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Sample records for newin-situ synthesis method

  1. High-gravity combustion synthesis and in situ melt infiltration: A new method for preparing cemented carbides

    International Nuclear Information System (INIS)

    Liu, Guanghua; Li, Jiangtao; Yang, Zengchao; Guo, Shibin; Chen, Yixiang

    2013-01-01

    A new method of high-gravity combustion synthesis and in situ melt infiltration is reported for preparing cemented carbides, where hot nickel melt is in situ synthesized from a highly exothermic combustion reaction and then infiltrated into tungsten carbide powder compacts. The as-prepared sample showed a homogeneous microstructure, and its relative density, hardness and flexural strength were 94.4%, 84 HRA and 1.49 GPa, respectively. Compared with conventional powder metallurgy approaches, high-gravity combustion synthesis offers a fast and furnace-free way to produce cemented carbides

  2. NewIn-situ synthesis method of magnesium matrix composites reinforced with TiC particulates

    Directory of Open Access Journals (Sweden)

    Zhang Xiuqing

    2006-12-01

    Full Text Available Magnesium matrix composites reinforced with TiC particulates was prepared using a new in-situ synthesis method of remelting and dilution technique. And measurements were performed on the composites. The results of x ray diffraction (XRD analysis confirmed that TiC particulates were synthesized during the sintering process, and they retained in magnesium matrix composites after the remelting and dilution processing. From the microstructure characterization and electron probe microanalysis (EPMA, we could see that fine TiC particulates distributed uniformly in the matrix material.

  3. A bio-inspired approach for in situ synthesis of tunable adhesive

    International Nuclear Information System (INIS)

    Sun, Leming; Yi, Sijia; Wang, Yongzhong; Pan, Kang; Zhong, Qixin; Zhang, Mingjun

    2014-01-01

    Inspired by the strong adhesive produced by English ivy, this paper proposes an in situ synthesis approach for fabricating tunable nanoparticle enhanced adhesives. Special attention was given to tunable features of the adhesive produced by the biological process. Parameters that may be used to tune properties of the adhesive will be proposed. To illustrate and validate the proposed approach, an experimental platform was presented for fabricating tunable chitosan adhesive enhanced by Au nanoparticles synthesized in situ. This study contributes to a bio-inspired approach for in situ synthesis of tunable nanocomposite adhesives by mimicking the natural biological processes of ivy adhesive synthesis. (paper)

  4. Hydrothermal Synthesis of Disulfide-Containing Uranyl Compounds. In Situ Ligand Synthesis versus Direct Assembly

    Energy Technology Data Exchange (ETDEWEB)

    Rowland, Clare E. [George Washington Univ., Washington, DC (United States); Belai, Nebebech [George Washington Univ., Washington, DC (United States); Knope, Karah E. [George Washington Univ., Washington, DC (United States); Cahill, Christopher L. [George Washington Univ., Washington, DC (United States)

    2010-01-29

    Three disulfide-containing uranyl compounds, [UO2(C7H4O2S)3]·H2O (1), [UO2(C7H4O2S)2(C7H5O2S)] (2), and [UO2(C7H4O2S)4] (3) have been hydrothermally synthesized. Both in situ disulfide bond formation from 3- and 4-mercaptobenzoic acid (C7H5O2S, MBA) to yield 3,3'- and 4,4'-dithiobisbenzoic acid (C14H8O4S2, DTBA) and direct assembly with the presynthesized dimeric ligands have been explored. While the starting materials 4-MBA and 4,4'-DTBA both yield 2 via in situ ligand synthesis and direct assembly, respectively, we observe the formation of 1 from the starting material 3-MBA via in situ ligand synthesis and of 3 from the direct assembly of the uranyl cation with 3,3'-DTBA. Concurrently with the synthesis of 1 and 2, we have observed the in situ formation of the crystalline dimeric organic species, 3,3'-DTBA, [(C7H5O2S)2] (4) and 4,4'-DTBA, [(C7H5O2S)2] (5). Herein we report the synthesis and crystallographic characterization of 1-5, as well as observations regarding the utility of product formation via direct assembly and in situ ligand synthesis.

  5. In situ synthesis of silver benzene-dithiolate hybrid films

    Energy Technology Data Exchange (ETDEWEB)

    Brenier, Roger, E-mail: roger.brenier@univ-lyon1.fr [Institut Lumière Matière, UMR 5306, Université Lyon 1-CNRS, Université de Lyon, Domaine Scientifique de La Doua, Batiment Kastler, 10 rue Ada Byron, 69622 Villeurbanne, Cedex (France); Piednoir, Agnès, E-mail: agnes.piednoir@univ-lyon1.fr [Institut Lumière Matière, UMR 5306, Université Lyon 1-CNRS, Université de Lyon, Domaine Scientifique de La Doua, Batiment Kastler, 10 rue Ada Byron, 69622 Villeurbanne, Cedex (France); Bertorelle, Franck, E-mail: franck.bertorelle@univ-lyon1.fr [Institut Lumière Matière, UMR 5306, Université Lyon 1-CNRS, Université de Lyon, Domaine Scientifique de La Doua, Batiment Kastler, 10 rue Ada Byron, 69622 Villeurbanne, Cedex (France); Penuelas, José, E-mail: jose.penuelas@ec-lyon.fr [Université de Lyon, Institut des Nanotechnologies de Lyon, Ecole Centrale de Lyon, CNRS, UMR 5270, 36 rue Guy de Collongues, F69134 Ecully (France); Grenet, Geneviève, E-mail: genevieve.grenet@ec-lyon.fr [Université de Lyon, Institut des Nanotechnologies de Lyon, Ecole Centrale de Lyon, CNRS, UMR 5270, 36 rue Guy de Collongues, F69134 Ecully (France)

    2016-02-01

    In this article, a method for in situ synthesis of silver benzene-dithiolate hybrid films is presented. Silver nanoparticles, generated on ZrO{sub 2} films, are transformed into silver benzene 1,4-dithiolate or, partially, into silver benzene 1,2-dithiolate after sample immersion in the corresponding thiol solutions. These transformations occur at room temperature owing to the catalytic action of ZrO{sub 2}. It is also shown that TiO{sub 2} in place of ZrO{sub 2} is very efficient, both for the catalytic generation of silver nanoparticles and for their further transformation in benzene 1,4-dithiolate compound. This latter semiconductor has an optical bandgap of about 3 eV and the film is made of touching nanoparticles in an amorphous state. Our work has potential applications in the electronic and photovoltaic fields. - Highlights: • A method for in situ synthesis of silver benzene-dithiolate hybrid semiconductor films is presented. • Silver nanoparticles are, first, generated on ZrO{sub 2} or on TiO{sub 2} coated silica substrates. • The samples are immersed in benzene dithiol solution for two days at room temperature. • During the immersion, the silver nanoparticles are transformed into silver benzene dithiolate. • The silver benzene dithiolate film is made of amorphous nanoparticles with a banbgap of 3 eV.

  6. Solvent-assisted in situ synthesis of cysteamine-capped silver nanoparticles

    Science.gov (United States)

    Oliva, José M.; Ríos de la Rosa, Julio M.; Sayagués, María J.; Sánchez-Alcázar, José A.; Merkling, Patrick J.; Zaderenko, Ana P.

    2018-03-01

    Silver nanoparticles offer a huge potential for biomedical applications owing to their exceptional properties and small size. Specifically, cysteamine-capped silver nanoparticles could form the basis for new anticancer therapies combining the cytotoxic effect of the silver core with the inherent antitumor activity of cysteamine, which inhibit cancer cell proliferation and suppress invasion and metastasis. In addition, the capability of the cysteamine coating monolayer to couple a variety of active principles and targeting (bio)molecules of interest proves key to the tailoring of this platform in order to exploit the pathophysiology of specific tumor types. Nevertheless, the chain length and conformational flexibility of cysteamine, together with its ability to attach to the surface of silver nanoparticles via both the thiol and the amine group, have made the in situ synthesis of these particles an especially challenging task. Herein we report a solvent-assisted in situ synthesis method that solves this problem. The obtained nanoparticles have been fully characterized by UV-visible absorption spectroscopy, Fourier transform infrared spectroscopy, transmission electron microscopy, electron diffraction measurement, high resolution transmission electron microscopy, scanning transmission electron microscopy, energy dispersive x-ray spectroscopy nanoanalysis, and dynamic light scattering measurement. Our synthesis method achieves extremely high yield and surface coating ratio, and colloidal stability over a wide range of pH values including physiological pH. Additionally, we have demonstrated that cysteamine-capped nanoparticles obtained by this method can be conjugated to an antibody for active targeting of the epidermal growth factor receptor, which plays an important role in the pathogenesis and progression of a wide variety of tumors, and induce cell death in human squamous carcinoma cells. We believe this method can be readily extended to combinations of noble

  7. Characterization and electrochemical performances of MoO2 modified LiFePO4/C cathode materials synthesized by in situ synthesis method

    International Nuclear Information System (INIS)

    He, Jichuan; Wang, Haibin; Gu, Chunlei; Liu, Shuxin

    2014-01-01

    Graphical abstract: The MoO 2 modified LiFePO 4 /C cathode materials were synthesized by in situ synthesis method. MoO 2 can sufficiently coat on the LiFePO 4 /C particles surface and does not alter LiFePO 4 crystal structure, and the adding of MoO 2 decreases the particles size and increases the tap density of cathode materials. The existence of MoO 2 improves electrochemical performance of LiFePO 4 cathode materials in specific capability and lithium ion diffusion and charge transfer resistance of cathode materials. - Highlights: • The MoO 2 modified LiFePO 4 /C cathode materials were synthesized by in situ synthesis method. • The existence of MoO 2 decreases the particles size and increases the tap density of cathode materials. • MoO 2 can sufficiently coat on the surface of LiFePO 4 /C cathode materials. • The existence of MoO 2 enhanced electrochemical performance of LiFePO 4 /C cathode materials. - Abstract: The MoO 2 modified LiFePO 4 /C cathode materials were synthesized by in situ synthesis method. Phase compositions and microstructures of the products were characterized by X-ray powder diffraction (XRD), SEM, TEM and EDS. Results indicate that MoO 2 can sufficiently coat on the LiFePO 4 surface and does not alter LiFePO 4 crystal structure, the existence of MoO 2 decreases the particles size and increases the tap density of cathode materials. The electrochemical behavior of cathode materials was analyzed using galvanostatic measurement, cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS). The results show that the existence of MoO 2 improves electrochemical performance of LiFePO 4 cathode materials in specific capability and lithium ion diffusion and charge transfer resistance. The initial charge–discharge specific capacity and apparent lithium ion diffusion coefficient increase, the charge transfer resistance decreases with MoO 2 content and maximizes around the MoO 2 content is 5 wt%. It has been had further proved that

  8. In situ X-ray powder diffraction studies of the synthesis of graphene oxide and formation of reduced graphene oxide

    International Nuclear Information System (INIS)

    Storm, Mie Møller; Johnsen, Rune E.; Norby, Poul

    2016-01-01

    Graphene oxide (GO) and reduced graphene oxide (rGO) are important materials in a wide range of fields. The modified Hummers methods, for synthesizing GO, and subsequent thermal reduction to rGO, are often employed for production of rGO. However, the mechanism behinds these syntheses methods are still unclear. We present an in situ X-ray diffraction study of the synthesis of GO and thermal reduction of GO. The X-ray diffraction revealed that the Hummers method includes an intercalation state and finally formation of additional crystalline material. The formation of GO is observed during both the intercalation and the crystallization stage. During thermal reduction of GO three stages were observed: GO, a disordered stage, and the rGO stage. The appearance of these stages depends on the heating ramp. The aim of this study is to provide deeper insight into the chemical and physical processes during the syntheses. - Graphical abstract: In situ X-ray diffraction results for of the modified Hummers synthesis and the thermal reduction of graphene oxide, revealing three stages for both syntheses as well as new GO diffraction peaks and unidentified crystalline material for the Hummers synthesis and a disordered stage for the thermal reduction of graphene oxide. Display Omitted - Highlights: • Hummers synthesis consists of three stages: dissolution, intercalation and crystal. • GO is produced early on during the synthesis and display new diffraction peaks. • An unidentified triclinic phase is observed for the Hummers synthesis. • Thermal reduction of GO display three stages: GO, a disordered stage and rGO. • In situ XRD indicate reformation of rGO even for fast heated thermal reduction.

  9. In situ X-ray powder diffraction studies of the synthesis of graphene oxide and formation of reduced graphene oxide

    Energy Technology Data Exchange (ETDEWEB)

    Storm, Mie Møller, E-mail: mmst@dtu.dk; Johnsen, Rune E.; Norby, Poul

    2016-08-15

    Graphene oxide (GO) and reduced graphene oxide (rGO) are important materials in a wide range of fields. The modified Hummers methods, for synthesizing GO, and subsequent thermal reduction to rGO, are often employed for production of rGO. However, the mechanism behinds these syntheses methods are still unclear. We present an in situ X-ray diffraction study of the synthesis of GO and thermal reduction of GO. The X-ray diffraction revealed that the Hummers method includes an intercalation state and finally formation of additional crystalline material. The formation of GO is observed during both the intercalation and the crystallization stage. During thermal reduction of GO three stages were observed: GO, a disordered stage, and the rGO stage. The appearance of these stages depends on the heating ramp. The aim of this study is to provide deeper insight into the chemical and physical processes during the syntheses. - Graphical abstract: In situ X-ray diffraction results for of the modified Hummers synthesis and the thermal reduction of graphene oxide, revealing three stages for both syntheses as well as new GO diffraction peaks and unidentified crystalline material for the Hummers synthesis and a disordered stage for the thermal reduction of graphene oxide. Display Omitted - Highlights: • Hummers synthesis consists of three stages: dissolution, intercalation and crystal. • GO is produced early on during the synthesis and display new diffraction peaks. • An unidentified triclinic phase is observed for the Hummers synthesis. • Thermal reduction of GO display three stages: GO, a disordered stage and rGO. • In situ XRD indicate reformation of rGO even for fast heated thermal reduction.

  10. In Situ Synthesis of Metal Nanoparticle Embedded Hybrid Soft Nanomaterials.

    Science.gov (United States)

    Divya, Kizhmuri P; Miroshnikov, Mikhail; Dutta, Debjit; Vemula, Praveen Kumar; Ajayan, Pulickel M; John, George

    2016-09-20

    The allure of integrating the tunable properties of soft nanomaterials with the unique optical and electronic properties of metal nanoparticles has led to the development of organic-inorganic hybrid nanomaterials. A promising method for the synthesis of such organic-inorganic hybrid nanomaterials is afforded by the in situ generation of metal nanoparticles within a host organic template. Due to their tunable surface morphology and porosity, soft organic materials such as gels, liquid crystals, and polymers that are derived from various synthetic or natural compounds can act as templates for the synthesis of metal nanoparticles of different shapes and sizes. This method provides stabilization to the metal nanoparticles by the organic soft material and advantageously precludes the use of external reducing or capping agents in many instances. In this Account, we exemplify the green chemistry approach for synthesizing these materials, both in the choice of gelators as soft material frameworks and in the reduction mechanisms that generate the metal nanoparticles. Established herein is the core design principle centered on conceiving multifaceted amphiphilic soft materials that possess the ability to self-assemble and reduce metal ions into nanoparticles. Furthermore, these soft materials stabilize the in situ generated metal nanoparticles and retain their self-assembly ability to generate metal nanoparticle embedded homogeneous organic-inorganic hybrid materials. We discuss a remarkable example of vegetable-based drying oils as host templates for metal ions, resulting in the synthesis of novel hybrid nanomaterials. The synthesis of metal nanoparticles via polymers and self-assembled materials fabricated via cardanol (a bioorganic monomer derived from cashew nut shell liquid) are also explored in this Account. The organic-inorganic hybrid structures were characterized by several techniques such as UV-visible spectroscopy, scanning electron microscopy (SEM), and

  11. In situ synthesis of nanocomposite membranes: comprehensive improvement strategy for direct methanol fuel cells.

    Science.gov (United States)

    Rao, Siyuan; Xiu, Ruijie; Si, Jiangju; Lu, Shanfu; Yang, Meng; Xiang, Yan

    2014-03-01

    In situ synthesis is a powerful approach to control nanoparticle formation and consequently confers extraordinary properties upon composite membranes relative to conventional doping methods. Herein, uniform nanoparticles of cesium hydrogen salts of phosphotungstic acid (CsPW) are controllably synthesized in situ in Nafion to form CsPW–Nafion nanocomposite membranes with both improved proton conductivity and methanol-crossover suppression. A 101.3% increase of maximum power density has been achieved relative to pristine Nafion in a direct methanol fuel cell (DMFC), indicating a potential pathway for large-scale fabrication of DMFC alternative membranes.

  12. In situ synthesis of copper nanoparticles on SBA-16 silica spheres

    Directory of Open Access Journals (Sweden)

    Asma Tufail Shah

    2016-07-01

    Full Text Available A chemical method for in situ synthesis of copper nanoparticles on SBA-16 silica spheres under ambient conditions has been reported. The silica support has been introduced into copper precursor solution before chemical reduction. Metal ions diffuse into mesopores (pore diameter 5–7 nm of silica where in situ reduction by hydrazine leads to formation of nanoparticles. These mesopores act as nanoreactor and their walls prevent metal particle’s agglomeration by providing a physical barrier. The obtained copper nanoparticles have been investigated by electron microscopy, X-ray diffraction, UV–Visible spectroscopy, Fourier transform Infra-red spectroscopy and thermogravimetric analyzer. SEM, TEM and UV–Visible spectroscopic images revealed that nanosized particles have been successfully synthesized by this method. Thermogravimetric investigations revealed that copper nanoparticles impregnated on silica were thermally more stable compared to unsupported nanoparticles. Silica not only helps in maintaining the particle size but also makes nanoparticles stable at high temperatures due to its thick pore walls. Macro sized silica support also makes separation/handling of nanoparticles easy and simple.

  13. Synthesis of nanosized (polymerization in miniemulsion employing in situ surfactant formation.

    Science.gov (United States)

    Guo, Yi; Zetterlund, Per B

    2011-10-18

    A novel method for synthesis of ultrafine polymeric nanoparticles of diameters less than 20 nm has been developed. The method is based on miniemulsion polymerization exploiting combination of the in situ surfactant generation approach (whereby the surfactant is formed at the oil-water interface by reaction between an organic acid and a base) and ultrasonication. Conventional radical polymerization and nitroxide-mediated radical polymerization of styrene have been conducted in miniemulsion using oleic acid/potassium hydroxide, demonstrating that particles with diameters less than 20 nm can be obtained by this approach at surfactant contents much lower than traditionally required in microemulsion polymerizations. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  14. Synthesis of mesoporous zeolite catalysts by in situ formation of carbon template over nickel nanoparticles

    DEFF Research Database (Denmark)

    Abildstrøm, Jacob Oskar; Kegnæs, Marina; Hytoft, Glen

    2016-01-01

    A novel synthesis procedure for the preparation of the hierarchical zeolite materials with MFI structure based on the carbon templating method with in situ generated carbon template is presented in this study. Through chemical vapour deposition of coke on nickel nanoparticles supported on silica...... oxide, a carbon-silica composite is obtained and exploited as a combined carbon template/silica source for zeolite synthesis. This approach has several advantages in comparison with conventional carbon templating methods, where relatively complicated preparative strategies involving multistep...... impregnation procedures and rather expensive chemicals are used. Removal of the carbon template by combustion results in zeolite single crystals with intracrystalline pore volumes between 0.28 and 0.48 cm3/g. The prepared zeolites are characterized by XRD, SEM, TEM and physisorption analysis. The isomerization...

  15. In situ X-ray powder diffraction, synthesis, and magnetic properties of InVO 3

    Science.gov (United States)

    Lundgren, Rylan J.; Cranswick, Lachlan M. D.; Bieringer, Mario

    2006-12-01

    We report the first synthesis and high-temperature in situ X-ray diffraction study of InVO 3. Polycrystalline InVO 3 has been prepared via reduction of InVO 4 using a carbon monoxide/carbon dioxide buffer gas. InVO 3 crystallizes in the bixbyite structure in space group Ia-3 (206) with a=9.80636(31) Å with In 3+/V 3+ disorder on the (8 b) and (24 d) cation sites. In situ powder X-ray diffraction experiments and thermal gravimetric analysis in a CO/CO 2 buffer gas revealed the existence of the metastable phase InVO 3. Bulk samples with 98.5(2)% purity were prepared using low-temperature reduction methods. The preparative methods limited the crystallinity of this new phase to approximately 225(50) Å. Magnetic susceptibility and neutron diffraction experiments suggest a spin-glass ground state for InVO 3.

  16. Combustion synthesis of advanced materials. [using in-situ infiltration technique

    Science.gov (United States)

    Moore, J. J.; Feng, H. J.; Perkins, N.; Readey, D. W.

    1992-01-01

    The combustion synthesis of ceramic-metal composites using an in-situ liquid infiltration technique is described. The effect of varying the reactants and their stoichiometry to provide a range of reactant and product species i.e. solids, liquids and gases, with varying physical properties e.g. thermal conductivity, on the microstructure and morphology of synthesized products is also described. Alternatively, conducting the combustion synthesis reaction in a reactive gas environment is also discussed, in which advantages can be gained from the synergistic effects of combustion synthesis and vapor phase transport. In each case, the effect of the presence or absence of gravity (density) driven fluid flow and vapor transport is discussed as is the potential for producing new and perhaps unique materials by conducting these SHS reactions under microgravity conditions.

  17. Synthesis of polypropylene/graphite nanocomposites by means of in situ polymerization

    International Nuclear Information System (INIS)

    Montagna, Larissa S.; Basso, Nara R.S.

    2009-01-01

    The nanotechnology presents a large field for research and development of new polymeric materials based in nanocomposites. This work is related to the synthesis of nanocomposites of polypropylene with graphite as filler. The sheets of graphite in nanometer dimensions were made by means of the chemical exfoliation and thermal treatment. The synthesis of the nanocomposites was carried through by means of the in situ polymerization using a metallocene catalyst and with different amounts of inorganic load (0,5; 1 and 2%). The synthesized nanocomposites were characterized by scanning electron microscopy (SEM) and X-Ray diffraction (XRD). (author)

  18. In situ synthesis of protein arrays.

    Science.gov (United States)

    He, Mingyue; Stoevesandt, Oda; Taussig, Michael J

    2008-02-01

    In situ or on-chip protein array methods use cell free expression systems to produce proteins directly onto an immobilising surface from co-distributed or pre-arrayed DNA or RNA, enabling protein arrays to be created on demand. These methods address three issues in protein array technology: (i) efficient protein expression and availability, (ii) functional protein immobilisation and purification in a single step and (iii) protein on-chip stability over time. By simultaneously expressing and immobilising many proteins in parallel on the chip surface, the laborious and often costly processes of DNA cloning, expression and separate protein purification are avoided. Recently employed methods reviewed are PISA (protein in situ array) and NAPPA (nucleic acid programmable protein array) from DNA and puromycin-mediated immobilisation from mRNA.

  19. In situ ETEM synthesis of NiGa alloy nanoparticles from nitrate salt solution

    DEFF Research Database (Denmark)

    Damsgaard, Christian Danvad; Duchstein, Linus Daniel Leonhard; Sharafutdinov, Irek

    2014-01-01

    Metallic alloy nanoparticles (NPs) are synthesized in situ in an environmental transmission electron microscope. Atomic level characterization of the formed alloy NPs is carried out at synthesis conditions by use of high-resolution transmission electron microscopy, electron diffraction and electron...

  20. In Situ Synchrotron X-Ray Diffraction Characterization of the Synthesis of Graphene Oxide and Reduced Graphene Oxide

    DEFF Research Database (Denmark)

    Storm, Mie Møller; Johnsen, Rune E.; Norby, Poul

    2015-01-01

    Graphene oxide (GO) and reduced graphene oxide (rGO) synthesised from GO, has a promising future in fields ranging from electronics to energy technologies[1]. GO may be synthesized by the modified Hummer’s method[2], where a mixture of potassium permanganate and concentrated sulfuric acid forms...... by placing a mixture of permanganate and sulphuric acid in a capillary next to graphite. The synthesis was then initiated by gently pushing the fluid mixture into the powder with N2 gas. The in situ XRD of the GO synthesis showed how the oxidation reaction proceeds in three separate stages, as seen in Figure...... 1. The first stage was the dissolution of potassium permanganate, followed by an intercalation stage and subsequent formation of crystalline material. The GO 001 diffraction peak was observed early during the synthesis, in the second stage, and the intensity of the 001 diffraction increased during...

  1. In situ environmental transmission electron microscope investigation of NiGa nanoparticle synthesis

    DEFF Research Database (Denmark)

    Damsgaard, Christian Danvad; Duchstein, Linus Daniel Leonhard; Elkjær, Christian Fink

    2011-01-01

    . Both Ni and Ga edges are observed in the spectra. Quantification of Ni:Ga ratio is hampered by the presence of the Ni L1 edge. The ETEM experiments have been supported by complementary in situ X-Ray Diffraction (XRD) measurements on synthesis of Ni5Ga3 catalyst on a high surface area silica support...... prepared by wet impregnation [2]. Although the in situ XRD was performed at significantly higher H2 flow (40 Nml/min) and pressure (100 kPa) the complimentary data correlates with the main temperature dependence of phase and structure and shows formation of the Ni5Ga3 phase for temperatures higher than 300...

  2. Comparison of in Situ and ex Situ Methods for Synthesis of Two-Photon Polymerization Polymer Nanocomposites

    Directory of Open Access Journals (Sweden)

    Qingchuan Guo

    2014-07-01

    Full Text Available This article reports about nanocomposites, which refractive index is tuned by adding TiO2 nanoparticles. We compare in situ/ex situ preparation of nanocomposites. Preparation procedure is described, properties of nanocomposites are compared, and especially we examine the applicability of two-photon polymerization (2PP of synthesized nanocomposites. All prepared samples exhibit suitable optical transparency at specific laser wavelengths. Three-dimensional structures were generated by means of two-photon polymerization effect induced by a femtosecond laser.

  3. Biomimetic composite microspheres of collagen/chitosan/nano-hydroxyapatite: In-situ synthesis and characterization.

    Science.gov (United States)

    Teng, Shu-Hua; Liang, Mian-Hui; Wang, Peng; Luo, Yong

    2016-01-01

    The collagen/chitosan/hydroxyapatite (COL/CS/HA) composite microspheres with a good spherical form and a high dispersity were successfully obtained using an in-situ synthesis method. The FT-IR and XRD results revealed that the inorganic phase in the microspheres was crystalline HA containing carbonate ions. The morphology of the composite microspheres was dependent on the HA content, and a more desirable morphology was achieved when 20 wt.% HA was contained. The composite microspheres exhibited a narrow particle distribution, most of which ranged from 5 to 10 μm. In addition, the needle-like HA nano-particles were uniformly distributed in the composite microspheres, and their crystallinity and crystal size decreased with the HA content. Copyright © 2015 Elsevier B.V. All rights reserved.

  4. Mechanism of Particle Formation in Silver/Epoxy Nanocomposites Obtained through a Visible-Light-Assisted in Situ Synthesis.

    Science.gov (United States)

    dell'Erba, Ignacio E; Martínez, Francisco D; Hoppe, Cristina E; Eliçabe, Guillermo E; Ceolín, Marcelo; Zucchi, Ileana A; Schroeder, Walter F

    2017-10-03

    A detailed understanding of the processes taking place during the in situ synthesis of metal/polymer nanocomposites is crucial to manipulate the shape and size of nanoparticles (NPs) with a high level of control. In this paper, we report an in-depth time-resolved analysis of the particle formation process in silver/epoxy nanocomposites obtained through a visible-light-assisted in situ synthesis. The selected epoxy monomer was based on diglycidyl ether of bisphenol A, which undergoes relatively slow cationic ring-opening polymerization. This feature allowed us to access a full description of the formation process of silver NPs before this was arrested by the curing of the epoxy matrix. In situ time-resolved small-angle X-ray scattering investigation was carried out to follow the evolution of the number and size of the silver NPs as a function of irradiation time, whereas rheological experiments combined with near-infrared and ultraviolet-visible spectroscopies were performed to interpret how changes in the rheological properties of the matrix affect the nucleation and growth of particles. The analysis of the obtained results allowed us to propose consistent mechanisms for the formation of metal/polymer nanocomposites obtained by light-assisted one-pot synthesis. Finally, the effect of a thermal postcuring treatment of the epoxy matrix on the particle size in the nanocomposite was investigated.

  5. Ex situ synthesis of G/α-Fe2O3 nanocomposite and its catalytic effect ...

    Indian Academy of Sciences (India)

    2017-07-25

    Jul 25, 2017 ... situ synthesis in the presence of α-Fe2O3 nanoparticles and GO solution. .... tion, washed several times with deionized water and ethanol and then dried at ..... where α is the extent of conversion, T is the temperature,. A is the ...

  6. Capsaicin Synthesis Requires in Situ Phenylalanine and Valine Formation in in Vitro Maintained Placentas from Capsicum chinense

    Directory of Open Access Journals (Sweden)

    Fray M. Baas-Espinola

    2016-06-01

    Full Text Available Capsaicinoids (CAP are nitrogenous metabolites formed from valine (Val and phenylalanine (Phe in the placentas of hot Capsicum genotypes. Placentas of Habanero peppers can incorporate inorganic nitrogen into amino acids and have the ability to secure the availability of the required amino acids for CAP biosynthesis. In order to determine the participation of the placental tissue as a supplier of these amino acids, the effects of blocking the synthesis of Val and Phe by using specific enzyme inhibitors were analyzed. Isolated placentas maintained in vitro were used to rule out external sources′ participation. Blocking Phe synthesis, through the inhibition of arogenate dehydratase, significantly decreased CAP accumulation suggesting that at least part of Phe required in this process has to be produced in situ. Chlorsulfuron inhibition of acetolactate synthase, involved in Val synthesis, decreased not only Val accumulation but also that of CAP, pointing out that the requirement for this amino acid can also be fulfilled by this tissue. The presented data demonstrates that CAP accumulation in in vitro maintained placentas can be accomplished through the in situ availability of Val and Phe and suggests that the synthesis of the fatty acid chain moiety may be a limiting factor in the biosynthesis of these alkaloids.

  7. Microwave assisted in situ synthesis of Ag–NaCMC films and their reproducible surface-enhanced Raman scattering signals

    International Nuclear Information System (INIS)

    Jiang, Tao; Li, Junpeng; Zhang, Li; Wang, Binbing; Zhou, Jun

    2014-01-01

    Graphical abstract: Two kinds of Ag–NaCMC films for surface-enhanced Raman scattering (SERS) were prepared by conventional heating and microwave assisted in situ reduction methods without any additional capping or reducing agents. A relatively narrow and symmetric surface plasmon resonance band was observed in the absorption spectra of the films fabricated by the microwave assisted in situ reduction method. More uniform silver nanoparticles (NPs) implied by the symmetric absorption spectrum were further confirmed by the scanning electron microscopy images. After the simulation of the E-field intensity distribution around the silver NPs in NaCMC film, the Raman scattering enhancement factors (EFs) of these films were then investigated with 4-mercaptobenzoic acid molecule as a SERS reporter. Improved reproducibility of SERS signal was obtained in the microwave assisted synthesized Ag–NaCMC film, although it maintained an EF as only 1.11 × 10 8 . The reproducible SERS signal of the Ag–NaCMC film is particularly attractive and this microwave assisted in situ reduction method is suitable for the production of excellent substrate for biosensor application. - Highlights: • The synthesis of Ag–NaCMC films was successfully fulfilled by a low-cost microwave method. • More uniform silver nanoparticles were observed in Ag–NaCMC film synthesized by microwave. • Improved reproducibility of SERS signal was obtained in microwave synthesized Ag–NaCMC film. - Abstract: Two kinds of Ag–NaCMC films for surface-enhanced Raman scattering (SERS) were prepared by conventional heating and microwave assisted in situ reduction methods without any additional capping or reducing agents. A relatively narrow and symmetric surface plasmon resonance band was observed in the absorption spectra of the films fabricated by the microwave assisted in situ reduction method. More uniform silver nanoparticles (NPs) implied by the symmetric absorption spectrum were further confirmed by

  8. In situ synthesis of fluorescent magnetosomes using an organic membrane as a soft template.

    Science.gov (United States)

    Ke, Wenjing; Zhang, Juhua; An, Xueqin; Zhang, Bo

    2017-05-04

    A novel approach was presented for the in situ synthesis of fluorescent magnetosomes by biological mineralization and carbonization processes for the first time. The surface structures, magnetism and fluorescence were studied, and the cytotoxicity tests and fluorescent trace in liposomes were probed. The fluorescent magnetosomes exhibit not only unique fluorescence and ferromagnetic properties but also low toxicity and superior imaging capability.

  9. Effect of silica particles modified by in-situ and ex-situ methods on the reinforcement of silicone rubber

    International Nuclear Information System (INIS)

    Song, Yingze; Yu, Jinhong; Dai, Dan; Song, Lixian; Jiang, Nan

    2014-01-01

    Highlights: • In-situ and ex-situ methods were applied to modify silica particles. • In-situ method was more beneficial to preparing silica particles with high BET surface area. • Silicone rubber filled with in-situ modified silica exhibits excellent mechanical and thermal properties. - Abstract: In-situ and ex-situ methods were applied to modify silica particles in order to investigate their effects on the reinforcement of silicone rubber. Surface area and pore analyzer, laser particle size analyzer, Fourier-transform infrared spectroscopy (FTIR), contact-angle instrument, and transmission electron microscope (TEM) were utilized to investigate the structure and properties of the modified silica particles. Dynamic mechanical thermal analyzer (DMTA) was employed to characterize the vulcanizing behavior and mechanical properties of the composites. Thermogravimetric analysis (TGA) was performed to test the thermal stability of the composites. FTIR and contact angle analysis indicated that silica particles were successfully modified by these two methods. The BET surface area and TEM results reflected that in-situ modification was more beneficial to preparing silica particles with irregular shape and higher BET surface area in comparison with ex-situ modification. The DMTA and TGA data revealed that compared with ex-situ modification, the in-situ modification produced positive influence on the reinforcement of silicone rubber

  10. Diffusion Control in the in Situ Synthesis of Iconic Metal-Organic Frameworks within an Ionic Polymer Matrix.

    Science.gov (United States)

    Lim, Jungho; Lee, Eun Ji; Choi, Jae Sun; Jeong, Nak Cheon

    2018-01-31

    Ionic polymers that possess ion-exchangeable sites have been shown to be a greatly useful platform to fabricate mixed matrices (MMs) where metal-organic frameworks (MOFs) can be in situ synthesized, although the in situ synthesis of MOF has been rarely studied. In this study, alginate (ALG), an anionic green polymer that possesses metal-ion-exchangeable sites, is employed as a platform of MMs for the in situ synthesis of iconic MOFs, HKUST-1, and MOF-74(Zn). We demonstrate for the first time that the sequential order of supplying MOF ingredients (metal ion and deprotonated ligand) into the alginate matrix leads to substantially different results because of a difference in the diffusion of the MOF components. For the examples examined, whereas the infusion of BTC 3- ligand into Cu 2+ -exchanged ALG engendered the eggshell-shaped HKUST-1 layers on the surface of MM spheres, the infusion of Cu 2+ ions into BTC 3- -included alginate engendered the high dispersivity and junction contact of HKUST-1 crystals in the alginate matrix. This fundamental property has been exploited to fabricate a flexible MOF-containing mixed matrix membrane by coincorporating poly(vinyl alcohol). Using two molecular dyes, namely, methylene blue and rhodamine 6G, further, we show that this in situ strategy is suitable for fabricating an MOF-MM that exhibits size-selective molecular uptake.

  11. In Situ Coupling of Ultrasound to Electro- and Photo-Deposition Methods for Materials Synthesis

    Directory of Open Access Journals (Sweden)

    Agnieszka Magdziarz

    2017-01-01

    Full Text Available This short review provides the current state-of-the-art of in situ coupling of ultrasound to chemical deposition methods. A synergetic action of the ultrasound and light radiation or electrical fields may result in new powerful methodologies, and these include sonophotodeposition and sonoelectrodeposition processes. The effect of ultrasound is explained on the base of different physical mechanisms emerging from cavitation phenomenon. Some possible mechanisms of the interactions between ultrasound and photochemical and electrochemical processes are discussed here. The application of sonophotodeposition and sonoelectrodeposition as green energy sources in the syntheses of different nanomaterials is also reviewed.

  12. Cost accounting method for in-situ leaching mines and its application

    International Nuclear Information System (INIS)

    Cheng Zongfang; Yang Yihan; Liu Zhanxiang; Lai Yongchun

    2008-01-01

    Cost structures and accounting method for in-situ leaching mines are studied according to the technical characteeristics of in-situ leaching. A method of cost forecast for in-situ leaching deposit or mine area is presented, and the application of this method is illustrated with examples. (authors)

  13. In situ synthesis of silver nanoparticles on the cotton fabrics modified by plasma induced vapor phase graft polymerization of acrylic acid for durable multifunction

    Energy Technology Data Exchange (ETDEWEB)

    Wang, C.X., E-mail: cxwang@mail.dhu.edu.cn [College of Textiles and Clothing, Yancheng Institute of Technology, Jiangsu, 224003 (China); Collaborative Innovation Center for Ecological Building, Materials and Environmental Protection Equipments, Jiangsu, 224051 (China); Laboratory for Advanced Technology in Environmental Protection, Jiangsu, 224051 (China); School of Textile and Clothing, Nantong University, Jiangsu, 226019 (China); Ren, Y. [School of Textile and Clothing, Nantong University, Jiangsu, 226019 (China); Lv, J.C.; Zhou, Q.Q.; Ma, Z.P.; Qi, Z.M.; Chen, J.Y.; Liu, G.L.; Gao, D.W. [College of Textiles and Clothing, Yancheng Institute of Technology, Jiangsu, 224003 (China); Lu, Z.Q. [College of Textiles and Clothing, Yancheng Institute of Technology, Jiangsu, 224003 (China); Collaborative Innovation Center for Ecological Building, Materials and Environmental Protection Equipments, Jiangsu, 224051 (China); Laboratory for Advanced Technology in Environmental Protection, Jiangsu, 224051 (China); Zhang, W. [College of Textiles and Clothing, Yancheng Institute of Technology, Jiangsu, 224003 (China); Jin, L.M. [Shanghai Institute of Applied Physics, Chinese Academy of Sciences, Shanghai, 201204 (China)

    2017-02-28

    Highlights: • A new means for multifunctional cotton fabrics by PIVPGP of AA and AgNPs synthesis. • Surface modification by PIVPGP of AA had a positive effect on AgNPs loading. • Antibacterial, self-cleaning and thermal stability were greatly improved. • AgNP loaded cotton fabric exhibited excellent laundering durability. • Mechanism of AgNPs in situ synthesis on cotton fabrics by PIVPGP of AA was proposed. - Abstract: A practical and ecological method for preparing the multifunctional cotton fabrics with excellent laundering durability was explored. Cotton fabrics were modified by plasma induced vapor phase graft polymerization (PIVPGP) of acrylic acid (AA) and subsequently silver nanoparticles (AgNPs) were in situ synthesized on the treated cotton fabrics. The AgNP loaded cotton fabrics were characterized by scanning electron microscope (SEM), energy dispersive X-ray (EDX), X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), antibacterial activity, self-cleaning activity, thermal stability and laundering durability, respectively. SEM observation and EDX, XPS and XRD analysis demonstrated the much more AgNPs deposition on the cotton fabrics modified by PIVPGP of AA. The AgNP loaded cotton fabrics also exhibited better antibacterial activity, self-cleaning activity, thermal stability and laundering durability. It was concluded that the surface modification of the cotton fabrics by PIVPGP of AA could increase the loading efficiency and binding fastness of AgNPs on the treated cotton fabrics, which could fabricate the cotton fabrics with durable multifunction. In addition, the mechanism of in situ synthesis of AgNPs on the cotton fabrics modified by PIVPGP of AA was proposed.

  14. Electrochemical synthesis, in situ spectroelectrochemistry of conducting indole-titanium dioxide and zinc oxide polymer nanocomposites for rechargeable batteries

    International Nuclear Information System (INIS)

    Parvin, Mohammad Hadi; Pirnia, Mahsa; Arjomandi, Jalal

    2015-01-01

    Highlights: • Two novel hybrid materials-based conducting PIn rechargeable batteries were developed. • The charge-discharging behavior of PIn-nanocomposite batteries were studied. • The characterization of samples has been done by in situ spectroelectrochemical method. • PIn-TiO 2 and ZnO nanocomposites were synthesized electrochemically on Au and ITO. • The PIn-TiO 2 and ZnO nanocomposites resistances were less than PIn. - Abstract: Electrochemical synthesis, in situ spectroelectrochemistry of conducting polyindole (PIn), polyindole-TiO 2 (PIn-TiO 2 ) and polyindole-ZnO (PIn-ZnO) nanocomposites were investigated. The PIn and polymer nanocomposites were tested electrochemically for rechargeable batteries. The films were characterized by means of CVs, in situ UV-visible, FT-IR spectroscopies, in situ resistivity measurements, energy dispersive X-ray (EDX), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The charge-discharging behavior of a Zn/1 M ZnSO 4 /PIn cell with a capacity of around 90 Ah Kg −1 and on open circuit potential of around 1.45 V was compared with Zn/1 M ZnSO 4 /PIn-nanocomposite. The potential differences of redox couples (ΔE) for nanocomposites films show very good reversibility. A positive shift of potential was observed for polymer nanocomposites during redox scan. A significant variability was observed for in situ conductivity of the PIn and polymer nanocomposites. During in situ UV-visible and FT-IR measurements, intermediate spectroscopic behavior and positive shifts of wavelengths were observed for PIn and polymer nanocomposites. The SEM, TEM and EDX of nanocomposite films show the presence of nano particle in PIn.

  15. Fluorescent in situ folding control for rapid optimization of cell-free membrane protein synthesis.

    Directory of Open Access Journals (Sweden)

    Annika Müller-Lucks

    Full Text Available Cell-free synthesis is an open and powerful tool for high-yield protein production in small reaction volumes predestined for high-throughput structural and functional analysis. Membrane proteins require addition of detergents for solubilization, liposomes, or nanodiscs. Hence, the number of parameters to be tested is significantly higher than with soluble proteins. Optimization is commonly done with respect to protein yield, yet without knowledge of the protein folding status. This approach contains a large inherent risk of ending up with non-functional protein. We show that fluorophore formation in C-terminal fusions with green fluorescent protein (GFP indicates the folding state of a membrane protein in situ, i.e. within the cell-free reaction mixture, as confirmed by circular dichroism (CD, proteoliposome reconstitution and functional assays. Quantification of protein yield and in-gel fluorescence intensity imply suitability of the method for membrane proteins of bacterial, protozoan, plant, and mammalian origin, representing vacuolar and plasma membrane localization, as well as intra- and extracellular positioning of the C-terminus. We conclude that GFP-fusions provide an extension to cell-free protein synthesis systems eliminating the need for experimental folding control and, thus, enabling rapid optimization towards membrane protein quality.

  16. Polyindole/ carboxylated-multiwall carbon nanotube composites produced by in-situ and interfacial polymerization

    International Nuclear Information System (INIS)

    Joshi, Leela; Singh, Arun Kumar; Prakash, Rajiv

    2012-01-01

    Composites of polyindole (PIn), a conducting polymer, with carboxylated-multiwalled carbon nanotubes (c-MWCNT/PIn) were synthesized; the synthesis was done using (i) two miscible solvents (in-situ method) and (ii) two immiscible solvents (interfacial method). A tubular composite, with a uniform coating of the polymer over c-MWCNTs, was observed in the case of interfacial synthesis. However, the in-situ synthesis of c-MWCNT/PIn composites exhibited a densely packed spherical morphology, with c-MWCNT incorporated within the polymer spheres. The spherical morphology was probably obtained due to fast polymerization kinetics and the formation of micelles in case of in-situ polymerization, whereas tubular morphology was obtained in case of interfacial polymerization due to the sufficient time provided for the growth of polymer chains over the c-MWCNT surfaces. Nanoscale electrical properties of composites, in a metal/(c-MWCNT/PIn) configuration, were studied using current sensing atomic force microscopy. Interfacial c-MWCNT/PIn composite, on Al metal substrate, exhibited a typical rectifying diode behavior. This composite had manifested enormous potential for electronic applications and fabrication of nanoscale organic devices. Highlights: ► Polyindole/c-MWNT nanocomposites produced by in-situ and interfacial polymerization. ► Densely packed spherical morphology was observed in in-situ polymerization route. ► Tubular core-shell morphology was observed in interfacial polymerization route. ► Interfacial nanocomposite manifested a nano-schottky junction with Al metal.

  17. Combining in situ characterization methods in one set-up: looking with more eyes into the intricate chemistry of the synthesis and working of heterogeneous catalysts.

    Science.gov (United States)

    Bentrup, Ursula

    2010-12-01

    Several in situ techniques are known which allow investigations of catalysts and catalytic reactions under real reaction conditions using different spectroscopic and X-ray methods. In recent years, specific set-ups have been established which combine two or more in situ methods in order to get a more detailed understanding of catalytic systems. This tutorial review will give a summary of currently available set-ups equipped with multiple techniques for in situ catalyst characterization, catalyst preparation, and reaction monitoring. Besides experimental and technical aspects of method coupling including X-ray techniques, spectroscopic methods (Raman, UV-vis, FTIR), and magnetic resonance spectroscopies (NMR, EPR), essential results will be presented to demonstrate the added value of multitechnique in situ approaches. A special section is focussed on selected examples of use which show new developments and application fields.

  18. Graphene oxide directed in-situ synthesis of Prussian blue for non-enzymatic sensing of hydrogen peroxide released from macrophages

    Energy Technology Data Exchange (ETDEWEB)

    Qiu, Weiwei; Zhu, Qionghua; Gao, Fei; Gao, Feng [College of Chemistry and Environment, Fujian Province Key Laboratory of Morden Analytical Science and Separation Technology, Minnan Normal University, Zhangzhou 363000 (China); Huang, Jiafu; Pan, Yutian [College of Biological Science and Technology, Minnan Normal University, Zhangzhou 363000 (China); Wang, Qingxiang, E-mail: axiang236@126.com [College of Chemistry and Environment, Fujian Province Key Laboratory of Morden Analytical Science and Separation Technology, Minnan Normal University, Zhangzhou 363000 (China)

    2017-03-01

    A novel electrochemical non-enzymatic hydrogen peroxide (H{sub 2}O{sub 2}) sensor has been developed based on Prussian blue (PB) and electrochemically reduced graphene oxide (ERGO). The GO was covalently modified on glassy carbon electrode (GCE), and utilized as a directing platform for in-situ synthesis of electroactive PB. Then the GO was electrochemically treated to reduction form to improve the effective surface area and electroactivity of the sensing interface. The fabrication process was characterized by scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX) and atomic force microscopy (AFM). The results showed that the rich oxygen containing groups play a crucial role for the successful synthesis of PB, and the obtained PB layer on the covalently immobilized GO has good stability. Electrochemical sensing assay showed that the modified electrode had tremendous electrocatalytic property for the reduction of H{sub 2}O{sub 2}. The steady-state current response increased linearly with H{sub 2}O{sub 2} concentrations from 5 μM to 1 mM with a fast response time (less than 3 s). The detection limit was estimated to be 0.8 μM. When the sensor was applied for determination of H{sub 2}O{sub 2} released from living cells of macrophages, satisfactory results were achieved. - Highlights: • Covalent method was applied for immobilization of GO on glassy carbon electrode. • GO directed in-situ synthesis of electroactive PB. • PB-ERGO composite shows high electrocatalytic activity toward H{sub 2}O{sub 2}. • The modified biosensor is capable of detecting H{sub 2}O{sub 2} released from living macrophages.

  19. Laser-induced incandescence (LII) diagnostic for in situ monitoring of nanoparticle synthesis in a high-pressure arc discharge

    Science.gov (United States)

    Yatom, Shurik; Vekselman, Vladislav; Mitrani, James; Stratton, Brentley; Raitses, Yevgeny; LaboratoryPlasma Nanosynthesis Team

    2016-10-01

    A DC arc discharge is commonly used for synthesis of carbon nanoparticles, including buckyballs, carbon nanotubes, and graphene flakes. In this work we show the first results of nanoparticles monitored during the arc discharge. The graphite electrode is vaporized by high current (60 A) in a buffer Helium gas leading to nanoparticle synthesis in a low temperature plasma. The arc was shown to oscillate, which can possibly influence the nano-synthesis. To visualize the nanoparticles in-situ we employ the LII technique. The nanoparticles with radii >50 nm, emerging from the arc area are heated with a short laser pulse and incandesce. The resulting radiation is captured with an ICCD camera, showing the location of the generated nanoparticles. The images of incandescence are studied together with temporally synchronized fast-framing imaging of C2 emission, to connect the dynamics of arc instabilities, C2 molecules concentration and nanoparticles. The time-resolved incandescence signal is analyzed with combination of ex-situ measurements of the synthesized nanoparticles and LII modeling, to provide the size distribution of produced nanoparticles. This work was supported by US Department of Energy, Office of Science, Basic Energy Sciences, Materials Sciences and Engineering Division.

  20. Synthesis of transparent ZnO/PMMA nanocomposite films through free-radical copolymerization of asymmetric zinc methacrylate acetate and in-situ thermal decomposition

    Energy Technology Data Exchange (ETDEWEB)

    Zhang Lin [Department of Chemistry, Nanchang University, 999 Xuefu Avenue, Nanchang 330031 (China); Institute of Polymers, Nanchang University, 999 Xuefu Avenue, Nanchang 330031 (China); Li Fan, E-mail: lfan@ncu.edu.cn [Institute of Polymers, Nanchang University, 999 Xuefu Avenue, Nanchang 330031 (China); Chen Yiwang, E-mail: ywchen@ncu.edu.cn [Department of Chemistry, Nanchang University, 999 Xuefu Avenue, Nanchang 330031 (China); Institute of Polymers, Nanchang University, 999 Xuefu Avenue, Nanchang 330031 (China); Wang Xiaofeng [Institute of Polymers, Nanchang University, 999 Xuefu Avenue, Nanchang 330031 (China)

    2011-08-15

    In this paper, a new and simple approach for in-situ preparation of transparent ZnO/poly(metyl methacrylate) (ZnO/PMMA) nanocomposite films was developed. Poly(methyl methacrylate)-co-poly(zinc methacrylate acetate) (PMMA-co-PZnMAAc) copolymer was synthesized via free-radical polymerization between methyl methacrylate (MMA) and zinc methacrylate acetate (ZnMAAc), where asymmetric ZnMAAc with only one terminal double bond (C=C) was applied to act as the precursor for ZnO nanocrystals and could avoid cross-link. Subsequently, transparent ZnO/PMMA nanocomposite films were obtained by in-situ thermal decomposition. Scanning electron microscope (SEM) image revealed that ZnO nanocrystals were homogeneously dispersed in PMMA matrix. With thermal decomposition time increasing, the absorption intensity in UV region and photoluminescence intensity of ZnO/PMMA nanocomposite films enhanced. However, the optical properties diminished when the thermal decomposition temperature increased. The TGA measurement displayed ZnO/PMMA nanocomposite films prepared by the in-situ synthesis method possessed better thermal stability compared with those prepared by the physical blending method and pristine PMMA films. - Highlights: > ZnO/PMMA hybrid films were prepared via free-radical polymerization and in-situ thermal decomposition. > ZnO NCs are homogeneously dispersed in the PMMA matrix and these films have good optical properties. > Thermal stability of these films is improved compared with those of physically blending ones.

  1. Synthesis of transparent ZnO/PMMA nanocomposite films through free-radical copolymerization of asymmetric zinc methacrylate acetate and in-situ thermal decomposition

    International Nuclear Information System (INIS)

    Zhang Lin; Li Fan; Chen Yiwang; Wang Xiaofeng

    2011-01-01

    In this paper, a new and simple approach for in-situ preparation of transparent ZnO/poly(metyl methacrylate) (ZnO/PMMA) nanocomposite films was developed. Poly(methyl methacrylate)-co-poly(zinc methacrylate acetate) (PMMA-co-PZnMAAc) copolymer was synthesized via free-radical polymerization between methyl methacrylate (MMA) and zinc methacrylate acetate (ZnMAAc), where asymmetric ZnMAAc with only one terminal double bond (C=C) was applied to act as the precursor for ZnO nanocrystals and could avoid cross-link. Subsequently, transparent ZnO/PMMA nanocomposite films were obtained by in-situ thermal decomposition. Scanning electron microscope (SEM) image revealed that ZnO nanocrystals were homogeneously dispersed in PMMA matrix. With thermal decomposition time increasing, the absorption intensity in UV region and photoluminescence intensity of ZnO/PMMA nanocomposite films enhanced. However, the optical properties diminished when the thermal decomposition temperature increased. The TGA measurement displayed ZnO/PMMA nanocomposite films prepared by the in-situ synthesis method possessed better thermal stability compared with those prepared by the physical blending method and pristine PMMA films. - Highlights: → ZnO/PMMA hybrid films were prepared via free-radical polymerization and in-situ thermal decomposition. → ZnO NCs are homogeneously dispersed in the PMMA matrix and these films have good optical properties. → Thermal stability of these films is improved compared with those of physically blending ones.

  2. Synthesis and characterization of PMMA/clay nanocomposites prepared by in situ polymerization assisted by sonication

    International Nuclear Information System (INIS)

    Prado, Bruna R.; Bartoli, Julio R.; Ito, Edson N.

    2015-01-01

    In this work is presented the synthesis of nanocomposites of poly(methyl methacrylate), PMMA, with organically montmorillonite (OMMT) modified clays by in situ polymerization assisted by sonication. A statistically designed experiment was used, central composing design (CCD), to study the effect of synthesis variables on the dispersion of nanoparticles in PMMA matrix. The processing and formulation factors studied were: energy of sonication and Flory-Huggins interaction parameter between PMMA and organoclay. The structural (XRD) and morphological (TEM) characterizations of the PMMA/OMMT nanocomposites are compared with the literature. It was observed significant exfoliation of OMMT modified with hydroxyl groups in the nanocomposites of PMMA, mainly at the low ultrasonic energy level (90 and 105 kJ) studied. (author)

  3. Combined synthesis and in situ coating of nanoparticles in the gas phase

    International Nuclear Information System (INIS)

    Laehde, Anna; Raula, Janne; Kauppinen, Esko I.

    2008-01-01

    Combined gas phase synthesis and coating of sodium chloride (NaCl) and lactose nanoparticles has been developed using an aerosol flow reactor. Nano-sized core particles were produced by the droplet-to-particle method and coated in situ by the physical vapour deposition of L-leucine vapour. The saturation of L-leucine in the reactor determined the resulting particle size and size distribution. In general, particle size increased with the addition of L-leucine and notable narrowing of the core particle size distribution was observed. In addition, homogeneous nucleation of the vapour, i.e. formation of pure L-leucine particles, was observed depending on the saturation conditions of L-leucine as well as the core particle characteristics. The effects of core particle properties, i.e. size and solid-state characteristics, on the coating process were studied by comparing the results for coated NaCl and lactose particles. During deposition, L-leucine formed a uniform coating on the surface of the core particles. The coating stabilised the nanoparticles and prevented the sintering of particles during storage.

  4. Smart swelling biopolymer microparticles by a microfluidic approach: synthesis, in situ encapsulation and controlled release.

    Science.gov (United States)

    Fang, Aiping; Cathala, Bernard

    2011-01-01

    This paper reports a microfluidic synthesis of biopolymer microparticles aiming at smart swelling. Monodisperse aqueous emulsion droplets comprising biopolymer and its cross-linking agent were formed in mineral oil and solidified in the winding microfluidic channels by in situ chaotic mixing, which resulted in internal chemical gelation for hydrogels. The achievement of pectin microparticles from in situ mixing pectin with its cross-linking agent, calcium ions, successfully demonstrates the reliability of this microfluidic synthesis approach. In order to achieve hydrogels with smart swelling, the following parameters and their impacts on the swelling behaviour, stability and morphology of microparticles were investigated: (1) the type of biopolymers (alginate or mixture of alginate and carboxymethylcellulose, A-CMC); (2) rapid mixing; (3) concentration and type of cross-linking agent. Superabsorbent microparticles were obtained from A-CMC mixture by using ferric chloride as an additional external cross-linking agent. The in situ encapsulation of a model protein, bovine serum albumin (BSA), was also carried out. As a potential protein drug-delivery system, the BSA release behaviours of the biopolymer particles were studied in simulated gastric and intestinal fluids. Compared with alginate and A-CMC microparticles cross-linked with calcium ions, A-CMC microparticles cross-linked with both calcium and ferric ions demonstrate a significantly delayed release. The controllable release profile, the facile encapsulation as well as their biocompatibility, biodegradability, mucoadhesiveness render this microfluidic approach promising in achieving biopolymer microparticles as protein drug carrier for site-specific release. Copyright © 2010 Elsevier B.V. All rights reserved.

  5. Polyhomologation based on in situ generated Boron-thexyl-silaboracyclic initiating sites: a novel strategy towards the synthesis of polyethylene-based complex architectures

    KAUST Repository

    Zhang, Zhen

    2015-04-10

    A novel strategy, based on the in situ generated Boron-thexyl-silaboracyclic initiating sites for the polyhomologation of dimethylsulfoxonium methylide, has been developed for the synthesis of complex polyethylene-based architectures. As examples, the synthesis of a 4-arm polyethylene star, three (polystyrene)(polyethylene)2 3-miktoarm stars and a PE-branched double graft copolymers are given.

  6. Nanoparticles of the superconductor MgB2: structural characterization and in situ study of synthesis kinetics

    International Nuclear Information System (INIS)

    Cui Chunxiang; Liu Debao; Shen Yutian; Sun Jinbin; Meng Fanbin; Wang Ru; Liu Shuangjin; Greer, A.L.; Chen, S.K.; Glowacki, B.A.

    2004-01-01

    Single-crystal MgB 2 nanoparticles, with diameters in the range 20-100 nm, have been synthesized in situ in the sample chamber of an X-ray diffractometer. The reaction kinetics are analyzed and related to the atomic-level structure of the particles as observed by high-resolution electron microscopy. Synthesis conditions may have a significant influence on microstructure and superconducting properties

  7. Aerobic method for the synthesis of nearly size-monodisperse bismuth nanoparticles from a redox non-innocent precursor

    Science.gov (United States)

    Winter, H.; Christopher-Allison, E.; Brown, A. L.; Goforth, A. M.

    2018-04-01

    Herein, we report an aerobic synthesis method to produce bismuth nanoparticles (Bi NPs) with average diameters in the range 40-80 nm using commercially available bismuth triiodide (BiI3) as the starting material; the method uses only readily available chemicals and conventional laboratory equipment. Furthermore, size data from replicates of the synthesis under standard reaction conditions indicate that this method is highly reproducible in achieving Bi NP populations with low standard deviations in the mean diameters. We also investigated the mechanism of the reaction, which we determined results from the reduction of a soluble alkylammonium iodobismuthate precursor species formed in situ. Under appropriate concentration conditions of iodobismuthate anion, we demonstrate that burst nucleation of Bi NPs results from reduction of Bi3+ by the coordinated, redox non-innocent iodide ligands when a threshold temperature is exceeded. Finally, we demonstrate phase transfer and silica coating of the Bi NPs, which results in stable aqueous colloids with retention of size, morphology, and colloidal stability. The resultant, high atomic number, hydrophilic Bi NPs prepared using this synthesis method have potential for application in emerging x-ray contrast and x-ray therapeutic applications.

  8. In-situ fabrication of hybrid polyoxometalate nanoparticles composite films

    International Nuclear Information System (INIS)

    Lan Yang; Mao Baodong; Wang Enbo; Song Yonghai; Kang Zhenhui; Wang Chunlei; Tian Chungui; Zhang Chao; Xu Lin; Li Zhuang

    2007-01-01

    Inorganic-organic hybrid nanoparticles multilayer films were fabricated by extending the method of nucleation and growth of particles in polymer assemblies. The polyelectrolyte matrix was constructed by layer-by-layer self-assembly method. Synthesis of polyoxometalate nanoparticles was achieved by alternately dipping the precursor polyelectrolyte matrix into AgNO 3 and H 4 SiW 12 O 40 aqueous solutions. Repeating the above synthesis process, Ag 4 SiW 12 O 40 nanoparticles with controllable diameters of 20 to 77 nm were synthesized in the multilayer films in-situ. UV-vis absorption spectra indicate that the nanoparticles grew gradually in the synthesis process. Transmission electron microscopy was used to observe the size and morphology of the nanoparticles

  9. Log-pile photonic crystal of CdS-polymer nanocomposites fabricated by combination of two-photon polymerization and in situ synthesis

    International Nuclear Information System (INIS)

    Sun, Z.-B.; Dong, X.-Z.; Chen, W.-Q.; Duan, X.-M.; Nakanishi, S.; Kawata, S.

    2007-01-01

    A log-pile photonic crystal of CdS nanoparticles-polymer nanocomposites was successfully fabricated by a novel method combining the two-photon polymerization technique and in situ synthesis of CdS nanoparticles in a polymer matrix. The photonic band gap of the three-dimensional (3D) log-pile photonic crystal is confirmed and becomes more effective for CdS nanoparticles-polymer nanocomposites than polymer doped with Cd 2+ ions, because the nanocomposites possess a higher refractive index than the polymer. The proposed concept in the new fabrication method for a 3D microstructure of polymer nanocomposites should be of critical importance in providing a general methodology for functionalization of materials via functional nanocomposites used in the field of laser microstructure fabrication. (orig.)

  10. Synthesis-on” and “synthesis-off” modes of carbon arc operation during synthesis of carbon nanotubes

    International Nuclear Information System (INIS)

    Yatom, Shurik; Selinsky, Rachel S.

    2017-01-01

    Arc discharge synthesis of single-walled carbon nanotubes (SWCNTs) remains largely uncontrollable, due to incomplete understanding of the synthetic process itself. Here, we show that synthesis of SWCNTs by a carbon arc may not constitute a single continuous process, but may instead consist of two distinct modes. One of these, a “synthesis-on” mode, produces the majority of the nanomaterials. During the synthesis-on mode, proportionally more carbon nanotubes are collected than in another mode, a “synthesis-off” mode. Both synthesis-on and synthesis-off modes for a typical arc configuration, employing a hollow anode filled with a mixture of powdered metal catalyst and graphite, were characterized by using in situ electrical, imaging, and spectroscopic diagnostics, along with ex situ imaging and spectroscopy. The synthesis-on mode duration is rare compared to the total arc run-time, helping to explain the poor selectivity found in the final collected products, a known inadequacy of arc synthesis. Finally, the rarity of the synthesis on mode occurence may be due to the synthesis off mode being more favorable energetically.

  11. In-situ synthesis of SiC particles by the structural evolution of TiCx in Al–Si melt

    International Nuclear Information System (INIS)

    Nie, Jinfeng; Li, Dakui; Wang, Enzhao; Liu, Xiangfa

    2014-01-01

    Highlights: • A facile method to in-situ synthesize SiC was developed utilizing the structural evolution of TiC x in Al–Si melt. • The SiC particles have the size range from 2.5 to 7.5 μm and a block-like morphology. • The SiC particles and (SiC + TiB 2 ) hybrid-particles reinforced Al–18Si composite were prepared. • The wear resistance effect of SiC on the based alloy was investigated. - Abstract: A facile method has been developed to in-situ synthesize SiC particles utilizing the structural instability and evolution of TiC x in Al–Si melt. It is considered that the synthesis of SiC particles occurs via the gradual reaction between TiC x and Si atoms, whilst Si content plays the crucial role in this approach. If the Si content in the melt is above 30%, TiC x directly reacts with Si and Al to form SiC, but the needle-like TiAl x Si y phase formed simultaneously will do harm to the mechanical properties of the composites. Thus, it is proposed to add B element in the melt to transform the TiAl x Si y into TiB 2 particles. Therefore, the SiC and (SiC + TiB 2 ) hybrid-particles reinforced Al–18Si composites were successfully prepared using the method. In the composites, the SiC particles have the size range from 2.5 to 7.5 μm and a block-like morphology. Furthermore, the mechanical properties of base alloy, including the wear resistance and macro-hardness, have been obviously improved by the in-situ SiC particles. Besides, the relevant underlying mechanisms are also discussed

  12. A Novel in situ Trigger Combination Method

    International Nuclear Information System (INIS)

    Buzatu, Adrian; Warburton, Andreas; Krumnack, Nils; Yao, Wei-Ming

    2012-01-01

    Searches for rare physics processes using particle detectors in high-luminosity colliding hadronic beam environments require the use of multi-level trigger systems to reject colossal background rates in real time. In analyses like the search for the Higgs boson, there is a need to maximize the signal acceptance by combining multiple different trigger chains when forming the offline data sample. In such statistically limited searches, datasets are often amassed over periods of several years, during which the trigger characteristics evolve and their performance can vary significantly. Reliable production cross-section measurements and upper limits must take into account a detailed understanding of the effective trigger inefficiency for every selected candidate event. We present as an example the complex situation of three trigger chains, based on missing energy and jet energy, to be combined in the context of the search for the Higgs (H) boson produced in association with a W boson at the Collider Detector at Fermilab (CDF). We briefly review the existing techniques for combining triggers, namely the inclusion, division, and exclusion methods. We introduce and describe a novel fourth in situ method whereby, for each candidate event, only the trigger chain with the highest a priori probability of selecting the event is considered. The in situ combination method has advantages of scalability to large numbers of differing trigger chains and of insensitivity to correlations between triggers. We compare the inclusion and in situ methods for signal event yields in the CDF WH search.

