structure and properties of a new lead fluoride borate, Pb{sub 3}OBO{sub 3}F

    Energy Technology Data Exchange (ETDEWEB)

    Zhao, Wenwu [Xinjiang Key Laboratory of Electronic Information Materials and Devices, Xinjiang Technical Institute of Physics and Chemistry, Chinese Academy of Sciences, 40-1 South Beijing Road, Urumqi 830011 (China); Graduate School of the Chinese Academy of Sciences, Beijing 100049 (China); Pan, Shilie, E-mail: slpan@ms.xjb.ac.cn [Xinjiang Key Laboratory of Electronic Information Materials and Devices, Xinjiang Technical Institute of Physics and Chemistry, Chinese Academy of Sciences, 40-1 South Beijing Road, Urumqi 830011 (China); Dong, Xiaoyu [Xinjiang Key Laboratory of Electronic Information Materials and Devices, Xinjiang Technical Institute of Physics and Chemistry, Chinese Academy of Sciences, 40-1 South Beijing Road, Urumqi 830011 (China); Graduate School of the Chinese Academy of Sciences, Beijing 100049 (China); Li, Junjie; Tian, Xuelin; Fan, Xiaoyun [Xinjiang Key Laboratory of Electronic Information Materials and Devices, Xinjiang Technical Institute of Physics and Chemistry, Chinese Academy of Sciences, 40-1 South Beijing Road, Urumqi 830011 (China); Chen, Zhaohui [Xinjiang Key Laboratory of Electronic Information Materials and Devices, Xinjiang Technical Institute of Physics and Chemistry, Chinese Academy of Sciences, 40-1 South Beijing Road, Urumqi 830011 (China); Physical and Chemical Detecting Center, Xinjiang University, Urumqi 830046 (China); Zhang, Fangfang [Xinjiang Key Laboratory of Electronic Information Materials and Devices, Xinjiang Technical Institute of Physics and Chemistry, Chinese Academy of Sciences, 40-1 South Beijing Road, Urumqi 830011 (China)

    2012-04-15

    Graphical abstract: The structure of Pb{sub 3}OBO{sub 3}F consists of two distortional Pb-centered tetrahedra and BO{sub 3} triangles which are all symmetrical with each other respectively in the gestalt structure to the extent that the Pb{sub 3}OBO{sub 3}F compound crystallizes in the symmetrical space group. Highlights: Black-Right-Pointing-Pointer Pb{sub 3}OBO{sub 3}F has been grown from PbO-PbF{sub 2}-B{sub 2}O{sub 3} system for the first time. Black-Right-Pointing-Pointer It crystallizes in the orthorhombic system, space group Pbcm. Black-Right-Pointing-Pointer Pb{sub 3}OBO{sub 3}F consists of Pb(1)O{sub 3}F tetrahedra, Pb(2)O{sub 4} tetrahedra and BO{sub 3} triangles. -- Abstract: A new compound, Pb{sub 3}OBO{sub 3}F, has been grown by the high temperature solution method from the PbO-PbF{sub 2}-B{sub 2}O{sub 3} system. It crystallizes in the orthorhombic system, space group Pbcm with unit-cell parameters a = 7.6313(14) Angstrom-Sign , b = 6.5229(12) Angstrom-Sign , c = 11.906(2) Angstrom-Sign , Z = 4, volume = 592.66(19) Angstrom-Sign {sup 3}. The structure of the compound is solved by the direct methods and refined to R{sub 1} = 0.0528 and wR{sub 2} = 0.1400. Pb{sub 3}OBO{sub 3}F consists of Pb(1)O{sub 3}F tetrahedra, Pb(2)O{sub 4} tetrahedra and BO{sub 3} triangles which build up the symmetrical chains extended along the c-axis. The powder X-ray diffraction pattern of the Pb{sub 3}OBO{sub 3}F has been measured. Functional groups presented in the sample were identified by Fourier transform infrared spectrum.

  9. New in situ generated acylhydrazidate-coordinated complexes and acylhydrazide molecules: Synthesis, structural characterization and photoluminescence property

    Science.gov (United States)

    Wang, Yan-Ning; Huo, Qi-Sheng; Zhang, Ping; Yu, Jie-Hui; Xu, Ji-Qing

    2016-10-01

    By utilizing the hydrothermal in situ acylation of organic acids with N2H4, three acylhydrazidate-coordinated compounds [Mn(L1)2(H2O)2] (L1 = 2,3-quinolinedicarboxylhydrazidate; HL1 = 2,3-dihydropyridazino[4,5-b] quinoline-1,4-dione) 1, [Mn2(ox)(L2)2(H2O)6]·2H2O (L2 = benzimidazolate-5,6-dicarboxylhydrazide; HL2 = 6,7-dihydro-1H-imidazo[4,5-g]phthalazine-5,8-dione; ox = oxalate) 2, and [Cd(HL3)(bpy)] (L3 = 4,5-di(3‧-carboxylphenyl)phthalhydrazidate; H3L3 = 6,7-dihydro-1H-imidazo[4,5-g]phthalazine-5,8-dione; bpy = 2,2‧-bipyridine) 3, as well as two acylhydrazide molecules L4 (L4 = oxepino[2,3,4-de:7,6,5-d‧e‧]diphthalazine-4,10(5H,9H)-dione) 4 and L5 (L5 = 4,5-dibromophthalhydrazide; L5 = 6,7-dibromo-2,3-dihydrophthalazine-1,4-dione) 5 were obtained. X-ray single-crystal diffraction analysis reveals that (i) 1 only possesses a mononuclear structure, but it self-assembles into a 2-D supramolecular network via the Nhydrazinesbnd H ⋯ Nhydrazine and Owsbnd H ⋯ Ohydroxylimino interactions; (ii) 2 exhibits a dinuclear structure. Ox acts as the linker, while L2 just serves as a terminal ligand; (iii) In 3, L3 acts as a 3-connected node to propagate the 7-coordinated Cd2 + centers into a 1-D double-chain structure; (iv) 4 is a special acylhydrazide molecule. Two sbnd OH groups for the intermediates 3,3‧-biphthalhydrazide further lose one water molecule to form 4; (v) 5 is a common monoacylhydrazide molecule. Via the Nhydrazinesbnd H ⋯ Ohydrazine, Ohydroxyliminosbnd H ⋯ Oacylamino and the π ⋯ π interactions, it self-assembles into a 2-D supramolecular network. The photoluminescence analysis reveals that 4 emits light with the maxima at 510 nm.

  10. Plasma-assisted synthesis and study of structural and magnetic properties of Fe/C core shell

    Science.gov (United States)

    Shinde, K. P.; Ranot, M.; Choi, C. J.; Kim, H. S.; Chung, K. C.

    2017-07-01

    Pure and carbon-encapsulated iron nanoparticles with an average diameter of 25 nm were synthesized by using the DC plasma arc discharge method. Fe core nanoparticles were encapsulated with carbon layer, which is acting as protection layer against both oxidation and chemical reaction. The morphology and the Fe/C core/shell structure of the nanoparticles were studied by using field emission scanning electron microscopy and transmission electron microscopy. The x-ray diffraction study showed that the α-Fe phase exists with γ-Fe as an impurity. The studied samples have been interrelated with the variation of saturation magnetization, remanent magnetization and coercive field with the amount of carbon coating. The pure α-Fe sample shows saturation magnetization = 172 emu/g, and coercive field = 150 Oe, on the other hand few layer carbon coated α-Fe sample shows saturation magnetization =169 emu/g with higher coercive field 398 Oe.

  11. Synthesis, structural, magnetic and optical properties of Sr2CoSn based inverse Heusler alloy nanoparticles

    Science.gov (United States)

    Asvini, V.; Saravanan, G.; Kalaiezhily, R. K.; Ravichandran, K.

    2018-05-01

    The peculiar ternary full Heusler alloy Sr2CoSn nanoparticles are synthesized by co-precipitation method. X- ray diffraction pattern confirms the formation of XA or Xα structure of Sr2CoSn. Using Williamson-Hall plot (W-H plot), we are able to use the uniform deformation model and get low value of strain induced broadening. UV-Visible absorption spectrum shows sharp absorption peak at 210 nm and the estimated band gap energy of Sr2CoSn Heusler alloy nanoparticles is Eg = 4.6 eV (from Tauc plot). The presence of Sr2CoSn with the particle size of approximately 90 nm was observed using high resolution scanning electron microscopy. The magnetization measurements were carried out using VSM and studied M verses H hysteresis studies.

  12. Plasma-assisted synthesis and study of structural and magnetic properties of Fe/C core shell

    Directory of Open Access Journals (Sweden)

    K. P. Shinde

    2017-07-01

    Full Text Available Pure and carbon-encapsulated iron nanoparticles with an average diameter of 25 nm were synthesized by using the DC plasma arc discharge method. Fe core nanoparticles were encapsulated with carbon layer, which is acting as protection layer against both oxidation and chemical reaction. The morphology and the Fe/C core/shell structure of the nanoparticles were studied by using field emission scanning electron microscopy and transmission electron microscopy. The x-ray diffraction study showed that the α-Fe phase exists with γ-Fe as an impurity. The studied samples have been interrelated with the variation of saturation magnetization, remanent magnetization and coercive field with the amount of carbon coating. The pure α-Fe sample shows saturation magnetization = 172 emu/g, and coercive field = 150 Oe, on the other hand few layer carbon coated α-Fe sample shows saturation magnetization =169 emu/g with higher coercive field 398 Oe.

  13. Synthesis and electrochemical sodium and lithium insertion properties of sodium titanium oxide with the tunnel type structure

    Science.gov (United States)

    Kataoka, Kunimitsu; Akimoto, Junji

    2016-02-01

    Polycrystalline sample of sodium titanium oxide Na2Ti4O9 with the tunnel-type structure was prepared by topotactic sodium extraction in air atmosphere from the as prepared Na3Ti4O9 sample. The starting Na3Ti4O9 compound was synthesized by solid state reaction at 1273 K in Ar atmosphere. The completeness of oxidation reaction from Na3Ti4O9 to Na2Ti4O9 was monitored by the change in color from dark blue to white, and was also confirmed by the Rietveld refinement using the powder X-ray diffraction data. The sodium deficient Na2Ti4O9 maintained the original Na2.08Ti4O9-type tunnel structure and had the monoclinic crystal system, space group C2/m, and the lattice parameters of a = 23.1698(3) Å, b = 2.9406(1) Å, c = 10.6038(2) Å, β = 102.422(3)°, and V = 705.57(2) Å3. The electrochemical measurements of thus obtained Na2Ti4O9 sample showed the reversible sodium insertion and extraction reactions at 1.1 V, 1.5 V, and 1.8 V vs. Na/Na+, and reversible lithium insertion and extraction reactions at around 1.4 V, 1.8 V, and 2.0 V vs. Li/Li+. The reversible capacity for the lithium cell was achieved to be 104 mAh g-1 at the 100th cycle.

  14. Ultrasound assisted green synthesis of cerium oxide nanoparticles using Prosopis juliflora leaf extract and their structural, optical and antibacterial properties

    Directory of Open Access Journals (Sweden)

    Arunachalam Thirunavukkarasu

    2018-03-01

    Full Text Available Cerium oxide nanoparticles (CONPs were prepared using ultrasound assisted leaf extract of Prosopis juliflora acting as a reducing as well as stabilizing agent. The synthesized CONPs were characterized by ultraviolet-visible absorption spectroscopy (UV-Vis, particle size analyzer (PSA, Fourier transform infrared spectroscopy (FT-IR, Raman spectroscopy, X-ray diffraction (XRD, X-ray photoelectron spectroscopy (XPS and high-resolution transmission electron microscopy (HRTEM. From the UV-Vis analysis, the optical band gap of the prepared CONPs (Eg = 3.62 eV was slightly increased as compared to the bulk ceria (Eg = 3.19 eV. The phytochemicals in the extract reduced the particle size to 3.7 nm ± 0.3 nm, as it is evident from the PSA. FT-IR results confirmed the Ce-O stretching bands by showing the peaks at 452 cm-1. The Raman spectrumshowed a characteristic peak shift for CONPs at 461.2 cm-1. XRD analysis revealed the cubic fluorite structure of the synthesizednanoparticles with the lattice constant, a of 5.415 Å and unit cell volume, V of 158.813 Å3. XPS signals were used to determine the concentration of Ce3+ and Ce4+ in the prepared CONPs and it was found that major amount of cerium exist in the Ce4+ state. HRTEM images showed spherical shaped particles with an average size of 15 nm. Furthermore, the antibacterial activity of the prepared CONPs was evaluated and their efficacies were compared with the conventional antibiotics using disc diffusion assay against a set of Gram positive (G+ bacteria (Staphylococcus aureus, Streptococcus pneumonia and Gram negative (G- bacteria (Pseudomonas aeruginosa, Proteus vulgaris. The results suggested that CONPs showed antibacterial activity with significant variations due to the differences in the membrane structure and cell wall composition among the two groups tested.

  15. Synthesis, crystal structure and photophysical properties of (E)-4-(4-(2-hydroxybenzylideneamino)benzyl)oxazolidin-2-one

    International Nuclear Information System (INIS)

    Kumari, Rekha; Varghese, Anitha; George, Louis

    2016-01-01

    A new Schiff base, (4-(benzylideneamino)benzyl)oxazolidin-2-one has been synthesised from 4-(4-aminobenzyl)oxazolidin-2-one and salicylaldehyde by a simple condensation reaction. Single-crystal X-ray analysis of (E)-4-(4-(2-hydroxybenzylideneamino) benzyl)oxazolidin-2-one (HBOA) revealed that there is a 1-D, slipped, face-to-face motif with off-set, head-to-tail stacked columns. Detailed studies on photophysical properties of the synthesised compound in solutions indicate their potential applications in the field of organic light emitting devices and nonlinear optical materials. Absorption and fluorescence study of HBOA has been conducted in a series of solvents with increasing polarity at room temperature. Ground and excited state dipole moments have been determined experimentally by using Lippert–Mataga polarity function, Bakhshiev solvent polarity parameter, Kawskii–Chamma–Viallet solvent polarity parameter and RichardtГ—Віs microscopic solvent polarity parameter. Due to the considerable π-electron density redistribution, the excited state dipole moment was found to be larger than that of the ground state. The ground state dipole moment value was determined by quantum chemical method which was used to estimate excited state dipole moment through solvatochromic correlations. Kamlet–Taft and Catalan methods were used to get the information of both non-specific solute–solvent interactions and hydrogen bonding interactions. TD-DFT (B3LYP/6-311G(d,p)) has been used for the determination of HOMO–LUMO energies. Mulliken charges and Molecular electrostatic potential were also evaluated from DFT calculations.

  16. Synthesis and electrochemical properties of nanosized LiFeO2 particles with a layered rocksalt structure for lithium batteries

    International Nuclear Information System (INIS)

    Hirayama, Masaaki; Tomita, Hiroki; Kubota, Kei; Ido, Hidekazu; Kanno, Ryoji

    2012-01-01

    Highlights: ► 40-nm-sized O3-LiFeO 2 exhibits higher discharge capacities and rate characteristics than 400-nm-sized O3-LiFeO 2 . ► The cation disorder of Li and Fe ions might have affected the electrochemical activity of the O3-LiFeO 2 nanoparticles. ► A phase change from a layered structure to a cubic structure during electrochemical cycling. ► The new cubic phase allowed a stable electrochemical reaction between 4.5 and 1.0 V. -- Abstract: Layered rocksalt-type LiFeO 2 particles (O3-LiFeO 2 ) with average particle sizes of ca. 40 and 400 nm were synthesized by an ion exchange reaction from α-NaFeO 2 precursors. X-ray diffraction (XRD) patterns and scanning electron microscopy (SEM) images confirmed the formation of nanosized O3-LiFeO 2 . 40-nm LiFeO 2 exhibited a higher discharge capacity (115 mAh g −1 ) than 400-nm LiFeO 2 (80 mAh g −1 ), and also had better rate characteristics. The downsizing effect and cation disorder between the lithium and iron layers may have improved the electrochemical activity of the LiFeO 2 particles. Transmission electron microscopy (TEM) observation indicated a phase transition from O3-LiFeO 2 to a cubic lattice system during the electrochemical process. The cubic lithium iron oxide exhibited stable electrochemical reactions based on the Fe 2+ /Fe 3+ and Fe 2+ /Fe 0 redox couples at voltages between 4.5 and 1.0 V. The discharge capacities of 40-nm LiFeO 2 were ca. 115, 210, and 390 mAh g −1 under cutoff voltages of 4.5–2.0 V, 4.5–1.5 V, and 4.5–1.0 V, respectively.

  17. Self-assembly of novel manganese (II) compounds based on bifunctional-group ligands: Synthesis, structures, and magnetic properties

    Science.gov (United States)

    Yan, Juan-zhi; Lu, Li-ping; Zhu, Miao-li; Feng, Si-si

    2018-06-01

    Four manganese (II) compounds are obtained by the reaction of manganese salts, triazole-derivatives and auxiliary reagents in aqueous solution or mix-solvents by routine or hydrothermal reactions. X-ray crystal structure analyses reveal that a neutral 0D compound [Mn(Hmctrz)2(H2O)2] (1) (H2mctrz = 1H-1,2,4-triazole-3-carboxylic acid) displays a centro-symmetric mononuclear octahedral entity with two Hmctrz- anions and two water molecules; two neutral 2D clusters [Mn(Hdctrz)(H2O)2]n (2) (H3dctrz = 1H-1,2,4-triazole-3,5-dicarboxylic acid) and [Mn2(pbtrz)(btca)]n·4nH2O (3) (pbtrz = 1,3-bis(1,2,4-triazol-1-yl)-propane&H4btca = benzene-1,2,4,5-tetracarboxylic acid) possess layer structures with Hdctrz2- linkers (2) and Mn(II)-pbtrz-Mn(II) building blocks periodically extended by μ-btca4- connectors (3); [Mn(pbtrz)]n·nOAc·nOH (4) shows a 3D diamond-shaped cationic framework with the anion void volume of 49.2%. Nitrogenous bases are used as the auxiliary ligand in compound 3 and the temple ligand in compounds 1, 2, and 4. Compounds 1-4 show antiferromagnetic coupling that has been fitted by different models with the molecular field approximate with D = - 0.129(1) cm-1 for 1, J = - 0.354(4) cm-1 for 2 and J = - 0.696(6) cm-1 for 3, respectively. The magnetic differences can be related to different superexchange interactions transmitted by the crystal lattice and/or the zero field splitting (ZFS) of the 6A1g single-ion states of 1 and the syn-anti-COO- of 2 as well as the mixed magnetic bridges of μ1-O and μ-pbtrz-μ-COO- of 3.

  18. Synthesis, spectroscopic, thermal and structural properties of 4-(2-aminoethyl)pyridinium tetracyanometallate(II) complexes

    Science.gov (United States)

    Karaağaç, Dursun; Kürkçüoğlu, Güneş Süheyla; Şenyel, Mustafa; Şahin, Onur

    2017-05-01

    In this study, three new complexes (4aepyH)2[Ni(CN)4] (1), (4aepyH)2[Pd(CN)4] (2) and (4aepyH)2[Pt(CN)4] (3) [4aepy = 4-(2-aminoethyl)pyridine] have been synthesized and characterized by elemental, thermal, vibrational (FT-IR and Raman) and single-crystal X-ray diffraction techniques. The crystallographic analyses reveal that the complexes crystallize in the monoclinic system, space group C2/c. The asymmetric units of the complexes contain one M(II) ion, two cyanide ligands and one non-coordinated the 4aepy ligand. Each M(II) ion is four coordinated with four cyanide-carbon atoms in a square planar geometry and the [M(CN)4]2- anions act as a counter ion. The 4aepyH cations in the complexes compose of the protonation of the 4aepy. The vibrational spectral data also supported to the crystal structures of the complexes. Thermal stabilities and decomposition products of the complexes were investigated in the temperature range 40-700 °C in the static air atmosphere.

  19. Synthesis, Crystal Structures, and Photoluminescent Properties of Two Supramolecular Architectures Based on Difunctional Ligands Containing Imidazolyl and Carboxyl Groups

    Directory of Open Access Journals (Sweden)

    Mei-An Zhu

    2017-07-01

    Full Text Available Two new supramolecular architectures, namely, [Cd(L12(H2O]n (1 and [Ni(L22(H2O]n (2, were synthesized by the reaction of corresponding metal salts of CdCl2·2.5H2O and NiCl2·6H2O with 2-(1H-imidazol-4-ylbenzoic acid (HL1 and 3-(1H-imidazol-4-ylbenzoic acid (HL2 respectively, and characterized by single-crystal X-ray diffraction, IR spectroscopy, elemental analysis and powder X-ray diffraction (PXRD. Both HL1 and HL2 ligands are deprotonated to be L1- and L2- anions that coordinate with Cd(II and Ni(II atoms to form two-dimensional (2D layer structure. Topologically, complex 1 is a 2D network with (4, 4 sql topology, while 2 is a typical 63-hcb topology net. Complex 1 exhibits intense light blue emission in the solid state at room temperature.

  20. Hydrothermal synthesis, structure, heterogeneous catalytic activity and photoluminescent properties of a novel homoleptic Sm(III)-organic framework

    Energy Technology Data Exchange (ETDEWEB)

    Ay, Burak [Department of Chemistry, Arts and Science Faculty,Çukurova University, 01330 Adana (Turkey); Yildiz, Emel, E-mail: eeyildiz@cu.edu.tr [Department of Chemistry, Arts and Science Faculty,Çukurova University, 01330 Adana (Turkey); Felts, Ashley C.; Abboud, Khalil A. [Department of Chemistry, University of Florida, Gainesville, FL 32611 (United States)

    2016-12-15

    A novel metal-organic framework, (H{sub 2}pip){sub n}[Sm{sub 2}(pydc){sub 4}(H{sub 2}O){sub 2}]{sub n} (1) (H{sub 2}pydc=2,6-pyridinedicarboxylic acid, H{sub 2}pip=piperazine) has been synthesized under hydrothermal conditions and characterized by the elemental analysis, inductively coupled plasma (ICP) spectrometer, fourier transform infrared (FT-IR) spectra, thermogravimetric analysis (TGA), single crystal X-ray diffraction analysis and powder X-ray diffraction (PXRD). The structure of 1 was determined to be three-dimensional, linked along Sm-O-Sm chains. The asymmetric unit consisted of one singly anionic fragment consisting of Sm(III) coordinated to two H{sub 2}pydc ligands and one water, and one half of a protonated H{sub 2}pip, which sits on an inversion center. 1 exhibited luminescence emission bands at 534 nm at room temperature when excited at 440 nm. Its thermal behavior and catalytic performance were investigated and the selectivity was measured as 100% for the oxidation of thymol to thymoquinone. - Graphical abstract: A novel 3D lanthanide-organic framework has been synthesized under hydrothermal conditions. The thermal behavior and catalytic performance of 1 were investigated and its selectivity was measured as 100% for the oxidation of thymol to thymoquinone.

  1. Synthesis and evaluation structure/extracting and complexing properties of new bi-topic ligands for group actinides extraction

    International Nuclear Information System (INIS)

    Bisson, J.

    2011-01-01

    The aim of this project is to design and study new extractants for spent nuclear fuel reprocessing. To decrease the long-term radiotoxicity of the waste, the GANEX process is an option to homogeneously recycle actinides. All actinides (U, Np, Pu, Am, Cm) would be extracted together from a highly acidic media and separated from fission products (especially from lanthanides). In this context, fourteen new bi-topic ligands constituted of a nitrogen poly-aromatic unit from the dipyridyl-phenanthroline and dipyridyl-1,3,5-triazine families and functionalized by amid groups were synthesized. Extraction studies performed with some of these ligands confirmed their interest to selectively separate actinides at different oxidation states from an aqueous solution 3M HNO 3 . To determine the influence of ligands structure on cation complexation, a study in a homogenous media (MeOH/H 2 O) has been carried out. Electro-spray ionization mass spectrometry have been used to characterize the complexes stoichiometries formed with several cations (Eu 3+ , Nd 3+ , Am 3+ , Pu 4+ and NpO 2 + ). Stability constants, evaluated by UV-Visible spectrophotometry, confirm the selectivity of these ligands toward actinides. Lanthanides and actinides complexes have also been characterized in the solid state by infra-red spectroscopy and X-Ray diffraction. Associated to nuclear magnetic resonance experiments and DFT calculations (Density Functional Theory), a better knowledge of their coordination mode was achieved. (author) [fr

  2. Highly transparent ITO thin films on photosensitive glass: sol-gel synthesis, structure, morphology and optical properties

    Energy Technology Data Exchange (ETDEWEB)

    Koroesi, Laszlo; Papp, Szilvia; Dekany, Imre [University of Szeged, Supramolecular and Nanostructured Materials Research Group of the Hungarian Academy of Sciences, Szeged (Hungary); Beke, Szabolcs [Italian Institute of Technology, Department of Nanophysics, Genova (Italy); Pecz, Bela; Horvath, Robert; Petrik, Peter; Agocs, Emil [Research Institute for Technical Physics and Materials Science, Budapest (Hungary)

    2012-05-15

    Conductive and highly transparent indium tin oxide (ITO) thin films were prepared on photosensitive glass substrates by the combination of sol-gel and spin-coating techniques. First, the substrates were coated with amorphous Sn-doped indium hydroxide, and these amorphous films were then calcined at 550 {sup circle} C to produce crystalline and electrically conductive ITO layers. The resulting thin films were characterized by means of scanning electron microscopy, UV-Vis spectroscopy, X-ray photoelectron spectroscopy and spectroscopic ellipsometry. The measurements revealed that the ITO films were composed of spherical crystallites around 20 nm in size with mainly cubic crystal structure. The ITO films acted as antireflection coatings increasing the transparency of the coated substrates compared to that of the bare supports. The developed ITO films with a thickness of {proportional_to}170-330 nm were highly transparent in the visible spectrum with sheet resistances of 4.0-13.7 k{omega}/sq. By coating photosensitive glass with ITO films, our results open up new perspectives in micro- and nano-technology, for example in fabricating conductive and highly transparent 3D microreactors. (orig.)

  3. Hydrothermal Synthesis and Structural Characterization of NiO/SnO2 Composites and Hydrogen Sensing Properties

    Directory of Open Access Journals (Sweden)

    Chao Wei

    2015-01-01

    Full Text Available Pure SnO2 and NiO doped SnO2 nanostructures were successfully synthesized via a simple and environment-friendly hydrothermal method. X-ray powder diffraction (XRD, scanning electron microscopy (SEM, energy dispersive X-ray spectroscopy (EDS, and X-ray photoelectron spectra (XPS were used to investigate the crystalline structures, surface morphologies and microstructures, and element components and their valences of the as-synthesized samples. Furthermore, planar chemical gas sensors based on the synthesized pure SnO2 and NiO/SnO2 composites were fabricated and their sensing performances to hydrogen, an important fault characteristic gas dissolved in power transformer oil, were investigated in detail. Gas sensing experiments indicate that the NiO/SnO2 composites showed much higher gas response and lower working temperature than those of pure SnO2, which could be ascribed to the formation of p-n heterojunctions between p-type NiO and n-type SnO2. These results demonstrate that the as-synthesized NiO/SnO2 composites a promising hydrogen sensing material.

  4. Morphologically controlled synthesis, structural and optical properties of CeO2/SnO2 nanocomposites

    Directory of Open Access Journals (Sweden)

    S. Usharani

    2017-09-01

    Full Text Available CeO2/SnO2 nanocomposites with different dimensional nanostructures were synthesized by a wet chemical method, using various surfactants such as SDS, CTAB and Triton X-100. The prepared CeO2/SnO2 samples were analyzed by X-ray diffraction (XRD, Fourier transform infrared (FTIR, Transmission electron microscopy (TEM, UV-Diffuse Reflectance Spectroscopy (UV-DRS, and Photoluminescence (PL spectroscopy. The XRD patterns reveal the presence of a mixed phase of SnO2 and CeO2; The TEM analysis showed the mixed morphology of uniformly dispersed spherical with ellipsoidal shape in the SDS assisted CeO2/SnO2 nanocomposites; whereas the nanostructure with spherical with hexagonal shapes was observed for the Triton X-100 assisted CeO2/SnO2 nanocomposites. The one dimensional (1D nanorod like structure observed for the CTAB assisted CeO2/SnO2 nanocomposites shows CTAB acting as a face-specific capping agent to form rod-shaped micelles. The room temperature photoluminescence emission studies of the CeO2/SnO2 nanocomposites showed strong peaks in the UV region, and several peaks in the visible region, which are likely to have originated from the oxygen vacancies and are potential materials for optoelectronic device applications. The UV results showed the absorption edges shifted to a high energy region and the blue shifts that occurred in all the samples.