  13. In-situ synthesis of hydrogen peroxide in a novel Zn-CNTs-O2 system

    Science.gov (United States)

    Gong, Xiao-bo; Yang, Zhao; Peng, Lin; Zhou, An-lan; Liu, Yan-lan; Liu, Yong

    2018-02-01

    A novel strategy of in-situ synthesis of hydrogen peroxide (H2O2) was formulated and evaluated. Oxygen was selectively reduced to H2O2 combined with electrochemical corrosion of zinc in the Zn-CNTs-O2 system. The ratio of zinc and CNTs, heat treatment temperature, and operational parameters such as composite dosage, initial pH, solution temperature, oxygen flow rate were systematically investigated to improve the efficiency of H2O2 generation. The Zn-CNTs composite (weight ratio of 2.5:1) prepared at 500 °C showed the maximum H2O2 accumulation concentration of 293.51 mg L-1 within 60 min at the initial pH value of 3.0, Zn-CNTs dosage of 0.4 g and oxygen flow rate of 400 mL min-1. The oxygen was reduced through two-electron pathway to hydrogen peroxide on CNTs while the zinc was oxidized in the system and the dissolved zinc ions convert to zinc hydroxide and depositing on the surface of CNTs. It was proposed that the increment of direct H2O2 production was caused by the improvement of the formed Zn/CNTs corrosion cell. This provides promising strategy for in-situ synthesis and utilization of hydrogen peroxide in the novel Zn-CNTs-O2 system, which enhances the environmental and economic attractiveness of the use of H2O2 as green oxidant for wastewater treatments.

  14. Polyhomologation based on in situ generated Boron-thexyl-silaboracyclic initiating sites: a novel strategy towards the synthesis of polyethylene-based complex architectures

    KAUST Repository

    Zhang, Zhen; Zhang, Hefeng; Gnanou, Yves; Hadjichristidis, Nikolaos

    2015-01-01

    A novel strategy, based on the in situ generated Boron-thexyl-silaboracyclic initiating sites for the polyhomologation of dimethylsulfoxonium methylide, has been developed for the synthesis of complex polyethylene-based architectures. As examples

  15. Fabrication of hard cermets by in-situ synthesis and infiltration of metal melts into WC powder compacts

    Directory of Open Access Journals (Sweden)

    Guanghua Liu

    2017-12-01

    Full Text Available Hard carbide cermets are prepared by in-situ synthesis and infiltration of metal melts into WC powder compacts. Ni–W and Ni–W–Cr metal melts are in-situ synthesized from thermite reactions and infiltrated into WC powder compacts under high-gravity. During the infiltration, W in the metal melts reacts with WC to form W2C, and more W2C and W are observed at the upper parts of the cermets than the lower parts. The cermets show a maximum hardness of 15.4 GPa, which is higher than most commercial cemented carbides, although they are not fully dense and have a porosity of 15–20%.

  16. Electrochemical studies, in-situ and ex-situ characterizations of different manganese compounds electrodeposited in aerated solutions; Etudes electrochimiques, suivis in-situ et caracterisations ex-situ de divers composes de manganese electrodeposes dans des solutions aerees

    Energy Technology Data Exchange (ETDEWEB)

    Peulon, S.; Lacroix, A.; Chausse, A. [Univ. d' Evry-val-d' Essonne, Laboratoire Analyse et Modelisation pour la Biologie et l' Environnement (LAMBE CNRS UMR 8587), 91 - Evry (France); Larabi-Gruet, N. [CEA Saclay, Dept. de Physico-Chimie (DEN/DPC/SECR/L3MR), 91 - Gif sur Yvette (France)

    2007-07-01

    This work deals with the electrodeposition of manganese compounds. A systematic study of the synthesis experimental conditions has been carried out, and the obtained depositions have been characterized by different ex-situ analyses methods (XRD, FTIR, SEM). The in-situ measurements of mass increase with a quartz microbalance during the syntheses have allowed to estimate the growth mechanisms which are in agreement with the ex-situ characterizations. The cation has an important role in the nature of the electrodeposited compounds. In presence of sodium, a mixed lamellar compound Mn(III)/Mn(IV), the birnessite, is deposited, whereas in presence of potassium, bixbyite is formed (Mn{sub 2}O{sub 3}), these two compounds having a main role in the environment. The substrate can also influence the nature of the formed intermediary compounds. Little studied compounds such as feitkneichtite ({beta}-MnOOH) and groutite ({alpha}-MnOOH) have been revealed. (O.M.)

  17. Ultrasound irradiation based in-situ synthesis of star-like Tragacanth gum/zinc oxide nanoparticles on cotton fabric.

    Science.gov (United States)

    Ghayempour, Soraya; Montazer, Majid

    2017-01-01

    Application of natural biopolymers for green and safe synthesis of zinc oxide nanoparticles on the textiles is a novel and interesting approach. The present study offers the use of natural biopolymer, Tragacanth gum, as the reducing, stabilizing and binding agent for in-situ synthesis of zinc oxide nanoparticles on the cotton fabric. Ultrasonic irradiation leads to clean and easy synthesis of zinc oxide nanoparticles in short-time at low-temperature. FESEM/EDX, XRD, FT-IR spectroscopy, DSC, photocatalytic activities and antimicrobial assay are used to characterize Tragacanth gum/zinc oxide nanoparticles coated cotton fabric. The analysis confirmed synthesis of star-like zinc oxide nanoparticles with hexagonal wurtzite structure on the cotton fabric with the average particle size of 62nm. The finished cotton fabric showed a good photocatalytic activity on degradation of methylene blue and 100% antimicrobial properties with inhibition zone of 3.3±0.1, 3.1±0.1 and 3.0±0.1mm against Staphylococcus aureus, Escherichia coli and Candida albicans. Copyright © 2016 Elsevier B.V. All rights reserved.

  18. In situ synthesis of N and Cu functionalized mesoporous FDU-14 resins and carbons for electrochemical hydrogen storage

    Energy Technology Data Exchange (ETDEWEB)

    Kong, AiGuo; Wang, WenJuan; Yang, Fan; Ding, HanMing; Shan, YongKui [Department of Chemistry, East China Normal University, ShangHai 200062 (China)

    2010-07-15

    N and Cu cooperatively functionalized mesoporous resin and carbon materials with bicontinuous cubic structure (FDU-14) were obtained by a novel synthesis method. In this method, block copolymers were used as the templates as well as the precursors for the preparation of these modifying mesoporous materials. The CuC{sub 2}O{sub 4} in the channels of mesoporous FDU-14 resins was gotten by in situ oxidation of the templates in a catalytic redox system containing Cu{sup 2+}, Al{sup 3+}, NO{sub 3}{sup -}, PO{sub 4}{sup 3-}, SO{sub 4}{sup 2-} ions. Simultaneously, the phenol-formaldehyde resin frameworks were in situ functionalized by the amine group resulting from the reduction of NO{sub 3}{sup -}, leading to the formation of N and CuC{sub 2}O{sub 4} modified mesoporous FDU-14 resin materials. Its pyrolysis at the different temperatures resulted in the production of N and Cu cooperatively functionalized mesoporous FDU-14 resin and carbon materials. The structure and composition of these materials were characterized by the X-ray power diffraction, transmission electron microscopy, N{sub 2} adsorption-desorption analysis, X-ray photoelectron spectroscopy, infrared spectroscopy, thermogravimetry analysis, and inductive coupled plasma emission spectroscopy. The electrochemical measurement indicated that N and Cu cooperatively functionalized mesoporous FDU-14 carbon materials possessed the enhanced electrochemical hydrogen storage performance. (author)

  19. “Best fit” framework synthesis: refining the method

    Science.gov (United States)

    2013-01-01

    Background Following publication of the first worked example of the “best fit” method of evidence synthesis for the systematic review of qualitative evidence in this journal, the originators of the method identified a need to specify more fully some aspects of this particular derivative of framework synthesis. Methods and Results We therefore present a second such worked example in which all techniques are defined and explained, and their appropriateness is assessed. Specified features of the method include the development of new techniques to identify theories in a systematic manner; the creation of an a priori framework for the synthesis; and the “testing” of the synthesis. An innovative combination of existing methods of quality assessment, analysis and synthesis is used to complete the process. This second worked example was a qualitative evidence synthesis of employees’ views of workplace smoking cessation interventions, in which the “best fit” method was found to be practical and fit for purpose. Conclusions The method is suited to producing context-specific conceptual models for describing or explaining the decision-making and health behaviours of patients and other groups. It offers a pragmatic means of conducting rapid qualitative evidence synthesis and generating programme theories relating to intervention effectiveness, which might be of relevance both to researchers and policy-makers. PMID:23497061

  20. In situ high-resolution transmission electron microscopy synthesis observation of nanostructured carbon coated LiFePO 4

    Science.gov (United States)

    Trudeau, M. L.; Laul, D.; Veillette, R.; Serventi, A. M.; Mauger, A.; Julien, C. M.; Zaghib, K.

    In situ high-resolution transmission electron microscopy (HRTEM) studies of the structural transformations that occur during the synthesis of carbon-coated LiFePO 4 (C-LiFePO 4) and heat treatment to elevated temperatures were conducted in two different electron microscopes. Both microscopes have sample holders that are capable of heating up to 1500 °C, with one working under high vacuum and the other capable of operating with the sample surrounded by a low gaseous environment. The C-LiFePO 4 samples were prepared using three different compositions of precursor materials with Fe(0), Fe(II) or Fe(III), a Li-containing salt and a polyethylene- block-poly(ethylene glycol)-50% ethylene oxide or lactose. The in situ TEM studies suggest that low-cost Fe(0) and a low-cost carbon-containing compound such as lactose are very attractive precursors for mass production of C-LiFePO 4, and that 700 °C is the optimum synthesis temperature. At temperatures higher than 800 °C, LiFePO 4 has a tendency to decompose. The same in situ measurements have been made on particles without carbon coat. The results show that the homogeneous deposit of the carbon deposit at 700 °C is the result of the annealing that cures the disorder of the surface layer of bare LiFePO 4. Electrochemical tests supported the conclusion that the C-LiFePO 4 derived from Fe(0) is the most attractive for mass production.

  1. Electrochemical studies, in-situ and ex-situ characterizations of different manganese compounds electrodeposited in aerated solutions

    International Nuclear Information System (INIS)

    Peulon, S.; Lacroix, A.; Chausse, A.; Larabi-Gruet, N.

    2007-01-01

    This work deals with the electrodeposition of manganese compounds. A systematic study of the synthesis experimental conditions has been carried out, and the obtained depositions have been characterized by different ex-situ analyses methods (XRD, FTIR, SEM). The in-situ measurements of mass increase with a quartz microbalance during the syntheses have allowed to estimate the growth mechanisms which are in agreement with the ex-situ characterizations. The cation has an important role in the nature of the electrodeposited compounds. In presence of sodium, a mixed lamellar compound Mn(III)/Mn(IV), the birnessite, is deposited, whereas in presence of potassium, bixbyite is formed (Mn 2 O 3 ), these two compounds having a main role in the environment. The substrate can also influence the nature of the formed intermediary compounds. Little studied compounds such as feitkneichtite (β-MnOOH) and groutite (α-MnOOH) have been revealed. (O.M.)

  2. Advanced hydraulic fracturing methods to create in situ reactive barriers

    International Nuclear Information System (INIS)

    Murdoch, L.

    1997-01-01

    This article describes the use of hydraulic fracturing to increase permeability in geologic formations where in-situ remedial action of contaminant plumes will be performed. Several in-situ treatment strategies are discussed including the use of hydraulic fracturing to create in situ redox zones for treatment of organics and inorganics. Hydraulic fracturing methods offer a mechanism for the in-situ treatment of gently dipping layers of reactive compounds. Specialized methods using real-time monitoring and a high-energy jet during fracturing allow the form of the fracture to be influenced, such as creation of assymmetric fractures beneath potential sources (i.e. tanks, pits, buildings) that should not be penetrated by boring. Some examples of field applications of this technique such as creating fractures filled with zero-valent iron to reductively dechlorinate halogenated hydrocarbons, and the use of granular activated carbon to adsorb compounds are discussed

  3. Mesoporous MEL, BEA, and FAU zeolite crystals obtained by in situ formation of carbon template over metal nanoparticles

    DEFF Research Database (Denmark)

    Abildstrøm, Jacob Oskar; Ali, Zahra Nasrudin; Mentzel, Uffe Vie

    2016-01-01

    Here, we report the synthesis and characterization of hierarchical zeolite materials with MEL, BEA and FAU structures. The synthesis is based on the carbon templating method with an in situ-generated carbon template. Through the decomposition of methane and deposition of coke over nickel nanopart......Here, we report the synthesis and characterization of hierarchical zeolite materials with MEL, BEA and FAU structures. The synthesis is based on the carbon templating method with an in situ-generated carbon template. Through the decomposition of methane and deposition of coke over nickel...... nanoparticles supported on silica, a carbon–silica composite is obtained and exploited as a combined carbon template/silica source for the zeolite synthesis. The mesoporous zeolite materials were all prepared by hydrothermal crystallization in alkaline media followed by removal of the carbon template...... by combustion, which results in zeolite single crystals with intracrystalline pore volumes of up to 0.44 cm3 g−1. The prepared zeolite structures are characterized by XRD, SEM, TEM and N2 physisorption measurements....

  4. In situ synthesis and modification of calcium carbonate nanoparticles via a bobbling method

    Institute of Scientific and Technical Information of China (English)

    2009-01-01

    Modified calcium carbonate (CaCO3) nanoparticles with cubic- and spindle-like configuration were synthesized in situ by the typical bobbling (gas-liquid-solid) method. The modifiers, such as sodium stearate, octadecyl dihydrogen phosphate (ODP) and oleic acid (OA), were used to obtain hydrophobic nanoparticles. The different modification effects of the modifiers were investigated by measuring the active ratio, whiteness and the contact angle. Moreover, transmission electron microscopy (TEM), X-ray diffraction (XRD) and thermogravimetry analysis (TGA analysis) were employed to characterize the obtained products. A preliminary reaction mechanism was discussed. According to the results, the active ratio of CaCO3 modified by ODP was ca. 99.9% and the value of whiteness was 97.3% when the dosage of modifiers reached 2%. The contact angle was 122.25° for the CaCO3 modified in the presence of sodium stearate, ODP and OA. When modified CaCO3 was filled into PVC, the mechanical properties of products were improved greatly such as rupture intensity, pull intensity and fuse temperature. The compatibility and affinity between the modified CaCO3 nanoparticles and the organic matrixes were greatly improved.

  5. In situ synthesis and modification of calcium carbonate nanoparticles via a bobbling method

    Institute of Scientific and Technical Information of China (English)

    ZHAO LiNa; FENG JingDong; WANG ZiChen

    2009-01-01

    Modified calcium carbonate (CaCO3) nanoparticles with cubic- and spindle-like configuration were synthesized in situ by the typical bobbling (gas-liquid-solid) method.The modifiers,such as sodium stearate,octadecyl dihydrogen phosphate (ODP) and oleic acid (OA),were used to obtain hydrophobic nanoparticles.The different modification effects of the modifiers were investigated by measuring the active ratio,whiteness and the contact angle.Moreover,transmission electron microscopy (TEM),X-ray diffraction (XRD) and thermogravimetry analysis (TGA analysis) were employed to characterize the obtained products.A preliminary reaction mechanism was discussed.According to the results,the active ratio of CaCO3 modified by ODP was ca.99.9% and the value of whiteness was 97.3% when the dosage of modifiers reached 2%.The contact angle was 122.25° for the CaCO3 modified in the presence of sodium stearate,ODP and OA.When modified CaCO3 was filled into PVC,the mechanical properties of products were improved greatly such as rupture intensity,pull intensity and fuse temperature.The compatibility and affinity between the modified CaCO3 nanoparticles and the organic matrixes were greatly improved.

  6. Photo and biocatalytic activities along with UV protection properties on polyester fabric through green in-situ synthesis of cauliflower-like CuO nanoparticles.

    Science.gov (United States)

    Rezaie, Ali Bashiri; Montazer, Majid; Rad, Mahnaz Mahmoudi

    2017-11-01

    In this paper, a facile environmentally friendly method is introduced for in-situ synthesis and fabrication of cauliflower-like CuO nanoparticles on the polyester fabric to produce photo and biocatalytic activities with UV protection properties on polyester fabric. The ash of burnt leaves and stems of Seidlitzia rosmarinus plant called Keliab was used as a natural and nontoxic alkaline source for simultaneous synthesis of CuO nanoparticles and surface modification of polyester without using any other compounds. The images of field-emission scanning electron microscopy, patterns of energy-dispersive spectroscopy, UV-visible spectrum and X-ray diffraction confirmed successful synthesis and loading of CuO nanoparticles on the polyester fabric. The treated fabrics showed very good antibacterial activities toward two pathogen bacteria including Staphylococcus aureus as a Gram-positive and Escherichia coli as a Gram-negative bacteria with no adverse effects on human dermal fibroblasts based on MTT test. The treated fabrics confirmed significant photocatalytic activity for degradation of methylene blue under sunlight, self-cleaning properties under UV light and also UV protection properties. Further a colorant effect along with an improvement in the wettability and mechanical properties of the treated fabrics were indicated. Overall, this method can be applied as a clean route for producing photo and bio active textiles protecting against UV irradiation. Copyright © 2017 Elsevier B.V. All rights reserved.

  7. In situ polymerization of monomers for polyphenylquinoxaline/graphite

    Science.gov (United States)

    Serafini, T. T.; Delvigs, P.; Vannucci, R. D.

    1973-01-01

    Methods currently used to prepare fiber reinforced, high temperature resistant polyphenylquinoxaline (PPQ) composites employ extremely viscous, low solids content solutions of high molecular weight PPQ polymers. An improved approach, described in this report, consists of impregnating the fiber with a solution of the appropriate monomers instead of a solution of previously synthesized high molecular weight polymer. Polymerization of the monomers occurs in situ on the fiber during the solvent removal and curing stages. The in situ polymerization approach greatly simplifies the fabrication of PPQ graphite fiber composites. The use of low viscosity monomeric type solutions facilitates fiber wetting, permits a high solids content, and eliminates the need for prior polymer synthesis.

  8. Characterization of VPO ammoxidation catalysts by in situ methods

    Energy Technology Data Exchange (ETDEWEB)

    Martin, A.; Luecke, B.; Brueckner, A.; Steinike, U. [Institut fuer Angewandte Chemie Berlin-Adlershof e.V., Berlin (Germany); Brzezinka, K.W. [Bundesanstalt fuer Materialforschung und -pruefung (BAM), Berlin (Germany); Meisel, M. [Humboldt-Universitaet, Berlin (Germany). Inst. fuer Chemie

    1998-12-31

    In-situ methods are well known as powerful tools in studying catalyst formation processes, their solid state properties under working conditions and the interaction with the feed, intermediates and products to reveal reaction mechanisms. This paper gives a short overview on results of intense studies using in-situ techniques to reveal VPO catalyst generation processes, interaction of educts, intermediates and products with VPO catalyst surfaces and mechanistic insights. Catalytic data of the ammoxidation of toluene on different VPOs complete these findings. The precursor-catalyst transformation processes were preferently investigated by in-situ XRD, in-situ Raman and in-situ ESR spectroscopy. The interaction of aromatic molecules and intermediates, resp., and VPO solid surfaces was followed by in-situ ESR and in-situ FTIR spectroscopy. Mechanistic information was mainly obtained using in-situ FTIR spectroscopy and the temporal-analysis-of-products (TAP) technique. Catalytic studies were carried out in a fixed-bed microreactor on pure (NH{sub 4}){sub 2}(VO){sub 3}(P{sub 2}O{sub 7}){sub 2}, generated [(NH{sub 4}){sub 2}(VO{sub 3})(P{sub 2}O{sub 7}){sub 2}+V{sub x}O{sub y}] catalysts, having different V{sub x}O{sub y} proportions by use of VOHPO{sub 4} x 1/2H{sub 2}O (V/P=1) and recently studied (VO){sub 3}(PO{sub 4}){sub 2} x 7 H{sub 2}O (V/P=1.5) precursors; the well-known (VO){sub 2}P{sub 2}O{sub 7} was used for comparison. (orig.)

  9. In situ synthesis of silver chloride nanoparticles into bacterial cellulose membranes

    International Nuclear Information System (INIS)

    Hu Weili; Chen Shiyan; Li Xin; Shi Shuaike; Shen Wei; Zhang Xiang; Wang Huaping

    2009-01-01

    In situ synthesis of silver chloride (AgCl) nanoparticles was carried out under ambient conditions in nanoporous bacterial cellulose (BC) membranes as nanoreactors. The growth of the nanoparticles was readily obtained by alternating dipping of BC membranes in the solution of silver nitrate or sodium chloride followed by a rinse step. X-ray diffraction (XRD) patterns indicated the existence of AgCl nanoparticles in the BC and scanning electron microscopy (SEM) images showed that the AgCl nanoparticles well dispersed on the surface of BC and penetrated into the BC network. The AgCl nanoparticle-impregnated BC membranes exhibited high hydrophilic ability and strong antimicrobial activity against Escherichia coli (Gram-negative) and Staphylococcus aureus (Gram-positive). The preparative procedure is facile and versatile, and provides a simple route to manufacturing of useful antimicrobial membranes, which would be a good alternative for antimicrobial wound dressing.

  10. Comparison between ex situ and in situ measurement methods for the assessment of radioactively contaminated land. Comparison between measurement methods for the characterisation of radioactively contaminated land

    International Nuclear Information System (INIS)

    Rostron, Peter D.; Ramsey, Michael H.; Heathcote, John A.

    2012-01-01

    In the UK, it is estimated that there may be 20,000,000 cubic metres of contaminated land at Sellafield alone. Harwell and Dounreay are known to have significant amounts of radioactive or nonradioactive contaminated land (NDA, 2006). It is therefore important to devise optimal methods for the characterisation of areas of land for radionuclide content, in order to enable cost-effective decommissioning. With chemical contaminants, ex situ measurements are made on a larger volume of soil than are in situ measurements, such as PXRF. However, the opposite is often true for the characterisation of radioactive contamination, when this involves the detection of penetrating radiation from γ-emitting radionuclides. This means that when investigating for hotspots of radioactive contamination at or near the ground surface, better coverage can be obtained using in situ methods. This leads to the question, what is the optimal strategy (e.g. percentage coverage, counting time) for in situ characterisation of radioactively contaminated land' Surveys on light-moderate contaminated areas of ground were conducted at Dounreay in order to compare the relative effectiveness of in situ and ex situ methods, both for the detection of radioactive hotspots and also for estimating the average radionuclide content of an area of ground. These surveys suggest that continuous coverage by in situ devices is more effective at hotspot detection, with ex situ laboratory measurements being less effective, although in one case elevated activity below 10 cm depth that was identified by ex situ measurement was not located by in situ measurement. The surveys also highlighted that careful choice of an appropriate spatial model is critical to the estimation of activity concentrations over averaging areas. Whereas continuous coverage may be considered necessary for hotspot identification, in the particular case of the detection of hot particles (where the particle is very small compared to the sampling

  11. Facile Low Temperature Hydrothermal Synthesis of BaTiO3 Nanoparticles Studied by In Situ X-ray Diffraction

    Directory of Open Access Journals (Sweden)

    Ola G. Grendal

    2018-06-01

    Full Text Available Ferroelectric materials are crucial for today’s technological society and nanostructured ferroelectric materials are important for the downscaling of devices. Controlled and reproducible synthesis of these materials are, therefore, of immense importance. Hydrothermal synthesis is a well-established synthesis route, with a large parameter space for optimization, but a better understanding of nucleation and growth mechanisms is needed for full utilization and control. Here we use in situ X-ray diffraction to follow the nucleation and growth of BaTiO3 formed by hydrothermal synthesis using two different titanium precursors, an amorphous titania precipitate slurry and a Ti-citric acid complex solution. Sequential Rietveld refinement was used to extract the time dependency of lattice parameters, crystallite size, strain, and atomic displacement parameters. Phase pure BaTiO3 nanoparticles, 10–15 nm in size, were successfully synthesized at different temperatures (100, 125, and 150 °C from both precursors after reaction times, ranging from a few seconds to several hours. The two precursors resulted in phase pure BaTiO3 with similar final crystallite size. Finally, two different growth mechanisms were revealed, where the effect of surfactants present during hydrothermal synthesis is discussed as one of the key parameters.

  12. Synthesis and characterization of PMMA/clay nanocomposites prepared by in situ polymerization assisted by sonication; Sintese e caracterizacao de nanocompositos de PMMA/MMTO via polimerizacao in situ assistida por ultrassom

    Energy Technology Data Exchange (ETDEWEB)

    Prado, Bruna R.; Bartoli, Julio R., E-mail: bartoli@unicamp.br [Universidade Estadual de Campinas (UNICAMP), Campinas, SP (Brazil); Ito, Edson N. [Universidade Federal do Rio Grande do Norte (UFRN), Natal, RN (Brazil)

    2015-07-01

    In this work is presented the synthesis of nanocomposites of poly(methyl methacrylate), PMMA, with organically montmorillonite (OMMT) modified clays by in situ polymerization assisted by sonication. A statistically designed experiment was used, central composing design (CCD), to study the effect of synthesis variables on the dispersion of nanoparticles in PMMA matrix. The processing and formulation factors studied were: energy of sonication and Flory-Huggins interaction parameter between PMMA and organoclay. The structural (XRD) and morphological (TEM) characterizations of the PMMA/OMMT nanocomposites are compared with the literature. It was observed significant exfoliation of OMMT modified with hydroxyl groups in the nanocomposites of PMMA, mainly at the low ultrasonic energy level (90 and 105 kJ) studied. (author)

  13. Synthesis mechanism of an Al-Ti-C grain refiner master alloy prepared by a new method

    Science.gov (United States)

    Zhang, B. Q.; Lu, L.; Lai, M. O.; Fang, H. S.; Ma, H. T.; Li, J. G.

    2003-08-01

    The mechanisms of in-situ synthesis of an Al-Ti-C grain-refiner master alloy, prepared by adding a powder mixture of potassium titanium fluoride and carbon into an aluminum melt, have been systematically studied. It was found that vigorous reactions occurred at the initial stage of reaction and then slowed down. After about 20 minutes, the reactions, which led the formation of blocky titanium aluminides and submicron titanium carbides in the aluminum matrix, appeared to reach completion. Potassium titanium fluoride reacted with aluminum and carbon at 724 °C and 736 °C, respectively, resulting in the formation of titanium aluminides and titanium carbides in the aluminum matrix as well as in the formation of a low-melting-point slag of binary potassium aluminofluorides. The reaction between potassium titanium fluoride and carbon is believed to be the predominant mechanism in the synthesis of TiC by this method.

  14. Synthesis of 2-phenylnaphthalenes from styryl-2-methoxybenzenes.

    Science.gov (United States)

    Mudududdla, Ramesh; Sharma, Rohit; Abbat, Sheenu; Bharatam, Prasad V; Vishwakarma, Ram A; Bharate, Sandip B

    2014-10-18

    A new simple and efficient method for the synthesis of 2-phenylnaphthalenes from electron-rich 1-styryl-2-methoxybenzenes has been described. The reaction proceeds via TFA catalyzed C-C bond cleavage followed by intermolecular [4+2]-Diels-Alder cycloaddition of an in situ formed styrenyl trifluoroacetate intermediate. The quantum chemical calculations identified the transition state for the cycloaddition reaction and helped in tracing the reaction mechanism. The method has been efficiently utilized for synthesis of the phenanthrene skeleton and a naphthalene-based potent and selective ER-β agonist.

  15. In situ Generated Ruthenium Catalyst Systems Bearing Diverse N-Heterocyclic Carbene Precursors for Atom-Economic Amide Synthesis from Alcohols and Amines.

    Science.gov (United States)

    Cheng, Hua; Xiong, Mao-Qian; Cheng, Chuan-Xiang; Wang, Hua-Jing; Lu, Qiang; Liu, Hong-Fu; Yao, Fu-Bin; Chen, Cheng; Verpoort, Francis

    2018-02-16

    The transition-metal-catalyzed direct synthesis of amides from alcohols and amines is herein demonstrated as a highly environmentally benign and atom-economic process. Among various catalyst systems, in situ generated N-heterocyclic carbene (NHC)-based ruthenium (Ru) halide catalyst systems have been proven to be active for this transformation. However, these existing catalyst systems usually require an additional ligand to achieve satisfactory results. In this work, through extensive screening of a diverse variety of NHC precursors, we discovered an active in situ catalyst system for efficient amide synthesis without any additional ligand. Notably, this catalyst system was found to be insensitive to the electronic effects of the substrates, and various electron-deficient substrates, which were not highly reactive with our previous catalyst systems, could be employed to afford the corresponding amides efficiently. Furthermore, mechanistic investigations were performed to provide a rationale for the high activity of the optimized catalyst system. NMR-scale reactions indicated that the rapid formation of a Ru hydride intermediate (signal at δ=-7.8 ppm in the 1 H NMR spectrum) after the addition of the alcohol substrate should be pivotal in establishing the high catalyst activity. Besides, HRMS analysis provided possible structures of the in situ generated catalyst system. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  16. Synthesis and luminescence properties of hybrid organic-inorganic transparent titania thin film activated by in-situ formed lanthanide complexes

    International Nuclear Information System (INIS)

    Wang Yige; Wang Li; Li Huanrong; Liu Peng; Qin Dashan; Liu Binyuan; Zhang Wenjun; Deng Ruiping; Zhang Hongjie

    2008-01-01

    Stable transparent titania thin films were fabricated at room temperature by combining thenoyltrifluoroacetone (TTFA)-modified titanium precursors with amphiphilic triblock poly(ethylene oxide)-poly(propylene oxide)-poly(ethylene oxide) (PEO-PPO-PEO, P123) copolymers. The obtained transparent titania thin films were systematically investigated by IR spectroscopy, PL emission and excitation spectroscopy and transmission electron microscopy. IR spectroscopy indicates that TTFA coordinates the titanium center during the process of hydrolysis and condensation. Luminescence spectroscopy confirms the in-situ formation of lanthanide complexes in the transparent titania thin film. TEM image shows that the in-situ formed lanthanide complexes were homogeneously distributed throughout the whole thin film. The quantum yield and the number of water coordinated to lanthanide metal center have been theoretically determined based on the luminescence data. - Graphical abstract: Novel stable luminescent organic-inorganic hybrid titania thin film with high transparency activated by in-situ formed lanthanide complexes have been obtained at room temperature via a simple one-pot synthesis approach by using TTFA-modified titanium precursor with amphiphilic triblock copolymer P123. The obtained hybrid thin film displays bright red (or green), near-monochromatic luminescence due to the in-situ formed lanthanide complex

  17. In Situ Synthesis of Reduced Graphene Oxide and Gold Nanocomposites for Nanoelectronics and Biosensing

    Directory of Open Access Journals (Sweden)

    Chen Peng

    2011-01-01

    Full Text Available Abstract In this study, an in situ chemical synthesis approach has been developed to prepare graphene–Au nanocomposites from chemically reduced graphene oxide (rGO in aqueous media. UV–Vis absorption, atomic force microscopy, scanning electron microscopy, transmission electron microscopy, and Raman spectroscopy were used to demonstrate the successful attachment of Au nanoparticles to graphene sheets. Configured as field-effect transistors (FETs, the as-synthesized single-layered rGO-Au nanocomposites exhibit higher hole mobility and conductance when compared to the rGO sheets, promising its applications in nanoelectronics. Furthermore, we demonstrate that the rGO-Au FETs are able to label-freely detect DNA hybridization with high sensitivity, indicating its potentials in nanoelectronic biosensing.

  18. An improved in situ method for determining depth distributions of gamma-ray emitting radionuclides

    International Nuclear Information System (INIS)

    Benke, R.R.; Kearfott, K.J.

    2001-01-01

    In situ gamma-ray spectrometry determines the quantities of radionuclides in some medium with a portable detector. The main limitation of in situ gamma-ray spectrometry lies in determining the depth distribution of radionuclides. This limitation is addressed by developing an improved in situ method for determining the depth distributions of gamma-ray emitting radionuclides in large area sources. This paper implements a unique collimator design with conventional radiation detection equipment. Cylindrically symmetric collimators were fabricated to allow only those gamma-rays emitted from a selected range of polar angles (measured off the detector axis) to be detected. Positioned with its axis normal to surface of the media, each collimator enables the detection of gamma-rays emitted from a different range of polar angles and preferential depths. Previous in situ methods require a priori knowledge of the depth distribution shape. However, the absolute method presented in this paper determines the depth distribution as a histogram and does not rely on such assumptions. Other advantages over previous in situ methods are that this method only requires a single gamma-ray emission, provides more detailed depth information, and offers a superior ability for characterizing complex depth distributions. Collimated spectrometer measurements of buried area sources demonstrated the ability of the method to yield accurate depth information. Based on the results of actual measurements, this method increases the potential of in situ gamma-ray spectrometry as an independent characterization tool in situations with unknown radionuclide depth distributions

  19. Nitroxide radicals formed in situ as polymer chain growth regulators

    International Nuclear Information System (INIS)

    Kolyakina, Elena V; Grishin, Dmitry F

    2009-01-01

    Published data on controlled synthesis of macromolecules using nitroxide radicals, formed in situ during polymerization, as polymer chain growth regulators are systematized and generalized. The attention is focused on the mechanism of polymer chain growth control during reversibly inhibited radical homopolymerization and the effect of structure of precursors and regulating additives on the polymerization kinetics of monomers of different nature and the molecular-mass characteristics of the polymers thus formed. The key methods for generation of nitroxide radicals directly during polymerization are considered. The prospects for development and practical use of these approaches for the synthesis of new polymeric materials are evaluated.

  20. In situ self-sacrificed template synthesis of vanadium nitride/nitrogen-doped graphene nanocomposites for electrochemical capacitors.

    Science.gov (United States)

    Liu, Hong-Hui; Zhang, Hong-Ling; Xu, Hong-Bin; Lou, Tai-Ping; Sui, Zhi-Tong; Zhang, Yi

    2018-03-15

    Vanadium nitride and graphene have been widely used as pseudo-capacitive and electric double-layer capacitor electrode materials for electrochemical capacitors, respectively. However, the poor cycling stability of vanadium nitride and the low capacitance of graphene impeded their practical applications. Herein, we demonstrated an in situ self-sacrificed template method for the synthesis of vanadium nitride/nitrogen-doped graphene (VN/NGr) nanocomposites by the pyrolysis of a mixture of dicyandiamide, glucose, and NH 4 VO 3 . Vanadium nitride nanoparticles of the size in the range of 2 to 7 nm were uniformly embedded into the nitrogen-doped graphene skeleton. Furthermore, the VN/NGr nanocomposites with a high specific surface area and pore volume showed a high specific capacitance of 255 F g -1 at 10 mV s -1 , and an excellent cycling stability (94% capacitance retention after 2000 cycles). The excellent capacitive properties were ascribed to the excellent conductivity of nitrogen-doped graphene, high surface area, high pore volume, and the synergistic effect between vanadium nitride and nitrogen-doped graphene.

  1. Synthesis and characterization of polypropylene/graphite nano composite preparation for in situ polymerization

    International Nuclear Information System (INIS)

    Montagna, L.S.; Fim, F. de C.; Galland, G.B.

    2010-01-01

    This paper presents the synthesis of polypropylene/graphite nanocomposites through in situ polymerization, using the metallocene catalyst C 20 H 16 Cl 2 Zr (dichloro(rac-ethylenebis(indenyl))zircon(IV)). The graphite nanosheets in nano dimensions were added to the polymer matrix in percentages of 0.6;1.0;4.2;4.8 and 6.0% (w/w). The TEM images indicated that the thickness of graphite nanosheets ranged from 4 to 60 nm and by means of XRD analysis it was observed that the physical and chemical treatment did not destroyed the graphite layers. The presence of nanosheets did not decrease the catalytic activity of the nanocomposites. TEM images and XRD analysis of nanocomposites showed a good dispersion of the graphite nanosheets in the polypropylene matrix. (author)

  2. In-situ synthesis of magnetic iron-oxide nanoparticle-nanofibre composites using electrospinning

    International Nuclear Information System (INIS)

    Burke, Luke; Mortimer, Chris J.; Curtis, Daniel J.; Lewis, Aled R.; Williams, Rhodri; Hawkins, Karl; Maffeis, Thierry G.G.; Wright, Chris J.

    2017-01-01

    We demonstrate a facile, one-step process to form polymer scaffolds composed of magnetic iron oxide nanoparticles (MNPs) contained within electrospun nano- and micro-fibres of two biocompatible polymers, Poly(ethylene oxide) (PEO) and Poly(vinyl pyrrolidone) (PVP). This was achieved with both needle and free-surface electrospinning systems demonstrating the scalability of the composite fibre manufacture; a 228 fold increase in fibre fabrication was observed for the free-surface system. In all cases the nanoparticle-nanofibre composite scaffolds displayed morphological properties as good as or better than those previously described and fabricated using complex multi-stage techniques. Fibres produced had an average diameter (Needle-spun: 125 ± 18 nm (PEO) and 1.58 ± 0.28 μm (PVP); Free-surface electrospun: 155 ± 31 nm (PEO)) similar to that reported previously, were smooth with no bead defects. Nanoparticle-nanofibre composites were characterised using scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), dynamic light scattering (DLS) (Nanoparticle average diameter ranging from 8 ± 3 nm to 27 ± 5 nm), XRD (Phase of iron oxide nanoparticles identified as magnetite) and nuclear magnetic resonance relaxation measurements (NMR) (T1/T2: 32.44 for PEO fibres containing MNPs) were used to verify the magnetic behaviour of MNPs. This study represents a significant step forward for production rates of magnetic nanoparticle-nanofibre composite scaffolds by the electrospinning technique. - Graphical abstract: We present a novel facile, one-step process for the in-situ synthesis of magnetic iron oxide nanoparticle-nanofibre composites using both needle and free-surface electrospinning. This is a significant step forward for production rates of magnetic nanoparticle-nanofibre scaffolds both in terms of fibre and nanoparticle production. - Highlights: • We present a novel process for the in-situ synthesis of magnetic iron oxide nanoparticle

  3. In-situ synthesis of magnetic iron-oxide nanoparticle-nanofibre composites using electrospinning

    Energy Technology Data Exchange (ETDEWEB)

    Burke, Luke; Mortimer, Chris J. [Biomaterials, Biofouling and Biofilms Engineering Laboratory (B3EL), Systems and Process Engineering Centre, College of Engineering, Swansea University, Fabian Way, Swansea SA1 8EN (United Kingdom); Systems and Process Engineering Centre, College of Engineering, Swansea University, Fabian Way, Swansea SA1 8EN (United Kingdom); Curtis, Daniel J.; Lewis, Aled R.; Williams, Rhodri [Systems and Process Engineering Centre, College of Engineering, Swansea University, Fabian Way, Swansea SA1 8EN (United Kingdom); Hawkins, Karl [Centre for NanoHealth (CNH), Swansea University, Singleton Park, Swansea SA2 8PP (United Kingdom); Maffeis, Thierry G.G. [Systems and Process Engineering Centre, College of Engineering, Swansea University, Fabian Way, Swansea SA1 8EN (United Kingdom); Wright, Chris J., E-mail: c.wright@swansea.ac.uk [Biomaterials, Biofouling and Biofilms Engineering Laboratory (B3EL), Systems and Process Engineering Centre, College of Engineering, Swansea University, Fabian Way, Swansea SA1 8EN (United Kingdom); Systems and Process Engineering Centre, College of Engineering, Swansea University, Fabian Way, Swansea SA1 8EN (United Kingdom); Centre for NanoHealth (CNH), Swansea University, Singleton Park, Swansea SA2 8PP (United Kingdom)

    2017-01-01

    We demonstrate a facile, one-step process to form polymer scaffolds composed of magnetic iron oxide nanoparticles (MNPs) contained within electrospun nano- and micro-fibres of two biocompatible polymers, Poly(ethylene oxide) (PEO) and Poly(vinyl pyrrolidone) (PVP). This was achieved with both needle and free-surface electrospinning systems demonstrating the scalability of the composite fibre manufacture; a 228 fold increase in fibre fabrication was observed for the free-surface system. In all cases the nanoparticle-nanofibre composite scaffolds displayed morphological properties as good as or better than those previously described and fabricated using complex multi-stage techniques. Fibres produced had an average diameter (Needle-spun: 125 ± 18 nm (PEO) and 1.58 ± 0.28 μm (PVP); Free-surface electrospun: 155 ± 31 nm (PEO)) similar to that reported previously, were smooth with no bead defects. Nanoparticle-nanofibre composites were characterised using scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDX), dynamic light scattering (DLS) (Nanoparticle average diameter ranging from 8 ± 3 nm to 27 ± 5 nm), XRD (Phase of iron oxide nanoparticles identified as magnetite) and nuclear magnetic resonance relaxation measurements (NMR) (T1/T2: 32.44 for PEO fibres containing MNPs) were used to verify the magnetic behaviour of MNPs. This study represents a significant step forward for production rates of magnetic nanoparticle-nanofibre composite scaffolds by the electrospinning technique. - Graphical abstract: We present a novel facile, one-step process for the in-situ synthesis of magnetic iron oxide nanoparticle-nanofibre composites using both needle and free-surface electrospinning. This is a significant step forward for production rates of magnetic nanoparticle-nanofibre scaffolds both in terms of fibre and nanoparticle production. - Highlights: • We present a novel process for the in-situ synthesis of magnetic iron oxide nanoparticle

  4. Entangled zinc-ditetrazolate frameworks involving in situ ligand synthesis and topological modulation by various secondary N-donor ligands

    International Nuclear Information System (INIS)

    Li Yunwu; Chen Weilin; Wang Yonghui; Li Yangguang; Wang Enbo

    2009-01-01

    The introduction of various secondary N-donor ligands into an in situ ditetrazolate-ligand synthesis system of terephthalonitrile, NaN 3 and ZnCl 2 led to the formation of three new entangled frameworks Zn(pdtz)(4,4'-bipy).3H 2 O (1), [Zn(pdtz)(bpp)] 2 .3H 2 O (2) and Zn(pdtz) 0.5 (N 3 )(2,2'-bipy) (3) (4,4'-bipy=4,4'-bipyridine; bpp=1,3-bis(4-pyridyl)propane; 2,2'-bipy=2,2'-bipyridine; H 2 pdtz=5,5'-1,4-phenylene-ditetrazole). The formation of pdtz 2- ligand involves the Sharpless [2+3] cycloaddition reaction between terephthalonitrile and NaN 3 in the presence of Zn 2+ ion as a Lewis-acid catalyst under hydrothermal conditions. Compound 1 exhibits a fivefold interpenetrating 3D framework based on the diamondoid topology. Compound 2 displays a twofold parallel interpenetrating framework based on the wavelike individual network. Compound 3 possesses a 2D puckered network. These new Zn-ditetrazolate frameworks are highly dependent on the modulation of different secondary N-donor ligands. Their luminescent properties were investigated. - Graphical abstract: Three new entangled frameworks were prepared by an in situ ditetrazolate-ligand synthesis system assisted with various auxiliary N-donor ligands. The entangled structures can be modulated by different secondary ligands.

  5. Demonstration of a collimated in situ method for determining depth distributions using gamma-ray spectrometry

    CERN Document Server

    Benke, R R

    2002-01-01

    In situ gamma-ray spectrometry uses a portable detector to quantify radionuclides in materials. The main shortcoming of in situ gamma-ray spectrometry has been its inability to determine radionuclide depth distributions. Novel collimator designs were paired with a commercial in situ gamma-ray spectrometry system to overcome this limitation for large area sources. Positioned with their axes normal to the material surface, the cylindrically symmetric collimators limited the detection of un attenuated gamma-rays from a selected range of polar angles (measured off the detector axis). Although this approach does not alleviate the need for some knowledge of the gamma-ray attenuation characteristics of the materials being measured, the collimation method presented in this paper represents an absolute method that determines the depth distribution as a histogram, while other in situ methods require a priori knowledge of the depth distribution shape. Other advantages over previous in situ methods are that this method d...

  6. Droplet-based microfluidic method for synthesis of microparticles

    CSIR Research Space (South Africa)

    Mbanjwa, MB

    2012-10-01

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

  7. One-step synthesis and structural features of CdS/montmorillonite nanocomposites.

    Science.gov (United States)

    Han, Zhaohui; Zhu, Huaiyong; Bulcock, Shaun R; Ringer, Simon P

    2005-02-24

    A novel synthesis method was introduced for the nanocomposites of cadmium sulfide and montmorillonite. This method features the combination of an ion exchange process and an in situ hydrothermal decomposition process of a complex precursor, which is simple in contrast to the conventional synthesis methods that comprise two separate steps for similar nanocomposite materials. Cadmium sulfide species in the composites exist in the forms of pillars and nanoparticles, the crystallized sulfide particles are in the hexagonal phase, and the sizes change when the amount of the complex for the synthesis is varied. Structural features of the nanocomposites are similar to those of the clay host but changed because of the introduction of the sulfide into the clay.

  8. In situ polymerization of monomers for polyphenylquinoxaline/graphite fiber composites

    Science.gov (United States)

    Serafini, T. T.; Delvigs, P.; Vannucci, R. D.

    1974-01-01

    Methods currently used to prepare fiber reinforced, high temperature resistant polyphenylquinoxaline (PPQ) composites employ extremely viscous, low solids content solutions of high molecular weight PPQ polymers. An improved approach, described in this report, consists of impregnating the fiber with a solution of the appropriate monomers instead of a solution of previously synthesized high molecular weight polymer. Polymerization of the monomers occurs in situ on the fiber during the solvent removal and curing stages. The in situ polymerization approach greatly simplifies the fabrication of PPQ graphite fiber composites. The use of low viscosity monomeric type solutions facilitates fiber wetting, permits a high solids content, and eliminates the need for prior polymer synthesis.

  9. Synthesis of aluminium nanoparticles by arc evaporation of an ...

    Indian Academy of Sciences (India)

    Administrator

    Abstract. Aluminium nanoparticles (Al Nps) are synthesized using arc discharge method by applying direct current between aluminium electrodes in liquid environment without any use of vacuum equipment, heat exchangers, high temperatures furnaces and inert gases. After synthesis of Al Nps, in situ coating process on.

  10. Single Step In Situ Synthesis and Optical Properties of Polyaniline/ZnO Nanocomposites

    Directory of Open Access Journals (Sweden)

    Deepali Sharma

    2014-01-01

    Full Text Available Polyaniline/ZnO nanocomposites were prepared by in situ oxidative polymerization of aniline monomer in the presence of different weight percentages of ZnO nanostructures. The steric stabilizer added to prevent the agglomeration of nanostructures in the polymer matrix was found to affect the final properties of the nanocomposite. ZnO nanostructures of various morphologies and sizes were prepared in the absence and presence of sodium lauryl sulphate (SLS surfactant under different reaction conditions like in the presence of microwave radiation (microwave oven, under pressure (autoclave, under vacuum (vacuum oven, and at room temperature (ambient condition. The conductivity of these synthesized nanocomposites was evaluated using two-probe method and the effect of concentration of ZnO nanostructures on conductivity was observed. X-ray diffraction (XRD, scanning electron microscopy (SEM, transmission electron microscopy (TEM, Fourier transform infrared spectroscopy (FTIR, and UV-visible (UV-VIS spectroscopy techniques were used to characterize nanocomposites. The optical energy band gap of the nanocomposites was calculated from absorption spectra and ranged between 1.5 and 3.21 eV. The reported values depicted the blue shift in nanocomposites as compared to the band gap energies of synthesized ZnO nanostructures. The present work focuses on the one-step synthesis and potential use of PANI/ZnO nanocomposite in molecular electronics as well as in optical devices.

  11. In situ investigation of catalysts for alcohol synthesis

    DEFF Research Database (Denmark)

    Duchstein, Linus Daniel Leonhard; Sharafutdinov, Irek; Wu, Qiongxiao

    consists of three complimentary in situ techniques: (1) Activity measurements based on a reactor connected to a gas chromatograph (GC), (2) In situ x-ray diffractometer (XRD) measurements based on a reactor cell connected to a mass spectrometer (MS), and (3) environmental TEM (ETEM) that allows...... distribution, measured both macroscopically (XRD) and microscopically (ETEM), with the catalytic activity....

  12. In situ methods for Li-ion battery research: A review of recent developments

    Science.gov (United States)

    Harks, P. P. R. M. L.; Mulder, F. M.; Notten, P. H. L.

    2015-08-01

    A considerable amount of research is being directed towards improving lithium-ion batteries in order to meet today's market demands. In particular in situ investigations of Li-ion batteries have proven extremely insightful, but require the electrochemical cell to be fully compatible with the conditions of the testing method and are therefore often challenging to execute. Advantageously, in the past few years significant progress has been made with new, more advanced, in situ techniques. Herein, a comprehensive overview of in situ methods for studying Li-ion batteries is given, with the emphasis on new developments and reported experimental highlights.

  13. Effect of aging hardening on in situ synthesis magnesium matrix composites

    International Nuclear Information System (INIS)

    Zhang Xiuqing; Liao Lihua; Ma Naiheng; Wang Haowei

    2006-01-01

    Magnesium matrix composites reinforced with TiC particulates was synthesized using in situ synthesis technique. The result of XRD revealed the presence of TiC in precursor blocks and TiC/AZ91 composites. Effect of aging hardening on the composites was described using Brinell hardness measurements and scanning electron microscopy (SEM). The results revealed that the aging hardening peak of TiC/AZ91 composite appeared earlier comparatively with that of AZ91 magnesium alloy. And the appearance of aging hardening peak was earlier under the higher aging temperature such as 200 deg. C. The precipitating behavior of Mg 17 Al 12 phase in AZ91 alloy and TiC/AZ91 composites was described. Little discontinuous was discovered in the composites, and the amount of continuous precipitate in the composite matrix is smaller comparatively to that of AZ91 alloy. These results were analyzed with the fine grain size, much more interface between TiC and magnesium and high-density dislocation in magnesium matrix, which was contributed to the addition of TiC particulates

  14. A combined in situ XAS-XRPD-Raman study of Fischer-Tropsch synthesis over a carbon supported Co catalyst

    DEFF Research Database (Denmark)

    Tsakoumis, Nikolaos E.; Dehghan, Roya; Johnsen, Rune

    2013-01-01

    A cobalt based Fischer-Tropsch synthesis (FTS) catalyst, supported on a carbon nanofibers/carbon felt composite (Co/CNF/CF) was studied in situ at realistic conditions. The catalyst was monitored by Xray absorption spectroscopy (XAS), high-resolution X-ray powder diffraction (HR-XRPD) and Raman...... spectroscopy, while changes in the gas phase were observed by mass spectrometry (MS). Transmission electron microscopy (TEM) was also applied to characterise the catalyst. The catalyst has a bimodal particle size distribution and exhibits a high deactivation rate. During the in situ study the catalyst appears...... to reduce further at the induction period of FTS, while crystallite growth is been detected in the same period. At steady state FTS the amount of metallic Co is constant. A change in the volumetric flow towards higher conversions did not affect the degree of reduction or the crystallite size of the catalyst...

  15. In situ chemical synthesis of ruthenium oxide/reduced graphene oxide nanocomposites for electrochemical capacitor applications.

    Science.gov (United States)

    Kim, Ji-Young; Kim, Kwang-Heon; Yoon, Seung-Beom; Kim, Hyun-Kyung; Park, Sang-Hoon; Kim, Kwang-Bum

    2013-08-07

    An in situ chemical synthesis approach has been developed to prepare ruthenium oxide/reduced graphene oxide (RGO) nanocomposites. It is found that as the C/O ratio increases, the number density of RuO2 nanoparticles decreases, because the chemical interaction between the Ru ions and the oxygen-containing functional groups provides anchoring sites where the nucleation of particles takes place. For electrochemical capacitor applications, the microwave-hydrothermal process was carried out to improve the conductivity of RGO in RuO2/RGO nanocomposites. The significant improvement in capacitance and high rate capability might result from the RuO2 nanoparticles used as spacers that make the interior layers of the reduced graphene oxide electrode available for electrolyte access.

  16. In-situ PXRD studies of ZnO nanoparticle growth: How do various salts influence the hydrothermal growth of ZnO?

    DEFF Research Database (Denmark)

    Bøjesen, Espen Drath

    ZnO is a material of great scientific and everyday relevance; it is used widely in all sorts of application. Synthesis of ZnO nanoparticles can be performed by a wide assortment of methods and a tremendous variety of sizes and shapes, it has been suggested that ZnO is the one known compound showing...... the broadest range of nanostructures. Previously many different in-situ characterization methods have been used to investigate the ZnO formation under various synthesis conditions; these include UV-VIS and SAXS. These methods were primarily used to give information on particle size of ZnO formed using soft...... chemical methods and non-aqueous solvents. In our work we have studied the formation of ZnO during hydrothermal syntheses using in-situ powder X-ray diffraction, thus enabling us to extract crystallographic as well as microstructural information. The data was analyzed using Rietveld refinement and whole...

  17. In situ synthesis of oriented NiS nanotube arrays on FTO as high-performance counter electrode for dye-sensitized solar cells

    Energy Technology Data Exchange (ETDEWEB)

    Li, Yan, E-mail: liyan-nwnu@163.com [Key Laboratory of Atomic and Molecular Physics & Functional Materials of Gansu Province, College of Physics and Electronic Engineering, Northwest Normal University, Lanzhou, 730070 (China); Chang, Yin [Key Laboratory of Atomic and Molecular Physics & Functional Materials of Gansu Province, College of Physics and Electronic Engineering, Northwest Normal University, Lanzhou, 730070 (China); Zhao, Yun [Laboratory of Clean Energy Chemistry and Materials, Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences, Lanzhou, 730000 (China); Wang, Jian; Wang, Cheng-wei [Key Laboratory of Atomic and Molecular Physics & Functional Materials of Gansu Province, College of Physics and Electronic Engineering, Northwest Normal University, Lanzhou, 730070 (China)

    2016-09-15

    Oriented nickel sulfide (NiS) nanotube arrays were successfully in-situ fabricated on conductive glass substrate and used directly as counter electrode for dye-sensitized solar cells without any post-processing. Compared with Pt counter electrode, for the beneficial effect of electronic transport along the axial direction through the arrays to the substrate, oriented NiS nanotube arrays exhibit both higher electrocatalytic activity for I{sub 3}{sup −} reduction and better electrochemical stability, resulting in a significantly improved power conversion efficiency of 9.8%. Such in-situ grown oriented sulfide semiconductor nanotube arrays is expected to lead a new class structure of composites for highly efficient cathode materials. - Highlights: • In-situ synthesis strategy was proposed to construct oriented NiS nanotube arrays. • Such oriented tube nanostructure benefits the electronic transport along the axial direction of the arrays. • As CE of DSSCs, NiS nanotube arrays exhibit both higher efficiency (9.8%) and electrochemical stability than Pt.

  18. Non-Aqueous Sol-Gel Synthesis of FePt Nanoparticles in the Absence of In Situ Stabilizers

    Directory of Open Access Journals (Sweden)

    Tobias Preller

    2018-05-01

    Full Text Available The synthesis of FePt nanocrystals is typically performed in an organic solvent at rather high temperatures, demanding the addition of the in situ stabilizers oleic acid and oleylamine to produce monomodal particles with well-defined morphologies. Replacing frequently-used solvents with organic media bearing functional moieties, the use of the stabilizers can be completely circumvented. In addition, various morphologies and sizes of the nanocrystals can be achieved by the choice of organic solvent. The kinetics of particle growth and the change in the magnetic behavior of the superparamagnetic FePt nanocrystals during the synthesis with a set of different solvents, as well as the resulting morphologies and stoichiometries of the nanoparticles were determined by powder X-ray diffraction (PXRD, small-angle X-ray scattering (SAXS, transmission electron microscopy (TEM, inductively coupled plasma optical emission spectroscopy (ICP-OES/mass spectrometry (ICP-MS, and superconducting quantum interference device (SQUID measurements. Furthermore, annealing of the as-prepared FePt nanoparticles led to the ordered L10 phase and, thus, to hard magnetic materials with varying saturation magnetizations and magnetic coercivities.

  19. The Advanced Aluminum Nitride Synthesis Methods and Its Applications: Patent Review.

    Science.gov (United States)

    Shishkin, Roman A; Elagin, Andrey A; Mayorova, Ekaterina S; Beketov, Askold R

    2016-01-01

    High purity nanosized aluminum nitride synthesis is a current issue for both industry and science. However, there is no up-to-date review considering the major issues and the technical solutions for different methods. This review aims to investigate the advanced methods of aluminum nitride synthesis and its development tendencies. Also the aluminum nitride application patents and prospects for development of the branch have been considered. The patent search on "aluminum nitride synthesis" has been carried out. The research activity has been analyzed. Special attention has been paid to the patenting geography and the leading researchers in aluminum nitride synthesis. Aluminum nitride synthesis methods have been divided into 6 main groups, the most studied approaches are carbothermal reduction (88 patents) and direct nitridation (107 patents). The current issues for each group have been analyzed; the main trends are purification of the final product and nanopowder synthesis. The leading researchers in aluminum nitride synthesis have represented 5 countries, namely: Japan, China, Russia, South Korea and USA. The main aluminum nitride application spheres are electronics (59,1 percent of applications) and new materials manufacturing (30,9 percent). The review deals with the state of the art data in nanosized aluminum nitride synthesis, the major issues and the technical solutions for different synthesis methods. It gives a full understanding of the development tendencies and of the current leaders in the sphere.

  20. Text-in-context: a method for extracting findings in mixed-methods mixed research synthesis studies.

    Science.gov (United States)

    Sandelowski, Margarete; Leeman, Jennifer; Knafl, Kathleen; Crandell, Jamie L

    2013-06-01

    Our purpose in this paper is to propose a new method for extracting findings from research reports included in mixed-methods mixed research synthesis studies. International initiatives in the domains of systematic review and evidence synthesis have been focused on broadening the conceptualization of evidence, increased methodological inclusiveness and the production of evidence syntheses that will be accessible to and usable by a wider range of consumers. Initiatives in the general mixed-methods research field have been focused on developing truly integrative approaches to data analysis and interpretation. The data extraction challenges described here were encountered, and the method proposed for addressing these challenges was developed, in the first year of the ongoing (2011-2016) study: Mixed-Methods Synthesis of Research on Childhood Chronic Conditions and Family. To preserve the text-in-context of findings in research reports, we describe a method whereby findings are transformed into portable statements that anchor results to relevant information about sample, source of information, time, comparative reference point, magnitude and significance and study-specific conceptions of phenomena. The data extraction method featured here was developed specifically to accommodate mixed-methods mixed research synthesis studies conducted in nursing and other health sciences, but reviewers might find it useful in other kinds of research synthesis studies. This data extraction method itself constitutes a type of integration to preserve the methodological context of findings when statements are read individually and in comparison to each other. © 2012 Blackwell Publishing Ltd.

  1. In-situ synthesis of Co_3O_4/graphite nanocomposite for high-performance supercapacitor electrode applications

    International Nuclear Information System (INIS)

    M, Gopalakrishnan; G, Srikesh; A, Mohan; V, Arivazhagan

    2017-01-01

    Highlights: • High surface area, which governs the specific capacitance. • High chemical and thermal stability. • Co_3O_4/graphite nanocomposite electrode shows lower resistance. - Abstract: In this work, a low cost and pollution free in-situ synthesis of phase pure Co_3O_4 nanoparticles and Co_3O_4/graphite nanocomposite have been successfully developed via co-precipitation method followed by the thermal treatment process. The prepared samples were characterized by powder X-ray diffraction, scanning electron microscope, high resolution transmission electron microscope, Fourier Transform Infrared Spectroscopy and electrochemical measurements. Electrochemical measurements such as cyclic voltammetry, galvanostatic charge–discharge, electrochemical impedance spectroscopy were carried out in 6 M KOH aqueous electrolytic solution. The results show the excellent maximum specific capacitive behavior of 239.5 F g"−"1 for pure and 395.04 F g"−"1 for Co_3O_4/graphite nanocomposite at a current density of 0.5 A g"−"1. This composite exhibits a good cyclic stability, with a small loss of 2.68% of maximum capacitance over a consecutive 1000 cycles. The investigation indicates that the prepared electrode material could be a potential and promising candidate for electrochemical supercapacitors.

  2. Facile Synthesis of In–Situ Nitrogenated Graphene Decorated by Few–Layer MoS2 for Hydrogen Evolution Reaction

    International Nuclear Information System (INIS)

    Dai, Xiaoping; Li, Zhanzhao; Du, Kangli; Sun, Hui; Yang, Ying; Zhang, Xin; Ma, Xingyu; Wang, Jie

    2015-01-01

    Graphical abstract: In–situ nitrogenated graphene–few layer MoS 2 composites are fabricated by combinating chemical and hydrothermal reduction. The resulting MoS 2 /N–rGO–HA by N 2 H 4 ·H 2 O and NH 3 ·H 2 O as co-reductant exhibits high activity and remarkable stability for hydrogen evolution reaction (HER). The excellent electro-catalytic performance is ascribed to the synergistic effects, confinement effects and highly dispersed MoS 2 nanosheets on N-doping rGO. Display Omitted -- Highlights: • In–situ nitrogenated graphene–few layer MoS 2 composites are fabricated by combinating chemical and hydrothermal co-reduction. • The resulting MoS 2 /N–rGO–HA exhibits high activity and remarkable stability for HER. • The excellent electro-catalytic performance is ascribed to the synergistic effects, confinement effects and highly dispersed MoS 2 nanosheets on N-doping rGO. -- Abstract: A facile one–step synthetic strategy by combinating chemical and hydrothermal reduction of graphene oxide and Mo precursor is proposed to fabricate in–situ nitrogenated graphene–few layer MoS 2 composite (MoS 2 /N–rGO–HA) for hydrogen evolution reaction (HER). The N–doping graphene nanosheets and highly dispersed MoS 2 nanosheets by ammonia and hydrozine as co–reductant have greatly promoted the N content, concentrations of pyridinic and graphitic N, the electron transport in electrodes, and assure high catalytic efficiency. The MoS 2 /N–rGO–HA composite exhibits extremely high activity in acidic solutions with a small onset potential of 100 mV and Tafel slope of 45 mV/dec, as well as a current density about 32.4 mA cm −2 at overpotential about 0.2 V. Moreover, such MoS 2 /N–rGO–HA electroncatalyst also shows an excellent stability during 1000 cycles with negligible loss of the cathodic current. This facile hydrothermal method could provide a promising strategy for the synthesis of in–situ nitrogen–doping graphene sheets and few

  3. A Synthesis of the Literature on Research Methods Education

    Science.gov (United States)

    Earley, Mark A.

    2014-01-01

    The purpose of this research synthesis is to examine the current research on teaching and learning research methods. The aims are to understand the themes present in the current literature and identify gaps in our understanding of how we teach, and how students learn, research methods. A synthesis of 89 studies generated three themes: (1)…

  4. New algorithms derived from the synthesis method. Application to diffusion problems

    International Nuclear Information System (INIS)

    Rouzaud, Philippe.

    1976-05-01

    Two algorithms to compute the neutron distribution in a nuclear reactor are presented. These algorithms, the iterative synthesis method (MSI) and the synthesis method by deflation (MSD), are derived from the classical synthesis method (MSC). They retain the most important advantages of MSC (computing time and memory storage reduced with regard to finite difference methods) and avoid its drawbacks: choice of trial functions; choice of weighting functions; choice of the number of terms (for MSD only). Extensive numerical checks of the three methods (MSC, MSI, MSD) were carried out on two fast reactor configurations described in plane geometry (X,Y). Monoenergetic and multigroup theories were successively used. The use of MSI and MSD allows a significant reduction of the discrepancies between the finite difference method and the synthesis method for the reactivity values and the flux distribution [fr

  5. Comparative study of in-situ filter test methods

    International Nuclear Information System (INIS)

    Marshall, M.; Stevens, D.C.

    1981-01-01

    Available methods of testing high efficiency particulate aerosol (HEPA) filters in-situ have been reviewed. In order to understand the relationship between the results produced by different methods a selection has been compared. Various pieces of equipment for generating and detecting aerosols have been tested and their suitability assessed. Condensation-nuclei, DOP (di-octyl phthalate) and sodium-flame in-situ filter test methods have been studied, using the 500 cfm (9000 m 3 /h) filter test rig at Harwell and in the field. Both the sodium-flame and DOP methods measure the penetration through leaks and filter material. However the measured penetration through filtered leaks depends on the aerosol size distribution and the detection method. Condensation-nuclei test methods can only be used to measure unfiltered leaks since condensation nuclei have a very low penetration through filtered leaks. A combination of methods would enable filtered and unfiltered leaks to be measured. A condensation-nucleus counter using n-butyl alcohol as the working fluid has the advantage of being able to detect any particle up to 1 μm in diameter, including DOP, and so could be used for this purpose. A single-particle counter has not been satisfactory because of interference from particles leaking into systems under extract, particularly downstream of filters, and because the concentration of the input aerosol has to be severely limited. The sodium-flame method requires a skilled operator and may cause safety and corrosion problems. The DOP method using a total light scattering detector has so far been the most satisfactory. It is fairly easy to use, measures reasonably low values of penetration and gives rapid results. DOP has had no adverse effect on HEPA filters over a long series of tests

  6. Synthesis of new pyrrole–pyridine-based ligands using an in situ Suzuki coupling method

    Directory of Open Access Journals (Sweden)

    Matthias Böttger

    2012-07-01

    Full Text Available The compounds 6-(pyrrol-2-yl-2,2‘-bipyridine, 2-(pyrrol-2-yl-1,10-phenanthroline and 2-(2-(N-methylbenz[d,e]imidazole-6-(pyrrol-2-yl-pyridine were synthesized by using an in situ generated boronic acid for the Suzuki coupling. Crystals of the products could be grown and exhibited interesting structures by X-ray analysis, one of them showing a chain-like network with the adjacent molecules linked to each other via intermolecular N–H…N hydrogen bonds.

  7. In situ generation of the Ohira-Bestmann reagent from stable sulfonyl azide: scalable synthesis of alkynes from aldehydes.

    Science.gov (United States)

    Jepsen, Tue Heesgaard; Kristensen, Jesper Langgaard

    2014-10-03

    We report an improved method for in situ generation of the Ohira-Bestmann reagent. Using the recently reported bench-stable imidazole-1-sulfonyl azide as diazotransfer reagent, this new method represents a scalable and convenient approach for the transformation of aldehydes into terminal alkynes. The method features an easier workup compared to the existing in situ protocol due to increased aqueous solubility of waste products.

  8. Modern methods for the synthesis of peptide-oligonucleotide conjugates

    International Nuclear Information System (INIS)

    Zubin, Evgenii M; Oretskaya, Tat'yana S; Romanova, Elena A

    2002-01-01

    The published data on the methods of chemical solution and solid-phase synthesis of peptide-oligonucleotide conjugates are reviewed. The known methods are systematised and their advantages and disadvantages are considered. The approaches to the solution synthesis of peptide-oligonucleotide conjugates are systematised according to the type of chemical bonds between the fragments, whereas those to the solid-phase synthesis are classified according to the procedure used for the preparation of conjugates, viz., stepwise elongation of oligonucleotide and peptide chains on the same polymeric support or solid-phase condensation of two presynthesised fragments. The bibliography includes 141 references.

  9. Synthesis of nano-sized amorphous boron powders through active dilution self-propagating high-temperature synthesis method

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Jilin [The State Key Laboratory of Advanced Technology for Materials Synthesis and Processing, Wuhan University of Technology, Wuhan 430070 (China); Gu, Yunle [School of Material Science and Engineering, Wuhan Institute of Technology, Wuhan 430073 (China); Li, Zili [The State Key Laboratory of Advanced Technology for Materials Synthesis and Processing, Wuhan University of Technology, Wuhan 430070 (China); Wang, Weimin, E-mail: wangwm@hotmail.com [The State Key Laboratory of Advanced Technology for Materials Synthesis and Processing, Wuhan University of Technology, Wuhan 430070 (China); Fu, Zhengyi [The State Key Laboratory of Advanced Technology for Materials Synthesis and Processing, Wuhan University of Technology, Wuhan 430070 (China)

    2013-06-01

    Graphical abstract: Nano-sized amorphous boron powders were synthesized by active dilution self-propagating high-temperature synthesis (SHS) method. The effects of endothermic reaction rate, the possible chemical reaction mechanism and active dilution model for synthesis of the product were also discussed. Highlights: ► Nano-sized amorphous boron powders were synthesized by active dilution self-propagating high-temperature synthesis method. ► The morphology, particle size and purity of the samples could be effectively controlled via changing the endothermic rate. ► The diluter KBH{sub 4} played an important role in active dilution synthesis of amorphous nano-sized boron powders. ► The active dilution method could be further popularized and become a common approach to prepare various inorganic materials. - Abstract: Nano-sized amorphous boron powders were synthesized by active dilution self-propagating high-temperature synthesis (SHS) method at temperatures ranging from 700 °C to 850 °C in a SHS furnace using Mg, B{sub 2}O{sub 3} and KBH{sub 4} as raw materials. Samples were characterized by X-ray powder diffraction (XRD), Laser particle size analyzer, Fourier transform infrared spectra (FTIR), X-ray energy dispersive spectroscopy (EDX), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and high-resolution transmission TEM (HRTEM). The boron powders demonstrated an average particle size of 50 nm with a purity of 95.64 wt.%. The diluter KBH{sub 4} played an important role in the active dilution synthesis of amorphous nano-sized boron powders. The effects of endothermic reaction rate, the possible chemical reaction mechanism and active dilution model for synthesis of the product were also discussed.

  10. Synthesis of nano-sized amorphous boron powders through active dilution self-propagating high-temperature synthesis method

    International Nuclear Information System (INIS)

    Wang, Jilin; Gu, Yunle; Li, Zili; Wang, Weimin; Fu, Zhengyi

    2013-01-01

    Graphical abstract: Nano-sized amorphous boron powders were synthesized by active dilution self-propagating high-temperature synthesis (SHS) method. The effects of endothermic reaction rate, the possible chemical reaction mechanism and active dilution model for synthesis of the product were also discussed. Highlights: ► Nano-sized amorphous boron powders were synthesized by active dilution self-propagating high-temperature synthesis method. ► The morphology, particle size and purity of the samples could be effectively controlled via changing the endothermic rate. ► The diluter KBH 4 played an important role in active dilution synthesis of amorphous nano-sized boron powders. ► The active dilution method could be further popularized and become a common approach to prepare various inorganic materials. - Abstract: Nano-sized amorphous boron powders were synthesized by active dilution self-propagating high-temperature synthesis (SHS) method at temperatures ranging from 700 °C to 850 °C in a SHS furnace using Mg, B 2 O 3 and KBH 4 as raw materials. Samples were characterized by X-ray powder diffraction (XRD), Laser particle size analyzer, Fourier transform infrared spectra (FTIR), X-ray energy dispersive spectroscopy (EDX), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and high-resolution transmission TEM (HRTEM). The boron powders demonstrated an average particle size of 50 nm with a purity of 95.64 wt.%. The diluter KBH 4 played an important role in the active dilution synthesis of amorphous nano-sized boron powders. The effects of endothermic reaction rate, the possible chemical reaction mechanism and active dilution model for synthesis of the product were also discussed

  11. Application of synthesis methods to two-dimensional fast reactor transient study

    International Nuclear Information System (INIS)

    Izutsu, Sadayuki; Hirakawa, Naohiro

    1978-01-01

    Space time synthesis and time synthesis codes were developed and applied to the space-dependent kinetics benchmark problem of a two-dimensional fast reactor model, and it was found both methods are accurate and economical for the fast reactor kinetics study. Comparison between the space time synthesis and the time synthesis was made. Also, in space time synthesis, the influence of the number of trial functions on the error and on the computing time and the effect of degeneration of expansion coefficients are investigated. The matrix factorization method is applied to the inversion of the matrix equation derived from the synthesis equation, and it is indicated that by the use of this scheme space-dependent kinetics problem of a fast reactor can be solved efficiently by space time synthesis. (auth.)

  12. Silver nanoparticles: Synthesis methods, bio-applications and properties.

    Science.gov (United States)

    Abbasi, Elham; Milani, Morteza; Fekri Aval, Sedigheh; Kouhi, Mohammad; Akbarzadeh, Abolfazl; Tayefi Nasrabadi, Hamid; Nikasa, Parisa; Joo, San Woo; Hanifehpour, Younes; Nejati-Koshki, Kazem; Samiei, Mohammad

    2016-01-01

    Silver nanoparticles size makes wide range of new applications in various fields of industry. Synthesis of noble metal nanoparticles for applications such as catalysis, electronics, optics, environmental and biotechnology is an area of constant interest. Two main methods for Silver nanoparticles are the physical and chemical methods. The problem with these methods is absorption of toxic substances onto them. Green synthesis approaches overcome this limitation. Silver nanoparticles size makes wide range of new applications in various fields of industry. This article summarizes exclusively scalable techniques and focuses on strengths, respectively, limitations with respect to the biomedical applicability and regulatory requirements concerning silver nanoparticles.

  13. In-situ synthesis of Ag nanoparticles by electron beam irradiation

    International Nuclear Information System (INIS)

    Gong, Jiangfeng; Liu, Hongwei; Jiang, Yuwen; Yang, Shaoguang; Liao, Xiaozhou; Liu, Zongwen; Ringer, Simon

    2015-01-01

    Ag nanoparticles were synthesized by electron beam irradiation in the transmission electron microscope chamber at room temperature and the growth mechanism was explored in detail. The sizes of the Ag nanoparticles are controlled by the electron beam current density. Two nanoparticle growth stages were identified. The first growth stage was dominated by the discharging effect, while the second stage was controlled by the heating effect. The nanoparticle synthesis method should be applicable to the synthesis of other metallic nanoparticles. - Highlights: • Ag nanoparticles were synthesized by electron beam irradiation in the transmission electron microscope chamber. • The sizes of the Ag nanoparticles are controlled by the electron beam current density. • The growth mechanism was studied, two growth stages were confirmed. • The first growth stage was dominated by the discharging effect, and the second stage was controlled by the heating effect.

  14. Efficient Synthesis of 1-Sulfonyl-1,2,3-triazoles

    Science.gov (United States)

    Raushel, Jessica; Fokin, Valery V.

    2010-01-01

    An efficient room temperature method for the synthesis of 1-sulfonyl-1,2,3-triazoles from in situ generated copper(I) acetylides and sulfonyl azides is described. Copper(I) thiophene-2-carboxylate (CuTC) catalyst produces the title compounds under both non-basic anhydrous and aqueous conditions in good yields. PMID:20931987

  15. Solid oxide electrode kinetics in light of in situ surface studies

    DEFF Research Database (Denmark)

    Mogensen, Mogens Bjerg

    2014-01-01

    The combination of in situ and in particular in operando characterization methods such as electrochemical impedance spectroscopy (EIS) on both technical and model electrode are well known ways to gain some practical insight in electrode reaction kinetics. Yet, is has become clear that in spite...... of the strengths it is not sufficient to reveal much details of the electrode mechanisms mainly because it provide average values only. Therefore it has to be combined with surface science methods in order to reveal the interface structure and composition. Ex situ methods have been very useful over the latest....... Furthermore, it seems that detailed mathematical modeling using new tools like COMSOL is necessary for the synthesis of the large amount of data for a well-characterized electrode into one physical meaningful picture. A brief review of literature an own data will be presented with a practical example of SOFC...

  16. Method for in situ carbon deposition measurement for solid oxide fuel cells

    Science.gov (United States)

    Kuhn, J.; Kesler, O.

    2014-01-01

    Previous methods to measure carbon deposition in solid oxide fuel cell (SOFC) anodes do not permit simultaneous electrochemical measurements. Electrochemical measurements supplemented with carbon deposition quantities create the opportunity to further understand how carbon affects SOFC performance and electrochemical impedance spectra (EIS). In this work, a method for measuring carbon in situ, named here as the quantification of gasified carbon (QGC), was developed. TGA experiments showed that carbon with a 100 h residence time in the SOFC was >99.8% gasified. Comparison of carbon mass measurements between the TGA and QGC show good agreement. In situ measurements of carbon deposition in SOFCs at varying molar steam/carbon ratios were performed to further validate the QGC method, and suppression of carbon deposition with increasing steam concentration was observed, in agreement with previous studies. The technique can be used to investigate in situ carbon deposition and gasification behavior simultaneously with electrochemical measurements for a variety of fuels and operating conditions, such as determining conditions under which incipient carbon deposition is reversible.

  17. The potential of high resolution ultrasonic in-situ methods

    International Nuclear Information System (INIS)

    Schuster, K.

    2010-01-01

    source and receivers and on the applied frequencies. With the help of identified phases in the ultrasonic wave field, their travel times and appropriate amplitudes kinematic and dynamic parameters are derived routinely. The most important are: P-wave velocity (longitudinal or compressional wave velocity (vp)), Sv-wave velocity (vertical polarised transversal or shear wave velocity (vsv), absolute amplitudes of first arrival (P-wave) and Sv-wave onset phases, normalised amplitudes of first arrival (P-wave) and Sv-wave onset phases, apparent frequency of first arrival phases (P-wave) and Sv-wave onset phases, in-situ dynamic elastic Poisson's ratio, in-situ dynamic elastic Young's modulus and in-situ dynamic elastic modulus of rigidity. The main qualities which were detected and/or characterised with the help of these parameters in the past years are: - Degree and extent of EDZ/EdZ. - Long and short term development of EDZ/EdZ (application of repetition measurements). - Borehole disturbed Zones (BdZ). - Small scale rock heterogeneities. - Seismic anisotropy. - Stress orientation via rotational interval velocity measurements. - Determination of dynamic elastic in-situ parameters. Results from repetition measurements showed the high reliability of the methods. Furthermore, in several experiments the ultrasonic methods were combined with other geotechnical or geophysical methods, for example permeability and geo-electrical methods. Results from a seismic anisotropy study at the Mont Terri Rock Laboratory are shown. Two sub-horizontal 2 m long boreholes with a distance of 1 m were used. Nearly 600 different ray paths were analysed. Depending on the angles of the ray paths (60 deg. -300 deg. and 120 deg. -240 deg. ) the P-wave velocities vary between 2600 and 3100 m/s. Lower velocities are supposed to be influenced by the EDZ. (authors)

  18. Simple method for preparing glucose biosensor based on in-situ polypyrrole cross-linked chitosan/glucose oxidase/gold bionanocomposite film.

    Science.gov (United States)

    Şenel, Mehmet

    2015-03-01

    A film of chitosan-polypyrrole-gold nanoparticles was fabricated by in-situ chemical synthesis method and its application in glucose biosensor was investigated. The obtained biosensor exhibited a high and reproducible sensitivity of 0.58μA/mM, response time ~4s, linear dynamic range from 1 to 20mM, correlation coefficient of R(2)=0.9981, and limit of detection (LOD), based on S/N ratio (S/N=3) of 0.068mM. A value of 1.83mM for the apparent Michaelis-Menten constant was obtained. The resulting bio-nanocomposite provided a suitable environment for the enzyme to retain its bioactivity at considerably extreme conditions, and the decorated gold nanoparticles in the bio-nanocomposite offer good affinity to enzyme. Copyright © 2014. Published by Elsevier B.V.

  19. Quantitative comparison of in situ soil CO2 flux measurement methods

    Science.gov (United States)

    Jennifer D. Knoepp; James M. Vose

    2002-01-01

    Development of reliable regional or global carbon budgets requires accurate measurement of soil CO2 flux. We conducted laboratory and field studies to determine the accuracy and comparability of methods commonly used to measure in situ soil CO2 fluxes. Methods compared included CO2...

  20. Multicomponent Synthesis of Isoindolinone Frameworks via RhIII -Catalysed in situ Directing Group-Assisted Tandem Oxidative Olefination/Michael Addition.

    Science.gov (United States)

    Wang, Liang; Liu, Xi; Liu, Jian-Biao; Shen, Jun; Chen, Qun; He, Ming-Yang

    2018-04-04

    A Rh III -catalysed three-component synthesis of isoindolinone frameworks via direct assembly of benzoyl chlorides, o-aminophenols and activated alkenes has been developed. The process involves in situ generation of o-aminophenol (OAP)-based bidentate directing group (DG), Rh III -catalysed tandem ortho C-H olefination and subsequent cyclization via aza-Michael addition. This protocol exhibits good chemoselectivity and functional group tolerance. Computational studies showed that the presence of hydroxyl group on the N-aryl ring could enhance the chemoselectivity of the reaction. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. Ammonia synthesis using magnetic induction method (MIM)

    Science.gov (United States)

    Puspitasari, P.; Razak, J. Abd; Yahya, N.

    2012-09-01

    The most challenging issues for ammonia synthesis is to get the high yield. New approach of ammonia synthesis by using Magnetic Induction Method (MIM) and the Helmholtz Coils has been proposed. The ammonia detection was done by using Kjeldahl Method and FTIR. The system was designed by using Autocad software. The magnetic field of MIM was vary from 100mT-200mT and the magnetic field for the Helmholtz coils was 14mT. The FTIR result shows that ammonia has been successfully formed at stretching peaks 1097,1119,1162,1236, 1377, and 1464 cm-1. UV-VIS result shows the ammonia bond at 195nm of wavelength. The ammonia yield was increase to 244.72μmole/g.h by using the MIM and six pairs of Helmholtz coils. Therefore this new method will be a new promising method to achieve the high yield ammonia at ambient condition (at 25δC and 1atm), under the Magnetic Induction Method (MIM).

  2. The synthesis method for design of electron flow sources

    Science.gov (United States)

    Alexahin, Yu I.; Molodozhenzev, A. Yu

    1997-01-01

    The synthesis method to design a relativistic magnetically - focused beam source is described in this paper. It allows to find a shape of electrodes necessary to produce laminar space charge flows. Electron guns with shielded cathodes designed with this method were analyzed using the EGUN code. The obtained results have shown the coincidence of the synthesis and analysis calculations [1]. This method of electron gun calculation may be applied for immersed electron flows - of interest for the EBIS electron gun design.

  3. Estimating grass and grass silage degradation characteristics by in situ and in vitro gas production methods

    Directory of Open Access Journals (Sweden)

    Danijel Karolyi

    2010-01-01

    Full Text Available Fermentation characteristics of grass and grass silage at different maturities were studied using in situ and in vitro gas production methods. In situ data determined difference between grass and silage. Degradable fraction decreased as grass matured while the undegradable fraction increased. Rate of degradation (kd was slower for silage than fresh grass. Gas production method (GP data showed that fermentation of degradable fraction was different between stage of maturity in both grass and silage. Other data did not show any difference with the exception for the rate of GP of soluble and undegradable fraction. The in situ degradation characteristics were estimated from GP characteristics. The degradable and undegradable fractions could be estimated by multiple relationships. Using the three-phases model for gas production kd and fermentable organic matter could be estimated from the same parameters. The only in situ parameter that could not be estimated with GP parameters was the soluble fraction. The GP method and the three phases model provided to be an alternative to the in situ method for animal feed evaluations.

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

    KAUST Repository

    Abulikemu, Mutalifu

    2014-11-05

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

  5. Synthesis of PANi-SiO2 Nanocomposite with In-Situ Polymerization Method: Nanoparticle Silica (NPS) Amorphous and Crystalline Phase

    Science.gov (United States)

    Munasir; Luvita, N. R. D.; Kusumawati, D. H.; Putri, N. P.; Triwikantoro; Supardi, Z. A. I.

    2018-03-01

    Silica which is synthesized from natural materials such as Bancar Tuban’s sand composited with Polyaniline (PANi), where the silica used are silica has an amorphous phase and cristobalite phase. In this research, the composite method used is in- situ polymerization, which is silica entered during the fabrication of PANi, then automatically silica will be substitute into the chain bonding of PANi. The aim of this research is to find out the results of a composite process using in-situ methods as well as differences in the morphology of PANi/a- SiO2 and PANi/c-SiO2. For the characterization of samples tested in the form of FTIR to determine the functional groups of the composite and SEM to determine the morphology of the sample. From the test results of FTIR are known composite possibility has occurred because there are several functional groups belonging to silica also functional groups belonging polyaniline, functional group that’s happened in wave numbers were almost identical between PANi/a-SiO2 and PANi/c-SiO2, but there are little differences were seen in the form of a graph generated from the peak and intensity that occurred charts for PANi/c-SiO2 has peak more pointed or sharp compared to PANi/a-SiO2 because that bond of crystal is strong, stiff and has a larger particle size than the amorphous composite. Then from the data of SEM seen clearly their morphological differences between PANi/a-SiO2 and PANi/c-SiO2 where polyaniline is composited with amorphous silica will have a fault that is not uniform or irregular different from PANi/c -SiO2 has a regular fault and this is corresponding with the nature of the typical structure of amorphous and crystalline.

  6. Poly I-lactide-layered double hydroxide nanocomposites via in situ polymerization of I-lactide

    DEFF Research Database (Denmark)

    Katiyar, Vimal; Gerds, N.; Koch, C.B.

    2010-01-01

    The use of clay nanofillers offers a potential route to improved barrier properties in polylactide films. Magnesium–aluminium layered double hydroxides (LDHs) are interesting in this respect and we therefore explored synthesis of PLA-LDH nanocomposites by ring-opening polymerization. This method ...... weight was significantly reduced when in-situ polymerization was conducted in the presence of the LDHs and we suggest that chain termination via LDH surface hydroxyl groups and/or metal-catalyzed degradation could be responsible.......The use of clay nanofillers offers a potential route to improved barrier properties in polylactide films. Magnesium–aluminium layered double hydroxides (LDHs) are interesting in this respect and we therefore explored synthesis of PLA-LDH nanocomposites by ring-opening polymerization. This method...

  7. In situ feeding rates of plantonic copepods: A comparison of four methods

    DEFF Research Database (Denmark)

    Kiørboe, Thomas; Møhlenberg, Flemming; Riisgård, Hans Ulrik

    1985-01-01

    into estimates of in situ algal grazing rates by means of independently estimated gut turnover times, and were compared with chlorophyll and particle-volume grazing rates of animals sampled simultaneously and incubated in water from the collection depth. In addition, egg-production rates of adult females were...... problems of the different methods are discussed, and it is concluded that they all approach representative (although minimum) estimates of in situ feeding rates....

  8. In situ thermal properties characterization using frequential methods

    Energy Technology Data Exchange (ETDEWEB)

    Carpentier, O.; Defer, D.; Antczak, E.; Chauchois, A.; Duthoit, B. [Laboratoire dArtois de Mecanique Thermique Instrumentation (LAMTI), FSA Universite dArtois, Technoparc Futura, 62400 Bethune (France)

    2008-07-01

    In numerous fields, especially that of geothermal energy, we need to know about the thermal behaviour of the soil now that the monitoring of renewable forms of energy is an ecological, economic and scientific issue. Thus heat from the soil is widely used for air-conditioning systems in buildings both in Canada and in the Scandinavian countries, and it is spreading. The effectiveness of this technique is based on the soils calorific potential and its thermophysical properties which will define the quality of the exchanges between the soil and a heat transfer fluid. This article puts forward a method to be used for the in situ thermophysical characterisation of a soil. It is based upon measuring the heat exchanges on the surface of the soil and on measuring a temperature a few centimetres below the surface. The system is light, inexpensive, well-suited to the taking of measurements in situ without the sensors used introducing any disturbance into the heat exchanges. Whereas the majority of methods require excitation, the one presented here is passive and exploits natural signals. Based upon a few hours of recording, the natural signals allow us to identify the soils thermophysical properties continuously. The identification is based upon frequency methods the quality of which can be seen when the thermophysical properties are injected into a model with finite elements by means of a comparison of the temperatures modelled and those actually measured on site. (author)

  9. In situ synthesis of α-MoO3/graphene composites as anode materials for lithium ion battery

    International Nuclear Information System (INIS)

    Liu, Chun-Ling; Wang, Yan; Zhang, Chen; Li, Xiao-Shan; Dong, Wen-Sheng

    2014-01-01

    The α-MoO 3 /graphene composites (MoO 3 /G) were prepared via an in situ hydrothermal synthesis. The composites were characterized using various characterization techniques including powder X-ray diffraction, transmission electron microscopy, scanning electron microscopy, X-ray photoelectron spectroscopy, and the electrochemical performance test. The results show that these MoO 3 /G composites exhibit high capacity and good cycle stability when used as the lithium-ion battery anode. Among all the samples, the MoO 3 /G-27 reveals the best electrochemical performance with an initial charge capacity of 977.7 mAh g −1 at a current density of 50 mA g −1 , the first coulombic efficiency of 69.5%. After eighty cycles the electrode still maintains a capacity of 869.2 mAh g −1 , giving high capacity retention of 88.9%. The good electrochemical performance of the composite anode is close related to its structure, in which the MoO 3 nanobelts are not only homogeneously anchored on the surface but also embedded in the interlayer of the graphene sheets; hence the volume change and aggregation of the MoO 3 nanobelts during lithium ion insertion/extraction process can be effectively hindered. On the other hand, graphene itself is an electronic conductor; the graphene and MoO 3 nanobelts connect closely, which offers large electrode/electrolyte contacting area, short path length for Li + transporting during lithium insertion and extraction. - Highlights: • The α-MoO 3 /graphene composites were prepared via an in situ hydrothermal synthesis. • The MoO 3 /G-27 anode delivers an initial reversible capacity of 977.7 mAh g −1 . • After 80 cycles it has a reversible capacity of 869.2 mAh g −1 at 50 mA g −1

  10. Synthesis and characterization of cationic lipid coated magnetic nanoparticles using multiple emulsions as microreactors

    Energy Technology Data Exchange (ETDEWEB)

    Akbaba, Hasan; Karagöz, Uğur [Ege University, Faculty of Pharmacy, Department of Pharmaceutical Biotechnology, 35100 Izmir (Turkey); Selamet, Yusuf [Izmir Institute of Technology, Faculty of Science, Department of Physics, 35433 Izmir (Turkey); Kantarcı, A. Gülten, E-mail: gulten.kantarci@ege.edu.tr [Ege University, Faculty of Pharmacy, Department of Pharmaceutical Biotechnology, 35100 Izmir (Turkey)

    2017-03-15

    The aim of this study was to develop a novel iron oxide nanoparticle synthesis method with in-situ surface coating. For this purpose multiple emulsions were used as microreactors for the first time and magnetic iron oxide particles synthesized in the core of cationic solid lipid nanoparticles. DLS, SEM, TEM, VSM, Raman Spectrometer, XRD, and XPS techniques were performed for characterization of the magnetic nanoparticles. Obtained magnetic nanoparticles are superparamagnetic and no additional process was needed for surface adjustments. They are positively charged as a result of cationic lipid coating and has appropriate particle size (<30 nm) for drug or nucleic acid delivery. Structure analysis showed that magnetic core material is in the form of magnetite. Saturation magnetization value was measured as 15–17 emu g{sup −1} for lipid coated magnetic nanoparticles obtained by multiple emulsion method which is reasonably sufficient for magnetic targeting. - Highlights: • A novel iron oxide nanoparticle synthesis method with in-situ surface coating. • Combining advantages of microemulsions and multiple emulsion methods. • Multiple emulsions were used as microreactors for magnetic nanoparticle synthesis. • Superparamagnetic iron oxide particles synthesized in the core of cationic lipids. • Possible delivery systems for nucleic acids, oil soluble compounds or drugs.

  11. Synthesis of 1 nm Pd Nanoparticles in a Microfluidic Reactor: Insights from in Situ X ray Absorption Fine Structure Spectroscopy and Small-Angle X ray Scattering

    Energy Technology Data Exchange (ETDEWEB)

    Karim, Ayman M.; Al Hasan, Naila M.; Ivanov, Sergei A.; Siefert, Soenke; Kelly, Ryan T.; Hallfors, Nicholas G.; Benavidez, Angelica D.; Kovarik, Libor; Jenkins, Aaron; Winans, R. E.; Datye, Abhaya K.

    2015-06-11

    In this paper we show that the temporal separation of nucleation and growth is not a necessary condition for the colloidal synthesis of monodisperse nanoparticles. The synthesis mechanism of Pd nanoparticles was determined by in situ XAFS and SAXS in a microfluidic reactor capable of millisecond up to an hour time resolution. The SAXS results showed two autocatalytic growth phases, a fast growth phase followed by a very slow growth phase. The steady increase in the number of particles throughout the two growth phases indicates the synthesis is limited by slow continuous nucleation. The transition from fast to slow growth was caused by rapid increase in bonding with the capping agent as shown by XAFS. Based on this fundamental understanding of the synthesis mechanism, we show that 1 nm monodisperse Pd nanoparticles can be synthesized at low temperature using a strong binding capping agent such as trioctylphosphine (TOP).

  12. In-situ spectrometry of 137Cs in the soil by unfolding method

    International Nuclear Information System (INIS)

    Fueloep, M.; Ragan, P.; Krnac, S.

    1995-01-01

    This contribution is aimed to the possibility of improving the in-situ gamma spectrometry to be independent on a knowledge about a depth distribution of 137 Cs in soil and sufficiently sensitive for the measurement of the post-Chernobyl 137 Cs at present, as well. The depth distribution of 137 Cs averaged over a large area of soil is obtained by unfolding of the detector responses to primary and in soil forward scattered photons. The proposed method employs detector with and without collimator. The 137 Cs distributions obtained in-situ measurements are analysed, and comparisons are made to the results obtained with soil sampling and with standard in-situ spectrometry, as well. 5 figs., 1 tab., 4 refs

  13. In situ synthesis of CdS/CdWO4/WO3 heterojunction films with enhanced photoelectrochemical properties

    Science.gov (United States)

    Zhan, Faqi; Li, Jie; Li, Wenzhang; Yang, Yahui; Liu, Wenhua; Li, Yaomin

    2016-09-01

    CdS/CdWO4/WO3 heterojunction films on fluorine-doped tin oxide (FTO) substrates are for the first time prepared as an efficient photoanode for photoelectrochemical (PEC) hydrogen generation by an in situ conversion process. The samples are characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM), ultraviolet visible spectrometry (UV-vis) and X-ray photoelectron spectroscopy (XPS). The CdS hollow spheres (∼80 nm) sensitized WO3 plate film with a CdWO4 buffer-layer exhibits increased visible light absorption and a significantly improved photoelectrochemical performance. The photocurrent density at 0 V (vs. Ag/AgCl) of the CdS/CdWO4/WO3 anode is ∼3 times higher than that of the CdWO4/WO3 anode, and ∼9 times higher than that of pure WO3 under illumination. The highest incident-photon-to-current-efficiency (IPCE) value increased from 16% to 63% when the ternary heterojunction was formed. This study demonstrates that the synthesis of ternary composite photocatalysts by the in situ conversion process may be a promising approach to achieve high photoelectric conversion efficiency.

  14. In situ synthesis carbonated hydroxyapatite layers on enamel slices with acidic amino acids by a novel two-step method

    International Nuclear Information System (INIS)

    Wu, Xiaoguang; Zhao, Xu; Li, Yi; Yang, Tao; Yan, Xiujuan; Wang, Ke

    2015-01-01

    In situ fabrication of carbonated hydroxyapatite (CHA) remineralization layer on an enamel slice was completed in a novel, biomimetic two-step method. First, a CaCO 3 layer was synthesized on the surface of demineralized enamel using an acidic amino acid (aspartic acid or glutamate acid) as a soft template. Second, at the same concentration of the acidic amino acid, rod-like carbonated hydroxyapatite was produced with the CaCO 3 layer as a sacrificial template and a reactant. The morphology, crystallinity and other physicochemical properties of the crystals were characterized using field emission scanning electron microscopy (FESEM), Fourier transform infrared spectrometry (FTIR), X-ray diffraction (XRD) and energy-dispersive X-ray analysis (EDAX), respectively. Acidic amino acid could promote the uniform deposition of hydroxyapatite with rod-like crystals via absorption of phosphate and carbonate ions from the reaction solution. Moreover, compared with hydroxyapatite crystals coated on the enamel when synthesized by a one-step method, the CaCO 3 coating that was synthesized in the first step acted as an active bridge layer and sacrificial template. It played a vital role in orienting the artificial coating layer through the template effect. The results show that the rod-like carbonated hydroxyapatite crystals grow into bundles, which are similar in size and appearance to prisms in human enamel, when using the two-step method with either aspartic acid or acidic glutamate (20.00 mmol/L). - Graphical abstract: FESEM images of enamel slices etched for 60 s and repaired by the two-step method with Glu concentration of 20.00 mmol/L. (A) The boundary (dotted line) of the repaired areas (b) and unrepaired areas (a). (Some selected areas of etched enamel slices were coated with a nail polish before the reaction, which was removed by acetone after the reaction); (B) high magnification image of Ga, (C) high magnification image of Gb. In situ fabrication of carbonated

  15. In situ synthesis carbonated hydroxyapatite layers on enamel slices with acidic amino acids by a novel two-step method

    Energy Technology Data Exchange (ETDEWEB)

    Wu, Xiaoguang [Department of Pediatric Dentistry, The Hospital of Stomatology, Jilin University, Changchun 130021 (China); Zhao, Xu [College of Chemistry, Jilin University, Changchun 130021 (China); Li, Yi, E-mail: lyi99@jlu.edu.cn [Department of Pediatric Dentistry, The Hospital of Stomatology, Jilin University, Changchun 130021 (China); Yang, Tao [Department of Stomatology, Children' s Hospital of Changchun, 130051 (China); Yan, Xiujuan; Wang, Ke [Department of Pediatric Dentistry, The Hospital of Stomatology, Jilin University, Changchun 130021 (China)

    2015-09-01

    In situ fabrication of carbonated hydroxyapatite (CHA) remineralization layer on an enamel slice was completed in a novel, biomimetic two-step method. First, a CaCO{sub 3} layer was synthesized on the surface of demineralized enamel using an acidic amino acid (aspartic acid or glutamate acid) as a soft template. Second, at the same concentration of the acidic amino acid, rod-like carbonated hydroxyapatite was produced with the CaCO{sub 3} layer as a sacrificial template and a reactant. The morphology, crystallinity and other physicochemical properties of the crystals were characterized using field emission scanning electron microscopy (FESEM), Fourier transform infrared spectrometry (FTIR), X-ray diffraction (XRD) and energy-dispersive X-ray analysis (EDAX), respectively. Acidic amino acid could promote the uniform deposition of hydroxyapatite with rod-like crystals via absorption of phosphate and carbonate ions from the reaction solution. Moreover, compared with hydroxyapatite crystals coated on the enamel when synthesized by a one-step method, the CaCO{sub 3} coating that was synthesized in the first step acted as an active bridge layer and sacrificial template. It played a vital role in orienting the artificial coating layer through the template effect. The results show that the rod-like carbonated hydroxyapatite crystals grow into bundles, which are similar in size and appearance to prisms in human enamel, when using the two-step method with either aspartic acid or acidic glutamate (20.00 mmol/L). - Graphical abstract: FESEM images of enamel slices etched for 60 s and repaired by the two-step method with Glu concentration of 20.00 mmol/L. (A) The boundary (dotted line) of the repaired areas (b) and unrepaired areas (a). (Some selected areas of etched enamel slices were coated with a nail polish before the reaction, which was removed by acetone after the reaction); (B) high magnification image of Ga, (C) high magnification image of Gb. In situ fabrication of

  16. Polypropylene/graphite nanocomposites by in situ polymerization

    International Nuclear Information System (INIS)

    Milani, Marceo A.; Galland, Giselda B.; Quijada, Raul

    2011-01-01

    This work presents the synthesis of nanocomposites of polypropylene/graphite by in situ polymerization using metallocene catalyst and graphene nanosheets. Initially was analyzed which of the metallocene catalysts rac-Et(Ind) 2 ZrCl 2 or rac-Me 2 Si(Ind) 2 ZrCl 2 produces polypropylene with mechanical properties more relevant. Then it were performed the in situ polymerization reactions to obtain the nanocomposites. The polymeric materials were characterized by XRD, DSC, GPC and DMTA. (author)

  17. Synthesis and characterization of polypropylene/graphite nano composite preparation for in situ polymerization; Sintese e caracterizacao de nanocompositos polipropileno/grafite obtidos pela polimerizacao in situ

    Energy Technology Data Exchange (ETDEWEB)

    Montagna, L.S.; Fim, F. de C.; Galland, G.B. [Universidade Federal do Rio Grande do Sul (UFRGS), Porto Alegre, RS (Brazil). Inst. de Quimica; Basso, N.R.S., E-mail: nrbass@pucrs.b [Pontificia Universidade Catolica do Rio Grande do Sul (PUC-RS), Porto Alegre, RS (Brazil)

    2010-07-01

    This paper presents the synthesis of polypropylene/graphite nanocomposites through in situ polymerization, using the metallocene catalyst C{sub 20}H{sub 16}Cl{sub 2}Zr (dichloro(rac-ethylenebis(indenyl))zircon(IV)). The graphite nanosheets in nano dimensions were added to the polymer matrix in percentages of 0.6;1.0;4.2;4.8 and 6.0% (w/w). The TEM images indicated that the thickness of graphite nanosheets ranged from 4 to 60 nm and by means of XRD analysis it was observed that the physical and chemical treatment did not destroyed the graphite layers. The presence of nanosheets did not decrease the catalytic activity of the nanocomposites. TEM images and XRD analysis of nanocomposites showed a good dispersion of the graphite nanosheets in the polypropylene matrix. (author)

  18. ADVANTAGES/DISADVANTAGES FOR ISCO METHODS IN-SITU FENTON OXIDATION IN-SITU PERMANGANATE OXIDATION

    Science.gov (United States)

    The advantages and disadvantages of in-situ Fenton oxidation and in-situ permanganate oxidation will be presented. This presentation will provide a brief overview of each technology and a detailed analysis of the advantages and disadvantages of each technology. Included in the ...

  19. Synthesis of highly dispersed platinum particles on carbon nanotubes by an in situ vapor-phase method

    International Nuclear Information System (INIS)

    Mercado-Zúñiga, C.; Vargas-García, J.R.; Hernández-Pérez, M.A.; Figueroa-Torres, M.Z.; Cervantes-Sodi, F.; Torres-Martínez, L.M.

    2014-01-01

    Highlights: • Highly dispersed Pt nanoparticles were prepared on functionalized carbon nanotubes. • A simple and competitive vapor-phase method was employed. • Carbonyl groups were assumed to be responsible for assisted decomposition of Pt-acac. • Pt particles were highly dispersed because carbonyl groups served as reaction sites. • Particles of 2.3 nm in size were highly dispersed even the high loading (27 wt%Pt). - Abstract: Highly dispersed Pt nanoparticles were prepared on functionalized multi-walled carbon nanotubes (f-MWCNTs) using a simple in situ vapor-phase method. The method consisted in two-step procedure in which an initial mixture of Pt precursor (Pt-acac) and f-MWCNTs was heated in a quartz tube reactor, first at 180 °C and then at 400 °C. Fourier transform infrared spectroscopy (FTIR–ATR), thermal gravimetric analysis (TGA) and X-ray diffraction (XRD) were used to follow the chemical and structural transformations of mixture components during heating steps. The functionalization of MWCNTs with HNO 3 /H 2 SO 4 solution resulted in formation of surface carbonyl groups. The FTIR–ATR and XRD results indicated that individual Pt-acac withstood heating at 180 °C, whereas it was dissociated when heated in contact with f-MWCNTs at the same temperature. Thus, the functional carbonyl groups were found to be responsible for assisted decomposition of Pt-acac at 180 °C. Since carbonyl groups served as reaction sites for decomposition of Pt-acac, the resulting particles were highly and homogeneously dispersed on the surface of MWCNTs even the relatively high metallic loading of 27 wt%. TEM observations revealed that crystalline Pt particles exhibit narrow size distribution with a mean size of 2.3 nm

  20. Synthesis of highly dispersed platinum particles on carbon nanotubes by an in situ vapor-phase method

    Energy Technology Data Exchange (ETDEWEB)

    Mercado-Zúñiga, C. [Depto. Ing. Metalurgia y Materiales, Instituto Politecnico Nacional, Mexico 07300 D.F. (Mexico); Vargas-García, J.R., E-mail: rvargasga@ipn.mx [Depto. Ing. Metalurgia y Materiales, Instituto Politecnico Nacional, Mexico 07300 D.F. (Mexico); Hernández-Pérez, M.A. [Depto. Ing. Metalurgia y Materiales, Instituto Politecnico Nacional, Mexico 07300 D.F. (Mexico); Figueroa-Torres, M.Z. [Depto. Eco-Materiales y Energia, Univ. Autonoma de Nuevo Leon, Nuevo Leon 66450 (Mexico); Cervantes-Sodi, F. [Depto. Fisica y Matematicas, Univ. Iberoamericana, Mexico 01209 D.F. (Mexico); Torres-Martínez, L.M. [Depto. Eco-Materiales y Energia, Univ. Autonoma de Nuevo Leon, Nuevo Leon 66450 (Mexico)

    2014-12-05

    Highlights: • Highly dispersed Pt nanoparticles were prepared on functionalized carbon nanotubes. • A simple and competitive vapor-phase method was employed. • Carbonyl groups were assumed to be responsible for assisted decomposition of Pt-acac. • Pt particles were highly dispersed because carbonyl groups served as reaction sites. • Particles of 2.3 nm in size were highly dispersed even the high loading (27 wt%Pt). - Abstract: Highly dispersed Pt nanoparticles were prepared on functionalized multi-walled carbon nanotubes (f-MWCNTs) using a simple in situ vapor-phase method. The method consisted in two-step procedure in which an initial mixture of Pt precursor (Pt-acac) and f-MWCNTs was heated in a quartz tube reactor, first at 180 °C and then at 400 °C. Fourier transform infrared spectroscopy (FTIR–ATR), thermal gravimetric analysis (TGA) and X-ray diffraction (XRD) were used to follow the chemical and structural transformations of mixture components during heating steps. The functionalization of MWCNTs with HNO{sub 3}/H{sub 2}SO{sub 4} solution resulted in formation of surface carbonyl groups. The FTIR–ATR and XRD results indicated that individual Pt-acac withstood heating at 180 °C, whereas it was dissociated when heated in contact with f-MWCNTs at the same temperature. Thus, the functional carbonyl groups were found to be responsible for assisted decomposition of Pt-acac at 180 °C. Since carbonyl groups served as reaction sites for decomposition of Pt-acac, the resulting particles were highly and homogeneously dispersed on the surface of MWCNTs even the relatively high metallic loading of 27 wt%. TEM observations revealed that crystalline Pt particles exhibit narrow size distribution with a mean size of 2.3 nm.

  1. Modified Synthesis of Erlotinib Hydrochloride

    Directory of Open Access Journals (Sweden)

    Leila Barghi

    2012-06-01

    Full Text Available Purpose: An improved and economical method has been described for the synthesis of erlotinib hydrochloride, as a useful drug in treatment of non-small-cell lung cancer. Methods: Erlotinib hydrochloride was synthesized in seven steps starting from 3, 4-dihydroxy benzoic acid. In this study, we were able to modify one of the key steps which involved the reduction of the 6-nitrobenzoic acid derivative to 6-aminobenzoic acid derivative. An inexpensive reagent such as ammonium formate was used as an in situ hydrogen donor in the presence of palladium/charcoal (Pd/C instead of hydrogen gas at high pressure. Results: This proposed method proceeded with 92% yield at room temperature. Synthesis of erlotinib was completed in 7 steps with overall yield of 44%.Conclusion: From the results obtained it can be concluded that the modified method eliminated the potential danger associated with the use of hydrogen gas in the presence of flammable catalysts. It should be mentioned that the catalyst was recovered after the reaction and could be used again.

  2. In Situ Studies and Magnetic Properties of the Cmcm Polymorph of LiCoPO4 with a Hierarchical Dumbbell-Like Morphology Synthesized by Easy Single-Step Polyol Synthesis

    Directory of Open Access Journals (Sweden)

    Carlos Alarcón-Suesca

    2016-11-01

    Full Text Available LiCoPO4 (LCP exists in three different structural modifications: LCP-Pnma (olivine structure, LCP-Pn21a (KNiPO4 structure type, and LCP-Cmcm (Na2CrO4 structure type. The synthesis of the LCP-Cmcm polymorph has been reported via high pressure/temperature solid-state methods and by microwave-assisted solvothermal synthesis. Phase transitions from both LCP-Pn21a and LCP-Cmcm to LCP-Pnma upon heating indicates a metastable behavior. However, a precise study of the structural changes during the heating process and the magnetic properties of LCP-Cmcm are hitherto unknown. Herein, we present the synthesis and characterization of LCP-Cmcm via a rapid and facile soft-chemistry approach using two different kinetically controlled pathways, solvothermal and polyol syntheses, both of which only require relatively low temperatures (~200 °C. Additionally, by polyol, method a dumbbell-like morphology is obtained without the use of any additional surfactant or template. A temperature-dependent in situ powder XRD shows a transition from LCP-Cmcm at room temperature to LCP-Pnma and finally to LCP-Pn21a at 575 and 725 °C, respectively. In addition to that, the determination of the magnetic susceptibility as a function of temperature indicates a long-range antiferromagnetic order below TN = 11 K at 10 kOe and 9.1 K at 25 kOe. The magnetization curves suggests the presence of a metamagnetic transition.

  3. High Ionic Conductivity of Composite Solid Polymer Electrolyte via In Situ Synthesis of Monodispersed SiO2 Nanospheres in Poly(ethylene oxide).

    Science.gov (United States)

    Lin, Dingchang; Liu, Wei; Liu, Yayuan; Lee, Hye Ryoung; Hsu, Po-Chun; Liu, Kai; Cui, Yi

    2016-01-13

    High ionic conductivity solid polymer electrolyte (SPE) has long been desired for the next generation high energy and safe rechargeable lithium batteries. Among all of the SPEs, composite polymer electrolyte (CPE) with ceramic fillers has garnered great interest due to the enhancement of ionic conductivity. However, the high degree of polymer crystallinity, agglomeration of ceramic fillers, and weak polymer-ceramic interaction limit the further improvement of ionic conductivity. Different from the existing methods of blending preformed ceramic particles with polymers, here we introduce an in situ synthesis of ceramic filler particles in polymer electrolyte. Much stronger chemical/mechanical interactions between monodispersed 12 nm diameter SiO2 nanospheres and poly(ethylene oxide) (PEO) chains were produced by in situ hydrolysis, which significantly suppresses the crystallization of PEO and thus facilitates polymer segmental motion for ionic conduction. In addition, an improved degree of LiClO4 dissociation can also be achieved. All of these lead to good ionic conductivity (1.2 × 10(-3) S cm(-1) at 60 °C, 4.4 × 10(-5) S cm(-1) at 30 °C). At the same time, largely extended electrochemical stability window up to 5.5 V can be observed. We further demonstrated all-solid-state lithium batteries showing excellent rate capability as well as good cycling performance.

  4. Methods and systems for in-situ electroplating of electrodes

    Science.gov (United States)

    Zappi, Guillermo Daniel; Zarnoch, Kenneth Paul; Huntley, Christian Andrew; Swalla, Dana Ray

    2015-06-02

    The present techniques provide electrochemical devices having enhanced electrodes with surfaces that facilitate operation, such as by formation of a porous nickel layer on an operative surface, particularly of the cathode. The porous metal layer increases the surface area of the electrode, which may result in increasing the efficiency of the electrochemical devices. The formation of the porous metal layer is performed in situ, that is, after the assembly of the electrodes into an electrochemical device. The in situ process offers a number of advantages, including the ability to protect the porous metal layer on the electrode surface from damage during assembly of the electrochemical device. The enhanced electrode and the method for its processing may be used in any number of electrochemical devices, and is particularly well suited for electrodes in an electrolyzer useful for splitting water into hydrogen and oxygen.

  5. Signal processing methods for in-situ creep specimen monitoring

    Science.gov (United States)

    Guers, Manton J.; Tittmann, Bernhard R.

    2018-04-01

    Previous work investigated using guided waves for monitoring creep deformation during accelerated life testing. The basic objective was to relate observed changes in the time-of-flight to changes in the environmental temperature and specimen gage length. The work presented in this paper investigated several signal processing strategies for possible application in the in-situ monitoring system. Signal processing methods for both group velocity (wave-packet envelope) and phase velocity (peak tracking) time-of-flight were considered. Although the Analytic Envelope found via the Hilbert transform is commonly applied for group velocity measurements, erratic behavior in the indicated time-of-flight was observed when this technique was applied to the in-situ data. The peak tracking strategies tested had generally linear trends, and tracking local minima in the raw waveform ultimately showed the most consistent results.

  6. Facile synthesis of antimony-doped tin oxide nanoparticles by a polymer-pyrolysis method

    International Nuclear Information System (INIS)

    Li, Yuan-Qing; Wang, Jian-Lei; Fu, Shao-Yun; Mei, Shi-Gang; Zhang, Jian-Min; Yong, Kang

    2010-01-01

    In this article, antimony-doped tin oxide (ATO) nanoparticles was synthesized by a facile polymer-pyrolysis method. The pyrolysis behaviors of the polymer precursors prepared via in situ polymerization of metal salts and acrylic acid were analyzed by simultaneous thermogravimetric and differential scanning calorimetry (TG-DSC). The structural and morphological characteristics of the products were studied by powder X-ray diffraction (XRD) and transmission electron microscope (TEM). The results reveal that the ATO nanoparticles calcined at 600 o C show good crystallinity with the cassiterite structure and cubic-spherical like morphology. The average particle size of ATO decreases from 200 to 15 nm as the Sb doping content increases from 5 mol% to 15 mol%. Electrical resistivity measurement shows that the resistivity for the 10-13 mol% Sb-doped SnO 2 nanoparticles is reduced by more than three orders compared with the pure SnO 2 nanoparticles. In addition, due to its versatility this polymer-pyrolysis method can be extended to facile synthesis of other doped n-type semiconductor, such as In, Ga, Al doped ZnO, Sn doped In 2 O 3 .

  7. Synthesis and application of in-situ molecularly imprinted silica monolithic in pipette-tip solid-phase microextraction for the separation and determination of gallic acid in orange juice samples.

    Science.gov (United States)

    Arabi, Maryam; Ghaedi, Mehrorang; Ostovan, Abbas

    2017-03-24

    A novel strategy was presented for the synthesis and application of functionalized silica monolithic as artificial receptor of gallic acid at micro-pipette tip. A sol-gel process was used to prepare the sorbent. In this in-situ polymerization reaction, tetraethyl orthosilicate (TEOS), 3-aminopropyl trimethoxysilane (APTMS), gallic acid and thiourea were used, respectively, as cross-linker, functionalized monomer, template and precursor to make crack-free and non-fragile structure. Such durable and inexpensive in-situ monolithic was successfully employed as useful tool for highly efficient extraction of gallic acid from orange juice samples. The effective parameters in extraction recovery were investigated and optimum conditions were obtained using experimental design methodology. Applying HPLC-UV for separation quantification at optimal conditions, the gallic acid was efficiently extracted without significant matrix interference. Good linearity for gallic acid in the range of 0.02-5.0mgL -1 with correlation coefficients of R 2 >0.999 revealed well applicability of the method for trace analysis. Copyright © 2017. Published by Elsevier B.V.

  8. Characterization of Silver Nanoparticle In Situ Synthesis on Porous Sericin Gel for Antibacterial Application

    Directory of Open Access Journals (Sweden)

    Gang Tao

    2016-01-01

    Full Text Available Sericin from Bombyx mori cocoon has good hydrophilicity, reaction activity, biocompatibility, and biodegradability, which has shown great potentials for biomedical materials. Here, an ultraviolet light-assisted in situ synthesis approach is developed to immobilize silver nanoparticles on the surface of sericin gel. The amount of silver nanoparticles immobilized on the surface of sericin gel could be regulated by the irradiation time. The porous structure and property of sericin gel were not affected by the modification of AgNPs, as evidenced by the observation of scanning electron microscopy, X-ray diffractometry, and Fourier transform infrared spectroscopy. Differential scanning calorimetry analysis showed that the modification of AgNPs increased the thermal stability of sericin gel. The growth curve of bacteria and inhibition zone assays suggested that the sericin gel modified with AgNPs had good antimicrobial activities against both Gram-negative and Gram-positive bacteria. This novel sericin has shown a great potential for biomedical purpose.

  9. Hydroxyapatite Fibers: A Review of Synthesis Methods

    Science.gov (United States)

    Qi, Mei-Li; He, Kun; Huang, Zhen-Nan; Shahbazian-Yassar, Reza; Xiao, Gui-Yong; Lu, Yu-Peng; Shokuhfar, Tolou

    2017-08-01

    Hydroxyapatite (HA) exhibits excellent biocompatibility, bioactivity, osteoconductivity, non-toxicity and so on, making it a perfect candidate for biomedical applications. However, HA is not qualified to be used in load-bearing sites due to its poor flexural strength and fracture toughness. Design, synthesis and application of fibrous HA is a promising strategy to overcome the inherent brittleness. This review provides a brief description of HA and hydroxyapatite fiber (HAF), then introduces different synthesis methods of HAF and highlights the inherent merits and drawbacks involved in each method. Finally, the future perspectives in this active research area are given. The purpose of this review is to acquaint the reader with this promising new field of biomaterials research and with emphasis on recent techniques to obtain continuous, uniform and long HAF.

  10. Photonic arbitrary waveform generator based on Taylor synthesis method

    DEFF Research Database (Denmark)

    Liao, Shasha; Ding, Yunhong; Dong, Jianji

    2016-01-01

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

  11. Facile In Situ Fabrication of Nanostructured Graphene–CuO Hybrid with Hydrogen Sulfide Removal Capacity

    Institute of Scientific and Technical Information of China (English)

    Sunil P.Lonkar; Vishnu V.Pillai; Samuel Stephen; Ahmed Abdala; Vikas Mittal

    2016-01-01

    A simple and scalable synthetic approach for one-step synthesis of graphene–Cu O(TRGC) nanocomposite by an in situ thermo-annealing method has been developed.Using graphene oxide(GO) and copper hydroxide as a precursors reagent,the reduction of GO and the uniform deposition of in situ formed Cu O nanoparticles on graphene was simultaneously achieved.The method employed no solvents,toxic-reducing agents,or organic modifiers.The resulting nanostructured hybrid exhibited improved H2 S sorption capacity of 1.5 mmol H2S/g-sorbent(3 g S/100 g-sorbent).Due to its highly dispersed sub-20 nm Cu O nanoparticles and large specific surface area,TRGC nanocomposite exhibits tremendous potential for energy and environment applications.

  12. In situ synthesis of CdS decorated titanate nanosheets with highly efficient visible-light-induced photoactivity

    International Nuclear Information System (INIS)

    Liu, Zhi; Fang, Pengfei; Liu, Fuwei; Zhang, Yupeng; Liu, Xinzhao; Lu, Dingze; Li, Delong; Wang, Shaojie

    2014-01-01

    Appropriately dispersed CdS nanoparticles were intimately embedded into titanate nanosheets (TNS) through ion-exchange and in situ sulfurization process. The sheet-like intermediates of titanate during the transforming process into nanotubes were firstly used as substrate for the decoration of CdS nanoparticles, and the synthesis route was achieved by ion-exchange process between titanate precursor and Cd 2+ ions solution, and the following sulfuration process by using Na 2 S solutions. The catalytic activity of the photocatalyst was investigated by photodegradation of Rhodamine B under visible light irradiation. With an optimal Cd/Ti molar ratio of 15%, the CdS/TNS composite exhibits the highest photocatalytic performance, which is approximately 5.4 times greater than that of pure TNS. The mechanism of the separation behavior of the photogenerated charges was also discussed.

  13. Synthesis of hydroxyapatite nanoparticles by Sonochemistry Method

    International Nuclear Information System (INIS)

    Cota, L.F.; Pereira, L.C.; Licona, K.P.M.; Lunz, J.N.; Ribeiro, A.A.; Morejon, L.

    2014-01-01

    bone implant substitute due to a great chemical similarity with the biological calcified tissues. Among synthesis conventional methods, the acoustic cavitation, induced by the sonochemical method, allows formation of nano powders. This work aimed to synthesize HAp nano-sized powders by using CaCl2. 2H2O and Na3PO4. 12H2O as precursors, along with pH and temperature control. The sonochemical method was accomplished by using different amplitudes (20%, 60% e 100%). To optimize the process, another synthesis at 60% ultrasound amplitude was performed, with the use of a peristaltic pump for dripping control. The HAp nano powders achieved were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), BET analysis, Scanning Electron Microscope/Field Emission Gun (SEM/FEG) combined with EDS. The results indicated the influence of the sonochemical methodology and drip controlling, on the chemical composition, crystallinity and nanoparticles morphology. (author)

  14. Synthesis of hydroxyapatite nanoparticles by Sonochemistry Method

    Energy Technology Data Exchange (ETDEWEB)

    Cota, L.F.; Pereira, L.C. [Coordenacao dos Programas de Pos-Graduacao em Engenharia (COPPE/UFRJ), Rio de Janeiro, RJ (Brazil); Licona, K.P.M.; Lunz, J.N.; Ribeiro, A.A. [Instituto Nacional de Tecnologia (DPCM/INT), Rio de Janeiro, RJ (Brazil); Morejon, L. [Universidad de La Habana (UH/BIOMAT), Habana (Cuba). Centro de Biomateriales

    2014-07-01

    bone implant substitute due to a great chemical similarity with the biological calcified tissues. Among synthesis conventional methods, the acoustic cavitation, induced by the sonochemical method, allows formation of nano powders. This work aimed to synthesize HAp nano-sized powders by using CaCl2. 2H2O and Na3PO4. 12H2O as precursors, along with pH and temperature control. The sonochemical method was accomplished by using different amplitudes (20%, 60% e 100%). To optimize the process, another synthesis at 60% ultrasound amplitude was performed, with the use of a peristaltic pump for dripping control. The HAp nano powders achieved were characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), BET analysis, Scanning Electron Microscope/Field Emission Gun (SEM/FEG) combined with EDS. The results indicated the influence of the sonochemical methodology and drip controlling, on the chemical composition, crystallinity and nanoparticles morphology. (author)

  15. In situ synthesis of bilayered gradient poly(vinyl alcohol)/hydroxyapatite composite hydrogel by directional freezing-thawing and electrophoresis method.

    Science.gov (United States)

    Su, Cui; Su, Yunlan; Li, Zhiyong; Haq, Muhammad Abdul; Zhou, Yong; Wang, Dujin

    2017-08-01

    Bilayered poly(vinyl alcohol) (PVA)/hydroxyapatite (HA) composite hydrogels with anisotropic and gradient mechanical properties were prepared by the combination of directional freezing-thawing (DFT) and electrophoresis method. Firstly, PVA hydrogels with aligned channel structure were prepared by the DFT method. Then, HA nanoparticles were in situ synthesized within the PVA hydrogels via electrophoresis. By controlling the time of the electrophoresis process, a bilayered gradient hydrogel containing HA particles in only half of the gel region was obtained. The PVA/HA composite hydrogel exhibited gradient mechanical strength depending on the distance to the cathode. The gradient initial tensile modulus ranging from 0.18MPa to 0.27MPa and the gradient initial compressive modulus from 0.33MPa to 0.51MPa were achieved. The binding strength of the two regions was relatively high and no apparent internal stress or defect was observed at the boundary. The two regions of the bilayered hydrogel also showed different osteoblast cell adhesion properties. Copyright © 2017 Elsevier B.V. All rights reserved.

  16. Nuclear methods for 'in-situ' geophysical investigations. 2

    International Nuclear Information System (INIS)

    Russell, J.P.; Oliver, D.W.

    1985-01-01

    There has been considerable effort expended by governmental, institutional, and private agencies in the development of suitable materials and instruments for application of nuclear methods for exploration and evaluation of mineral, oil, and gas resources. As a consequence of the peculiar circumstances of in situ investigations, much of the apparatus is, of design and construction, specifically adapted to the environment of the borehole (limited lateral dimension, high temperature and pressure, deep boreholes, etc.) which differs considerably from laboratory conditions. Meeting the needs for reliability and stability under adverse conditions of operation has led to often unique and innovative instrumentation. Much of the development effort has been provided by commercial service organizations whose interests require many details be maintained as proprietary. In addition, the tailoring of services to meet varying environmental and informational constraints has led to a wide range of instrument designs. As a result, it is difficult to provide an exhaustive description of all apparatus available for in situ investigations, rather, in this instance, systems and subsystems will be generically discussed. Radiation sources, detectors, and borehole probe designs are covered. (Auth.)

  17. Intermatrix Synthesis as a rapid, inexpensive and reproducible methodology for the in situ functionalization of nanostructured surfaces with quantum dots

    Science.gov (United States)

    Bastos-Arrieta, Julio; Muñoz, Jose; Stenbock-Fermor, Anja; Muñoz, Maria; Muraviev, Dmitri N.; Céspedes, Francisco; Tsarkova, Larisa A.; Baeza, Mireia

    2016-04-01

    Intermatrix Synthesis (IMS) technique has proven to be a valid methodology for the in situ incorporation of quantum dots (QDs) in a wide range of nanostructured surfaces for the preparation of advanced hybrid-nanomaterials. In this sense, this communication reports the recent advances in the application of IMS for the synthesis of CdS-QDs with favourable distribution on sulfonated polyetherether ketone (SPEEK) membrane thin films (TFs), multiwall carbon nanotubes (MWCNTs) and nanodiamonds (NDs). The synthetic route takes advantage of the ion exchange functionality of the reactive surfaces for the loading of the QDs precursor and consequent QDs appearance by precipitation. The benefits of such modified nanomaterials were studied using CdS-QDs@MWCNTs hybrid-nanomaterials. CdS-QDs@MWCNTs has been used as conducting filler for the preparation of electrochemical nanocomposite sensors, which present electrocatalytic properties. Finally, the optical properties of the QDs contained on MWCNTs could allow a new procedure for the analytical detection of nanostructured carbon allotropes in water.

  18. One-step synthesis and characterization of CoS-Nanoparticles decorated multi-walled carbon nanotubes

    CSIR Research Space (South Africa)

    Kesavan Pillai, Sreejarani

    2009-02-01

    Full Text Available of applications. It is vital to develop efficient methods to attach quantum dots onto the sidewalls of CNTs whose structures have been preserved intact. In this study, a simple and facile one-step synthesis approach for the in situ mineralisation of Co...