  5. Synthesis, structure, and thermal properties of soluble hydrazinium germanium(IV) and tin(IV) selenide salts.

    Science.gov (United States)

    Mitzi, David B

    2005-05-16

    The crystal structures of two hydrazinium-based germanium(IV) and tin(IV) selenide salts are determined. (N(2)H(5))(4)Ge(2)Se(6) (1) [I4(1)cd, a = 12.708(1) Angstroms, c = 21.955(2) Angstroms, Z = 8] and (N(2)H(4))(3)(N(2)H(5))(4)Sn(2)Se(6) (2) [P, a = 6.6475(6) Angstroms, b = 9.5474(9) Angstroms, c = 9.8830(10) Angstroms, alpha = 94.110(2) degrees, beta = 99.429(2) degrees, gamma = 104.141(2) degrees, Z = 1] each consist of anionic dimers of edge-sharing metal selenide tetrahedra, M(2)Se(6)(4-) (M = Ge or Sn), separated by hydrazinium cations and, for 2, additional neutral hydrazine molecules. Substantial hydrogen bonding exists among the hydrazine/hydrazinium molecules as well as between the hydrazinium cations and the selenide anions. Whereas the previously reported tin(IV) sulfide system, (N(2)H(5))(4)Sn(2)S(6), decomposes cleanly to microcrystalline SnS(2) when heated to 200 degrees C in an inert atmosphere, higher temperatures (>300 degrees C) are required to dissociate selenium from 1 and 2 for the analogous preparations of single-phase metal selenides. The metal chalcogenide salts are highly soluble in hydrazine, as well as in a variety of amines and DMSO, highlighting the potential usefulness of these compounds as precursors for the solution deposition of the corresponding metal chalcogenide films.

  6. Unexpected ferromagnetic interaction in a new tetranuclear copper(II) complex: synthesis, crystal structure, magnetic properties, and theoretical studies.

    Science.gov (United States)

    Fondo, Matilde; García-Deibe, Ana M; Corbella, Monstserrat; Ruiz, Eliseo; Tercero, Javier; Sanmartín, Jesús; Bermejo, Manuel R

    2005-07-11

    The new tetranuclear carbonate complex [Cu2L)2(CO3)] x 8H2O (1 x 8H2O) (H3L = (2-(2-hydroxyphenyl)-1,3-bis[4-(2-hydroxyphenyl)-3-azabut-3-enyl]-1,3-imidazolidine) has been obtained by two different synthetic routes and fully characterized. Recrystallization of 1 x 8H2O in methanol yields single crystals of {[(Cu2L)2(CO3)]}2 x 12H2O (1 x 6H2O), suitable for X-ray diffraction studies. The crystal structure of 1 x 6H2O shows two crystallographically different tetranuclear molecules in the asymmetric unit, 1a and 1b. Both molecules can be understood as self-assembled from two dinuclear [Cu2L]+ cations, joined by a mu4-eta(2):eta(1):eta(1) carbonate ligand. The copper atoms of each crystallographically different [(Cu2L)2(CO3)] molecule present miscellaneous coordination polyhedra: in both 1a and 1b, two metal centers are in square pyramidal environments, one displays a square planar chromophore and the other one has a geometry that can be considered as an intermediate between square pyramid and trigonal bipyramid. Magnetic studies reveal net intramolecular ferromagnetic coupling between the metal atoms. Density functional calculations allow the assignment of the different magnetic coupling constants and explain the unexpected ferromagnetic behavior, because of the presence of an unusual NCN bridging moiety and countercomplementarity of the phenoxo (or carbonate) and NCN bridges.

  7. Synthesis, structure, magnetic, electrical and electrochemical properties of Al, Cu and Mg doped MnO{sub 2}

    Energy Technology Data Exchange (ETDEWEB)

    Hashem, Ahmed M., E-mail: ahmedh242@yahoo.com [National Research Centre, Inorganic Chemistry Department, Behoes St., Dokki, Cairo (Egypt); Institute for Complex Materials, IFW Dresden, Helmholtzstr. 20, D-01069 Dresden (Germany); Abuzeid, Hanaa M. [National Research Centre, Inorganic Chemistry Department, Behoes St., Dokki, Cairo (Egypt); Narayanan, N. [Institute for Complex Materials, IFW Dresden, Helmholtzstr. 20, D-01069 Dresden (Germany); Ehrenberg, Helmut [Institute for Complex Materials, IFW Dresden, Helmholtzstr. 20, D-01069 Dresden (Germany); Materials Science, Technische Universitaet Darmstadt, Petersenstr. 23, D-64287 Darmstadt (Germany); Julien, C.M. [Universite Pierre et Marie Curie, Physicochimie des Electrolytes, Colloides et Sciences Analytiques (PECSA), 4 place Jussieu, 75005 Paris (France)

    2011-10-17

    Highlights: {yields} Al, Mg and Cu doped MnO{sub 2} as cathode in Li-ion batteries. {yields} Pure phase MnO{sub 2} for virgin and doped MnO{sub 2} were obtained. {yields} Doping elements improve the electrical conductivity of MnO{sub 2}. {yields} Electrochemical behaviour of MnO{sub 2} improved after doping by Al, Mg and Cu. - Abstract: Pure and doped manganese dioxides were prepared by wet-chemical method using fumaric acid and potassium permanganate as raw materials. X-ray diffraction patterns show that pure and Al, Cu and Mg doped manganese dioxides (d-MnO{sub 2}) crystallized in the cryptomelane-MnO{sub 2} structure. Thermal analysis show that, with the assistance of potassium ions inside the 2 x 2 tunnel, the presence of Al, Cu and Mg doping elements increases the thermal stability of d-MnO{sub 2}. The electrical conductivity of d-MnO{sub 2} increases in comparison with pure MnO{sub 2}, while Al-doped MnO{sub 2} exhibits the lower resistivity. As shown in the magnetic measurements, the value of the experimental effective magnetic moment of Mn ions decreases with introduction of dopants, which is attributed to the presence of a mixed valency of high-spin state Mn{sup 4+}/Mn{sup 3+}. Doped MnO{sub 2} materials show good capacity retention in comparison with virgin MnO{sub 2}. Al-doped MnO{sub 2} shows the best electrochemical results in terms of capacity retention and recharge efficiency.

  8. Synthesis, structure and magnetic properties of La{sub 3}Co{sub 2}SbO{sub 9}: A double perovskite with competing antiferromagnetic and ferromagnetic interactions

    Energy Technology Data Exchange (ETDEWEB)

    Franco, D.G.; Fuertes, V.C.; Blanco, M.C. [INFIQC (CONICET), Departamento de Fisicoquimica, Facultad de Ciencias Quimicas, Universidad Nacional de Cordoba, Ciudad Universitaria, X5000HUA Cordoba (Argentina); Fernandez-Diaz, M.T. [Institute Laue-Langevin (ILL) 156X, F-38042 Grenoble Cedex 9 (France); Sanchez, R.D., E-mail: rodo@cab.cnea.gov.ar [Centro Atomico Bariloche, CNEA and Instituto Balseiro, Universidad Nacional de Cuyo, Av. Bustillo 9500, 8400 Rio Negro (Argentina); Carbonio, R.E., E-mail: carbonio@fcq.unc.edu.ar [INFIQC (CONICET), Departamento de Fisicoquimica, Facultad de Ciencias Quimicas, Universidad Nacional de Cordoba, Ciudad Universitaria, X5000HUA Cordoba (Argentina)

    2012-10-15

    The synthesis, structural characterization, and magnetic properties of La{sub 3}Co{sub 2}SbO{sub 9} double perovskite are reported. The crystal structure has been refined by X-ray and neutron powder diffraction data in the monoclinic space group P2{sub 1}/n. Co{sup 2+} and Sb{sup 5+} have the maximum order allowed for the La{sub 3}Co{sub 2}SbO{sub 9} stoichiometry. Rietveld refinements of powder neutron diffraction data show that at room temperature the cell parameters are a=5.6274(2) A, b=5.6842(2) A, c=7.9748(2) A and {beta}=89.999(3) Degree-Sign . Magnetization measurements indicate the presence of ferromagnetic correlations with T{sub C}=55 K attributed to the exchange interactions for non-linear Co{sup 2+}-O-Sb{sup 5+}-O-Co{sup 2+} paths. The effective magnetic moment obtained experimentally is {mu}{sub exp}=4.38 {mu}{sub B} (per mol Co{sup 2+}), between the theoretical one for spin only (3.87 {mu}{sub B}) and spin-orbit value (6.63 {mu}{sub B}), indicating partially unquenched contribution. The low magnetization value at high magnetic field and low temperature (1 {mu}{sub B}/f.u., 5 T and 5 K) and the difference between ZFC and FC magnetization curves (at 5 kOe) indicate that the ferromagnetism do not reach a long range order and that the material has an important magnetic frustration. - Graphical abstract: Co-O-Co (Yellow octahedra only) rich zones (antiferromagnetic) are in contact with Co-O-Sb-O-Co (Red and yellow octahedra) rich zones (Ferromagnetic) to give the peculiar magnetic properties, as a consequence, a complex hysteresis loop can be observed composed by a main and irreversible curve in all the measured range, superimposed with a ferromagnetic component at low fields. Highlights: Black-Right-Pointing-Pointer La{sub 3}Co{sub 2}SbO{sub 9} has small Goldschmidt Tolerance Factor (t) due to the small size of La{sup 3+}. Black-Right-Pointing-Pointer Small t determines an angle for the path Co{sup 2+}-O-Sb{sup 5+}-O-Co{sup 2+} of 153 Degree-Sign . Black

  9. Synthesis, structure and magnetic properties of La3Co2SbO9: A double perovskite with competing antiferromagnetic and ferromagnetic interactions

    International Nuclear Information System (INIS)

    Franco, D.G.; Fuertes, V.C.; Blanco, M.C.; Fernández-Díaz, M.T.; Sánchez, R.D.; Carbonio, R.E.

    2012-01-01

    The synthesis, structural characterization, and magnetic properties of La 3 Co 2 SbO 9 double perovskite are reported. The crystal structure has been refined by X-ray and neutron powder diffraction data in the monoclinic space group P2 1 /n. Co 2+ and Sb 5+ have the maximum order allowed for the La 3 Co 2 SbO 9 stoichiometry. Rietveld refinements of powder neutron diffraction data show that at room temperature the cell parameters are a=5.6274(2) Å, b=5.6842(2) Å, c=7.9748(2) Å and β=89.999(3)°. Magnetization measurements indicate the presence of ferromagnetic correlations with T C =55 K attributed to the exchange interactions for non-linear Co 2+ –O–Sb 5+ –O–Co 2+ paths. The effective magnetic moment obtained experimentally is μ exp =4.38 μ B (per mol Co 2+ ), between the theoretical one for spin only (3.87 μ B ) and spin-orbit value (6.63 μ B ), indicating partially unquenched contribution. The low magnetization value at high magnetic field and low temperature (1 μ B /f.u., 5 T and 5 K) and the difference between ZFC and FC magnetization curves (at 5 kOe) indicate that the ferromagnetism do not reach a long range order and that the material has an important magnetic frustration. - Graphical abstract: Co–O–Co (Yellow octahedra only) rich zones (antiferromagnetic) are in contact with Co–O–Sb–O–Co (Red and yellow octahedra) rich zones (Ferromagnetic) to give the peculiar magnetic properties, as a consequence, a complex hysteresis loop can be observed composed by a main and irreversible curve in all the measured range, superimposed with a ferromagnetic component at low fields. Highlights: ► La 3 Co 2 SbO 9 has small Goldschmidt Tolerance Factor (t) due to the small size of La 3+ . ► Small t determines an angle for the path Co 2+ –O–Sb 5+ –O–Co 2+ of 153°. ► Ferromagnetism is attributed to exchange interactions for Co 2+ –O–Sb 5+ –O–Co 2+ paths. ► Ferromagnetic nanoclusters are embedded in an antiferromagnetic

  10. Synthesis, crystal structure and luminescent properties of lanthanide extended structure with asymmetrical dinuclear units based on 2-(methylthio)benzoic acid

    Energy Technology Data Exchange (ETDEWEB)

    Oliveira, Cristiane K.; Souza, Viviane P. de; Luz, Leonis L. da [Departamento de Química Fundamental, UFPE, 50.740-560 Recife, PE (Brazil); Menezes Vicenti, Juliano R. de [Escola de Química e Alimento, FURG, 96203-900 Rio Grande, RS (Brazil); Burrow, Robert A. [Departamento de Química, UFSM, 97105-900 Santa Maria, RS (Brazil); Severino Alves; Longo, Ricardo L. [Departamento de Química Fundamental, UFPE, 50.740-560 Recife, PE (Brazil); Malvestiti, Ivani, E-mail: ivani@ufpe.br [Departamento de Química Fundamental, UFPE, 50.740-560 Recife, PE (Brazil)

    2016-02-15

    The extended structures [Ln{sub 2}(L){sub 6}(OH{sub 2}){sub 4}] with L=2-(methylthio)benzoato (2-CH{sub 3}S–C{sub 6}H{sub 4}COO{sup −}) and Ln=Tb (1), Eu (2) and Gd (3) were successfully synthesized and characterized. The single crystal structure of compound 1 was determined and showed an extended structure made up of asymmetrical dinuclear units with the formula catena-poly[{Tb(H_2O)_4}-(μ-L-1κO:2κO'){sub 2}-{Tb(L-κO,O')_2}-(μ-L-1κO:2κO'){sub 2}]. In the molecule of 1, there are two distinct metal sites. The Tb atom in site 1 is bound to four coordinated water molecules and four oxygen atoms from four different benzoate ligands, two of which bridge to site 2 Tb atoms on one side and two to site 2 Tb atoms on the other side. The site 2 Tb atom is bound to four oxygen atoms from two chelating benzoate ligands and four oxygen atoms from four different benzoate ligands, two of which bridge to site 1 Tb atoms on one side and two to site 1 Tb atoms on the other side. The bridging benzoate ligands extend the framework in one-dimension with alternating site 1/site 2 Tb atoms. The luminescent properties of these asymmetric dinuclear extended structures are quite peculiar and showed a single emitting lanthanide center. The quantum yields of 1 (ca. 50–55%) is practically independent of the excitation energy, whereas those of 2 are vanishing small (<1%) when excited at the ligand states and become sizable (ca. 10–20%) upon excitation at the intra-4f manifold. To reconcile these experimental observations in conjunction with the spectral data for compounds 1 and 3, a strong interaction between the lanthanide emitting states at sites 1 and 2 was proposed. For compound 1, the numerical solutions of the rate equations provided evidences that when the transition rates between the emitting states at both sites are larger than the highest decaying rate of these states, the system becomes an effective single emitter. This establishes, for the first time

  11. Novel metal-organic and supramolecular 3D frameworks constructed from flexible biphenyl-2,5,3‧-tricarboxylate blocks: Synthesis, structural features and properties

    Science.gov (United States)

    You, Ao; Li, Yu; Zhang, Ze-Min; Zou, Xun-Zhong; Gu, Jin-Zhong; Kirillov, Alexander M.; Chen, Jin-Wei; Chen, Yun-Bo

    2017-10-01

    Biphenyl-2,5,3‧-tricarboxylic acid (H3L) was selected as an unexplored tricarboxylate building block and applied for the hydrothermal synthesis of three novel coordination compounds, namely a 0D tetramer [Co4(HL)2(μ3-HL)2(phen)6(H2O)2]·3H2O (1) and two 3D metal-organic frameworks (MOFs) [Cd3(μ5-L)(μ6-L)(py)(μ-H2O)2(H2O)]n·H2O (2) and [Zn3(μ4-L)2(2,2‧-bpy)(μ-4,4‧-bpy)]n·2H2O (3). These products were easily generated in aqueous medium from the corresponding metal(II) chlorides, H3L, and various N-donor ancillary ligands, selected from 1,10-phenanthroline (phen), pyridine (py), 2,2‧-bipyridine (2,2‧-bpy), and 4,4‧-bipyridine (4,4‧-bpy). Compounds 1-3 were isolated as stable crystalline solids and were fully characterized by IR and UV-vis spectroscopy, elemental, thermogravimetric (TGA), powder (PXRD) and single-crystal X-ray diffraction analyses. Compound 1 possesses a discrete tetracobalt(II) structure, which is extended into a 3D H-bonded network with the pcu topology. In contrast, MOF 2 discloses a very complex trinodal 4,5,12-connected net with an undocumented topology, while MOF 3 features the nce/I topological framework. The magnetic (for 1) and luminescence (for 2 and 3) properties were also studied and discussed. The present study thus widens a still very limited family of metal-organic and supramolecular frameworks driven by flexible biphenyl-2,5,3‧-tricarboxylate building blocks.

  12. Synthesis, microstructure, and physical properties of metallic barcode nanowires

    Science.gov (United States)

    Park, Bum Chul; Kim, Young Keun

    2017-05-01

    With rapid progress in nanotechnology, nanostructured materials have come closer to our life. Single-component nanowires are actively investigated because of their novel properties, attributed to their nanoscale dimensions and adjustable aspect ratio, but their technical limitations cannot be resolved easily. Heterostructured nanomaterials gained attention as alternatives because they can improve the existing single-component structure or add new functions to it. Among them, barcode nanowires (BNWs), comprising at least two different functional segments, can perform multiple functions for use in biomedical sensors, information encoding and security, and catalysts. BNW applications require reliable response to the external field. Hence, researchers have been attempting to improve the reliability of synthesis and regulate the properties precisely. This article highlights the recent progress and prospects for the synthesis, properties, and applications of metallic BNWs with focus on the dependence of the magnetic, optical, and mechanical properties on material, composition, shape, and microstructure.

  13. Synthesis and properties of nickel cobalt boron nanoparticles

    Science.gov (United States)

    Patel, J.; Pankhurst, Q. A.; Parkin, I. P.

    2005-01-01

    Amorphous cobalt nickel boride nanoparticles were synthesised by chemical reduction synthesis in aqueous solution. Careful control of synthesis conditions and post reaction oxidation enabled the nanoparticles to be converted into a core-shell structure comprising of an amorphous Co-Ni-B core and an outer metal oxide sheet. These particles had interesting magnetic properties including saturation magnetisations and coercivities of the order of 80 emu/g and 170 Oe respectively, making them suitable for a potential use as an exchange-pinned magnetic material.

  14. Dextran Nanoparticle Synthesis and Properties.

    Science.gov (United States)

    Wasiak, Iga; Kulikowska, Aleksandra; Janczewska, Magdalena; Michalak, Magdalena; Cymerman, Iwona A; Nagalski, Andrzej; Kallinger, Peter; Szymanski, Wladyslaw W; Ciach, Tomasz

    2016-01-01

    Dextran is widely exploited in medical products and as a component of drug-delivering nanoparticles (NPs). Here, we tested whether dextran can serve as the main substrate of NPs and form a stable backbone. We tested dextrans with several molecular masses under several synthesis conditions to optimize NP stability. The analysis of the obtained nanoparticles showed that dextran NPs that were synthesized from 70 kDa dextran with a 5% degree of oxidation of the polysaccharide chain and 50% substitution with dodecylamine formed a NP backbone composed of modified dextran subunits, the mean diameter of which in an aqueous environment was around 100 nm. Dextran NPs could be stored in a dry state and reassembled in water. Moreover, we found that different chemical moieties (e.g., drugs such as doxorubicin) can be attached to the dextran NPs via a pH-dependent bond that allows release of the drug with lowering pH. We conclude that dextran NPs are a promising nano drug carrier.

  15. 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.

  16. Synthesis, properties and reactivity of intramolecular hypercoordinate silicon complexes

    International Nuclear Information System (INIS)

    Nikolin, A A; Negrebetsky, V V

    2014-01-01

    The state of the art of the chemistry of hypercoordinate silicon compounds is analyzed. Published data on the current top-priority approaches to the preparative synthesis of these compounds and on their properties, structures and reactivity are summarized and generalized. Relying on the results obtained by modern physicochemical methods, the possible mechanisms of stereodynamic processes occurring in the coordination units of hypercoordinate silicon complexes are discussed. The bibliography includes 157 references

  17. A sodium gadolinium phosphate with two different types of tunnel structure: Synthesis, crystal structure, and optical properties of Na3GdP2O8

    International Nuclear Information System (INIS)

    Fang, M.; Cheng, W.-D.; Zhang, H.; Zhao, D.; Zhang, W.-L.; Yang, S.-L.

    2008-01-01

    A sodium gadolinium phosphate crystal, Na 3 GdP 2 O 8 , has been synthesized by a high-temperature solution reaction, and it exhibits a new structural family of the alkali-metal-rare-earth phosphate system. Although many compounds with formula M 3 LnP 2 O 8 have been reported, but they were shown to be orthorhombic [R. Salmon, C. Parent, M. Vlasse, G. LeFlem, Mater. Res. Bull. 13 (1978) 439] rather than monoclinic as shown in this paper. Single-crystal X-ray diffraction analysis shows the structure to be monoclinic with space group C2/c and the cell parameters: a=27.55 (25), b=5.312 (4), c=13.935(11) A, β=91.30(1) o , and V=2038.80 A 3 , Z=4. Its structure features a three-dimensional GdP 2 O 8 3- anionic framework with two different types of interesting tunnels at where Na atoms are located by different manners. The framework is constructed by Gd polyhedra and isolated PO 4 tetrahedra. It is different from the structure of K 3 NdP 2 O 8 [R. Salmon, C. Parent, M. Vlasse, G. LeFlem, Mater. Res. Bull. 13 (1978) 439] with space group P2 1 /m that shows only one type of tunnel. The emission spectrum and the absorption spectrum of the compound have been investigated. Additionally, the calculations of band structure, density of states, dielectric constants, and refractive indexes have been also performed with the density functional theory method. The obtained results tend to support the experimental data. - Graphical abstract: Projection of the structure of Na 3 GdP 2 O 8 with a unit cell edge along the b-axis. The Na-O bonds are omitted for clarity

  18. Synthesis and optical properties studies

    Directory of Open Access Journals (Sweden)

    N.A. El-Ghamaz

    2017-01-01

    Full Text Available 4-(4-Amino-1,5-dimethyl-2-phenyl-1,2-dihydro-pyrazol-3-ylideneamino-phenol (L1 and 4-(4-Amino-1,5-dimethyl-2-phenyl-1,2-dihydro-pyrazol-3-ylideneamino-benzoic acid (L2 have been synthesized by the condensation reaction of 4-aminoantipyrine (4-AAP and 4-aminophenol or 4-aminobenzoic acid in ethanolic solution and are characterized by various physico-chemical techniques. Thin films of L1 and L2 have been prepared by the conventional spin coating technique. X-ray diffraction patterns (XRD show an amorphous nature for both powder and thin films for L1 and L2 ligands. The optical absorption and refraction properties of L1 and L2 are investigated by spectrophotometric techniques at normal incidence of light in the wavelength range of 200–2500 nm. The absorption spectra show two peaks in the UV region which correspond to π → π∗ transition and a peak in UV–Vis region which may correspond to n → π∗ transition. The values of dispersion parameters Eo, Ed, εL, ε∞ and N/m* are calculated according to the single oscillator model. The presence of the OH group increases the value of ε∞ from 3.21 to 3.32 and the value of N/m* from 7.38 × 1053 to 2.08 × 1054 m−3Kg−1. The optical band transition is found to be indirect allowing fundamental energy gap values of 3.4 and 3.9 eV and onset energy gap values of 2.1 and 2.6 eV for L1 and L2, respectively.

  19. Synthesis, Crystal Structures, Magnetic Properties, and Theoretical Investigation of a New Series of NiII-LnIII-WV Heterotrimetallics: Understanding the SMM Behavior of Mixed Polynuclear Complexes.

    Science.gov (United States)

    Vieru, Veacheslav; Pasatoiu, Traian D; Ungur, Liviu; Suturina, Elizaveta; Madalan, Augustin M; Duhayon, Carine; Sutter, Jean-Pascal; Andruh, Marius; Chibotaru, Liviu F

    2016-12-05

    The polynuclear compounds containing anisotropic metal ions often exhibit efficient barriers for blocking of magnetization at fairly arbitrary geometries. However, at variance with mononuclear complexes, which usually become single-molecule magnets (SMM) under the sole requirement of a highly axial crystal field at the metal ion, the factors influencing the SMM behavior in polynuclear complexes, especially, with weakly axial magnetic ions, still remain largely unrevealed. As an attempt to clarify these conditions, we present here the synthesis, crystal structures, magnetic behavior, and ab initio calculations for a new series of Ni II -Ln III -W V trimetallics, [(CN) 7 W(CN)Ni(H 2 O)(valpn)Ln(H 2 O) 4 ]·H 2 O (Ln = Y 1, Eu 2, Gd 3, Tb 4, Dy 5, Lu 6). The surprising finding is the absence of the magnetic blockage even for compounds involving strongly anisotropic Dy III and Tb III metal ions. This is well explained by ab initio calculations showing relatively large transversal components of the g-tensor in the ground exchange Kramers doublets of 1 and 4 and large intrinsic tunneling gaps in the ground exchange doublets of 3 and 5. In order to get more insight into this behavior, another series of earlier reported compounds with the same trinuclear [W V Ni II Ln III ] core structure, [(CN) 7 W(CN)Ni(dmf)(valdmpn)Ln(dmf) 4 ]·H 2 O (Ln = Gd III 7, Tb III 8a, Dy III 9, Ho III 10), [(CN) 7 W(CN)Ni(H 2 O)(valdmpn)Tb(dmf) 2.5 (H 2 O) 1.5 ]·H 2 O·0.5dmf 8b, and [(CN) 7 W(CN)Ni(H 2 O)(valdmpn)Er(dmf) 3 (H 2 O) 1 ]·H 2 O·0.5dmf 11, has been also investigated theoretically. In this series, only 8b exhibits SMM behavior which is confirmed by the present ab initio calculations. An important feature for the entire series is the strong ferromagnetic coupling between Ni(II) and W(V), which is due to an almost perfect trigonal dodecahedron geometry of the octacyano wolframate fragment. The reason why only 8b is an SMM is explained by positive zero-field splitting on the nickel

  20. Synthesis and atomic scale characterization of Er2O3 nanoparticles: enhancement of magnetic properties and changes in the local structure

    Science.gov (United States)

    Corrêa, Eduardo L.; Bosch-Santos, Brianna; Freitas, Rafael S.; Potiens, Maria da Penha A.; Saiki, Mitiko; Carbonari, Artur W.

    2018-05-01

    In the investigation reported in this paper a modified thermal decomposition method was developed to produce very small Er2O3 nanoparticles (NPs). Particles structure, shape and size were characterized by x-ray diffraction and transmission electron microscopy which showed that the synthesis by thermal decomposition under O2 atmosphere produced very small and monodisperse NPs, allowing the investigation of finite-size and surface effects. Results of magnetization measurements showed that the smallest particles present the highest values of susceptibility that decrease as particle size increases. Specific heat measurements indicate that the sample with the smallest NPs (diameter ∼5 nm) has a Néel temperature of 0.54 K. The local structure of particles was investigated by measurements of hyperfine interactions with perturbed angular correlation spectroscopy using 111Cd as probe nuclei replacing the cationic sites. Results showed that the relative population of sites 8b increases in both the core and surface layer of particles.