  19. Methods for the thematic synthesis of qualitative research in systematic reviews

    Directory of Open Access Journals (Sweden)

    Harden Angela

    2008-07-01

    Full Text Available Abstract Background There is a growing recognition of the value of synthesising qualitative research in the evidence base in order to facilitate effective and appropriate health care. In response to this, methods for undertaking these syntheses are currently being developed. Thematic analysis is a method that is often used to analyse data in primary qualitative research. This paper reports on the use of this type of analysis in systematic reviews to bring together and integrate the findings of multiple qualitative studies. Methods We describe thematic synthesis, outline several steps for its conduct and illustrate the process and outcome of this approach using a completed review of health promotion research. Thematic synthesis has three stages: the coding of text 'line-by-line'; the development of 'descriptive themes'; and the generation of 'analytical themes'. While the development of descriptive themes remains 'close' to the primary studies, the analytical themes represent a stage of interpretation whereby the reviewers 'go beyond' the primary studies and generate new interpretive constructs, explanations or hypotheses. The use of computer software can facilitate this method of synthesis; detailed guidance is given on how this can be achieved. Results We used thematic synthesis to combine the studies of children's views and identified key themes to explore in the intervention studies. Most interventions were based in school and often combined learning about health benefits with 'hands-on' experience. The studies of children's views suggested that fruit and vegetables should be treated in different ways, and that messages should not focus on health warnings. Interventions that were in line with these suggestions tended to be more effective. Thematic synthesis enabled us to stay 'close' to the results of the primary studies, synthesising them in a transparent way, and facilitating the explicit production of new concepts and hypotheses

  20. A light-assisted in situ embedment of silver nanoparticles to prepare functionalized fabrics

    Directory of Open Access Journals (Sweden)

    Toh HS

    2017-11-01

    Full Text Available Her Shuang Toh,1 Roxanne Line Faure,2 Liyana Bte Mohd Amin,1 Crystal Yu Fang Hay,1 Saji George1,3 1Centre of Sustainable Nanotechnology, School of Chemical and Life Sciences, Nanyang Polytechnic, Singapore, Singapore; 2DUT Analyses Biologiques et Biochimiques, IUT Génie Biologique, Dijon, France; 3Department of Food Science and Agricultural Chemistry, Macdonald Campus, McGill University, Sainte-Anne-de-Bellevue, QC, Canada Abstract: This article presents a simple, one-step, in situ generation of silver nanoparticle-functionalized fabrics with antibacterial properties, circumventing the conventional, multistep, time-consuming methods. Silver nanoparticle formation was studied with a library of capping agents (branched polyethylenimine [BPEI] of molecular weight [Mw] 10,000 and 25,000, polyvinylpyrrolidone, polyethylene glycol, polyvinylalcohol and citrate mixed with silver nitrate. The mixture was then exposed to an assortment of light wavelengths (ultraviolet, infrared and simulated solar light for studying the light-assisted synthesis of nanoparticles. The formation of nanoparticles corresponded with the reducing capabilities of the polymers wherein BPEI gave the best response. Notably, the irradiation wavelengths had little effect on the formation of the nanoparticle when the total irradiation energy was kept constant. The feasibility of utilizing this method for in situ nanoparticle synthesis on textile fabrics (towel [100% cotton], gauze [100% cotton], rayon, felt [100% polyester] and microfiber [15% nylon, 85% polyester] was verified by exposing the fabrics soaked in an aqueous solution of 1% (w/v AgNO3 and 1% (w/v BPEI (Mw 25,000 to light. The formation of nanoparticles on fabrics and their retention after washing was verified using scanning electron microscopy and quantified by inductively coupled plasma optical emission spectrometry. The functional property of the fabric as an antibacterial surface was successfully demonstrated using

  1. In Situ Synthesis of Al-Si-Cu Alloy During Brazing Process and Mechanical Property of Brazing Joint

    Directory of Open Access Journals (Sweden)

    LONG Wei-min

    2016-06-01

    Full Text Available The Al-Si-Cu alloy system is considered to be a promising choice of filler metal for aluminium alloys brazing due to its high strength and low melting point. The greatest obstacle is its lack of plastic forming ability and being difficult to be processed by conventional methods. This disadvantage is ascribed to the considerable amount of brittle CuAl2 intermetallic compound which forms when alloy composition is around the ternary eutectic point. In order to overcome this deficiency, authors of this article proposed to synthesize Al-Si-Cu filler metal by using in situ synthesis method, and the structure and properties of brazing joints were studied. The results show that AlSi alloy is used as the wrap layer, and CuAl alloy is used as the powder core in the composite brazing wire, the two alloys have similar melting points. The machinability of the composite brazing wire is much superior to the traditional Al-Si-Cu filler metal. During the induction brazing of 3A21 alloy, when using AlSi-CuAl composite filler wire, AlSi and CuAl alloys melt almost simultaneously, then after short time holding, Al-Si-Cu braze filler is obtained, the brazing seam has uniform composition and good bonding interface, also, the shearing strength of the brazing joints is higher than the joint brazed by conventional Al-Si-Cu filler metal.

  2. Maximum super angle optimization method for array antenna pattern synthesis

    DEFF Research Database (Denmark)

    Wu, Ji; Roederer, A. G

    1991-01-01

    Different optimization criteria related to antenna pattern synthesis are discussed. Based on the maximum criteria and vector space representation, a simple and efficient optimization method is presented for array and array fed reflector power pattern synthesis. A sector pattern synthesized by a 2...

  3. Formation factor logging in-situ by electrical methods. Background and methodology

    International Nuclear Information System (INIS)

    Loefgren, Martin; Neretnieks, Ivars

    2002-10-01

    Matrix diffusion has been identified as one of the most important mechanisms governing the retardation of radionuclides escaping from a deep geological repository for nuclear waste. Radionuclides dissolved in groundwater flowing in water-bearing fractures will diffuse into water filled micropores in the rock. Important parameters governing the matrix diffusion are the formation factor, the surface diffusion and sorption. This report focuses on the formation factor in undisturbed intrusive igneous rock and the possibility of measuring this parameter in-situ. The background to and the methodology of formation factor logging in-situ by electrical methods are given. The formation factor is here defined as a parameter only depending on the geometry of the porous system and not on the diffusing specie. Traditionally the formation factor has been measured by through diffusion experiments on core samples, which are costly and time consuming. It has been shown that the formation factor could also be measured by electrical methods that are faster and less expensive. Previously this has only been done quantitatively in the laboratory on a centimetre or decimetre scale. When measuring the formation factor in-situ in regions with saline groundwater only the rock resistivity and the pore water resistivity are needed. The rock resistivity could be obtained by a variety of geophysical downhole tools. Water-bearing fractures disturb the measurements and data possibly affected by free water has to be sorted out. This could be done without loosing too much data if the vertical resolution of the tool is high enough. It was found that the rock resistivity tool presently used by SKB are neither quantitative or have enough vertical resolution. Therefore the slimhole Dual-Laterolog from Antares was tested with good results. This tool has a high vertical resolution and gives quantitative rock resistivities that need no correction. At present there is no method of directly obtaining the

  4. Formation factor logging in-situ by electrical methods. Background and methodology

    Energy Technology Data Exchange (ETDEWEB)

    Loefgren, Martin; Neretnieks, Ivars [Royal Inst. of Tech., Stockholm (Sweden). Dept. of Chemical Engineering and Technology

    2002-10-01

    Matrix diffusion has been identified as one of the most important mechanisms governing the retardation of radionuclides escaping from a deep geological repository for nuclear waste. Radionuclides dissolved in groundwater flowing in water-bearing fractures will diffuse into water filled micropores in the rock. Important parameters governing the matrix diffusion are the formation factor, the surface diffusion and sorption. This report focuses on the formation factor in undisturbed intrusive igneous rock and the possibility of measuring this parameter in-situ. The background to and the methodology of formation factor logging in-situ by electrical methods are given. The formation factor is here defined as a parameter only depending on the geometry of the porous system and not on the diffusing specie. Traditionally the formation factor has been measured by through diffusion experiments on core samples, which are costly and time consuming. It has been shown that the formation factor could also be measured by electrical methods that are faster and less expensive. Previously this has only been done quantitatively in the laboratory on a centimetre or decimetre scale. When measuring the formation factor in-situ in regions with saline groundwater only the rock resistivity and the pore water resistivity are needed. The rock resistivity could be obtained by a variety of geophysical downhole tools. Water-bearing fractures disturb the measurements and data possibly affected by free water has to be sorted out. This could be done without loosing too much data if the vertical resolution of the tool is high enough. It was found that the rock resistivity tool presently used by SKB are neither quantitative or have enough vertical resolution. Therefore the slimhole Dual-Laterolog from Antares was tested with good results. This tool has a high vertical resolution and gives quantitative rock resistivities that need no correction. At present there is no method of directly obtaining the

  5. In situ measurement of conductivity during nanocomposite film deposition

    International Nuclear Information System (INIS)

    Blattmann, Christoph O.; Pratsinis, Sotiris E.

    2016-01-01

    Highlights: • Flame-made nanosilver dynamics are elucidated in the gas-phase & on substrates. • The resistance of freshly depositing nanosilver layers is monitored. • Low T g polymers facilitate rapid synthesis of conductive films. • Conductive nanosilver films form on top of or within the polymer depending on MW. - Abstract: Flexible and electrically conductive nanocomposite films are essential for small, portable and even implantable electronic devices. Typically, such film synthesis and conductivity measurement are carried out sequentially. As a result, optimization of filler loading and size/morphology characteristics with respect to film conductivity is rather tedious and costly. Here, freshly-made Ag nanoparticles (nanosilver) are made by scalable flame aerosol technology and directly deposited onto polymeric (polystyrene and poly(methyl methacrylate)) films during which the resistance of the resulting nanocomposite is measured in situ. The formation and gas-phase growth of such flame-made nanosilver, just before incorporation onto the polymer film, is measured by thermophoretic sampling and microscopy. Monitoring the nanocomposite resistance in situ reveals the onset of conductive network formation by the deposited nanosilver growth and sinternecking. The in situ measurement is much faster and more accurate than conventional ex situ four-point resistance measurements since an electrically percolating network is detected upon its formation by the in situ technique. Nevertheless, general resistance trends with respect to filler loading and host polymer composition are consistent for both in situ and ex situ measurements. The time lag for the onset of a conductive network (i.e., percolation) depends linearly on the glass transition temperature (T g ) of the host polymer. This is attributed to the increased nanoparticle-polymer interaction with decreasing T g . Proper selection of the host polymer in combination with in situ resistance monitoring

  6. Applying flow chemistry: methods, materials, and multistep synthesis.

    Science.gov (United States)

    McQuade, D Tyler; Seeberger, Peter H

    2013-07-05

    The synthesis of complex molecules requires control over both chemical reactivity and reaction conditions. While reactivity drives the majority of chemical discovery, advances in reaction condition control have accelerated method development/discovery. Recent tools include automated synthesizers and flow reactors. In this Synopsis, we describe how flow reactors have enabled chemical advances in our groups in the areas of single-stage reactions, materials synthesis, and multistep reactions. In each section, we detail the lessons learned and propose future directions.

  7. Synthesis and thermal characterization of CdS nano crystals in previously formed template of maleic anhydride-octene 1-vinyl butyl terpolymer

    International Nuclear Information System (INIS)

    Akbarov, O.H; Mammadova, R.E; Malikov, E.Y.

    2008-01-01

    Full text: Nano crystals have dimensions in the range 10100 nm. Crystals in this size range possess unique properties, which enable scientists to manufacture materials and devices capable of performing unimaginable tasks. For that reason synthesis of this semiconductor nano crystals is expedient. Many useful methods have been used for preparing sulphide semiconductor nano crystals, such as colloidal chemistry method, sol-gel method, inverse micelle method, in situ synthesis and assemble on polymer template. The most significant method is in situ synthesis and assemble of sulphide semiconductor nano crystals on polymer. Compared with other methods, the stability of nanoparticles is improved by the protection and confinement of the copolymer. Because of confinement and protection effects of template environmental risk is prevented in this method. On the base of this principles in situ synthesis of CdS nano crystals in maleic anhydride-octene 1-vinyl butyl terpolymer was realized in this scientific work. First of all in specific condition maleic anhydride, octene 1, and vinyl butyl ether were polymerized to form a terpolymer as the result of radical ter polymerization. In second step CdS nano crystals were synthesized in N,N-dimethylformamide solution of maleic anhydride-octene 1-vinyl butyl terpolymer through the reaction of thiourea with cadmium chloride. In this process CdCI 2 x 2.5H 2 O was dissolved in N,N-dimethylformamide solution of previously formed terpolymer and was heated in 90 0 C temperature for 4 hours with vigorous stirring. Then desired amount of thiourea in N,N-dimethylformamide was quickly injected into the reaction flask using a syringe. The reaction continued for another 1 hour, and a yellow clear solution was obtained, which indicated the formation of CdS nano crystals

  8. Acid-promoted Bicyclization of Diaryl Alkynes: Synthesis of 2H-Indazoles with in situ Generated Diazonium Salt as Nitrogen Source.

    Science.gov (United States)

    Zhang, Cheng; Chang, Sailan; Dong, Shanliang; Qiu, Lihua; Xu, Xinfang

    2018-06-08

    An unprecedented transition-metal-free tandem bicyclization of diaryl alkynes has been disclosed, which provides a streamlined access to a range of polycyclic 2H-indazoles in high to excellent yields. The salient features of this reaction include readily available starting materials, good functional group compatibility, mild reaction conditions, no column chromatography, high bond-formation efficiency, and ease in further transformations. Notably, this is the first example for the synthesis of 2H-indazoles with in situ generated diazonium salt as the nitrogen source, and a mechanistic rationale involving an acid-promoted tandem diazonium salt formation/bicyclization process is discussed.

  9. Evaluation and selection of in-situ leaching mining method using analytic hierarchy process

    International Nuclear Information System (INIS)

    Zhao Heyong; Tan Kaixuan; Liu Huizhen

    2007-01-01

    According to the complicated conditions and main influence factors of in-situ leaching min- ing, a model and processes of analytic hierarchy are established for evaluation and selection of in-situ leaching mining methods based on analytic hierarchy process. Taking a uranium mine in Xinjiang of China for example, the application of this model is presented. The results of analyses and calculation indicate that the acid leaching is the optimum project. (authors)

  10. Methods for the synthesis of donor-acceptor cyclopropanes

    Science.gov (United States)

    Tomilov, Yu V.; Menchikov, L. G.; Novikov, R. A.; Ivanova, O. A.; Trushkov, I. V.

    2018-03-01

    The interest in cyclopropane derivatives is caused by the facts that, first, the three-carbon ring is present in quite a few natural and biologically active compounds and, second, compounds with this ring are convenient building blocks for the synthesis of diverse molecules (acyclic, alicyclic and heterocyclic). The carbon–carbon bonds in cyclopropane are kinetically rather inert; hence, they need to be activated to be involved in reactions. An efficient way of activation is to introduce vicinal electron-donating and electron-withdrawing substituents into the ring; these substrates are usually referred to as donor-acceptor cyclopropanes. This review gives a systematic account of the key methods for the synthesis of donor-acceptor cyclopropanes. The most important among them are reactions of nucleophilic alkenes with diazo compounds and iodonium ylides and approaches based on reactions of electrophilic alkenes with sulfur ylides (the Corey–Chaykovsky reaction). Among other methods used for this purpose, noteworthy are cycloalkylation of CH-acids, addition of α-halocarbonyl compounds to alkenes, cyclization via 1,3-elimination, reactions of alkenes with halocarbenes followed by reduction, the Simmons–Smith reaction and some other. The scope of applicability and prospects of various methods for the synthesis of donor-acceptor cyclopropanes are discussed. The bibliography includes 530 references.

  11. Synthesis method for using in the design of an electron gun for gyrotion

    International Nuclear Information System (INIS)

    Silva, C.A.B.

    1987-09-01

    In this work a synthesis method is applied to the design of an electron gun for a 94GHz gyrotron. Using the synthesis method, it is found the shape of the electrodes compatible with the laminar flow which minimizes the action of space change on the electron velocity dispersion. A sistematic procedure is presented to fuid the parameters of the synthesis method which, in turn, are closely related to the characteristics of the aptoclechonic system. (author) [pt

  12. In situ NMR studies of reactions on catalysts

    Energy Technology Data Exchange (ETDEWEB)

    Haw, James F [Texas A and M Univ., College Station, TX (United States). Dept. of Chemistry

    1994-12-31

    Zeolites are useful in the synthesis of fine chemicals. The systematic understanding of organic chemistry of zeolite catalysis may contribute to: the elucidation of reaction mechanisms of existing catalytic processes; the discovery of new catalytic reactions; the application of zeolite catalysis to the synthesis of fine chemicals. This work presents species of zeolites identified by in situ NMR; reactions of organic chemicals on zeolites and proposes mechanisms as well as reactivity trends 3 refs., 7 tabs.

  13. An in situ infrared study of dimethyl carbonate synthesis from carbon dioxide and methanol over zirconia

    International Nuclear Information System (INIS)

    Jung, Kyeong Taek; Bell, Alexis T.

    2001-01-01

    The mechanism of dimethyl carbonate (DMC) synthesis from methanol and carbon dioxide over monoclinic zirconia has been investigated using in situ infrared spectroscopy. The dissociative adsorption of methanol occurs more slowly than the adsorption of carbon dioxide, but the species formed from methanol are bound more strongly. Upon adsorption, the oxygen atom of methanol binds to coordinately unsaturated Zr4+ cations present at the catalyst surface. Rapid dissociation of the adsorbed methanol leads to the formation of a methoxide group (Zr-OCH3) and the release of a proton, which reacts with a surface hydroxyl group to produce water. Carbon dioxide inserts in the Zr-O bond of the methoxide to form a mondentate methyl carbonate group (Zr-OC(O)OCH3). This process is facilitated by the interactions of C and O atoms in CO2 with Lewis acid-base pairs of sites (Zr4+O2-) on the surface of the catalyst. Methyl carbonate species can also be produced via the reaction of methanol with carbon dioxide adsorbed in the form of bicarbonate species with methanol, a process that results in the transfer of a methyl group to the carbonate and restores a hydroxyl group to the zirconia surface. The decomposition of DMC on monoclinic zirconia has also been investigated and has been observed to occur via the reverse of the processes described for the synthesis of DMC

  14. A method to provide rapid in situ determination of tip radius in dynamic atomic force microscopy

    International Nuclear Information System (INIS)

    Santos, Sergio; Guang Li; Souier, Tewfik; Gadelrab, Karim; Chiesa, Matteo; Thomson, Neil H.

    2012-01-01

    We provide a method to characterize the tip radius of an atomic force microscopy in situ by monitoring the dynamics of the cantilever in ambient conditions. The key concept is that the value of free amplitude for which transitions from the attractive to repulsive force regimes are observed, strongly depends on the curvature of the tip. In practice, the smaller the value of free amplitude required to observe a transition, the sharper the tip. This general behavior is remarkably independent of the properties of the sample and cantilever characteristics and shows the strong dependence of the transitions on the tip radius. The main advantage of this method is rapid in situ characterization. Rapid in situ characterization enables one to continuously monitor the tip size during experiments. Further, we show how to reproducibly shape the tip from a given initial size to any chosen larger size. This approach combined with the in situ tip size monitoring enables quantitative comparison of materials measurements between samples. These methods are set to allow quantitative data acquisition and make direct data comparison readily available in the community.

  15. Interactive modeling-synthesis-characterization approach towards controllable in situ self-assembly of artificial pinning centers in RE-123 films

    Science.gov (United States)

    Wu, Judy; Shi, Jack

    2017-10-01

    Raising critical current density J c in high temperature superconductors (HTSs) is an important strategy towards performance-cost balanced HTS technology for commercialization. The development of strong nanoscale artificial pinning centers (APCs) in HTS, such as YBa2Cu3O7 or RE-123 in general, represents one of the most exciting progressions in HTS material research in the last decade. Significantly raised J c has been demonstrated in APC/RE-123 nanocomposites by enhanced pinning on magnetic vortices in magnetic fields towards that demanded in practical applications. Among other processes, strain-mediated self-organization has been explored extensively for in situ formation of the APCs based on fundamental physics design rules. The desire in controlling the morphology, dimension, orientation, and concentration of APCs has led to a fundamental question on how strains interact in determining APCs at a macroscopic scale. Answering this question demands an interactive modeling-synthesis-characterization approach towards a thorough understanding of fundamental physics governing the strain-mediated self-organization of the APCs in the APC/RE-123 nanocomposites. Such an understanding is the key for a leap forward from the traditionally empirical method to materials-by-design to enable an optimal APC landscape to be achieved in epitaxial films of APC/YBCO nanocomposites under a precise guidance of fundamental physics. The paper intends to provide a review of recent progress made in the controllable generation of APCs using the interactive modeling-synthesis-characterization approach. The emphasis will be given to the understanding so far achieved using such an approach on the collective effect of the strain field on the morphology, dimension, and orientation of APCs in epitaxial APC/RE-123 nanocomposite films.

  16. In situ synthesis of magnetic CaraPVA IPN nanocomposite hydrogels and controlled drug release

    International Nuclear Information System (INIS)

    Mahdavinia, Gholam Reza; Etemadi, Hossein

    2014-01-01

    In this work, the magnetic nanocomposite hydrogels that focused on targeted drug delivery were synthesized by incorporation of polyvinyl alcohol (PVA), kappa-carrageenan (Cara), and magnetite Fe 3 O 4 nanoparticles. The magnetic nanoparticles were obtained in situ in the presence of a mixture of polyvinyl alcohol/kappa-carrageenan (CaraPVA). The produced magnetite-polymers were cross-linked with freezing–thawing technique and subsequent with K + solution. The synthesized hydrogels were thoroughly characterized by transmittance electron microscopy (TEM), scanning electron microscopy (SEM), X-ray diffraction (XRD), thermal gravimetric analysis (TGA), Fourier transform infrared spectroscopy (FT-IR), and vibrating sample magnetometer (VSM) techniques. The dynamic swelling kinetic models of hydrogels were analyzed according to the first- and second-order kinetic models and were found that the experimental kinetics data followed the second-order model well. Drug loading and release efficiency were evaluated by diclofenac sodium (DS) as the model drug. The in vitro drug release studies from hydrogels exhibited significant behaviors on the subject of physiological simulated pHs and external magnetic fields. Investigation on the antibacterial activity revealed the ability of drug-loaded hydrogels to inactivate the Gram-positive Staphylococcus aureus (S. aureus) bacteria. The mucoadhesive properties of the hydrogels were studied and the hydrogels containing kappa-carrageenan showed good mucoadhesiveness in both simulated gastric and intestinal conditions. - Highlights: • In situ synthesis of magnetic kappa-carrageenan/PVA nanocomposite hydrogel. • Low salt sensitivity of magnetic nanocomposite hydrogels was observed. • The release of diclofenac sodium from hydrogels was pH-dependent. • The release of diclofenac sodium from magnetic hydrogels was affected by external magnetic field. • The hydrogels containing carrageenan component showed high mucoadhesiveness

  17. In situ synthesis of magnetic CaraPVA IPN nanocomposite hydrogels and controlled drug release

    Energy Technology Data Exchange (ETDEWEB)

    Mahdavinia, Gholam Reza, E-mail: grmnia@maragheh.ac.ir; Etemadi, Hossein

    2014-12-01

    In this work, the magnetic nanocomposite hydrogels that focused on targeted drug delivery were synthesized by incorporation of polyvinyl alcohol (PVA), kappa-carrageenan (Cara), and magnetite Fe{sub 3}O{sub 4} nanoparticles. The magnetic nanoparticles were obtained in situ in the presence of a mixture of polyvinyl alcohol/kappa-carrageenan (CaraPVA). The produced magnetite-polymers were cross-linked with freezing–thawing technique and subsequent with K{sup +} solution. The synthesized hydrogels were thoroughly characterized by transmittance electron microscopy (TEM), scanning electron microscopy (SEM), X-ray diffraction (XRD), thermal gravimetric analysis (TGA), Fourier transform infrared spectroscopy (FT-IR), and vibrating sample magnetometer (VSM) techniques. The dynamic swelling kinetic models of hydrogels were analyzed according to the first- and second-order kinetic models and were found that the experimental kinetics data followed the second-order model well. Drug loading and release efficiency were evaluated by diclofenac sodium (DS) as the model drug. The in vitro drug release studies from hydrogels exhibited significant behaviors on the subject of physiological simulated pHs and external magnetic fields. Investigation on the antibacterial activity revealed the ability of drug-loaded hydrogels to inactivate the Gram-positive Staphylococcus aureus (S. aureus) bacteria. The mucoadhesive properties of the hydrogels were studied and the hydrogels containing kappa-carrageenan showed good mucoadhesiveness in both simulated gastric and intestinal conditions. - Highlights: • In situ synthesis of magnetic kappa-carrageenan/PVA nanocomposite hydrogel. • Low salt sensitivity of magnetic nanocomposite hydrogels was observed. • The release of diclofenac sodium from hydrogels was pH-dependent. • The release of diclofenac sodium from magnetic hydrogels was affected by external magnetic field. • The hydrogels containing carrageenan component showed high

  18. In-situ spectrometry of {sup 137}Cs in the soil by unfolding method

    Energy Technology Data Exchange (ETDEWEB)

    Fueloep, M; Ragan, P [Inst. of Preventive and Clinical Medicine, 833301 Bratislava (Slovakia); Krnac, S [Slovak Technical Univ., Bratislava (Slovakia)

    1996-12-31

    This contribution is aimed to the possibility of improving the in-situ gamma spectrometry to be independent on a knowledge about a depth distribution of {sup 137}Cs in soil and sufficiently sensitive for the measurement of the post-Chernobyl {sup 137}Cs at present, as well. The depth distribution of {sup 137}Cs averaged over a large area of soil is obtained by unfolding of the detector responses to primary and in soil forward scattered photons. The proposed method employs detector with and without collimator. The {sup 137}Cs distributions obtained in-situ measurements are analysed, and comparisons are made to the results obtained with soil sampling and with standard in-situ spectrometry, as well. 5 figs., 1 tab., 4 refs.

  19. Synthesis of CdS nanocrystals in polymeric films studied by in-situ GID and GISAXS

    KAUST Repository

    Di Luccio, Tiziana; Carbone, Dina; Masala, Silvia; Ramachandran, Karthik; Kornfield, Julie

    2015-01-01

    In this work, we describe the synthesis of CdS nanocrystals in thin polymeric films by in-situ Grazing Incidence Diffraction (GID) and Grazing Incidence Small Angle Scattering (GISAXS). The 2D GISAXS patterns indicate how the precursor structure is altered as the temperature is varied from 25°C to 300°C. At 150°C, the CdS nanocrystals start to arrange themselves in a hexagonal lattice with a lattice parameter of 27 A. The diffraction intensity from the hexagonal lattice reaches a maximum at 170"C and decreases steadily upon further heating above 220°C indicating loss of symmetry. Correspondingly, the GID scans at 170°C show strong crystalline peaks from cubic CdS nanocrystals that are about 2 nm size. The results indicate that a temperature of 170°C is sufficient to synthesize CdS nanocrystals without degradation of the polymer matrix (Topas) in thin films (about 30nm). © 2015 Materials Research Society.

  20. Synthesis of CdS nanocrystals in polymeric films studied by in-situ GID and GISAXS

    KAUST Repository

    Di Luccio, Tiziana

    2015-07-07

    In this work, we describe the synthesis of CdS nanocrystals in thin polymeric films by in-situ Grazing Incidence Diffraction (GID) and Grazing Incidence Small Angle Scattering (GISAXS). The 2D GISAXS patterns indicate how the precursor structure is altered as the temperature is varied from 25°C to 300°C. At 150°C, the CdS nanocrystals start to arrange themselves in a hexagonal lattice with a lattice parameter of 27 A. The diffraction intensity from the hexagonal lattice reaches a maximum at 170"C and decreases steadily upon further heating above 220°C indicating loss of symmetry. Correspondingly, the GID scans at 170°C show strong crystalline peaks from cubic CdS nanocrystals that are about 2 nm size. The results indicate that a temperature of 170°C is sufficient to synthesize CdS nanocrystals without degradation of the polymer matrix (Topas) in thin films (about 30nm). © 2015 Materials Research Society.

  1. Comparison of in situ DGT measurement with ex situ methods for predicting cadmium bioavailability in soils with combined pollution to biotas.

    Science.gov (United States)

    Wang, Peifang; Liu, Cui; Yao, Yu; Wang, Chao; Wang, Teng; Yuan, Ye; Hou, Jun

    2017-05-01

    To assess the capabilities of the different techniques in predicting Cadmium (Cd) bioavailability in Cd-contaminated soils with the addition of Zn, one in situ technique (diffusive gradients in thin films; DGT) was compared with soil solution concentration and four widely used single-step extraction methods (acetic acid, EDTA, sodium acetate and CaCl 2 ). Wheat and maize were selected as tested species. The results demonstrated that single Cd-polluted soils inhibited the growth of wheat and maize significantly compared with control plants; the shoot and root biomasses of the plants both dropped significantly (P 0.9) between Cd concentrations in two plants and Cd bioavailability indicated by each method in soils. Consequently, the results indicated that the DGT technique could be regarded as a good predictor of Cd bioavailability to plants, comparable to soil solution concentration and the four single-step extraction methods. Because the DGT technique can offer in situ data, it is expected to be widely used in more areas.

  2. Investigations into low pressure methanol synthesis

    DEFF Research Database (Denmark)

    Sharafutdinov, Irek

    The central topic of this work has been synthesis, characterization and optimization of novel Ni-Ga based catalysts for hydrogenation of CO2 to methanol. The overall goal was to search for materials that could be used as a low temperature (and low pressure) methanol synthesis catalyst....... This is required for small scale delocalized methanol production sites, where installation of energy demanding compression units should be avoided. The work was triggered by DFT calculations, which showed that certain bimetallic systems are active towards methanol synthesis from CO2 and H2 at ambient pressure...... containing 5:3 molar ratio of Ni:Ga, the intrinsic activity (methanol production rate per active surface area) is comparable to that of highly optimised Cu/ZnO/Al2O3. Formation of the catalyst was investigated with the aid of in-situ XRD and in-situ XAS techniques. The mechanism of alloying was proposed...

  3. 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...

  4. What is the most appropriate knowledge synthesis method to conduct a review? Protocol for a scoping review

    Directory of Open Access Journals (Sweden)

    Kastner Monika

    2012-08-01

    Full Text Available Abstract Background A knowledge synthesis attempts to summarize all pertinent studies on a specific question, can improve the understanding of inconsistencies in diverse evidence, and can identify gaps in research evidence to define future research agendas. Knowledge synthesis activities in healthcare have largely focused on systematic reviews of interventions. However, a wider range of synthesis methods has emerged in the last decade addressing different types of questions (e.g., realist synthesis to explore mediating mechanisms and moderators of interventions. Many different knowledge synthesis methods exist in the literature across multiple disciplines, but locating these, particularly for qualitative research, present challenges. There is a need for a comprehensive manual for synthesis methods (quantitative/qualitative or mixed, outlining how these methods are related, and how to match the most appropriate knowledge synthesis method to answer a research question. The objectives of this scoping review are to: 1 conduct a systematic search of the literature for knowledge synthesis methods across multi-disciplinary fields; 2 compare and contrast the different knowledge synthesis methods; and, 3 map out the specific steps to conducting the knowledge syntheses to inform the development of a knowledge synthesis methods manual/tool. Methods We will search relevant electronic databases (e.g., MEDLINE, CINAHL, grey literature, and discipline-based listservs. The scoping review will consider all study designs including qualitative and quantitative methodologies (excluding economic analysis or clinical practice guideline development, and identify knowledge synthesis methods across the disciplines of health, education, sociology, and philosophy. Two reviewers will pilot-test the screening criteria and data abstraction forms, and will independently screen the literature and abstract the data. A three-step synthesis process will be used to map the

  5. Synthesis of Fe3O4/polypyrrole/polyaniline nanocomposites by in-situ method and their electromagnetic absorbing properties

    Directory of Open Access Journals (Sweden)

    Bingzhen Li

    2017-05-01

    Full Text Available Fe3O4/PPy/PANI (Fe3O4/polypyrrole/polyaniline nanocomposites with excellent microwave absorbing properties have been successfully synthesized and characterized systematically. In detail, Fe3O4 nanoparticles were prepared via an environmental friendly, modified co-precipitation method. Afterward, two conductive polymers, PPy and PANI, were deposited onto the surface of Fe3O4 nanoparticles by in-situ polymerization of pyrrole and aniline. PPy and PANI was “glued” by the strong affinity between the carbonyl groups of PPy and the conjugated chains of PANI. The obtained Fe3O4/PPy/PANI nanocomposites have been found to possess excellent microwave absorbing property with the absorption bandwidth of 10.7 GHz (6.7–17.4 GHz and maximum reflection loss at 10.1 GHz (−40.2 dB. It proves that the combination of ultra-small Fe3O4 nanoparticles with two different conductive polymers have a great potential in the application of microwave absorbing materials.

  6. In-situ gamma spectrometry method for determination of environmental gamma dose

    International Nuclear Information System (INIS)

    Conti, Claudio de Carvalho

    1995-07-01

    This work tries to establish a methodology for germanium detectors calibration, normally used for in situ gamma ray spectrometry, for determining the environmental exposure rate in function of the energy of the incident photons. For this purpose a computer code has been developed, based on the stripping method, for the computational spectra analysis to calculate the contribution of the partial absorption of the gamma rays (Compton effect) in the active and nonactive parts of the detector. The resulting total absorption spectrum is then converted to fluence distribution in function of the energy for the photons reaching the detector, which is then used to calculate the exposure rate or kerma in air. The unfolding and fluency convention parameters are determined by detector calibration using point gamma sources. The method is validated by comparison of the results against the calculated exposure rate at a point of interest for the standards. This method is used for the direct measurement of the exposure rate distribution in function of the energy at the site, in situ measurement technic, leading to rapid results during an emergency situation and also used for indoor measurements. (author)

  7. In-situ synthesis of Co{sub 3}O{sub 4}/graphite nanocomposite for high-performance supercapacitor electrode applications

    Energy Technology Data Exchange (ETDEWEB)

    M, Gopalakrishnan, E-mail: gopalkphy@gmail.com [Department of Physics, Vivekanandha College of Arts and Science for Women, Tiruchengode, Namakkal, 637205, Tamilnadu (India); G, Srikesh [Department of Chemistry, Material Electrochemistry Lab, Karunya University, Coimbatore 641114, Tamilnadu (India); A, Mohan [Department of Physics, Thin Film Laboratory, Karunya University, Coimbatore 641114, Tamilnadu (India); V, Arivazhagan [Department of Physics and Technology, University of Bergen, Bergen (Norway)

    2017-05-01

    Highlights: • High surface area, which governs the specific capacitance. • High chemical and thermal stability. • Co{sub 3}O{sub 4}/graphite nanocomposite electrode shows lower resistance. - Abstract: In this work, a low cost and pollution free in-situ synthesis of phase pure Co{sub 3}O{sub 4} nanoparticles and Co{sub 3}O{sub 4}/graphite nanocomposite have been successfully developed via co-precipitation method followed by the thermal treatment process. The prepared samples were characterized by powder X-ray diffraction, scanning electron microscope, high resolution transmission electron microscope, Fourier Transform Infrared Spectroscopy and electrochemical measurements. Electrochemical measurements such as cyclic voltammetry, galvanostatic charge–discharge, electrochemical impedance spectroscopy were carried out in 6 M KOH aqueous electrolytic solution. The results show the excellent maximum specific capacitive behavior of 239.5 F g{sup −1} for pure and 395.04 F g{sup −1} for Co{sub 3}O{sub 4}/graphite nanocomposite at a current density of 0.5 A g{sup −1}. This composite exhibits a good cyclic stability, with a small loss of 2.68% of maximum capacitance over a consecutive 1000 cycles. The investigation indicates that the prepared electrode material could be a potential and promising candidate for electrochemical supercapacitors.

  8. Li4Ti5O12 thin-film electrodes by in-situ synthesis of lithium alkoxide for Li-ion microbatteries

    International Nuclear Information System (INIS)

    Mosa, J.; Aparicio, M.; Tadanaga, K.; Hayashi, A.; Tatsumisago, M.

    2014-01-01

    Rechargeable thin-film batteries have recently become the topic of widespread research for use as efficient energy storage devices. Spinel Li 4 Ti 5 O 12 has been considered as one of the most prospective anode materials for Li-ion batteries because of its excellent reversibility and long cycle life. We report here the sol–gel synthesis and coating preparation of spinel thin-film Li 4 Ti 5 O 12 electrodes for Li-ion microbatteries using lithium ethoxide produced in situ that reacts with titanium alkoxide to produce the precursor solution without particle precipitation. This synthesis procedure reduces the thermal treatment to obtain a pure phase at only 700 °C and 15 minutes. The physical and structural characterization of the 300 nm Li 4 Ti 5 O 12 coatings shows a very homogeneous distribution of elements and a pure spinel phase. Galvanostatic discharge-charge tests indicate maximum discharge capacities of 152 mA h g −1 when the material is treated at 700 °C for 15 minutes

  9. Method and apparatus for producing synthesis gas

    Science.gov (United States)

    Hemmings, John William; Bonnell, Leo; Robinson, Earl T.

    2010-03-03

    A method and apparatus for reacting a hydrocarbon containing feed stream by steam methane reforming reactions to form a synthesis gas. The hydrocarbon containing feed is reacted within a reactor having stages in which the final stage from which a synthesis gas is discharged incorporates expensive high temperature materials such as oxide dispersed strengthened metals while upstream stages operate at a lower temperature allowing the use of more conventional high temperature alloys. Each of the reactor stages incorporate reactor elements having one or more separation zones to separate oxygen from an oxygen containing feed to support combustion of a fuel within adjacent combustion zones, thereby to generate heat to support the endothermic steam methane reforming reactions.

  10. In situ probing of temperature in radio frequency thermal plasma using Yttrium ion emission lines during synthesis of yttria nanoparticles

    Science.gov (United States)

    Dhamale, G. D.; Tiwari, N.; Mathe, V. L.; Bhoraskar, S. V.; Ghorui, S.

    2017-07-01

    Particle feeding is used in the most important applications of radio frequency (r.f.) thermal plasmas like synthesis of nanoparticles and particle spheroidization. The study reports an in-situ investigation of radial distribution of temperature in such devices using yttrium ion emission lines under different rates of particle loading during synthesis of yttria nanoparticles. A number of interesting facts about the response of r.f. plasma to the rate of particle loading, hitherto unknown, are revealed. Observed phenomena are supported with experimental data from fast photographic experiments and actual synthesis results. The use of the Abel inversion technique together with simultaneous multi-track acquisition of emission spectra from different spatial locations using a CCD based spectrometer allowed us to extract accurate distribution of temperature inside the plasma in the presence of inherent instabilities. The temperature profiles of this type of plasma have been measured possibly for the first time while particles are being fed into the plasma. Observed changes in the temperature profiles as the particle feed rate increases are very significant. Reaction forces resulting from particle evaporation, and increased skin depth owing to the decrease in electrical conductivity in the edge region are proposed as the two different mechanisms to account for the observed changes in the temperature profile as the powder feed rate is increased. Quantitative analyses supporting the proposed mechanisms are presented.

  11. SYNTHESIS METHODS OF ALGEBRAIC NORMAL FORM OF MANY-VALUED LOGIC FUNCTIONS

    Directory of Open Access Journals (Sweden)

    A. V. Sokolov

    2016-01-01

    Full Text Available The rapid development of methods of error-correcting coding, cryptography, and signal synthesis theory based on the principles of many-valued logic determines the need for a more detailed study of the forms of representation of functions of many-valued logic. In particular the algebraic normal form of Boolean functions, also known as Zhegalkin polynomial, that well describe many of the cryptographic properties of Boolean functions is widely used. In this article, we formalized the notion of algebraic normal form for many-valued logic functions. We developed a fast method of synthesis of algebraic normal form of 3-functions and 5-functions that work similarly to the Reed-Muller transform for Boolean functions: on the basis of recurrently synthesized transform matrices. We propose the hypothesis, which determines the rules of the synthesis of these matrices for the transformation from the truth table to the coefficients of the algebraic normal form and the inverse transform for any given number of variables of 3-functions or 5-functions. The article also introduces the definition of algebraic degree of nonlinearity of the functions of many-valued logic and the S-box, based on the principles of many-valued logic. Thus, the methods of synthesis of algebraic normal form of 3-functions applied to the known construction of recurrent synthesis of S-boxes of length N = 3k, whereby their algebraic degrees of nonlinearity are computed. The results could be the basis for further theoretical research and practical applications such as: the development of new cryptographic primitives, error-correcting codes, algorithms of data compression, signal structures, and algorithms of block and stream encryption, all based on the perspective principles of many-valued logic. In addition, the fast method of synthesis of algebraic normal form of many-valued logic functions is the basis for their software and hardware implementation.

  12. Synthesis activity-based zymography for detection of lipases and esterases.

    Science.gov (United States)

    Kwon, Min-A; Kim, Hyun Suk; Hahm, Dae-Hyun; Song, Jae Kwang

    2011-04-01

    A new zymography method for lipases and esterases was developed on the basis of the esterification reaction between fatty acids and alcohols. The enzymes were separated by SDS-PAGE and native PAGE. The gel was washed and then incubated in an aqueous solution containing fatty acids (oleic acid 18:1 or caprylic acid 8:0) and dodecanol. Synthesis was visualized by in situ precipitation of water-insoluble and non-diffusible fatty acid esters, such as dodecyl oleate and dodecyl octanoate. The synthesis activity-based zymography was confirmed with different enzyme samples, including commercial lipase preparations, purified recombinant lipase and cutinase, and crude culture supernatants of lipolytic enzyme-producing soil bacteria.

  13. Laser Based In Situ Techniques: Novel Methods for Generating Extreme Conditions in TEM Samples

    Energy Technology Data Exchange (ETDEWEB)

    Taheri, M; Lagrange, T; Reed, B; Armstrong, M; Campbell, G; DeHope, W; Kim, J; King, W; Masiel, D; Browning, N

    2008-02-25

    The Dynamic Transmission Electron Microscope (DTEM) is introduced as a novel tool for in situ processing of materials. Examples of various types of dynamic studies outline the advantages and differences of laser-based heating in the DTEM in comparison to conventional (resistive) heating in situ TEM methods. We demonstrate various unique capabilities of the drive laser, namely, in situ processing of nanoscale materials, rapid and high temperature phase transformations, and controlled thermal activation of materials. These experiments would otherwise be impossible without the use of the DTEM drive laser. Thus, the potential of the DTEM to as a new technique to process and characterize the growth of a myriad of micro and nanostructures is demonstrated.

  14. In situ synthesis carbonated hydroxyapatite layers on enamel slices with acidic amino acids by a novel two-step method.

    Science.gov (United States)

    Wu, Xiaoguang; Zhao, Xu; Li, Yi; Yang, Tao; Yan, Xiujuan; Wang, Ke

    2015-09-01

    In situ fabrication of carbonated hydroxyapatite (CHA) remineralization layer on an enamel slice was completed in a novel, biomimetic two-step method. First, a CaCO3 layer was synthesized on the surface of demineralized enamel using an acidic amino acid (aspartic acid or glutamate acid) as a soft template. Second, at the same concentration of the acidic amino acid, rod-like carbonated hydroxyapatite was produced with the CaCO3 layer as a sacrificial template and a reactant. The morphology, crystallinity and other physicochemical properties of the crystals were characterized using field emission scanning electron microscopy (FESEM), Fourier transform infrared spectrometry (FTIR), X-ray diffraction (XRD) and energy-dispersive X-ray analysis (EDAX), respectively. Acidic amino acid could promote the uniform deposition of hydroxyapatite with rod-like crystals via absorption of phosphate and carbonate ions from the reaction solution. Moreover, compared with hydroxyapatite crystals coated on the enamel when synthesized by a one-step method, the CaCO3 coating that was synthesized in the first step acted as an active bridge layer and sacrificial template. It played a vital role in orienting the artificial coating layer through the template effect. The results show that the rod-like carbonated hydroxyapatite crystals grow into bundles, which are similar in size and appearance to prisms in human enamel, when using the two-step method with either aspartic acid or acidic glutamate (20.00 mmol/L). Copyright © 2015 Elsevier B.V. All rights reserved.

  15. In Situ Synthesis of Mn3 O4 Nanoparticles on Hollow Carbon Nanofiber as High-Performance Lithium-Ion Battery Anode.

    Science.gov (United States)

    Zhang, Dan; Li, Guangshe; Fan, Jianming; Li, Baoyun; Li, Liping

    2018-04-26

    The practical applications of Mn 3 O 4 in lithium-ion batteries are greatly hindered by fast capacity decay and poor rate performance as a result of significant volume changes and low electrical conductivity. It is believed that the synthesis of nanoscale Mn 3 O 4 combined with carbonaceous matrix will lead to a better electrochemical performance. Herein, a convenient route for the synthesis of Mn 3 O 4 nanoparticles grown in situ on hollow carbon nanofiber (denoted as HCF/Mn 3 O 4 ) is reported. The small size of Mn 3 O 4 particles combined with HCF can significantly alleviate volume changes and electrical conductivity; the strong chemical interactions between HCF and Mn 3 O 4 would improve the reversibility of the conversion reaction for MnO into Mn 3 O 4 and accelerate charge transfer. These features endow the HCF/Mn 3 O 4 composite with superior cycling stability and rate performance if used as the anode for lithium-ion batteries. The composite delivers a high discharge capacity of 835 mA h g -1 after 100 cycles at 200 mA g -1 , and 652 mA h g -1 after 240 cycles at 1000 mA g -1 . Even at 2000 mA g -1 , it still shows a high capacity of 528 mA h g -1 . The facile synthetic method and outstanding electrochemical performance of the as-prepared HCF/Mn 3 O 4 composite make it a promising candidate for a potential anode material for lithium-ion batteries. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

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

    International Nuclear Information System (INIS)

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

    2013-01-01

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

  17. Synthesis method validation for Super-Phenix 1 start-up core studies

    International Nuclear Information System (INIS)

    Pipaud, J.Y.; Gastaldo, G.; Giacometti, C.

    1980-09-01

    This paper aims at presenting the systematic studies performed in order to check and to improve the synthesis method wich is used to optimize the configuration of the SUPER-PHENIX 1 start-up core versus the diluent subassembly location and the control rod ring insertion. A special attention is paid to the choice of the trial functions when the two rod rings have different insertion depths. Present limits of the synthesis method are given and further improvements are indicated

  18. Synthesis of 1D Bragg gratings by a layer-aggregation method.

    Science.gov (United States)

    Capmany, José; Muriel, Miguel A; Sales, Salvador

    2007-08-15

    We present what we believe to be a novel method for the synthesis of complex 1D (fiber and waveguide) Bragg gratings, which is based on an impedance reconstruction layer aggregation technique. The main advantage brought by the method is the possibility of synthesizing structures containing defects or discontinuities of the size of the local period, a feature that is not possible with prior reported methods. In addition, this enhanced spatial resolution allows the synthesis of very strong fiber Bragg grating devices providing convergent solutions. The method directly renders the refractive index profile n(z) as it does not rely on the coupled-mode theory.

  19. Fabrication of Nanocarbon Composites Using In Situ Chemical Vapor Deposition and Their Applications.

    Science.gov (United States)

    He, Chunnian; Zhao, Naiqin; Shi, Chunsheng; Liu, Enzuo; Li, Jiajun

    2015-09-23

    Nanocarbon (carbon nanotubes (CNTs) and graphene (GN)) composites attract considerable research interest due to their fascinating applications in many fields. Here, recent developments in the field of in situ chemical vapor deposition (CVD) for the design and controlled preparation of advanced nanocarbon composites are highlighted, specifically, CNT-reinforced bulk structural composites, as well as CNT, GN, and CNT/GN functional composites, together with their practical and potential applications. In situ CVD is a very attractive approach for the fabrication of composites because of its engaging features, such as its simplicity, low-cost, versatility, and tunability. The morphologies, structures, dispersion, and interface of the resulting nanocarbon composites can be easily modulated by varying the experimental parameters (such as temperature, catalysts, carbon sources, templates or template catalysts, etc.), which enables a great potential for the in situ synthesis of high-quality nanocarbons with tailored size and dimension for constructing high-performance composites, which has not yet been achieved by conventional methods. In addition, new trends of the in situ CVD toward nanocarbon composites are discussed. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  20. Perspective: Toward "synthesis by design": Exploring atomic correlations during inorganic materials synthesis

    Science.gov (United States)

    Soderholm, L.; Mitchell, J. F.

    2016-05-01

    Synthesis of inorganic extended solids is a critical starting point from which real-world functional materials and their consequent technologies originate. However, unlike the rich mechanistic foundation of organic synthesis, with its underlying rules of assembly (e.g., functional groups and their reactivities), the synthesis of inorganic materials lacks an underpinning of such robust organizing principles. In the latter case, any such rules must account for the diversity of chemical species and bonding motifs inherent to inorganic materials and the potential impact of mass transport on kinetics, among other considerations. Without such assembly rules, there is less understanding, less predictive power, and ultimately less control of properties. Despite such hurdles, developing a mechanistic understanding for synthesis of inorganic extended solids would dramatically impact the range of new material discoveries and resulting new functionalities, warranting a broad call to explore what is possible. Here we discuss our recent approaches toward a mechanistic framework for the synthesis of bulk inorganic extended solids, in which either embryonic atomic correlations or fully developed phases in solutions or melts can be identified and tracked during product selection and crystallization. The approach hinges on the application of high-energy x-rays, with their penetrating power and large Q-range, to explore reaction pathways in situ. We illustrate this process using two examples: directed assembly of Zr clusters in aqueous solution and total phase awareness during crystallization from K-Cu-S melts. These examples provide a glimpse of what we see as a larger vision, in which large scale simulations, data-driven science, and in situ studies of atomic correlations combine to accelerate materials discovery and synthesis, based on the assembly of well-defined, prenucleated atomic correlations.

  1. Multi-line split DNA synthesis: a novel combinatorial method to make high quality peptide libraries

    Directory of Open Access Journals (Sweden)

    Ueno Shingo

    2004-09-01

    Full Text Available Abstract Background We developed a method to make a various high quality random peptide libraries for evolutionary protein engineering based on a combinatorial DNA synthesis. Results A split synthesis in codon units was performed with mixtures of bases optimally designed by using a Genetic Algorithm program. It required only standard DNA synthetic reagents and standard DNA synthesizers in three lines. This multi-line split DNA synthesis (MLSDS is simply realized by adding a mix-and-split process to normal DNA synthesis protocol. Superiority of MLSDS method over other methods was shown. We demonstrated the synthesis of oligonucleotide libraries with 1016 diversity, and the construction of a library with random sequence coding 120 amino acids containing few stop codons. Conclusions Owing to the flexibility of the MLSDS method, it will be able to design various "rational" libraries by using bioinformatics databases.

  2. Rapid in situ synthesis of spherical microflower Pt/C catalyst via spray-drying for high performance fuel cell application

    Energy Technology Data Exchange (ETDEWEB)

    Balgis, R.; Ogi, T.; Okuyama, K. [Department of Chemical Engineering, Graduate School of Engineering, Hiroshima University, Higashi Hiroshima, Hiroshima (Japan); Anilkumar, G.M.; Sago, S. [Research and Development Centre, Noritake Co., Ltd., Higashiyama, Miyoshi, Aichi (Japan)

    2012-08-15

    A facile route for the rapid in situ synthesis of platinum nanoparticles on spherical microflower carbon has been developed. An aqueous precursor slurry containing carbon black, polystyrene latex (PSL), polyvinyl alcohol, and platinum salt was spray-dried, followed by calcination to simultaneously reduce platinum salt and to decompose PSL particles. Prepared Pt/C catalyst showed high-performance electrocatalytic activity with excellent durability. The mass activity and specific activity values were 132.26 mA mg{sup -1} Pt and 207.62 {mu}A cm{sup -2} Pt, respectively. This work presents a future direction for the production of high-performance Pt/C catalyst in an industrial scale. (Copyright copyright 2012 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  3. Synthesis of Pt nanoparticles on electrochemically reduced graphene oxide by potentiostatic and alternate current methods

    International Nuclear Information System (INIS)

    Molina, J.; Fernández, J.; Río, A.I. del; Bonastre, J.; Cases, F.

    2014-01-01

    Reduced graphene oxide (RGO) has been synthesized on Pt wires by means of a potentiodynamic method between + 0.6 V and − 1.4 V for 20 scans. Cyclic voltammetry characterization of the coatings showed the typical capacitative behavior of graphene. Pt nanoparticles were synthesized on Pt–RGO electrodes by means of potentiostatic methods and a comparison between different synthesis potentials (− 0.16, 0, + 0.2 and + 0.4 V) for the same synthesis charge (mC·cm −2 ) was established. The electrodes obtained were characterized in 0.5 M H 2 SO 4 solution to observe the characteristic oxidation and reduction processes of the Pt surface. A 0.5 M H 2 SO 4 /0.5 M CH 3 OH solution was used to measure the catalytic properties of the deposits against methanol oxidation. The most appropriate potential to perform the synthesis was 0 V followed by − 0.16 V and + 0.2 V. The morphology of the coatings varied depending on the potential applied as observed by scanning electron microscopy. Alternate current methods were also used to synthesize Pt nanoparticles and compare the results with the traditional potentiostatic method. Different frequencies were used: 0.1, 1, 10, 100, 1000 and 10 000 Hz. Alternate current synthesis is more efficient than traditional potentiostatic methods, obtaining more electroactive coatings with less effective synthesis time. - Highlights: • Reduced graphene oxide has been obtained by electrochemical reduction on Pt wires. • Pt nanoparticles have been obtained potentiostatically at different potentials. • Pt nanoparticles have been obtained by ac methods with different frequencies. • ac synthesis is a better synthesis method than potentiostatic synthesis

  4. In-Situ Hydrothermal Synthesis of Bi-Bi2O2CO3 Heterojunction Photocatalyst with Enhanced Visible Light Photocatalytic Activity

    Science.gov (United States)

    Kar, Prasenjit; Maji, Tuhin Kumar; Nandi, Ramesh; Lemmens, Peter; Pal, Samir Kumar

    2017-04-01

    Bismuth containing nanomaterials recently received increasing attention with respect to environmental applications because of their low cost, high stability and nontoxicity. In this work, Bi-Bi2O2CO3 heterojunctions were fabricated by in-situ decoration of Bi nanoparticles on Bi2O2CO3 nanosheets via a simple hydrothermal synthesis approach. X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and high-resolution TEM (HRTEM) were used to confirm the morphology of the nanosheet-like heterostructure of the Bi-Bi2O2CO3 composite. Detailed ultrafast electronic spectroscopy reveals that the in-situ decoration of Bi nanoparticles on Bi2O2CO3 nanosheets exhibit a dramatically enhanced electron-hole pair separation rate, which results in an extraordinarily high photocatalytic activity for the degradation of a model organic dye, methylene blue (MB) under visible light illumination. Cycling experiments revealed a good photochemical stability of the Bi-Bi2O2CO3 heterojunction under repeated irradiation. Photocurrent measurements further indicated that the heterojunction incredibly enhanced the charge generation and suppressed the charge recombination of photogenerated electron-hole pairs.

  5. Piping dynamic analysis by the synthesis method

    International Nuclear Information System (INIS)

    Bezler, P.; Curreri, J.R.

    1976-01-01

    Since piping systems are a frequent source of noise and vibrations, their efficient dynamic analysis is imperative. As an alternate to more conventional analyses methods, an application of the synthesis method to piping vibrations analyses is demonstrated. Specifically, the technique is illustrated by determining the normal modes and natural frequencies of a composite bend from the normal mode and natural frequency data of two component parts. A comparison of the results to those derived for the composite bend by other techniques is made

  6. Finite element design for the HPHT synthesis of diamond

    Science.gov (United States)

    Li, Rui; Ding, Mingming; Shi, Tongfei

    2018-06-01

    The finite element method is used to simulate the steady-state temperature field in diamond synthesis cell. The 2D and 3D models of the China-type cubic press with large deformation of the synthesis cell was established successfully, which has been verified by situ measurements of synthesis cell. The assembly design, component design and process design for the HPHT synthesis of diamond based on the finite element simulation were presented one by one. The temperature field in a high-pressure synthetic cavity for diamond production is optimized by adjusting the cavity assembly. A series of analysis about the influence of the pressure media parameters on the temperature field are examined through adjusting the model parameters. Furthermore, the formation mechanism of wasteland was studied in detail. It indicates that the wasteland is inevitably exists in the synthesis sample, the distribution of growth region of the diamond with hex-octahedral is move to the center of the synthesis sample from near the heater as the power increasing, and the growth conditions of high quality diamond is locating at the center of the synthesis sample. These works can offer suggestion and advice to the development and optimization of a diamond production process.

  7. In situ green synthesis of antimicrobial carboxymethyl chitosan-nanosilver hybrids with controlled silver release.

    Science.gov (United States)

    Huang, Siqi; Yu, Zhiming; Zhang, Yang; Qi, Chusheng; Zhang, Shifeng

    2017-01-01

    In order to fabricate antimicrobial carboxymethyl chitosan-nanosilver (CMC-Ag) hybrids with controlled silver release, this study demonstrated comparable formation via three synthetic protocols: 1) carboxymethyl chitosan (CMC) and glucose (adding glucose after AgNO 3 ), 2) CMC and glucose (adding glucose before AgNO 3 ), and 3) CMC only. Under principles of green chemistry, the synthesis was conducted in an aqueous medium exposed to microwave irradiation for 10 minutes with nontoxic chemicals. The structure and formation mechanisms of the three CMC-Ag hybrids were explored using X-ray diffraction, ultraviolet-visible spectroscopy, transmission electron microscopy, and Fourier-transform infrared analyses. Additionally, antimicrobial activity and in vitro silver release of the three synthesized hybrids were investigated in detail. The results revealed that a large number of stable, uniform, and small silver nanoparticles (AgNPs) were synthesized in situ on CMC chains via protocol 1. AgNPs were well dispersed with narrow size distribution in the range of 6-20 nm, with mean diameter only 12.22±2.57 nm. The addition of glucose resulted in greater AgNP synthesis. The order of addition of glucose and AgNO 3 significantly affected particle size and size distribution of AgNPs. Compared to CMC alone and commercially available AgNPs, the antimicrobial activities of three hybrids were significantly improved. Of the three hybrids, CMC-Ag1 synthesized via protocol 1 exhibited better antimicrobial activity than CMC-Ag2 and CMC-Ag3, and showed more effective inhibition of Staphylococcus aureus than Escherichia coli . Due to strong coordination and electrostatic interactions between CMC and silver and good steric protection provided by CMC, CMC-Ag1 displayed stable and continuous silver release and better performance in retaining silver for prolonged periods than CMC-Ag2 and CMC-Ag3.

  8. In situ green synthesis of antimicrobial carboxymethyl chitosan–nanosilver hybrids with controlled silver release

    Science.gov (United States)

    Huang, Siqi; Yu, Zhiming; Zhang, Yang; Qi, Chusheng; Zhang, Shifeng

    2017-01-01

    In order to fabricate antimicrobial carboxymethyl chitosan–nanosilver (CMC-Ag) hybrids with controlled silver release, this study demonstrated comparable formation via three synthetic protocols: 1) carboxymethyl chitosan (CMC) and glucose (adding glucose after AgNO3), 2) CMC and glucose (adding glucose before AgNO3), and 3) CMC only. Under principles of green chemistry, the synthesis was conducted in an aqueous medium exposed to microwave irradiation for 10 minutes with nontoxic chemicals. The structure and formation mechanisms of the three CMC-Ag hybrids were explored using X-ray diffraction, ultraviolet-visible spectroscopy, transmission electron microscopy, and Fourier-transform infrared analyses. Additionally, antimicrobial activity and in vitro silver release of the three synthesized hybrids were investigated in detail. The results revealed that a large number of stable, uniform, and small silver nanoparticles (AgNPs) were synthesized in situ on CMC chains via protocol 1. AgNPs were well dispersed with narrow size distribution in the range of 6–20 nm, with mean diameter only 12.22±2.57 nm. The addition of glucose resulted in greater AgNP synthesis. The order of addition of glucose and AgNO3 significantly affected particle size and size distribution of AgNPs. Compared to CMC alone and commercially available AgNPs, the antimicrobial activities of three hybrids were significantly improved. Of the three hybrids, CMC-Ag1 synthesized via protocol 1 exhibited better antimicrobial activity than CMC-Ag2 and CMC-Ag3, and showed more effective inhibition of Staphylococcus aureus than Escherichia coli. Due to strong coordination and electrostatic interactions between CMC and silver and good steric protection provided by CMC, CMC-Ag1 displayed stable and continuous silver release and better performance in retaining silver for prolonged periods than CMC-Ag2 and CMC-Ag3. PMID:28458539

  9. Histidine as a catalyst in organic synthesis: A facile in situ synthesis ...

    Indian Academy of Sciences (India)

    Unknown

    They are also used in the synthesis of many nitrogen-containing biologically ... addition to hydroxylamine, results in formation of an imine, azoxy compound 15, ... GC-MS, m/z: 211 (M+), 194 (base peak); 13C NMR (DMSO-d6) δ : 31⋅14 ...

  10. Electrochemical Performance of LixMn2-yFeyO4-zClz Synthesized Through In-Situ Glycine Nitrate Combustion

    Science.gov (United States)

    2016-06-13

    Electrochemical Performance of LixMn2-yFeyO4-zClz Synthesized Through In-Situ Glycine Nitrate Combustion Ashley L. Ruth, Paula C. Latorre, and...sites as well as the formation of Mn3+ ions via the Jahn- Teller effect. The use of the glycine nitrate combustion synthesis produces small particles at...advantage of submicron ceramic synthesis, namely the glycine nitrate combustion process (GNP), we propose the capability for in-situ B-site doping

  11. Computational method and system for modeling, analyzing, and optimizing DNA amplification and synthesis

    Science.gov (United States)

    Vandersall, Jennifer A.; Gardner, Shea N.; Clague, David S.

    2010-05-04

    A computational method and computer-based system of modeling DNA synthesis for the design and interpretation of PCR amplification, parallel DNA synthesis, and microarray chip analysis. The method and system include modules that address the bioinformatics, kinetics, and thermodynamics of DNA amplification and synthesis. Specifically, the steps of DNA selection, as well as the kinetics and thermodynamics of DNA hybridization and extensions, are addressed, which enable the optimization of the processing and the prediction of the products as a function of DNA sequence, mixing protocol, time, temperature and concentration of species.

  12. Using Converter Dust to Produce Low Cost Cementitious Composites by in situ Carbon Nanotube and Nanofiber Synthesis

    Directory of Open Access Journals (Sweden)

    Péter Ludvig

    2011-03-01

    Full Text Available Carbon nanotubes (CNTs and nanofibers (CNFs were synthesized on clinker and silica fume particles in order to create a low cost cementitious nanostructured material. The synthesis was carried out by an in situ chemical vapor deposition (CVD process using converter dust, an industrial byproduct, as iron precursor. The use of these materials reduces the cost, with the objective of application in large-scale nanostructured cement production. The resulting products were analyzed by scanning electron microscopy (SEM, transmission electron microscopy (TEM and thermogravimetric analysis (TGA and were found to be polydisperse in size and to have defective microstructure. Some enhancement in the mechanical behavior of cement mortars was observed due to the addition of these nano-size materials. The contribution of these CNTs/CNFs to the mechanical strength of mortar specimens is similar to that of high quality CNTs incorporated in mortars by physical mixture.

  13. Semiconductor/metal nanocomposites formed by in situ reduction method in multilayer thin films

    International Nuclear Information System (INIS)

    Song Yanli; Wang Enbo; Tian Chungui; Mao Baodong; Wang Chunlei

    2009-01-01

    A layer-by-layer adsorption and in situ reduction method was adopted for synthesizing semiconductor/metal nanocomposites in multilayer ultra-thin films. Alternate adsorption of ZnO nanoparticles modified with poly(ethyleneimine), hydrogentetrachloroaurate and poly(styrenesulfonate) sodium results in the formation of ZnO/AuCl 4 - -loaded multilayer films. In situ reduction of the incorporated metal ions by heating yields ZnO/Au nanocomposites in the films. UV-vis absorption spectroscopy and X-ray photoelectron spectroscopy were used to characterize the components of the composite films. UV-vis spectra indicate regular growth of the films. The electrochemistry behavior of the multilayer films was studied in detail on indium tin oxide electrode. The combined results suggest that the layer-by-layer adsorption and subsequent reduction method used here provides an effective way to synthesize ZnO/Au nanocomposites in the polymer matrix

  14. Synthesis of Pt nanoparticles on electrochemically reduced graphene oxide by potentiostatic and alternate current methods

    Energy Technology Data Exchange (ETDEWEB)

    Molina, J.; Fernández, J.; Río, A.I. del; Bonastre, J.; Cases, F., E-mail: fjcases@txp.upv.es

    2014-03-01

    Reduced graphene oxide (RGO) has been synthesized on Pt wires by means of a potentiodynamic method between + 0.6 V and − 1.4 V for 20 scans. Cyclic voltammetry characterization of the coatings showed the typical capacitative behavior of graphene. Pt nanoparticles were synthesized on Pt–RGO electrodes by means of potentiostatic methods and a comparison between different synthesis potentials (− 0.16, 0, + 0.2 and + 0.4 V) for the same synthesis charge (mC·cm{sup −2}) was established. The electrodes obtained were characterized in 0.5 M H{sub 2}SO{sub 4} solution to observe the characteristic oxidation and reduction processes of the Pt surface. A 0.5 M H{sub 2}SO{sub 4}/0.5 M CH{sub 3}OH solution was used to measure the catalytic properties of the deposits against methanol oxidation. The most appropriate potential to perform the synthesis was 0 V followed by − 0.16 V and + 0.2 V. The morphology of the coatings varied depending on the potential applied as observed by scanning electron microscopy. Alternate current methods were also used to synthesize Pt nanoparticles and compare the results with the traditional potentiostatic method. Different frequencies were used: 0.1, 1, 10, 100, 1000 and 10 000 Hz. Alternate current synthesis is more efficient than traditional potentiostatic methods, obtaining more electroactive coatings with less effective synthesis time. - Highlights: • Reduced graphene oxide has been obtained by electrochemical reduction on Pt wires. • Pt nanoparticles have been obtained potentiostatically at different potentials. • Pt nanoparticles have been obtained by ac methods with different frequencies. • ac synthesis is a better synthesis method than potentiostatic synthesis.