  1. [Ag67(SPhMe2)32(PPh3)8]3+: Synthesis, Total Structure, and Optical Properties of a Large Box-Shaped Silver Nanocluster

    KAUST Repository

    Alhilaly, Mohammad J.; Bootharaju, Megalamane Siddaramappa; Joshi, Chakra Prasad; Besong, Tabot M.D.; Emwas, Abdul-Hamid M.; Juarez-Mosqueda, Rosalba; Kaappa, Sami; Malola, Sami; Adil, Karim; Shkurenko, Aleksander; Hakkinen, Hannu; Eddaoudi, Mohamed; Bakr, Osman

    2016-01-01

    Engineering the surface ligands of metal nanoparticles is critical in designing unique arrangements of metal atoms. Here, we report the synthesis and total structure determination of a large box-shaped Ag-67 nanocluster (NC) protected by a mixed shell of thiolate (2,4-dimethylbenzenethiolate, SPhMe2) and phosphine (triphenylphosphine, PPh3) ligands. Single crystal X-ray diffraction (SCXRD) and electrospray ionization mass spectrometry (ESI-MS) revealed the cluster formula to be [Ag-67(SPhMe2)(32)(PPh3)(8)](3+). The crystal structure shows an Ag-23 metal core covered by a layer of Ag44S32P8 arranged in the shape of a box. The Ag-13, core was formed through an unprecedented centered cuboctahedron, i.e., Ag-13, unlike the common centered Ag-13 icosahedron geometry. Two types of ligand motifs, eight AgS3P and eight bridging thiols, were found to stabilize the whole cluster. The optical spectrum of this NC displayed highly structured multiple absorption peaks. The electronic structure and optical spectrum of Ag-67 were computed using time-dependent density functional theory (TDDFT) for both the full cluster [Ag-67(SPhMe2)(32)(PPh3)(8)](3+) and a reduced model [Ag-67(SH)(32)(PH3)(8)](3+). The lowest metal-to-metal transitions in the range 500-800 nm could be explained by considering the reduced model that shows almost identical electronic states to 32 free electrons in a jellium box. The successful synthesis of the large box-shaped Ag-67 NC facilitated by the combined use of phosphine and thiol paves the way for synthesizing other metal clusters with unprecedented shapes by judicious choice of thiols and phosphines.

  2. [Ag67(SPhMe2)32(PPh3)8]3+: Synthesis, Total Structure, and Optical Properties of a Large Box-Shaped Silver Nanocluster

    KAUST Repository

    Alhilaly, Mohammad J.

    2016-10-13

    Engineering the surface ligands of metal nanoparticles is critical in designing unique arrangements of metal atoms. Here, we report the synthesis and total structure determination of a large box-shaped Ag-67 nanocluster (NC) protected by a mixed shell of thiolate (2,4-dimethylbenzenethiolate, SPhMe2) and phosphine (triphenylphosphine, PPh3) ligands. Single crystal X-ray diffraction (SCXRD) and electrospray ionization mass spectrometry (ESI-MS) revealed the cluster formula to be [Ag-67(SPhMe2)(32)(PPh3)(8)](3+). The crystal structure shows an Ag-23 metal core covered by a layer of Ag44S32P8 arranged in the shape of a box. The Ag-13, core was formed through an unprecedented centered cuboctahedron, i.e., Ag-13, unlike the common centered Ag-13 icosahedron geometry. Two types of ligand motifs, eight AgS3P and eight bridging thiols, were found to stabilize the whole cluster. The optical spectrum of this NC displayed highly structured multiple absorption peaks. The electronic structure and optical spectrum of Ag-67 were computed using time-dependent density functional theory (TDDFT) for both the full cluster [Ag-67(SPhMe2)(32)(PPh3)(8)](3+) and a reduced model [Ag-67(SH)(32)(PH3)(8)](3+). The lowest metal-to-metal transitions in the range 500-800 nm could be explained by considering the reduced model that shows almost identical electronic states to 32 free electrons in a jellium box. The successful synthesis of the large box-shaped Ag-67 NC facilitated by the combined use of phosphine and thiol paves the way for synthesizing other metal clusters with unprecedented shapes by judicious choice of thiols and phosphines.

  3. Antibacterial Barbituric Acid Analogues Inspired from Natural 3-Acyltetramic Acids; Synthesis, Tautomerism and Structure and Physicochemical Property-Antibacterial Activity Relationships

    Directory of Open Access Journals (Sweden)

    Yong-Chul Jeong

    2015-02-01

    Full Text Available The synthesis, tautomerism and antibacterial activity of novel barbiturates is reported. In particular, 3-acyl and 3-carboxamidobarbiturates exhibited antibacterial activity, against susceptible and some resistant Gram-positive strains of particular interest is that these systems possess amenable molecular weight, rotatable bonds and number of proton-donors/acceptors for drug design as well as less lipophilic character, with physicochemical properties and ionic states that are similar to current antibiotic agents for oral and injectable use. Unfortunately, the reduction of plasma protein affinity by the barbituric core is not sufficient to achieve activity in vivo. Further optimization to reduce plasma protein affinity and/or elevate antibiotic potency is therefore required, but we believe that these systems offer unusual opportunities for antibiotic drug discovery.

  4. Hidróxidos duplos lamelares: síntese, estrutura, propriedades e aplicações Layered double hydroxides: structure, synthesis, properties and applications

    Directory of Open Access Journals (Sweden)

    Eduardo Luis Crepaldi

    1998-06-01

    Full Text Available The layered double hydroxides, known as anionic clays and represented by the general formula [M2+1-x M3+x (OH 2]x+ Am-x/m·nH 2O, are a group of materials which are of much interest currently. They present a variety of potential applications as adsorbents, catalysts and catalyst support, ion-exchangers, antacids and as a polymer stabilizer. It is possible to obtain a broad variety of layered double hydroxides (LDHs, depending on the identity and ratio of the cations M2+ and M3+, as well as the interlamelar anion. The aim of this review is to give out some information about this class of materials, concerning to the synthesis, characterization, properties and applications.

  5. Synthesis and tribological properties of antimony N, N-diethanoldithiocarbamate

    Institute of Scientific and Technical Information of China (English)

    李丽; 黄可龙; 瞿龙; 舒万艮

    2001-01-01

    Antimony N, N-diethanoldithiocarbamate was synthesized with diethanolamine, antimony trioxide and carbon disulfide. The influences of temperature, reaction time, solvents and their dosages were investigated, and the optimum synthesis conditions were: reaction temperature 15~20 ℃, reaction time 2.5 h, 250 mL CH3OH as solvent and the hot CH3OH as recrystallization solvent. Element analysis, IR, 1HNMR and 13CNMR spectra were used to study its chemical composition and molecular structure. Antimony N, N-diethanol-dithiocarbamate was added in the base oil, and its properties of wear resistance and extreme pressure were studied by FB, FD and WSD. The synthesis product behaves per fectly as wear resistance and extreme pressure additive and its extreme pressure property is superior to its wear resistance property. The mechanism of tribological action was discussed by using XPS and AES spectra, and the reason of good wear resistance and extreme pressure properties is that the synthesis product decompose element C, S and N.

  6. SYNTHESIS, CRYSTAL STRUCTURE AND MAGNETIC ...

    African Journals Online (AJOL)

    Preferred Customer

    Much of the current effort on such extended hybrid metal organic complexes is ... In this paper, we report the synthesis, single crystal X-ray diffraction analysis and ..... with g = 2.0 (0.37 cm3 mol−1 K), and smoothly increases to a value of 0.45 ...

  7. Synthesis, crystal structure and electrical properties of the tetrahedral quaternary chalcogenides CuM{sub 2}InTe{sub 4} (M=Zn, Cd)

    Energy Technology Data Exchange (ETDEWEB)

    Nolas, George S., E-mail: gnolas@usf.edu [Department of Physics, University of South Florida, Tampa, FL 33620 (United States); Hassan, M. Shafiq; Dong, Yongkwan [Department of Physics, University of South Florida, Tampa, FL 33620 (United States); Martin, Joshua [Material Measurement Laboratory, National Institute of Standards and Technology (NIST), Gaithersburg, MD 20899 (United States)

    2016-10-15

    Quaternary chalcogenides form a large class of materials that continue to be of interest for energy-related applications. Certain compositions have recently been identified as possessing good thermoelectric properties however these materials typically have the kesterite structure type with limited variation in composition. In this study we report on the structural, optical and electrical properties of the quaternary chalcogenides CuZn{sub 2}InTe{sub 4} and CuCd{sub 2}InTe{sub 4} which crystallize in the modified zinc-blende crystal structure, and compare their properties with that of CuZn{sub 2}InSe{sub 4}. These p-type semiconductors have direct band gaps of about 1 eV resulting in relatively high Seebeck coefficient and resistivity values. This work expands on the research into quaternary chalcogenides with new compositions and structure types in order to further the fundamental investigation of multinary chalcogenides for potential thermoelectrics applications. - Graphical abstract: The structural, optical and electrical properties of the quaternary chalcogenides CuZn{sub 2}InTe{sub 4} and CuCd{sub 2}InTe{sub 4} are reported for the first time. The unique crystal structure allows for relatively good electrical transports and therefore potential for thermoelectric applications. - Highlights: • The physical properties of CuZn{sub 2}InTe{sub 4} and CuCd{sub 2}InTe{sub 4} are reported for the first time. • These materials have potential for thermoelectric applications. • Their direct band gaps also suggest potential for photovoltaics applications.

  8. Uranium hetero-bimetallic complexes: synthesis, structure and magnetic properties; Complexes heterobimetalliques de l'uranium: synthese, structure et proprietes magnetiques

    Energy Technology Data Exchange (ETDEWEB)

    Le Borgne, Th

    2000-10-04

    The aim of this thesis is to synthesize molecular complexes with uranium and transition metal ions in close proximity, to determine the nature of the magnetic interaction between them. We decided to use Schiff bases as assembling ligands, which are unusual for uranium (IV). Although the simplest Schiff bases, such as H{sub 2}Salen, lead to ligand exchange reactions, the bi-compartmental Schiff base H{sub 4}L{sup 6} (bis(3-hydroxy-salicylidene) - 2,2-dimethyl-propylene) allows the crystal structure determination of the complex [L{sup 6}Cu(pyr)]U[L{sup 6}Cu].2pyr, obtained by reaction of the metallo-ligand H{sub 2}L{sup 6}Cu with U(acac){sub 4}. In this manner, the complexes [L{sup 6}Co(pyr)]{sub 2}U and [L{sup 6}Ni(pyr)]{sub 2}U.pyr were also isolated, as well as the compounds in which the paramagnetic ions have been exchanged by the diamagnetic ions Zn{sup II}, Zr{sup IV} and Th{sup IV}': [L{sup 6}Zn(pyr)]{sub 2}U, [L{sup 6}Cu]{sub 2}Zr and [L{sup 6}Cu(pyr)]Th[L{sup 6}Cu].2pyr. These complexes are the first which involve three metallic centres assembling by the means of a hexa-dentate Schiff base. The crystalline structures show, for all these complexes, the outstanding orthogonal arrangement of the two fragments L{sup 6}M around the central atom which is in a dodecahedral environment of eight oxygen atoms of two Schiff bases. The syntheses of the isostructural complexes Cu2{sup II} and Zn{sub 2}U in which the uranium (IV) ion is close, in the first one, to the paramagnetic ion Cu{sup II} and, in the second one, to the diamagnetic ion Zn{sup II}, has allowed the use of the empiric method to determine the nature of the magnetic interaction between an f element and a transition metal. The comparison of the magnetic behaviour of two complexes Cu{sub 2}U and Zn{sub 2}U, expressed by the variation of {chi}T vs T, reveals the ferromagnetic interaction in the heart of the triad Cu-U-Cu. The magnetic behaviour of the complexes Cu{sub 2}Th et Cu{sub 2}Zr which does not

  9. Synthesis, microstructure and mechanical properties of ceria ...

    Indian Academy of Sciences (India)

    Unknown

    ceria stabilized zirconia powders with improved mechanical properties. Ce–ZrO2 with 20 wt% ... structural ceramic materials (Garvie et al 1975; Evans and. Cannon 1986) ... thermal expansion matching with that of iron alloys. (Tsukuma and ...

  10. 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-

  11. Barium hexaferrite nanoparticles: Synthesis and magnetic properties

    International Nuclear Information System (INIS)

    Martirosyan, K.S.; Galstyan, E.; Hossain, S.M.; Wang Yiju; Litvinov, D.

    2011-01-01

    Carbon combustion synthesis is applied to rapid and energy efficient fabrication of crystalline barium hexaferrite nanoparticles with the average particle size of 50-100 nm. In this method, the exothermic oxidation of carbon nanoparticles with an average size of 5 nm with a surface area of 80 m 2 /g generates a self-propagating thermal wave with maximum temperatures of up to 1000 deg. C. The thermal front rapidly propagates through the mixture of solid reactants converting it to the hexagonal barium ferrite. Carbon is not incorporated in the product and is emitted from the reaction zone as a gaseous CO 2 . The activation energy for carbon combustion synthesis of BaFe 12 O 19 was estimated to be 98 kJ/mol. A complete conversion to hexagonal barium ferrite is obtained for carbon concentration exceeding 11 wt.%. The magnetic properties H c ∼3000 Oe and M s ∼50.3 emu/g of the compact sintered ferrites compare well with those produced by other synthesis methods.

  12. Synthesis, structure, optical, photoluminescence and magnetic properties of K2[Co(C2O4)2(H2O)2]·4H2O

    Science.gov (United States)

    Narsimhulu, M.; Hussain, K. A.

    2018-06-01

    The synthesis, crystal structure, optical, photoluminescence and magnetic behaviour of potassium bis(oxalato)cobaltate(II)tertrahydrate{K2[Co(C2O4)2(H2O)2]·4H2O} are described. The compound was grown at room temperature from mixture of aqueous solutions by slow evaporation method. The X-ray crystallographic data showed that the compound belongs to the monoclinic crystal system with P21/n space group and Z = 4. The UV-visible diffuse absorbance spectra exhibited bands at 253, 285 and 541 nm in the visible and ultraviolet regions. The optical band gap of the compound was estimated as 3.4 eV. At room temperature, an intense photoluminescence was observed from this material around 392 nm when it excited at 254 nm. The variable temperature dc magnetic susceptibility measurements exposed paramagnetic behaviour at high temperatures and antiferromagnetic ordering at low temperatures.

  13. Synthesis, Structure and Properties of Two Novel 2D Zinc(II) Coordination Polymers based on Fluconazole and Benzene Carboxylic Acid

    Energy Technology Data Exchange (ETDEWEB)

    Pan, Ganghong; Tang, Jingniu; Xu, Wenjia; Liang, Peng; Huang, Zhongjing [Guangxi University for Nationalities, Nanning (China)

    2013-12-15

    The design and synthesis of coordination polymers have aroused great interest owing to their intriguing aesthetic structures and potential applications in nonlinear optics, gas storage, ion exchange, luminescence, magnetism and catalysis. Self-assembly of bridging organic ligands (connectors) and multi-connected metal ions can give rise to various types of interesting coordination polymers. Since metal ion Zn(II) with d{sup 10} electronic configuration permits a variety of coordination numbers and geometries which are not dependent on ligand field stabilization but on ligand size and charge, it is well suited for the construction of various coordination polymers. Its borderline hardness allows the coordination of N, O and S donor atoms.

  14. Synthesis, properties, crystal structures, and semiconductor characteristics of naphtho[1,2-b:5,6-b']dithiophene and -diselenophene derivatives.

    Science.gov (United States)

    Shinamura, Shoji; Miyazaki, Eigo; Takimiya, Kazuo

    2010-02-19

    In this paper we present the synthesis, structures, characterization, and applications to field-effect transistors (FETs) of naphtho[1,2-b:5,6-b']dithiophene (NDT) and -diselenophene (NDS) derivatives. Treatment of 1,5-dichloro-2,6-diethynylnaphthalenes, easily derived from commercially available 2,6-dihydroxynaphthalene, with sodium chalcogenide afforded a straightforward access to NDTs and NDSs including the parent and dioctyl and diphenyl derivatives. Physicochemical evaluations of NDT and NDS derivatives showed that these heteroarenes have a similar electronic structure with isomeric [1]benzothieno[2,3-b][1]benzothiophene (BTBT) and [1]benzoselenopheneno[2,3-b][1]benzoselenophene (BSBS) derivatives, respectively. Although attempts to fabricate solution-processed field-effect transistors (FETs) with soluble dioctyl-NDT (C(8)-NDT) and -NDS (C(8)-NDS) failed, diphenyl derivatives (DPh-NDT and DPh-NDS) afforded vapor-processed FETs showing field-effect mobility as high as 0.7 cm(2) V(-1) s(-1). These results indicated that NDT and NDS are new potential heteroarene core structures for organic semiconducting materials.

  15. Er{sup 3+}-doped Y{sub 2}O{sub 3} obtained by polymeric precursor: Synthesis, structure and upconversion emission properties

    Energy Technology Data Exchange (ETDEWEB)

    Perrella, Rafael V.; Santos, Daniela P. dos [Grupo de Pesquisa em Química de Materiais – (GPQM), Departamento de Ciências Naturais, Universidade Federal de São João del-Rei, Campus Dom Bosco, Praça Dom Helvécio, 74, 36301-160 São João del-Rei, MG (Brazil); Poirier, Gael Y. [Instituto de Ciência e Tecnologia, Universidade Federal de Alfenas, Cidade Universitária, 37715400 Poços de Caldas, MG (Brazil); Góes, Márcio S. [Universidade Federal da Integração Latino-Americana (UNILA), Av. Tancredo Neves, 6731 – Bloco 4, Cx P. 2044, CEP: 85867-970 Foz do Iguaçu, PR (Brazil); Ribeiro, Sidney José L. [Instituto de Química, UNESP, P.O. Box 355, 14800-970 Araraquara, SP (Brazil); Schiavon, Marco A. [Grupo de Pesquisa em Química de Materiais – (GPQM), Departamento de Ciências Naturais, Universidade Federal de São João del-Rei, Campus Dom Bosco, Praça Dom Helvécio, 74, 36301-160 São João del-Rei, MG (Brazil); and others

    2014-05-01

    The relentless pursuit for materials containing rare earth ions with photoluminescent properties has led to several studies with applications in the development of new technologies. The main focus of this work is the preparation of Er{sup 3+}-doped polycrystalline Y{sub 2}O{sub 3} with photoluminescent properties using PEG as an organic precursor and heat-treated at different temperatures. The methodology used in this synthesis is highly attractive due to its high feasibility for improved technology and low cost for preparing materials. The behavior of the viscous resin has been evaluated and the final compounds exhibited the formation of a cubic polycrystalline phase, which is able to support variations in Er{sup 3+} doping concentrations up to 10 mol%, without significant changes in the polycrystalline parameters. The values of the nanocrystallite size calculated by Scherrer's equation showed direct dependence on the heat-treatment temperature as well as the Er{sup 3+} concentration. Intense emission in the visible region under excitation at 980 nm was attributed to an upconversion phenomenon assigned to the intraconfigurational f–f transitions of Er{sup 3+} ions. The upconversion mechanism was investigated and it was demonstrated that the higher intense emission in the red region in comparison to the emission in the green region is related to the crystallite size. The studies about the intensity showed the dependence of upconversion emission of power source, indicating that two-photon are responsible for the green and red photoluminescence. These polycrystalline materials exhibit properties that make them promising for use in solar energy systems, C-telecom band or solid-state laser devices. - Highlights: • Intense red upconversion emission. • Very easy way to prepare the material. • Potential application in solar cells. • Application for C-telecom band.

  16. Synthesis and characterization of structural, morphological and photosensor properties of Cu0.1Zn0.9S thin film prepared by a facile chemical method

    Science.gov (United States)

    Gubari, Ghamdan M. M.; Ibrahim Mohammed S., M.; Huse, Nanasaheb P.; Dive, Avinash S.; Sharma, Ramphal

    2018-05-01

    The Cu0.1Zn0.9S thin film was grown by facile chemical bath deposition (CBD) method on glass substrates at 60°C. The structural, morphological, photosensor properties of the as-grown thin film has been investigated. The structural and phase confirmation of the as-grown thin film was carried out by X-ray diffraction (XRD) technique and Raman spectroscopy. The FE-SEM images showed that the thin films are well covered with material on an entire glass substrate. From the optical absorption spectrum, the direct band gap energy for the Cu0.1Zn0.9S thin film was found to be ˜3.16 eV at room temperature. The electrical properties were measured at room temperature in the voltage range ±2.5 V, showed a drastic enhancement in current under light illumination with the highest photosensitivity of ˜72 % for 260 W.

  17. Diamond nanowires: fabrication, structure, properties, and applications.

    Science.gov (United States)

    Yu, Yuan; Wu, Liangzhuan; Zhi, Jinfang

    2014-12-22

    C(sp(3) )C-bonded diamond nanowires are wide band gap semiconductors that exhibit a combination of superior properties such as negative electron affinity, chemical inertness, high Young's modulus, the highest hardness, and room-temperature thermal conductivity. The creation of 1D diamond nanowires with their giant surface-to-volume ratio enhancements makes it possible to control and enhance the fundamental properties of diamond. Although theoretical comparisons with carbon nanotubes have shown that diamond nanowires are energetically and mechanically viable structures, reproducibly synthesizing the crystalline diamond nanowires has remained challenging. We present a comprehensive, up-to-date review of diamond nanowires, including a discussion of their synthesis along with their structures, properties, and applications. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  18. Large-scale synthesis of hierarchical-structured weissite (Cu2−xTe) flake arrays and their catalytic properties

    International Nuclear Information System (INIS)

    Cao, Xinjiang; Yan, Shancheng; Ortiz, Lazarus Santiago; Liang, Gaofeng; Sun, Bo; Huang, Ningping; Xiao, Zhongdang

    2014-01-01

    Graphical abstract: - Highlights: • Large-scale Cu 2−x Te flake arrays grown on copper foam were synthesized. • They possess superior catalytic efficiency on methylene blue with the assistance of H 2 O 2 . • The effects of preparing conditions on the growth of Cu 2−x Te flake arrays were investigated. - Abstract: Large-scale weissite (Cu 2−x Te) flake arrays with three-dimensional (3D) hierarchical structure have been successfully fabricated via a facile one-step solution-phase strategy through the reaction of tellurium powder and copper foam. At the end of the reaction Cu 2−x Te flakes were distributed evenly on the surface of a porous solid copper substrate. Field-emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM) analysis showed the abundance of flakes grown on the 3D porous copper architecture, while X-ray diffraction (XRD) and energy-dispersive X-ray spectra (EDS) were used to determine the crystal structure and phase composition of these products. A series of experiments discovered that the size and morphology of the products could be affected by some reactive parameters including the reaction time, synthesis temperature and volume ratio of absolute ethanol/deionized water. Catalysis experiments using the in situ synthesized of Cu 2−x Te flakes to catalyze the degradation of methylene blue (MB) demonstrated the strong catalytic ability of these flakes

  19. Synthesis, crystal structure refinement, and nonlinear-optical properties of CaB{sub 3}O{sub 5}(OH): Comparative crystal chemistry of calcium triborates

    Energy Technology Data Exchange (ETDEWEB)

    Yamnova, N. A., E-mail: aks.crys@gmail.com; Aksenov, S. M. [Moscow State University, Faculty of Geology (Russian Federation); Stefanovich, S. Yu. [Moscow State University, Faculty of Chemistry (Russian Federation); Volkov, A. S.; Dimitrova, O. V. [Moscow State University, Faculty of Geology (Russian Federation)

    2015-09-15

    Calcium triborate CaB{sub 3}O5(OH) obtained by hydrothermal synthesis in the Ca(OH){sub 2}–H{sub 3}BO{sub 3}–Na{sub 2}CO{sub 3}–KCl system is studied by single-crystal X-ray diffraction. The parameters of the orthorhombic unit cell are as follows: a = 13.490(1), b = 6.9576(3), and c = 4.3930(2) Å; V = 412.32(3) Å{sup 3} and space group Pna2{sub 1}. The structure is refined in the anisotropic approximation of the atomic displacement parameters to R = 4.28% using 972 vertical bar F vertical bar > 4σ(F). It is confirmed that the crystal structure of Ca triborate CaB{sub 3}O{sub 5}(OH) is identical to that described earlier. The hydrogen atom is localized. An SHG signal stronger than that of the quartz standard is registered. The phase transition of calcium triborate into calciborite is found on heating. The comparative crystal-chemical analysis of a series of borates with the general chemical formula 2CaO · 3B{sub 2}O{sub 3} · nH{sub 2}O (n = 0–13) with the constant CaO: B{sub 2}O{sub 3}= 2: 3 ratio and variable content of water is performed.

  20. Synthesis, crystal structure refinement, and nonlinear-optical properties of CaB3O5(OH): Comparative crystal chemistry of calcium triborates

    International Nuclear Information System (INIS)

    Yamnova, N. A.; Aksenov, S. M.; Stefanovich, S. Yu.; Volkov, A. S.; Dimitrova, O. V.

    2015-01-01

    Calcium triborate CaB 3 O5(OH) obtained by hydrothermal synthesis in the Ca(OH) 2 –H 3 BO 3 –Na 2 CO 3 –KCl system is studied by single-crystal X-ray diffraction. The parameters of the orthorhombic unit cell are as follows: a = 13.490(1), b = 6.9576(3), and c = 4.3930(2) Å; V = 412.32(3) Å 3 and space group Pna2 1 . The structure is refined in the anisotropic approximation of the atomic displacement parameters to R = 4.28% using 972 vertical bar F vertical bar > 4σ(F). It is confirmed that the crystal structure of Ca triborate CaB 3 O 5 (OH) is identical to that described earlier. The hydrogen atom is localized. An SHG signal stronger than that of the quartz standard is registered. The phase transition of calcium triborate into calciborite is found on heating. The comparative crystal-chemical analysis of a series of borates with the general chemical formula 2CaO · 3B 2 O 3 · nH 2 O (n = 0–13) with the constant CaO: B 2 O 3 = 2: 3 ratio and variable content of water is performed

  1. SYNTHESIS, CHARACTERIZATION AND CRYSTAL STRUCTURES ...

    African Journals Online (AJOL)

    B. S. Chandravanshi

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

  2. SYNTHESIS, CHARACTERIZATION AND CRYSTAL STRUCTURE ...

    African Journals Online (AJOL)

    Preferred Customer

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

  3. The comparative study of the structural and the electrical properties of the nano spinel ferrites prepared by the soft mehanochemical synthesis

    Directory of Open Access Journals (Sweden)

    Sekulić D.L.

    2014-01-01

    Full Text Available Nano spinel ferrites MFe2O4 (M=Ni, Mn, Zn were obtained by soft mechanochemical synthesis in a planetary ball mill. The appropriate mixture of oxide and hydroxide powders was used as initial compounds. All of this mixture of powders was mechanically activated, uniaxial pressed and sintered at 1100°C/2h. The phase composition of the powders and sintered samples were analyzed by XRD and Raman spectroscopy. Morphologies were examined by SEM. In this study, the AC-conductivity and DC-resistivity of sintered samples of MFe2O4 (M= Ni, Mn, Zn ferrites were measured at different frequencies and at room temperature. The values of the electrical conductivities show an increase with increasing temperature, which indicated the semiconducting behavior of the studied ferrites. The conduction phenomenon of the investigated samples could be explained on the basis of hopping model. The complex impedance spectroscopy analysis was used to study the effect of grain and grain boundary on the electrical properties of all three obtained ferrites [Projekat Ministarstva nauke Republike Srbije, br. III 45003

  4. Facile hydrothermal synthesis of alpha manganese sesquioxide (α-Mn2O3) nanodumb-bells: Structural, magnetic, optical and photocatalytic properties

    International Nuclear Information System (INIS)

    Gnanam, S.; Rajendran, V.

    2013-01-01

    Highlights: ► α-Mn 2 O 3 nanoparticles sizes of 35–42 nm have been prepared by hydrothermal process. ► Shapes of α-Mn 2 O 3 : Dumb-bell, Cauliflower, spherical with rod, spherical with wires. ► The strong UV emission can be attributed to high purity and perfect crystallinity. ► Photocatalytic activity of α–Mn 2 O 3 was studied by degradation of Remazol red B dye. - Abstract: Nanometer scale cubic bixbyite α-Mn 2 O 3 has been synthesized by a facile hydrothermal method, at a temperature of 450 °C in the presence of various surfactants. The X-ray diffraction (XRD) analysis shows that the average crystallite size of the sample is ∼35–42 nm. The shapes of the α-Mn 2 O 3 nanoparticles include: Dumb-bell-like (anionic surfactant), Cauliflower-like (nonionic surfactant), spherical with rods (cationic surfactant) and spherical with wires (surface modifier). The shapes of α-Mn 2 O 3 nanoparticles depend on the type of surfactant used in the synthesis. The magnetic property of the anionic surfactant assisted sample was primarily studied, using the vibrating sample magnetometer (VSM). The optical absorption spectra confirmed the effectiveness of the selected capping agents, as the anionic capped α-Mn 2 O 3 colloids absorbed at shorter wavelength than the other agents, indicating a much smaller crystallite size. The property of strong UV emissions may be attributed to the high purity and perfect crystallinity of the as-prepared α-Mn 2 O 3 . The surfactants-assisted catalyst was tested for its photocatalytic activity towards the photodegradation of the harmful organic dye Remazol Red B, using a multilamp photo reactor. Possible formation mechanisms have also been proposed for the as-synthesized anionic surfactant assisted samples.

  5. Organoactinide chemistry: synthesis, structure, and solution dynamics

    International Nuclear Information System (INIS)

    Brennan, J.G.

    1985-12-01

    This thesis considers three aspects of organoactinide chemistry. In chapter one, a bidentate phosphine ligand was used to kinetically stabilize complexes of the type Cp 2 MX 2 . Ligand redistribution processes are present throughout the synthetic work, as has often been observed in uranium cyclopentadienyl chemistry. The effects of covalent M-L bonding on the solution and solid state properties of U(III) coordination complexes are considered. In particular, the nature of the more subtle interaction between the metal and the neutral ligand are examined. Using relative basicity data obtained in solution, and solid state structural data (and supplemented by gas phase photoelectron measurements), it is demonstrated that the more electron rich U(III) centers engage in significant U → L π-donation. Trivalent uranium is shown to be capable of acting either as a one- or two-electron reducing agent toward a wide variety of unsaturated organic and inorganic molecules, generating molecular classes unobtainable via traditional synthetic approaches, as well as offering an alternative synthetic approach to molecules accessible via metathesis reactions. Ligand redistribution processes are again observed, but given the information concerning ligand lability, this reactivity pattern is applied to the synthesis of pure materials inaccessible from redox chemistry. 214 refs., 33 figs., 10 tabs

  6. Synthesis, crystal structure and luminescent properties of a new pyrochlore type tungstate CsGa0.333W1.667O6

    Science.gov (United States)

    Zhao, Dan; Zhao, Ji; Fan, Yun-Chang; Ma, Zhao; Zhang, Rui-Juan; Liu, Bao-Zhong

    2018-06-01

    High temperature solution reaction leads to a new tungstate compound CsGa0.333W1.667O6, whose structure was determined by single-crystal X-ray diffraction analysis. The results show that it crystallizes in pyrochlore structure with cubic space group Fd-3m and a = 10.2529 (13) Å. In this structure, Ga and W atoms are in a statistical disorder manner. The self-activated luminescent properties CsGa0.333W1.667O6 were studied. Under the excitation of 323 nm, the emission spectrum exhibits a blue emission centered at 466 nm with the chromaticity coordinates (0.1838, 0.1814).

  7. Porous Materials - Structure and Properties

    DEFF Research Database (Denmark)

    Nielsen, Anders

    1997-01-01

    The paper presents some viewpoints on the description of the pore structure and the modelling of the properties of the porous building materials. Two examples are given , where it has been possible to connect the pore structure to the properties: Shrinkage of autoclaved aerated concrete...

  8. Two-dimensional layer architecture assembled by Keggin polyoxotungstate, Cu(II)-EDTA complex and sodium linker: Synthesis, crystal structures, and magnetic properties

    International Nuclear Information System (INIS)

    Liu Hong; Xu Lin; Gao Guanggang; Li Fengyan; Yang Yanyan; Li Zhikui; Sun Yu

    2007-01-01

    Reaction of Keggin polyoxotungstate with copper(II)-EDTA (EDTA=ethylenediamine tetraacetate) complex under mild conditions led to the formation of hybrid inorganic-organic compounds Na 4 (OH)[(Cu 2 EDTA)PW 12 O 40 ].17H 2 O (1) and Na 4 [(Cu 2 EDTA)SiW 12 O 40 ].19H 2 O (2). The single-crystal X-ray diffraction analyses reveal their two structural features: (1) one-dimensional chain structure consisting of Keggin polyoxotungstate and copper(II)-EDTA complex; (2) Two-dimensional layer architecture assembled by the one-dimensional chain structure and sodium linker. The results of magnetic measurements in the temperature range 300-2 K indicated the existence of ferromagnetic exchange interactions between the Cu II ions for both compounds. In addition, TGA analysis, IR spectra, and electrochemical properties were also investigated to well characterize these two compounds. - Graphical abstract: Two new polyoxometalate-based hybrids, Na 4 (OH)[Cu 2 (EDTA)PW 12 O 40 ].17H 2 O (1) and Na 4 [Cu 2 (EDTA)SiW 12 O 40 ].19H 2 O (2), have been synthesized and structurally characterized, which consist of one-dimensional chain structure assembled by Keggin polyoxotungstate and copper(II)-EDTA complex. The chains are further connected to form two-dimensional layer architecture assembled by the one-dimensional chain structure and sodium linker

  9. Assembling Metal Ions Induced Cyanide-Bridged Heterometallic 1D and Ion-Pair Complexes: Synthesis, Crystal Structures and Magnetic Properties

    International Nuclear Information System (INIS)

    Kong, Lingqian; Zhao, Zengdian; Chen, Kexun; Wang, Ping; Zhang, Daopeng

    2013-01-01

    We obtained a heterobimetallic one-dimensional cyanide-bridged Mn(II)-Ni(II) complex and an Co(III)-Ni(II) ion-pair complex with [Ni(CN) 4 ] 2- as building block and M(II)-phenanthroline (M = Mn, Co) compounds as assembling segment. The different structural types of complexes 1 and 2 indicate that the property of the metal ions the assembling segment contained have obvious influence on the structure of the cyanide-bridged complex. Investigation over the magnetic properties of complex 1 reveals an overall weak antiferromagnetic coupling between the adjacent Mn(II) ions bridged by the antiferromagnetic [-NC-Ni-CN-] unit. Among of all the molecular magnetism systems, for the well known reasons, cyanide-containing complexes have been widely employed as bridges to assemble homo/hetero-metallic molecular magnetic materials by using the cyanide bridge transferring magnetic coupling between the neighboring paramagnetic ions, in whichsome showed interesting magnetic properties, such as high-Tc magnets, spin crossover materials, single-molecule magnets (SMMs) and single-chain magnets (SCMs)

  10. Assembling Metal Ions Induced Cyanide-Bridged Heterometallic 1D and Ion-Pair Complexes: Synthesis, Crystal Structures and Magnetic Properties

    Energy Technology Data Exchange (ETDEWEB)

    Kong, Lingqian [Liaocheng Univ., Liaocheng (China); Zhao, Zengdian; Chen, Kexun; Wang, Ping; Zhang, Daopeng [Shandong Univ. of Technology, Zibo (China)

    2013-07-15

    We obtained a heterobimetallic one-dimensional cyanide-bridged Mn(II)-Ni(II) complex and an Co(III)-Ni(II) ion-pair complex with [Ni(CN){sub 4}]{sup 2-} as building block and M(II)-phenanthroline (M = Mn, Co) compounds as assembling segment. The different structural types of complexes 1 and 2 indicate that the property of the metal ions the assembling segment contained have obvious influence on the structure of the cyanide-bridged complex. Investigation over the magnetic properties of complex 1 reveals an overall weak antiferromagnetic coupling between the adjacent Mn(II) ions bridged by the antiferromagnetic [-NC-Ni-CN-] unit. Among of all the molecular magnetism systems, for the well known reasons, cyanide-containing complexes have been widely employed as bridges to assemble homo/hetero-metallic molecular magnetic materials by using the cyanide bridge transferring magnetic coupling between the neighboring paramagnetic ions, in whichsome showed interesting magnetic properties, such as high-Tc magnets, spin crossover materials, single-molecule magnets (SMMs) and single-chain magnets (SCMs)

  11. Open-chain poly(organophosphazenes). Synthesis and properties

    International Nuclear Information System (INIS)

    Vinogradova, Svetlana V; Tur, Dzidra R; Vasnev, Valery A

    1998-01-01

    Various methods for the synthesis of open-chain poly(organophosphazenes) are considered. The mechanism of polymerisation of hexachlorocyclotriphosphazene and the basic principles of formation of poly(organophosphazene) macromolecules by polymeranalogous reactions of poly(dichloro-phosphazene) with various nucleophilic reagents are analysed from a new viewpoint. The potential of this synthetic method for targeted design of poly(organophosphazenes) of various structures is shown. The possibility of synthesising poly(organophosphazenes) by polymerisation of cyclophosphazenes is also discussed. The problem of unit non-uniformity of poly(organophosphazenes) and its influence on the properties of these polymers are considered. The properties of poly(organophosphazenes) are considered in detail and it is shown that these polymers possess unusual valuable properties, which provide opportunities for their successful practical application. The bibliography includes 276 references.

  12. Synthesis, Properties and Potential Applications of Porous Graphene: A Review

    Institute of Scientific and Technical Information of China (English)

    Paola Russo; Anming Hu; Giuseppe Compagnini

    2013-01-01

    Since the discovery of graphene, many efforts have been done to modify the graphene structure for integrating this novel material to nanoelectronics, fuel cells, energy storage devices and in many other applications. This leads to the production of different types of graphene-based materials, which possess properties different from those of pure graphene. Porous graphene is an example of this type of materials. It can be considered as a graphene sheet with some holes/pores within the atomic plane. Due to its spongy structure, porous graphene can have potential applications as membranes for molecular sieving, energy storage components and in nanoelectronics. In this review, we present the recent progress in the synthesis of porous graphene. The properties and the potential applications of this new material are also discussed.

  13. Synthesis, characterization and theoretical investigations of the structure, electronic properties and third-order nonlinearity optics (NLO) of M(DPIP)₂.

    Science.gov (United States)

    Li, Kang; Tang, Guodong; Kou, ShanShan; Culnane, Lance F; Zhang, Yu; Song, Yinglin; Li, Rongqing; Wei, Changmei

    2015-03-15

    Three complexes of M(DPIP)2 (M=Cu, Co, Zn as 1, 2, 3) were synthesized and characterized by elemental analysis, IR, UV-Vis, thermogravimetry, and X-ray diffraction. Their nonlinear optical properties were measured by the Z-scan technique and yielded a normalized transmittance of about 70% for complex 1 (45 μJ pulse), and 93% for complex 3 (68 μJ pulse at the focus point). The nonlinear absorption coefficient, β, is 1.4×10(-11) m/W for 1 and 5.6×10(-13) m/W for 3, and the third-order nonlinear refraction index, n2, is 1.0×10(-18) m(2)/W for 3. Complex 1 shows self-defocusing property, while complex 3 exhibits self-focusing property. The thermogravimetric results show that the frame structure of compounds 1-3 begin to collapse at 400, 250 and 280°C, respectively, which suggests that they elicit excellent thermal stability. This research aims to provide better understanding of these compounds, and offer preliminary explanations for the significant differences between compounds 1-3, in order to potentially help in the designing of future novel materials with NLO properties. Copyright © 2014 Elsevier B.V. All rights reserved.

  14. Synthesis, characterization and theoretical investigations of the structure, electronic properties and third-order nonlinearity optics (NLO) of M(DPIP)2

    Science.gov (United States)

    Li, Kang; Tang, Guodong; Kou, ShanShan; Culnane, Lance F.; Zhang, Yu; Song, Yinglin; Li, Rongqing; Wei, Changmei

    2015-03-01

    Three complexes of M(DPIP)2 (M = Cu, Co, Zn as 1, 2, 3) were synthesized and characterized by elemental analysis, IR, UV-Vis, thermogravimetry, and X-ray diffraction. Their nonlinear optical properties were measured by the Z-scan technique and yielded a normalized transmittance of about 70% for complex 1 (45 μJ pulse), and 93% for complex 3 (68 μJ pulse at the focus point). The nonlinear absorption coefficient, β, is 1.4 × 10-11 m/W for 1 and 5.6 × 10-13 m/W for 3, and the third-order nonlinear refraction index, n2, is 1.0 × 10-18 m2/W for 3. Complex 1 shows self-defocusing property, while complex 3 exhibits self-focusing property. The thermogravimetric results show that the frame structure of compounds 1-3 begin to collapse at 400, 250 and 280 °C, respectively, which suggests that they elicit excellent thermal stability. This research aims to provide better understanding of these compounds, and offer preliminary explanations for the significant differences between compounds 1-3, in order to potentially help in the designing of future novel materials with NLO properties.

  15. Structured synthesis of MEMS using evolutionary approaches

    DEFF Research Database (Denmark)

    Fan, Zhun; Wang, Jiachuan; Achiche, Sofiane

    2008-01-01

    In this paper, we discuss the hierarchy that is involved in a typical MEMS design and how evolutionary approaches can be used to automate the hierarchical synthesis process for MEMS. The paper first introduces the flow of a structured MEMS design process and emphasizes that system-level lumped...

  16. Effect of polyvinyl alcohol content and after synthesis neutralization on structure, mechanical properties and cytotoxicity of sol-gel derived hybrid foams

    Directory of Open Access Journals (Sweden)

    Agda Aline Rocha de Oliveira

    2009-06-01

    Full Text Available Bioactive glass/polymer hybrids are promising materials for biomedical applications because they combine the bioactivity of these glasses with the flexibility of polymers. In this work it was evaluated the effect of increasing the PVA content of the on structural characteristics and mechanical properties of hybrid. The hybrids were prepared with 70 wt. (% SiO2-30 wt. (% CaO and PVA fractions of 20 to 60 wt. (% by the sol-gel method. The structural and mechanical characterization was done by FTIR, SEM and compression tests. To reduce the acidic character of the hybrids due to the catalysts added, different neutralization solutions were tested. The calcium acetate alcoholic solution was the best neutralizing method, resulting in foams with final pH of about 7.0 and small sample contraction. The foams presented porosity of 60-85 wt. (% and pore diameters of 100-500 μm with interconnected structure. An increase of PVA fraction in the hybrids improved their mechanical properties. The scaffolds produced provided a good environment for the adhesion and proliferation of osteoblasts.

  17. Synthesis of Beam Lines with Necessary Properties

    CERN Document Server

    Andrianov, Serge

    2005-01-01

    In this paper a new approach to the problem of synthesis of beam lines is discussed. Usually this problem can be overcome by the use of numerical simulation and optimal control theory methods. But this results in sufficiently great number of variable parameters and functions. Obviously, that this degrades quality of a modeling procedure. The suggested approach is demonstrated on a problem of a microprobe design problem. Essence of the problem is that necessary to design a high precision focusing system which satisfies some additional conditions. For solution of this problem we use an algebraic treatment based on Lie algebraic methods and computer algebra techniques. Using the symmetry ideology this approach allows rewriting beam properties to enough simple conditions for control parameters and functions. This leads a set of desired solutions and show results in some most suitable form. Moreover, this approach decreases the number of variable parameters.

  18. Synthesis, magnetic properties and electronic structure of the S  =  ½ uniform spin chain system InCuPO5

    Science.gov (United States)

    Koteswararao, B.; Hazra, Binoy K.; Rout, Dibyata; Srinivasarao, P. V.; Srinath, S.; Panda, S. K.

    2017-07-01

    We have studied the structural and magnetic properties and electronic structure of the compound InCuPO5 synthesized by a solid state reaction method. The structure of InCuPO5 comprises S  =  ½ uniform spin chains formed by corner-shared CuO4 units. Magnetic susceptibility (χ(T)) data show a broad maximum at about 65 K, a characteristic feature of one-dimensional (1D) magnetism. The χ(T) data are fitted to the coupled S  =  ½ Heisenberg antiferromagnetic (HAFM) uniform chain model that gives the intra-chain coupling (J/k B) between nearest-neighbor Cu2+ ions as  -100 K and the ratio of inter-chain to intra-chain coupling (J‧/J) as about 0.07. The exchange couplings estimated from the magnetic data analysis are in good agreement with the values computed from the electronic structure calculations based on the density functional theory  +  Hubbard U (DFT  +  U) approach. The combination of theoretical and experimental analysis confirms that InCuPO5 is a candidate material for weakly coupled S  = ½ uniform chains. A detailed theoretical analysis of the electronic structure further reveals that the system is insulating with a gap of 2.4 eV and a local moment of 0.70 µ B/Cu.

  19. Ternary rare earth sulfide CaCe2S4: Synthesis and characterization of stability, structure, and photoelectrochemical properties in aqueous media

    Science.gov (United States)

    Sotelo, Paola; Orr, Melissa; Galante, Miguel Tayar; Hossain, Mohammad Kabir; Firouzan, Farinaz; Vali, Abbas; Li, Jun; Subramanian, Mas; Longo, Claudia; Rajeshwar, Krishnan; Macaluso, Robin T.

    2018-06-01

    A red-orange rare earth ternary chalcogenide, CaCe2S4, was prepared in powder form by solid-state synthesis. The structural details of this compound were determined by powder X-ray diffraction. The optical band gap of CaCe2S4 was determined by diffuse reflectance spectroscopy (DRS) to be 2.1 eV, consistent with the observed red-orange color. Quantitative colorimetry measurements also support the observed color and band gap of CaCe2S4. Both direct and indirect optical transitions were gleaned from Tauc analyses of the DRS data. Photoelectrochemistry experiments on CaCe2S4 films showed n-type semiconductor behavior. Analyses of these data via the Butler-Gärtner model afforded a flat-band potential of - 0.33 V (vs. Ag/AgCl/KCl 4 M) in pH 9 aqueous sulfite electrolyte. The potential and limitations of this material for solar water splitting and photocatalytic environmental remediation (e.g., dye photodegradation) are finally presented against the backdrop of its photoelectrochemical stability and surface hole transfer kinetics in aqueous electrolytes.

  20. Synthesis, crystal structure and photoluminescent properties of Eu{sup 3+} ion-activated R{sub 4}MoO{sub 9} (R = Y, Gd, and Lu)

    Energy Technology Data Exchange (ETDEWEB)

    Li, Huaiyong [Department of Materials Science and Engineering, Liaocheng University, Liaocheng 252059 (China); Moon, Byung Kee; Choi, Byung Chun [Department of Physics, Pukyong National University, Busan 608-737 (Korea, Republic of); Jeong, Jung Hyun, E-mail: jhjeong@pknu.ac.kr [Department of Physics, Pukyong National University, Busan 608-737 (Korea, Republic of); Yang, Hyun Kyoung [Jeju Global Research Center, Korea Institute of Energy Research, Jeju 695-971 (Korea, Republic of); Jang, Kiwan; Lee, Ho Sueb [Department of Physics, Changwon National University, Changwon 641-773 (Korea, Republic of); Yi, Soung Soo [Department of Electronic Material Engineering, Silla University, Busan 617-736 (Korea, Republic of)

    2013-05-15

    Rare earth molybdates R{sub 4}MoO{sub 9} (R = Y, Gd, and Lu) with Eu{sup 3+} ion-doped were synthesized by solid-state reaction. The phase structure, optical absorption and photoluminescence properties of the as-prepared powder samples were studied. The powder X-ray diffraction patterns indicated that all the compounds crystallized in a hexagonal structure, and the lattice parameters reduced in the order of the ionic radii of R. The UV–visible diffuse reflectance spectra revealed that the compounds had a strong absorption of near-UV light due to the excitation of MoO{sub 6} groups in the host lattices. The energy absorbed by the host lattices could then be transferred to doped Eu{sup 3+} ions, resulting in red emission due to the f–f transitions of Eu{sup 3+} ions. The optical absorption and photoluminescence properties of the compounds indicated that they might be candidates as the color-conversion red phosphors for solid-state lighting. - Highlights: ► Structure, optical and photoluminescence properties of Eu{sup 3+} ion-activated R{sub 4}MoO{sub 9} were studied. ► Energy transfer from MoO{sub x} to Eu{sup 3+} can be used to convert near-UV to red light. ► R{sub 4}MoO{sub 9}:Eu might be candidate for color-conversion red phosphors excited by near-UV light.

  1. Synthesis, Structure and Fluorescence Properties of 5,17-Distyryl-25,26,27,28-tetraproproxycalix[4]arenes in the Cone Conformation

    DEFF Research Database (Denmark)

    Larsen, Mogens; Krebs, Frederik C; Jørgensen, Mikkel

    1998-01-01

    The HWE (Horner-Wadsworth-Emmons) reaction performed on the easily obtainable 5,17-diformyl- calix[4]arenes (cone) with arylmethyl phosphorus ylides yielded 5,17-distyryl-25,26,27, 28-tetrapropoxycalix[4]arenes (cone) in high yield and purely in the E/E configuration. Compounds 2-5 were prepared...... this way containing bromine. Subsequent bromine-lithium exchange and reaction with trimethoxyborane yielded the boryl- substituted 5,17-distyrylcalix[4] arenes 6-7a. The structures of 3, 5, and 7a were determined by X-ray diffraction. The photophysical properties of 2 were established by absorption...

  2. Large-scale synthesis of hierarchical-structured weissite (Cu{sub 2−x}Te) flake arrays and their catalytic properties

    Energy Technology Data Exchange (ETDEWEB)

    Cao, Xinjiang [State Key Laboratory of Bioelectronics (Chien-Shiung Wu Lab), School of Biological Science and Medical Engineering, Southeast University, Si Pai Lou 2#, Nanjing 210096 (China); Yan, Shancheng [School of Geography and Biological Information, Nanjing University of Posts and Telecommunications, Nanjing 210046 (China); Ortiz, Lazarus Santiago; Liang, Gaofeng; Sun, Bo; Huang, Ningping [State Key Laboratory of Bioelectronics (Chien-Shiung Wu Lab), School of Biological Science and Medical Engineering, Southeast University, Si Pai Lou 2#, Nanjing 210096 (China); Xiao, Zhongdang, E-mail: zdxiao@seu.edu.cn [State Key Laboratory of Bioelectronics (Chien-Shiung Wu Lab), School of Biological Science and Medical Engineering, Southeast University, Si Pai Lou 2#, Nanjing 210096 (China)

    2014-03-01

    Graphical abstract: - Highlights: • Large-scale Cu{sub 2−x}Te flake arrays grown on copper foam were synthesized. • They possess superior catalytic efficiency on methylene blue with the assistance of H{sub 2}O{sub 2}. • The effects of preparing conditions on the growth of Cu{sub 2−x}Te flake arrays were investigated. - Abstract: Large-scale weissite (Cu{sub 2−x}Te) flake arrays with three-dimensional (3D) hierarchical structure have been successfully fabricated via a facile one-step solution-phase strategy through the reaction of tellurium powder and copper foam. At the end of the reaction Cu{sub 2−x}Te flakes were distributed evenly on the surface of a porous solid copper substrate. Field-emission scanning electron microscopy (FESEM) and transmission electron microscopy (TEM) analysis showed the abundance of flakes grown on the 3D porous copper architecture, while X-ray diffraction (XRD) and energy-dispersive X-ray spectra (EDS) were used to determine the crystal structure and phase composition of these products. A series of experiments discovered that the size and morphology of the products could be affected by some reactive parameters including the reaction time, synthesis temperature and volume ratio of absolute ethanol/deionized water. Catalysis experiments using the in situ synthesized of Cu{sub 2−x}Te flakes to catalyze the degradation of methylene blue (MB) demonstrated the strong catalytic ability of these flakes.

  3. New Synthesis, Structure and Analgesic Properties of Methyl 1-R-4-Methyl-2,2-Dioxo-1H-2λ6,1-Benzothiazine-3-Carboxylates

    Directory of Open Access Journals (Sweden)

    Liliana Azotla-Cruz

    2017-01-01

    Full Text Available According to the principles of the methodology of bioisosteric replacements a series of methyl 1-R-4-methyl-2,2-dioxo-1H-2λ6,1-benzothiazine-3-carboxylates has been obtained as potential analgesics. In addition, a fundamentally new strategy for the synthesis of compounds of this chemical class involving the introduction of N-alkyl substituent at the final stage in 2,1-benzothiazine nucleus already formed has been proposed. Using nuclear magnetic resonance (NMR spectroscopy, mass spectrometry and X-ray diffraction analysis it has been proven that in the DMSO/K2CO3 system the reaction of methyl 4-methyl-2,2-dioxo-1H-2λ6,1-benzothiazine-3-carboxylate and alkyl halides leads to formation of N-substituted derivatives with good yields regardless of the structure of the alkylating agent. The peculiarities of NMR (1Н and 13С spectra of the compounds synthesized, their mass spectrometric behavior and the spatial structure are discussed. In N-benzyl derivative the ability to form a monosolvate with methanol has been found. According to the results of the pharmacological testing conducted on the model of the thermal tail-flick it has been determined that replacement of 4-ОН-group in methyl 1-R-4-hydroxy-2,2-dioxo-1H-2λ6,1-benzothiazine-3-carboxylates for the methyl group is actually bioisosteric since all methyl 1-R-4-methyl-2,2-dioxo-1H-2λ6,1-benzothiazine-3-carboxylates synthesized demonstrated a statistically significant analgesic effect. The majority of the substances can inhibit the thermal pain response much more effective than piroxicam in the same dose. Under the same conditions as an analgesic the N-methyl-substituted analog exceeds not only piroxicam, but more active meloxicam as well. Therefore, it deserves in-depth biological studies on other experimental models.

  4. SYNTHESIS, CHARACTERIZATION, AND CRYSTAL STRUCTURE ...

    African Journals Online (AJOL)

    a

    KEY WORDS: Barium, Crystal structure, 2,6-Pyridinedicarboxylic acid .... The rational design of novel metal-organic frameworks has attracted great ..... Bond, A.D.; Jones, W. Supramolecular Organization and Materials Design, Jones, W.; Rao,.

  5. Synthesis, electronic structure and luminescent properties of a new red-emitting phosphor GdBiW2O9:Eu3+

    Science.gov (United States)

    Xie, Zhi; Zhou, Weiwei; Zhao, Wang; Zhang, Hao; Hu, Qichang; Xu, Xuee

    2017-10-01

    Red phosphor of GdBiW2O9:Eu3+ was prepared by solid-state reaction method. The phase purity and structure of the samples were characterized by XRD. The electronic structures of GdBiW2O9 host were estimated by DFT calculation. The PLE and PL spectra were also investigated. The optimal luminescent properties of GdBiW2O9:Eu3+ phosphors were obtained at 900 °C with 40 mol% of Eu3+ concentration. The phosphors can be excited efficiently by 396 nm NUV light and emit intense red light peaking at 618 nm. The results indicate GdBiW2O9:Eu3+ can act as a potential red-emitting phosphor for LEDs application.

  6. Facile hydrothermal synthesis of alpha manganese sesquioxide ({alpha}-Mn{sub 2}O{sub 3}) nanodumb-bells: Structural, magnetic, optical and photocatalytic properties

    Energy Technology Data Exchange (ETDEWEB)

    Gnanam, S., E-mail: gnanam.nanoscience@gmail.com [Department of Physics, Presidency College, Chennai 600005, Tamilnadu (India); Rajendran, V. [Department of Physics, Presidency College, Chennai 600005, Tamilnadu (India)

    2013-02-15

    Highlights: Black-Right-Pointing-Pointer {alpha}-Mn{sub 2}O{sub 3} nanoparticles sizes of 35-42 nm have been prepared by hydrothermal process. Black-Right-Pointing-Pointer Shapes of {alpha}-Mn{sub 2}O{sub 3}: Dumb-bell, Cauliflower, spherical with rod, spherical with wires. Black-Right-Pointing-Pointer The strong UV emission can be attributed to high purity and perfect crystallinity. Black-Right-Pointing-Pointer Photocatalytic activity of {alpha}-Mn{sub 2}O{sub 3} was studied by degradation of Remazol red B dye. - Abstract: Nanometer scale cubic bixbyite {alpha}-Mn{sub 2}O{sub 3} has been synthesized by a facile hydrothermal method, at a temperature of 450 Degree-Sign C in the presence of various surfactants. The X-ray diffraction (XRD) analysis shows that the average crystallite size of the sample is {approx}35-42 nm. The shapes of the {alpha}-Mn{sub 2}O{sub 3} nanoparticles include: Dumb-bell-like (anionic surfactant), Cauliflower-like (nonionic surfactant), spherical with rods (cationic surfactant) and spherical with wires (surface modifier). The shapes of {alpha}-Mn{sub 2}O{sub 3} nanoparticles depend on the type of surfactant used in the synthesis. The magnetic property of the anionic surfactant assisted sample was primarily studied, using the vibrating sample magnetometer (VSM). The optical absorption spectra confirmed the effectiveness of the selected capping agents, as the anionic capped {alpha}-Mn{sub 2}O{sub 3} colloids absorbed at shorter wavelength than the other agents, indicating a much smaller crystallite size. The property of strong UV emissions may be attributed to the high purity and perfect crystallinity of the as-prepared {alpha}-Mn{sub 2}O{sub 3}. The surfactants-assisted catalyst was tested for its photocatalytic activity towards the photodegradation of the harmful organic dye Remazol Red B, using a multilamp photo reactor. Possible formation mechanisms have also been proposed for the as-synthesized anionic surfactant assisted samples.