  15. Realist synthesis: illustrating the method for implementation research

    Directory of Open Access Journals (Sweden)

    Rycroft-Malone Jo

    2012-04-01

    Full Text Available Abstract Background Realist synthesis is an increasingly popular approach to the review and synthesis of evidence, which focuses on understanding the mechanisms by which an intervention works (or not. There are few published examples of realist synthesis. This paper therefore fills a gap by describing, in detail, the process used for a realist review and synthesis to answer the question ‘what interventions and strategies are effective in enabling evidence-informed healthcare?’ The strengths and challenges of conducting realist review are also considered. Methods The realist approach involves identifying underlying causal mechanisms and exploring how they work under what conditions. The stages of this review included: defining the scope of the review (concept mining and framework formulation; searching for and scrutinising the evidence; extracting and synthesising the evidence; and developing the narrative, including hypotheses. Results Based on key terms and concepts related to various interventions to promote evidence-informed healthcare, we developed an outcome-focused theoretical framework. Questions were tailored for each of four theory/intervention areas within the theoretical framework and were used to guide development of a review and data extraction process. The search for literature within our first theory area, change agency, was executed and the screening procedure resulted in inclusion of 52 papers. Using the questions relevant to this theory area, data were extracted by one reviewer and validated by a second reviewer. Synthesis involved organisation of extracted data into evidence tables, theming and formulation of chains of inference, linking between the chains of inference, and hypothesis formulation. The narrative was developed around the hypotheses generated within the change agency theory area. Conclusions Realist synthesis lends itself to the review of complex interventions because it accounts for context as well as

  16. Synthesis of ZnO nanorods-Au nanoparticles hybrids via in-situ plasma sputtering-assisted method for simultaneous electrochemical sensing of ascorbic acid and uric acid

    Energy Technology Data Exchange (ETDEWEB)

    Hou, Chao [College of Life Information Science & Instrument Engineering, Hangzhou Dianzi University, Hangzhou 310018 (China); Liu, Hongying, E-mail: liuhongying@hdu.edu.cn [College of Life Information Science & Instrument Engineering, Hangzhou Dianzi University, Hangzhou 310018 (China); State Key Laboratory of Analytical Chemistry for Life Science, School of Chemistry & Chemical Engineering, Nanjing University, Nanjing 210093 (China); Zhang, Dan; Yang, Chi [Department of Pharmacy, Nantong University, Nantong 226001 (China); Zhang, Mingzhen [College of Life Information Science & Instrument Engineering, Hangzhou Dianzi University, Hangzhou 310018 (China)

    2016-05-05

    In this study, ZnO nanorods-Au nanoparticles (ZnO NRs-Au NPs) hybrids were prepared using an in-situ plasma sputtering-assisted method without any template. Characterization results from scanning electron microscopy, high-resolution transmission electron microscopy, and energy dispersive X-ray spectroscopy showed that Au NPs are highly dispersed and tightly anchored on the surface of ZnO NRs. The size and surface coverage of Au NPs were well controlled by plasma sputtering time. Moreover, the hybrids exhibited excellent electrocatalytic properties towards oxidation of ascorbic acid (AA) and uric acid (UA) due to large surface area of Au NPs and ZnO NRs, and thus can be used as electrochemical sensors. Differential pulse voltammetry results showed that AA and UA could be detected simultaneously by ZnO NRs-Au NPs hybrids modified glassy carbon electrode. The linear ranges for AA and UA are 0.1 to 4 mM and 0.01 to 0.4 mM, respectively. The results suggest promising future applications in clinical diagnosis. - Highlights: • ZnO nanorods-Au nanoparticles were synthesized by in-situ plasma sputtering method. • Influence of sputtering time on the formation of Au nanoparticles was studied. • It exhibited a strong electrocatalytic activity toward the oxidation of ascorbic acid and uric acid. • A portable and cheap approach for simultaneous detection of ascorbic acid and uric acid was developed.

  17. Synthesis of ZnO nanorods-Au nanoparticles hybrids via in-situ plasma sputtering-assisted method for simultaneous electrochemical sensing of ascorbic acid and uric acid

    International Nuclear Information System (INIS)

    Hou, Chao; Liu, Hongying; Zhang, Dan; Yang, Chi; Zhang, Mingzhen

    2016-01-01

    In this study, ZnO nanorods-Au nanoparticles (ZnO NRs-Au NPs) hybrids were prepared using an in-situ plasma sputtering-assisted method without any template. Characterization results from scanning electron microscopy, high-resolution transmission electron microscopy, and energy dispersive X-ray spectroscopy showed that Au NPs are highly dispersed and tightly anchored on the surface of ZnO NRs. The size and surface coverage of Au NPs were well controlled by plasma sputtering time. Moreover, the hybrids exhibited excellent electrocatalytic properties towards oxidation of ascorbic acid (AA) and uric acid (UA) due to large surface area of Au NPs and ZnO NRs, and thus can be used as electrochemical sensors. Differential pulse voltammetry results showed that AA and UA could be detected simultaneously by ZnO NRs-Au NPs hybrids modified glassy carbon electrode. The linear ranges for AA and UA are 0.1 to 4 mM and 0.01 to 0.4 mM, respectively. The results suggest promising future applications in clinical diagnosis. - Highlights: • ZnO nanorods-Au nanoparticles were synthesized by in-situ plasma sputtering method. • Influence of sputtering time on the formation of Au nanoparticles was studied. • It exhibited a strong electrocatalytic activity toward the oxidation of ascorbic acid and uric acid. • A portable and cheap approach for simultaneous detection of ascorbic acid and uric acid was developed.

  18. Intermatrix Synthesis as a rapid, inexpensive and reproducible methodology for the in situ functionalization of nanostructured surfaces with quantum dots

    Energy Technology Data Exchange (ETDEWEB)

    Bastos-Arrieta, Julio, E-mail: julio.bastos@upc.edu [Department of Chemical Engineering, Universitat Politècnica de Catalunya, Av. Diagonal 647, 08028 Barcelona (Spain); Department of Chemistry, Universitat Autònoma de Barcelona, 08193 Barcelona (Spain); Muñoz, Jose, E-mail: josemaria.munoz@uab.cat [Department of Chemistry, Universitat Autònoma de Barcelona, 08193 Barcelona (Spain); Stenbock-Fermor, Anja, E-mail: stenbock@dwi.rwth-aachen.de [DWI – Leibniz-Institut für Interaktive Materialien, Aachen 52056 (Germany); Muñoz, Maria, E-mail: Maria.Munoz@uab.cat [Department of Chemistry, Universitat Autònoma de Barcelona, 08193 Barcelona (Spain); Muraviev, Dmitri N., E-mail: Dimitri.Muraviev@uab.es [Department of Chemistry, Universitat Autònoma de Barcelona, 08193 Barcelona (Spain); Céspedes, Francisco, E-mail: francisco.cespedes@uab.cat [Department of Chemistry, Universitat Autònoma de Barcelona, 08193 Barcelona (Spain); Tsarkova, Larisa A., E-mail: tsarkova@dwi.rwth-aachen.de [DWI – Leibniz-Institut für Interaktive Materialien, Aachen 52056 (Germany); Baeza, Mireia, E-mail: MariaDelMar.Baeza@uab.cat [Department of Chemistry, Universitat Autònoma de Barcelona, 08193 Barcelona (Spain)

    2016-04-15

    Graphical abstract: - Highlights: • Nanodiamond functionalization with CdS quantum dots. • Approach for carbon nanotube detection in water samples. • Simple functionalization of thin polymeric nanolayers with quantum dots. - Abstract: Intermatrix Synthesis (IMS) technique has proven to be a valid methodology for the in situ incorporation of quantum dots (QDs) in a wide range of nanostructured surfaces for the preparation of advanced hybrid-nanomaterials. In this sense, this communication reports the recent advances in the application of IMS for the synthesis of CdS-QDs with favourable distribution on sulfonated polyetherether ketone (SPEEK) membrane thin films (TFs), multiwall carbon nanotubes (MWCNTs) and nanodiamonds (NDs). The synthetic route takes advantage of the ion exchange functionality of the reactive surfaces for the loading of the QDs precursor and consequent QDs appearance by precipitation. The benefits of such modified nanomaterials were studied using CdS-QDs@MWCNTs hybrid-nanomaterials. CdS-QDs@MWCNTs has been used as conducting filler for the preparation of electrochemical nanocomposite sensors, which present electrocatalytic properties. Finally, the optical properties of the QDs contained on MWCNTs could allow a new procedure for the analytical detection of nanostructured carbon allotropes in water.

  19. Intermatrix Synthesis as a rapid, inexpensive and reproducible methodology for the in situ functionalization of nanostructured surfaces with quantum dots

    International Nuclear Information System (INIS)

    Bastos-Arrieta, Julio; Muñoz, Jose; Stenbock-Fermor, Anja; Muñoz, Maria; Muraviev, Dmitri N.; Céspedes, Francisco; Tsarkova, Larisa A.; Baeza, Mireia

    2016-01-01

    Graphical abstract: - Highlights: • Nanodiamond functionalization with CdS quantum dots. • Approach for carbon nanotube detection in water samples. • Simple functionalization of thin polymeric nanolayers with quantum dots. - Abstract: Intermatrix Synthesis (IMS) technique has proven to be a valid methodology for the in situ incorporation of quantum dots (QDs) in a wide range of nanostructured surfaces for the preparation of advanced hybrid-nanomaterials. In this sense, this communication reports the recent advances in the application of IMS for the synthesis of CdS-QDs with favourable distribution on sulfonated polyetherether ketone (SPEEK) membrane thin films (TFs), multiwall carbon nanotubes (MWCNTs) and nanodiamonds (NDs). The synthetic route takes advantage of the ion exchange functionality of the reactive surfaces for the loading of the QDs precursor and consequent QDs appearance by precipitation. The benefits of such modified nanomaterials were studied using CdS-QDs@MWCNTs hybrid-nanomaterials. CdS-QDs@MWCNTs has been used as conducting filler for the preparation of electrochemical nanocomposite sensors, which present electrocatalytic properties. Finally, the optical properties of the QDs contained on MWCNTs could allow a new procedure for the analytical detection of nanostructured carbon allotropes in water.

  20. Study of Colloidal Gold Synthesis Using Turkevich Method

    Science.gov (United States)

    Rohiman, Asep; Anshori, Isa; Surawijaya, Akhmadi; Idris, Irman

    2011-12-01

    The synthesis of colloidal gold or Au-nanoparticles (Au-NPs) by reduction of chloroauric acid (HAuCl4) with sodium citrate was done using Turkevich method. We prepare HAuCl4 solution by dissolving gold wires (99.99%) into aqua regia solution. To initiate the Au-NPs synthesis 0.17 ml of 1 % chloroauric acid solution was heated to the boiling point and then 10 ml of 1 % sodium citrate was added to the boiling solution with a constant stirring in order to maintain a homogenous solution. A color of faint gray was observed in the solution approximately one minute and in a period of 2-3 minutes later, it further darkened to deep wine and red color. It showed that the gold solution has reduced to Au-NPs. The effect of process temperature on the size of Au-NPs prepared by sodium citrate reduction has also been investigated. With increasing temperature of Au-NPs synthesis, smaller-size Au-NPs were obtained. The higher temperatures shorten the time needed to achieve activation energy for reduction process. The resulting Au-NPs has been characterized by scanning Electron Microscope (SEM), showing the size of Au-NPs average diameter is ˜20-27 nm. The resulting colloidal gold will be used as catalyst for Si nanowires growth using VLS method.

  1. Synthesis of nanocrystalline Y2O3 in a specially designed atmospheric pressure radio frequency thermal plasma reactor

    International Nuclear Information System (INIS)

    Dhamale, G. D.; Mathe, V. L.; Bhoraskar, S. V.; Sahasrabudhe, S. N.; Ghorui, S.

    2015-01-01

    Synthesis of yttrium oxide nanoparticles in a specially designed radio frequency thermal plasma reactor is reported. Good crystallinity, narrow size distribution, low defect state concentration, high purity, good production rate, single-step synthesis, and simultaneous formation of nanocrystalline monoclinic and cubic phases are some of the interesting features observed. Synthesized particles are characterized through X-ray diffraction, transmission electron microscopy, scanning electron microscopy, Fourier transform infrared spectroscopy, thermo-luminescence (TL), and Brunauer–Emmett–Teller surface area analysis. Polymorphism of the nanocrystalline yttria is addressed in detail. Synthesis mechanism is explored through in-situ emission spectroscopy. Post-synthesis environmental effects and possible methods to eliminate the undesired phases are probed. Defect states are investigated through the study of TL spectra

  2. Unscheduled DNA synthesis after β-irradiation of mouse skin in situ

    International Nuclear Information System (INIS)

    Ootsuyama, Akira; Tanooka, Hiroshi

    1986-01-01

    The skin of ICR mouse was irradiated with β-rays from 90 Sr- 90 Y with surface doses up to 30 krad. Unscheduled DNA synthesis (UDS) was measured by autoradiography after labeling the skin with radioactive thymidine using the forceps-clamping method. The level of UDS in epithelial cells of the skin was detected as an increasing function of radiation dose. Fibroblastic cells, compared with epithelial cells and hair follicle cells at the same depth of the skin, showed a lower level of UDS, indicating a lower DNA repair activity in fibroblasts. Cancer risk of the skin was discussed. (Auth.)

  3. A direct method for the synthesis of orthogonally protected furyl- and thienyl- amino acids.

    Science.gov (United States)

    Hudson, Alex S; Caron, Laurent; Colgin, Neil; Cobb, Steven L

    2015-04-01

    The synthesis of unnatural amino acids plays a key part in expanding the potential application of peptide-based drugs and in the total synthesis of peptide natural products. Herein, we report a direct method for the synthesis of orthogonally protected 5-membered heteroaromatic amino acids.

  4. One-Pot Microwave-Assisted Synthesis of Graphene/Layered Double Hydroxide (LDH) Nanohybrids

    Institute of Scientific and Technical Information of China (English)

    Sunil P Lonkar; Jean-Marie Raquez; Philippe Dubois

    2015-01-01

    A facile and rapid method to synthesize graphene/layered double hydroxide (LDH) nanohybrids by a micro-wave technique is demonstrated. The synthesis procedure involves hydrothermal crystallization of Zn–Al LDH at the same time in situ reduction of graphene oxide (GO) to graphene. The microstructure, composition, and morphology of the resulting graphene/LDH nanohybrids were characterized. The results confirmed the formation of nanohybrids and the reduction of graphene oxide. The growth mechanism of LDH and in situ reduction of GO were discussed. The LDH sheet growth was found to prevent the scrolling of graphene layers in resulting hybrids. The electrochemical properties exhibit superior performance for graphene/Zn–Al LDH hybrids over pristine graphene. The present approach may open a strategy in hybridizing graphene with multimetallic nano-oxides and hydroxides using microwave method.

  5. One-Pot Microwave-Assisted Synthesis of Graphene/Layered Double Hydroxide(LDH) Nanohybrids

    Institute of Scientific and Technical Information of China (English)

    Sunil P.Lonkar; Jean-Marie Raquez; Philippe Dubois

    2015-01-01

    A facile and rapid method to synthesize graphene/layered double hydroxide(LDH)nanohybrids by a microwave technique is demonstrated.The synthesis procedure involves hydrothermal crystallization of Zn–Al LDH at the same time in situ reduction of graphene oxide(GO)to graphene.The microstructure,composition,and morphology of the resulting graphene/LDH nanohybrids were characterized.The results confirmed the formation of nanohybrids and the reduction of graphene oxide.The growth mechanism of LDH and in situ reduction of GO were discussed.The LDH sheet growth was found to prevent the scrolling of graphene layers in resulting hybrids.The electrochemical properties exhibit superior performance for graphene/Zn–Al LDH hybrids over pristine graphene.The present approach may open a strategy in hybridizing graphene with multimetallic nano-oxides and hydroxides using microwave method.

  6. Method for innovative synthesis-design of chemical process flowsheets

    DEFF Research Database (Denmark)

    Kumar Tula, Anjan; Gani, Rafiqul

    Chemical process synthesis-design involve the identification of the processing route to reach a desired product from a specified set of raw materials, design of the operations involved in the processing route, the calculations of utility requirements, the calculations of waste and emission...... to the surrounding and many more. Different methods (knowledge-based [1], mathematical programming [2], hybrid, etc.) have been proposed and are also currently employed to solve these synthesis-design problems. D’ Anterroches [3] proposed a group contribution based approach to solve the synthesis-design problem...... of chemical processes, where, chemical process flowsheets could be synthesized in the same way as atoms or groups of atoms are synthesized to form molecules in computer aided molecular design (CAMD) techniques [4]. That, from a library of building blocks (functional process-groups) and a set of rules to join...

  7. Simple Synthesis Method for Alumina Nanoparticle

    Directory of Open Access Journals (Sweden)

    Daniel Damian

    2017-11-01

    Full Text Available Globally, the human population steady increase, expansion of urban areas, excessive industrialization including in agriculture, caused not only decrease to depletion of non-renewable resources, a rapid deterioration of the environment with negative impact on water quality, soil productivity and of course quality of life in general. This paper aims to prepare size controlled nanoparticles of aluminum oxide using a simple synthesis method. The morphology and dimensions of nanomaterial was investigated using modern analytical techniques: SEM/EDAX and XRD spectroscopy.

  8. Origins, Methods and Advances in Qualitative Meta-Synthesis

    Science.gov (United States)

    Nye, Elizabeth; Melendez-Torres, G. J.; Bonell, Chris

    2016-01-01

    Qualitative research is a broad term encompassing many methods. Critiques of the field of qualitative research argue that while individual studies provide rich descriptions and insights, the absence of connections drawn between studies limits their usefulness. In response, qualitative meta-synthesis serves as a design to interpret and synthesise…

  9. Method for in situ determination cation exchange capacities of subsurface formations

    International Nuclear Information System (INIS)

    Fertl, W.H.; Welker, D.W.

    1980-01-01

    A method is disclosed for the in situ examination of each subsurface formation penetrated by a borehole to ascertain the cation exchange capacity of such formations within a geological region. Natural γ ray logging is used to develop signals functionally related to the total γ radiation and to the potassium-40, uranium and thorium energy-band radiations. A first borehole is traversed by a potential γ ray spectrometer to provide selected measurements of natural γ radiation. Core samples are taken from the logged formation and laboratory tests performed to determine the cation exchange capacity thereof. The cation exchange capacities thus are developed then correlated with selected parameters provided by the γ ray spectrometer to establish functional relationships. Cation exchange capacities of formations in subsequent boreholes within the region are then determined in situ by use of the natural γ ray spectrometer and these established relationships. (author)

  10. Synthesis method of asymmetric gold particles.

    Science.gov (United States)

    Jun, Bong-Hyun; Murata, Michael; Hahm, Eunil; Lee, Luke P

    2017-06-07

    Asymmetric particles can exhibit unique properties. However, reported synthesis methods for asymmetric particles hinder their application because these methods have a limited scale and lack the ability to afford particles of varied shapes. Herein, we report a novel synthetic method which has the potential to produce large quantities of asymmetric particles. Asymmetric rose-shaped gold particles were fabricated as a proof of concept experiment. First, silica nanoparticles (NPs) were bound to a hydrophobic micro-sized polymer containing 2-chlorotritylchloride linkers (2-CTC resin). Then, half-planar gold particles with rose-shaped and polyhedral structures were prepared on the silica particles on the 2-CTC resin. Particle size was controlled by the concentration of the gold source. The asymmetric particles were easily cleaved from the resin without aggregation. We confirmed that gold was grown on the silica NPs. This facile method for synthesizing asymmetric particles has great potential for materials science.

  11. An in-situ measuring method for planar straightness error

    Science.gov (United States)

    Chen, Xi; Fu, Luhua; Yang, Tongyu; Sun, Changku; Wang, Zhong; Zhao, Yan; Liu, Changjie

    2018-01-01

    According to some current problems in the course of measuring the plane shape error of workpiece, an in-situ measuring method based on laser triangulation is presented in this paper. The method avoids the inefficiency of traditional methods like knife straightedge as well as the time and cost requirements of coordinate measuring machine(CMM). A laser-based measuring head is designed and installed on the spindle of a numerical control(NC) machine. The measuring head moves in the path planning to measure measuring points. The spatial coordinates of the measuring points are obtained by the combination of the laser triangulation displacement sensor and the coordinate system of the NC machine, which could make the indicators of measurement come true. The method to evaluate planar straightness error adopts particle swarm optimization(PSO). To verify the feasibility and accuracy of the measuring method, simulation experiments were implemented with a CMM. Comparing the measurement results of measuring head with the corresponding measured values obtained by composite measuring machine, it is verified that the method can realize high-precise and automatic measurement of the planar straightness error of the workpiece.

  12. Facile synthesis of AgCl/polydopamine/Ag nanoparticles with in-situ laser improving Raman scattering effect

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Yan; Zhang, Wenqi; Wang, Lin; Wang, Feng, E-mail: wangfeng@shnu.edu.cn; Yang, Haifeng

    2017-01-15

    Highlights: • AgCl/PDA/AgNPs (polydopamine (PDA) adlayer covered cubic AgCl core inlaid with Ag nanoparticles (AgNPs)) was fabricated for in-situ SERS detection. • Such SERS substrate shows in-situ laser improving Raman scattering effect due to the generation of more AgNPs. • Enhancement factor could reach 10{sup 7}. • Such SERS substrate shows good reproducibility and long term stability. - Abstract: We reported a simple and fast method to prepare a composite material of polydopamine (PDA) adlayer covered cubic AgCl core, which was inlaid with Ag nanoparticles (NPs), shortly named as AgCl/PDA/AgNPs. The resultant AgCl/PDA/AgNPs could be employed as surface-enhanced Raman scattering (SERS) substrate for in-situ detection and the SERS activity could be further greatly improved due to the production of more AgNPs upon laser irradiation. With 4-mercaptopyridine (4-Mpy) as the probe molecule, the enhancement factor could reach 10{sup 7}. Additionally, such SERS substrate shows good reproducibility with relative standard deviation of 7.32% and long term stability (after storage for 100 days under ambient condition, SERS intensity decay is less than 25%). In-situ elevating SERS activity of AgCl/PDA/AgNPs induced by laser may be beneficial to sensitive analysis in practical fields.

  13. Universal chitosan-assisted synthesis of Ag-including heterostructured nanocrystals for label-free in situ SERS monitoring.

    Science.gov (United States)

    Cai, Kai; Xiao, Xiaoyan; Zhang, Huan; Lu, Zhicheng; Liu, Jiawei; Li, Qin; Liu, Chen; Foda, Mohamed F; Han, Heyou

    2015-12-07

    A universal chitosan-assisted method was developed to synthesize various Ag-including heterostructured nanocrystals, in which chelation probably plays a vital role. The as-prepared Ag/Pd heterostructured nanocrystals show outstanding properties when used as bifunctional nanocomposites in label-free in situ SERS monitoring of Pd-catalyzed reaction.

  14. In-Situ Synchrotron X-ray Study of the Phase and Texture Evolution of Ceria and Superconductor Films Deposited by Chemical Solution Method

    DEFF Research Database (Denmark)

    Yue, Zhao; Grivel, Jean-Claude; He, Dong

    2012-01-01

    In situ synchrotron x-ray diffraction is used to study the phase and texture formation of ceria based films and superconductor films deposited by the chemical solution method on technical substrates. Combined analysis using in situ synchrotron x-ray diffraction, thermogravimetry/differential ther......In situ synchrotron x-ray diffraction is used to study the phase and texture formation of ceria based films and superconductor films deposited by the chemical solution method on technical substrates. Combined analysis using in situ synchrotron x-ray diffraction, thermogravimetry...

  15. In situ growth of metal particles on 3D urchin-like WO3 nanostructures.

    Science.gov (United States)

    Xi, Guangcheng; Ye, Jinhua; Ma, Qiang; Su, Ning; Bai, Hua; Wang, Chao

    2012-04-18

    Metal/semiconductor hybrid materials of various sizes and morphologies have many applications in areas such as catalysis and sensing. Various organic agents are necessary to stabilize metal nanoparticles during synthesis, which leads to a layer of organic compounds present at the interfaces between the metal particles and the semiconductor supports. Generally, high-temperature oxidative treatment is used to remove the organics, which can extensively change the size and morphology of the particles, in turn altering their activity. Here we report a facile method for direct growth of noble-metal particles on WO(3) through an in situ redox reaction between weakly reductive WO(2.72) and oxidative metal salts in aqueous solution. This synthetic strategy has the advantages that it takes place in one step and requires no foreign reducing agents, stabilizing agents, or pretreatment of the precursors, making it a practical method for the controlled synthesis of metal/semiconductor hybrid nanomaterials. This synthetic method may open up a new way to develop metal-nanoparticle-loaded semiconductor composites. © 2012 American Chemical Society

  16. Novel in-situ lamella fabrication technique for in-situ TEM.

    Science.gov (United States)

    Canavan, Megan; Daly, Dermot; Rummel, Andreas; McCarthy, Eoin K; McAuley, Cathal; Nicolosi, Valeria

    2018-03-29

    In-situ transmission electron microscopy is rapidly emerging as the premier technique for characterising materials in a dynamic state on the atomic scale. The most important aspect of in-situ studies is specimen preparation. Specimens must be electron transparent and representative of the material in its operational state, amongst others. Here, a novel fabrication technique for the facile preparation of lamellae for in-situ transmission electron microscopy experimentation using focused ion beam milling is developed. This method involves the use of rotating microgrippers during the lift-out procedure, as opposed to the traditional micromanipulator needle and platinum weld. Using rotating grippers, and a unique adhesive substance, lamellae are mounted onto a MEMS device for in-situ TEM annealing experiments. We demonstrate how this technique can be used to avoid platinum deposition as well as minimising damage to the MEMS device during the thinning process. Our technique is both a cost effective and readily implementable alternative to the current generation of preparation methods for in-situ liquid, electrical, mechanical and thermal experimentation within the TEM as well as traditional cross-sectional lamella preparation. Copyright © 2018 Elsevier B.V. All rights reserved.

  17. One-pot in situ redox synthesis of hexacyanoferrate/conductive polymer hybrids as lithium-ion battery cathodes.

    Science.gov (United States)

    Wong, Min Hao; Zhang, Zixuan; Yang, Xianfeng; Chen, Xiaojun; Ying, Jackie Y

    2015-09-14

    An efficient and adaptable method is demonstrated for the synthesis of lithium hexacyanoferrate/conductive polymer hybrids for Li-ion battery cathodes. The hybrids were synthesized via a one-pot method, involving a redox-coupled reaction between pyrrole monomers and the Li3Fe(CN)6 precursor. The hybrids showed much better cyclability relative to reported Prussian Blue (PB) analogs.

  18. Size-controlled in situ synthesis and photo-responsive properties of silver/poly(methyl methacrylate) nanocomposite films with high silver content

    Energy Technology Data Exchange (ETDEWEB)

    Chen Cheng; Li Junguo [State Key Laboratory of Advanced Technology for Materials Synthesis and Processing, Wuhan University of Technology, Wuhan 430070 (China); Luo Guoqiang, E-mail: qhy2013@163.com [State Key Laboratory of Advanced Technology for Materials Synthesis and Processing, Wuhan University of Technology, Wuhan 430070 (China); Xiong Yuanlu; Zhang Qiang; Shen Lianmeng [State Key Laboratory of Advanced Technology for Materials Synthesis and Processing, Wuhan University of Technology, Wuhan 430070 (China)

    2012-10-01

    Highlights: Black-Right-Pointing-Pointer Ag/PMMA nanocomposite films with high silver content are prepared by in situ synthesis. Black-Right-Pointing-Pointer The size of Ag nanoparticles can be controlled by reaction time. Black-Right-Pointing-Pointer The electrical properties of Ag/PMMA nanocomposites films shows enhancement compared with the pure PMMA. Black-Right-Pointing-Pointer The recycle photo-responsive properties of Ag/PMMA nanocomposite films are proposed. - Abstract: Ag/PMMA nanocomposites have attracted much attention due to its superior mechanical, optical and electrical properties. In this article, Ag/PMMA nanocomposite films with high silver content (20 wt%) have been successfully in situ synthesized. UV-vis analysis, transmission electron microscopy (TEM), current-voltage (I-V) analysis, hall effect measurement system and electrochemical workstation are used to characterize the nanocomposite films. The results reveal that silver nanoparticles (NPs) homogeneously distribute in PMMA films and the particles size of silver NPs which has been controlled from 1.68 to 6.98 nm. Ag/PMMA nanocomposite films show electrical properties due to the conduction paths created by Ag nanoparticles. With the increasing diameter of silver NPs, the current density decreases and resistivity increases, respectively. Photo-responsive properties of Ag/PMMA nanocomposite films indicate that conduction paths could be destroyed by illumination and rebuilt in dark condition.

  19. Size-controlled in situ synthesis and photo-responsive properties of silver/poly(methyl methacrylate) nanocomposite films with high silver content

    International Nuclear Information System (INIS)

    Chen Cheng; Li Junguo; Luo Guoqiang; Xiong Yuanlu; Zhang Qiang; Shen Lianmeng

    2012-01-01

    Highlights: ► Ag/PMMA nanocomposite films with high silver content are prepared by in situ synthesis. ► The size of Ag nanoparticles can be controlled by reaction time. ► The electrical properties of Ag/PMMA nanocomposites films shows enhancement compared with the pure PMMA. ► The recycle photo-responsive properties of Ag/PMMA nanocomposite films are proposed. - Abstract: Ag/PMMA nanocomposites have attracted much attention due to its superior mechanical, optical and electrical properties. In this article, Ag/PMMA nanocomposite films with high silver content (20 wt%) have been successfully in situ synthesized. UV–vis analysis, transmission electron microscopy (TEM), current–voltage (I–V) analysis, hall effect measurement system and electrochemical workstation are used to characterize the nanocomposite films. The results reveal that silver nanoparticles (NPs) homogeneously distribute in PMMA films and the particles size of silver NPs which has been controlled from 1.68 to 6.98 nm. Ag/PMMA nanocomposite films show electrical properties due to the conduction paths created by Ag nanoparticles. With the increasing diameter of silver NPs, the current density decreases and resistivity increases, respectively. Photo-responsive properties of Ag/PMMA nanocomposite films indicate that conduction paths could be destroyed by illumination and rebuilt in dark condition.

  20. How the Elderly Can Use Scientific Knowledge to Solve Problems While Designing Toys: A Retrospective Analysis of the Design of a Working UFO

    Science.gov (United States)

    Chen, Mei-Yung; Hong, Jon-Chao; Hwang, Ming-Yueh; Wong, Wan-Tzu

    2013-01-01

    The venerable aphorism "an old dog cannot learn new tricks" implies that the elderly rarely learn anything new--in particular, scientific knowledge. On the basis of "learning by doing," the present study emphasized knowledge application (KA) as elderly subjects collaborated on the design of a toy flying saucer (UFO). Three…

  1. Facile, low temperature synthesis of SnO_2/reduced graphene oxide nanocomposite as anode material for lithium-ion batteries

    International Nuclear Information System (INIS)

    Hou, Chau-Chung; Brahma, Sanjaya; Weng, Shao-Chieh; Chang, Chia-Chin; Huang, Jow-Lay

    2017-01-01

    Highlights: • Facile, one-pot, low temperature synthesis of SnO_2-RGO composite. • In-situ reduction of graphene oxide and growth of SnO_2 nanoparticle. • Concentration of reductant during synthesis affects the properties significantly. • SnO_2-RGO composite shows good rate capability and stable capacitance. • Synthesis method is energy efficient and scalable for other metal oxides. - Abstract: We demonstrate a facile, single step, low temperature and energy efficient strategy for the synthesis of SnO_2-reduced graphene oxide (RGO) nanocomposite where the crystallization of SnO_2 nanoparticles and the reduction of graphene oxide takes place simultaneously by an in situ chemical reduction process. The electrochemical property of the SnO_2-RGO composite prepared by using low concentrations of reducing agent shows better Li storage performance, good rate capability (378 mAh g"−"1 at 3200 mA g"−"1) and stable capacitance (522 mAh g"−"1 after 50 cycles). Increasing the reductant concentration lead to crystallization of high concentration of SnO_2 nanoparticle aggregation and degrade the Li ion storage property.

  2. Ion transport membrane reactor systems and methods for producing synthesis gas

    Science.gov (United States)

    Repasky, John Michael

    2015-05-12

    Embodiments of the present invention provide cost-effective systems and methods for producing a synthesis gas product using a steam reformer system and an ion transport membrane (ITM) reactor having multiple stages, without requiring inter-stage reactant injections. Embodiments of the present invention also provide techniques for compensating for membrane performance degradation and other changes in system operating conditions that negatively affect synthesis gas production.

  3. Systematic process synthesis and design methods for cost effective waste minimization

    International Nuclear Information System (INIS)

    Biegler, L.T.; Grossman, I.E.; Westerberg, A.W.

    1995-01-01

    We present progress on our work to develop synthesis methods to aid in the design of cost effective approaches to waste minimization. Work continues to combine the approaches of Douglas and coworkers and of Grossmann and coworkers on a hierarchical approach where bounding information allows it to fit within a mixed integer programming approach. We continue work on the synthesis of reactors and of flexible separation processes. In the first instance, we strive for methods we can use to reduce the production of potential pollutants, while in the second we look for ways to recover and recycle solvents

  4. Systematic process synthesis and design methods for cost effective waste minimization

    Energy Technology Data Exchange (ETDEWEB)

    Biegler, L.T.; Grossman, I.E.; Westerberg, A.W. [Carnegie Mellon Univ., Pittsburgh, PA (United States)

    1995-12-31

    We present progress on our work to develop synthesis methods to aid in the design of cost effective approaches to waste minimization. Work continues to combine the approaches of Douglas and coworkers and of Grossmann and coworkers on a hierarchical approach where bounding information allows it to fit within a mixed integer programming approach. We continue work on the synthesis of reactors and of flexible separation processes. In the first instance, we strive for methods we can use to reduce the production of potential pollutants, while in the second we look for ways to recover and recycle solvents.

  5. A general method for synthesis continuous silver nanoshells on dielectric colloids

    International Nuclear Information System (INIS)

    Chen Dong; Liu Huiyu; Liu Jianshu; Ren Xianglin; Meng Xianwei; Wu Wei; Tang Fangqiong

    2008-01-01

    A method for the controlled synthesis of silver nanoshells on various dielectric colloids, such as silica and polystyrene is presented in this study. The complexation of triethanolamine and silver ions is applied here to moderate the availability of the silver ions in the reaction solution, which directly affect the coating process. The morphologies of the particles were studied with transmission electron microscopy and their crystallinity and chemical composition were confirmed by X-ray and electron diffraction. The synthesis conditions were investigated and experimental results show that compact silver shells with easily controlled thickness can be deposited on dielectric cores by this method

  6. Current status and future directions for in situ transmission electron microscopy

    DEFF Research Database (Denmark)

    Taheri, Mitra L.; Stach, Eric A.; Arslan, Ilke

    2016-01-01

    This review article discusses the current and future possibilities for the application of in situ transmission electron microscopy to reveal synthesis pathways and functional mechanisms in complex and nanoscale materials. The findings of a group of scientists, representing academia, government labs...

  7. Novel method for synthesis of silver nanoparticles and their application on wool

    Energy Technology Data Exchange (ETDEWEB)

    Boroumand, Majid Nasiri [Shahid Bahonar University of Kerman, Kerman (Iran, Islamic Republic of); Montazer, Majid [Amirkabir University of Technology, Tehran (Iran, Islamic Republic of); Simon, Frank [Leibniz-Institut für Polymerforschung Dresden e.V., Dresden (Germany); Liesiene, Jolanta [Faculty of Chemical Technology, Kaunas University of Technology, Kaunas (Lithuania); Šaponjic, Zoran [Vinča Institute of Nuclear Sciences, University of Belgrade, Belgrade (Serbia); Dutschk, Victoria, E-mail: v.dutschk@utwente.nl [Faculty of Engineering Technology, University of Twente, Enschede (Netherlands)

    2015-08-15

    Graphical abstract: Tentative mechanism for reduction of Ag{sup +} by polyphenols having two hydroxy groups in ortho-position – the use of silver nanoparticles and an aqueous solution of extracted dye from Pomegranate peel as a reducing agent for synthesis silver nanoparticles from silver nitrate. - Highlights: • A new method for the synthesis of silver nanoparticles suitable to impart antibacterial properties of wool fabric proposed. • Silver nanopartilces were synthesized by a biochemical reduction method. • An aqueous solution of extracted dye from Pomegranate peel was used as a reducing agent for synthesis of silver nanoparticles from silver nitrate. - Abstract: In this study, a new method for the synthesis of silver nanoparticles (AgNPs) suitable to impart antibacterial properties of wool fabric is proposed. AgNPs were synthesized by a biochemical reduction method. An aqueous solution of extracted dye from Pomegranate peel was used as a reducing agent for the synthesis of AgNPs from silver nitrate. The ratio of dye to silver nitrate concentration (R{sub Dye}/{sub Ag} = [Dye]/[AgNO{sub 3}]) is the influencing factor in the synthesis of silver nanoparticles. The nanoparticles formation was followed by UV/Vis absorption spectroscopy. The size and shape of AgNPs were studied by transmission electron microscopy (TEM). The size distribution and Zetapotential of nanoparticles were evaluated using diffraction light scattering (DLS) measurements. The antibacterial potential of biosynthesized silver nanoparticles against Escherichia coli (E. coli) was examined qualitatively and quantitatively. Kinetic analysis of the bacteria reduction using AgNPs synthesized in different way was performed. AgNPs were applied on wool fabrics by exhaustion. The changes in surface morphology of wool fibers after AgNPs loading were studied using scanning electron microscopy (SEM). The amounts of silver deposited on wool fabrics at different pH and temperature were compared applying

  8. Novel method for synthesis of silver nanoparticles and their application on wool

    International Nuclear Information System (INIS)

    Boroumand, Majid Nasiri; Montazer, Majid; Simon, Frank; Liesiene, Jolanta; Šaponjic, Zoran; Dutschk, Victoria

    2015-01-01

    Graphical abstract: Tentative mechanism for reduction of Ag + by polyphenols having two hydroxy groups in ortho-position – the use of silver nanoparticles and an aqueous solution of extracted dye from Pomegranate peel as a reducing agent for synthesis silver nanoparticles from silver nitrate. - Highlights: • A new method for the synthesis of silver nanoparticles suitable to impart antibacterial properties of wool fabric proposed. • Silver nanopartilces were synthesized by a biochemical reduction method. • An aqueous solution of extracted dye from Pomegranate peel was used as a reducing agent for synthesis of silver nanoparticles from silver nitrate. - Abstract: In this study, a new method for the synthesis of silver nanoparticles (AgNPs) suitable to impart antibacterial properties of wool fabric is proposed. AgNPs were synthesized by a biochemical reduction method. An aqueous solution of extracted dye from Pomegranate peel was used as a reducing agent for the synthesis of AgNPs from silver nitrate. The ratio of dye to silver nitrate concentration (R Dye / Ag = [Dye]/[AgNO 3 ]) is the influencing factor in the synthesis of silver nanoparticles. The nanoparticles formation was followed by UV/Vis absorption spectroscopy. The size and shape of AgNPs were studied by transmission electron microscopy (TEM). The size distribution and Zetapotential of nanoparticles were evaluated using diffraction light scattering (DLS) measurements. The antibacterial potential of biosynthesized silver nanoparticles against Escherichia coli (E. coli) was examined qualitatively and quantitatively. Kinetic analysis of the bacteria reduction using AgNPs synthesized in different way was performed. AgNPs were applied on wool fabrics by exhaustion. The changes in surface morphology of wool fibers after AgNPs loading were studied using scanning electron microscopy (SEM). The amounts of silver deposited on wool fabrics at different pH and temperature were compared applying energy

  9. Gaining Control over Radiolytic Synthesis of Uniform Sub-3-nanometer Palladium Nanoparticles: Use of Aromatic Liquids in the Electron Microscope

    Energy Technology Data Exchange (ETDEWEB)

    Abellan Baeza, Patricia; Parent, Lucas R.; Al Hasan, Naila M.; Park, Chiwoo; Arslan, Ilke; Karim, Ayman M.; Evans, James E.; Browning, Nigel D.

    2016-01-07

    Synthesizing nanomaterials of uniform shape and size is of critical importance to access and manipulate the novel structure-property relationships arising at the nanoscale. In this work we synthesize Pd nanoparticles with well-controlled size using in situ liquid-stage scanning transmission electron microscopy (STEM) and demonstrate a match between the reaction kinetics and products of the radiolytic and chemical syntheses of size-stabilized Pd nanoparticles. We quantify the effect of electron dose on the nucleation kinetics, and compare these results with in situ small angle X-ray scattering (SAXS) experiments investigating the effect of temperature during chemical synthesis. This work introduces methods for precise control of nanoparticle synthesis in the STEM and provides a means to uncover the fundamental processes behind the size and shape stabilization of nanoparticles.

  10. Synthesis and Characterization of WO3/Graphene Nanocomposites for Enhanced Photocatalytic Activities by One-Step In-Situ Hydrothermal Reaction

    Directory of Open Access Journals (Sweden)

    Xiaoxiao Hu

    2018-01-01

    Full Text Available Tungsten trioxide (WO3 nanorods are synthesized on the surface of graphene (GR sheets by using a one-step in-situ hydrothermal method employing sodium tungstate (Na2WO4·2H2O and graphene oxide (GO as precursors. The resulting WO3/GR nanocomposites are characterized by X-ray diffraction, Raman spectroscopy, transmission electron microscopy, scanning electron microscopy and X-ray photoelectron spectroscopy. The results confirm that the interface between WO3 nanorod and graphene contains chemical bonds. The enhanced optical absorption properties are measured by UV-vis diffuse reflectance spectra. The photocatalytic activity of the WO3/GR nanocomposites under visible light is evaluated by the photodegradation of methylene blue, where the degradation rate of WO3/GR nanocomposites is shown to be double that of pure WO3. This is attributed to the synergistic effect of graphene and the WO3 nanorod, which greatly enhances the photocatalytic performance of the prepared sample, reduces the recombination of the photogenerated electron-hole pairs and increases the visible light absorption efficiency. Finally, the photocatalytic mechanism of the WO3/GR nanocomposites is presented. The synthesis of the prepared sample is convenient, direct and environmentally friendly. The study reports a highly efficient composite photocatalyst for the degradation of contaminants that can be applied to cleaning up the environment.

  11. Measuring Protein Synthesis Rate In Living Object Using Flooding Dose And Constant Infusion Methods

    OpenAIRE

    Ulyarti, Ulyarti

    2018-01-01

    Constant infusion is a method used for measuring protein synthesis rate in living object which uses low concentration of amino acid tracers. Flooding dose method is another technique used to measure the rate of protein synthesis which uses labelled amino acid together with large amount of unlabelled amino acid.  The latter method was firstly developed to solve the problem in determination of precursor pool arise from constant infusion method.  The objective of this writing is to com...

  12. METHODS OF SYNTHESIS EIGHT-TELLURIUM-CONTAINING HETEROCYCLES WITH MORE HETEROATOMS

    Directory of Open Access Journals (Sweden)

    G. M. Abakarov

    2013-01-01

    Full Text Available In this article systematized and summarized data on the synthesis of neweight-embered tellurium-containing heterocycles and new preparative methods described above produce heterocyclic tellurium.

  13. Synthesis of titanium carbide from wood by self-propagating high temperature synthesis

    Directory of Open Access Journals (Sweden)

    Sutham Niyomwas

    2010-05-01

    Full Text Available Titanium carbide (TiC particles were obtained in situ by a self-propagating high temperature synthesis (SHS of wooddust with TiO2 and Mg. The reaction was carried out in a SHS reactor under static argon gas at the pressure of 0.5 MPa. Thestandard Gibbs energy minimization method was used to calculate the equilibrium composition of the reacting species. Theeffects of increasing Mg mole ratio to the precursor mixture of TiO2 and wood dusts were investigated. XRD and SEManalyses indicate a complete reaction of the precursors to yield TiC-MgO as a product composite. The synthesized compositeswere leached with 0.1M HCl acid solution to obtain TiC particles as final products.

  14. Duality of solar UV-B radiation and relevant dosimetry: vitamin D synthesis versus skin erythema

    Science.gov (United States)

    Terenetskaya, Irina P.

    2003-06-01

    Solar ultraviolet radiation (UVR) gives rise to beneficial or adverse health effects depending on the dose. Excessive UV exposures are associated with acute and chronic health effect but in appropriate doses UV sunlight is advisable. Important biological function of UVR is initiation of endogenous synthesis of vitamin D in human skin. A useful method based on an in vitro model of vitamin D synthesis ('D-dosimeter') has been specially developed to measure the vitamin D synthetic capacity of sunlight in situ. For the first time laboratory and field tests have been performed to link commonly used erythemal units (MEDs) and previtamin D accumulation.

  15. Evaluation of Methods for In-Situ Calibration of Field-Deployable Microphone Phased Arrays

    Science.gov (United States)

    Humphreys, William M.; Lockard, David P.; Khorrami, Mehdi R.; Culliton, William G.; McSwain, Robert G.

    2017-01-01

    Current field-deployable microphone phased arrays for aeroacoustic flight testing require the placement of hundreds of individual sensors over a large area. Depending on the duration of the test campaign, the microphones may be required to stay deployed at the testing site for weeks or even months. This presents a challenge in regards to tracking the response (i.e., sensitivity) of the individual sensors as a function of time in order to evaluate the health of the array. To address this challenge, two different methods for in-situ tracking of microphone responses are described. The first relies on the use of an aerial sound source attached as a payload on a hovering small Unmanned Aerial System (sUAS) vehicle. The second relies on the use of individually excited ground-based sound sources strategically placed throughout the array pattern. Testing of the two methods was performed in microphone array deployments conducted at Fort A.P. Hill in 2015 and at Edwards Air Force Base in 2016. The results indicate that the drift in individual sensor responses can be tracked reasonably well using both methods. Thus, in-situ response tracking methods are useful as a diagnostic tool for monitoring the health of a phased array during long duration deployments.

  16. In Situ Tracking Kinetic Pathways of Li+/Na+ Substitution during Ion-Exchange Synthesis of LixNa1.5-xVOPO4F0.5.

    Science.gov (United States)

    Park, Young-Uk; Bai, Jianming; Wang, Liping; Yoon, Gabin; Zhang, Wei; Kim, Hyungsub; Lee, Seongsu; Kim, Sung-Wook; Looney, J Patrick; Kang, Kisuk; Wang, Feng

    2017-09-13

    Ion exchange is a ubiquitous phenomenon central to wide industrial applications, ranging from traditional (bio)chemical separation to the emerging chimie douce synthesis of materials with metastable structure for batteries and other energy applications. The exchange process is complex, involving substitution and transport of different ions under non-equilibrium conditions, and thus difficult to probe, leaving a gap in mechanistic understanding of kinetic exchange pathways toward final products. Herein, we report in situ tracking kinetic pathways of Li + /Na + substitution during solvothermal ion-exchange synthesis of Li x Na 1.5-x VOPO 4 F 0.5 (0 ≤ x ≤ 1.5), a promising multi-Li polyanionic cathode for batteries. The real-time observation, corroborated by first-principles calculations, reveals a selective replacement of Na + by Li + , leading to peculiar Na + /Li + /vacancy orderings in the intermediates. Contradicting the traditional belief of facile topotactic substitution via solid solution reaction, an abrupt two-phase transformation occurs and predominantly governs the kinetics of ion exchange and transport in the 1D polyanionic framework, consequently leading to significant difference of Li stoichiometry and electrochemical properties in the exchanged products. The findings may help to pave the way for rational design of ion exchange synthesis for making new materials.

  17. A novel method for synthesis of {sup 56}Co-radiolabelled silica nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Cydzik, I. [Institute for Health and Consumer Protection, European Commission, Joint Research Centre (Italy); Bilewicz, A. [Institute of Nuclear Chemistry and Technology (Poland); Abbas, K. [Institute for Transuranium Elements (Ispra Site), European Commission, Joint Research Centre (Italy); Simonelli, F.; Bulgheroni, A.; Holzwarth, U., E-mail: uwe.holzwarth@jrc.ec.europa.eu; Gibson, N. [Institute for Health and Consumer Protection, European Commission, Joint Research Centre (Italy)

    2012-10-15

    A method for synthesis of radiolabelled amorphous silica nanoparticles is presented. The method is based on the well-known Stoeber process with the exception that {sup 56}Co radiotracer is introduced into one of the precursor materials prior to the initiation of the nanoparticle synthesis. The {sup 56}Co was prepared by proton irradiation of an iron foil, followed by dissolution in hydrochloric acid and {sup 56}Co/Fe radiochemical separation. In order to determine the residual Fe in the {sup 56}Co radiotracer solution, ICP-MS measurements were performed. Nanoparticles in the size range 20-100 nm were synthesised and characterised by gamma spectrometry, ICP-MS, XRD, DLS, and Zeta potential measurement. It was shown that the size and Zeta potential of the nanoparticles was roughly the same following synthesis with or without added {sup 56}Co, and in both cases, the structure was that of amorphous silica. It was found that 99.5 % of the {sup 56}Co was bound into the nanoparticles during synthesis, and centrifugation experiments confirmed that the radiolabels were stably incorporated into the silica matrix.

  18. Synthesis and characterization of hydrogen-bond acidic functionalized graphene

    Science.gov (United States)

    Yang, Liu; Han, Qiang; Pan, Yong; Cao, Shuya; Ding, Mingyu

    2014-05-01

    Hexafluoroisopropanol phenyl group functionalized materials have great potential in the application of gas-sensitive materials for nerve agent detection, due to the formation of strong hydrogen-bonding interactions between the group and the analytes. In this paper, take full advantage of ultra-large specific surface area and plenty of carbon-carbon double bonds and hexafluoroisopropanol phenyl functionalized graphene was synthesized through in situ diazonium reaction between -C=C- and p-hexafluoroisopropanol aniline. The identity of the as-synthesis material was confirmed by transmission electron microscopy, Raman spectroscopy, ultraviolet visible spectroscopy, X-ray photoelectron spectroscopy and thermo gravimetric analysis. The synthesis method is simply which retained the excellent physical properties of original graphene. In addition, the novel material can be assigned as an potential candidate for gas sensitive materials towards organophosphorus nerve agent detection.

  19. Facile, low temperature synthesis of SnO{sub 2}/reduced graphene oxide nanocomposite as anode material for lithium-ion batteries

    Energy Technology Data Exchange (ETDEWEB)

    Hou, Chau-Chung; Brahma, Sanjaya; Weng, Shao-Chieh [Department of Materials Science and Engineering, National Cheng Kung University, Tainan 70001, Taiwan, ROC (China); Chang, Chia-Chin [Department of Greenergy, National University of Tainan, Tainan 70005, Taiwan, ROC (China); Huang, Jow-Lay, E-mail: jlh888@mail.ncku.edu.tw [Department of Materials Science and Engineering, National Cheng Kung University, Tainan 70001, Taiwan, ROC (China); Department of Chemical and Materials Engineering, National University of Kaohsiung, Kaohsiung 81148, Taiwan, ROC (China); Center for Micro/Nano Science and Technology, National Cheng Kung University, Tainan 70101, Taiwan, ROC (China)

    2017-08-15

    Highlights: • Facile, one-pot, low temperature synthesis of SnO{sub 2}-RGO composite. • In-situ reduction of graphene oxide and growth of SnO{sub 2} nanoparticle. • Concentration of reductant during synthesis affects the properties significantly. • SnO{sub 2}-RGO composite shows good rate capability and stable capacitance. • Synthesis method is energy efficient and scalable for other metal oxides. - Abstract: We demonstrate a facile, single step, low temperature and energy efficient strategy for the synthesis of SnO{sub 2}-reduced graphene oxide (RGO) nanocomposite where the crystallization of SnO{sub 2} nanoparticles and the reduction of graphene oxide takes place simultaneously by an in situ chemical reduction process. The electrochemical property of the SnO{sub 2}-RGO composite prepared by using low concentrations of reducing agent shows better Li storage performance, good rate capability (378 mAh g{sup −1} at 3200 mA g{sup −1}) and stable capacitance (522 mAh g{sup −1} after 50 cycles). Increasing the reductant concentration lead to crystallization of high concentration of SnO{sub 2} nanoparticle aggregation and degrade the Li ion storage property.

  20. Sound Cross-synthesis and Morphing Using Dictionary-based Methods

    DEFF Research Database (Denmark)

    Collins, Nick; Sturm, Bob L.

    2011-01-01

    Dictionary-based methods (DBMs) provide rich possibilities for new sound transformations; as the analysis dual to granular synthesis, audio signals are decomposed into `atoms', allowing interesting manipulations. We present various approaches to audio signal cross-synthesis and cross-analysis via...... atomic decomposition using scale-time-frequency dictionaries. DBMs naturally provide high-level descriptions of a signal and its content, which can allow for greater control over what is modified and how. Through these models, we can make one signal decomposition influence that of another to create cross......-synthesized sounds. We present several examples of these techniques both theoretically and practically, and present on-going and further work....

  1. Improvements in in-situ filter test methods using a total light-scattering detector

    International Nuclear Information System (INIS)

    Marshall, M.; Stevens, D.C.

    1986-01-01

    This paper presents research aimed at providing useful data on a commonly used technique; a DOP (di-2-ethylhexyl phthalate) aerosol and a total light-scattering photometer. Methods of increasing the sensitivity of this technique are described. Alternative methods of in-situ filter testing are also considered. The sensitivity of a typical, modern, total light-scattering photometer, as a function of particle diameter, has a broad maximum in mass terms between 0.1 and 0.4 um. At its maximum usable sensitivity the instrument can detect approx. 1 particle/cm 3 . This response can be explained by light scattering theory and particle loss in the instrument inlet. The mass median diameter of the aerosols produced by various DOP generators varies from 0.2 to 1.0μm. Experiments with good quality HEPA filters indicate a maximum penetration for particles of 0.15 - 0.2μm. Details of the studies are given and the consequences discussed. It is shown that filter penetration of -3 % can be measured in-situ with existing equipment. Methods of extending the sensitivity to measure a penetration of approx.10 -5 % are described. (author)

  2. Comparison of some aspects of the in situ and in vitro methods in evaluation of neutral detergent fiber digestion.

    Science.gov (United States)

    Krizsan, S J; Jančík, F; Ramin, M; Huhtanen, P

    2013-02-01

    The objective of the present study was to compare digestion rates (kd) of NDF for different feeds estimated with the in situ method or derived from an automated gas in vitro system. A meta-analysis was conducted to evaluate how in situ derived kd of NDF related to in vivo digestibility of NDF. Furthermore, in vitro true digestibility of the feed samples incubated within filter bags or dispersed in the medium was compared, and kd for insoluble and soluble components of those feeds were estimated. Four different concentrates and 4 forages were used in this study. Two lactating Swedish Red cows fed a diet of 60% grass silage and 40% concentrate on DM basis were used for in situ incubations and for collection of rumen fluid. The feed samples were ground through a 2.0-mm screen before the in situ incubations and a 1.0-mm screen before the in vitro gas incubations. In situ nylon bags were introduced into the rumen for determination of kd of NDF. Additional kinetic data were produced from isolated NDF and intact samples subjected to in vitro incubations in which gas production was recorded for 72 h. Samples were weighed in the bottles or within filter bags (for fiber and in vitro studies) that were placed in the bottles. The interaction between feed and method was significant (P production recordings. The meta-analysis suggested that in situ derived kd of NDF were biased and underestimated in vivo digestibility of NDF. Digestion rates of the intact samples were lower for all feeds, except for the hay, when incubated within the bags compared with dispersed in the medium (P < 0.01). Less OM and NDF were digested for all feeds when incubated within bags than dispersed in the medium (P < 0.01). It is concluded from the in vitro study that microbial activity within the bags is less than in the medium. Significant interactions between method (in situ vs. in vitro) and feed suggest that one or both methods result in biased estimates of digestion kinetics.

  3. In-situ sulfuration synthesis of sandwiched spherical tin sulfide/sulfur-doped graphene composite with ultra-low sulfur content

    Science.gov (United States)

    Zhao, Bing; Yang, Yaqing; Wang, Zhixuan; Huang, Shoushuang; Wang, Yanyan; Wang, Shanshan; Chen, Zhiwen; Jiang, Yong

    2018-02-01

    SnS is widely studied as anode materials since of its superior structural stability and physicochemical property comparing with other Sn-based composites. Nevertheless, the inconvenience of phase morphology control and excessive consumption of sulfur sources during synthesis hinder the scalable application of SnS nanocomposites. Herein, we report a facile in-situ sulfuration strategy to synthesize sandwiched spherical SnS/sulfur-doped graphene (SnS/S-SG) composite. An ultra-low sulfur content with approximately stoichiometric ratio of Sn:S can effectively promote the sulfuration reaction of SnO2 to SnS and simultaneous sulfur-doping of graphene. The as-prepared SnS/S-SG composite shows a three-dimensional interconnected spherical structure as a whole, in which SnS nanoparticles are sandwiched between the multilayers of graphene sheets forming a hollow sphere. The sandwiched sphere structure and high S doping amount can improve the binding force between SnS and graphene, as well as the structural stability and electrical conductivity of the composite. Thus, a high reversibility of conversion reaction, promising specific capacity (772 mAh g-1 after 100 cycles at 0.1 C) and excellent rate performance (705 and 411 mAh g-1 at 1 C and 10 C, respectively) are exhibited in the SnS/S-SG electrode, which are much higher than that of the SnS/spherical graphene synthesized by traditional post-sulfuration method.

  4. In situ catalytic synthesis of high-graphitized carbon-coated LiFePO4 nanoplates for superior Li-ion battery cathodes.

    Science.gov (United States)

    Ma, Zhipeng; Fan, Yuqian; Shao, Guangjie; Wang, Guiling; Song, Jianjun; Liu, Tingting

    2015-02-04

    The low electronic conductivity and one-dimensional diffusion channel along the b axis for Li ions are two major obstacles to achieving high power density of LiFePO4 material. Coating carbon with excellent conductivity on the tailored LiFePO4 nanoparticles therefore plays an important role for efficient charge and mass transport within this material. We report here the in situ catalytic synthesis of high-graphitized carbon-coated LiFePO4 nanoplates with highly oriented (010) facets by introducing ferrocene as a catalyst during thermal treatment. The as-obtained material exhibits superior performances for Li-ion batteries at high rate (100 C) and low temperature (-20 °C), mainly because of fast electron transport through the graphitic carbon layer and efficient Li(+)-ion diffusion through the thin nanoplates.

  5. Analysis of random response of structure with uncertain parameters. Combination of substructure synthesis method and hierarchy method

    International Nuclear Information System (INIS)

    Iwatsubo, Takuzo; Kawamura, Shozo; Mori, Hiroyuki.

    1995-01-01

    In this paper, the method to obtain the random response of a structure with uncertain parameters is proposed. The proposed method is a combination of the substructure synthesis method and the hierarchy method. The concept of the proposed method is that the hierarchy equation of each substructure is obtained using the hierarchy method, and the hierarchy equation of the overall structure is obtained using the substructure synthesis method. Using the proposed method, the reduced order hierarchy equation can be obtained without analyzing the original whole structure. After the calculation of the mean square value of response, the reliability analysis can be carried out based on the first passage problem and Poisson's excursion rate. As a numerical example of structure, a simple piping system is considered. The damping constant of the support is considered as the uncertainty parameter. Then the random response is calculated using the proposed method. As a result, the proposed method is useful to analyze the random response in terms of the accuracy, computer storage and calculation time. (author)

  6. IN-SITU MEASURING METHOD OF RADON AND THORON DIFFUSION COEFFICIENT IN SOIL

    Directory of Open Access Journals (Sweden)

    V.S. Yakovleva

    2014-06-01

    Full Text Available A simple and valid in-situ measurement method of effective diffusion coefficient of radon and thoron in soil and other porous materials was designed. The analysis of numerical investigation of radon and thoron transport in upper layers of soil revealed that thoron flux density from the earth surface does not depend on soil gas advective velocity and varies only with diffusion coefficient changes. This result showed the advantages of thoron using versus radon using in the suggested method. The comparison of the new method with existing ones previously developed. The method could be helpful for solving of problems of radon mass-transport in porous media and gaseous exchange between soil and atmosphere.

  7. Methanol synthesis beyond chemical equilibrium

    NARCIS (Netherlands)

    van Bennekom, J. G.; Venderbosch, R. H.; Winkelman, J. G. M.; Wilbers, E.; Assink, D.; Lemmens, K. P. J.; Heeres, H. J.

    2013-01-01

    In commercial methanol production from syngas, the conversion is thermodynamically limited to 0.3-0.7 leading to large recycles of non-converted syngas. This problem can be overcome to a significant extent by in situ condensation of methanol during its synthesis which is possible nowadays due to the

  8. A practical method for in-situ thickness determination using energy distribution of beta particles

    International Nuclear Information System (INIS)

    Yalcin, S.; Gurler, O.; Gundogdu, O.; Bradley, D.A.

    2012-01-01

    This paper discusses a method to determine the thickness of an absorber using the energy distribution of beta particles. An empirical relationship was obtained between the absorber thickness and the energy distribution of beta particles transmitted through. The thickness of a polyethylene radioactive source cover was determined by exploiting this relationship, which has largely been left unexploited allowing us to determine the in-situ cover thickness of beta sources in a fast, cheap and non-destructive way. - Highlights: ► A practical and in-situ unknown cover thickness determination ► Cheap and readily available compared to other techniques. ► Beta energy spectrum.

  9. A practical method for in-situ thickness determination using energy distribution of beta particles

    Energy Technology Data Exchange (ETDEWEB)

    Yalcin, S., E-mail: syalcin@kastamonu.edu.tr [Kastamonu University, Education Faculty, 37200 Kastamonu (Turkey); Gurler, O. [Physics Department, Faculty of Arts and Sciences, Uludag University, Gorukle Campus, 16059 Bursa (Turkey); Gundogdu, O. [Kocaeli University, Umuttepe Campus, 41380 Kocaeli (Turkey); Bradley, D.A. [CNRP, Department of Physics, Faculty of Engineering and Physical Sciences, University of Surrey, Guildford GU2 7XH (United Kingdom)

    2012-01-15

    This paper discusses a method to determine the thickness of an absorber using the energy distribution of beta particles. An empirical relationship was obtained between the absorber thickness and the energy distribution of beta particles transmitted through. The thickness of a polyethylene radioactive source cover was determined by exploiting this relationship, which has largely been left unexploited allowing us to determine the in-situ cover thickness of beta sources in a fast, cheap and non-destructive way. - Highlights: Black-Right-Pointing-Pointer A practical and in-situ unknown cover thickness determination Black-Right-Pointing-Pointer Cheap and readily available compared to other techniques. Black-Right-Pointing-Pointer Beta energy spectrum.

  10. Electrochemically assisted organosol method for Pt-Sn nanoparticle synthesis and in situ deposition on graphite felt support: Extended reaction zone anodes for direct ethanol fuel cells

    Energy Technology Data Exchange (ETDEWEB)

    Lycke, Derek R.; Gyenge, Elod L. [Department of Chemical and Biological Engineering, The University of British Columbia, 2360 East Mall, Vancouver, BC (Canada)

    2007-03-20

    Two electrochemically assisted variants of the Boenneman organosol method were developed for Pt-Sn nanoparticle synthesis and in situ deposition on graphite felt electrodes (e.g. thickness up to 2 mm). Tetraoctylammonium triethylhydroborate N(C{sub 8}H{sub 17}){sub 4}BH(C{sub 2}H{sub 5}){sub 3} was employed as colloid stabilizer and reductant dissolved in tetrahydrofuran (THF). The role of the electric field at a low deposition current density of 1.25 mA cm{sup -2} was mainly electrophoretic causing the migration and adsorption of N(C{sub 8}H{sub 17}){sub 4}BH(C{sub 2}H{sub 5}){sub 3} on the graphite felt surface where it reduced the PtCl{sub 2}-SnCl{sub 2} mixture. Faradaic electrodeposition was detected mostly for Sn. Typical Pt-Sn loadings were between 0.4 and 0.9 mg cm{sup -2} depending on the type of pre-deposition exposure of the graphite felt: surfactant-adsorption and metal-adsorption variant, respectively. The catalyst surface area and Pt:Sn surface area ratio was determined by anodic striping of an underpotential deposited Cu monolayer. The two deposition variants gave different catalyst surfaces: total area 233 and 76 cm{sup 2} mg{sup -1}, with Pt:Sn surface area ratio of 3.5:1 and 7.7:1 for surfactant and metal adsorption, respectively. Regarding electrocatalysis of ethanol oxidation, voltammetry and chronopotentiometry studies corroborated by direct ethanol fuel cell experiments using 0.5 M H{sub 2}SO{sub 4} as electrolyte, showed that due to a combination of higher catalyst load and Pt:Sn surface ratio, the graphite felt anodes prepared by the metal-adsorption variant gave better performance. The catalyzed graphite felt provided an extended reaction zone for ethanol electrooxidation and it gave higher catalyst mass specific peak power outputs compared to literature data obtained using gas diffusion anodes with carbon black supported Pt-Sn nanoparticles. (author)

  11. In situ-synthesized cadmium sulfide nanowire photosensor with a parylene passivation layer for chemiluminescent immunoassays.