  7. Synthesis, crystal structure and optical properties of two new layered cadmium iodates: Cd(IO3)X (X=Cl, OH)

    International Nuclear Information System (INIS)

    Yang, Bing-Ping; Mao, Jiang-Gao

    2014-01-01

    Systematic explorations of new compounds in the cadmium iodate system by hydrothermal reactions led to two layered iodates, namely, Cd(IO 3 )X (X=Cl, OH). Cd(IO 3 )Cl crystallizes in the orthorhombic space group Cmca (No. 64) whereas Cd(IO 3 )(OH) crystallizes in the orthorhombic space group Pnma (No. 62). Cd(IO 3 )Cl displays a unique double layered structure composed of 1 ∞ [Cd−O 3 Cl] n chains. Cadmium octahedrons form a 1D chain along the a-axis through edge sharing, and such chains are further interconnected via IO 3 groups to form a special double layer on (020) plane. Cd(IO 3 )(OH) also exhibits a layered structure that is composed of cadmium cations, IO 3 groups and hydroxyl ions. Within a layer, chains of CdO 6 edge-shared octahedra are observed along the b-axis. And these chains are connected by IO 3 groups into a layer parallel to the bc plane. Spectroscopic characterizations, elemental analysis, and thermogravimetric analysis for the reported two compounds are also presented. - Graphical abstract: Two new layered cadmium iodates Cd(IO 3 )X (X=Cl, OH) are reported. Cd(IO 3 )Cl features a unique double layered structure whereas Cd(IO 3 )(OH) displays an ordinary layered structure. - Highlights: • Two new layered cadmium iodates Cd(IO 3 )X (X=Cl, OH) are reported. • Cd(IO 3 )Cl features a unique double layered structure. • Cd(IO 3 )(OH) displays an ordinary layered structure. • The spectroscopic and thermal properties have been studied in detail

  8. Thiocyanate cadmium(II) complexes of 2,4,6-tri(2-pyridyl)-1,3,5-triazine – Synthesis, structure and luminescence properties

    International Nuclear Information System (INIS)

    Nawrot, I.; Machura, B.; Kruszynski, R.

    2014-01-01

    Two new thiocyanate cadmium(II) complexes of 2,4,6-tri(2-pyridyl)-1,3,5-triazine were synthesized and characterized. The resulted complexes [Cd(SCN)(NO 3 )(tptz)(H 2 O)] (1) and [Cd(SCN) 2 (tptz)(MeOH)] (2) were studied by IR, UV–vis spectroscopy and single crystal X-ray analysis. The luminescent properties of 1 and 2 were studied in solution and solid state and compared with the free ligand. To get detailed insight into the electronic structure and spectroscopic properties of [Cd(SCN)(NO 3 )(tptz)(H 2 O)] and [Cd(SCN) 2 (tptz)(MeOH)], the density functional theory (DFT) and time-dependent DFT (TD-DFT) calculations were performed. - Highlights: • Two novel thiocyanate cadmium(II) compounds of 2,4,6-tri(2-pyridyl)-1,3,5-triazine were synthesized. • The compounds were identified by IR, UV–vis spectroscopy and X-ray analysis. • The fluorescence properties of the complexes were examined and compared with the free ligand. • The electronic spectra were investigated at the TD-DFT level employing B3LYP/LANL2DZ

  9. Synthesis and formation process of SrSO{sub 4}:Sm{sup 3+} phosphors with hierarchical structures and its electron trapping luminescence properties

    Energy Technology Data Exchange (ETDEWEB)

    Sun, Jiayue, E-mail: jiayue_sun@126.com; Sun, Guangchao; Xue, Bing; Cui, Dianpeng

    2013-10-15

    Highlights: •SrSO{sub 4} flower-like structures were synthesized by a aqueous solution route. •The as-prepared SrSO{sub 4} crystals have high crystalline. •The flower-like structures are composed of well aligned microtablets. •SrSO{sub 4} nuclei spontaneous attach by an “oriented attachment” process. •The SrSO{sub 4} crystals have excellent electron trapping luminescence properties. -- Abstract: Novel three-dimensional (3D) flower-like Strontium sulfate (SrSO{sub 4}) microstructures with hierarchical architecture were successfully fabricated by using Sr(NO{sub 3}){sub 2} react with Na{sub 2}SO{sub 4} aqueous solution under ambient conditions at room temperature. The SrSO{sub 4} flower-like microcrystals have a uniform diameter of about 10 μm, which are composed of numerous well-aligned single tablet-like SrSO{sub 4} crystals oriented radially to their center. The growth mechanism of the flower-like hierarchical celestine particles is discussed to obtain a better understanding on their formation process. XRD patterns confirm the single crystal phase of SrSO{sub 4}. In the photoluminescence property investigations of SrSO{sub 4}:Sm{sup 3+}, narrow bands observed are well identified with the electronic transition configurations of Sm{sup 3+}. The temperature-dependent photoluminescence spectra show that the temperature of maximum emission intensity is 25 °C. The thermal stability and electron trapping luminescence properties were also characterized.

  10. Coordination-organometallic hybrid materials based on the trinuclear M(II)-Ru(II) (M=Ni and Zn) complexes: Synthesis, structural characterization, luminescence and electrochemical properties

    Science.gov (United States)

    Pawal, S. B.; Lolage, S. R.; Chavan, S. S.

    2018-02-01

    A new series of trinuclear complexes of the type Ni[R-C6H4Ndbnd CH(O)C6H3Ctbnd CRu(dppe)2Cl]2 (1a-c) and Zn[Rsbnd C6H4Ndbnd CH(O)C6H3Ctbnd CRu(dppe)2Cl]2 (2a-c) have been prepared from the reaction of trans-[RuCl(dppe)2Ctbnd Csbnd C6H3(OH)(CHO)] (1) with aniline, 4-nitroaniline and 4-methoxyaniline (R1-3) in presence of nickel acetate and zinc acetate in CH2Cl2/MeOH (1:1) mixture. The structural properties of the complexes have been characterized by elemental analyses and spectroscopic techniques viz. FTIR, UV-Visible, 1H NMR and 31P NMR spectral studies. The crystal structure and morphology of the hybrid complexes was investigated with the help of X-ray powder diffraction (XRPD), Scanning electron microscopy (SEM) and Transmission electron microscopy (TEM). The thermal properties of 1a-c and 2a-c were studied by thermogravimetric (TG) analysis. The electrochemical behaviour of the complexes reveals that all complexes displayed a quasireversible redox behaviour corresponding to Ru(II)/Ru(III) and Ni(II)/Ni(III) couples for 1a-c and only Ru(II)/Ru(III) couple for 2a-c. All complexes are emissive in solution at room temperature revealing the influence of substituents and solvent polarity on emission properties of the complexes.

  11. Synthesis, structure and electrochemical properties of LiNaCo{sub 0.5}Fe{sub 0.5}PO{sub 4}F fluoride-phosphate

    Energy Technology Data Exchange (ETDEWEB)

    Fedotov, Stanislav S. [Department of Chemistry, Lomonosov Moscow State University, 119991 Moscow (Russian Federation); Skoltech Center for Electrochemical Energy Storage, Skolkovo Institute of Science and Technology, 143026 Moscow (Russian Federation); Kuzovchikov, Sergey M.; Khasanova, Nellie R.; Drozhzhin, Oleg A.; Filimonov, Dmitriy S. [Department of Chemistry, Lomonosov Moscow State University, 119991 Moscow (Russian Federation); Karakulina, Olesia M.; Hadermann, Joke [EMAT, University of Antwerp, Groenenborgerlaan 171, B-2020 Antwerp (Belgium); Abakumov, Artem M. [Department of Chemistry, Lomonosov Moscow State University, 119991 Moscow (Russian Federation); Skoltech Center for Electrochemical Energy Storage, Skolkovo Institute of Science and Technology, 143026 Moscow (Russian Federation); EMAT, University of Antwerp, Groenenborgerlaan 171, B-2020 Antwerp (Belgium); Antipov, Evgeny V. [Department of Chemistry, Lomonosov Moscow State University, 119991 Moscow (Russian Federation)

    2016-10-15

    LiNaCo{sub 0.5}Fe{sub 0.5}PO{sub 4}F fluoride-phosphate was synthesized via conventional solid-state and novel freeze-drying routes. The crystal structure was refined based on neutron powder diffraction (NPD) data and validated by electron diffraction (ED) and high-resolution transmission electron microscopy (HRTEM). The alkali ions are ordered in LiNaCo{sub 0.5}Fe{sub 0.5}PO{sub 4}F and the transition metals jointly occupy the same crystallographic sites. The oxidation state and oxygen coordination environment of the Fe atoms were verified by {sup 57}Fe Mössbauer spectroscopy. Electrochemical tests of the LiNaCo{sub 0.5}Fe{sub 0.5}PO{sub 4}F cathode material demonstrated a reversible activity of the Fe{sup 3+}/Fe{sup 2+} redox couple at the electrode potential near 3.4 V and minor activity of the Co{sup 3+}/Co{sup 2+} redox couple over 5 V vs Li/Li{sup +}. The material exhibited the discharge capacity of more than 82% (theo.) regarding Fe{sup 3+}/Fe{sup 2+} in the 2.4÷4.6 V vs Li/Li{sup +} potential range. - Graphical abstract: The ball-polyhedral representation of the LiNaCo{sub 0.5}Fe{sub 0.5}PO{sub 4}F crystal structure. The MO{sub 4}F{sub 2} units are depicted as blue octahedra, PO{sub 4} units as orange tetrahedra, sodium atoms are designated as yellow (Na1), lithium – red and brown (Li2, Li3 resp.), fluorine – green, oxygen – violet spheres. - Highlights: • Freeze-drying method was successfully applied to the synthesis of LiNaCo{sub 0.5}Fe{sub 0.5}PO{sub 4}F. • The crystal structure of LiNaCo{sub 0.5}Fe{sub 0.5}PO{sub 4}F was refined based on NPD and validated by ED and HRTEM. • LiNaCo{sub 0.5}Fe{sub 0.5}PO{sub 4}F demonstrated a reversible Li de/intercalation in the 2.5÷4.6 V vs Li/Li{sup +} range.

  12. Component mode synthesis in structural dynamics

    International Nuclear Information System (INIS)

    Reddy, G.R.; Vaze, K.K.; Kushwaha, H.S.

    1993-01-01

    In seismic analysis of Nuclear Reactor Structures and equipments eigen solution requires large computer time. Component mode synthesis is an efficient technique with which one can evaluate dynamic characteristics of a large structure with minimum computer time. Due to this reason it is possible to do a coupled analysis of structure and equipment which takes into account the interaction effects. Basically in this the method large size structure is divided into small substructures and dynamic characteristics of individual substructure are determined. The dynamic characteristics of entire structure are evaluated by synthesising the individual substructure characteristics. Component mode synthesis has been applied in this paper to the analysis of a tall heavy water upgrading tower. Use of fixed interface normal modes, constrained modes, attachment modes in the component mode synthesis using energy principle and using Ritz vectors have been discussed. The validity of this method is established by solving fixed-fixed beam and comparing the results obtained by conventional and classical method. The eigen value problem has been solved using simultaneous iteration method. (author)

  13. Synthesis, structural and spectroscopic properties of acentric triple molybdate Cs{sub 2}NaBi(MoO{sub 4}){sub 3}

    Energy Technology Data Exchange (ETDEWEB)

    Savina, A.A. [Laboratory of Oxide Systems, Baikal Institute of Nature Management, SB RAS, Ulan-Ude 670047 (Russian Federation); Department of Chemistry, Buryat State University, Ulan-Ude 670000 (Russian Federation); Atuchin, V.V., E-mail: atuchin@isp.nsc.ru [Laboratory of Optical Materials and Structures, Rzhanov Institute of Semiconductor Physics, SB RAS, Novosibirsk 630090 (Russian Federation); Functional Electronics Laboratory, Tomsk State University, Tomsk 634050 (Russian Federation); Laboratory of Semiconductor and Dielectric Materials, Novosibirsk State University, Novosibirsk 630090 (Russian Federation); Solodovnikov, S.F. [Laboratory of Crystal Chemistry, Nikolaev Institute of Inorganic Chemistry, SB RAS, Novosibirsk 630090 (Russian Federation); Department of Natural Sciences, Novosibirsk State University, Novosibirsk 630090 (Russian Federation); Solodovnikova, Z.A. [Laboratory of Crystal Chemistry, Nikolaev Institute of Inorganic Chemistry, SB RAS, Novosibirsk 630090 (Russian Federation); Krylov, A.S. [Laboratory of Molecular Spectroscopy, Kirensky Institute of Physics, SB RAS, Krasnoyarsk 660036 (Russian Federation); Maximovskiy, E.A. [Laboratory of Epitaxial Layers, Nikolaev Institute of Inorganic Chemistry, SB RAS, Novosibirsk 630090 (Russian Federation); Laboratory of Research Methods of Composition and Structure of Functional Materials, Novosibirsk State University, Novosibirsk 630090 (Russian Federation); Molokeev, M.S. [Laboratory of Crystal Structure, Kirensky Institute of Physics, SB RAS, Krasnoyarsk 660036 (Russian Federation); Oreshonkov, A.S [Laboratory of Molecular Spectroscopy, Kirensky Institute of Physics, SB RAS, Krasnoyarsk 660036 (Russian Federation); Department of Photonics and Laser Technology, Siberian Federal University, Krasnoyarsk 660079 (Russian Federation); Pugachev, A.M. [Laboratory of Condenced Matter Spectroscopy, Institute of Automation and Electrometry, SB RAS, Novosibirsk 90, 630090 (Russian Federation); and others

    2015-05-15

    New ternary molybdate Cs{sub 2}NaBi(MoO{sub 4}){sub 3} is synthesized in the system Na{sub 2}MoO{sub 4}–Cs{sub 2}MoO{sub 4}–Bi{sub 2}(MoO{sub 4}){sub 3}. The structure of Cs{sub 2}NaBi(MoO{sub 4}){sub 3} of a new type is determined in noncentrosymmetric space group R3c, a=10.6435(2), c=40.9524(7) Å, V=4017.71(13) Å{sup 3}, Z=12 in anisotropic approximation for all atoms taking into account racemic twinning. The structure is completely ordered, Mo atoms are tetrahedrally coordinated, Bi(1) and Bi(2) atoms are in octahedra, and Na(1) and Na(2) atoms have a distorted trigonal prismatic coordination. The Cs(1) and Cs(2) atoms are in the framework cavities with coordination numbers 12 and 10, respectively. No phase transitions were found in Cs{sub 2}NaBi(MoO{sub 4}){sub 3} up to the melting point at 826 K. The compound shows an SHG signal, I{sub 2w}/I{sub 2w}(SiO{sub 2})=5 estimated by the powder method. The vibrational properties are evaluated by Raman spectroscopy, and 26 narrow lines are measured. - Graphical abstract: - Highlights: • The crystal structure of Cs{sub 2}NaBi(MoO{sub 4}){sub 3} is defined. • The molybdate Cs{sub 2}NaBi(MoO{sub 4}){sub 3} is stable up to melting point at 826 K. • Vibrational properties of Cs{sub 2}NaBi(MoO{sub 4}){sub 3} are evaluated by Raman spectroscopy.

  14. Synthesis, crystal structure, electrical properties, and sodium transport pathways of the new arsenate Na{sub 4}Co{sub 7}(AsO{sub 4}){sub 6}

    Energy Technology Data Exchange (ETDEWEB)

    Ben Smida, Youssef; Marzouki, Riadh [Université de Tunis El Manar, Laboratoire de Matériaux et Cristallochimie, Faculté des Sciences de Tunis, Campus Universitaire, 2092 Manar II, Tunis (Tunisia); Georges, Samuel [Université Grenoble Alpes, Laboratoire d’Electrochimie et de Physicochimie des Matériaux et des Interfaces LEPMI, F-38000 Grenoble (France); Kutteh, Ramzi [Bragg Institute, Australian Nuclear Science and Technology Organisation (ANSTO), New Illawarra Road, Lucas Heights, New South Wales 2234 (Australia); Avdeev, Maxim [Bragg Institute, Australian Nuclear Science and Technology Organisation (ANSTO), New Illawarra Road, Lucas Heights, New South Wales 2234 (Australia); School of Chemistry, University of Sydney, Sydney, New South Wales 2006 (Australia); Guesmi, Abderrahmen; Zid, Mohamed Faouzi [Université de Tunis El Manar, Laboratoire de Matériaux et Cristallochimie, Faculté des Sciences de Tunis, Campus Universitaire, 2092 Manar II, Tunis (Tunisia)

    2016-07-15

    A new sodium cobalt (II) arsenate Na{sub 4}Co{sub 7}(AsO{sub 4}){sub 6} has been synthesized by a solid-state reaction and its crystal structure determined from single crystal X-ray diffraction data. It crystallizes in the monoclinic system, space group C2/m, with a=10.7098(9) Å, b=14.7837(9) Å, c=6.6845(7) Å, and β=105.545(9)°. The structure is described as a three-dimensional framework built up of corner-edge sharing CoO{sub 6}, CoO{sub 4} and AsO{sub 4} polyhedra, with interconnecting channels along [100] in which the Na{sup +} cations are located. The densest ceramics with relative density of 94% was obtained by ball milling and optimization of sintering temperature, and its microstructure characterized by scanning electron microscopy. The electrical properties of the ceramics were studied over a temperature interval from 280 °C to 560 °C using the complex impedance spectroscopy over the range of 13 MHz–5 Hz. The ionic bulk conductivity value of the sample at 360 °C is 2.51 10{sup −5} S cm{sup −1} and the measured activation energy is Ea=1 eV. The sodium migration pathways in the crystal structure were investigated computationally using the bond valence site energy (BVSE) model and classical molecular dynamics (MD) simulations. - Graphical abstract: Correlation between crystal structure, microstructure and ionic conductivity . Display Omitted - Highlights: • A new arsenate Na{sub 4}Co{sub 7}(AsO{sub 4}){sub 6} was prepared by solid state reaction. • Its crystal structure was determined by powder X-ray diffraction. • Na{sup +} ionic conductivity was probed by complex impedance spectroscopy. • Na{sup +} conduction pathways were modeled by bond-valence method and molecular dynamics.

  15. Synthesis and conformational properties of oligonucleotides incorporating 2'-O-phosphorylated ribonucleotides as structural motifs of pre-tRNA splicing intermediates.

    Science.gov (United States)

    Tsuruoka, H; Shohda, K; Wada, T; Sekine, M

    2000-11-03

    To synthesize oligonucleotides containing 2'-O-phosphate groups, four kinds of ribonucleoside 3'-phosphoramidite building blocks 6a-d having the bis(2-cyano-1,1-dimethylethoxy)thiophosphoryl (BCMETP) group were prepared according to our previous phosphorylation procedure. These phosphoramidite units 6a-d were not contaminated with 3'-regioisomers and were successfully applied to solid-phase synthesis to give oligodeoxyuridylates 15, 16 and oligouridylates 21, 22. Self-complementary Drew-Dickerson DNA 12mers 24-28 replaced by a 2'-O-phosphorylated ribonucleotide at various positions were similarly synthesized. In these syntheses, it turned out that KI(3) was the most effective reagent for oxidative desulfurization of the initially generated thiophosphate group to the phosphate group on polymer supports. Without using this conversion step, a tridecadeoxyuridylate 17 incorporating a 2'-O-thiophosphorylated uridine derivative was also synthesized. To investigate the effect of the 2'-phosphate group on the thermal stability and 3D-structure of DNA(RNA) duplexes, T(m) measurement of the self-complementary oligonucleotides obtained and MD simulation of heptamer duplexes 33-36 were carried out. According to these analyses, it was suggested that the nucleoside ribose moiety phosphorylated at the 2'-hydroxyl function predominantly preferred C2'-endo to C3'-endo conformation in DNA duplexes so that it did not significantly affect the stability of the DNA duplex. On the other hand, the 2'-modified ribose moiety was expelled to give a C3'-endo conformation in RNA duplexes so that the RNA duplexes were extremely destabilized.

  16. Synthesis, structural characterization and selectively catalytic properties of metal-organic frameworks with nano-sized channels: A modular design strategy

    International Nuclear Information System (INIS)

    Qiu Lingguang; Gu Lina; Hu Gang; Zhang Lide

    2009-01-01

    Modular design method for designing and synthesizing microporous metal-organic frameworks (MOFs) with selective catalytical activity was described. MOFs with both nano-sized channels and potential catalytic activities could be obtained through self-assembly of a framework unit and a catalyst unit. By selecting hexaaquo metal complexes and the ligand BTC (BTC=1,3,5-benzenetricarboxylate) as framework-building blocks and using the metal complex [M(phen) 2 (H 2 O) 2 ] 2+ (phen=1,10-phenanthroline) as a catalyst unit, a series of supramolecular MOFs 1-7 with three-dimensional nano-sized channels, i.e. [M 1 (H 2 O) 6 ].[M 2 (phen) 2 (H 2 O) 2 ] 2 .2(BTC).xH 2 O (M 1 , M 2 =Co(II), Ni(II), Cu(II), Zn(II), or Mn(II), phen=1,10-phenanthroline, BTC=1,3,5-benzenetricarboxylate, x=22-24), were synthesized through self-assembly, and their structures were characterized by IR, elemental analysis, and single-crystal X-ray diffraction. These supramolecular microporous MOFs showed significant size and shape selectivity in the catalyzed oxidation of phenols, which is due to catalytic reactions taking place in the channels of the framework. Design strategy, synthesis, and self-assembly mechanism for the construction of these porous MOFs were discussed. - Grapical abstract: A modular design strategy has been developed to synthesize microporous metal-organic frameworks with potential catalytic activity by self-assembly of the framework-building blocks and the catalyst unit

  17. Synthesis, crystal structures, and optical properties of the π-π interacting pyrrolo[2,3-b]quinoxaline derivatives containing 2-thienyl substituent

    Science.gov (United States)

    Goszczycki, Piotr; Stadnicka, Katarzyna; Brela, Mateusz Z.; Grolik, Jarosław; Ostrowska, Katarzyna

    2017-10-01

    Three (E/Z)-diastereoisomers, based on pyrrolo[2,3-b]quinoxaline system as fluorophore and containing: 2-thienylmethyl (1), bis(2-thienylmethyl)-2-aminoethyl (3a), bis(2-thienylmethyl)-3-aminopropyl (3b) groups as substituents, were synthesized and characterized by X-ray structural analysis, PXRD, NMR, UV-Vis as well as fluorescence. These compounds are non-fluorescent in acetonitrile solution, however, they exhibit aggregation induced emission enhancement (AIEE) upon water addition and in solid state. X-ray structural analysis revealed that molecules with 2-thienylmethyl and bis(2-thienylmethyl)-2-aminoethyl groups form dimers and π-stacks through π-π interactions between anitiparallel oriented pyrroloquinoxaline cores with interplanar distances 3.45 Å and 3.20 Å, respectively. Conformation of bis(2-thienylmethyl)-3-aminopropyl group is imposed by incorporated DMSO-d6 solvent molecule and weak intermolecular S-π and CH-π interactions, that prevents π-π interaction between fluorophore cores. The correlation between crystal structure and fluorescent properties of synthesized molecules was discussed. The DFT calculations were performed to rationalize the differences between considered systems.

  18. Synthesis and structure of a new layered oxyfluoride Sr{sub 2}ScO{sub 3}F with photocatalytic property

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Yongkun; Tang, Kaibin, E-mail: kbtang@ustc.edu.cn; Zhu, Baichuan; Wang, Dake; Hao, Qiaoyan; Wang, Yan

    2015-05-15

    Highlights: • A new oxyfluoride compound Sr{sub 2}ScO{sub 3}F was prepared by a solid state route. • The structure of this compound was determined by GSAS program based on XRD data. • The photocatalytic property was investigated under UV irradiation. - Abstract: A new Ruddlesden–Popper type scandium oxyfluoride, Sr{sub 2}ScO{sub 3}F, was synthesized by a conventional solid state reaction route. The detailed structure of Sr{sub 2}ScO{sub 3}F was investigated using X-ray diffraction (XRD) and selected area electron diffraction (SAED). The disorder distribution pattern of fluorine anions was determined by the {sup 19}F nuclear magnetic resonance (NMR) spectrum. The compound crystallizes in a K{sub 2}NiF{sub 4}-type tetragonal structure (space group I4/mmm) with O/F anions disordered over the apical sites of the perovskite-type Sc(O,F){sub 6} octahedron layers interleaved with strontium cations. Ultraviolet–visible (UV–vis) diffuse reflection spectrum of the prepared Sr{sub 2}ScO{sub 3}F indicates that it has an absorption in the UV–vis region. The photocatalytic activity of Sr{sub 2}ScO{sub 3}F was further investigated, showing an effective photodegradation of Rhodamine-B (RB) within 2 h under UV light irradiation.

  19. Materials by design--exploiting the unique properties of pulsed laser deposition for the synthesis of novel hard materials and structures

    International Nuclear Information System (INIS)

    Willmott, P.R.; Spillmann, H.

    2002-01-01

    Novel multilayer thin film structures with an (A-B-C-B) four-sublayer periodicity were synthesized using pulsed reactive crossed-beam laser ablation. The layers were based on transition metal carbonitrides in which one sublayer (A=TiC x N 1-x ) was optimized for its high hardness, another (C=ZrC x N 1-x ) for its low frictional properties, and a third (B=VC x N 1-x ) which acted as a barrier to dislocation propagation. Control of growth and stoichiometry was facilitated by using thermally stable gases as sources for the carbon and nitrogen which were activated by collisions with the ablation plasma. It was discovered that the ablation yields of Ti, V, and Zr were almost identical, so that the sublayer thickness was directly proportional to the number of ablated shots per sublayer metal. The four-sublayer structures were harder (H-bar=35 GPa) than corresponding bilayer structures (H-bar=30 GPa) in which the VC x N 1-x sublayers were missing. Further improvements are expected by optimizing the sublayer ratios and the absolute period thickness

  20. Synthesis, structure, and electrochemistry and magnetic properties of a novel 1D homochiral MnIII(5-Brsalen) coordination polymer with left-handed helical character

    Science.gov (United States)

    Dong, Dapeng; Yu, Naisen; Zhao, Haiyan; Liu, Dedi; Liu, Jia; Li, Zhenghua; Liu, Dongping

    2016-01-01

    A novel homochiral manganese (III) Mn(5-Brsalen) coordination polymer with left-handed helical character by spontaneous resolution on crystallization by using Mn(5-Brsalen) and 4,4-bipyridine, [MnIII(5-Brsalen)(4,4-bipy)]·ClO4·CH3OH (1) (4,4-bipy = 4,4-bipyridine) has been synthesized and structurally characterized by X-ray single-crystal diffraction, elemental analysis and infrared spectroscopy. In compound 1, each manganese(III) anion is six-coordinate octahedral being bonded to four atoms of 5-Brsalen ligand in an equatorial plane and two nitrogen atoms from a 4,4-bipyridine ligand in axial positions. The structure of compound 1 can be described a supramolecular 2D-like structure which was formed by the intermolecular π-stacking interactions between the neighboring chains of the aromatic rings of 4,4-bipyridine and 5-Brsalen molecules. UV-vis absorption spectrum, electrochemistry and magnetic properties of the compound 1 have also been studied.

  1. Magnetically frustrated double perovskites: synthesis, structural properties, and magnetic order of Sr{sub 2}BOsO{sub 6} (B = Y, In, Sc)

    Energy Technology Data Exchange (ETDEWEB)

    Paul, Avijit Kumar; Sarapulova, Angelina; Adler, Peter; Kanungo, Sudipta; Mikhailova, Daria; Schnelle, Walter; Hu, Zhiwei; Kuo, Changyang; Yan, Binghai; Felser, Claudia; Tjeng, Liu Hao [Max-Planck-Institut fuer Chemische Physik fester Stoffe,Dresden (Germany); Reehuis, Manfred [Helmholtz-Zentrum Berlin fuer Materialien und Energie, Berlin (Germany); Siruguri, Vasudeva; Rayaprol, Sudhindra [UGC-DAE Consortium for Scientific Research (CSR), Mumbai Centre, Mumbai (India); Soo, Yunlian [Department of Physics, National Tsing Hua University, Hsinchu (China); Jansen, Martin [Max-Planck-Institut fuer Chemische Physik fester Stoffe,Dresden (Germany); Max-Planck-Institut fuer Festkoerperforschung, Stuttgart (Germany)

    2015-02-15

    Double perovskites Sr{sub 2}BOsO{sub 6} (B = Y, In, and Sc) were prepared from the respective binary metal oxides, and their structural, magnetic, and electronic properties were investigated. At room temperature all these compounds crystallize in the monoclinic space group P2{sub 1}/n. They contain magnetic osmium (Os{sup 5+}, t{sub 2g}{sup 3}) ions and are antiferromagnetic insulators with Neel temperatures T{sub N} = 53 K, 26 K, and 92 K for B = Y, In, and Sc, respectively. Powder neutron diffraction studies on Sr{sub 2}YOsO{sub 6} and Sr{sub 2}InOsO{sub 6} showed that the crystal structures remain unchanged down to 3 K. The Y and In compounds feature a type I antiferromagnetic spin structure with ordered Os moments of 1.91 μ{sub B} and 1.77 μ{sub B}, respectively. The trend in T{sub N} does not simply follow the development of the lattice parameters, which suggests that d{sup 0} compared to d{sup 10} ions on the B site favor a somewhat different balance of exchange interactions in the frustrated Os{sup 5+} fcc-like lattice. (Copyright copyright 2015 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  2. Structural Properties of Ferroelectric Perovskites

    National Research Council Canada - National Science Library

    Vanderbilt, David

    1998-01-01

    Under this research grant, we carried out realistic first-principles computer calculations of the ground-state and finite-temperature structural and dielectric properties of cubic perovskite materials...

  3. Controllable synthesis of Ln3+ (Ln = Tb, Eu) doped zinc phosphate nano-/micro-structured materials: phase, morphology and luminescence properties

    Science.gov (United States)

    Yue, Dan; Lu, Wei; Li, Chunyang; Zhang, Xinlei; Liu, Chunxia; Wang, Zhenling

    2014-01-01

    Ln3+ (Ln = Tb, Eu) doped zinc phosphate tetrahydrate (ZPT:Ln3+) and ammonium zinc phosphate (AZP:Ln3+) nano-/micro-structured materials were synthesized in aqueous solution without the addition of any structure-directing agent. The phase structures, morphologies and luminescence properties of the as-synthesized samples were investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), transmission electron microscopy (TEM), photoluminescence (PL) spectroscopy and lifetime. These investigations indicate that different phosphate sources MnH(3-n)PO4 (M = NH4+ or Na+, n = 1, 2, 3) can lead to the altering of morphology from nanosheet to microflower, but have no significant effect on the phase structure of the samples. The microlump, nanosheet, and microflower (constructed by the primary microlumps or nanosheets) of orthorhombic ZPT:Ln3+ could be selectively prepared by adjusting the pH value from 3.5 to 7.0. A mixture of orthorhombic ZPT:Ln3+ and monoclinic AZP:Ln3+ with a microflower morphology was obtained when the pH value was adjusted to 8.0. Monoclinic AZP:Ln3+ microplate, microcube and nanoparticle morphologies were obtained at pH values of 8.5, 9.0 and 11.0 respectively. The phase transformation and growth mechanism of the diverse morphologies were proposed, and ZPT:Ln3+ (Ln3+ = Eu or Tb) samples exhibit red or green emission under the excitation of UV light.Ln3+ (Ln = Tb, Eu) doped zinc phosphate tetrahydrate (ZPT:Ln3+) and ammonium zinc phosphate (AZP:Ln3+) nano-/micro-structured materials were synthesized in aqueous solution without the addition of any structure-directing agent. The phase structures, morphologies and luminescence properties of the as-synthesized samples were investigated by X-ray diffraction (XRD), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), transmission electron microscopy (TEM), photoluminescence (PL) spectroscopy and lifetime. These

  4. Metal-organic and supramolecular networks driven by 5-chloronicotinic acid: Hydrothermal self-assembly synthesis, structural diversity, luminescent and magnetic properties

    Energy Technology Data Exchange (ETDEWEB)

    Gao, Zhu-Qing, E-mail: zqgao2008@163.com [School of Chemical and Biological Engineering, Taiyuan University of Science and Technology, Taiyuan 030021 (China); Li, Hong-Jin [School of Chemical and Biological Engineering, Taiyuan University of Science and Technology, Taiyuan 030021 (China); Gu, Jin-Zhong, E-mail: gujzh@lzu.edu.cn [College of Chemistry and Chemical Engineering, Lanzhou University, Lanzhou 730000 (China); Zhang, Qing-Hua [School of Chemical and Biological Engineering, Taiyuan University of Science and Technology, Taiyuan 030021 (China); Kirillov, Alexander M. [Centro de Química Estrutural, Complexo I, Instituto Superior Técnico, Universidade de Lisboa, Av. Rovisco Pais, 1049–001 Lisbon (Portugal)

    2016-09-15

    Four new crystalline solids, namely [Co{sub 2}(µ{sub 2}-5-Clnic){sub 2}(µ{sub 3}-5-Clnic){sub 2}(µ{sub 2}-H{sub 2}O)]{sub n} (1), [Co(5-Clnic){sub 2}(H{sub 2}O){sub 4}]·2(5-ClnicH) (2), [Pb(µ{sub 2}-5-Clnic){sub 2}(phen)]{sub n} (3), and [Cd(5-Clnic){sub 2}(phen){sub 2}]·3H{sub 2}O (4) were generated by hydrothermal self-assembly methods from the corresponding metal(II) chlorides, 5-chloronicotinic acid (5-ClnicH) as a principal building block, and 1,10-phenanthroline (phen) as an ancillary ligand (optional). All the products 1–4 were characterized by IR spectroscopy, elemental analysis, thermogravimetric (TGA), powder X-ray diffraction (PXRD) and single-crystal X-ray diffraction. Their structures range from an intricate 3D metal-organic network 1 with the 3,6T7 topology to a ladder-like 1D coordination polymer 3 with the 2C1 topology, whereas compounds 2 and 4 are the discrete 0D monomers. The structures of 2 and 4 are further extended (0D→2D or 0D→3D) by hydrogen bonds, generating supramolecular networks with the 3,8L18 and ins topologies, respectively. Synthetic aspects, structural features, thermal stability, magnetic (for 1) and luminescent (for 3 and 4) properties were also investigated and discussed. - Graphical abstract: A new series of crystalline solids was self-assembled and fully characterized; their structural, topological, luminescent and magnetic features were investigated. Display Omitted.

  5. Synthesis, structure and two-photon absorption properties of a new multi-branched compound, 1,2,4,5-tetrakis(4-pyridylvinyl)benzene

    International Nuclear Information System (INIS)

    Wang Lei; Tao Xutang; Yang Jiaxiang; Yu Wentao; Ren Yan; Xin Qian; Liu Zhi; Jiang Minhua

    2004-01-01

    A conjugated and symmetric multi-branched compound, 1,2,4,5-tetrakis(4-pyridylvinyl)benzene (TKPVB), has been synthesized and the crystal structures of TKPVB and its intermediate, 1,2,4,5-tetrakis(dimethoxyphosphorylmethyl)benzene, were determined by diffraction method. TKPVB with four units of 4-vinylpyridine moieties attached to the central benzene core presents an A-π-A general framework, where A is a π-deficient pyridine ring. The single-photon and two-photon absorption and fluorescence properties in different solvents of varying polarity have been investigated. It is also found that the one- and two-photon-induced fluorescence spectra are quite similar, which indicate that the one- and two-photon allowed-excited states are the same

  6. Synthesis of nanoparticles of manganese MnFe2O4 by co-precipitation micellar ferrite: structural and magnetic properties

    International Nuclear Information System (INIS)

    Alvarez-Paneque, A.; Diaz, S.; Diaz, C.; Santiago-Jacinto, E.; Reguera, E.

    2008-01-01

    Full text: The microemulsion method was used in reverse, shaped micelles by dodecyl of sodium (NaDBS) in toluene/water system, for MnFe2O4 manganese ferrite magnetic nanoparticles. Were also variants of heat treatments to improve the crystallinity of the material obtained. These were, treatments to reflux to 100 ° C or treatments in an inert atmosphere at temperatures that were varied between 350 and 600 ° C. The retrieved material was characterized by x-ray diffraction (XRD), transmission electron microscopy of high and low resolution (HR-TEM and TEM, respectively), Mössbauer Spectroscopy and vibrational magnetometry. Powder XRD patterns revealed the formation of phase MnFe2O4, cubic type Spinel, of space group Fd3m, accompanied by the minority phase Hematite (a-Fe203) group spatial R-3 c. The size of the nanoparticles was estimated from the profile setting from the pattern of powder by the method of Le Bail, obtaining sizes mean that varied between 5 and 25 mn depending on the heat treatment to which they were subjected. This result was corroborated from TEM micrographs. The vibrational magnetometer showed that the smaller MnFe2O4 nanoparticles, prepared following this route of synthesis They presented a superparamagnetic behavior at room temperature (coercive field and) remanence approximately zeros), which was also confirmed by the study of Mössbauer Spectroscopy. Was also the magnetically inactive layer thickness, of around 0.9 nm, responsible for the decrease in the values of saturation magnetization (as) to decrease the size of nanoparticles. Was obtained a set of nanoparticles with superparamagnetic behavior based in the MnFe2O4 around 5.9 NM in diameter and a-Fe203 around 6.6 NM, as phase secondary. They managed to get this material and the desired magnetic properties optimum crystallinity, applying heat treatment variant proposed in this work, and that It consists of making a reflux at 100 ° C, before the treatment on solid phase under flow N2

  7. Synthesis, crystal structures, and luminescent properties of Cd(II) coordination polymers assembled from semi-rigid multi-dentate N-containing ligand

    Energy Technology Data Exchange (ETDEWEB)

    Yuan, Gang; Shao, Kui-Zhan; Chen, Lei; Liu, Xin-Xin [Institute of Functional Material Chemistry, Faculty of Chemistry, Northeast Normal University, Changchun 130024, Jilin (China); Su, Zhong-Min, E-mail: zmsu@nenu.edu.cn [Institute of Functional Material Chemistry, Faculty of Chemistry, Northeast Normal University, Changchun 130024, Jilin (China); Ma, Jian-Fang [Institute of Functional Material Chemistry, Faculty of Chemistry, Northeast Normal University, Changchun 130024, Jilin (China)

    2012-12-15

    Three new polymers, [Cd(L){sub 2}(H{sub 2}O){sub 2}]{sub n} (1), [Cd{sub 3}(L){sub 2}({mu}{sub 3}-OH){sub 2}({mu}{sub 2}-Cl){sub 2}(H{sub 2}O){sub 2}]{sub n} (2), {l_brace}[Cd{sub 2}(L){sub 2}(nic){sub 2}(H{sub 2}O){sub 2}]{center_dot}H{sub 2}O{r_brace}{sub n} (3) (HL=5-(4-((1H-1,2,4-triazol-1-yl)methyl)phenyl)-1H-tetrazole, Hnic=nicotinic acid) have been prepared and structurally characterized. Compounds 1 and 2 display 2D monomolecular layers built by the inter-linking single helical chains and L{sup -} ligands connecting chain-like [Cd({mu}{sub 3}-OH)({mu}{sub 2}-Cl)]{sub n} secondary building units, respectively. Compound 3 is constructed from the mixed ligands and possesses a (3,4)-connected framework with (4{center_dot}8{sup 2})(4{center_dot}8{sup 2}{center_dot}10{sup 3}) topology. Moreover, the fluorescent properties of HL ligand and compounds 1-3 are also been investigated. - Graphical abstract: Three new coordination polymers based on the semi-rigid multidentate N-donor ligand have been successfully synthesized by hydrothermal reaction. Complexes 1 and 2 exhibit the 2D layers formed by inter-linking single helices and L{sup -} anions bridging 1D chain-like SBUs, respectively. Complex 3 is buit by L{sup -} and assistant nic{sup -} ligands connecting metal centers and possesses a (3,4)-connected framework with (4 Multiplication-Sign 8{sup 2})(4 Multiplication-Sign 8{sup 2} Multiplication-Sign 10{sup 3}) topology. Moreover, these complexes display fluorescent properties indicating that they may have potential applications as optical materials. Highlights: Black-Right-Pointing-Pointer Three Cd-compounds were prepared from semi-rigid HL ligand with different N-containing groups. Black-Right-Pointing-Pointer They exhibit diverse structures from 2D monomolecular layer to 3D covalent framework. Black-Right-Pointing-Pointer The HL ligands displayed various coordination modes under different reaction conditions. Black-Right-Pointing-Pointer These compounds exhibit

  8. 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.

  9. Synthesis, structure, and luminescence properties of SrSiAl2O3N2:Eu(2+) phosphors for light-emitting devices and field emission displays.

    Science.gov (United States)

    Wang, Xicheng; Zhao, Zhengyan; Wu, Quansheng; Li, Yanyan; Wang, Chuang; Mao, Aijun; Wang, Yuhua

    2015-06-28

    A series of SrSiAl2O3N2:Eu(2+) (0.005 ≤x≤ 0.05) phosphors were successfully synthesized through a pressureless, facile, and efficient solid state route. The crystal structure, band structure, and their photoluminescence and cathodoluminescence properties were investigated in detail. The phosphors exhibit rod shape morphology with a uniform Eu(2+) distribution. Under n-UV excitation the emission spectra shift from 477 to 497 nm with an increase of Eu(2+) concentration. The concentration quenching mechanism of Eu(2+) emission was dominated by the dipole-dipole interaction. The thermal stability is comparable to that of the commercial Ba2SiO4:Eu(2+) phosphor. The phosphor also exhibits high current saturation and high resistance under low voltage electron bombardment. All the results indicate that the SrSiAl2O3N2:Eu(2+) phosphors can be considered as candidates for application in both white LEDs and FEDs.

  10. Synthesis and photoluminescence properties of Sm{sup 3+}substituted glaserite-type orthovanadates K{sub 3}Y[VO{sub 4}]{sub 2} with monoclinic structure

    Energy Technology Data Exchange (ETDEWEB)

    Duke John David, A., E-mail: dukejohndavid02@gmail.com [Voorhees College, Vellore, Tamil Nadu (India); Muhammad, G. Shakil [Islamiah College, Vaniyambadi, Tamil Nadu (India); Sivakumar, V. [National Institute of Technology (NIT), Rourkela (India)

    2016-09-15

    A novel phosphor of Glaserite type Orthovanadate K{sub 3}Y[VO{sub 4}]{sub 2} substituted with the trivalent rare-earth Sm{sup 3+} ions were synthesized by the conventional high temperature solid-state reaction method, their structural characterization and photoluminescent properties were investigated by X-ray diffraction and spectrofluorimetry. The phase-purity of glaserite structure in the synthesized compound was verified by XRD study. The morphology was measured by FESEM. Host lattice emits broad-band green color and it is originated from the [VO{sub 4}]{sup 3−}. Photoluminescence studies of Sm{sup 3+} activated samples show orange red emission. The charge transfer behaviours from [VO{sub 4}]{sup 3−} to Sm{sup 3+} ions (host to activator) in K{sub 3}Y{sub (1−x)}[VO{sub 4}]{sub 2}: {sub x}Sm{sup 3+} phosphors have been confirmed by photoluminescence and PL decay life time measurement. No concentration quenching was observed even for higher concentration of the dopant Sm{sup 3+} ions. The CIE chromaticity color coordinate values were calculated and it is very much closer to the NTSC standards. All the results clearly indicate that self-activated K{sub 3}Y{sub 1−x}[VO{sub 4}]{sub 2} with the rare earth {sub x}Sm{sup 3+} activated phosphors show great potential as a phosphor material for near-UV based white LEDs.

  11. Effect of reduction enhancer on a radiolytic synthesis of carbon-supported Pt–Cu nanoparticles and their structural and electrochemical properties

    Energy Technology Data Exchange (ETDEWEB)

    Kugai, Junichiro, E-mail: jkugai@kobe-kosen.ac.jp [Kobe City College of Technology, Department of Applied Chemistry (Japan); Kubota, Chihiro; Okazaki, Tomohisa; Seino, Satoshi; Nakagawa, Takashi [Osaka University, Graduate School of Engineering (Japan); Nitani, Hiroaki [High Energy Accelerator Research Organization, Institute of Materials Structure Science (IMSS) (Japan); Yamamoto, Takao A. [Osaka University, Graduate School of Engineering (Japan)

    2015-06-15

    In order to clarify the effect of reduction enhancer on the nanoparticle formation process and their structural and catalytic properties, carbon-supported Pt–Cu nanoparticles were synthesized by electron beam irradiation on an aqueous precursor solution in the presence/absence of reduction enhancer. In the absence of reduction enhancer, tetravalent platinum oxide particles of approximately 1 nm in diameter were formed on carbon support with copper barely precipitated, while in the presence of 2-propanol or ethylene glycol or glucose both platinum and copper precipitated as few-nanometer-sized alloy particles together with copper oxides. It was suggested that the metal nuclei produced upon electron beam irradiation do not have enough lifetime without reduction enhancer due to fast oxidation of the nuclei by oxidizing radicals, while the reduction enhancer scavenges these oxidizing radicals preventing oxidation of metallic clusters and prolonging their lifetime. Ethylene glycol gave smaller and better alloyed particles with less copper oxides compared to 2-propanol since the carbonyl compounds derived from oxidation of ethylene glycol protect metallic clusters from oxidation further prolonging their lifetime. In the electrochemical measurements, the methanol oxidation activities of Pt–Cu/C catalysts were well explained by their structural characteristics.

  12. Synthesis, structures and properties of Cu(II) and Mn(II) complexes with 1,10-phenanthroline-2-carboxylic acid and 2,2'-bipyridine ligands.

    Science.gov (United States)

    Sun, Jingya; Xu, Huanzhi

    2010-11-15

    Four new 2,2'-bipyridine and 1,10-phenanthroline complexes, namely [Mn(phenca)(2)]·(H(2)O)(2) (1), [Cu(4)(phen)(4)(OH-)(4)(H(2)O)(2)](DMF)(4)(ClO(4)-)(4)(H(2)O) (2), [Cu(2)(2,2-bipy)(2)(C(2)O(4)2-)(H(2)O)(2)(NO(3))(2)] (3) and [Cu(2,2-bipy)(2)(ClO(4)-)](ClO(4)-) (4) (2,2'-bpy = 2,2'-bipyridine, Hphenca = 1,10-phenanthroline-2-carboxylic acid) have been synthesized by a hydrothermal reaction. The products were characterized by elemental analysis, infrared spectroscopy and X-ray crystal diffraction. While strong hydrogen bonds play central roles in the formation of the 3D structure, the combined influence of the weak interactions such as π···π interactions is also evident in the structures. A preliminary investigation on the ion exchange properties of the complexes is presented.

  13. Synthesis and luminescent properties of CaCO3:Eu3+@SiO2 phosphors with core-shell structure

    Science.gov (United States)

    Liu, Min; Kang, Ming; Chen, Kexu; Mou, Yongren; Sun, Rong

    2018-03-01

    Integrating the processes of preparation of CaCO3:Eu3+ and its surface-coating, core-shell structured CaCO3:Eu3+@SiO2 phosphors with red emission were synthesized by the carbonation method and surface precipitation procedure using sodium silicate as silica source. The phase structure, thermal stability, morphology and luminescent property of the as-synthesized samples were characterized by X-ray diffraction, Fourier transform infrared spectrum, thermal analysis, field-emission scanning electron microscopy, transmission electron microscope and photoluminescence spectra. The experimental results show that Eu3+ ions as the luminescence center are divided into two types: one is at the surface of the CaCO3 and the other inhabits the site of Ca2+. For CaCO3:Eu3+@SiO2 phosphors, the SiO2 layers are continuously coated on the surface of CaCO3:Eu3+ and show a typical core-shell structure. After coated with SiO2 layer, the luminous intensity and the compatibility with the rubber matrix increase greatly. Additionally, the luminous intensity increases with the increasing of Eu3+ ions concentration in CaCO3 core and concentration quenching occurs when Eu3+ ions concentration exceeds 7.0 mol%, while it is 5.0 mol% for CaCO3:Eu3+ phosphors. Therefore, preparation of CaCO3:Eu3+@SiO2 phosphors can not only simplify the experimental process through integrating the preparation of CaCO3:Eu3+ and SiO2 layer, but also effectively increase the luminous intensities of CaCO3:Eu3+ phosphors. The as-obtained phosphors may have potential applications in the fields of optical materials and functional polymer composite materials, such as plastics and rubbers.

  14. A two-dimensional zinc(II) coordination polymer based on mixed dimethyl succinate and bipyridine ligands: synthesis, structure, thermostability and luminescence properties.

    Science.gov (United States)

    Liu, Yang; Feng, Yong Lan; Fu, Wei Wei

    2016-04-01

    From the viewpoint of crystal engineering, the construction of crystalline polymeric materials requires a rational choice of organic bridging ligands for the self-assembly process. Multicarboxylate ligands are of particular interest due to their strong coordination activity towards metal ions, as well as their various coordination modes and versatile conformations. The structural chemistry of dicarboxylate-based coordination polymers of transition metals has been developed through the grafting of N-containing organic linkers into carboxylate-bridged transition metal networks. A new luminescent two-dimensional zinc(II) coordination polymer containing bridging 2,2-dimethylsuccinate and 4,4'-bipyridine ligands, namely poly[[aqua(μ2-4,4'-bipyridine-κ(2)N:N')bis(μ3-2,2-dimethylbutanedioato)-κ(4)O(1),O(1'):O(4):O(4');κ(5)O(1):O(1),O(4):O(4),O(4')-dizinc(II)] dihydrate], {[Zn2(C6H8O4)2(C10H8N2)(H2O)]·2H2O}n, has been synthesized under hydrothermal conditions and characterized by single-crystal X-ray diffraction and elemental, IR and thermogravimetric analyses. In the structure, the 2,2-dimethylsuccinate ligands link linear tetranuclear Zn(II) subunits into one-dimensional chains along the c axis. 4,4'-Bipyridine acts as a tethering ligand expanding these one-dimensional chains into a two-dimensional layered structure. Hydrogen-bonding interactions between the water molecules (both coordinated and free) and carboxylate O atoms strengthen the packing of the layers. Furthermore, the luminescence properties of the complex were investigated. The compound exhibits a blue photoluminescence in the solid state at room temperature and may be a good candidate for potential hybrid inorganic-organic photoactive materials.

  15. High-pressure synthesis and structural, physical properties of CaIr1-xPtxO3 and CaIr1-xRhxO3

    Science.gov (United States)

    Hirai, S.; Bromiley, G. D.; Klemme, S.; Irifune, T.; Ohfuji, H.; Attfield, P.; Nishiyama, N.

    2010-12-01

    Since the discovery of the perovskite to post-perovskite transition in MgSiO3 in a laser-heated DAC, wide attention has been focussed on the post-perovskite phase of MgSiO3. This is because the post-perovskite phase is likely to play a key role in Earth’s lowermost mantle, and because the perovskite to post-perovskite transition can explain many features of the D” seismic discontinuity. While it is meaningful to conduct further studies of MgSiO3, the post-perovskite phase of MgSiO3 cannot be quenched to ambient pressure/temperature conditions. Thus, further studies must be conducted using analogue compounds of MgSiO3 post-perovskite, which are quenchable to ambient pressure/temperature conditions. The post-perovskite phase of MgSiO3 crystallizes in a layered structure with CaIrO3-structure. Therefore, it is useful to investigate compounds with CaIrO3-structure. There are only four quenchable oxides with CaIrO3-structure reported to date: CaIrO3, CaPtO3, CaRhO3 and CaRuO3. CaIrO3 can be synthesized at ambient pressure, whilst the other three oxides can only be obtained at high pressure/temperature conditions using a multi-anvil apparatus. Further studies on these materials have revealed structural phase transitions at high P-T and a metal-insulator transition by hole doping. In the case of CaIrO3, The post-perovskite phase of CaIrO3 synthesized at 2GPa, 1373K transforms into a perovskite phase at 2GPa, 1673K. In other words, the perovskite phase can be synthesized at temperatures higher than those needed for synthesizing the post-perovskite phase. This is also the case for CaRhO3 (6GPa, 1873K) and CaRuO3 (23GPa, 1343K), while CaPtO3 remained post-perovskite at higher temperatures. We have succeeded in synthesizing solid solutions between CaIrO3, CaPtO3 and CaRhO3. We have found the systematic change in structural and physical properties of post-perovskite oxides, with composition and P-T, which broadens the future opportunity for studying post-perovskite systems

  16. Synthesis and superconducting properties of niobium germanium

    International Nuclear Information System (INIS)

    Kihlstrom, K.E.

    1982-01-01

    By carefully controlling temperature homogeneity during preparation of the Nb 3 Ge samples, homogeneous films have been prepared of high-T/sub c/Nb 3 Ge. Homogeneity is demonstrated by a sharp transition width (ΔT/sub c/ 6 amps/cm 2 which are the highest ever reported for any material at this temperature. The successful film synthesis has made it possible to study the superconducting properties of Nb 3 Ge. High quality A15 NbGe/(SiO/sub x/)/Pb tunnel juctions on electron beam codeposited oxygen-doped Nb 3 Ge have been fabricated. 2Δ/(k/sub B/T/sub c/ rises from the BCS limit in Ge-poor samples to become strong coupled (2Δk/sub B/T/sub c/ approx. 4.35) as stoichiometry is approached. The electron-phonon spectral function α 2 F(ω) and related microscopic parameters were obtained. As the T/sub c/ and gap increase, a movement of the lowest phonon branch to lower energies is observed with a resultant decrease in (ω 2 ). Thus lambda increases with T/sub c/ while (ω 2 ) decreases in agreement with the idea that mode softening is a major factor in the increase of T/sub c/ with approach to stoichiometry as previously found in Nb 3 Al by Kwo and Geballe

  17. Synthesis and properties of superheavy elements

    CERN Document Server

    Hofmann, S

    2003-01-01

    The nuclear shell model predicts that the next doubly magic shell-closure beyond sup 2 sup 0 sup 8 Pb is at a proton number Z = 114, 120, or 126 and at a neutron number N = 172 or 184. The outstanding of experimental investigations is the exploration of this region of spherical 'SuperHeavy Elements' (SHEs). Experimental methods are described which allowed for the identification of elements 107 to 112 in studies of cold fusion reactions based on lead and bismuth targets. Also presented are data which were obtained on the synthesis of elements 112, 114, and 116 in investigation of hot fusion reactions using actinide targets. The decay data reveal that for the heaviest elements, the dominant decay mode is alpha emission, not fission. Decay properties as well as reaction cross- sections are compared with the results of theoretical studies. Finally, plans are presented for the further development of the experimental set-up and the application of new techniques. At a higher sensitivity, the exploration of the regio...

  18. Synthesis, structural and optical properties of pure and rare-earth ion doped TiO{sub 2} nanowire arrays by a facile hydrothermal technique

    Energy Technology Data Exchange (ETDEWEB)

    Bandi, Vengala Rao; Raghavan, Chinnambedu Murugesan; Grandhe, Bhaskar kumar; Kim, Sang Su [Department of Physics, Changwon National University, Changwon 641-773 (Korea, Republic of); Jang, Kiwan, E-mail: kwjang@changwon.ac.kr [Department of Physics, Changwon National University, Changwon 641-773 (Korea, Republic of); Shin, Dong-Soo [Department of Chemistry, Changwon National University, Changwon 641-773 (Korea, Republic of); Yi, Soung-Soo [Department of Photonics, Silla University, Busan 617-736 (Korea, Republic of); Jeong, Jung-Hyun [Department of Physics, Pukyong National University, Busan 608-737 (Korea, Republic of)

    2013-11-29

    Single crystalline pure and rare-earth metal ions (Eu{sup 3+} and Ce{sup 3+}) doped TiO{sub 2} nanowire arrays were prepared on conductive fluorine doped indium tin oxide substrates by a facile hydrothermal method. Initially the conditions and parameters were optimized to prepare the high quality TiO{sub 2} nanowire arrays in the absence of organic additives. The average diameter and length of the TiO{sub 2} nanowire were found to be ∼ 30–50 nm and ∼ 0.5–1.5 μm, respectively. The formations of rutile phase structure in all the samples were confirmed by x-ray diffractometric analysis while the transmission electron microscopy confirms the single crystallinity and the maximum orientation of growth direction along [001] for the as-grown TiO{sub 2} nanowire. The optical properties of all the samples were analyzed using photoluminescence spectroscopy. The photocatalytic properties of the pure and doped TiO{sub 2} were investigated for the decomposition of organic toludine blue-O dye under ultraviolet irradiation. The result demonstrates that the Ce{sup 3+}: TiO{sub 2} decomposed almost 90% of the organic dye within 80 min. - Highlights: • Rare-earth (RE) doped TiO{sub 2} nanowire arrays were prepared by hydrothermal method • RE doping enhanced the growth rate of TiO{sub 2} nanowire arrays • The catalysts used to check their photocatalytic activity by toludine blue-O dye • RE doped TiO2 act as unprecedented photocatalyst for organic dye decomposition.