    Science.gov (United States)

    Im, Ju-Hee; Kim, Hong-Rae; An, Byoung-Gi; Chang, Young Wook; Kang, Min-Jung; Lee, Tae-Geol; Son, Jin Gyeng; Park, Jae-Gwan; Pyun, Jae-Chul

    2017-06-15

    The direct in situ synthesis of cadmium sulfide (CdS) nanowires (NWs) was presented by direct synthesis of CdS NWs on the gold surface of an interdigitated electrode (IDE). In this work, we investigated the effect of a strong oxidant on the surfaces of the CdS NWs using X-ray photoelectron spectroscopy, transmission electron microscopy, and time-of-flight secondary ion mass spectrometry. We also fabricated a parylene-C film as a surface passivation layer for in situ-synthesized CdS NW photosensors and investigated the influence of the parylene-C passivation layer on the photoresponse during the coating of parylene-C under vacuum using a quartz crystal microbalance and a photoanalyzer. Finally, we used the in situ-synthesized CdS NW photosensor with the parylene-C passivation layer to detect the chemiluminescence of horseradish peroxidase and luminol and applied it to medical detection of carcinoembryonic antigen. Copyright © 2017 Elsevier B.V. All rights reserved.

  12. Methods for providing intermediates in the synthesis of atorvastatin.

    NARCIS (Netherlands)

    Dömling, Alexander Stephan Siegfried

    2016-01-01

    The invention relates to the field of medicinal chemistry, In particular, it relates to methods for providing intermediates in the synthesis of Atorvastatin, a competitive inhibitor of HMG-Co A reductase. Provided is a process for providing a compound having a Formula (I) or a pharmaceutically

  13. Gaining Control over Radiolytic Synthesis of Uniform Sub-3-nanometer Palladium Nanoparticles: Use of Aromatic Liquids in the Electron Microscope.

    Science.gov (United States)

    Abellan, Patricia; Parent, Lucas R; Al Hasan, Naila; Park, Chiwoo; Arslan, Ilke; Karim, Ayman M; Evans, James E; Browning, Nigel D

    2016-02-16

    Synthesizing nanomaterials of uniform shape and size is of critical importance to access and manipulate the novel structure-property relationships arising at the nanoscale, such as catalytic activity. In this work, we synthesize Pd nanoparticles with well-controlled size in the sub-3 nm range using scanning transmission electron microscopy (STEM) in combination with an in situ liquid stage. We use an aromatic hydrocarbon (toluene) as a solvent that is very resistant to high-energy electron irradiation, which creates a net reducing environment without the need for additives to scavenge oxidizing radicals. The primary reducing species is molecular hydrogen, which is a widely used reductant in the synthesis of supported metal catalysts. We propose a mechanism of particle formation based on the effect of tri-n-octylphosphine (TOP) on size stabilization, relatively low production of radicals, and autocatalytic reduction of Pd(II) compounds. We combine in situ STEM results with insights from in situ small-angle X-ray scattering (SAXS) from alcohol-based synthesis, having similar reduction potential, in a customized microfluidic device as well as ex situ bulk experiments. This has allowed us to develop a fundamental growth model for the synthesis of size-stabilized Pd nanoparticles and demonstrate the utility of correlating different in situ and ex situ characterization techniques to understand, and ultimately control, metal nanostructure synthesis.

  14. Application of methods of discrete mathematics at modular synthesis of mechatronic devices

    OpenAIRE

    Nikiforov, S.; Nikiforov, B.; Mandarov, E.; Rabdanova, N.

    2010-01-01

    The article is devoted to application of methods of discrete mathematics (the theory of counts, the method of matrix code and others) and synthesis of executive mechanisms of mechatronic handling devices

  15. Learning spinal manipulation: A best-evidence synthesis of teaching methods.

    Science.gov (United States)

    Stainsby, Brynne E; Clarke, Michelle C S; Egonia, Jade R

    2016-10-01

    The purpose of this study was to evaluate the effectiveness of different reported methods used to teach spinal manipulative therapy to chiropractic students. For this best-evidence literature synthesis, 5 electronic databases were searched from 1900 to 2015. Eligible studies were critically appraised using the criteria of the Scottish Intercollegiate Guidelines Network. Scientifically admissible studies were synthesized following best-evidence synthesis principles. Twenty articles were critically appraised, including 9 randomized clinical trials, 9 cohort studies, and 2 systematic reviews/meta-analyses. Eleven articles were accepted as scientifically admissible. The type of teaching method aids included a Thrust in Motion cervical manikin, instrumented cardiopulmonary reanimation manikin, padded contact with a load cell, instrumented treatment table with force sensor/transducer, and Dynadjust instrument. Several different methods exist in the literature for teaching spinal manipulative therapy techniques; however, future research in this developing area of chiropractic education is proposed. It is suggested that various teaching methods be included in the regular curricula of chiropractic colleges to aid in developing manipulation skills, efficiency, and knowledge of performance.

  16. In situ synthesis of carbon nanotubes decorated with palladium nanoparticles using arc-discharge in solution method

    International Nuclear Information System (INIS)

    Bera, Debasis; Kuiry, Suresh C.; McCutchen, Matthew; Seal, Sudipta; Heinrich, Helge; Slane, Grady C.

    2004-01-01

    A unique, simple, inexpensive, and one-step synthesis route to produce carbon nanotubes (CNTs) decorated with palladium nanoparticles using a simplified dc arc-discharge in solution is reported. Zero-loss energy filtered transmission electron microscopy and scanning transmission electron microscopy confirm the presence of 3 nm palladium nanoparticles. Such palladium nanoparticles form during the reduction of palladium tetra-chloro-square-planar complex. The deconvoluted x-ray photoelectron spectroscopy envelope shows the presence of palladium on the decorated CNTs. The energy dispersive spectroscopy suggests no functionalization of atomic chlorine to the sidewall of the CNTs. The presence of dislodged graphene sheets with wavy morphology supports the formation of CNTs through the 'scroll mechanism'

  17. Waste utilization for the controlled synthesis of nanosized hydroxyapatite

    Energy Technology Data Exchange (ETDEWEB)

    Nayar, Suprabha, E-mail: Suprabha.nayar@gmail.com [National Metallurgical Laboratory, Jamshedpur (India); Guha, Avijit [National Metallurgical Laboratory, Jamshedpur (India)

    2009-05-05

    This work uses biomolecules in waste and medicinally important materials for the synthesis of hydroxyapatite nanoparticles. Orange and potato peel, eggshell, papaya leaf and calendula flower extracts have varied biomolecules, which exert a significant, control on the in situ synthesis of nanosized hydroxyapatite particles. The biomimetic synthesis of inorganic particles using known matrices is already well established, however, there are only a few reports using compound extracts. The synthesized nanocomposite has been characterized using X-ray diffraction, Fourier transform infrared spectroscopy and scanning electron microscopy studies. Role of varied biomolecules in controlled inorganic synthesis may have tremendous technological impact.

  18. In situ anisotropic parameter determination using refraction seismic and VSP methods

    Energy Technology Data Exchange (ETDEWEB)

    Leslie, J.M.; Lawton, D.C. (Calgary Univ., AB (Canada))

    1999-01-01

    A prime concern in the time-to-depth conversion of reflection seismic data is seismic anisotropy, because it can produce velocity anomalies in seismic data that mimic the structural plays of interest to the petroleum prospector in both size and shape. Ongoing techniques of time-to-depth conversion of P-wave seismic data do not handle the travel time and velocity distortions caused by seismic anisotropy, particularly in areas of complex geologic structures. To address this problem, the first step is to know which rock units are anisotropic and measure their anisotropic parameters. Laboratory means are available, but there are problems with these mainly with shales because of their fissile nature. In situ measurements are preferable because they yield a more robust value, and at the University of Calgary such measurements were undertaken using refraction seismic and vertical seismic profiling (VSP) methods. Results indicate that the two Thomsen anisotropic parameters of interest can be determined from the VSP experiment, but these values are slightly less than those obtained using the refraction technique. This may be because of the sensitivity of the shot statics which arises from the direct travel time measurement of the technique. The experiment yields another method to measure velocity anisotropy, in situ, where steeply dipping strata outcrop, which allows for the accurate measurement of the anisotropic parameters for use in depth migration routines. 4 refs.

  19. In situ anisotropic parameter determination using refraction seismic and VSP methods

    Energy Technology Data Exchange (ETDEWEB)

    Leslie, J.M.; Lawton, D.C. [Calgary Univ., AB (Canada)

    1999-11-01

    A prime concern in the time-to-depth conversion of reflection seismic data is seismic anisotropy, because it can produce velocity anomalies in seismic data that mimic the structural plays of interest to the petroleum prospector in both size and shape. Ongoing techniques of time-to-depth conversion of P-wave seismic data do not handle the travel time and velocity distortions caused by seismic anisotropy, particularly in areas of complex geologic structures. To address this problem, the first step is to know which rock units are anisotropic and measure their anisotropic parameters. Laboratory means are available, but there are problems with these mainly with shales because of their fissile nature. In situ measurements are preferable because they yield a more robust value, and at the University of Calgary such measurements were undertaken using refraction seismic and vertical seismic profiling (VSP) methods. Results indicate that the two Thomsen anisotropic parameters of interest can be determined from the VSP experiment, but these values are slightly less than those obtained using the refraction technique. This may be because of the sensitivity of the shot statics which arises from the direct travel time measurement of the technique. The experiment yields another method to measure velocity anisotropy, in situ, where steeply dipping strata outcrop, which allows for the accurate measurement of the anisotropic parameters for use in depth migration routines. 4 refs.

  20. An Expedient Method for the Synthesis of Thiosemicarbazones under Microwave Irradiation in Solvent-free Medium

    Institute of Scientific and Technical Information of China (English)

    LI, Jian-Ping; ZHENG, Peng-Zhi; ZHU, Jun-Ge; LIU, Rui-Jie; QU, Gui-Rong

    2006-01-01

    A simple, efficient and eco-friendly method for the synthesis of thiosemicarbazones from thiosemicarbazides and aldehyde under microwave irradiation has been reported, and no solvent and catalyst were used. And the technique of microwave irradiation coupled with solvent-free condition proved to be a quite valuable method in the organic synthesis.

  1. Comparison of Two Methods of Ruminal Digestibility Determination (in situ and in vitro of Pomegranate Seed Pulp

    Directory of Open Access Journals (Sweden)

    Mohammad Hassan Fathi Nasri

    2016-08-01

    Full Text Available Introduction Using of agro-industrial by-products in diet of livestock not only reduces the production costs but also can dwindle the use of human foods in animal nutrition and competition between human and livestock. Thus, proper use of these by-products in animal nutrition and identification of new and low cost feed resources may be one of the priorities in livestock husbandry of our country. Pomegranate seed pulp (PSP is a by-product of the industrial decoction of pomegranate. Iran with annually production of more than 900 tons of pomegranates is one of the most important regions of pomegranate cultivation and PSP produced from pomegranate processing factories may be extensively used in animal nutrition. Digestibility determination of feeds is one of the most effective ways to evaluate their nutritional value. In addition, there is a strong relationship between feeds digestibility and performance of animal. There are in vivo, in vitro and in situ methods to determine the digestibility of feeds. Although in vivo methods are reference for digestibility values of feeds and are of high precision but they are usually expensive and time consuming. In addition, these methods do not provide any information related to ruminal degradability kinetic of nutrients. The aim of this study was comparison of two methods of ruminal degradability determination methods namely, in situ (nylon bag and in vitro (Daisy incubator, using dried and ensiled pomegranate seed pulp (PSP. Materials and Methods The PSP used in this study was prepared from Anaryan Co. in Ferdows, Iran. Decocted pomegranate was a mixture of Yazd varieties which were harvested at early autumn of 1389. Two types of PSP as dried and ensiled were used to compare the methods of ruminal digestibility determination, pervasively. The PSP silage was prepared by ensiling of wet PSP (containing 475 g/kg DM in 3 kg bins (4 replicatesand with density of 650 kg wet PSP per cubic meter for 60 days and dried

  2. In-situ gamma spectrometry method for determination of environmental gamma dose; Metodo de espectrometria gamma in situ para determinacao de dose gama ambiental

    Energy Technology Data Exchange (ETDEWEB)

    Conti, Claudio de Carvalho

    1995-07-15

    This work tries to establish a methodology for germanium detectors calibration, normally used for in situ gamma ray spectrometry, for determining the environmental exposure rate in function of the energy of the incident photons. For this purpose a computer code has been developed, based on the stripping method, for the computational spectra analysis to calculate the contribution of the partial absorption of the gamma rays (Compton effect) in the active and nonactive parts of the detector. The resulting total absorption spectrum is then converted to fluence distribution in function of the energy for the photons reaching the detector, which is then used to calculate the exposure rate or kerma in air. The unfolding and fluency convention parameters are determined by detector calibration using point gamma sources. The method is validated by comparison of the results against the calculated exposure rate at a point of interest for the standards. This method is used for the direct measurement of the exposure rate distribution in function of the energy at the site, in situ measurement technic, leading to rapid results during an emergency situation and also used for indoor measurements. (author)

  3. A SYNTHESIS METHOD OF BASIC TERNARY BENT-SQUARES BASED ON THE TRIAD SHIFT OPERATOR

    Directory of Open Access Journals (Sweden)

    O. N. Zhdanov

    2017-01-01

    Full Text Available Practical application of advanced algebraic constructions in modern communication systems based on MC-CDMA (Multi Code Code Division Multiple Access technology and in cryptography necessitates their further research. One of the most commonly used advanced algebraic construction is the binary bent-function having a uniform amplitude spectrum of the Walsh-Hadamard transform and, accordingly, having the maximal distance from the codewords of affine code. In addition to the binary bent-functions researchers are currently focuses on the development of synthesis methods of their many-valued analogues. In particular, one of the most effective methods for the synthesis of many-valued bent-functions is the method based on the Agievich bent-squares. In this paper, we developed a regular synthesis method of the ternary bent-squares on the basis of an arbitrary spectral vector and the regular operator of the triad shift. The classification of spectral vectors of lengths N = 3 and N = 9 is performed. On the basis of spectral classification more precise definition of many-valued bent-sequences is given, taking into account the existence of the phenomenon of many-valued bent-sequences for the length, determined by odd power of base. The paper results are valuable for practical use: the development of new constant amplitude codes for MC-CDMA technology, cryptographic primitives, data compression algorithms, signal structures, algorithms of block and stream encryption, based on advanced principles of many-valued logic. The developed bent-squares design method is also a basis for further theoretical research: development of methods of the permutation of rows and columns of basic bent-squares and their sign coding, synthesis of composite bent-squares. In addition, the data on the spectral classification of vectors give the task of constructing the synthesis methods of bent-functions of lengths N = 32k+1, k Є ℕ.

  4. Novel RNA hybridization method for the in situ detection of ETV1, ETV4, and ETV5 gene fusions in prostate cancer.

    Science.gov (United States)

    Kunju, Lakshmi P; Carskadon, Shannon; Siddiqui, Javed; Tomlins, Scott A; Chinnaiyan, Arul M; Palanisamy, Nallasivam

    2014-09-01

    The genetic basis of 50% to 60% of prostate cancer (PCa) is attributable to rearrangements in E26 transformation-specific (ETS) (ERG, ETV1, ETV4, and ETV5), BRAF, and RAF1 genes and overexpression of SPINK1. The development and validation of reliable detection methods are warranted to classify various molecular subtypes of PCa for diagnostic and prognostic purposes. ETS gene rearrangements are typically detected by fluorescence in situ hybridization and reverse-transcription polymerase chain reaction methods. Recently, monoclonal antibodies against ERG have been developed that detect the truncated ERG protein in immunohistochemical assays where staining levels are strongly correlated with ERG rearrangement status by fluorescence in situ hybridization. However, specific antibodies for ETV1, ETV4, and ETV5 are unavailable, challenging their clinical use. We developed a novel RNA in situ hybridization-based assay for the in situ detection of ETV1, ETV4, and ETV5 in formalin-fixed paraffin-embedded tissues from prostate needle biopsies, prostatectomy, and metastatic PCa specimens using RNA probes. Further, with combined RNA in situ hybridization and immunohistochemistry we identified a rare subset of PCa with dual ETS gene rearrangements in collisions of independent tumor foci. The high specificity and sensitivity of RNA in situ hybridization provides an alternate method enabling bright-field in situ detection of ETS gene aberrations in routine clinically available PCa specimens.

  5. Method for in situ or ex situ bioremediation of hexavalent chromium contaminated soils and/or groundwater

    Science.gov (United States)

    Turick, Charles E.; Apel, William W.

    1997-10-28

    A method of reducing the concentration of Cr(VI) in a liquid aqueous residue comprises the steps of providing anaerobic Cr(VI) reducing bacteria, mixing the liquid aqueous residue with a nutrient medium to form a mixture, and contacting the mixture with the anaerobic Cr(VI) reducing bacteria such that Cr(VI) is reduced to Cr(III). The anaerobic Cr(VI) reducing bacteria appear to be ubiquitous in soil and can be selected by collecting a soil sample, diluting the soil sample with a sterile diluent to form a diluted sample, mixing the diluted sample with an effective amount of a nutrient medium and an effective amount of Cr(VI) to form a mixture, and incubating the mixture in the substantial absence of oxygen such that growth of Cr(VI) sensitive microorganisms is inhibited and growth of the anaerobic Cr(VI) reducing bacteria is stimulated. A method of in situ bioremediation of Cr(VI) contaminated soil and/or groundwater is also disclosed.

  6. Synthesis of cyclopentadiene-fused chromanones via one-pot multicomponent reactions.

    Science.gov (United States)

    Ghandi, Mehdi; Ghomi, Ali-Tabatabaei; Kubicki, Maciej

    2013-03-15

    We have developed one-pot method for the synthesis of functionalized novel cyclopentadiene-fused chromanone scaffolds. A variety of 4-oxo-2,4-dihydrocyclopenta[c]chromene-1,2-dicarboxylates were obtained in moderate to good yields via condensation of 2-hydroxybenzaldehydes and ethyl acetoacetate with 1:1 acetylenecarboxylate-isocyanides in toluene. These reactions presumably proceed via reaction of the in situ generated 3-acetyl-2H-chromen-2-ones with acetylenecarboxylate-isocyanide zwitterionic intermediates through Michael addition/intramolecular cyclization and double [1,5] acyl shift rearrangement cascade.

  7. Estimation of In Situ Stresses with Hydro-Fracturing Tests and a Statistical Method

    Science.gov (United States)

    Lee, Hikweon; Ong, See Hong

    2018-03-01

    At great depths, where borehole-based field stress measurements such as hydraulic fracturing are challenging due to difficult downhole conditions or prohibitive costs, in situ stresses can be indirectly estimated using wellbore failures such as borehole breakouts and/or drilling-induced tensile failures detected by an image log. As part of such efforts, a statistical method has been developed in which borehole breakouts detected on an image log are used for this purpose (Song et al. in Proceedings on the 7th international symposium on in situ rock stress, 2016; Song and Chang in J Geophys Res Solid Earth 122:4033-4052, 2017). The method employs a grid-searching algorithm in which the least and maximum horizontal principal stresses ( S h and S H) are varied, and the corresponding simulated depth-related breakout width distribution as a function of the breakout angle ( θ B = 90° - half of breakout width) is compared to that observed along the borehole to determine a set of S h and S H having the lowest misfit between them. An important advantage of the method is that S h and S H can be estimated simultaneously in vertical wells. To validate the statistical approach, the method is applied to a vertical hole where a set of field hydraulic fracturing tests have been carried out. The stress estimations using the proposed method were found to be in good agreement with the results interpreted from the hydraulic fracturing test measurements.

  8. Detection of protein-protein interactions by ribosome display and protein in situ immobilisation.

    Science.gov (United States)

    He, Mingyue; Liu, Hong; Turner, Martin; Taussig, Michael J

    2009-12-31

    We describe a method for identification of protein-protein interactions by combining two cell-free protein technologies, namely ribosome display and protein in situ immobilisation. The method requires only PCR fragments as the starting material, the target proteins being made through cell-free protein synthesis, either associated with their encoding mRNA as ribosome complexes or immobilised on a solid surface. The use of ribosome complexes allows identification of interacting protein partners from their attached coding mRNA. To demonstrate the procedures, we have employed the lymphocyte signalling proteins Vav1 and Grb2 and confirmed the interaction between Grb2 and the N-terminal SH3 domain of Vav1. The method has promise for library screening of pairwise protein interactions, down to the analytical level of individual domain or motif mapping.

  9. Peptide Synthesis Method and Solid Support for Use in the Method

    DEFF Research Database (Denmark)

    1994-01-01

    A method for the solid-phase synthesis of peptides or proteins in high yield and high purity uses a solid support consisting of a functionalized polystyrene-grafted polymer substrate, the grafted polystyrene chains being substantially non-cross-linked and having a chain molecular weight, not incl...... is immersed in a solution of optionally substituted styrene monomer in an alcohol such as methanol, the volume percentage of styrene in the solution preferably being about 30% v/v, and subjected to gamma irradiation....

  10. Investigating an organ-targeting platform based on hydroxyapatite nanoparticles using a novel in situ method of radioactive {sup 125}Iodine labeling

    Energy Technology Data Exchange (ETDEWEB)

    Ignjatović, Nenad [Centre for Fine Particles Processing and Nanotechnologies, Institute of Technical Sciences of the Serbian Academy of Science and Arts, Knez Mihailova 35/4, 11000 Belgrade (Serbia); Vranješ Djurić, Sanja [Laboratory for Radioisotopes, Vinča Institute of Nuclear Sciences, University of Belgrade, PO Box 522, 11001 Belgrade (Serbia); Mitić, Žarko [Faculty of Medicine, Department of Pharmacy, University of Niš, Bulevar dr Zorana Đinđića 81, 18000 Niš (Serbia); Janković, Drina [Laboratory for Radioisotopes, Vinča Institute of Nuclear Sciences, University of Belgrade, PO Box 522, 11001 Belgrade (Serbia); Uskoković, Dragan, E-mail: dragan.uskokovic@itn.sanu.ac.rs [Centre for Fine Particles Processing and Nanotechnologies, Institute of Technical Sciences of the Serbian Academy of Science and Arts, Knez Mihailova 35/4, 11000 Belgrade (Serbia)

    2014-10-01

    In this study, we have investigated the synthesis of nanoparticles of hydroxyapatite (HAp) and hydroxyapatite coated with chitosan (HAp/Ch) and the chitosan-poly-D,L-lactide-co-glycolide polymer blend (HAp/Ch-PLGA) as an organ-targeting system. We have examined and defined the final destination, as well as the dynamics and the pathways of the synthesized particles following intravenous administration in vivo. The XRD, ZP, FT-IR and SEM analyses have confirmed that the hydroxyapatite nanoparticles with d{sub 50} = 72 nm are coated with polymers. Radioactive 125-Iodine ({sup 125}I), a low energy gamma emitter, was used to develop a novel in situ method for the radiolabeling of particles and investigation of their biodistribution. {sup 125}I-labeled particles exhibited high stability in saline and serum over the second day, which justified their use in the following in vivo studies. The biodistribution of {sup 125}I-labeled particles after intravenous injection in rats differed significantly: HAp particles mostly targeted the liver, HAp/Ch the spleen and the liver, while HAp/Ch-PLGA targeted the lungs. Twenty-four hours post injection, HAp particles were excreted completely, while both {sup 125}I-HAp/Ch and {sup 125}I-HAp/Ch-PLGA were retained in the body for a prolonged period of time with more than 20% of radioactivity still found in different organs. - Highlights: • An organ-targeting carrier based on nano-hydroxyapatite • In situ labeling • Biodistribution of {sup 125}I-labeled HAp particles.

  11. Effect of tamoxifen in RAFT miniemulsion polymerization during the synthesis of polymer nanoparticles

    Directory of Open Access Journals (Sweden)

    Tailane Sant'Anna Moreira

    2014-01-01

    Full Text Available Tamoxifen (TXF is currently the only hormonal agent used for treatment of breast cancer. Although very effective, TXF presents low solubility in water, which affects its absorption and bioavailability. A common strategy to overcome this barrier is the formulation of a drug delivery system (DDS in order to increase the drug stability and improve the treatment effectiveness. Reversible addition-fragmentation chain transfer (RAFT polymerization is the most versatile method of controlled/living radical polymerization (CLRP, allowing for synthesis of well-defined polymers and being adapted to a wide range of polymerization systems. Miniemulsion polymerization is a dispersed system that is commonly used to prepare nanoparticles (NP with 50 to 500 nm of diameter. The aim of this work was to evaluate the effect of the in situ incorporation of TXF during miniemulsion conventional and RAFT polymerizations, using methyl methacrylate (MMA as monomer. Although the in situ addition of TXF promoted a slight reduction of the reaction rate, it did not affect the final particle size distribution of the latex or the molecular weight control exerted by the RAFT agent. The obtained results suggest that in situ incorporation of TXF during the synthesis of polymer NP via RAFT polymerization allows for production of a polymer DDS for different uses, such as the breast cancer treatment.

  12. New In Situ Synthesis Method for Fe3O4/Flake Graphite Nanosheet Composite Structure and Its Application in Anode Materials of Lithium-Ion Batteries

    Directory of Open Access Journals (Sweden)

    Chenhao Qian

    2018-01-01

    Full Text Available High-pressure torsion (HPT, a severe plastic deformation (SPD method, is rarely used in the manufacturing process of functional materials. In the present work, the authors creatively proposed using HPT as an alternative method an approach for high energy ball-milling in the preparation of an Fe3O4 and lamellar graphite nanosheet (GNS composite material. The corresponding electrochemical experiments verified that the in situ synthesized Fe3O4/GNS composite material has good lithium-storage performance and that it can retain good capacity (548.2 mA h g−1 even after several hundred cycles with high current density (8 C. Meanwhile, this performance has directly confirmed that SPD technique has great potential for the preparation of anode materials of lithium-ion batteries, especially in manufacturing metallic functional nanomaterials.

  13. Synthesis of azaphenanthridines via anionic ring closure

    DEFF Research Database (Denmark)

    Hansen, Henriette Møller; Lysén, M.; Begtrup, M.

    2005-01-01

    A new and convergent synthesis of azaphenanthridines via an anionic ring closure is reported. Ortho-lithiation/in situ borylation of cyanopyridines produces the corresponding cyanopyridylboronic esters, which undergo a Suzuki-Miyaura cross-coupling to give the key intermediates. Addition of lithium...

  14. In situ optical emission study on the role of C2 in the synthesis of singlewalled carbon nanotubes

    CSIR Research Space (South Africa)

    Motaung, DE

    2010-01-01

    Full Text Available applications. In this study, the authors have applied in situ optical emission spectroscopy (OES) to study the plasma in the laser-furnace method to synthesize SWCNTs. In particular, the authors have investigated the temporal and spatial behavior of C2 as well...

  15. Matrix diffusion studies by electrical conductivity methods. Comparison between laboratory and in-situ measurements

    International Nuclear Information System (INIS)

    Ohlsson, Y.; Neretnieks, I.

    1998-01-01

    Traditional laboratory diffusion experiments in rock material are time consuming, and quite small samples are generally used. Electrical conductivity measurements, on the other hand, provide a fast means for examining transport properties in rock and allow measurements on larger samples as well. Laboratory measurements using electrical conductivity give results that compare well to those from traditional diffusion experiments. The measurement of the electrical resistivity in the rock surrounding a borehole is a standard method for the detection of water conducting fractures. If these data could be correlated to matrix diffusion properties, in-situ diffusion data from large areas could be obtained. This would be valuable because it would make it possible to obtain data very early in future investigations of potentially suitable sites for a repository. This study compares laboratory electrical conductivity measurements with in-situ resistivity measurements from a borehole at Aespoe. The laboratory samples consist mainly of Aespoe diorite and fine-grained granite and the rock surrounding the borehole of Aespoe diorite, Smaaland granite and fine-grained granite. The comparison shows good agreement between laboratory measurements and in-situ data

  16. In situ crystallization of b-oriented MFI films on plane and curved substrates coated with a mesoporous silica layer

    KAUST Repository

    Deng, Zhiyong

    2013-05-01

    A simple and reproducible method is presented for preparing b-oriented MFI films on plane (disc) and curved (hollow fiber) supports by in situ hydrothermal synthesis. A mesoporous silica (sub-)layer was pre-coated on the supports by dip coating followed by a rapid thermal calcination step (973 K during 1 min) to reduce the number of grain boundaries while keeping the hydrophilic behavior of silica. The role of the silica sub-layer is not only to smoothen the substrate surface, but also to provide a silica source to promote the nucleation and growth of zeolite crystals via a heterogeneous nucleation mechanism (zeolitization), and adsorb zeolite moieties generated in the synthesis solution via a homogeneous nucleation mechanism. A monolayer of b-oriented MFI crystals was obtained on both supports after 3 h synthesis time with a moderate degree of twinning on the surface. © 2013 Elsevier Ltd.

  17. A general mixed boundary model reduction method for component mode synthesis

    NARCIS (Netherlands)

    Voormeeren, S.N.; Van der Valk, P.L.C.; Rixen, D.J.

    2010-01-01

    A classic issue in component mode synthesis (CMS) methods is the choice for fixed or free boundary conditions at the interface degrees of freedom (DoF) and the associated vibration modes in the components reduction base. In this paper, a novel mixed boundary CMS method called the “Mixed

  18. Multicomponent synthesis of spiropyrrolidine analogues derived from vinylindole/indazole by a 1,3-dipolar cycloaddition reaction

    Directory of Open Access Journals (Sweden)

    Manjunatha Narayanarao

    2016-12-01

    Full Text Available A new series of spiropyrrolidine compounds containing indole/indazole moieties as side chains have been accomplished via a one-pot multicomponent synthesis. The method uses the 1,3-dipolar cycloaddition reaction between N-alkylvinylindole/indazole and azomethine ylides, prepared in situ from cyclic/acyclic amino acids. The 1,3-dipolar cycloaddition proceeds efficiently under thermal conditions to afford the regio- and stereospecific cyclic adducts.

  19. Design of convergent pierce electron gun of accelerator for radiation sterilization by the method of synthesis

    International Nuclear Information System (INIS)

    Kong Xiaoxiao; Li Quanfeng

    2003-01-01

    A synthesis technique for the preliminary design of convergent Pierce electron guns is introduced briefly which has a series of advantages over the traditional methods. A thermal cathode electron gun used in the accelerator for radiation sterilization with the synthesis method is redesigned, and the validity of this method is proved. Based on the preliminary design parameters given by the synthesis method, a simulating calculation program, EGUN, was used in the numerical figure design of the focusing electrode and the anode. The final results can meet the engineering requirement as the current being 1A, the normalized emittance being less than 4 mm·mrad, and the final current density showing uniformity

  20. The SENSEI Generic In Situ Interface

    Energy Technology Data Exchange (ETDEWEB)

    Ayachit, Utkarsh [Kitware, Inc., Clifton Park, NY (United States); Whitlock, Brad [Intelligent Light, Rutherford, NJ (United States); Wolf, Matthew [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Loring, Burlen [Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States); Geveci, Berk [Kitware, Inc., Clifton Park, NY (United States); Lonie, David [Kitware, Inc., Clifton Park, NY (United States); Bethel, E. Wes [Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States)

    2017-04-11

    The SENSEI generic in situ interface is an API that promotes code portability and reusability. From the simulation view, a developer can instrument their code with the SENSEI API and then make make use of any number of in situ infrastructures. From the method view, a developer can write an in situ method using the SENSEI API, then expect it to run in any number of in situ infrastructures, or be invoked directly from a simulation code, with little or no modification. This paper presents the design principles underlying the SENSEI generic interface, along with some simplified coding examples.

  1. Calibration of HPGe detector for in situ measurements of 137Cs in soil by 'peak to valley' method

    International Nuclear Information System (INIS)

    Fueloep, M.

    2000-01-01

    The contamination of soil with gamma-ray emitters can be measured in two ways: soil sampling method and in situ spectrometry of the ambient gamma-ray radiation. The conventional soil sampling method has two disadvantages: samples may not be representative for a large areas and determination of the depth distribution of radionuclide requires the measurement of several samples taken from different depths. In situ measurement of a radionuclide activity in soil is more sensitive and provides more representative data than data obtained by soil sample collection and subsequent laboratory analysis. In emergency situations time to assess the contamination is critical. For rapid assessment of the deposited activity direct measurement of ambient gamma-ray radiation are used. In order to obtain accurate measurements of radionuclides in the soil, the detector should be placed on relatively even and open terrain. It is our customary practice to place the detector 1 m above the soil surface. At this height, a tripod-mounted detector can be handled easily and still provide a radius of view for gamma emitting sources out to about 10 m. The 'field of view' actually varies, being somewhat larger for higher sources. Depending upon source energy, the detector effectively sees down to a depth of 15-30 cm. Commonly used method for field gamma spectrometry is method by Beck (1). The most important disadvantages of in situ spectrometry by Beck are that the accuracy of the analysis depends on a separate knowledge of the radioactivity distribution with soil depth. This information can be obtained by calculations using data from in situ measurements and energy dependence of absorption and scattering of photons in soil and track length distribution of photons in soil (2). A method of in situ measurements of 137 Cs in soil where radionuclide distribution in soil profile is calculated by unfolding of detector responses in the full energy peak net area at 0.662 MeV and in the valley under the

  2. Conductive cotton prepared by polyaniline in situ polymerization using laccase.

    Science.gov (United States)

    Zhang, Ya; Dong, Aixue; Wang, Qiang; Fan, Xuerong; Cavaco-Paulo, Artur; Zhang, Ying

    2014-09-01

    The high-redox-potential catalyst laccase, isolated from Aspergillus, was first used as a biocatalyst in the oxidative polymerization of water-soluble conductive polyaniline, and then conductive cotton was prepared by in situ polymerization under the same conditions. The polymerization of aniline was performed in a water dispersion of sodium dodecylbenzenesulfonate (SDBS) micellar solution with atmospheric oxygen serving as the oxidizing agent. This method is ecologically clean and permits a greater degree of control over the kinetics of the reaction. The conditions for polyaniline synthesis were optimized. Characterizations of the conducting polyaniline and cotton were carried out using Fourier transform infrared spectroscopy, UV-vis spectroscopy, cyclic voltammetry, the fabric induction electrostatic tester, and the far-field EMC shielding effectiveness test fixture.

  3. Synthesis of metal-organic framework films by pore diffusion method

    Science.gov (United States)

    Murayama, Naohiro; Nishimura, Yuki; Kajiro, Hiroshi; Kishida, Satoru; Kinoshita, Kentaro; Tottori Univ Team; Nippon Steel; Sumitomo Metal Co. Collaboration; Tottori Integrated Frontier Resaerch Center (Tifrec) Collaboration; Tottori University Electronic Display Resaerch Center (Tedrec) Collaboration

    Metal-organic frameworks (MOFs) presents high controllability in designing the nano-scale pore, and this enable molecular storages, catalysts, gas sensors, gas separation membranes, and electronic devices for next-generation. Therefore, a simple method for film synthesis of MOFs compared with conventional methods [1] is strongly required. In this paper, we provide pore diffusion method, in which a substrate containing constituent metals of MOF is inserted in solution that includes only linker molecules of MOF. As a result, 2D growth of MOF was effectively enhanced, and the formation of flat and dense MOF films was attained. The growth time, t, dependence of film thickness, d, can be expressed by the relation of d = Aln(t + 1) + B, where A and B are constants. It means that ionized coppers diffuse through the pores of MOFs and the synthesis reaction proceeds at the MOF/solvent interface. We demonstrated the fabrication of a HKUST-1/Cu-TPA hetero structure by synthesizing a Cu-TPA film continuously after the growth of a HKUST-1 film on the CuOx substrate.

  4. Synthesis of hydrophobic peptides : An Fmoc “Solubilising Tail” method

    NARCIS (Netherlands)

    Choma, Christin T.; Robillard, George T.; Englebretsen, Darren R.

    1998-01-01

    The development of an Fmoc method for synthesis and purification of hydrophobic peptides using a “solubihsing tail” strategy is described. Peptide-constructs of the form hydrophobic peptide-[CHmb ester]-solubilising peptide were synthesised. Procedures for forming the 4-Hmb ester linkage, and

  5. Synthesis of lithium niobate and monocrystal growth by Czochralski method

    International Nuclear Information System (INIS)

    Balzuweit, K.

    1988-01-01

    The qualitative analysis of lithium niobate by x-ray analysis and optical microscopy is presented. The lithium niobate compound was obtained by synthesis using niobium oxides and lithium carbonates. The lithium niobate monocrystal growth was done by Czochralski method. (M.C.K.)

  6. In situ single-atom array synthesis using dynamic holographic optical tweezers

    Science.gov (United States)

    Kim, Hyosub; Lee, Woojun; Lee, Han-gyeol; Jo, Hanlae; Song, Yunheung; Ahn, Jaewook

    2016-01-01

    Establishing a reliable method to form scalable neutral-atom platforms is an essential cornerstone for quantum computation, quantum simulation and quantum many-body physics. Here we demonstrate a real-time transport of single atoms using holographic microtraps controlled by a liquid-crystal spatial light modulator. For this, an analytical design approach to flicker-free microtrap movement is devised and cold rubidium atoms are simultaneously rearranged with 2N motional degrees of freedom, representing unprecedented space controllability. We also accomplish an in situ feedback control for single-atom rearrangements with the high success rate of 99% for up to 10 μm translation. We hope this proof-of-principle demonstration of high-fidelity atom-array preparations will be useful for deterministic loading of N single atoms, especially on arbitrary lattice locations, and also for real-time qubit shuttling in high-dimensional quantum computing architectures. PMID:27796372

  7. Comparison of in vitro and in situ methods in evaluation of forage digestibility in ruminants.

    Science.gov (United States)

    Krizsan, S J; Nyholm, L; Nousiainen, J; Südekum, K-H; Huhtanen, P

    2012-09-01

    The objective of this study was to compare the application of different in vitro and in situ methods in empirical and mechanistic predictions of in vivo OM digestibility (OMD) and their associations to near-infrared reflectance spectroscopy spectra for a variety of forages. Apparent in vivo OMD of silages made from alfalfa (n = 2), corn (n = 9), corn stover (n = 2), grass (n = 11), whole crops of wheat and barley (n = 8) and red clover (n = 7), and fresh alfalfa (n = 1), grass hays (n = 5), and wheat straws (n = 5) had previously been determined in sheep. Concentrations of indigestible NDF (iNDF) in all forage samples were determined by a 288-h ruminal in situ incubation. Gas production of isolated forage NDF was measured by in vitro incubations for 72 h. In vitro pepsin-cellulase OM solubility (OMS) of the forages was determined by a 2-step gravimetric digestion method. Samples were also subjected to a 2-step determination of in vitro OMD based on buffered rumen fluid and pepsin. Further, rumen fluid digestible OM was determined from a single 96-h incubation at 38°C. Digestibility of OM from the in situ and the in vitro incubations was calculated according to published empirical equations, which were either forage specific or general (1 equation for all forages) within method. Indigestible NDF was also used in a mechanistic model to predict OMD. Predictions of OMD were evaluated by residual analysis using the GLM procedure in SAS. In vitro OMS in a general prediction equation of OMD did not display a significant forage-type effect on the residuals (observed - predicted OMD; P = 0.10). Predictions of OMD within forage types were consistent between iNDF and the 2-step in vitro method based on rumen fluid. Root mean square error of OMD was least (0.032) when the prediction was based on a general forage equation of OMS. However, regenerating a simple regression for iNDF by omitting alfalfa and wheat straw reduced the root mean square error of OMD to 0

  8. Experimental methods for in situ studies of morphology development during flow

    DEFF Research Database (Denmark)

    Lyngaae-Jørgensen, Jørgen

    1996-01-01

    A short overview of in situ methods is given. Multiple laminates of thin films is believed to represent unstable transition structures in many processing operations. A hypotesis for the break up is that first thin cylinders are formed . At a later stage these cylinders break up to spheres...... breakup mechanism involving creation of parallel layers of thin, filmlike formations parallel with the original film is observed. These layers then break up to a final state encompasing nearly spherical drops spread over a thickness much larger (by orders of magnitude) than the original film thickness....

  9. Reducing Water Sensitivity of Chitosan Biocomposite Films Using Gliadin Particles Made by In Situ Method

    Directory of Open Access Journals (Sweden)

    Dajian Huang

    2017-11-01

    Full Text Available In order to sustain rapid expansion in the field of biocomposites, it is necessary to develop novel fillers that are biodegradable, and easy to disperse and obtain. In this work, gliadin particles (GPs fabricated through an in situ method have been reported as fillers for creating chitosan (CS-based biocomposite films. In general, the particles tend to agglomerate in the polymer matrix at high loading (approximately >10% in the biopolymer/particles composites prepared by the traditional solution-blending method. However, the micrographs of biocomposites confirmed that the GPs are well dispersed in the CS matrix in all CS/GPs composites even at a high loading of 30% in this study. It was found that the GPs could improve the mechanical properties of the biocomposites. In addition, the results of moisture uptake and solubility in water of biocomposites showed that water resistance of biocomposites was enhanced by the introduction of GPs. These results suggested that GPs fabricated through an in situ method could be a good candidate for use in biopolymer-based composites.

  10. Immobilization methods for the rapid total chemical synthesis of proteins on microtiter plates.

    Science.gov (United States)

    Zitterbart, Robert; Krumrey, Michael; Seitz, Oliver

    2017-07-01

    The chemical synthesis of proteins typically involves the solid-phase peptide synthesis of unprotected peptide fragments that are stitched together in solution by native chemical ligation (NCL). The process is slow, and throughput is limited because of the need for repeated high performance liquid chromatography purification steps after both solid-phase peptide synthesis and NCL. With an aim to provide faster access to functional proteins and to accelerate the functional analysis of synthetic proteins by parallelization, we developed a method for the high performance liquid chromatography-free synthesis of proteins on the surface of microtiter plates. The method relies on solid-phase synthesis of unprotected peptide fragments, immobilization of the C-terminal fragment and on-surface NCL with an unprotected peptide thioester in crude form. Herein, we describe the development of a suitable immobilization chemistry. We compared (i) formation of nickel(II)-oligohistidine complexes, (ii) Cu-based [2 + 3] alkine-azide cycloaddition and (iii) hydrazone ligation. The comparative study identified the hydrazone ligation as most suitable. The sequence of immobilization via hydrazone ligation, on-surface NCL and radical desulfurization furnished the targeted SH3 domains in near quantitative yield. The synthetic proteins were functional as demonstrated by an on-surface fluorescence-based saturation binding analysis. Copyright © 2017 European Peptide Society and John Wiley & Sons, Ltd. Copyright © 2017 European Peptide Society and John Wiley & Sons, Ltd.

  11. Amphoteric Borylketenimines: Versatile Intermediates in the Synthesis of Borylated Heterocycles.

    Science.gov (United States)

    Kaldas, Sherif J; O'Keefe, Kowan T V; Mendoza-Sanchez, Rodrigo; Yudin, Andrei K

    2017-07-21

    We report the first synthesis of amphoteric borylketenimines from ethynyl N-methyliminodiacetic acid (MIDA) boronate and sulfonyl azides via copper catalysis. In situ trapping of these intermediates with various nucleophiles provided access to novel borylated azetidimines, iminocoumarins, amides, iminooxetanes, and amidines. The described strategy based on borylketenimines offers high levels of chemo- and regioselectivity, enabling the synthesis of unprecedented borylated molecules. This work highlights the unexplored utility of borylketenimines in the synthesis of potentially bioactive molecules. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  12. Novel in situ radiotracer methods for the direct and indirect study of chromate adsorption on alumina

    International Nuclear Information System (INIS)

    Gancs, L.; Nemeth, Z.; Horanyi, G.

    2002-01-01

    Radiotracer methods, particularly the radiotracer thin foil method, provide unique possibility of in situ monitoring of chromate adsorption on powdered adsorbents. Two different versions of the thin foil method can be distinguished. In the direct method, the species to be studied is labelled and the radiation measured gives direct information on the adsorption of this species. In the indirect method, a different labelled indicator species is added to the system and the adsorption of this species is followed and the adsorption of the species to be studied is determined based on analysis of the competitive adsorption processes. Both methods were used in the present study. In the in situ methods, the radiation measured consists of two main parts, one coming from the solution background, the other originating from the adsorption layer. In the case of the thin foil method using isotopes emitting soft β - radiation or low energy X-ray the solution background is governed and minimised by self-absorption of the radiation. In the direct study we applied an experimental methodology based on the energy selective measurement of the characteristic K α,β X-radiation emitted by the 51 Cr-labelled chromate species, whereas 35 S-labelled sulphate ions were used as the indicator species in the indirect study. (P.A.)

  13. Synthesis of nanosilver on polyamide fabric using silver/ammonia complex

    Energy Technology Data Exchange (ETDEWEB)

    Montazer, Majid, E-mail: tex5mm@aut.ac.ir [Textile Department, Functional Fibrous Structures and Environmental Enhancement (FFSEE), Amirkabir University of Technology, Hafez Avenue, Tehran (Iran, Islamic Republic of); Shamei, Ali; Alimohammadi, Farbod [Young Researchers Club, Tehran South Branch, Islamic Azad University, Tehran (Iran, Islamic Republic of)

    2014-05-01

    In this paper, a novel synthesis method for nanosilver has been introduced on or within the polymeric chains of polyamide 6 fabric by using silver/ammonia complex [Ag(NH{sub 3}){sub 2}]{sup +}. The silver complex was reduced directly by functional groups of polyamide chains without using any additional chemical reducing agents. The polyamide fabric was also stabilized with formation of new linkages between the polymeric chains of the nylon fabric through silver nanoparticle synthesis. The presence of nanosilver on the fabric was confirmed by UV–vis spectra, EDX patterns and XRD patterns. In addition, X-ray photoelectron spectroscopy (XPS) was utilized to identify the chemical state of silver in a range of silver oxide and silver metal. The SEM images confirmed the presence of nanosilver on the polyamide within the size of 20 and 150 nm. Excellent antibacterial properties were achieved with the treated fabrics against Staphylococcus aureus and Escherichia coli. Further, the antibacterial properties of the polyamide fabric treated with 35 mg/L silver/ammonia were durable against washing as they only decreased to 98.6% after 20 washes. In addition, some other properties of the treated fabrics including color changes, dimensional stability, water droplet adsorption, and reflectance spectrum are reported and thoroughly discussed. - Highlights: • Novel in situ synthesis of nanosilver on polyamide 6 • Synthesis of nanosilver without using external stabilizing and reducing agent • Synthesis of nanosilver particles within molecular chains of polyamide 6 • Producing antibacterial polyamide 6 using 35 mg/L Ag/ammonia complex • Obtaining durable antibacterial properties on polyamide 6 by this method.

  14. Synthesis of nanosilver on polyamide fabric using silver/ammonia complex

    International Nuclear Information System (INIS)

    Montazer, Majid; Shamei, Ali; Alimohammadi, Farbod

    2014-01-01

    In this paper, a novel synthesis method for nanosilver has been introduced on or within the polymeric chains of polyamide 6 fabric by using silver/ammonia complex [Ag(NH 3 ) 2 ] + . The silver complex was reduced directly by functional groups of polyamide chains without using any additional chemical reducing agents. The polyamide fabric was also stabilized with formation of new linkages between the polymeric chains of the nylon fabric through silver nanoparticle synthesis. The presence of nanosilver on the fabric was confirmed by UV–vis spectra, EDX patterns and XRD patterns. In addition, X-ray photoelectron spectroscopy (XPS) was utilized to identify the chemical state of silver in a range of silver oxide and silver metal. The SEM images confirmed the presence of nanosilver on the polyamide within the size of 20 and 150 nm. Excellent antibacterial properties were achieved with the treated fabrics against Staphylococcus aureus and Escherichia coli. Further, the antibacterial properties of the polyamide fabric treated with 35 mg/L silver/ammonia were durable against washing as they only decreased to 98.6% after 20 washes. In addition, some other properties of the treated fabrics including color changes, dimensional stability, water droplet adsorption, and reflectance spectrum are reported and thoroughly discussed. - Highlights: • Novel in situ synthesis of nanosilver on polyamide 6 • Synthesis of nanosilver without using external stabilizing and reducing agent • Synthesis of nanosilver particles within molecular chains of polyamide 6 • Producing antibacterial polyamide 6 using 35 mg/L Ag/ammonia complex • Obtaining durable antibacterial properties on polyamide 6 by this method

  15. Direct Synthesis of H2O2 over Ti-Containing Molecular Sieves Supported Gold Catalysts: A Comparative Study for In-situ-H2O2-ODS of Fuel

    International Nuclear Information System (INIS)

    Zhang, Han; Song, Haiyan; Chen, Chunxia; Han, Fuqin; Hu, Shaozheng; Liu, Guangliang; Chen, Ping; Zhao, Zhixi

    2013-01-01

    Direct synthesis of H 2 O 2 and in situ oxidative desulfurization of model fuel over Au/Ti-HMS and Au/TS-1 catalysts has been comparatively investigated in water or methanol. Maximum amount (82%) of active Au 0 species for H 2 O 2 synthesis was obtained. Au/Ti-HMS and Au/TS-1 exhibited the contrary performances in H 2 O 2 synthesis as CH 3 OH/H 2 O ratio of solvent changed. H 2 O 2 decomposition and hydrogenation in water was inhibited by the introduction of methanol. Effect of O 2 /H 2 ratio on H 2 O 2 concentration, H 2 conversion and H 2 O 2 selectivity revealed a relationship between H 2 O 2 generation and H2 consumption. The highest dibenzothiophene removal rate (83.2%) was obtained over Au/Ti-HMS in methanol at 1.5 of O 2 /H 2 ratio and 60 .deg. C. But removal of thiophene over Au/TS-1 should be performed in water without heating to obtain a high removal rate (61.3%). Meanwhile, H 2 conversion and oxidative desulfurization selectivity of H 2 were presented

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

    Directory of Open Access Journals (Sweden)

    Muhammad Faizan Shareef

    2017-10-01

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

  17. An in-situ chemical reaction deposition of nanosized wurtzite CdS thin films

    International Nuclear Information System (INIS)

    Chu Juan; Jin Zhengguo; Cai Shu; Yang Jingxia; Hong Zhanglian

    2012-01-01

    Nanocrystalline CdS thin films were deposited on glass substrates by an ammonia-free in-situ chemical reaction synthesis technique using cadmium cationic precursor solid films as reaction source and sodium sulfide based solutions as anionic reaction medium. Effects of ethanolamine addition to the cadmium cationic precursor solid films, deposition cycle numbers and annealing treatments in Ar atmosphere on structure, morphology, chemical composition and optical properties of the resultant films were investigated by X-ray diffraction, field emission scanning electron microscope, energy dispersive X-ray analysis and UV–Vis spectra measurements. The results show that CdS thin films deposited by the in-situ chemical reaction synthesis have wurtzite structure with (002) plane preferential orientation and crystallite size is in the range of 16 nm–19 nm. The growth of film thickness is almost constant with deposition cycle numbers and about 96 nm per cycle.

  18. A new in-situ method to determine the apparent gas diffusion coefficient of soils

    Science.gov (United States)

    Laemmel, Thomas; Paulus, Sinikka; Schack-Kirchner, Helmer; Maier, Martin

    2015-04-01

    Soil aeration is an important factor for the biological activity in the soil and soil respiration. Generally, gas exchange between soil and atmosphere is assumed to be governed by diffusion and Fick's Law is used to describe the fluxes in the soil. The "apparent soil gas diffusion coefficient" represents the proportional factor between the flux and the gas concentration gradient in the soil and reflects the ability of the soil to "transport passively" gases through the soil. One common way to determine this coefficient is to take core samples in the field and determine it in the lab. Unfortunately this method is destructive and needs laborious field work and can only reflect a small fraction of the whole soil. As a consequence insecurity about the resulting effective diffusivity on the profile scale must remain. We developed a new in-situ method using new gas sampling device, tracer gas and inverse soil gas modelling. The gas sampling device contains several sampling depths and can be easily installed into vertical holes of an auger, which allows for fast installation of the system. At the lower end of the device inert tracer gas is injected continuously. The tracer gas diffuses into the surrounding soil. The resulting distribution of the tracer gas concentrations is used to deduce the diffusivity profile of the soil. For Finite Element Modeling of the gas sampling device/soil system the program COMSOL is used. We will present the results of a field campaign comparing the new in-situ method with lab measurements on soil cores. The new sampling pole has several interesting advantages: it can be used in-situ and over a long time; so it allows following modifications of diffusion coefficients in interaction with rain but also vegetation cycle and wind.

  19. In-situ testing methods using radioactive tracers

    International Nuclear Information System (INIS)

    Sauzay, G.

    1976-01-01

    Some typical applications of tracer techniques in hydrology are presented: study of the extraction of sands and gravels in a estuary; in-situ study of the transport of sediments by the swell at a depth ranging from 8 to 22m; study of the transport of sands on the site Bonne Anse - Saint Palais [fr

  20. In situ reduction of as-prepared γ-Iron Oxide Nanoparticles

    DEFF Research Database (Denmark)

    Garbus, Pelle Gorm; Ahlburg, Jakob; Christensen, Mogens

    -ray diffraction measurement. The as-prepared maghemite nanoparticles were synthesized by the continuous decomposition of solutes in supercritical hydrothermal flow synthesis [3, 4]. The reagent used was ferric ammonium citrate (C6H8O7•xFe(III)•yNH3) that under hydrothermal flow synthesis decomposes into the γ......-iron oxide Fe2O3. The reduction of maghemite to body centered cubic (BCC) iron does not go through a detectable intermediate state.1.Jensen, K.M., et al., Mechanisms for iron oxide formation under hydrothermal conditions: an in situ total scattering study. ACS nano, 2014. 8(10): p. 10704-10714.2.Andersen, H...

  1. Absorption mechanism of three curcumin constituents through in situ intestinal perfusion method

    Directory of Open Access Journals (Sweden)

    Y.-H. Wang

    2017-09-01

    Full Text Available This study aimed to investigate the absorption mechanism of three curcumin constituents in rat small intestines. Self-emulsification was used to solubilize the three curcumin constituents, and the rat in situ intestinal perfusion method was used to study factors on drug absorption, including drug mass concentration, absorption site, and the different types and concentrations of absorption inhibitors. Within the scope of experimental concentrations, three curcumin constituents were absorbed in rat small intestines through the active transport mechanism.

  2. Case studies illustrating in-situ remediation methods for soil and groundwater contaminated with petrochemicals

    Energy Technology Data Exchange (ETDEWEB)

    Dixon, Robert A; Lance, P E; Downs, A; Kier, Brian P [EMCON Northwest Inc., Portland, OR (United States)

    1994-12-31

    Four case studies of successful in-situ remediation are summarized illustrating cost-effective methods to remediate soil and groundwater contaminated with volatile and non-volatile petrochemicals. Each site is in a different geologic environment with varying soil types and with and without groundwater impact. The methods described include vadose zone vapor extraction, high-vacuum vapor extraction combined with groundwater tab.le depression, air sparging with groundwater recovery and vapor extraction, and bio remediation of saturated zone soils using inorganic nutrient and oxygen addition

  3. Case studies illustrating in-situ remediation methods for soil and groundwater contaminated with petrochemicals

    Energy Technology Data Exchange (ETDEWEB)

    Dixon, Robert A.; Lance, P.E.; Downs, A.; Kier, Brian P. [EMCON Northwest Inc., Portland, OR (United States)

    1993-12-31

    Four case studies of successful in-situ remediation are summarized illustrating cost-effective methods to remediate soil and groundwater contaminated with volatile and non-volatile petrochemicals. Each site is in a different geologic environment with varying soil types and with and without groundwater impact. The methods described include vadose zone vapor extraction, high-vacuum vapor extraction combined with groundwater tab.le depression, air sparging with groundwater recovery and vapor extraction, and bio remediation of saturated zone soils using inorganic nutrient and oxygen addition

  4. Comparison study for the CCME reference method for determination of PHC in soil by using internal and external standard methods and by using silica gel column cleanup and in-situ silica gel cleanup methods

    International Nuclear Information System (INIS)

    Wang, Z.; Fingas, M.; Sigouin, L.; Yang, C.; Hollebone, B.

    2003-01-01

    The assessment, cleanup, and remediation of hydrocarbon contaminated sites is covered in the Reference Method for Canada-Wide Standard for Petroleum Hydrocarbons-Tier 1 Method. It replaces several analytical methods used in the past by some laboratories and jurisdictions in Canada. The authors conducted two comparative evaluations to validate the Tier 1 Analytical Method. The first compared the Internal and External Standard Methods, and the second compared the Silica Gel Column Cleanup Method with the In-situ Silica Gel Cleanup Method. The Canadian Council of Ministers of the Environment (CCME) Tier 1 Method recommends and requires the External Standard Method to determine petroleum hydrocarbons (PHC) in soil samples. The Internal Method is widely used to quantify various organic and inorganic pollutants in environmental samples. The Tier 1 Method offers two options for the same extract cleanup. They are: Option A - In-situ Silica Gel Cleanup, and Option B - Silica Gel Column Cleanup. Linearity, precision, and PHC quantification results were the parameters considered for diesel and motor oil solutions, for diesel spiked soil samples, and for motor oil spiked soil samples. It was concluded that both the External and Internal Standard Methods for gas chromatograph (GC) determination of PHC in soil possess their own advantages. The PHC results obtained using the In-Situ Silica Gel Cleanup Method were lower than those obtained with the Silica Gel Column Cleanup Methods. The more efficient and effective sample cleanup method proved to be the Silica Gel Column Method. 13 refs., 7 tabs., 7 figs

  5. Rapid synthesis of single-phase bismuth ferrite by microwave-assisted hydrothermal method

    Energy Technology Data Exchange (ETDEWEB)

    Cao, Wenqian [College of Materials Science and Engineering, China Jiliang University, 258 Xueyuan Street, Xiasha Higher Education District, Hangzhou 310018, Zhejiang Province (China); Chen, Zhi, E-mail: zchen0@gmail.com [College of Materials Science and Engineering, China Jiliang University, 258 Xueyuan Street, Xiasha Higher Education District, Hangzhou 310018, Zhejiang Province (China); Gao, Tong; Zhou, Dantong; Leng, Xiaonan; Niu, Feng [College of Materials Science and Engineering, China Jiliang University, 258 Xueyuan Street, Xiasha Higher Education District, Hangzhou 310018, Zhejiang Province (China); Zhu, Yuxiang [College of Materials Science and Engineering, China Jiliang University, 258 Xueyuan Street, Xiasha Higher Education District, Hangzhou 310018, Zhejiang Province (China); Tianjin Key Laboratory of Marine Resources and Chemistry, Tianjin University of Science and Technology, Tianjin (China); Qin, Laishun, E-mail: qinlaishun@yeah.net [College of Materials Science and Engineering, China Jiliang University, 258 Xueyuan Street, Xiasha Higher Education District, Hangzhou 310018, Zhejiang Province (China); Wang, Jiangying; Huang, Yuexiang [College of Materials Science and Engineering, China Jiliang University, 258 Xueyuan Street, Xiasha Higher Education District, Hangzhou 310018, Zhejiang Province (China)

    2016-06-01

    This paper describes on the fast synthesis of bismuth ferrite by the simple microwave-assisted hydrothermal method. The phase transformation and the preferred growth facets during the synthetic process have been investigated by X-ray diffraction. Bismuth ferrite can be quickly prepared by microwave hydrothermal method by simply controlling the reaction time, which is further confirmed by Fourier Transform infrared spectroscopy and magnetic measurement. - Graphical abstract: Single-phase BiFeO{sub 3} could be realized at a shortest reaction time of 65 min. The reaction time has strong influences on the phase transformation and the preferred growth facets. - Highlights: • Rapid synthesis (65 min) of BiFeO{sub 3} by microwave-assisted hydrothermal method. • Reaction time has influence on the purity and preferred growth facets. • FTIR and magnetic measurement further confirm the pure phase.

  6. Rapid synthesis of single-phase bismuth ferrite by microwave-assisted hydrothermal method

    International Nuclear Information System (INIS)

    Cao, Wenqian; Chen, Zhi; Gao, Tong; Zhou, Dantong; Leng, Xiaonan; Niu, Feng; Zhu, Yuxiang; Qin, Laishun; Wang, Jiangying; Huang, Yuexiang

    2016-01-01

    This paper describes on the fast synthesis of bismuth ferrite by the simple microwave-assisted hydrothermal method. The phase transformation and the preferred growth facets during the synthetic process have been investigated by X-ray diffraction. Bismuth ferrite can be quickly prepared by microwave hydrothermal method by simply controlling the reaction time, which is further confirmed by Fourier Transform infrared spectroscopy and magnetic measurement. - Graphical abstract: Single-phase BiFeO_3 could be realized at a shortest reaction time of 65 min. The reaction time has strong influences on the phase transformation and the preferred growth facets. - Highlights: • Rapid synthesis (65 min) of BiFeO_3 by microwave-assisted hydrothermal method. • Reaction time has influence on the purity and preferred growth facets. • FTIR and magnetic measurement further confirm the pure phase.

  7. In situ TEM electromechanical testing of nanowires and nanotubes.

    Science.gov (United States)

    Espinosa, Horacio D; Bernal, Rodrigo A; Filleter, Tobin

    2012-11-05

    The emergence of one-dimensional nanostructures as fundamental constituents of advanced materials and next-generation electronic and electromechanical devices has increased the need for their atomic-scale characterization. Given its spatial and temporal resolution, coupled with analytical capabilities, transmission electron microscopy (TEM) has been the technique of choice in performing atomic structure and defect characterization. A number of approaches have been recently developed to combine these capabilities with in-situ mechanical deformation and electrical characterization in the emerging field of in-situ TEM electromechanical testing. This has enabled researchers to establish unambiguous synthesis-structure-property relations for one-dimensional nanostructures. In this article, the development and latest advances of several in-situ TEM techniques to carry out mechanical and electromechanical testing of nanowires and nanotubes are reviewed. Through discussion of specific examples, it is shown how the merging of several microsystems and TEM has led to significant insights into the behavior of nanowires and nanotubes, underscoring the significant role in-situ techniques play in the development of novel nanoscale systems and materials. Copyright © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  8. Amide Synthesis from Alcohols and Amines by the Extrusion of Dihydrogen

    DEFF Research Database (Denmark)

    Nordstrøm, Lars Ulrik Rubæk; Vogt, Henning; Madsen, R.

    2008-01-01

    An environmentally friendly method for synthesis of amides is presented where a simple ruthenium catalyst mediates the direct coupling between an alcohol and an amine with the liberation of two molecules of dihydrogen. The active catalyst is generated in situ from an easily available ruthenium...... complex, an N-heterocyclic carbene and a phosphine. The reaction allows primary alcohols to be coupled with primary alkyamines to afford the corresponding secondary amides in good yields. The amide formation presumably proceeds through a catalytic cycle where the intermediate aldehyde and hemiaminal...

  9. Building block synthesis using the polymerase chain assembly method.

    Science.gov (United States)

    Marchand, Julie A; Peccoud, Jean

    2012-01-01

    De novo gene synthesis allows the creation of custom DNA molecules without the typical constraints of traditional cloning assembly: scars, restriction site incompatibility, and the quest to find all the desired parts to name a few. Moreover, with the help of computer-assisted design, the perfect DNA molecule can be created along with its matching sequence ready to download. The challenge is to build the physical DNA molecules that have been designed with the software. Although there are several DNA assembly methods, this section presents and describes a method using the polymerase chain assembly (PCA).