  19. Synthesis, structural characterization and dielectric properties of Nb doped BaTiO3/SiO2 core–shell heterostructure

    International Nuclear Information System (INIS)

    Cernea, M.; Vasile, B.S.; Boni, A.; Iuga, A.

    2014-01-01

    Highlights: • Optimal parameters for preparation by sol–gel of core–shell (BT-Nb 0.005 )/SiO 2 are presented in this paper. • Single crystalline BT-Nb 0.005 /SiO 2 core–shell composite with ∼34 nm shell thick was prepared. • The core–shell ceramic exhibits good dielectric properties and ferroelectric characteristics. -- Abstract: Perovskite complex ceramic oxides, BaTiO 3 doped with 0.5 mol%Nb 2 O 5 and then nanocoated with SiO 2 (abbreviated as BT-Nb 0.005 /SiO 2 ) was successful prepared using conventional sol–gel processing. Phase composition, particle morphology, structure, and electric properties of BT-Nb 0.005 core and BT-Nb 0.005 /SiO 2 core–shell were examined and compared, using X-ray diffraction, transmission electron microscopy and, dielectric and ferroelectric measurements. Core–shell composite with well-defined perovskite tetragonal phase of BaTiO 3 was achieved. Furthermore, single crystalline BT-Nb 0.005 /SiO 2 core–nanoshell heterostructure with ∼34 nm shell thick was prepared, which is a novelty in ferroelectrics field. The ferroelectric quality of BT-Nb 0.005 has suffered an alteration when the (BT-Nb 0.005 )/SiO 2 core–shell heterostructure was realized. One-dimensional BT-Nb 0.005 /SiO 2 core–shell heterostructure exhibits an improvement of dielectric losses and a decrease of dielectric constant, compared to uncoated BT-Nb 0.005 . The (BT-Nb 0.005 )/SiO 2 core–shell material could be interesting for application in the composite capacitors

  20. Seven new Zn(II)/Cd(II) coordination polymers with 2-(hydroxymethyl)-1H-benzo[d]imidazole-5-carboxylic acid: Synthesis, structures and properties

    Science.gov (United States)

    Wang, Xin-Fang; Zhou, Sheng-Bin; Du, Ceng-Ceng; Wang, Duo-Zhi; Jia, Dianzeng

    2017-08-01

    Using a new simi-rigid multitopic ligand 2-(hydroxymethyl)-1H-benzo[d]imidazole-5-carboxylic acid (H2L), seven new coordination polymers [Zn3(L)2(μ2-OH)2]n (1), {[Zn2(HL)2(H2O)2]·SiF6}n (2), [Zn(HL)(SCN)]n (3), {[Zn2(HL)2(SO4)]·(4,4‧-bpy)}n (4) [4,4‧-bpy =4,4‧-bipyridine], {[Zn(HL)2]·2H2O}n (5), {[Cd(HL)2]·2H2O}n (6) and [Cd2(HL)2(H2O)2(SO4)]n (7) have been successfully obtained from H2L ligand under solvothermal conditions and structurally characterized by single-crystal X-ray diffraction, elemental analysis, thermogravimetric analysis, powder X-ray diffraction and IR spectroscopy. In addition, UV-vis diffuse-reflectance spectra demonstrate wide band gaps. Complex 1 features a 3D topological net of {412·63} with the stoichiometry (6-c), contains 1D channels with the accessible solvent volume of 42.1%. 3, 4, 5 and 6 have a 1D chain structure, 5 and 6 further assemble to form 2D sheet and 3D supramolecular frameworks by hydrogen-bonding interactions, respectively. Complexes 2 and 7 possess a 2D layered structure, and the 2D supramolecular network of 2 can be rationalized to be four-connected {44·62} topological sql network with the dinuclear units, while 7 shows a 3-nodal 2D net with a point symbol of {63}. Moreover, the fluorescent emission, fluorescence lifetimes of 1-7 have been investigated and discussed. Interesting enough, complex 1 showed high efficiency for catalyzing the Knoevenagel condensation reaction between 4-substituted aromatic aldehydes and malononitrile as selective heterogeneous catalyst. The CPs combining catalytic and fluorescent properties could further meet the requirement as a multifunctional material. Seven new Zn(II)/Cd(II) coordination polymers with simi-rigid multitopic ligand, [(2-(hydroxymethyl)-1H-benzo[d]imidazole-5-carboxylic acid) (H2L)] have been successfully obtained and structurally characterized by single-crystal X-ray diffraction, elemental analysis, thermogravimetric analysis, powder X-ray diffraction and IR

  1. Marine Nucleosides: Structure, Bioactivity, Synthesis and Biosynthesis

    Directory of Open Access Journals (Sweden)

    Ri-Ming Huang

    2014-12-01

    Full Text Available Nucleosides are glycosylamines that structurally form part of nucleotide molecules, the building block of DNA and RNA. Both nucleosides and nucleotides are vital components of all living cells and involved in several key biological processes. Some of these nucleosides have been obtained from a variety of marine resources. Because of the biological importance of these compounds, this review covers 68 marine originated nucleosides and their synthetic analogs published up to June 2014. The review will focus on the structures, bioactivities, synthesis and biosynthetic processes of these compounds.

  2. Synthesis and properties of novel 4,5-diaminonaphthalimides

    International Nuclear Information System (INIS)

    Morris, I.P.

    1999-07-01

    This thesis presents work carried out into the synthesis and properties of Novel 4,5-diaminonaphthalimides. Previous work had identified that these compounds could be synthesised through a short reaction sequence but a very limited number of examples had been produced. With some modifications, the structure of 4,5-diaminonaphthalimides suggests a number of applications. The diamine functionality suggests the formation of complexes and if chiral amines were used asymmetric synthesis is a possibility. Naphthalimides are known to intercalate into DNA and so compounds of this nature may have interesting anti-cancer activity. Finally diaminonaphthalimides are strongly fluorescent and this in combination with the chelation potential of the diamine functionality may afford ion and molecular sensors. The first section of this thesis reviews these areas of research and demonstrates how diaminonaphthalimides might contribute to these areas. The second section describes the synthesis of 4,5-diaminonaphthalimides and illustrates the variety of compounds that may be synthesised. In addition this section explores the applications to fluorescence sensing and asymmetric synthesis. 4,5-Diaminonaphthalimides are shown to undergo chelation enhanced quenching (CHEQ) and chelation enhanced fluorescence (CHEF) with various transition metal ions. The precise features are shown to be dependent on the metal ion present. The mass spectroscopic results discussed in this section show 4,5-diaminonaphthalimides to be a new class of supramolecular compound as they show pre-assembly around alkali earth metal ions. 4,5-Diaminonaphthalimides were also used as catalysts in asymmetric reactions where they show some catalytic activity in the addition of diethylzinc to benzaldehyde. (author)

  3. Synthesis and radioactive properties of the heaviest nuclei

    International Nuclear Information System (INIS)

    Oganesyan, Yu.Ts.

    1996-01-01

    Experimental investigations on the synthesis and study of properties of faraway transactinide elements confirm the predictions of macro-microscopic theory on the existence of closed shells in the region of heavy deformed nuclei. It has been demonstrated experimentally that nuclear structure plays a decisive role in the stability of superheavy nuclides. Based on the experimental confirmation of the main provisions of the theory and after the introduction of a necessary correction into the calculation the properties of heavier nuclides in the region of spherical shells Z=114 and N=180-184 have been predicted. Here a substantial increase in the stability of nuclei is also expected. All the nuclei synthesized by now, were obtained in fusion reactions with a formation of a compound nucleus, the transition of which to the ground state takes place with the emission of neutrons and gamma-rays. Both the reactions of cold and hot fusion of nuclei can be used for the synthesis of new nuclei. Nevertheless, new experimental data on the fusion mechanism are required, since a number of theoretical descriptions of the fusion dynamics of complex nuclear systems need a substantial revising. One can assume that the reactions of the type 244 Pu, 248 Cm + 48 Ca are still within the current potential of the accelerators and experimental technique. This potential, nevertheless, is still to be implemented. 37 refs., 6 figs

  4. A novel yellow-emitting SrAlSi4N7:Ce3+ phosphor for solid state lighting: Synthesis, electronic structure and photoluminescence properties

    Science.gov (United States)

    Ruan, Jian; Xie, Rong-Jun; Funahashi, Shiro; Tanaka, Yoshinori; Takeda, Takashi; Suehiro, Takayuki; Hirosaki, Naoto; Li, Yuan-Qiang

    2013-12-01

    Ce3+-doped and Ce3+/Li+-codoped SrAlSi4N7 phosphors were synthesized by gas pressure sintering of powder mixtures of Sr3N2, AlN, α-Si3N4, CeN and Li3N. The phase purity, electronic crystal structure, photoluminescence properties of SrAlSi4N7:Ce3+(Ce3+/Li+) were investigated in this work. The band structure calculated by the DMol3 code shows that SrAlSi4N7 has a direct band gap of 3.87 eV. The single crystal analysis of Ce3+-doped SrAlSi4N7 indicates a disordered Si/Al distribution and nitrogen vacnacy defects. SrAlSi4N7 was identified as a major phase of the fired powders, and Sr5Al5Si21N35O2 and AlN as minor phases. Both Ce3+ and Ce3+/Li+ doped SrAlSi4N7 phosphors can be efficiently excited by near-UV or blue light and show a broadband yellow emission peaking around 565 nm. A highest external quantum efficiency of 38.3% under the 450 nm excitation was observed for the Ce3+/Li+-doped SrAlSi4N7 (5 mol%). A white light LED lamp with color temperature of 6300 K and color rendering index of Ra=78 was achieved by combining Sr0.97Al1.03Si3.997N\\94\\maccounttest14=t0005_18193 7:Ce3+0.03 with a commercial blue InGaN chip. It indicates that SrAlSi4N7:Ce3+ is a promising yellow emitting down-conversion phosphor for white LEDs.

  5. Three Cyanide-Bridged One-Dimensional Single Chain Co"I"I"I-Mn"I"I Complexes: Rational Design, Synthesis, Crystal Structures and Magnetic Properties

    International Nuclear Information System (INIS)

    Zhang, Daopeng; Zhao, Zengdian; Wang, Ping; Chen, Xia

    2012-01-01

    Two pyridinecarboxamide dicyanidecobalt(III) building blocks and two mononuclear seven-coordinated macrocycle manganese(II) compounds have been rationally selected to assemble cyanide-bridged heterobimetallic complexes, resulting in three cyanide-bridged Co"I"I"I-Mn"I"I complexes. Single X-ray diffraction analysis show that these complexes {[Mn(L"1)][Co(bpb)]}ClO_4·CH_3OH·0.5H_2O (1), {[Mn(L"2)][Co(bpb)]}ClO_4·0.5CH_3OH (2) and {[Mn(L"1)][Cobpmb]}ClO_4·H_2O (3) (L"1 = 3,6-diazaoctane-1,8-diamine, L"2 = 3,6-dioxaoctano-1,8- diamine: bpb"2"- = 1,2-bis(pyridine-2-carboxamido)benzenate, bpmb"2"- = 1,2-bis(pyridine-2-carboxamido)-4- methyl-benzenate) all present predictable one-dimensional single chain structures. The molecular structures of these one-dimensional complexes consists of alternating units of [Mn(L)]"2"+ (L = L"1 or L"2) and [Co(L')(CN)_2]"- (L' = bpb"2"-, or bpmb"2"-), forming a cyanide-bridged cationic polymeric chain with free ClO_4"- as the balance anion. The coordination geometry of manganese(II) ion in the three one-dimensional complexes is a slightly distorted pentagonal-bipyrimidal with two cyanide nitrogen atoms at the trans positions and N_5 or N_3O_2 coordinating mode at the equatorial plane from ligand L"1 or L"2. Investigation over magnetic properties of these complexes reveals that the very weak magnetic coupling between neighboring Mn(II) ions connected by the diamagnetic dicyanidecobalt(III) building block. A best-fit to the magnetic susceptibility of complex 1 leads to the magnetic coupling constants J = .0.084(3) cm"-"1

  6. Synthesis of Nanocrystalline CaWO4 as Low-Temperature Co-fired Ceramic Material: Processing, Structural and Physical Properties

    Science.gov (United States)

    Vidya, S.; Solomon, Sam; Thomas, J. K.

    2013-01-01

    Nanocrystalline scheelite CaWO4, a promising material for low-temperature co-fired ceramic (LTCC) applications, has been successfully synthesized through a single-step autoignition combustion route. Structural analysis of the sample was performed by powder x-ray diffraction (XRD), Fourier-transform infrared spectroscopy, and Raman spectroscopy. The XRD analysis revealed that the as-prepared sample was single phase with scheelite tetragonal structure. The basic optical properties and optical constants of the CaWO4 nanopowder were studied using ultraviolet (UV)-visible absorption spectroscopy, which showed that the material was a wide-bandgap semiconductor with bandgap of 4.7 eV at room temperature. The sample showed poor transmittance in the ultraviolet region but maximum transmission in the visible/near-infrared regions. The photoluminescence spectra recorded at different temperatures showed intense emission in the green region. The particle size estimated from transmission electron microscopy was 23 nm. The feasibility of CaWO4 for LTCC applications was studied from its sintering behavior. The sample was sintered at a relatively low temperature of 810°C to high density, without using any sintering aid. The surface morphology of the sintered sample was analyzed by scanning electron microscopy. The dielectric constant and loss factor of the sample measured at 5 MHz were found to be 10.50 and 1.56 × 10-3 at room temperature. The temperature coefficient of the dielectric constant was -88.71 ppm/°C. The experimental results obtained in this work demonstrate the potential of nano-CaWO4 as a low-temperature co-fired ceramic as well as an excellent luminescent material.

  7. Synthesis, structural and optical properties of ZnO spindle/reduced graphene oxide composites with enhanced photocatalytic activity under visible light irradiation

    Science.gov (United States)

    Prabhu, S.; Pudukudy, M.; Sohila, S.; Harish, S.; Navaneethan, M.; Navaneethan, D.; Ramesh, R.; Hayakawa, Y.

    2018-05-01

    In the present work, spindle-shaped ZnO and reduced graphene oxide sheets were successfully synthesized by a hydrothermal method and then ZnO/r-GO composite was prepared by a direct solution mixing method. Various characterization results confirmed the interior and surface decoration of spindle-shaped ZnO on the reduced graphene oxide sheets. The phase formation, crystalline structure, morphology, surface states and optical properties were characterized using Powder X-ray diffraction (XRD), Field emission scanning electron microscopy (FESEM), Transmission electron microscopy (TEM), X-ray photoelectron spectroscopy (XPS), Fourier Transform Infrared Spectroscopy (FTIR) and UV-Vis spectroscopy. The X-ray diffraction analysis showed the formation of the hexagonal wurtzite crystalline structure of ZnO with high crystalline quality. The band gap of the ZnO/r-GO composite was found to be low (3.03eV) compared to the band gap of spindle shaped ZnO (3.13 eV), as calculated from optical studies. The spindle-like morphology of the single crystalline ZnO was clearly shown in the electron microscopic images. The chemical bonding and surface states of the samples were studied using XPS measurement. Moreover, a possible growth mechanism for the ZnO spindle was proposed. The catalytic activity of the as-synthesized samples was evaluated for the photodegradation of methylene blue under visible light irradiation. Among the synthesized samples, the ZnO/r-GO composite showed higher degradation efficiency of 93% and successfully reused for four consecutive run without any activity loss.

  8. Synthesis and electrochemical properties of layered structure Li[Ni0.5Co0.25Mn0.25]O2 cathode material

    International Nuclear Information System (INIS)

    Prathibha, G.; Rosaiah, P.; Reddy, B. Purusottam; Ganesh, K. Sivajee; Hussain, O. M.

    2015-01-01

    Lithium ion (Li-ion) batteries are currently the energy source of choice for cell phones, laptops, and other mobile electronic devices due to their balance of high energy density with high power density compared to other electrochemical energy carriers. In the present study, mixed hydroxide method is used to prepare Li[Ni 0.5 Co 0.25 Mn 0.25 ]O 2 from the precursors and analyze qualitatively and studied the electrochemical properties. The XRD spectrum exhibited predominant (003) orientation at 2θ =18.39 o corresponding to hexagonal layered structure of R3m symmetry with evaluated lattice parameters are a= 2.84 Å, c= 14.43 Å. Raman measurements were performed to understand the microstructure and vibrational modes of the prepared sample. From the electrochemical (EC) studies an initial discharge capacity of about 140 mAhg −1 with good cyclic stability was observed for the prepared sample in the potential range 0.0 −1.0V in aqueous medium

  9. One-step synthesis of bird cage-like ZnO and other controlled morphologies: Structural, growth mechanism and photocatalytic properties

    International Nuclear Information System (INIS)

    Yang, Shuo; Wang, Jian; Li, Xiuyan; Zhai, Hongju; Han, Donglai; Wei, Bing; Wang, Dandan; Yang, Jinghai

    2014-01-01

    Highlights: • ZnO nanocage arrays were synthesized by a one-step etching route. • ZnO nanocage exhibit higher photocatalytic activity than other samples. • The different photocatalytic activities of different samples were analyzed. • The formation mechanism of ZnO nanocages was proposed. - Abstract: ZnO nanocages and other nanostructures have been synthesized via a simple one-pot hydrothermal method with different reaction times. It is worth mentioning that this is a completely green method which does not require any other chemicals except that Zn foil served as Zn source in the experiment. X-ray diffraction (XRD), Scanning electron microscopy (SEM), transmission electron microscopy (TEM), photoluminescence (PL) and UV–Vis diffuse reflection spectra were used to characterize the crystallinity, morphology and optical property of ZnO structures. Growth mechanisms of ZnO were proposed based on these results. Furthermore, ZnO films with different morphologies and crystal growth habits exhibited different activities to rhodamine B degradation. The influence of the reaction time on the morphology of ZnO films and the effect of the morphologies on the photocatalytic activity are discussed

  10. Anisotropic nanomaterials: Synthesis, optical and magnetic properties, and applications

    Science.gov (United States)

    Banholzer, Matthew John

    As nanoscience and nanotechnology mature, anisotropic metal nanostructures are emerging in a variety of contexts as valuable class of nanostructures due to their distinctive attributes. With unique properties ranging from optical to magnetic and beyond, these structures are useful in many new applications. Chapter two discusses the nanodisk code: a linear array of metal disk pairs that serve as surface-enhanced Raman scattering substrates. These multiplexing structures employ a binary encoding scheme, perform better than previous nanowires designs (in the context of SERS) and are useful for both convert encoding and tagging of substrates (based both on spatial disk position and spectroscopic response) as well as biomolecule detection (e.g. DNA). Chapter three describes the development of improved, silver-based nanodisk code structures. Work was undertaken to generate structures with high yield and reproducibility and to reoptimize the geometry of each disk pair for maximum Raman enhancement. The improved silver structures exhibit greater enhancement than Au structures (leading to lower DNA detection limits), convey additional flexibility, and enable trinary encoding schemes where far more unique structures can be created. Chapter four considers the effect of roughness on the plasmonic properties of nanorod structures and introduces a novel method to smooth the end-surfaces of nanorods structures. The smoothing technique is based upon a two-step process relying upon diffusion control during nanowires growth and selective oxidation after each step of synthesis is complete. Empirical and theoretical work show that smoothed nanostructures have superior and controllable optical properties. Chapter five concerns silica-encapsulated gold nanoprisms. This encapsulation allows these highly sensitive prisms to remain stable and protected in solution, enabling their use as class-leading sensors. Theoretical study complements the empirical work, exploring the effect of

  11. A novel yellow-emitting SrAlSi4N7:Ce3+ phosphor for solid state lighting: Synthesis, electronic structure and photoluminescence properties

    International Nuclear Information System (INIS)

    Ruan, Jian; Xie, Rong-Jun; Funahashi, Shiro; Tanaka, Yoshinori; Takeda, Takashi; Suehiro, Takayuki; Hirosaki, Naoto; Li, Yuan-Qiang

    2013-01-01

    Ce 3+ -doped and Ce 3+ /Li + -codoped SrAlSi 4 N 7 phosphors were synthesized by gas pressure sintering of powder mixtures of Sr 3 N 2 , AlN, α-Si 3 N 4 , CeN and Li 3 N. The phase purity, electronic crystal structure, photoluminescence properties of SrAlSi 4 N 7 :Ce 3+ (Ce 3+ /Li + ) were investigated in this work. The band structure calculated by the DMol 3 code shows that SrAlSi 4 N 7 has a direct band gap of 3.87 eV. The single crystal analysis of Ce 3+ -doped SrAlSi 4 N 7 indicates a disordered Si/Al distribution and nitrogen vacnacy defects. SrAlSi 4 N 7 was identified as a major phase of the fired powders, and Sr 5 Al 5 Si 21 N 35 O 2 and AlN as minor phases. Both Ce 3+ and Ce 3+ /Li + doped SrAlSi 4 N 7 phosphors can be efficiently excited by near-UV or blue light and show a broadband yellow emission peaking around 565 nm. A highest external quantum efficiency of 38.3% under the 450 nm excitation was observed for the Ce 3+ /Li + -doped SrAlSi 4 N 7 (5 mol%). A white light LED lamp with color temperature of 6300 K and color rendering index of Ra=78 was achieved by combining Sr 0.97 Al 1.03 Si 3.997 N/94/maccounttest14=t0005 1 8193 7 :Ce 3+ 0.03 with a commercial blue InGaN chip. It indicates that SrAlSi 4 N 7 :Ce 3+ is a promising yellow emitting down-conversion phosphor for white LEDs. - Graphical abstract: One-phosphor converted white light-emitting diode (LED) was fabricated by combining a blue LED chip and a yellow-emitting SrAlSi4N7:Ce 3+ phosphor (see inset), which has the color rendering index of 78 and color temperature of 6300 K. - Highlights: • We reported a new yellow nitride phosphor suitable for solid state lighting. • We solved the crystal structure and evidenced a disordered Si/Al distribution. • We fabricated a high color rendering white LEDs by using a single SrAlSi4N7:Ce

  12. Structure-function-property-design interplay in biopolymers: spider silk.

    Science.gov (United States)

    Tokareva, Olena; Jacobsen, Matthew; Buehler, Markus; Wong, Joyce; Kaplan, David L

    2014-04-01

    Spider silks have been a focus of research for almost two decades due to their outstanding mechanical and biophysical properties. Recent advances in genetic engineering have led to the synthesis of recombinant spider silks, thus helping to unravel a fundamental understanding of structure-function-property relationships. The relationships between molecular composition, secondary structures and mechanical properties found in different types of spider silks are described, along with a discussion of artificial spinning of these proteins and their bioapplications, including the role of silks in biomineralization and fabrication of biomaterials with controlled properties. Copyright © 2013 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

  13. Cd(II)-coordination polymers based on tetracarboxylic acid and diverse bis(imidazole) ligands: Synthesis, structural diversity and photoluminescence properties

    Energy Technology Data Exchange (ETDEWEB)

    Arıcı, Mürsel, E-mail: marici@ogu.edu.tr [Department of Chemistry, Faculty of Arts and Sciences, Eskişehir Osmangazi University, 26480 Eskişehir (Turkey); Yeşilel, Okan Zafer [Department of Chemistry, Faculty of Arts and Sciences, Eskişehir Osmangazi University, 26480 Eskişehir (Turkey); Taş, Murat [Department of Science Education, Education Faculty, Ondokuz Mayıs University, 55139 Samsun (Turkey)

    2017-01-15

    Three new Cd(II)-coordination polymers, namely, ([Cd{sub 2}(μ{sub 6}-ao{sub 2}btc)(μ-1,5-bipe){sub 2}]·2H{sub 2}O){sub n} (1), ([Cd{sub 2}(μ{sub 6}-ao{sub 2}btc)(μ-1,4-bix){sub 2}]{sub n}·2DMF) (2) and ([Cd{sub 2}(μ{sub 8}-abtc)(μ-1,4-betix)]·DMF·H{sub 2}O){sub n} (3) (ao{sub 2}btc=di-oxygenated form of 3,3′,5,5′-azobenzenetetracarboxylate, 1,5-bipe: 1,5-bis(imidazol-1yl)pentane, 1,4-bix=1,4-bis(imidazol-1ylmethyl)benzene, 1,4-betix=1,4-bis(2-ethylimidazol-1ylmethyl)benzene) were synthesized with 3,3′,5,5′-azobenzenetetracarboxylic acid and flexible, semi-flexible and semi-flexible substituted bis(imidazole) linkers. They were characterized by IR spectroscopy, elemental analysis, single-crystal X-ray diffraction, powder X-ray diffractions (PXRD) and thermal analyses (TG/DTA). Complexes 1–3 exhibited structural diversities depending on flexible, semi-flexible and semi-flexible substituted bis(imidazole) ligands. Complex 1 was 2D structure with 3,6L18 topology. Complex 2 had a 3D pillar-layered framework with the rare sqc27 topology. When semi-flexible substituted bis(imidazole) linker was used, 3D framework of complex 3 was obtained with the paddlewheel Cd{sub 2}(CO{sub 2}){sub 4}-type binuclear SBU. Moreover, thermal and photoluminescence properties of the complexes were determined in detailed. - Graphical abstract: In this study, three novel Cd(II)-coordination polymers were synthesized with 3,3′,5,5′-azobenzenetetracarboxylic acid and flexible, semi-flexible and semi-flexible substituted bis(imidazole) linkers. They were characterized by IR spectroscopy, elemental analysis, single-crystal X-ray diffraction, powder X-ray diffractions (PXRD) and thermal analyses (TG/DTA). Complexes 1–3 exhibited structural diversities depending on flexible, semi-flexible and semi-flexible substituted bis(imidazole) ligands. Complex 1 was 2D structure with 3,6L18 topology. Complex 2 had a 3D pillar-layered framework with the rare sqc27 topology. When semi

  14. Synthesis, crystal structure, thermal analysis and dielectric properties of Rb4(SO4)(HSO4)2(H3AsO4) compound

    Science.gov (United States)

    Belhaj Salah, M.; Nouiri, N.; Jaouadi, K.; Mhiri, T.; Zouari, N.

    2018-01-01

    A new inorganic Rb4(SO4)(HSO4)2(H3AsO4) compound was prepared. It was found to crystallize in the monoclinic system (P21 space group) with the following lattice parameters: a = 5868 (1) Å, b = 13,579(2) Å, c = 11,809 (3) Å and β = 94,737 (1)°. The structure is characterized by SO42-, HSO4- and H3AsO4 tetrahedra connected by hydrogen bridge to form two types of dimmer (H(8)S(2)O4- … S(1)O42- and H(12)S(2)O4- … H3AsO4). These dimmers are interconnected by both hydrogen bonds O(14)sbnd H(14)· · ·O(4) and O(15)sbnd H(15)· · ·O(2). They are also linked by the hydrogen bridge assured by the hydrogen atoms H(2), H(3) and H(4) of the H3AsO4 group to build the chain S(1)O4⋯H3AsO4 which are parallel to the ''a'',direction. The rubidium cations are coordinated by eight oxygen atoms with Rbsbnd O distance ranging from 2893(8) to 3.415(6) Å. The existence of Osbnd H and (S/As)sbnd O bonds in the structure at room temperature has been confirmed by IR and Raman spectroscopy in the frequency ranges 4000-400 cm-1and 1200 - 50 cm-1, respectively. Thermal analysis of Rb4(HSO4)(HSO4)2(H3AsO4) showed that the transformation to high temperature phase occurs at 407 K by one-step process. Thermal decomposition of the product takes place at much higher temperatures, with an onset of approximately 522 K. The first transition detected by differential scanning calorimetry (DSC) was also analyzed by dielectric and conductivity measurements using the impedance spectroscopy techniques. The conductivity in the high temperature phase at 428 K is 1.04 × 10-3 Ω-1 cm-1, and the activation energy for the proton transport is 0.36 eV. The conductivity relaxation parameters associated with the high disorder protonic conduction have been examined from analysis of the M"/M"max spectrum measured in a wide temperature range. Transport properties of this material appear to be due to the proton hopping mechanism. The obtained results show that this transition is protonic by nature.