  10. Methods for synthesis of semiconductor nanocrystals and thermoelectric compositions

    Science.gov (United States)

    Chen, Gang (Inventor); Poudel, Bed (Inventor); Kumar, Shankar (Inventor); Dresselhaus, Mildred (Inventor); Ren, Zhifeng (Inventor); Wang, Wenzhong (Inventor)

    2007-01-01

    The present invention provides methods for synthesis of IV VI nanostructures, and thermoelectric compositions formed of such structures. In one aspect, the method includes forming a solution of a Group IV reagent, a Group VI reagent and a surfactant. A reducing agent can be added to the solution, and the resultant solution can be maintained at an elevated temperature, e.g., in a range of about 20.degree. C. to about 360.degree. C., for a duration sufficient for generating nanoparticles as binary alloys of the IV VI elements.

  11. Sample-based engine noise synthesis using an enhanced pitch-synchronous overlap-and-add method.

    Science.gov (United States)

    Jagla, Jan; Maillard, Julien; Martin, Nadine

    2012-11-01

    An algorithm for the real time synthesis of internal combustion engine noise is presented. Through the analysis of a recorded engine noise signal of continuously varying engine speed, a dataset of sound samples is extracted allowing the real time synthesis of the noise induced by arbitrary evolutions of engine speed. The sound samples are extracted from a recording spanning the entire engine speed range. Each sample is delimitated such as to contain the sound emitted during one cycle of the engine plus the necessary overlap to ensure smooth transitions during the synthesis. The proposed approach, an extension of the PSOLA method introduced for speech processing, takes advantage of the specific periodicity of engine noise signals to locate the extraction instants of the sound samples. During the synthesis stage, the sound samples corresponding to the target engine speed evolution are concatenated with an overlap and add algorithm. It is shown that this method produces high quality audio restitution with a low computational load. It is therefore well suited for real time applications.

  12. Development of new methods in modern selective organic synthesis: preparation of functionalized molecules with atomic precision

    International Nuclear Information System (INIS)

    Ananikov, V P; Khemchyan, L L; Ivanova, Yu V; Dilman, A D; Levin, V V; Bukhtiyarov, V I; Sorokin, A M; Prosvirin, I P; Romanenko, A V; Simonov, P A; Vatsadze, S Z; Medved'ko, A V; Nuriev, V N; Nenajdenko, V G; Shmatova, O I; Muzalevskiy, V M; Koptyug, I V; Kovtunov, K V; Zhivonitko, V V; Likholobov, V A

    2014-01-01

    The challenges of the modern society and the growing demand of high-technology sectors of industrial production bring about a new phase in the development of organic synthesis. A cutting edge of modern synthetic methods is introduction of functional groups and more complex structural units into organic molecules with unprecedented control over the course of chemical transformation. Analysis of the state-of-the-art achievements in selective organic synthesis indicates the appearance of a new trend — the synthesis of organic molecules, biologically active compounds, pharmaceutical substances and smart materials with absolute selectivity. Most advanced approaches to organic synthesis anticipated in the near future can be defined as 'atomic precision' in chemical reactions. The present review considers selective methods of organic synthesis suitable for transformation of complex functionalized molecules under mild conditions. Selected key trends in the modern organic synthesis are considered including the preparation of organofluorine compounds, catalytic cross-coupling and oxidative cross-coupling reactions, atom-economic addition reactions, methathesis processes, oxidation and reduction reactions, synthesis of heterocyclic compounds, design of new homogeneous and heterogeneous catalytic systems, application of photocatalysis, scaling up synthetic procedures to industrial level and development of new approaches to investigation of mechanisms of catalytic reactions. The bibliography includes 840 references

  13. 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

  14. Heterotopic cardiac transplantation decreases the capacity for rat myocardial protein synthesis

    International Nuclear Information System (INIS)

    Klein, I.; Samarel, A.M.; Welikson, R.; Hong, C.

    1991-01-01

    Heterotopic cardiac isografts are vascularly perfused hearts that maintain structural and functional integrity for prolonged periods of time. When placed in an infrarenal location, the heart is hemodynamically unloaded and undergoes negative growth, leading to cardiac atrophy. At 7 and 14 days after transplantation, the transplanted heart was decreased in size compared with the in situ heart (p less than 0.001). To assess the possible mechanism(s) to account for this reduction in size we studied in vivo rates of total left ventricular (LV) protein synthesis, total LV RNA content, and 18S ribosomal RNA content by nucleic acid hybridization. The LV protein synthetic rate was 4.7 and 5.3 mg/day in the in situ heart and was significantly decreased to 2.9 and 2.7 mg/day in the transplanted hearts at 7 and 14 days, respectively. LV RNA content of the transplant declined to 53% and 48% of the in situ value at 7 and 14 days, respectively. Hybridization studies revealed that LV 18S ribosomal subunit content was reduced proportionately to total RNA in the heterotopic hearts. As a result of these changes, there was no significant difference in the efficiency of total LV protein synthesis between the in situ and transplanted hearts. The present studies demonstrate that the hemodynamic unloading and cardiac atrophy that is characteristic of heterotopic cardiac transplantation is accompanied by a decrease in LV total RNA content and 18S RNA, resulting in a decreased capacity for myocardial protein synthesis

  15. Method for local temperature measurement in a nanoreactor for in situ high-resolution electron microscopy.

    Science.gov (United States)

    Vendelbo, S B; Kooyman, P J; Creemer, J F; Morana, B; Mele, L; Dona, P; Nelissen, B J; Helveg, S

    2013-10-01

    In situ high-resolution transmission electron microscopy (TEM) of solids under reactive gas conditions can be facilitated by microelectromechanical system devices called nanoreactors. These nanoreactors are windowed cells containing nanoliter volumes of gas at ambient pressures and elevated temperatures. However, due to the high spatial confinement of the reaction environment, traditional methods for measuring process parameters, such as the local temperature, are difficult to apply. To address this issue, we devise an electron energy loss spectroscopy (EELS) method that probes the local temperature of the reaction volume under inspection by the electron beam. The local gas density, as measured using quantitative EELS, is combined with the inherent relation between gas density and temperature, as described by the ideal gas law, to obtain the local temperature. Using this method we determined the temperature gradient in a nanoreactor in situ, while the average, global temperature was monitored by a traditional measurement of the electrical resistivity of the heater. The local gas temperatures had a maximum of 56 °C deviation from the global heater values under the applied conditions. The local temperatures, obtained with the proposed method, are in good agreement with predictions from an analytical model. Copyright © 2013 Elsevier B.V. All rights reserved.

  16. In-situ uranium leaching

    International Nuclear Information System (INIS)

    Dotson, B.J.

    1986-01-01

    This invention provides a method for improving the recovery of mineral values from ore bodies subjected to in-situ leaching by controlling the flow behaviour of the leaching solution. In particular, the invention relates to an in-situ leaching operation employing a foam for mobility control of the leaching solution. A foam bank is either introduced into the ore bed or developed in-situ in the ore bed. The foam then becomes a diverting agent forcing the leaching fluid through the previously non-contacted regions of the deposit

  17. In situ synthesis, characterization, and catalytic performance of tungstophosphoric acid encapsulated into the framework of mesoporous silica pillared clay.

    Science.gov (United States)

    Li, Baoshan; Liu, Zhenxing; Han, Chunying; Ma, Wei; Zhao, Songjie

    2012-07-01

    Mesoporous silica pillared clay (SPC) incorporated with tungstophosphoric acid (HPW) has been synthesized via in situ introducing P and W source in the acidic suspension of the clay interlayer template during the formation of the silica pillared clay. The samples were characterized by XRD, XRF, FT-IR, TG-DTA, N(2) adsorption-desorption, and SEM techniques. The results showed that the HPW formed by in situ method has been effectively introduced into the framework of mesoporous silica pillared clay and its Keggin structure remained perfectly after formation of the materials. In addition, samples with similar HPW loadings were also prepared by impregnation method using SPC as the support. HPW in the incorporated samples was better dispersed into the silica pillared clay than in the impregnated samples. The results of catalytic tests indicated that the encapsulated materials demonstrated better catalytic performance than the impregnated samples in oxidative desulfurization (ODS) of dibenzothiophene (DBT). Copyright © 2012 Elsevier Inc. All rights reserved.

  18. Scalable Analysis Methods and In Situ Infrastructure for Extreme Scale Knowledge Discovery

    Energy Technology Data Exchange (ETDEWEB)

    Bethel, Wes [Lawrence Berkeley National Lab. (LBNL), Berkeley, CA (United States)

    2016-07-24

    The primary challenge motivating this team’s work is the widening gap between the ability to compute information and to store it for subsequent analysis. This gap adversely impacts science code teams, who are able to perform analysis only on a small fraction of the data they compute, resulting in the very real likelihood of lost or missed science, when results are computed but not analyzed. Our approach is to perform as much analysis or visualization processing on data while it is still resident in memory, an approach that is known as in situ processing. The idea in situ processing was not new at the time of the start of this effort in 2014, but efforts in that space were largely ad hoc, and there was no concerted effort within the research community that aimed to foster production-quality software tools suitable for use by DOE science projects. In large, our objective was produce and enable use of production-quality in situ methods and infrastructure, at scale, on DOE HPC facilities, though we expected to have impact beyond DOE due to the widespread nature of the challenges, which affect virtually all large-scale computational science efforts. To achieve that objective, we assembled a unique team of researchers consisting of representatives from DOE national laboratories, academia, and industry, and engaged in software technology R&D, as well as engaged in close partnerships with DOE science code teams, to produce software technologies that were shown to run effectively at scale on DOE HPC platforms.

  19. Enhanced Enzymatic Production of Cephalexin at High Substrate Concentration with in situ Product Removal by Complexation

    Directory of Open Access Journals (Sweden)

    Dengchao Li

    2008-01-01

    Full Text Available Cephalexin (CEX was synthesized with 7-amino-3-deacetoxycephalosporanic acid (7-ADCA and D(–-phenylglycine methyl ester (PGME using immobilized penicillin G acylase from Escherichia coli. It was found that substrate concentration and in situ product could remarkably influence the ratio of synthesis to hydrolysis (S/H and the efficiency of CEX synthesis. The optimal ratio of enzyme to substrate was 65 IU/mM 7-ADCA. High substrate concentration improved the 7-ADCA conversion from 61 to 81 % in the process without in situ product removal (ISPR, while in the synthetic process with ISPR, high substrate concentration increased the 7-ADCA conversion from 88 to 98 %. CEX was easily separated from CEX/β-naphthol complex and its purity and overall yield were 99 and 70 %, respectively.

  20. A novel fabrication technology of in situ TiB2/6063Al composites: High energy ball milling and melt in situ reaction

    International Nuclear Information System (INIS)

    Zhang, S.-L.; Yang, J.; Zhang, B.-R.; Zhao, Y.-T.; Chen, G.; Shi, X.-X.; Liang, Z.-P.

    2015-01-01

    Highlights: • This paper presents a novel technology to fabricate the TiB 2 /6063Al composites. • The novel technology decreases in situ reaction temperature and shortens the time. • The reaction mechanism of in situ reaction at the low temperature is discussed. • Effect of ball milling time and in situ reaction time on the composites is studied. - Abstract: TiB 2 /6063Al matrix composites are fabricated from Al–TiO 2 –B 2 O 3 system by the technology combining high energy ball milling with melt in situ reaction. The microstructure and tensile properties of the composites are investigated by XRD, SEM, EDS, TEM and electronic tensile testing. The results indicate that high energy ball milling technology decreases the in situ reaction temperature and shortens the reaction time for Al–TiO 2 –B 2 O 3 system in contrast with the conventional melt in situ synthesis. The morphology of in situ TiB 2 particles is exhibited in irregular shape or nearly circular shape, and the average size of the particles is less than 700 nm, thereinto the minimum size is approximately 200 nm. In addition, the morphology and size of the reinforced particles are affected by the time of ball milling and in situ reaction. TEM images indicate that the interface between 6063Al matrix and TiB 2 particles is clear and no interfacial outgrowth is observed. Tensile testing results show that the as-cast TiB 2 /6063Al composites exhibit a much higher strength, reaching 191 MPa, which is 1.23 times as high as the as-cast 6063Al matrix. Besides, the tensile fracture surface of the composites displays the dimple-fracture character

  1. Phosphorene – The two-dimensional black phosphorous: Properties, synthesis and applications

    International Nuclear Information System (INIS)

    Khandelwal, Apratim; Mani, Karthick; Karigerasi, Manohar Harsha; Lahiri, Indranil

    2017-01-01

    Highlights: • Reviews recent progress in phosphorene research, a new 2D material. • Anisotropic properties are reviewed and compared with other 2D materials. • Synthesis methods of black phosphorus and phosphorene are discussed. • Prospective applications inspired from the intrinsic properties are also discussed. • Challenges and future scope for this promising material is included. - Abstract: Black phosphorus (BP) is known to human beings for almost a century. It started receiving more attention of scientists and researchers worldwide in last three years, with its ability to exist in two-dimensional (2D) form, popularly known as phosphorene. In the post-graphene-discovery period, phosphorene is probably receiving most attention, owing to its excellent properties and hence, high potential for practical applications in the field of electronics, energy and infrastructure. In this article, attractive properties of phosphorene, which makes it unique and comparable with graphene or transition metal dichalcogenides (TMDs), are highlighted. As the question of its environmental instability remains critical, a comprehensive overview of synthesis methods of phosphorene and black phosphorus are presented, to inspire in-situ methods of phosphorene synthesis and fabrication towards improving further investigation into this wonder material. In addition, the article also focuses on opportunities in nano-electronics, optoelectronics, energy conversion/storage, sensors etc arising from phosphorene’s remarkable properties.

  2. Phosphorene – The two-dimensional black phosphorous: Properties, synthesis and applications

    Energy Technology Data Exchange (ETDEWEB)

    Khandelwal, Apratim; Mani, Karthick; Karigerasi, Manohar Harsha; Lahiri, Indranil, E-mail: indrafmt@iitr.ac.in

    2017-07-15

    Highlights: • Reviews recent progress in phosphorene research, a new 2D material. • Anisotropic properties are reviewed and compared with other 2D materials. • Synthesis methods of black phosphorus and phosphorene are discussed. • Prospective applications inspired from the intrinsic properties are also discussed. • Challenges and future scope for this promising material is included. - Abstract: Black phosphorus (BP) is known to human beings for almost a century. It started receiving more attention of scientists and researchers worldwide in last three years, with its ability to exist in two-dimensional (2D) form, popularly known as phosphorene. In the post-graphene-discovery period, phosphorene is probably receiving most attention, owing to its excellent properties and hence, high potential for practical applications in the field of electronics, energy and infrastructure. In this article, attractive properties of phosphorene, which makes it unique and comparable with graphene or transition metal dichalcogenides (TMDs), are highlighted. As the question of its environmental instability remains critical, a comprehensive overview of synthesis methods of phosphorene and black phosphorus are presented, to inspire in-situ methods of phosphorene synthesis and fabrication towards improving further investigation into this wonder material. In addition, the article also focuses on opportunities in nano-electronics, optoelectronics, energy conversion/storage, sensors etc arising from phosphorene’s remarkable properties.

  3. Facile method for the synthesis of gold nanoparticles using an ion coater

    Science.gov (United States)

    Lee, Seung Han; Jung, Hyun Kyu; Kim, Tae Cheol; Kim, Chang Hee; Shin, Chang Hwan; Yoon, Tae-Sik; Hong, A.-Ra; Jang, Ho Seong; Kim, Dong Hun

    2018-03-01

    Herein we report a metal nanoparticle synthesis method based on a physical vapor deposition process instead of the conventional wet process of chemical reactions in liquids. A narrow size distribution of synthesized gold nanoparticles was obtained using an ion coater on glycerin at low vapor pressure. The nanoparticle size could be modulated by controlling the sputtering conditions especially the discharge current. Due to the formation of gold nanoparticles, a surface plasmon resonance peak appeared at ∼530 nm in the absorption spectrum. The surface plasmon resonance peak exhibited red-shift with increasing size of the gold nanoparticles. Our results provide a simple, environmental friendly method for the synthesis of metal nanoparticles by combine low-cost deposition apparatus and a liquid medium, which is free from toxic reagents.

  4. Synthesis of core-shell heterostructured Cu/Cu2O nanowires monitored by in situ XRD as efficient visible-light photocatalysts

    KAUST Repository

    Chen, Wei

    2013-01-01

    Core-shell heterostructured Cu/Cu2O nanowires with a high aspect ratio were synthesized from Cu foam using a novel oxidation/reduction process. In situ XRD was used as an efficient tool to acquire phase transformation details during the temperature-programmed oxidation of Cu foam and the subsequent reduction process. Based on knowledge of the crucial phase transformation, optimal synthesis conditions for producing high-quality CuO and core-shell Cu/Cu2O nanowires were determined. In favor of efficient charge separation induced by the special core-shell heterostructure and the advanced three-dimensional spatial configuration, Cu/Cu2O nanowires exhibited superior visible-light activity in the degradation of methylene blue. The present study illustrates a novel strategy for fabricating efficiently core-shell heterostructured nanowires and provides the potential for developing their applications in electronic devices, for environmental remediation and in solar energy utilization fields. This journal is © The Royal Society of Chemistry.

  5. In situ synthesis of NiAl–NbB2 composite powder through combustion synthesis

    International Nuclear Information System (INIS)

    Shokati, Ali Akbar; Parvin, Nader; Sabzianpour, Naser; Shokati, Mohammad; Hemmati, Ali

    2013-01-01

    Highlights: ► A Novel NiAl matrix composite powder with 0–40 wt.% NbB 2 was synthesized. ► Composite powders were synthesized by thermal explosion reaction of Ni–Al–Nb–B system. ► Microhardness of NiAl considerably increased with raising NbB 2 content. ► Synthesized composite powders is a good candidate as precursor for thermal barrier application. - Abstract: Synthesis of a novel NiAl matrix composite powder reinforced with 0–40 wt.% NbB 2 by combustion synthesis in thermal explosion mode was investigated. The elemental powders of Ni, Al, Nb, and amorphous boron were used as starting material. For all compositions final products consisted of only the NiAl and NbB 2 phases. Coarser NbB 2 with a relatively uniform distribution in NiAl matrix was formed with rising NbB 2 content. Microhardness of NiAl considerably increased from 377 ± 13 HV 0.05 to 866 ± 81 HV 0.05 for NiAl with 40 wt.% NbB 2 . High microhardness, proper size and distribution of NbB 2 in NiAl matrix make it a good candidate as precursor for thermal spray application.

  6. Enhanced active aluminum content and thermal behaviour of nano-aluminum particles passivated during synthesis using thermal plasma route

    International Nuclear Information System (INIS)

    Mathe, Vikas L.; Varma, Vijay; Raut, Suyog; Nandi, Amiya Kumar; Pant, Arti; Prasanth, Hima; Pandey, R.K.; Bhoraskar, Sudha V.; Das, Asoka K.

    2016-01-01

    Graphical abstract: - Highlights: • Synthesis of nano crystalline Al (nAl) using DC thermal plasma reactor. • In situ passivation of nAl by palmitic acid and air. • Enhanced active aluminum content obtained for palmitic acid passivated nAl. • Palmitic acid passivated nAl are quite stable in humid atmospheres. - Abstract: Here, we report synthesis and in situ passivation of aluminum nanoparticles using thermal plasma reactor. Both air and palmitc acid passivation was carried out during the synthesis in the thermal plasma reactor. The passivated nanoparticles have been characterized for their structural and morphological properties using X-ray diffraction (XRD) and transmission electron microscopy (TEM) techniques. In order to understand nature of passivation vibrational spectroscopic analysis have been carried out. The enhancement in active aluminum content and shelf life for a palmitic acid passivated nano-aluminum particles in comparison to the air passivated samples and commercially available nano Al powder (ALEX) has been observed. Thermo-gravimetric analysis was used to estimate active aluminum content of all the samples under investigation. In addition cerimetric back titration method was also used to estimate AAC and the shelf life of passivated aluminum particles. Structural, microstructural and thermogravomateric analysis of four year aged passivated sample also depicts effectiveness of palmitic acid passivation.

  7. Enhanced active aluminum content and thermal behaviour of nano-aluminum particles passivated during synthesis using thermal plasma route

    Energy Technology Data Exchange (ETDEWEB)

    Mathe, Vikas L., E-mail: vlmathe@physics.unipune.ac.in [Department of Physics, Savitribai Phule Pune University, Pune 411007, Maharashtra (India); Varma, Vijay; Raut, Suyog [Department of Physics, Savitribai Phule Pune University, Pune 411007, Maharashtra (India); Nandi, Amiya Kumar; Pant, Arti; Prasanth, Hima; Pandey, R.K. [High Energy Materials Research Lab, Sutarwadi, Pune 411021, Maharashtra (India); Bhoraskar, Sudha V. [Department of Physics, Savitribai Phule Pune University, Pune 411007, Maharashtra (India); Das, Asoka K. [Utkal University, VaniVihar, Bhubaneswar, Odisha 751004 (India)

    2016-04-15

    Graphical abstract: - Highlights: • Synthesis of nano crystalline Al (nAl) using DC thermal plasma reactor. • In situ passivation of nAl by palmitic acid and air. • Enhanced active aluminum content obtained for palmitic acid passivated nAl. • Palmitic acid passivated nAl are quite stable in humid atmospheres. - Abstract: Here, we report synthesis and in situ passivation of aluminum nanoparticles using thermal plasma reactor. Both air and palmitc acid passivation was carried out during the synthesis in the thermal plasma reactor. The passivated nanoparticles have been characterized for their structural and morphological properties using X-ray diffraction (XRD) and transmission electron microscopy (TEM) techniques. In order to understand nature of passivation vibrational spectroscopic analysis have been carried out. The enhancement in active aluminum content and shelf life for a palmitic acid passivated nano-aluminum particles in comparison to the air passivated samples and commercially available nano Al powder (ALEX) has been observed. Thermo-gravimetric analysis was used to estimate active aluminum content of all the samples under investigation. In addition cerimetric back titration method was also used to estimate AAC and the shelf life of passivated aluminum particles. Structural, microstructural and thermogravomateric analysis of four year aged passivated sample also depicts effectiveness of palmitic acid passivation.

  8. The method for the in-situ leaching of a uranium mining

    International Nuclear Information System (INIS)

    Chen Zhen; Xu Xianyi; Wang Xuemin

    2011-01-01

    The paper reviews the main factors of in-situ leaching for uranium mining. A kind of technique called dilution with few reagent is put forward to the in-situ leaching of sandstone-type uranium deposit with high TDS. This technique can not only effectively prevent the pipe plug, but also can improve the economic benefits. (authors)

  9. Optimization of One-Step In Situ Transesterification Method for Accurate Quantification of EPA in Nannochloropsis gaditana

    Directory of Open Access Journals (Sweden)

    Yuting Tang

    2016-11-01

    Full Text Available Microalgae are a valuable source of lipid feedstocks for biodiesel and valuable omega-3 fatty acids. Nannochloropsis gaditana has emerged as a promising producer of eicosapentaenoic acid (EPA due to its fast growth rate and high EPA content. In the present study, the fatty acid profile of Nannochloropsis gaditana was found to be naturally high in EPA and devoid of docosahexaenoic acid (DHA, thereby providing an opportunity to maximize the efficacy of EPA production. Using an optimized one-step in situ transesterification method (methanol:biomass = 90 mL/g; HCl 5% by vol.; 70 °C; 1.5 h, the maximum fatty acid methyl ester (FAME yield of Nannochloropsis gaditana cultivated under rich condition was quantified as 10.04% ± 0.08% by weight with EPA-yields as high as 4.02% ± 0.17% based on dry biomass. The total FAME and EPA yields were 1.58- and 1.23-fold higher separately than that obtained using conventional two-step method (solvent system: methanol and chloroform. This one-step in situ method provides a fast and simple method to measure fatty acid methyl ester (FAME yields and could serve as a promising method to generate eicosapentaenoic acid methyl ester from microalgae.

  10. Synthesis, thermal properties and applications of polymer-clay nanocomposites

    International Nuclear Information System (INIS)

    Meneghetti, Paulo; Qutubuddin, Syed

    2006-01-01

    Polymer-clay nanocomposites constitute a new class of materials in which the polymer matrix is reinforced by uniformly dispersed inorganic particles (usually 10 wt.% or less) having at least one dimension in the nanometer scale. Nanocomposites exhibit improved properties when compared to pure polymer or conventional composites, such as enhanced mechanical and thermal properties, reduced gas permeability, and improved chemical stability. In this work, the synthesis of poly(methyl methacrylate) (PMMA)/clay nanocomposites is described via two methods: in situ and emulsion polymerization. The in situ technique follows a two-step process: ion-exchange of the clay to make it hydrophobic, and polymerization after dispersing the functionalized clay in the monomer. The emulsion technique combines the two steps of the in situ method into one by conducting ion-exchange and polymerization in an aqueous medium in the same reactor. The clay (montmorillonite, MMT) is functionalized with a zwitterionic surfactant, octadecyl-dimethyl betaine (C18DMB). Partially exfoliated nanocomposite, observed by transmission electron microscopy (TEM), was obtained by emulsion polymerization with 10 wt.% clay. Glass transition temperature (T g ) of this nanocomposite was 18 deg. C higher than pure PMMA. With the same clay content, in situ polymerization produced intercalated nanocomposite with T g 10 deg. C lower than the emulsion nanocomposite. The storage modulus of partially exfoliated nanocomposite was superior to the intercalated structure and to the pure polymer. Using nanocomposite technology, novel PMMA nanocomposite gel electrolytes were synthesized exhibiting improved ionic conductivity and stable lithium interfacial resistance. Nanocomposites can also be used for gas storage and packaging applications as demonstrated by high barrier polymer-clay films

  11. Synthesis, thermal properties and applications of polymer-clay nanocomposites

    Energy Technology Data Exchange (ETDEWEB)

    Meneghetti, Paulo [Chemical Engineering Department, Case Western Reserve University, 10900 Euclid Ave. Cleveland, OH 44106 (United States); Qutubuddin, Syed [Chemical Engineering Department, Case Western Reserve University, 10900 Euclid Ave. Cleveland, OH 44106 (United States)]. E-mail: sxq@case.edu

    2006-03-15

    Polymer-clay nanocomposites constitute a new class of materials in which the polymer matrix is reinforced by uniformly dispersed inorganic particles (usually 10 wt.% or less) having at least one dimension in the nanometer scale. Nanocomposites exhibit improved properties when compared to pure polymer or conventional composites, such as enhanced mechanical and thermal properties, reduced gas permeability, and improved chemical stability. In this work, the synthesis of poly(methyl methacrylate) (PMMA)/clay nanocomposites is described via two methods: in situ and emulsion polymerization. The in situ technique follows a two-step process: ion-exchange of the clay to make it hydrophobic, and polymerization after dispersing the functionalized clay in the monomer. The emulsion technique combines the two steps of the in situ method into one by conducting ion-exchange and polymerization in an aqueous medium in the same reactor. The clay (montmorillonite, MMT) is functionalized with a zwitterionic surfactant, octadecyl-dimethyl betaine (C18DMB). Partially exfoliated nanocomposite, observed by transmission electron microscopy (TEM), was obtained by emulsion polymerization with 10 wt.% clay. Glass transition temperature (T {sub g}) of this nanocomposite was 18 deg. C higher than pure PMMA. With the same clay content, in situ polymerization produced intercalated nanocomposite with T {sub g} 10 deg. C lower than the emulsion nanocomposite. The storage modulus of partially exfoliated nanocomposite was superior to the intercalated structure and to the pure polymer. Using nanocomposite technology, novel PMMA nanocomposite gel electrolytes were synthesized exhibiting improved ionic conductivity and stable lithium interfacial resistance. Nanocomposites can also be used for gas storage and packaging applications as demonstrated by high barrier polymer-clay films.

  12. Thiolated xyloglucan: Synthesis, characterization and evaluation as mucoadhesive in situ gelling agent.

    Science.gov (United States)

    Mahajan, Hitendra S; Tyagi, Vinod Kumar; Patil, Ravindra R; Dusunge, Sanket B

    2013-01-16

    The objective of present study was to enhance bioadhesive potential of xyloglucan by thiolation. Thiolation of xyloglucan was achieved with esterification with thioglycolic acid. Thiolated xyloglucan was characterized by NMR, DSC, and XRD analysis. Thiolated xyloglucan was determined to possess 4mmol of thiol groups/g of polymer by Ellman's method. Comparative evaluation of mucoadhesive property of ondansetron containing in situ gel system of xyloglucan and thiolated xyloglucan using sheep nasal mucosa revealed higher ex vivo bioadhesion time of thiolated xyloglucan as compared to xyloglucan. Improved mucoadhesive property of thiolated xyloglucan over the xyloglucan can be attributed to the formation of disulfide bond between mucus and thiolated xyloglucan. Ex vivo permeation study conducted using sheep nasal showed improved drug permeation in formulation based on thiolated xyloglucan. In conclusion, thiolation of xyloglucan improves its bioadhesion and drug permeation without affecting the resultant gel properties. Copyright © 2012 Elsevier Ltd. All rights reserved.

  13. Measuring serotonin synthesis: from conventional methods to PET tracers and their (pre)clinical implications

    Energy Technology Data Exchange (ETDEWEB)

    Visser, Anniek K.D.; Waarde, Aren van; Willemsen, Antoon T.M. [University of Groningen, University Medical Center Groningen, Department of Nuclear Medicine and Molecular Imaging, Groningen (Netherlands); Bosker, Fokko J. [University of Groningen, University Medical Center Groningen, University Center of Psychiatry, Groningen (Netherlands); Luiten, Paul G.M. [University of Groningen, Center for Behavior and Neurosciences, Department of Molecular Neurobiology, Haren (Netherlands); Boer, Johan A. den [University of Groningen, University Medical Center Groningen, Department of Nuclear Medicine and Molecular Imaging, Groningen (Netherlands); University of Groningen, University Medical Center Groningen, University Center of Psychiatry, Groningen (Netherlands); Kema, Ido P. [University of Groningen, University Medical Center Groningen, Department of Laboratory Medicine, Groningen (Netherlands); Dierckx, Rudi A.J.O. [University of Groningen, University Medical Center Groningen, Department of Nuclear Medicine and Molecular Imaging, Groningen (Netherlands); University Hospital Ghent, Department of Nuclear Medicine, Ghent (Belgium)

    2011-03-15

    The serotonergic system of the brain is complex, with an extensive innervation pattern covering all brain regions and endowed with at least 15 different receptors (each with their particular distribution patterns), specific reuptake mechanisms and synthetic processes. Many aspects of the functioning of the serotonergic system are still unclear, partially because of the difficulty of measuring physiological processes in the living brain. In this review we give an overview of the conventional methods of measuring serotonin synthesis and methods using positron emission tomography (PET) tracers, more specifically with respect to serotonergic function in affective disorders. Conventional methods are invasive and do not directly measure synthesis rates. Although they may give insight into turnover rates, a more direct measurement may be preferred. PET is a noninvasive technique which can trace metabolic processes, like serotonin synthesis. Tracers developed for this purpose are {alpha}-[{sup 11}C]methyltryptophan ([{sup 11}C]AMT) and 5-hydroxy-L-[{beta}-{sup 11}C]tryptophan ([{sup 11}C]5-HTP). Both tracers have advantages and disadvantages. [{sup 11}C]AMT can enter the kynurenine pathway under inflammatory conditions (and thus provide a false signal), but this tracer has been used in many studies leading to novel insights regarding antidepressant action. [{sup 11}C]5-HTP is difficult to produce, but trapping of this compound may better represent serotonin synthesis. AMT and 5-HTP kinetics are differently affected by tryptophan depletion and changes of mood. This may indicate that both tracers are associated with different enzymatic processes. In conclusion, PET with radiolabelled substrates for the serotonergic pathway is the only direct way to detect changes of serotonin synthesis in the living brain. (orig.)

  14. A novel fabrication technology of in situ TiB{sub 2}/6063Al composites: High energy ball milling and melt in situ reaction

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, S.-L.; Yang, J. [School of Materials Science and Engineering, Jiangsu University, Zhenjiang, Jiangsu 212013 (China); Zhang, B.-R. [School of Mechanical Engineering, Qilu University of Technology, Jinan, Shandong 250022 (China); Zhao, Y.-T., E-mail: 278075525@qq.com [School of Materials Science and Engineering, Jiangsu University, Zhenjiang, Jiangsu 212013 (China); Chen, G.; Shi, X.-X.; Liang, Z.-P. [School of Materials Science and Engineering, Jiangsu University, Zhenjiang, Jiangsu 212013 (China)

    2015-08-05

    Highlights: • This paper presents a novel technology to fabricate the TiB{sub 2}/6063Al composites. • The novel technology decreases in situ reaction temperature and shortens the time. • The reaction mechanism of in situ reaction at the low temperature is discussed. • Effect of ball milling time and in situ reaction time on the composites is studied. - Abstract: TiB{sub 2}/6063Al matrix composites are fabricated from Al–TiO{sub 2}–B{sub 2}O{sub 3} system by the technology combining high energy ball milling with melt in situ reaction. The microstructure and tensile properties of the composites are investigated by XRD, SEM, EDS, TEM and electronic tensile testing. The results indicate that high energy ball milling technology decreases the in situ reaction temperature and shortens the reaction time for Al–TiO{sub 2}–B{sub 2}O{sub 3} system in contrast with the conventional melt in situ synthesis. The morphology of in situ TiB{sub 2} particles is exhibited in irregular shape or nearly circular shape, and the average size of the particles is less than 700 nm, thereinto the minimum size is approximately 200 nm. In addition, the morphology and size of the reinforced particles are affected by the time of ball milling and in situ reaction. TEM images indicate that the interface between 6063Al matrix and TiB{sub 2} particles is clear and no interfacial outgrowth is observed. Tensile testing results show that the as-cast TiB{sub 2}/6063Al composites exhibit a much higher strength, reaching 191 MPa, which is 1.23 times as high as the as-cast 6063Al matrix. Besides, the tensile fracture surface of the composites displays the dimple-fracture character.

  15. A simple enzymic method for the synthesis of [32P]phosphoenolpyruvate

    International Nuclear Information System (INIS)

    Parra, F.

    1982-01-01

    A rapid and simple enzymic method is described for the synthesis of [ 32 P]phosphoenolpyruvate from [ 32 P]Psub(i), with a reproducible yield of 74%. The final product was shown to be a good substrate for pyruvate kinase (EC 2.7.1.40). (author)

  16. Experimental and mathematical simulation techniques for determining an in-situ response testing method for neutron sensors used in reactor power plant protection systems

    International Nuclear Information System (INIS)

    Behbahani, A.

    1983-01-01

    An analytical neutron sensor response model and methods for transient response measurements of neutron sensors (compensated ionization chamber), including possible in-situ techniques have been developed and evaluated to meet the provisions of Draft Standard ISA Sd67.06, IEEE 338-1977, and NRC Guide 1.118. One in-situ method requires the perturbation of the high voltage detector (sensor) power supply and measurement of the sensor response. The response to a perturbation of the power supply is related to the response of the sensor to a transient change in neutron flux. Random signal analysis is another in-situ technique to monitor the neutron sensor response. In this method the power spectrum of the inherent fluctuations from the neutron sensor output (current in CIC) are measured and evaluated. Transient response techniques (including in-situ methods) are experimentally and analytically evaluated to identify the mechanisms which may cause degradation in the response of the neutron sensors. The objective of the experimental evaluation was to correlate the measured response time using transient radiation flux changes and power supply perturbation. The objective of the analytical model of the different sensor response was to predict response time and degradation mechanisms

  17. Effect of plagiochin E, an antifungal macrocyclic bis(bibenzyl), on cell wall chitin synthesis in Candida albicans

    Institute of Scientific and Technical Information of China (English)

    Xiu-zhen WU; Ai-xia CHENG; Ling-mei SUN; Hong-xiang LOU

    2008-01-01

    Aim: To investigate the effect of plagiochin E (PLE), an antifungal macrocyclic bis(bibenzyl) isolated from liverwort Marchantia polymorpha L, on cell wall chitin synthesis in Candida albicans. Methods: The effect of PLE on chitin synthesis in Candida albicans was investigated at the cellular and molecular lev-els. First, the ultrastructural changes were observed under transmission electron microscopy (TEM). Second, the effects of PLE on chitin synthetase (Chs) activi-ties in vitro were assayed using 6-O-dansyl-N-acetylglucosamine as a fluorescent substrate, and its effect on chitin synthesis in situ was assayed by spheroplast regeneration. Finally, real-time RT-PCR was performed to assay its effect on the expression of Chs genes (CHS). Results: Observation under TEM showed that the structure of the cell wall in Candida albicans was seriously damaged, which suggested that the antifungal activity of PLE was associated with its effect on the cell wail. Enzymatic assays and spheroplast regeneration showed that PLE inhibited chitin synthesis in vitro and in situ. The results of the PCR showed that PLE significantly downregulated the expression of CHS1, and upregulated the expression of CHS2 and CHS3. Because different Chs is regulated at different stages of transcription and post-translation, the downregulation of CHS1 would decrease the level of Chs 1 and inhibit its activity, and the inhibitory effects of PLE on Chs2 and Chs3 would be at the post-translational level or by the inhibi-tion on the enzyme-active center. Conclusion: These results indicate that the antifungal activity of PLE would be attributed to its inhibitory effect on cell wall chitin synthesis in Candida albicans.

  18. Graphene-Reinforced Aluminum Matrix Composites: A Review of Synthesis Methods and Properties

    Science.gov (United States)

    Chen, Fei; Gupta, Nikhil; Behera, Rakesh K.; Rohatgi, Pradeep K.

    2018-03-01

    Graphene-reinforced aluminum (Gr-Al) matrix nanocomposites (NCs) have attracted strong interest from both research and industry in high-performance weight-sensitive applications. Due to the vastly different bonding characteristics of the Al matrix (metallic) and graphene (in-plane covalent + inter-plane van der Waals), the graphene phase has a general tendency to agglomerate and phase separate in the metal matrix, which is detrimental for the mechanical and chemical properties of the composite. Thus, synthesis of Gr-Al NCs is extremely challenging. This review summarizes the different methods available to synthesize Gr-Al NCs and the resulting properties achieved in these NCs. Understanding the effect of processing parameters on the realized properties opens up the possibility of tailoring the synthesis methods to achieve the desired properties for a given application.

  19. Graphene-Reinforced Aluminum Matrix Composites: A Review of Synthesis Methods and Properties

    Science.gov (United States)

    Chen, Fei; Gupta, Nikhil; Behera, Rakesh K.; Rohatgi, Pradeep K.

    2018-06-01

    Graphene-reinforced aluminum (Gr-Al) matrix nanocomposites (NCs) have attracted strong interest from both research and industry in high-performance weight-sensitive applications. Due to the vastly different bonding characteristics of the Al matrix (metallic) and graphene (in-plane covalent + inter-plane van der Waals), the graphene phase has a general tendency to agglomerate and phase separate in the metal matrix, which is detrimental for the mechanical and chemical properties of the composite. Thus, synthesis of Gr-Al NCs is extremely challenging. This review summarizes the different methods available to synthesize Gr-Al NCs and the resulting properties achieved in these NCs. Understanding the effect of processing parameters on the realized properties opens up the possibility of tailoring the synthesis methods to achieve the desired properties for a given application.

  20. One-step route to a hybrid TiO2/TixW1−xN nanocomposite by in situ selective carbothermal nitridation

    Directory of Open Access Journals (Sweden)

    Zoë Schnepp, Martin J Hollamby, Masahiko Tanaka, Yoshitaka Matsushita, Yoshio Katsuya and Yoshio Sakka

    2012-01-01

    Full Text Available Metal oxide/nitride nanocomposites have many existing and potential applications, e.g. in energy conversion or ammonia synthesis. Here, a hybrid oxide/nitride nanocomposite (anatase/TixW1−xN was synthesized by an ammonia-free sol–gel route. Synchrotron x-ray diffraction, complemented with electron microscopy and thermogravimetric analysis, was used to study the structure, composition and mechanism of formation of the nanocomposite. The nanocomposite contained nanoparticles (<5 nm diameter of two highly intermixed phases. This was found to arise from controlled nucleation and growth of a single oxide intermediate from the gel precursor, followed by phase separation and in situ selective carbothermal nitridation. Depending on the preparation conditions, the composition varied from anatase/TixW1−xN at low W content to an isostructural mixture of Ti-rich and W-rich TixW1−xN at high W content. In situ selective carbothermal nitridation offers a facile route to the synthesis of nitride-oxide nanocomposites. This conceptually new approach is a significant advance from previous methods, which generally require ammonolysis of a pre-synthesized oxide.

  1. In Situ PDF Study of the Nucleation and Growth of Intermetallic PtPb Nanocrystals

    DEFF Research Database (Denmark)

    Saha, Dipankar; Bojesen, Espen D.; Mamakhel, Mohammad Aref Hasen

    2017-01-01

    The mechanism of Pt and PtPb nanocrystal formation under supercritical ethanol conditions has been investigated by means of in situ X-ray total scattering and pair distribution function (PDF) analysis. The metal complex structures of two different platinum precursor solutions, chloroplatinic acid...... supercritical ethanol process for obtaining phase-pure hexagonal PtPb nanocrystals. The study thus highlights the importance of in situ studies in revealing atomic-scale information about nucleation mechanisms, which can be used in design of specific synthesis pathways, and the new continuous-flow process...

  2. Optimal synthesis of a four-bar linkage by method of controlled deviation

    Directory of Open Access Journals (Sweden)

    Bulatović Radovan R.

    2004-01-01

    Full Text Available This paper considers optimal synthesis of a four-bar linkage by method of controlled deviations. The advantage of this approximate method is that it allows control of motion of the coupler in the four-bar linkage so that the path of the coupler is in the prescribed environment around the given path on the segment observed. The Hooke-Jeeves’s optimization algorithm has been used in the optimization process. Calculation expressions are not used as the method of direct searching, i.e. individual comparison of the calculated value of the objective function is made in each iteration and the moving is done in the direction of decreasing the value of the objective function. This algorithm does not depend on the initial selection of the projected variables. All this is illustrated on an example of synthesis of a four-bar linkage whose coupler point traces a straight line, i.e. passes through sixteen prescribed points lying on one straight line. .

  3. In Situ Hybridization of Pulp Fibers Using Mg-Al Layered Double Hydroxides

    Directory of Open Access Journals (Sweden)

    Carl-Erik Lange

    2015-04-01

    Full Text Available Inorganic Mg2+ and Al3+ containing layered double hydroxide (LDH particles were synthesised in situ from aqueous solution onto chemical pulp fibers of pine (Pinus sylvestris. High super saturated (hss solution with sodium carbonate produced LDH particles with an average diameter of 100–200 nm. Nano-size (70 nm LDH particles were found from fibers external surface and, to a lesser degree, from the S2 cell wall after synthesis via low super saturated (lss route. The synthesis via slow urea hydrolysis (Uhyd yielded micron and clay sized LDH (2–5 μm and enabled efficient fiber densification via mineralization of S2 fiber wall layer as indicated by TEM and compliance analysis. The Uhyd method decreased fiber compliance up to 50%. Reduction in the polymerisation degree of cellulose was observed with capillary viscometry. Thermogravimetric analysis showed that the hybridization with LDH reduced the exothermic heat, indicating, that this material can be incorporated in flame retardant applications. Fiber charge was assessed by Fibers 2015, 3 104 adsorption expermients with methylene blue (MB and metanil yellow (MY. Synthesis via lss route retained most of the fibres original charge and provided the highest capacity (10 μmol/g for anionic MY, indicating cationic character of hybrid fibers. Our results suggested that mineralized fibers can be potentially used in advanced applications such as biocomposites and adsorbent materials.

  4. In situ visualization of newly synthesized proteins in environmental microbes using amino acid tagging and click chemistry

    Science.gov (United States)

    Hatzenpichler, Roland; Scheller, Silvan; Tavormina, Patricia L; Babin, Brett M; Tirrell, David A; Orphan, Victoria J

    2014-01-01

    Here we describe the application of a new click chemistry method for fluorescent tracking of protein synthesis in individual microorganisms within environmental samples. This technique, termed bioorthogonal non-canonical amino acid tagging (BONCAT), is based on the in vivo incorporation of the non-canonical amino acid L-azidohomoalanine (AHA), a surrogate for l-methionine, followed by fluorescent labelling of AHA-containing cellular proteins by azide-alkyne click chemistry. BONCAT was evaluated with a range of phylogenetically and physiologically diverse archaeal and bacterial pure cultures and enrichments, and used to visualize translationally active cells within complex environmental samples including an oral biofilm, freshwater and anoxic sediment. We also developed combined assays that couple BONCAT with ribosomal RNA (rRNA)-targeted fluorescence in situ hybridization (FISH), enabling a direct link between taxonomic identity and translational activity. Using a methanotrophic enrichment culture incubated under different conditions, we demonstrate the potential of BONCAT-FISH to study microbial physiology in situ. A direct comparison of anabolic activity using BONCAT and stable isotope labelling by nano-scale secondary ion mass spectrometry (15NH3 assimilation) for individual cells within a sediment-sourced enrichment culture showed concordance between AHA-positive cells and 15N enrichment. BONCAT-FISH offers a fast, inexpensive and straightforward fluorescence microscopy method for studying the in situ activity of environmental microbes on a single-cell level. PMID:24571640

  5. Comprehensive validation scheme for in situ fiber optics dissolution method for pharmaceutical drug product testing.

    Science.gov (United States)

    Mirza, Tahseen; Liu, Qian Julie; Vivilecchia, Richard; Joshi, Yatindra

    2009-03-01

    There has been a growing interest during the past decade in the use of fiber optics dissolution testing. Use of this novel technology is mainly confined to research and development laboratories. It has not yet emerged as a tool for end product release testing despite its ability to generate in situ results and efficiency improvement. One potential reason may be the lack of clear validation guidelines that can be applied for the assessment of suitability of fiber optics. This article describes a comprehensive validation scheme and development of a reliable, robust, reproducible and cost-effective dissolution test using fiber optics technology. The test was successfully applied for characterizing the dissolution behavior of a 40-mg immediate-release tablet dosage form that is under development at Novartis Pharmaceuticals, East Hanover, New Jersey. The method was validated for the following parameters: linearity, precision, accuracy, specificity, and robustness. In particular, robustness was evaluated in terms of probe sampling depth and probe orientation. The in situ fiber optic method was found to be comparable to the existing manual sampling dissolution method. Finally, the fiber optic dissolution test was successfully performed by different operators on different days, to further enhance the validity of the method. The results demonstrate that the fiber optics technology can be successfully validated for end product dissolution/release testing. (c) 2008 Wiley-Liss, Inc. and the American Pharmacists Association

  6. A green and efficient method for the synthesis of homodimeric (β ...

    African Journals Online (AJOL)

    ... derivatives by intramolecular cyclization in various yields. Of particular interest is the use of the water as solvent of reaction and in absence of catalyst. Also these operating conditions protect the environment and economic points of view. Keywords: aqueous synthesis; bioactivity; dihydropyridine; dimedone; green method; ...

  7. Evaluation of biological activities of nanocrystalline zirconia synthesis via combustion method

    International Nuclear Information System (INIS)

    Thakare, V.G.; Omanwar, S.K.; Bhatkar, V.B.; Wadegaokar, P.A.

    2016-01-01

    The objective of the following study was synthesis of nanocrystalline zirconia by modified solution combustion synthesis method and evaluation of its structural and biological properties. The sample was characterized by powder X-ray diffraction (XRD), Field Emission Scanning Electron Microscopy (FESEM) and evaluated for cytotoxicity study using 3T3 mouse fibroblast cells, the antibacterial property are investigated by spread plate method against E. coli bacterial pathogen and studied for degradation using phosphate buffered saline (PBS) solution. The XRD pattern shows that the monoclinic phase of nanocrystalline zirconia was obtained. The FESEM images showed that the prepared sample consists of particles in the range of 45 nm and homogenous particle size distribution. The sample of zirconia has excellent tissue biocompatibility and does not show any toxicity towards normal 3T3 mouse fibroblast cells. It also inhibited the bacterial growth. The sample shows stability at physiological condition and does not show degradation. (author)

  8. In Situ Formation of Steroidal Supramolecular Gels Designed for Drug Release

    Directory of Open Access Journals (Sweden)

    Hana Bunzen

    2013-03-01

    Full Text Available In this work, a steroidal gelator containing an imine bond was synthesized, and its gelation behavior as well as a sensitivity of its gels towards acids was investigated. It was shown that the gels were acid-responsive, and that the gelator molecules could be prepared either by a conventional synthesis or directly in situ during the gel forming process. The gels prepared by both methods were studied and it was found that they had very similar macro- and microscopic properties. Furthermore, the possibility to use the gels as carriers for aromatic drugs such as 5-chloro-8-hydroxyquinoline, pyrazinecarboxamide, and antipyrine was investigated and the prepared two-component gels were studied with regard to their potential applications in drug delivery, particularly in a pH-controlled drug release.

  9. Full-scale demonstration of EBS construction technology I. Block, pellet and in-situ compaction method

    International Nuclear Information System (INIS)

    Toguri, Satohito; Asano, Hidekazu; Takao, Hajime; Matsuda, Takeshi; Amemiya, Kiyoshi

    2008-01-01

    (i) Bentonite Block: Applicability of manufacturing technology of buffer material was verified by manufacturing of full scale bentonite ring which consists of one-eight (1/8) dividing block (Outside Diameter (OD): 2.220 mm H: 300 mm). Density characteristic, dimension and scale effect, which were considered the tunnel environment under transportation, were evaluated. Vacuum suction technology was selected as handling technology for the ring. Hoisting characteristic of vacuum suction technology was presented through evaluation of the mechanical property of buffer material, the friction between blocks, etc. by using a full-scale bentonite ring (OD 2.200 mm, H 300 mm). And design of bentonite block and emplacement equipment were presented in consideration of manufacturability of the block, stability of handling and improvement of emplacement efficiency. (ii) Bentonite Pellet Filling: Basic characteristics such as water penetration, swelling and thermal conductivity of various kinds of bentonite pellet were collected by laboratory scale tests. Applicability of pellet filling technology was evaluated by horizontal filling test using a simulated full-scale drift tunnel (OD 2.200 mm, L 6 m) . Filling density, grain size distribution, etc. were also measured. (iii) In-Situ Compaction of Bentonite: Dynamic compaction method (heavy weight fall method) was selected as in-situ compaction technology. Compacting examination which used a full scale disposal pit (OD 2.360 mm) was carried out. Basic specification of compacting equipment and applicability of in-situ compaction technology were presented. Density, density distribution of buffer material and energy acted on the wall of the pit, were also measured. (author)

  10. Solution combustion synthesis of metal oxide nanomaterials for energy storage and conversion

    Science.gov (United States)

    Li, Fa-Tang; Ran, Jingrun; Jaroniec, Mietek; Qiao, Shi Zhang

    2015-10-01

    The design and synthesis of metal oxide nanomaterials is one of the key steps for achieving highly efficient energy conversion and storage on an industrial scale. Solution combustion synthesis (SCS) is a time- and energy-saving method as compared with other routes, especially for the preparation of complex oxides which can be easily adapted for scale-up applications. This review summarizes the synthesis of various metal oxide nanomaterials and their applications for energy conversion and storage, including lithium-ion batteries, supercapacitors, hydrogen and methane production, fuel cells and solar cells. In particular, some novel concepts such as reverse support combustion, self-combustion of ionic liquids, and creation of oxygen vacancies are presented. SCS has some unique advantages such as its capability for in situ doping of oxides and construction of heterojunctions. The well-developed porosity and large specific surface area caused by gas evolution during the combustion process endow the resulting materials with exceptional properties. The relationship between the structural properties of the metal oxides studied and their performance is discussed. Finally, the conclusions and perspectives are briefly presented.

  11. In Situ Formation of Carbon Nanomaterials on Bulk Metallic Materials

    Directory of Open Access Journals (Sweden)

    J. Y. Xu

    2014-01-01

    Full Text Available Carbon nanomaterials were synthesized in situ on bulk 316L stainless steel, pure cobalt, and pure nickel by hybrid surface mechanical attrition treatment (SMAT. The microstructures of the treated samples and the resulted carbon nanomaterials were investigated by SEM and TEM characterizations. Different substrates resulted in different morphologies of products. The diameter of carbon nanomaterials is related to the size of the nanograins on the surface layer of substrates. The possible growth mechanism was discussed. Effects of the main parameters of the synthesis, including the carbon source and gas reactant composition, hydrogen, and the reaction temperature, were studied. Using hybrid SMAT is proved to be an effective way to synthesize carbon nanomaterials in situ on surfaces of metallic materials.

  12. Application of tomographics methods for determination of rock failure in situ

    Directory of Open Access Journals (Sweden)

    Pandula Blažej

    1996-03-01

    Full Text Available Rock Failure determination closely connects with optimalization of rock disintegration as well excavation of underground openings. The aim of this optimalization is than to reach desired fragmentation during the blasting as well as choose the most suitable excavation technology. Study of rock failure can be very useful to reach this goal. In practice it can be done on the basis of personal technological experiences of blasting operator obtained in long term experiences in situ conditions. Because in many cases that experiences can not be utilised, it is necessary to learn against more precise rock failure evaluation. It can also down the costs of disintegration as well as excavation. The paper deals with results of common geophysical methods and methods of seismic tomography achieved at the hidden rock failure determination in the rock masses of the Ruzin dam during projecting the outlet equipment.

  13. Cross-Aldol Reaction of Activated Carbonyls with Nitrosocarbonyl Intermediates: Stereoselective Synthesis toward α-Hydroxy-β-amino Esters and Amides.

    Science.gov (United States)

    Mallik, Sumitava; Bhajammanavar, Vinod; Ramakrishna, Isai; Baidya, Mahiuddin

    2017-07-21

    A practical and flexible strategy toward α-hydroxy-β-amino esters and amides, which are important biological motifs, based on an organocatalytic cross-aldol reaction of in situ-generated nitrosocarbonyl intermediates followed by hydrogenation is presented. The protocol features operational simplicity, high yields, a wide substrate scope, and high regio- and diastereoselectivity profiles. The utility of this method was showcased through the synthesis of bestatin analogues and indole formation.

  14. Direct synthesis of L1 type Fe-Pt nanoparticles using microwave-polyol method

    International Nuclear Information System (INIS)

    Minami, Rumiko; Kitamoto, Yoshitaka; Chikata, Tsukasa; Kato, Shunsaku

    2005-01-01

    We report the synthesis of Fe-Pt nanoparticles with microwave irradiation during polyol-reduction reaction. Chemically ordered Fe-Pt nanoparticles with L1 structure are fabricated at 250 deg. C using a microwave-polyol method without any post-synthesis treatments. Moessbauer analyses reveal the nanoparticles have partially ordered L1 structure. The partially ordered Fe-Pt nanoparticles exhibit coercivity of 3.4 kOe, saturation magnetization of 49 emu/g, and anisotropy field of 83 kOe at room temperature

  15. Synthesis of micro- and nanodiamonds by the method of oxy- acetylene combustion flame

    International Nuclear Information System (INIS)

    Sabitov, S; Medyanova, B; Partizan, G; Koshanova, A; Mansurova, M; Lesbayev, B; Mansurov, B; Merkibayev, Ye

    2016-01-01

    This work presents the results of experiments on synthesis of micro- and nanodiamonds by the method of oxy-acetylene torch on the surface of pre-deposited copper thin films. The influence of the thickness of the buffer copper film and the concentration ratio of oxygen and acetylene on the structure formation of the deposited samples was investigated during performed experiments. Studies by Raman scattering and scanning electron microscopy showed that the synthesis of micro- and nano-diamonds occurs under certain experimental conditions. (paper)

  16. Scalable Analysis Methods and In Situ Infrastructure for Extreme Scale Knowledge Discovery

    Energy Technology Data Exchange (ETDEWEB)

    Duque, Earl P.N. [J.M. Smith International, LLC, Rutherford, NJ (United States). DBA Intelligent Light; Whitlock, Brad J. [J.M. Smith International, LLC, Rutherford, NJ (United States). DBA Intelligent Light

    2017-08-25

    High performance computers have for many years been on a trajectory that gives them extraordinary compute power with the addition of more and more compute cores. At the same time, other system parameters such as the amount of memory per core and bandwidth to storage have remained constant or have barely increased. This creates an imbalance in the computer, giving it the ability to compute a lot of data that it cannot reasonably save out due to time and storage constraints. While technologies have been invented to mitigate this problem (burst buffers, etc.), software has been adapting to employ in situ libraries which perform data analysis and visualization on simulation data while it is still resident in memory. This avoids the need to ever have to pay the costs of writing many terabytes of data files. Instead, in situ enables the creation of more concentrated data products such as statistics, plots, and data extracts, which are all far smaller than the full-sized volume data. With the increasing popularity of in situ, multiple in situ infrastructures have been created, each with its own mechanism for integrating with a simulation. To make it easier to instrument a simulation with multiple in situ infrastructures and include custom analysis algorithms, this project created the SENSEI framework.

  17. RNA detection in situ with FISH-STICs.

    Science.gov (United States)

    Sinnamon, John R; Czaplinski, Kevin

    2014-02-01

    The ability to detect RNA molecules in situ has long had important applications for molecular biological studies. Enzyme or dye-labeled antisense in vitro runoff transcripts and synthetic oligodeoxynucleotides (ODN) both have a proven track record of success, but each of these also has scientific and practical drawbacks and limitations to its use. We devised a means to use commercially synthesized oligonucleotides as RNA-FISH probes without further modification and show that such probes work well for detection of RNA in cultured cells. This approach can bind a high concentration of fluorescent ODN to a short stretch of an RNA using commercial DNA synthesis outlets available to any laboratory. We call this approach for creating in situ hybridization probes Fluorescence In Situ Hybridization with Sequential Tethered and Intertwined ODN Complexes (FISH-STICs). We demonstrate that one FISH-STIC probe can detect mRNA molecules in culture, and that probe detection can be improved by the addition of multiple probes that can be easily adapted for robust mRNA quantification. Using FISH-STICs, we demonstrate a nonoverlapping distribution for β-actin and γ-actin mRNA in cultured fibroblasts, and the detection of neuron-specific transcripts within cultured primary hippocampal neurons.

  18. Four Models of In Situ Simulation

    DEFF Research Database (Denmark)

    Musaeus, Peter; Krogh, Kristian; Paltved, Charlotte

    2014-01-01

    Introduction In situ simulation is characterized by being situated in the clinical environment as opposed to the simulation laboratory. But in situ simulation bears a family resemblance to other types of on the job training. We explore a typology of in situ simulation and suggest that there are f......Introduction In situ simulation is characterized by being situated in the clinical environment as opposed to the simulation laboratory. But in situ simulation bears a family resemblance to other types of on the job training. We explore a typology of in situ simulation and suggest...... that there are four fruitful approaches to in situ simulation: (1) In situ simulation informed by reported critical incidents and adverse events from emergency departments (ED) in which team training is about to be conducted to write scenarios. (2) In situ simulation through ethnographic studies at the ED. (3) Using...... the following processes: Transition processes, Action processes and Interpersonal processes. Design and purpose This abstract suggests four approaches to in situ simulation. A pilot study will evaluate the different approaches in two emergency departments in the Central Region of Denmark. Methods The typology...

  19. Synthesis of large CZTSe nanoparticles through a two-step hot-injection method

    DEFF Research Database (Denmark)

    Engberg, Sara Lena Josefin; Li, Zhenggang; Lek, Jun Yan

    2015-01-01

    Grain boundaries in Cu2ZnSn(SxSe1x)4 (CZTSSe) thin films act as a defect that reduces the mobility of the charges. Hence one way to improve the performance of these thin film solar cells is to increase the grain size in the films. Most of the synthesis methods published so far for CZTSSe colloidal...... molecules, solvents and precursors, and by controlling the initial monomer concentration. Additionally, we show how our new synthesis route can be utilized to achieve targeted ratios of CZTS and CZTSe nanoparticles to be used for mixed-phase CZTSSe thin films....

  20. In situ synthesis of molecularly imprinted nanoparticles in porous support membranes using high-viscosity polymerization solvents.

    Science.gov (United States)

    Renkecz, Tibor; László, Krisztina; Horváth, Viola

    2012-06-01

    There is a growing need in membrane separations for novel membrane materials providing selective retention. Molecularly imprinted polymers (MIPs) are promising candidates for membrane functionalization. In this work, a novel approach is described to prepare composite membrane adsorbers incorporating molecularly imprinted microparticles or nanoparticles into commercially available macroporous filtration membranes. The polymerization is carried out in highly viscous polymerization solvents, and the particles are formed in situ in the pores of the support membrane. MIP particle composite membranes selective for terbutylazine were prepared and characterized by scanning electron microscopy and N₂ porosimetry. By varying the polymerization solvent microparticles or nanoparticles with diameters ranging from several hundred nanometers to 1 µm could be embedded into the support. The permeability of the membranes was in the range of 1000 to 20,000 Lm⁻²  hr⁻¹  bar⁻¹. The imprinted composite membranes showed high MIP/NIP (nonimprinted polymer) selectivity for the template in organic media both in equilibrium-rebinding measurements and in filtration experiments. The solid phase extraction of a mixture of the template, its analogs, and a nonrelated compound demonstrated MIP/NIP selectivity and substance selectivity of the new molecularly imprinted membrane. The synthesis technique offers a potential for the cost-effective production of selective membrane adsorbers with high capacity and high throughput. Copyright © 2012 John Wiley & Sons, Ltd.

  1. Preparation of high temperature superconductor ceramics using cuban reactives. Optimization of the synthesis method

    International Nuclear Information System (INIS)

    Leyva Fabelo, A.; Cruz, C.; Aragon, B.; Suarez, J.C.; Mora, M.

    1991-01-01

    Results of the crystallographic characterization of a group of Cuban Products, which are evaluated to be employed in HTSC fabrication are presented in this paper. The first results on the synthesis of HTSC (RBa 2 Cu 3 0 7δ , R= Y, La, Nd) using Cuban reactives, are presented. The so called 'solid state reaction method of synthesis' was optimized, obtaining a critical temperature of more than 93 k

  2. In situ growth of capping-free magnetic iron oxide nanoparticles on liquid-phase exfoliated graphene

    NARCIS (Netherlands)

    Tsoufis, T.; Syrgiannis, Z.; Akhtar, N.; Prato, M.; Katsaros, F.; Sideratou, Z.; Kouloumpis, A.; Gournis, D.; Rudolf, P.

    2015-01-01

    We report a facile approach for the in situ synthesis of very small iron oxide nanoparticles on the surface of high-quality graphene sheets. Our synthetic strategy involved the direct, liquid-phase exfoliation of highly crystalline graphite (avoiding any oxidation treatment) and the subsequent

  3. The Synthesis of "N"-Benzyl-2-Azanorbornene via Aqueous Hetero Diels-Alder Reaction: An Undergraduate Project in Organic Synthesis and Structural Analysis

    Science.gov (United States)

    Sauvage, Xavier; Delaude, Lionel

    2008-01-01

    The synthesis of "N"-benzyl-2-azanorbornene via aqueous hetero Diels-Alder reaction of cyclopentadiene and benzyliminium chloride formed in situ from benzylamine hydrochloride and formaldehyde is described. Characterization of the product was achieved by IR and NMR spectroscopies. The spectral data acquired are thoroughly discussed. Numerous…

  4. Enzyme Engineering for In Situ Immobilization.

    Science.gov (United States)

    Rehm, Fabian B H; Chen, Shuxiong; Rehm, Bernd H A

    2016-10-14

    Enzymes are used as biocatalysts in a vast range of industrial applications. Immobilization of enzymes to solid supports or their self-assembly into insoluble particles enhances their applicability by strongly improving properties such as stability in changing environments, re-usability and applicability in continuous biocatalytic processes. The possibility of co-immobilizing various functionally related enzymes involved in multistep synthesis, conversion or degradation reactions enables the design of multifunctional biocatalyst with enhanced performance compared to their soluble counterparts. This review provides a brief overview of up-to-date in vitro immobilization strategies while focusing on recent advances in enzyme engineering towards in situ self-assembly into insoluble particles. In situ self-assembly approaches include the bioengineering of bacteria to abundantly form enzymatically active inclusion bodies such as enzyme inclusions or enzyme-coated polyhydroxyalkanoate granules. These one-step production strategies for immobilized enzymes avoid prefabrication of the carrier as well as chemical cross-linking or attachment to a support material while the controlled oriented display strongly enhances the fraction of accessible catalytic sites and hence functional enzymes.