  15. Effects of synthesis conditions on structure and surface properties of SmMn{sub 2}O{sub 5} mullite-type oxide

    Energy Technology Data Exchange (ETDEWEB)

    Thampy, Sampreetha; Ibarra, Venessa; Lee, Yun-Ju [Department of Materials Science and Engineering, University of Texas at Dallas, Richardson, TX 75080 (United States); McCool, Geoffrey [Nanostellar Inc., 3696 Haven Avenue, Redwood City, CA 94063 (United States); Cho, Kyeongjae [Department of Materials Science and Engineering, University of Texas at Dallas, Richardson, TX 75080 (United States); Hsu, Julia W.P., E-mail: jwhsu@utdallas.edu [Department of Materials Science and Engineering, University of Texas at Dallas, Richardson, TX 75080 (United States)

    2016-11-01

    Highlights: • Investigate the effects of calcination temperature and precipitation pH on crystallinity, phase purity, particle size, surface composition, and NO adsorption capacity of SmMn{sub 2}O{sub 5}. • High calcination temperature increases mullite phase purity but decreases specific surface area (SSA). • Mullite phase purity is independent of pH while SSA monotonically increases. • SSA and surface Mn/Sm ratio determine NO uptake. - Abstract: A mixed-phase compound that contains SmMn{sub 2}O{sub 5} mullite-type oxides has been reported to display excellent catalytic activity for nitric oxide (NO) oxidation. Here we investigate the effects of calcination temperature and precipitation pH on structural, physical, chemical, and surface properties of SmMn{sub 2}O{sub 5}. As the calcination temperature increases from 750 °C to 1000 °C, mullite phase purity increases from 74% to 100%, while specific surface area (SSA) decreases from 23.6 m{sup 2}/g to 5.1 m{sup 2}/g with particle size increases correspondingly. Mullite phase purity (87%) is independent of pH between 8.5–10.4, whereas SSA monotonically increases from 12.5 m{sup 2}/g at pH 8.1 to 27.4 m{sup 2}/g at pH 13. X-ray photoelectron spectroscopy (XPS) studies reveal that the surface Mn/Sm ratio is similar to the bulk value and is unaffected by calcination temperature and pH values up to 10.4, whereas sample precipitated at pH 13 is surface-rich in Sm. NO chemisorption studies show that the SSA and surface Mn/Sm ratio determine NO uptake by SmMn{sub 2}O{sub 5} mullite oxides.

  16. Hydrothermal synthesis, structural elucidation, spectroscopic studies, thermal behavior and luminescence properties of a new 3-d compound: FeAlF2(C10H8N2)(HPO4)2(H2O)

    Science.gov (United States)

    Bouzidia, Nabaa; Salah, Najet; Hamdi, Besma; Ben Salah, Abdelhamid

    2017-04-01

    The study of metal phosphate has been a proactive field of research thanks to its applied and scientific importance, especially in terms of the development of optical devices such as solid state lasers as well as optical fibers. The present paper seeks to investigate the synthesis, crystal structure, elemental analysis and properties of FeAlF2(C10H8N2)(HPO4)2(H2O) compound investigated by spectroscopic studies (FT-IR and FT-Raman), thermal behavior and luminescence. The Hirshfeld surface analysis and 2-D fingerprint plot have been performed to explore the behavior of these weak interactions and crystal cohesion. This investigation shows that the molecules are connected by hydrogen bonds of the type Osbnd H⋯O and Osbnd H⋯F. In addition, the 2,2'‒bipyridine ligand plays a significant role in the construction of 3-D supramolecular framework via π‒π stacking. FT‒IR and FT‒Raman spectra were used so as to ease the responsibilities of the vibration modes of the title compound. The thermal analysis (TGA) study shows a mass loss evolution as a temperature function. Finally, the optical properties were evaluated by photoluminescence spectroscopy.

  17. Polymer nanotube nanocomposites: synthesis, properties, and applications

    National Research Council Canada - National Science Library

    Mittal, Vikas

    2010-01-01

    ... in these commercially important areas of polymer technology. It sums up recent advances in nanotube composite synthesis technology, provides basic introduction to polymer nanotubes nanocomposite technology for the readers new to this field, provides valuable...

  18. Synthesis and structural and photoswitchable properties of novel chiral host molecules: axis chiral 2,2'-dihydroxy-1,1'-binaphthyl-appended stiff-stilbene.

    Science.gov (United States)

    Shimasaki, Toshiaki; Kato, Shin-ichiro; Ideta, Keiko; Goto, Kenta; Shinmyozu, Teruo

    2007-02-16

    Novel photoswitchable chiral hosts having an axis chiral 2,2'-dihydroxy-1,1'-binaphthyl (BINOL)-appended stiff-stilbene, trans-(R,R)- and -(S,S)-1, were synthesized by palladium-catalyzed Suzuki-Miyaura coupling and low-valence titanium-catalyzed McMurry coupling as key steps, and they were fully characterized by various NMR spectral techniques. The enantiomers of trans-1 showed almost complete mirror images in the CD spectra, where two split Cotton effects (exciton coupling) were observed in the beta-transitions of the naphthyl chromophore at 222 and 235 nm, but no Cotton effect was observed in the stiff-stilbene chromophore at 365 nm. The structures of (R)-10 and trans-(R,R)-1 were confirmed by X-ray structural analysis. The optimized structure of cis-1 by MO calculations has a wide chiral cavity of 7-8 A in diameter, whereas trans-1 cannot form an intramolecular cavity based on the X-ray data. Irradiation of (R,R)-trans-1 with black light (lambda = 365 nm) in CH3CN or benzene at 23 degrees C led to the conversion to the corresponding cis-isomer, as was monitored by 1H NMR, UV-vis, and CD spectra. At the photostationary state, the cis-1/trans-1 ratio was 86/14 in benzene or 75/25 in CH3CN. On the other hand, irradiation of the cis-1/trans-1 (75/25) mixture in CH3CN with an ultra-high-pressure Hg lamp at 23 degrees C (lambda = 410 nm) led to the photostationary state, where the cis-1/trans-1 ratio was estimated to be 9/91 on the basis of the 1H NMR spectra. The cis-trans and trans-cis interconversions could be repeated 10 times without decomposition of the C=C double bond. Thus, a new type of photoswitchable molecule has been developed, and trans-1 and cis-1 were quite durable under irradiation conditions. The guest binding properties of the BINOL moieties of trans- and cis-(R,R)-1 with F-, Cl-, and H2PO4- were examined by 1H NMR titration in CDCl3. Similar interaction with F- and Cl- was observed in trans-1 (host/guest = 1/1, Kassoc = (1.0 +/- 0.13) x 103 for F

  19. Total synthesis, structure, and oral absorption of a thiazole cyclic peptide, sanguinamide A

    DEFF Research Database (Denmark)

    Nielsen, Daniel S; Hoang, Huy N; Lohman, Rink-Jan

    2012-01-01

    The first total synthesis and three-dimensional solution structure are reported for sanguinamide A, a thiazole-containing cyclic peptide from the sea slug H. sanguineus. Solution phase fragment synthesis, solid phase fragment assembly, and solution macrocyclization were combined to give (1) in 10......% yield. Spectral properties were identical for the natural product, requiring revision of its structure from (2) to (1). Intramolecular transannular hydrogen bonds help to bury polar atoms, which enables oral absorption from the gut....

  20. Structure, bioactivity, and synthesis of methylated flavonoids.

    Science.gov (United States)

    Wen, Lingrong; Jiang, Yueming; Yang, Jiali; Zhao, Yupeng; Tian, Miaomiao; Yang, Bao

    2017-06-01

    Methylated flavonoids are an important type of natural flavonoid derivative with potentially multiple health benefits; among other things, they have improved bioavailability compared with flavonoid precursors. Flavonoids have been documented to have broad bioactivities, such as anticancer, immunomodulation, and antioxidant activities, that can be elevated, to a certain extent, by methylation. Understanding the structure, bioactivity, and bioavailability of methylated flavonoids, therefore, is an interesting topic with broad potential applications. Though methylated flavonoids are widely present in plants, their levels are usually low. Because developing efficient techniques to produce these chemicals would likely be beneficial, we provide an overview of their chemical and biological synthesis. © 2017 New York Academy of Sciences.

  1. Synthesis of Structures Related to Antifreeze Glycoproteins

    OpenAIRE

    Fyrner, Timmy

    2005-01-01

    In this thesis, synthesis of structures related to antifreeze glycoproteins (AFGPs) are presented. Synthetic routes to a protected carbohydrate derivative, 2,3,4,6-tetra-O-benzyl-β-galactopyranosyl-(1→3)-2-deoxy-2-azido-4,6-di-O-benzyl-β-D-thio-1-galactopyranoside, and a tBu-Ala-Thr-Ala-Fmoc tripeptide, are described. These compounds are meant to be used in the assembly of AFGPs and analogues thereof. A Gal-GlcN disaccharide was synthesized via glycosylation between the donor, bromo-2-O-benzo...

  2. Synthesis, Optical Properties and Applications for New Trianguleniums Derivatives

    DEFF Research Database (Denmark)

    Santella, Marco

    The development of new types of emissive organic dyes is an exciting area of research due to the applicability of these compounds in a wide range of disciplines. Cationic triangulenium salts are highly stable carbenium ions with a planar conformation. The convenient and versatile synthetic proced...... focused on the synthesis of thioether para substituted dyes, where the reactivity of various para-methoxy substituted propeller shaped cations towards different alkyl thiols was examined. Furthermore, ringclosure reactions of these thioether bearing propellers in order to obtain trioxa...... structures. These dyes possess excellent emissive properties with possible applications as cell staining agents or as fluorescent probes. Lastly, I focused on the use of triangulenes as binding group for molecular electronics. It has been shown that TATA can form self-assembled monolayers (SAMs) on a gold...

  3. Two series of reactant's ratio-dependent lanthanide organic frameworks derived from nicotinic acid N-oxide and oxalate: synthesis, crystal structures and luminescence properties.

    Science.gov (United States)

    Yu, Yanyan; Zhang, Lijuan; Zhou, Yunshan; Zuhra, Zareen

    2015-03-14

    Two series of lanthanide(III)–organic frameworks with the molecular formula [Ln2(NNO)2(OX)2(H2O)4]n (Ln = Eu 1, Tb 2, Sm 3, Dy 4, Gd 5) and [Ln2(NNO)4(OX)(H2O)2]n (Ln = Eu 6, Tb 7, Sm 8, Dy 9, Gd 10) were synthesized successfully under the same hydrothermal conditions with nicotinic N-oxide (HNNO) and oxalic acid (H2OX) as the mixed ligands merely through varying the molar ratio of the reactants. The compounds were characterized by IR, elemental analysis, UV, TG-DTA and powder X-ray diffraction (XRD). X-ray single-crystal diffraction analyses of compounds 1 and 7 selected as representatives and powder XRD analysis of the compounds revealed that both the series of compounds feature three-dimensional (3-D) open frameworks, and crystallize in the triclinic P1 space group while with different unit cell parameters. In compound 1, pairs of Eu(3+) ions and pairs of NNO(−) ligands connect with each other alternately to form a 1-D infinite Eu-NNO double chain, the adjacent 1-D double-chains are then joined together through OX(2−) ligands leading to a 2D layer, the 2-D layers are further ‘pillared’ by OX(2−) ligands resulting in a 3-D framework. In compound 7, the 1-D Tb-NNO infinite chain and its 2-D layer are formed in an almost similar fashion to that in compound 1. The difference between the structures of the two compounds 1 and 7 is that the adjacent 2-D layers in compound 7 are further connected by NNO(−) ligands resulting in a 3-D framework. The photoluminescence properties and energy transfer mechanism of the compounds were studied systematically. The energy level of the lowest triplet states of the HNNO ligand (23148 cm(−1)) was determined based on the phosphorescence spectrum of compound 5 at 77 K. The (5)D0 (Eu(3+)) and (5)D4 (Tb(3+)) emission lifetimes are 0.46 ms, 0.83 ms, 0.69 ms and 0.89 ms and overall quantum yields are 1.03%, 3.29%, 2.58% and 3.78% for the compounds 1, 2, 6 and 7, respectively.

  4. Synthesis and structure of two-dimensional transition-metal dichalcogenides

    KAUST Repository

    Shi, Yumeng; Zhang, Hua; Chang, Wen-Hao; Shin, Hyeon Suk; Li, Lain-Jong

    2015-01-01

    Two-dimensional (2D) transition-metal dichalcogenides (TMDCs) exhibit unique electrical, optical, thermal, and mechanical properties, which enable them to be used as building blocks in compact and lightweight integrated electronic systems. The controllable and reliable synthesis of atomically thin TMDCs is essential for their practical application. Recent progress in large-area synthesis of monolayer TMDCs paves the way for practical production of various 2D TMDC layers. The intrinsic optical and electrical properties of monolayer TMDCs can be defined by stoichiometry during synthesis. By manipulating the lattice structure or layer stacking manner, it is possible to create atomically thin van der Waals materials with unique and unexplored physical properties. In this article, we review recent developments in the synthesis of TMDC monolayers, alloys, and heterostructures, which shine light on the design of novel TMDCs with desired functional properties.

  5. Synthesis and structure of two-dimensional transition-metal dichalcogenides

    KAUST Repository

    Shi, Yumeng

    2015-07-13

    Two-dimensional (2D) transition-metal dichalcogenides (TMDCs) exhibit unique electrical, optical, thermal, and mechanical properties, which enable them to be used as building blocks in compact and lightweight integrated electronic systems. The controllable and reliable synthesis of atomically thin TMDCs is essential for their practical application. Recent progress in large-area synthesis of monolayer TMDCs paves the way for practical production of various 2D TMDC layers. The intrinsic optical and electrical properties of monolayer TMDCs can be defined by stoichiometry during synthesis. By manipulating the lattice structure or layer stacking manner, it is possible to create atomically thin van der Waals materials with unique and unexplored physical properties. In this article, we review recent developments in the synthesis of TMDC monolayers, alloys, and heterostructures, which shine light on the design of novel TMDCs with desired functional properties.

  6. Synthesis, structure and optical properties of thin films form GeS2-In2S3 system deposited by thermal co-evaporation

    Czech Academy of Sciences Publication Activity Database

    Todorov, R.; Petkov, K.; Kincl, Miloslav; Černošková, E.; Vlček, Milan; Tichý, Ladislav

    2014-01-01

    Roč. 558, 2 May (2014), s. 298-305 ISSN 0040-6090 Institutional support: RVO:61389013 Keywords : chalcogenide glasses * thin films * optical properties Subject RIV: CA - Inorganic Chemistry Impact factor: 1.759, year: 2014

  7. The synthesis and decay properties of the heaviest elements

    International Nuclear Information System (INIS)

    Oganesyan, Yu.Ts.

    2000-01-01

    The synthesis and the study of radioactive properties of new elements is considered with respect to the existence of the 'islands of stability' of hypothetical superheavy elements predicted by the theory more than 35 years ago. Experimental data demonstrating an enhanced stability of nuclei in the vicinity of deformed shells with Z=108 and N=162 is discussed from the point of view of advent into more heavy and much more stable nuclides near the predicted spherical shells Z=114-122 and N=184 following after the doubly magic nucleus 208 Pb. The author presents the results of experiments on the synthesis of isotopes of elements 114 and 116 in the fusion reactions with 48 Ca. In these reactions the decay chains of heavy atoms consisting of sequential α-decays interrupted by spontaneous fission have been observed. The decay energies and probabilities are compared with predictions of different theoretical models describing the structure of heavy nuclei. The obtained results are considered as the first experimental evidence of the existence of domains of stability of superheavy nuclei which substantially extends the boundaries of existence of chemical elements

  8. The Synthesis and Decay Properties of the Heaviest Elements

    CERN Document Server

    Oganessian, Yu T

    2000-01-01

    The synthesis and the study of radioactive properties of new elements is considered with respect to the existence of the "islands of stability" of hypothetical superheavy elements predicted by the theory more than 35 years ago. Experimental data demonstrating an enhanced stability of nuclei in the vicinity of deformed shells with Z=108 and N=162 is discussed from the point of view of advent into more heavy and much more stable nuclides near the predicted spherical shells Z=114-122 and N=184 following after the doubly magic nucleus ^{208}Pb. The author presents the results of experiments on the synthesis of isotopes of elements 114 and 116 in the fusion reactions with ^{48}Ca. In these reactions the decay chains of heavy atoms consisting of sequential alpha-decays interrupted by spontaneous fission have been observed. The decay energies and probabilities are compared with predictions of different theoretical models describing the structure of heavy nuclei. The obtained results are considered as the first exper...

  9. Plasma synthesis of nanostructures for improved thermoelectric properties

    International Nuclear Information System (INIS)

    Petermann, Nils; Hecht, Christian; Schulz, Christof; Wiggers, Hartmut; Stein, Niklas; Schierning, Gabi; Theissmann, Ralf; Stoib, Benedikt; Brandt, Martin S

    2011-01-01

    The utilization of silicon-based materials for thermoelectrics is studied with respect to the synthesis and processing of doped silicon nanoparticles from gas phase plasma synthesis. It is found that plasma synthesis enables the formation of spherical, highly crystalline and soft-agglomerated materials. We discuss the requirements for the formation of dense sintered bodies, while keeping the crystallite size small. Small particles a few tens of nanometres and below that are easily achievable from plasma synthesis, and a weak surface oxidation, both lead to a pronounced sinter activity about 350 K below the temperature usually needed for the successful densification of silicon. The thermoelectric properties of our sintered materials are comparable to the best results found for nanocrystalline silicon prepared by methods other than plasma synthesis.

  10. Wall grid structure for interior scene synthesis

    KAUST Repository

    Xu, Wenzhuo

    2015-02-01

    We present a system for automatically synthesizing a diverse set of semantically valid, and well-arranged 3D interior scenes for a given empty room shape. Unlike existing work on layout synthesis, that typically knows potentially needed 3D models and optimizes their location through cost functions, our technique performs the retrieval and placement of 3D models by discovering the relationships between the room space and the models\\' categories. This is enabled by a new analytical structure, called Wall Grid Structure, which jointly considers the categories and locations of 3D models. Our technique greatly reduces the amount of user intervention and provides users with suggestions and inspirations. We demonstrate the applicability of our approach on three types of scenarios: conference rooms, living rooms and bedrooms.

  11. Synthesis and Properties of Group IV Graphane Analogues

    Science.gov (United States)

    Goldberger, Joshua

    Similar to how carbon networks can be sculpted into low-dimensional allotropes such as fullerenes, nanotubes, and graphene with fundamentally different properties, it is possible to create similar ligand terminated sp3-hybridized honeycomb graphane derivatives containing Ge or Sn that feature unique and tunable properties. Here, we will describe our recent success in the creation of hydrogen and organic-terminated group IV graphane analogues, from the topochemical deintercalation of precursor Zintl phases, such as CaGe2. We will discuss how the optical, electronic, and thermal properties of these materials can be systematically controlled by substituting either the surface ligand or via alloying with other Group IV elements. Additionally, we have also developed an epitopotaxial approach for integrating precise thicknesses of germanane layers onto Ge wafers that combines the epitaxial deposition of CaGe2 precursor phases with the topotactic interconversion into the 2D material. Finally, we will describe our recent efforts on the synthesis and crystal structures of Sn-containing graphane alloys in order to access novel topological phenomena predicted to occur in these graphanes.

  12. Superheavy Element Synthesis and Nuclear Structure

    International Nuclear Information System (INIS)

    Ackermann, D.

    2009-01-01

    The search for the next closed proton and neutron shells beyond 2 08P b has yielded a number of exciting results in terms of the synthesis of new elements [1,2,3]. The superheavy elements (SHE), however, are a nuclear structure phenomenon. They owe their existence to the quantum mechanical origin of shell correction energies without which they would not be bound. In recent years the development of efficient experimental set-ups including separators and advanced particle and photon detection arrangements allowed for more and more detailed nuclear structure studies for nuclei at and beyond Z=100. A review of those recent achievements is given in ref. [4]. Among the most interesting features is the observation of K-isomeric states. Experimentally about 14 cases have been identified in the region of Z>96 as shown in Fig. 1. K-isomers or indications of their existence have been found for almost all even-Z elements in the region Z=100 to 110. We could recently establish and/or confirm such states in the even-even isotopes 2 52,254N o [5]. The heaviest nucleus where such a state was found is 2 70D s with Z=110 as we reported in 2001 [6]. Those nuclear structure studies lay out the grounds for a detailed understanding of these heavy and high-Z nuclear systems, and contribute at the same time valuable information to preparation of strategies to successfully continue the hunt for the localisation of the next spherical proton and neutron shells after 2 08P b. The recent activities for both SHE synthesis and nuclear structure investigations at GSI will be reported.(author)

  13. Structural properties of matrix metalloproteinases.

    Science.gov (United States)

    Bode, W; Fernandez-Catalan, C; Tschesche, H; Grams, F; Nagase, H; Maskos, K

    1999-04-01

    Matrix metalloproteinases (MMPs) are involved in extracellular matrix degradation. Their proteolytic activity must be precisely regulated by their endogenous protein inhibitors, the tissue inhibitors of metalloproteinases (TIMPs). Disruption of this balance results in serious diseases such as arthritis, tumour growth and metastasis. Knowledge of the tertiary structures of the proteins involved is crucial for understanding their functional properties and interference with associated dysfunctions. Within the last few years, several three-dimensional MMP and MMP-TIMP structures became available, showing the domain organization, polypeptide fold and main specificity determinants. Complexes of the catalytic MMP domains with various synthetic inhibitors enabled the structure-based design and improvement of high-affinity ligands, which might be elaborated into drugs. A multitude of reviews surveying work done on all aspects of MMPs have appeared in recent years, but none of them has focused on the three-dimensional structures. This review was written to close the gap.

  14. The Synthesis and Luminescence-spectroscopic Properties of Fluorescent Condensation Polymers

    Science.gov (United States)

    Barashkov, Nikolai N.

    1985-07-01

    The results of studies on the synthesis of polycondensation phosphorus-containing aliphatic and aromatic polymers as well as the products of polymer-analogue transformations with phosphorus-groups in the side chain are examined. The light absorption and luminescent properties of the polymers obtained and of model compounds having an analogous structure are discussed. The bibliography includes 108 references.

  15. 2D and 3D organisation of nano-particles: synthesis and specific properties

    International Nuclear Information System (INIS)

    Taleb, Abdelhafed

    1998-01-01

    The first part of this research thesis addresses the synthesis of nano-particles of silver and cobalt in the inverse micellar system, and highlights the feasibility of two- and three-dimensional structures of these particles. The author first presents the micellar system (micro-emulsions, surfactant, properties of inverse micelles, functionalized inverse micelles, application to the synthesis of nano-particles), and then reports the study of the synthesis and organisation of colloids in 2D and 3D. He also reports the study of optical properties of metallic colloids: free electron approximation, optical properties of electron gases, optical properties of colloids, optical response of two-dimensional and three-dimensional nano-structures. The magnetic properties of colloids are then studied: magnetism of the massive metallic state, magnetic properties of nano-particles (influence of size, interactions and field, notions of magnetic order and disorder), effect of organisation. The second part of this thesis is made of a set of published articles: Synthesis of highly mono-disperse silver nano-particles from AOT reverse micelles (a way to 2D and 3D self-organisation), Optical properties of self-assembled 2D and 3D super-lattices of silver nano-particles, Collective optical properties of silver nano-particles organised in 2D super-lattices, Self assembled in 2D cobalt nano-sized particles, Self organisation of magnetic nano-sized cobalt particles, Organisation in 2D cobalt nano-particles (synthesis, characterization and magnetic properties) [fr

  16. Structure-controlled synthesis and electrochemical properties of NH_4V_3O_8 as cathode material for Lithium ion batteries

    International Nuclear Information System (INIS)

    Cheng, Yayi; Huang, Jianfeng; Li, Jiayin; Cao, Liyun; Xu, Zhanwei; Wu, Jianpeng; Cao, Shanshan; Hu, Hailing

    2016-01-01

    NH_4V_3O_8 flower, nanobelt, lath and sheet were synthesized using a facile microwave hydrothermal method. The formation mechanism of NH_4V_3O_8 with various structures was proposed. As an cathode in Li-ion battery, the NH_4V_3O_8 nanobelt with one-dimensional structure as well as nanosized morphology, presents excellent cycling stability and enhanced rate capability when comparing with other NH_4V_3O_8 structures. Further study finds that the NH_4V_3O_8 nanobelt could provide high Li ion diffusion, excellent structural stability and good reversibility during the charge/discharge process, indicating a strong connection between the morphology and the electrochemical performance of NH_4V_3O_8 cathode.

  17. Synthesis, microstructures and properties of {gamma}-aluminum oxynitride

    Energy Technology Data Exchange (ETDEWEB)

    Wang Xidong; Wang Fuming; Li Wenchao

    2003-02-15

    This paper deals with the synthesis, microstructures and properties of {gamma}-aluminum oxynitride (AlON). The thermodynamic properties of AlON were analyzed and the Gibbs energy of AlON with different compositions and temperatures were evaluated. Based on thermodynamic studies, AlON has been synthesized. The microstructures, mechanical properties and oxidation resistance of the synthetic AlON have been examined and discussed.

  18. Synthesis, structural and surface morphological characterizations of ...

    African Journals Online (AJOL)

    Sulfated zirconia (SZ) nanoparticles (NPs) were successfully synthesized and deposited via chemical route called sol-gel technique. The structural, morphological, and optical properties the samples were investigated by X-ray diffraction (XRD), Energy Dispersive X-ray Spectrometry (EDX), Scanning Electron Microscopy ...

  19. Synthesis, characterization and crystal structure of a ...

    African Journals Online (AJOL)

    The Mo atom in the complex is in octahedral coordination. Thermal stability of the complex has also been studied. KEY WORDS: Molybdenum complex, Hydrazone ligand, Crystal structure, X-ray diffraction, Thermal property. Bull. Chem. Soc. Ethiop. 2014, 28(3), 409-414. DOI: http://dx.doi.org/10.4314/bcse.v28i3.10 ...

  20. The synthesis of porous Co3O4 micro cuboid structures by solvothermal approach and investigation of its gas sensing properties and catalytic activity

    International Nuclear Information System (INIS)

    Jamil, Saba; Jing, Xiaoyan; Wang, Jun; Li, Songnan; Liu, Jingyuan; Zhang, Milin

    2013-01-01

    Graphical abstract: - Highlights: • Micro cuboid Co 3 O 4 particle prepared by solvothermal method. • Study of morphology of synthesized cuboids before and after calcinations. • Investigation of formation mechanism of porous Co 3 O 4 from cuboid CoCO 3 . • Investigation of gas sensing properties of porous Co 3 O 4 . • Study of catalytic activity of product. - Abstract: The cobalt carbonate cuboids are prepared by adopting a simple solvothermal approach by using diethylene glycol and water in specific ratio as solvent. The prepared cobalt carbonate is subjected to different instrumentation to investigate its morphology and other properties. It is clear from the scanning electron microscopy (SEM) and transmission electron microscopy (TEM) that the product is distinct cuboid in shape with a size of approximately 3 μm from each face of the cube. Each particle of cuboid cobalt carbonate seems to comprise of layer by layer assembly of unit cells that consequently leads to a cuboid geometry. The cuboid cobalt carbonate was calcined at 700 °C in a furnace under argon atmosphere that decompose cobalt carbonate into porous Co 3 O 4 with the loosely packed arrangement of nano architectures. The gas sensing properties and catalytic activity of porous cuboids Co 3 O 4 are also investigated

  1. Mercury coordination polymers with flexible ethane-1,2-diyl-bis-(pyridyl-3-carboxylate): Synthesis, structures, thermal and luminescent properties

    Energy Technology Data Exchange (ETDEWEB)

    Vallejos, Javier [Departamento de Química, Universidad Católica del Norte, Av. Angamos 0610, Antofagasta (Chile); Brito, Iván, E-mail: ivanbritob@yahoo.com [Departamento de Quimica, Universidad de Antofagasta, Av. Angamos 601, Antofa