  5. Statistical Optimization of Synthesis of Manganese Carbonates Nanoparticles by Precipitation Methods

    International Nuclear Information System (INIS)

    Javidan, A.; Rahimi-Nasrabadi, M.; Davoudi, A.A.

    2011-01-01

    In this study, an orthogonal array design (OAD), OA9, was employed as a statistical experimental method for the controllable, simple and fast synthesis of manganese carbonate nanoparticle. Ultrafine manganese carbonate nanoparticles were synthesized by a precipitation method involving the addition of manganese ion solution to the carbonate reagent. The effects of reaction conditions, for example, manganese and carbonate concentrations, flow rate of reagent addition and temperature, on the diameter of the synthesized manganese carbonate nanoparticle were investigated. The effects of these factors on the width of the manganese carbonate nanoparticle were quantitatively evaluated by the analysis of variance (ANOVA). The results showed that manganese carbonate nanoparticle can be synthesized by controlling the manganese concentration, flow rate and temperature. Finally, the optimum conditions for the synthesis of manganese carbonate nanoparticle by this simple and fast method were proposed. The results of ANOVA showed that 0.001 mol/ L manganese ion and carbonate reagents concentrations, 2.5 mL/ min flow rate for the addition of the manganese reagent to the carbonate solution and 0 degree Celsius temperature are the optimum conditions for producing manganese carbonate nanoparticle with 75 ± 25 nm width. (author)

  6. In-Situ Simulation

    DEFF Research Database (Denmark)

    Bjerregaard, Anders Thais; Slot, Susanne; Paltved, Charlotte

    2015-01-01

    , and organisational characteristic. Therefore, it might fail to fully mimic real clinical team processes. Though research on in situ simulation in healthcare is in its infancy, literature is abundant on patient safety and team training1. Patient safety reporting systems that identify risks to patients can improve......Introduction: In situ simulation offers on-site training to healthcare professionals. It refers to a training strategy where simulation technology is integrated into the clinical encounter. Training in the simulation laboratory does not easily tap into situational resources, e.g. individual, team...... patient safety if coupled with training and organisational support. This study explored the use of critical incidents and adverse events reports for in situ simulation and short-term observations were used to create learning objectives and training scenarios. Method: This study used an interventional case...

  7. In situ measurement of the mass concentration of flame-synthesized nanoparticles using quartz-crystal microbalance

    International Nuclear Information System (INIS)

    Hevroni, A; Golan, H; Fialkov, A; Tsionsky, V; Markovich, G; Cheskis, S; Rahinov, I

    2011-01-01

    A novel in situ method for measurement of mass concentration of nanoparticles (NPs) formed in flames is proposed. In this method, the deposition rate of NPs collected by a molecular beam sampling system is measured by quartz-crystal microbalance (QCM). It is the only existing method which allows direct measurement of NP mass concentration profiles in flames. The feasibility of the method was demonstrated by studying iron oxide NP formation in low-pressure methane/oxygen/nitrogen flames doped with iron pentacarbonyl. The system was tested under fuel-lean and fuel-rich flame conditions. Good agreement between measured QCM deposition rates and their estimations obtained by the transmission electron microscopy analysis of samples collected from the molecular beam has been demonstrated. The sensitivity of the method is comparable to that of particle mass spectrometry (PMS). Combination of the QCM technique with PMS and/or optical measurements can provide new qualitative information which is important for elucidation of the mechanisms governing the NP flame synthesis

  8. REGULAR METHOD FOR SYNTHESIS OF BASIC BENT-SQUARES OF RANDOM ORDER

    Directory of Open Access Journals (Sweden)

    A. V. Sokolov

    2016-01-01

    Full Text Available The paper is devoted to the class construction of the most non-linear Boolean bent-functions of any length N = 2k (k = 2, 4, 6…, on the basis of their spectral representation – Agievich bent squares. These perfect algebraic constructions are used as a basis to build many new cryptographic primitives, such as generators of pseudo-random key sequences, crypto graphic S-boxes, etc. Bent-functions also find their application in the construction of C-codes in the systems with code division multiple access (CDMA to provide the lowest possible value of Peak-to-Average Power Ratio (PAPR k = 1, as well as for the construction of error-correcting codes and systems of orthogonal biphasic signals. All the numerous applications of bent-functions relate to the theory of their synthesis. However, regular methods for complete class synthesis of bent-functions of any length N = 2k are currently unknown. The paper proposes a regular synthesis method for the basic Agievich bent squares of any order n, based on a regular operator of dyadic shift. Classification for a complete set of spectral vectors of lengths (l = 8, 16, … based on a criterion of the maximum absolute value and set of absolute values of spectral components has been carried out in the paper. It has been shown that any spectral vector can be a basis for building bent squares. Results of the synthesis for the Agievich bent squares of order n = 8 have been generalized and it has been revealed that there are only 3 basic bent squares for this order, while the other 5 can be obtained with help the operation of step-cyclic shift. All the basic bent squares of order n = 16 have been synthesized that allows to construct the bent-functions of length N = 256. The obtained basic bent squares can be used either for direct synthesis of bent-functions and their practical application or for further research in order to synthesize new structures of bent squares of orders n = 16, 32, 64, …

  9. Dynamic analysis of large structures with uncertain parameters based on coupling component mode synthesis and perturbation method

    Directory of Open Access Journals (Sweden)

    D. Sarsri

    2016-03-01

    Full Text Available This paper presents a methodological approach to compute the stochastic eigenmodes of large FE models with parameter uncertainties based on coupling of second order perturbation method and component mode synthesis methods. Various component mode synthesis methods are used to optimally reduce the size of the model. The statistical first two moments of dynamic response of the reduced system are obtained by the second order perturbation method. Numerical results illustrating the accuracy and efficiency of the proposed coupled methodological procedures for large FE models with uncertain parameters are presented.

  10. An exploratory study on the driving method of speech synthesis based on the human eye reading imaging data

    Science.gov (United States)

    Gao, Pei-pei; Liu, Feng

    2016-10-01

    With the development of information technology and artificial intelligence, speech synthesis plays a significant role in the fields of Human-Computer Interaction Techniques. However, the main problem of current speech synthesis techniques is lacking of naturalness and expressiveness so that it is not yet close to the standard of natural language. Another problem is that the human-computer interaction based on the speech synthesis is too monotonous to realize mechanism of user subjective drive. This thesis introduces the historical development of speech synthesis and summarizes the general process of this technique. It is pointed out that prosody generation module is an important part in the process of speech synthesis. On the basis of further research, using eye activity rules when reading to control and drive prosody generation was introduced as a new human-computer interaction method to enrich the synthetic form. In this article, the present situation of speech synthesis technology is reviewed in detail. Based on the premise of eye gaze data extraction, using eye movement signal in real-time driving, a speech synthesis method which can express the real speech rhythm of the speaker is proposed. That is, when reader is watching corpora with its eyes in silent reading, capture the reading information such as the eye gaze duration per prosodic unit, and establish a hierarchical prosodic pattern of duration model to determine the duration parameters of synthesized speech. At last, after the analysis, the feasibility of the above method is verified.

  11. HER2 testing in the UK: recommendations for breast and gastric in-situ hybridisation methods

    LENUS (Irish Health Repository)

    Bartlett, J. M. S.

    2011-01-01

    These guidelines supplement existing guidelines on HER2 testing by immunohistochemistry and in-situ hybridisation(ISH) methods in the UK. They provide a specific focus on aspects of guidance relevant to HER2 ISH testing methods, both fluorescent and chromogenic. They are formulated to give advice on methodology, interpretation and quality control for ISH-based testing of HER2 status in common tumour types, including both breast and gastric tumours. The aim is to ensure that all ISH-based testing is accurate, reliable and timely.

  12. New method of synthesis and in vitro studies of a porous biomaterial

    International Nuclear Information System (INIS)

    Wers, E.; Lefeuvre, B.; Pellen-Mussi, P.; Novella, A.; Oudadesse, H.

    2016-01-01

    Biomaterials for bone reconstruction represent a widely studied area. In this paper, a new method of synthesis of a porous glass–ceramic obtained by thermal treatment is presented. The prepared biomaterial was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and induced couple plasma-optical emission spectroscopy (ICP-OES), mercury porosimetry and by the Archimedes method. In vitro evaluations in a simulated body fluid (SBF) and in contact with SaOS_2 human osteoblasts were also carried out. The porous glass–ceramic is composed of a total porous network of 60% suitable for body fluid and cell infiltration, with pore sizes varying from 60 nm to 143 μm. The presence of two crystalline phases decreases the kinetic of bioactivity compared to an amorphous biomaterial (bioactive glass). A hydroxyapatite layer appears from 15 days of immersion on the surface and inside the pores, showing a biodegradation and a bioactivity in four steps. Cytotoxicity assessments present an increase of the cellular viability after 72 h proving the non-cytotoxic effect of the glass–ceramic. Thus, the results of these different studies indicate that the porous biomaterial may have a potential application for the bone regeneration. This paper also presents the novelty of this method. It is a rapid synthesis which combines simplicity and low cost. This represents an advantage for an eventual industrialization. - Highlights: • The new method of synthesis of a porous glass–ceramic is reproducible. • The porous glass–ceramic possesses a total porosity of 60%. • The biomaterial shows a bioactivity in four steps with hydroxyapatite formation. • 82% of cellular viability is observed on the surface of the biomaterial.

  13. New method of synthesis and in vitro studies of a porous biomaterial

    Energy Technology Data Exchange (ETDEWEB)

    Wers, E., E-mail: wers.eric@hotmail.com [Equipe Chimie du Solide et Matériaux, UMR CNRS 6226, Sciences Chimiques de Rennes, Université de Rennes 1, Université Européenne de Bretagne, 263 avenue du Général Leclerc, 35042 Rennes Cedex (France); Lefeuvre, B. [Equipe Chimie du Solide et Matériaux, UMR CNRS 6226, Sciences Chimiques de Rennes, Université de Rennes 1, Université Européenne de Bretagne, 263 avenue du Général Leclerc, 35042 Rennes Cedex (France); Pellen-Mussi, P.; Novella, A. [Equipe Chimie du Solide et Matériaux, UMR CNRS 6226, Sciences Chimiques de Rennes, Université de Rennes 1, Université Européenne de Bretagne, 2 avenue du Professeur Léon Bernard, 35042 Rennes Cedex (France); Oudadesse, H. [Equipe Chimie du Solide et Matériaux, UMR CNRS 6226, Sciences Chimiques de Rennes, Université de Rennes 1, Université Européenne de Bretagne, 263 avenue du Général Leclerc, 35042 Rennes Cedex (France)

    2016-04-01

    Biomaterials for bone reconstruction represent a widely studied area. In this paper, a new method of synthesis of a porous glass–ceramic obtained by thermal treatment is presented. The prepared biomaterial was characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and induced couple plasma-optical emission spectroscopy (ICP-OES), mercury porosimetry and by the Archimedes method. In vitro evaluations in a simulated body fluid (SBF) and in contact with SaOS{sub 2} human osteoblasts were also carried out. The porous glass–ceramic is composed of a total porous network of 60% suitable for body fluid and cell infiltration, with pore sizes varying from 60 nm to 143 μm. The presence of two crystalline phases decreases the kinetic of bioactivity compared to an amorphous biomaterial (bioactive glass). A hydroxyapatite layer appears from 15 days of immersion on the surface and inside the pores, showing a biodegradation and a bioactivity in four steps. Cytotoxicity assessments present an increase of the cellular viability after 72 h proving the non-cytotoxic effect of the glass–ceramic. Thus, the results of these different studies indicate that the porous biomaterial may have a potential application for the bone regeneration. This paper also presents the novelty of this method. It is a rapid synthesis which combines simplicity and low cost. This represents an advantage for an eventual industrialization. - Highlights: • The new method of synthesis of a porous glass–ceramic is reproducible. • The porous glass–ceramic possesses a total porosity of 60%. • The biomaterial shows a bioactivity in four steps with hydroxyapatite formation. • 82% of cellular viability is observed on the surface of the biomaterial.

  14. Effect of synthesis method on the preparation of lanthanum chromite for using as ceramic pigment

    International Nuclear Information System (INIS)

    Dantas, G.C.B.; Ferreira, K.M.B.; Pimentel, P.M.; Melo, D.M.A.; Gomes, D.K.S.; Costa, A.F.

    2016-01-01

    In this paper, LaCrO3 perovskites were synthesized by two synthesis methods, in order to compare these methods in function of microstructure and optical properties. The synthesis routes employed were a method that use gelatin as organic precursor and microwave assisted auto-combustion. The resulting powders were calcined at 800 ° C and 1000 ° C for obtaining the perovskite phase. Then, they were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM); UV-Visible spectroscopy and colorimetric analysis for color identification. No significant changes were observed in the powders synthesized by two routes. The oxides presented orthorhombic perovskite structure. The powders synthesized by the gelatin method were single phase. Chromite lanthanide presented grayish hue being darker in perovskites calcined at higher temperatures. (author)

  15. ''In situ'' electronic testing method of a neutron detector performance

    International Nuclear Information System (INIS)

    Gonzalez, J.M.; Levai, F.

    1987-01-01

    The method allows detection of any important change in the electrical characteristics of a neutron sensor channel. It checks the response signal produced by an electronic detector circuit when a pulse generator is connected as input signal in the high voltage supply. The electronic circuit compares the detector capacitance value, previously measured, against a reference value, which is adjusted in a window type comparator electronic circuit to detect any important degrading condition of the capacitance value in a detector-cable system. The ''in-situ'' electronic testing method of neutron detector performance has been verified in a laboratory atmosphere to be a potential method to detect any significant change in the capacitance value of a nuclear sensor and its connecting cable, also checking: detector disconnections, cable disconnections, length changes of the connecting cable, electric short-opened circuits in the sensor channel, and any electrical trouble in the detector-connector-cable system. The experimental practices were carried out by simulation of several electric changes in a nuclear sensor-cable system from a linear D.C. channel which measures reactor power during nuclear reactor operation. It was made at the Training Reactor Electronic Laboratory. The results and conclusions obtained at the Laboratory were proved, satisfactorily, in the Electronic Instrumentation of Budapest Technical University Training Reactor, Hungary

  16. Voltammetric, in-situ spectroelectrochemical and in-situ electrocolorimetric characterization of phthalocyanines

    Energy Technology Data Exchange (ETDEWEB)

    Koca, Atif [Department of Chemical Engineering, Faculty of Engineering, Marmara University, Goeztepe, 34722 Istanbul (Turkey)], E-mail: akoca@eng.marmara.edu.tr; Bayar, Serife; Dincer, Hatice A. [Department of Chemistry, Technical University of Istanbul, Maslak, 34469 Istanbul (Turkey); Gonca, Erguen [Department of Chemistry, Fatih University, TR34500 B.Cekmece, Istanbul (Turkey)

    2009-04-01

    In this work, electrochemical, and in-situ spectroelectrochemical characterization of the metallophthalocyanines bearing tetra-(1,1-(dicarbethoxy)-2-(2-methylbenzyl))-ethyl 3,10,17,24-tetra chloro groups were performed. Voltammetric and in-situ spectroelectrochemical measurements show that while cobalt phthalocyanine complex gives both metal-based and ring-based redox processes, zinc and copper phthalocyanines show only ring-based reduction and oxidation processes. The redox processes are generally diffusion-controlled, reversible and one-electron transfer processes. Differently lead phthalocyanine demetallized during second oxidation reaction while it was stable during reduction processes. An in-situ electrocolorimetric method, based on the 1931 CIE (Commission Internationale de l'Eclairage) system of colorimetry, has been applied to investigate the color of the electro-generated anionic and cationic forms of the complexes for the first time in this study.

  17. Evaluation of magnetic properties of NI-ZN ferrites obtained by different synthesis methods

    International Nuclear Information System (INIS)

    Simoes, A.N.; Neiva, L.S.; Simoes, V.N.; Gama, L.; Gomes Filho, A.C.; Oliveira, J.B.L.

    2012-01-01

    Ceramic oxides that exhibit ferromagnetic behavior represent important commercial products for the electronics industry and are commonly known as ferrites. The Ni-Zn ferrites are considered to be one of the most versatile and soft due to its high electrical resistivity and low eddy current losses. Thus, this study aims to evaluate the magnetic properties of Ni-Zn ferrite obtained by the Pechini and combustion reaction. After synthesis the powders were characterized by XRD, SEM, BET and magnetic measurements. The results showed that for both methods of synthesis used was the formation of the spinel phase of Ni-Zn ferrite. The micrographs show that the powders obtained by both methods have regular shapes and spherical. Were determined by BET surface area is 26 m 2 /g by the Pechini and 13 m 2 /g by combustion. And the samples synthesized by Pechini method obtained the best magnetic characteristics (author)

  18. Synthesis of Acridine-based DNA Bis-intercalating Agents

    Directory of Open Access Journals (Sweden)

    P. Mack

    2001-02-01

    Full Text Available Methods for the synthesis of N1, N8-bis(9-acridinyl-N4-(4-hydroxybenzyl-spermidine and N1, N7-(hydroxybenzyl-bis-(3-aminopropylamine were investigated. Thus monocyanoethylation of 4-methoxybenzylamine followed by treatment with 4-chlorobutyronitrile gave the dinitrile N-(2-cyanoethyl-N-(3-cyanopropyl-4-methoxybenzylamine. Subsequent in situ reduction with lithium aluminium hydride gave the corresponding diamine. Biscyanoethylation of 4-methoxybenzylamine with 2 mole of acrylonitrile followed by reduction yielded the diamine N, N-bis-(3-aminopropyl-4-methoxybenzylamine. Both diamines reacted smoothly with 9-methoxyacridine to give the bis-(9-acridinyl compounds 11 and 15 but with 4,5-dimethyl-9-methoxyacridine, the bis compound 16 was produced in only low yields. Demethylation of the dinitriles by a variety of approaches all failed to give the corresponding hydroxybenzyl derivatives. These studies yielded useful methylated tyrosine derivatives which could also be iodinated. This study has been useful for elucidating chemical methods needed for the synthesis of the desired tyrosine-based bis acridine compound and for alerting us to the need to synthesise a more labile protected tyrosine intermediate which will be easily deprotected to afford the desired tyrosine-based bis acridine compound.

  19. Morphology Changes of Co Catalyst Nanoparticles at the Onset of Fischer-Tropsch Synthesis

    DEFF Research Database (Denmark)

    Høydalsvik, Kristin; Fløystad, Jostein B.; Voronov, Alexey

    2014-01-01

    Cobalt nanoparticles play an important role as catalysts for the Fischer-Tropsch synthesis, which is an attractive route for production of synthetic fuels. It is of particular interest to understand the varying conversion rate during the first hours after introducing synthesis gas (H-2 and CO......) to the system. To this end, several in situ characterization studies have previously been done on both idealized model systems and commercially relevant catalyst nanoparticles, using bulk techniques, such as X-ray powder diffraction and X-ray absorption spectroscopy. Since catalysis takes place at the surface...... of the cobalt particles, it is important to develop methods to gain surface-specific structural information under realistic processing conditions. We addressed this challenge using small-angle X-ray scattering (SAXS), a technique exploiting the penetrating nature of X-rays to provide information about particle...

  20. A general strategy toward the rational synthesis of metal tungstate nanostructures using plasma electrolytic oxidation method

    Energy Technology Data Exchange (ETDEWEB)

    Jiang, Yanan; Liu, Baodan, E-mail: baodanliu@imr.ac.cn; Zhai, Zhaofeng; Liu, Xiaoyuan; Yang, Bing; Liu, Lusheng; Jiang, Xin, E-mail: xjiang@imr.ac.cn

    2015-11-30

    Graphical abstract: A general strategy for the rational synthesis of tungstate nanostructure has been developed based on plasma electrolytic oxidation (PEO) technology (up). Using this method, ZnWO{sub 4} and NiWO{sub 4} nanostructures with controllable morphologies and superior crystallinity can be easily obtained (down), showing obvious advantage in comparison with conventional hydrothermal and sol–gel methods. - Highlights: • Plasma electrolyte oxidation (PEO) method has been used for the rational synthesis of tungstate nanostructures. • ZnWO{sub 4} nanoplates have strong mechanical adhesion with porous TiO{sub 2} film substrate. • The morphology and dimensional size of ZnWO{sub 4} nanostructures can be selectively tailored by controlling the annealing temperature and growth time. • The PEO method can be widely applied to the growth of various metal oxides. - Abstract: A new method based on conventional plasma electrolytic oxidation (PEO) technology has been developed for the rational synthesis of metal tungstate nanostructures. Using this method, ZnWO{sub 4} and NiWO{sub 4} nanostructures with controllable morphologies (nanorods, nanosheets and microsheets) and superior crystallinity have been synthesized. It has been found that the morphology diversity of ZnWO{sub 4} nanostructures can be selectively tailored through tuning the electrolyte concentration and annealing temperatures, showing obvious advantages in comparison to traditional hydrothermal and sol–gel methods. Precise microscopy analyses on the cross section of the PEO coating and ZnWO{sub 4} nanostructures confirmed that the precursors initially precipitated in the PEO coating and its surface during plasma discharge process are responsible for the nucleation and subsequent growth of metal tungstate nanostructures by thermal annealing. The method developed in this work represents a general strategy toward the rational synthesis of metal oxide nanostructures and the formation mechanism of

  1. A general strategy toward the rational synthesis of metal tungstate nanostructures using plasma electrolytic oxidation method

    International Nuclear Information System (INIS)

    Jiang, Yanan; Liu, Baodan; Zhai, Zhaofeng; Liu, Xiaoyuan; Yang, Bing; Liu, Lusheng; Jiang, Xin

    2015-01-01

    Graphical abstract: A general strategy for the rational synthesis of tungstate nanostructure has been developed based on plasma electrolytic oxidation (PEO) technology (up). Using this method, ZnWO 4 and NiWO 4 nanostructures with controllable morphologies and superior crystallinity can be easily obtained (down), showing obvious advantage in comparison with conventional hydrothermal and sol–gel methods. - Highlights: • Plasma electrolyte oxidation (PEO) method has been used for the rational synthesis of tungstate nanostructures. • ZnWO 4 nanoplates have strong mechanical adhesion with porous TiO 2 film substrate. • The morphology and dimensional size of ZnWO 4 nanostructures can be selectively tailored by controlling the annealing temperature and growth time. • The PEO method can be widely applied to the growth of various metal oxides. - Abstract: A new method based on conventional plasma electrolytic oxidation (PEO) technology has been developed for the rational synthesis of metal tungstate nanostructures. Using this method, ZnWO 4 and NiWO 4 nanostructures with controllable morphologies (nanorods, nanosheets and microsheets) and superior crystallinity have been synthesized. It has been found that the morphology diversity of ZnWO 4 nanostructures can be selectively tailored through tuning the electrolyte concentration and annealing temperatures, showing obvious advantages in comparison to traditional hydrothermal and sol–gel methods. Precise microscopy analyses on the cross section of the PEO coating and ZnWO 4 nanostructures confirmed that the precursors initially precipitated in the PEO coating and its surface during plasma discharge process are responsible for the nucleation and subsequent growth of metal tungstate nanostructures by thermal annealing. The method developed in this work represents a general strategy toward the rational synthesis of metal oxide nanostructures and the formation mechanism of metal tungstate nanostructures fabricated by

  2. In Situ One-Step Synthesis of Hierarchical Nitrogen-Doped Porous Carbon for High Performance Supercapacitors

    Energy Technology Data Exchange (ETDEWEB)

    Jeon, Ju Won [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Texas A & M Univ., College Station, TX (United States); Sharma, Ronish [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Meduri, Praveen [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Arey, Bruce W. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Schaef, Herbert T. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Lutkenhaus, Jodie [Texas A & M Univ., College Station, TX (United States); Lemmon, John P. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Thallapally, Praveen K. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Nandasiri, Manjula I. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); McGrail, B. Peter [Pacific Northwest National Lab. (PNNL), Richland, WA (United States); Nune, Satish K. [Pacific Northwest National Lab. (PNNL), Richland, WA (United States)

    2014-04-30

    Electrochemical performance of the existing state-of-the art capacitors is not very high, key scientific barrier is that its charge storage mechanism wholly depends on adsorption of electrolyte on electrode. We present a novel method for the synthesis of nitrogen -doped porous carbons and address the drawback by precisely controlling composition and surface area. Nitrogen-doped porous carbon was synthesized using a self-sacrificial template technique without any additional nitrogen and carbon sources. They exhibited exceptionally high capacitance (239 Fg-1) due to additional pseudocapacitance originating from doped nitrogen. Cycling tests showed no obvious capacitance decay even after 10,000 cycles, which meets the requirement of commercial supercapacitors. Our method is simple and highly efficient for the production of large quantities of nitrogen-doped porous carbons.

  3. In situ measurement of the efficiency of filtration installations in the nuclear industry by the soda-fluorescein (uranin) aerosol method: AFNOR standard NFX 44.011

    International Nuclear Information System (INIS)

    Dupoux, J.

    1981-01-01

    The in situ measurement of the efficiency of filtering installations in the French nuclear industry using the soda-fluorescein (uraniun) aerosol method is presented. A brief description and the interest of the method are discussed. Its use for the location of defects in filter elements and for in situ control of casing with tandem HEPA filter stages is described

  4. A comparison of different methods for in-situ determination of heat losses form district heating pipes

    Energy Technology Data Exchange (ETDEWEB)

    Boehm, Benny [Technical Univ. of Denmark, Dept. of Energy Engineering (Denmark)

    1996-11-01

    A comparison of different methods for in-situ determination of heat losses has been carried out on a 273 mm transmission line in Copenhagen. Instrumentation includes temperature sensors, heat flux meters and an infrared camera. The methods differ with regard to time consumption and costs of applying the specific method, demand on accuracy of temperature measurements, sensitivity to computational parameters, e.g. the thermal conductivity of the soil, response to transients in water temperature and the ground, and steady state assumptions in the model used in the interpretation of the measurements. Several of the applied methods work well. (au)

  5. Pattern classification by memristive crossbar circuits using ex situ and in situ training

    Science.gov (United States)

    Alibart, Fabien; Zamanidoost, Elham; Strukov, Dmitri B.

    2013-06-01

    Memristors are memory resistors that promise the efficient implementation of synaptic weights in artificial neural networks. Whereas demonstrations of the synaptic operation of memristors already exist, the implementation of even simple networks is more challenging and has yet to be reported. Here we demonstrate pattern classification using a single-layer perceptron network implemented with a memrisitive crossbar circuit and trained using the perceptron learning rule by ex situ and in situ methods. In the first case, synaptic weights, which are realized as conductances of titanium dioxide memristors, are calculated on a precursor software-based network and then imported sequentially into the crossbar circuit. In the second case, training is implemented in situ, so the weights are adjusted in parallel. Both methods work satisfactorily despite significant variations in the switching behaviour of the memristors. These results give hope for the anticipated efficient implementation of artificial neuromorphic networks and pave the way for dense, high-performance information processing systems.

  6. Optimization of an auto-thermal ammonia synthesis reactor using cyclic coordinate method

    Science.gov (United States)

    A-N Nguyen, T.; Nguyen, T.-A.; Vu, T.-D.; Nguyen, K.-T.; K-T Dao, T.; P-H Huynh, K.

    2017-06-01

    The ammonia synthesis system is an important chemical process used in the manufacture of fertilizers, chemicals, explosives, fibers, plastics, refrigeration. In the literature, many works approaching the modeling, simulation and optimization of an auto-thermal ammonia synthesis reactor can be found. However, they just focus on the optimization of the reactor length while keeping the others parameters constant. In this study, the other parameters are also considered in the optimization problem such as the temperature of feed gas enters the catalyst zone, the initial nitrogen proportion. The optimal problem requires the maximization of an objective function which is multivariable function and subject to a number of equality constraints involving the solution of coupled differential equations and also inequality constraint. The cyclic coordinate search was applied to solve the multivariable-optimization problem. In each coordinate, the golden section method was applied to find the maximum value. The inequality constraints were treated using penalty method. The coupled differential equations system was solved using Runge-Kutta 4th order method. The results obtained from this study are also compared to the results from the literature.

  7. Nanocrystalline functional materials and nanocomposites synthesis through aerosol routes

    Directory of Open Access Journals (Sweden)

    Milošević Olivera B.

    2003-01-01

    Full Text Available This paper represents the results of the design of functional nanocrystalline powders and nanocomposites using chemical reactions in aerosols. The process involves ultrasonic aerosol formation (mist generators with the resonant frequencies of 800 kHz, 1.7 and 2.5 MHz from precursor salt solutions and control over the aerosol decomposition in a high-temperature tubular flow reactor. During decomposition, the aerosol droplets undergo evaporation/drying, precipitation and thermolysis in a single-step process. Consequently, spherical, solid, agglomerate-free submicronic particles are obtained. The particle morphology, revealed as a composite structure consisting of primary crystallites smaller than 20 nm was analysed by several methods (XRD, DSC/DTA, SEM, TEM and discussed in terms of precursor chemistry and process parameters. Following the initial attempts, a more detailed aspect of nanocrystalline particle synthesis was demonstrated for the case of nanocomposites based on ZnO-MeO (MeO=Bi Cr+, suitable for electronic applications, as well as an yttrium-aluminum base complex system, suitable for phosphorus applications. The results imply that parts of the material structure responsible for different functional behaviour appear through in situ aerosol synthesis by processes of intraparticle agglomeration, reaction and sintering in the last synthesis stage.

  8. Design and Synthesis of novel CuxGeOy/Cu/C nanowires by in situ chemical reduction process with highly reversible capacity for Lithium Batteries

    International Nuclear Information System (INIS)

    Wang, Linlin; Zhang, Xiaozhu; Peng, Xia; Tang, Kaibin

    2015-01-01

    The synthesis and use of ternary metal oxides/metal particles/carbon hybrids, especially 1D naowires composed of MGeO 3 /M/C hybrids for energy storage, remains very few reports. In this work, 1D Cu x GeO y /Cu/C NWs (x < 1, y < 3) were successfully prepared by a simple method involving chemical reduction process and simultaneous carbon coating. It was found that through the polydopamine(PDA)-assisted chemical reduction process performed on the CuGeO 3 NWs, the phase partially transformed to a mixture of crystalline Cu (∼70 nm) and amorphous Cu x GeO y NWs with carbon coating, but the nanowire-shaped morphology was maintained. Electrochemical measurements showed that the Cu x GeO y /Cu/C NWs exhibited a stable reversible capacity of ∼900 mA h g −1 after 100 cycles. Even at 800 mA g −1 , it also exhibited excellent high rate capacity of 350 mA h g −1 . The newly generated Cu x GeO y @Cu@CNWs exhibit enhanced cycle stability with high lithium-storage capability compared to that of the as-preparedCuGeO 3 NWs. (*) The in situ-synthesized Cu nanoparticles, amorphous state and carbon coating might play an important role in activating and enhancing the reversibility of the conversion reaction of Cu x GeO y . In addition, this effective synthetic method might provide the methodology for the development of other ternary metal oxides/metal particles/carbon hybrids materials for energy storage.

  9. A Review of Carbon Nanomaterials’ Synthesis via the Chemical Vapor Deposition (CVD) Method

    Science.gov (United States)

    Manawi, Yehia M.; Samara, Ayman; Al-Ansari, Tareq; Atieh, Muataz A.

    2018-01-01

    Carbon nanomaterials have been extensively used in many applications owing to their unique thermal, electrical and mechanical properties. One of the prime challenges is the production of these nanomaterials on a large scale. This review paper summarizes the synthesis of various carbon nanomaterials via the chemical vapor deposition (CVD) method. These carbon nanomaterials include fullerenes, carbon nanotubes (CNTs), carbon nanofibers (CNFs), graphene, carbide-derived carbon (CDC), carbon nano-onion (CNO) and MXenes. Furthermore, current challenges in the synthesis and application of these nanomaterials are highlighted with suggested areas for future research. PMID:29772760

  10. A Review of Carbon Nanomaterials’ Synthesis via the Chemical Vapor Deposition (CVD Method

    Directory of Open Access Journals (Sweden)

    Yehia M. Manawi

    2018-05-01

    Full Text Available Carbon nanomaterials have been extensively used in many applications owing to their unique thermal, electrical and mechanical properties. One of the prime challenges is the production of these nanomaterials on a large scale. This review paper summarizes the synthesis of various carbon nanomaterials via the chemical vapor deposition (CVD method. These carbon nanomaterials include fullerenes, carbon nanotubes (CNTs, carbon nanofibers (CNFs, graphene, carbide-derived carbon (CDC, carbon nano-onion (CNO and MXenes. Furthermore, current challenges in the synthesis and application of these nanomaterials are highlighted with suggested areas for future research.

  11. One-step in situ synthesis of SnO2/graphene nanocomposites and its application as an anode material for Li-ion batteries.

    Science.gov (United States)

    Liang, Junfei; Wei, Wei; Zhong, Da; Yang, Qinglin; Li, Lidong; Guo, Lin

    2012-01-01

    A facile one-step solution-based process to in situ synthesize SnO(2)/graphene (SG) nanocomposites was developed, by using the mixture of dimethyl sulfoxide (DMSO) and H(2)O as both solvent and reactant. The reduction of graphene oxide (GO) and the in situ formation of SnO(2) nanoparticles were realized in one step. The electrochemical experiments showed the composites provided a better Li-storage performance. The method presented in this paper may provide an effective, economic, and green strategy for the preparation of metal-oxide/graphene nanocomposites. © 2011 American Chemical Society

  12. An Efficient Method for the N-Bromosuccinimide Catalyzed Synthesis of Indolyl-Nitroalkanes

    Directory of Open Access Journals (Sweden)

    Ching-Fa Yao

    2009-10-01

    Full Text Available An efficient and practical method for the synthesis of indolyl-nitroalkane derivatives catalyzed by N-bromosuccinimide is described. The generality of this method was demonstrated by synthesizing an array of diverse 3-substituted indole derivatives by the reaction of different β-nitrostyrenes with various substituted indoles. Simple reaction conditions accompanied by good yields of indolyl-nitroalkanes are the merits of this methodology.

  13. Self-propagating high-temperature synthesis of TiC-WC composite materials

    International Nuclear Information System (INIS)

    Mas-Guindal, M.J.; Contreras, L.; Turrillas, X.; Vaughan, G.B.M.; Kvick, A.; Rodriguez, M.A.

    2006-01-01

    TiC-WC composites have been obtained in situ by self-propagating high-temperature synthesis (SHS) from a mixture of compacted powders of elemental titanium, tungsten and graphite. The Rietveld method has proved to be a useful tool to quantify the different phases in the reaction and calculate the cell parameters of the solid solution found in the products. The reaction has also been followed in real time by X-ray diffraction at the European Synchrotron Radiation Facility (ESRF ID-11 Materials Science Beamline). The mechanism of the reaction is discussed in terms of the diffusion of liquid titanium to yield titanium carbide with a solid solution of tungsten. The microstructures of the materials obtained by this method are presented

  14. Solution (in situ leach) mining of uranium: an overview

    International Nuclear Information System (INIS)

    Kuhaida, A.J. Jr.; Kelly, M.J.

    1978-01-01

    Increases in the demand for and price of uranium have made in-situ mining an attractive alternative to the open-pit and underground U mining methods. Up to 50% of the known ore-bearing sandstone in the western U.S. can be mined using the in-situ mining method. In-situ mining also offers a significant environmental advantage. Restoration of the contaminated groundwater is discussed

  15. Study of tryptophan assisted synthesis of gold nanoparticles by combining UV-Vis, fluorescence, and SERS spectroscopy

    International Nuclear Information System (INIS)

    Iosin, Monica; Baldeck, Patrice; Astilean, Simion

    2010-01-01

    We developed a rapid and non-toxic method for the preparation of colloidal gold nanoparticles (GNPs) by using tryptophan (Trp) as reducing/stabilizing agent. We show that the temperature has a major influence on the kinetics of gold ion reduction and the crystal growth, higher temperatures favoring the synthesis of anisotropic nanoparticles (triangles and hexagons). The as-synthesized nanostructures were characterized by UV-Vis absorption spectroscopy, transmission electron microscopy (TEM), X-ray diffraction (XRD), fluorescence, and surface-enhanced Raman scattering (SERS) spectroscopy. The UV-Vis measurements confirmed that temperature is a critical factor in the synthesis process, having a major effect on the shape of the synthesized GNPs. Moreover, fluorescence spectroscopy was able to monitor the quenching of the Trp fluorescence during the in situ synthesis of GNPs. Using Trp as molecular analyte to evaluate the SERS efficiency of as-prepared GNPs at different temperatures, we demonstrated that the Raman enhancement of the synthesized gold nanoplates is higher than that of the gold spherical nanoparticles.

  16. Difunctionalization of alkenes with iodine and tert-butyl hydroperoxide (TBHP) at room temperature for the synthesis of 1-(tert-butylperoxy)-2-iodoethanes.

    Science.gov (United States)

    Wang, Hao; Chen, Cui; Liu, Weibing; Zhu, Zhibo

    2017-01-01

    We developed a direct vicinal difunctionalization of alkenes with iodine and TBHP at room temperature. This iodination and peroxidation in a one-pot synthesis produces 1-( tert -butylperoxy)-2-iodoethanes, which are inaccessible through conventional synthetic methods. This method generates multiple radical intermediates in situ and has excellent regioselectivity, a broad substrate scope and mild conditions. The iodine and peroxide groups of 1-( tert -butylperoxy)-2-iodoethanes have several potential applications and allow further chemical modifications, enabling the preparation of synthetically valuable molecules.

  17. New Synthesis and Tritium Labeling of a Selective Ligand for Studying High-Affinity γ-Hydroxybutyrate (GHB) Binding Sites

    DEFF Research Database (Denmark)

    Vogensen, Stine B.; Marek, Ales; Bay, Tina

    2013-01-01

    3-Hydroxycyclopent-1-enecarboxylic acid (HOCPCA, 1) is a potent ligand for the high-affinity GHB binding sites in the CNS. An improved synthesis of 1 together with a very efficient synthesis of [3H]-1 is described. The radiosynthesis employs in situ generated lithium trimethoxyborotritide. Screen...

  18. Modular in situ-Functionalization Strategy: Multicomponent Polymerization via Palladium/Norbornene Cooperative Catalysis.

    Science.gov (United States)

    Yoon, Ki-Young; Dong, Guangbin

    2018-05-23

    Herein, we report the palladium/norbornene cooperatively catalyzed polymerization, which simplifies synthesis of functional aromatic polymers, including conjugated polymers. Specifically, an A2B2C-type multicomponent polymerization is developed using ortho-amination/ipso-alkynylation reaction for preparing various amine-functionalized arylacetylene-containing polymers. Within a single catalytic cycle, the amine side-chains are site-selectively installed in situ via C-H activation during the polymerization process, which represents a major difference from conventional cross-coupling polymerizations. This in situ-functionalization strategy enables modular incorporation of functional side-chains from simple monomers, thereby conveniently affording a diverse range of functional polymers. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  19. DOE In Situ Remediation Integrated Program

    International Nuclear Information System (INIS)

    Yow, J.L. Jr.

    1993-01-01

    The In Situ Remediation Integrated Program (ISRP) supports and manages a balanced portfolio of applied research and development activities in support of DOE environmental restoration and waste management needs. ISRP technologies are being developed in four areas: containment, chemical and physical treatment, in situ bioremediation, and in situ manipulation (including electrokinetics). the focus of containment is to provide mechanisms to stop contaminant migration through the subsurface. In situ bioremediation and chemical and physical treatment both aim to destroy or eliminate contaminants in groundwater and soils. In situ manipulation (ISM) provides mechanisms to access contaminants or introduce treatment agents into the soil, and includes other technologies necessary to support the implementation of ISR methods. Descriptions of each major program area are provided to set the technical context of the ISM subprogram. Typical ISM needs for major areas of in situ remediation research and development are identified

  20. Applications of in situ hybridization to plant-improvement

    International Nuclear Information System (INIS)

    Abbasi, F.M.

    2004-01-01

    In situ hybridization is a powerful method for characteristic alien addition and substitution lines. RFLP analysis can identify the presence of a particular individual chromosome, but whether they are as a pair or as a single chromosome cannot be determined. In situ hybridization has become established as an essential method in cell and molecular biology. It is able to link DNA sequences with their organization and physical position. The rate of technology-development in the field of in situ hybridization has been rapid: radioactive probes are now rarely used, while labeling methods, fluorochromes, chromosomes and tissue-preparation methods, microscope and imaging technology have all useful in functional genomics and localization of transgenes on the chromosomes. (author)

  1. Synthesis and characterization of copper nanofluid by a novel one-step method

    International Nuclear Information System (INIS)

    Kumar, S. Ananda; Meenakshi, K. Shree; Narashimhan, B.R.V.; Srikanth, S.; Arthanareeswaran, G.

    2009-01-01

    This paper presents a novel one-step method for the preparation of stable, non-agglomerated copper nanofluids by reducing copper sulphate pentahydrate with sodium hypophosphite as reducing agent in ethylene glycol as base fluid by means of conventional heating. This is an in situ, one-step method which gives high yield of product with less time consumption. The characterization of the nanofluid is done by particle size analyzer, X-ray diffraction topography, UV-vis analysis and Fourier transform infrared spectroscopy (FT-IR) followed by the study of thermal conductivity of nanofluid by the transient hot wire method

  2. Final Report Scalable Analysis Methods and In Situ Infrastructure for Extreme Scale Knowledge Discovery

    Energy Technology Data Exchange (ETDEWEB)

    O' Leary, Patrick [Kitware, Inc., Clifton Park, NY (United States)

    2017-09-13

    The primary challenge motivating this project is the widening gap between the ability to compute information and to store it for subsequent analysis. This gap adversely impacts science code teams, who can perform analysis only on a small fraction of the data they calculate, resulting in the substantial likelihood of lost or missed science, when results are computed but not analyzed. Our approach is to perform as much analysis or visualization processing on data while it is still resident in memory, which is known as in situ processing. The idea in situ processing was not new at the time of the start of this effort in 2014, but efforts in that space were largely ad hoc, and there was no concerted effort within the research community that aimed to foster production-quality software tools suitable for use by Department of Energy (DOE) science projects. Our objective was to produce and enable the use of production-quality in situ methods and infrastructure, at scale, on DOE high-performance computing (HPC) facilities, though we expected to have an impact beyond DOE due to the widespread nature of the challenges, which affect virtually all large-scale computational science efforts. To achieve this objective, we engaged in software technology research and development (R&D), in close partnerships with DOE science code teams, to produce software technologies that were shown to run efficiently at scale on DOE HPC platforms.

  3. A novel method for the in situ determination of concentration gradients in the electrolyte of Li-ion Batteries

    NARCIS (Netherlands)

    Zhou, J.; Danilov, D.; Notten, P.H.L.

    2006-01-01

    An electrochemical method has been developed for the in situ determination of concentration gradients in the electrolyte of sealed Li-ion batteries by measuring the potential difference between microreference electrodes. Formulas relating the concentration gradient and the potential difference

  4. Synthesis of nitrogen-doped graphene via solid microwave method

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Li, E-mail: zhangli379@sohu.com [School of Electrical Engineering, Dalian University of Technology, Dalian, Liaoning 116024 (China); Ji, Bingcheng, E-mail: debbo.jee@outlook.com [School of Electrical Engineering, Dalian University of Technology, Dalian, Liaoning 116024 (China); Wang, Kai [School of Electrical Engineering, Dalian University of Technology, Dalian, Liaoning 116024 (China); Song, Jinyan [School of Information Engineering, Dalian Ocean University, Dalian, Liaoning 116024 (China)

    2014-07-01

    Graphical abstract: - Highlights: • A direct solid microwave method is developed to prepare nitrogen-doped graphene. • The method consists of two steps, namely the functionalization and microwave irradiation. • Melamine can serve as not only functionalizing agent but also nitrogen source. - Abstract: In this paper, we propose a solid microwave-mediated method for scalable production of nitrogen-doped graphene sheets (NGS) using low-cost industrial material melamine as functionalizing agent and nitrogen source. The strong interaction of microwaves with graphene oxide has been fully utilized to generate in situ heating that induces the decompose melamine and nitrogen doping of graphene. The morphology, structure, and components of the as-produced nitrogen-doped graphene are characterized by scanning electron microscopy (SEM), transmission electron microscope (TEM), Brunauer–Emmett–Teller (BET), pore-size distribution (PSD), Fourier transform infrared spectroscopy (FTIR), X-ray photoelectron spectra (XPS), X-ray diffraction (XRD), and Raman spectroscopy. The results show NGS can be successfully synthesized via this strategy.

  5. Synthesis of nitrogen-doped graphene via solid microwave method

    International Nuclear Information System (INIS)

    Zhang, Li; Ji, Bingcheng; Wang, Kai; Song, Jinyan

    2014-01-01

    Graphical abstract: - Highlights: • A direct solid microwave method is developed to prepare nitrogen-doped graphene. • The method consists of two steps, namely the functionalization and microwave irradiation. • Melamine can serve as not only functionalizing agent but also nitrogen source. - Abstract: In this paper, we propose a solid microwave-mediated method for scalable production of nitrogen-doped graphene sheets (NGS) using low-cost industrial material melamine as functionalizing agent and nitrogen source. The strong interaction of microwaves with graphene oxide has been fully utilized to generate in situ heating that induces the decompose melamine and nitrogen doping of graphene. The morphology, structure, and components of the as-produced nitrogen-doped graphene are characterized by scanning electron microscopy (SEM), transmission electron microscope (TEM), Brunauer–Emmett–Teller (BET), pore-size distribution (PSD), Fourier transform infrared spectroscopy (FTIR), X-ray photoelectron spectra (XPS), X-ray diffraction (XRD), and Raman spectroscopy. The results show NGS can be successfully synthesized via this strategy

  6. In Situ Monitoring of the Mechanosynthesis of the Archetypal Metal-Organic Framework HKUST-1: Effect of Liquid Additives on the Milling Reactivity.

    Science.gov (United States)

    Stolar, Tomislav; Batzdorf, Lisa; Lukin, Stipe; Žilić, Dijana; Motillo, Cristina; Friščić, Tomislav; Emmerling, Franziska; Halasz, Ivan; Užarević, Krunoslav

    2017-06-05

    We have applied in situ monitoring of mechanochemical reactions by high-energy synchrotron powder X-ray diffraction to study the role of liquid additives on the mechanochemical synthesis of the archetypal metal-organic framework (MOF) HKUST-1, which was one of the first and is still among the most widely investigated MOF materials to be synthesized by solvent-free procedures. It is shown here how the kinetics and mechanisms of the mechanochemical synthesis of HKUST-1 can be influenced by milling conditions and additives, yielding on occasion two new and previously undetected intermediate phases containing a mononuclear copper core, and that finally rearrange to form the HKUST-1 architecture. On the basis of in situ data, we were able to tune and direct the milling reactions toward the formation of these intermediates, which were isolated and characterized by spectroscopic and structural means and their magnetic properties compared to those of HKUST-1. The results have shown that despite the relatively large breadth of analysis available for such widely investigated materials as HKUST-1, in situ monitoring of milling reactions can help in the detection and isolation of new materials and to establish efficient reaction conditions for the mechanochemical synthesis of porous MOFs.

  7. Advances in heterocycle synthesis via [3+m]-cycloaddition reactions involving an azaoxyallyl cation as the key intermediate.

    Science.gov (United States)

    Xuan, Jun; Cao, Xia; Cheng, Xiao

    2018-05-17

    Heterocyclic compounds are widely found in many natural isolates and medicinally relevant compounds, as well as some fine chemicals. The development of general and efficient methods for the construction of heterocyclic compounds is one of the most important tasks in synthetic organic chemistry. Along these lines, [3+m]-cycloaddition reactions involving in situ generated azaoxyallyl cations as the 3-atom units have emerged as a powerful method for the synthesis of nitrogen-containing heterocycles. In this feature article, we highlight recent advances in this rapidly growing area, mainly focusing on the reaction design as well as the reaction mechanism.

  8. Fabrication of Titanium Diboride-Cu Composite by Self-High Temperature Synthesis plus Quick Press

    Institute of Scientific and Technical Information of China (English)

    Jinyong ZHANG; Zhengyi FU; Weimin WANG

    2005-01-01

    Titanium diboride based composites, good candidates for contact materials, have high hardness, Young's modulus,high temperature stability, and excellent electrical, thermal conductivity. However a good interface of TiB2/Cu is very difficult to achieve for oxidation of TiB2. To avoid this oxidation behavior, the in situ combusting synthesis technology, SHS, was used to prepare TiB2/Cu composite. Thecharacters of Ti-B-xCu SHS were studied in detail,such as combustion temperature, products phases and grain size. Based on the experimental results a proper technology way of self-high temperature synthesis plus quick press (SHS/QP) was determined and compact TiB2/Cu composites with relative density over than 97 pct of the theoretical were fabricated by this method. The properties and microstructures of these TiB2 based composites were also investigated.

  9. In situ formation of ZrB2 particulates and their influence on microstructure and tensile behavior of AA7075 aluminum matrix composites

    Directory of Open Access Journals (Sweden)

    J. David Raja Selvam

    2017-02-01

    Full Text Available In situ synthesis of aluminum matrix composites (AMCs has become a popular method due to several advantages over conventional stir casting method. In the present study, AA7075/ZrB2 AMCs reinforced with various content of ZrB2 particulates (0, 3, 6, 9 and 12 wt.% were synthesized by the in situ reaction of molten aluminum with inorganic salts K2ZrF6 and KBF4. The composites were characterized using XRD, OM, SEM, EBSD and TEM. The XRD patterns revealed the formation of ZrB2 particulates without the presence of any other compounds. The formation of ZrB2 particulates refined the grains of aluminum matrix extensively. Most of the ZrB2 particulates were located near the grain boundaries. The ZrB2 particulates exhibited various morphologies including spherical, cylindrical and hexagonal shapes. The size of the ZrB2 particulates was in the order of nano, sub micron and micron level. A good interfacial bonding was observed between the aluminum matrix and the ZrB2 particulates. The in situ formed ZrB2 particulates enhanced the mechanical properties such as microhardness and the ultimate tensile strength. Various strengthening mechanisms were identified.

  10. Macrokinetics of carbon nanotubes synthesis by the chemical vapor deposition method

    Science.gov (United States)

    Rukhov, Artem; Dyachkova, Tatyana; Tugolukov, Evgeny; Besperstova, Galina

    2017-11-01

    A new approach to studying and developing basic processes which take place on the surface of a metal catalyst during the thermal decomposition of carbonaceous substances in the carbon nanotubes synthesis by the chemical vapor deposition method was proposed. In addition, an analysis was made of the interrelationships between these thermal, diffusion, hydrodynamic and other synthesis processes. A strong effect of the catalyst regeneration stage on the stage of nanotube formation has been shown. Based on the developed approach, a mathematical model was elaborated. Comparison of the calculation and the experiment carried out with the NiO-MgO catalyst at propane flow rate of 50 mL/min (standard conditions) and ethanol flow rate 0.3 mL/min (liq.) has revealed a discrepancy of less than 10%.

  11. High-yield Synthesis of Multiwalled Carbon Nanotube by Mechanothermal Method

    Directory of Open Access Journals (Sweden)

    Manafi SA

    2009-01-01

    Full Text Available Abstract This study reports on the mechanothermal synthesis of multiwalled carbon nanotube (MWCNTs from elemental graphite powder. Initially, high ultra-active graphite powder can be obtained by mechanical milling under argon atmosphere. Finally, the mechanical activation product is heat-treated at 1350°C for 2–4 h under argon gas flow. After heat-treatment, active graphite powders were successfully changed into MWCNTs with high purity. The XRD analyses showed that in the duration 150 h of milling, all the raw materials were changed to the desired materials. From the broadening of the diffraction lines in the XRD patterns, it was concluded that the graphite crystallites were nanosized, and raising the milling duration resulted in the fineness of the particles and the increase of the strain. The structure and morphology of MWCNTs were investigated using scanning electron microscopy (SEM and high-resolution transmission electron microscopy (HRTEM. The yield of MWCNTs was estimated through SEM and TEM observations of the as-prepared samples was to be about 90%. Indeed, mechanothermal method is of interest for fundamental understanding and improvement of commercial synthesis of carbon nanotubes (CNTs. As a matter of fact, the method of mechanothermal guarantees the production of MWCNTs suitable for different applications.

  12. Synthesis of thermoplastic starch-bacterial cellulose nanocomposites via in situ fermentation

    OpenAIRE

    Osorio, Marlon A.; Restrepo, David; Velásquez-Cock, Jorge A.; Zuluaga, Robin O.; Montoya, Ursula; Rojas, Orlando; Gañán, Piedad F.; Marin, Diana; Castro, Cristina I.

    2014-01-01

    In this paper, a nanocomposite based on thermoplastic starch (TPS) reinforced with bacterial cellulose (BC) nanoribbons was synthesized by in situ fermentation and chemical crosslinking. BC nanoribbons were produced by a Colombian native strain of Gluconacetobacter medellinensis; the nanocomposite was plasticized with glycerol and crosslinked with citric acid. The reinforcement percentage in the nanocomposites remained constant throughout the fermentation time because of the TPS absorption ca...

  13. Bioinspired Synthesis of Monolithic and Layered Aerogels.

    Science.gov (United States)

    Han, Xiao; Hassan, Khalil T; Harvey, Alan; Kulijer, Dejan; Oila, Adrian; Hunt, Michael R C; Šiller, Lidija

    2018-04-25

    Aerogels are the least dense and most porous materials known to man, with potential applications from lightweight superinsulators to smart energy materials. To date their use has been seriously hampered by their synthesis methods, which are laborious and expensive. Taking inspiration from the life cycle of the damselfly, a novel ambient pressure-drying approach is demonstrated in which instead of employing low-surface-tension organic solvents to prevent pore collapse during drying, sodium bicarbonate solution is used to generate pore-supporting carbon dioxide in situ, significantly reducing energy, time, and cost in aerogel production. The generic applicability of this readily scalable new approach is demonstrated through the production of granules, monoliths, and layered solids with a number of precursor materials. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  14. One-Pot Multicomponent Coupling Methods for the Synthesis of Diastereo- and Enantioenriched (Z)-Trisubstituted Allylic Alcohols

    Science.gov (United States)

    Kerrigan, Michael H.; Jeon, Sang-Jin; Chen, Young K.; Salvi, Luca; Carroll, Patrick J.; Walsh, Patrick J.

    2009-01-01

    (Z)-Trisubstituted allylic alcohols are widespread structural motifs in natural products and biologically active compounds but are difficult to directly prepare. Introduced herein is a general one-pot multicomponent coupling method for the synthesis of (Z)-α,α,β-trisubstituted allylic alcohols. (Z)-Trisubstituted vinylzinc reagents are formed in situ by initial hydroboration of 1-bromo-1-alkynes. Addition of dialkylzinc reagents induces a 1,2-metallate rearrangement that is followed by a boron-to-zinc transmetallation. The resulting vinylzinc reagents add to a variety of prochiral aldehydes to produce racemic (Z)-trisubstituted allylic alcohols. When enantioenriched aldehyde substrates are employed (Z)-trisubstituted allylic alcohols are isolated with high dr (>20:1 in many cases). For example, vinylation of enantioenriched benzyl protected α- and β-hydroxy propanal derivatives furnished the expected anti-Felkin addition products via chelation control. Surprisingly, silyl protected α-hydroxy aldehydes also afford anti-Felkin addition products. A protocol for the catalytic asymmetric addition of (Z)-trisubstituted vinylzinc reagents to prochiral aldehydes with a (−)-MIB-based catalyst has also been developed. Several additives were investigated as inhibitors of the Lewis acidic alkylzinc halide byproducts, which promote the background reaction to form the racemate. α-Ethyl and α-cyclohexyl (Z)-trisubstituted allylic alcohols can now be synthesized with excellent levels of enantioselectivity in the presence of diamine inhibitors. PMID:19476375

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

    Science.gov (United States)

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

    2018-03-01

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

  16. Differential sensitivity to aphidicolin of replicative DNA synthesis and ultraviolet-induced unscheduled DNA synthesis in vivo in mammalian cells

    International Nuclear Information System (INIS)

    Seki, Shuji; Hosogi, Nobuo; Oda, Takuzo

    1984-01-01

    In vivo in mammalian cells, ultraviolet-induced unscheduled DNA synthesis was less sensitive to aphidicolin than was replicative DNA synthesis. Replicative DNA synthesis in HeLa, HEp-2, WI-38 VA-13 and CV-1 cells was inhibited more than 97 % by aphidicolin at 10 μg/ml, whereas aphidicolin inhibition of DNA synthesis in ultraviolet-irradiated cells varied between 30 % and 90 % depending on cell types and assay conditions. Aphidicolin inhibition of unscheduled DNA synthesis (UDS) in HeLa cells increased gradually with increasing aphidicolin concentration and reached approximately 90 % at 100 μg/ml aphidicolin. A significant fraction of UDS in ultraviolet-irradiated HEp-2 cells was resistant to aphidicolin even at 300 μg/ml. Considered along with related information reported previously, the present results suggest that both aphidicolin-sensitive and insensitive DNA polymerases, DNA polymerase α and a non-α DNA polymerase (possibly DNA polymerase β), are involved in in situ UDS in these ultraviolet-irradiated cells. Comparison of staphylococcal nuclease sensitivity between DNAs repaired in the presence and in the absence of aphidicolin in HEp-2 cells suggested that the involvement of DNA polymerase α in UDS favored DNA synthesis in the intranucleosomal region. (author)

  17. Exploration and characterization of new synthesis methods for C60 colloidal suspensions in water

    Science.gov (United States)

    Hilburn, Martha E.

    Buckminsterfullerene, C60, has been used in the production of several commercial products from badminton racquets and lubricants for their mechanical properties to cosmetics and even dietary supplements for their "antioxidant" properties. Multi-ton production of C60 began in 2003 encouraging serious consideration of its fate in the environment in the case of an accidental release or improper disposal. Although C60 is practically insoluble in water, it readily forms stable aqueous colloidal suspensions (termed nC60) through solvent exchange methods or long-term vigorous stirring in water. Two new solvent exchange methods for synthesizing nC60 are presented. These methods combine key advantages of multiple existing synthesis methods including high yield, narrow particle size distribution, short synthesis time, and an absence of solvents such as tetrahydrofuran that have historically caused problems in laboratory synthesized aggregates. The resulting samples are attractive candidates for use in controlled environmental impact, biological, and toxicity studies. An improved method for quantifying residual solvents in nC60 samples utilizing solid phase micro extraction gas chromatography mass spectrometry (SPME-GC-MS) is also discussed.

  18. In situ one-pot synthesis of graphene–polyaniline nanofiber composite for high-performance electrochemical capacitors

    International Nuclear Information System (INIS)

    Jin, Yuhong; Fang, Mou; Jia, Mengqiu

    2014-01-01

    In this work, graphene–polyaniline nanofiber (G/PANI-F) composite is prepared through a new and one-pot method that includes the reduction of graphene oxide (GO) by aniline and then followed by in-situ polymerization. Aniline plays the two roles in this method: as a chemical reducing agent to reduce GO to graphene and as a monomer to prepare polyaniline nanofiber (PANI-F). Fourier transform infrared spectroscopy, X-ray diffraction, Raman spectra, X-ray photoelectron spectroscopy and transmission electron microscopy are employed to confirm that GO can be reduced by aniline and PANI-F can be deposited on the surface of graphene. The electrochemical properties of G/PANI-F composite electrode are measured by using cyclic voltammetry, galvanostatic charge–discharge test and electrochemical impedance spectroscopy. The G/PANI-F composite electrode exhibits enhanced specific capacitance of 965 F g −1 at 0.5 A g −1 and the capacity retention is 90% after 2000 cycles.

  19. Asymmetric synthesis II more methods and applications

    CERN Document Server

    Christmann, Mathias

    2012-01-01

    After the overwhelming success of 'Asymmetric Synthesis - The Essentials', narrating the colorful history of asymmetric synthesis, this is the second edition with latest subjects and authors. While the aim of the first edition was mainly to honor the achievements of the pioneers in asymmetric syntheses, the aim of this new edition was bringing the current developments, especially from younger colleagues, to the attention of students. The format of the book remained unchanged, i.e. short conceptual overviews by young leaders in their field including a short biography of the authors. The growing multidisciplinary research within chemistry is reflected in the selection of topics including metal catalysis, organocatalysis, physical organic chemistry, analytical chemistry, and its applications in total synthesis. The prospective reader of this book is a graduate or undergraduate student of advanced organic chemistry as well as the industrial chemist who wants to get a brief update on the current developments in th...

  20. In-situ preparation of functionalized molecular sieve material and a methodology to remove template

    Science.gov (United States)

    Yadav, Rekha; Ahmed, Maqsood; Singh, Arvind Kumar; Sakthivel, Ayyamperumal

    2016-03-01

    A series of diaminosilane-functionalized silicoaluminophosphate molecular sieve (SAPO-37) was prepared by in-situ synthesis, and a novel method was developed for the selective removal of structure directing agent (SDA)/template from the functionalized SAPO-37.The complete removal of the SDA was evident according to FT-IR, TGA, 13C MAS-NMR and elemental analysis. The developed method was found to be efficient for removal of template from microporous molecular sieve viz., SAPO-37 and can be applied for other microporous molecular sieves such as SAPO-5, SAPO-40, etc. The powder XRD pattern of the template-removed samples showed a highly crystalline SAPO-37 phase. Argentometric titration revealed that more than 90% of diamine functionality exposed on the surface was accessible for catalytic applications. The resultant materials showed promising activity for ring opening of epoxide with aniline to yield β-amino-alcohol.

  1. In-situ preparation of functionalized molecular sieve material and a methodology to remove template.

    Science.gov (United States)

    Yadav, Rekha; Ahmed, Maqsood; Singh, Arvind Kumar; Sakthivel, Ayyamperumal

    2016-03-10

    A series of diaminosilane-functionalized silicoaluminophosphate molecular sieve (SAPO-37) was prepared by in-situ synthesis, and a novel method was developed for the selective removal of structure directing agent (SDA)/template from the functionalized SAPO-37.The complete removal of the SDA was evident according to FT-IR, TGA, (13)C MAS-NMR and elemental analysis. The developed method was found to be efficient for removal of template from microporous molecular sieve viz., SAPO-37 and can be applied for other microporous molecular sieves such as SAPO-5, SAPO-40, etc. The powder XRD pattern of the template-removed samples showed a highly crystalline SAPO-37 phase. Argentometric titration revealed that more than 90% of diamine functionality exposed on the surface was accessible for catalytic applications. The resultant materials showed promising activity for ring opening of epoxide with aniline to yield β-amino-alcohol.

  2. Image analyzing method to evaluate in situ bioluminescence from an obligate anaerobe cultivated under various dissolved oxygen concentrations.

    Science.gov (United States)

    Ninomiya, Kazuaki; Yamada, Ryuji; Matsumoto, Masami; Fukiya, Satoru; Katayama, Takane; Ogino, Chiaki; Shimizu, Nobuaki

    2013-02-01

    An image analyzing method was developed to evaluate in situ bioluminescence expression, without exposing the culture sample to the ambient oxygen atmosphere. Using this method, we investigated the effect of dissolved oxygen concentration on bioluminescence from an obligate anaerobe Bifidobacterium longum expressing bacterial luciferase which catalyzes an oxygen-requiring bioluminescent reaction. Copyright © 2012 The Society for Biotechnology, Japan. Published by Elsevier B.V. All rights reserved.

  3. Cochrane Qualitative and Implementation Methods Group guidance series-paper 3: methods for assessing methodological limitations, data extraction and synthesis, and confidence in synthesized qualitative findings.

    Science.gov (United States)

    Noyes, Jane; Booth, Andrew; Flemming, Kate; Garside, Ruth; Harden, Angela; Lewin, Simon; Pantoja, Tomas; Hannes, Karin; Cargo, Margaret; Thomas, James

    2018-05-01

    The Cochrane Qualitative and Implementation Methods Group develops and publishes guidance on the synthesis of qualitative and mixed-method implementation evidence. Choice of appropriate methodologies, methods, and tools is essential when developing a rigorous protocol and conducting the synthesis. Cochrane authors who conduct qualitative evidence syntheses have thus far used a small number of relatively simple methods to address similarly written questions. Cochrane has invested in methodological work to develop new tools and to encourage the production of exemplar reviews to show the value of more innovative methods that address a wider range of questions. In this paper, in the series, we report updated guidance on the selection of tools to assess methodological limitations in qualitative studies and methods to extract and synthesize qualitative evidence. We recommend application of Grades of Recommendation, Assessment, Development, and Evaluation-Confidence in the Evidence from Qualitative Reviews to assess confidence in qualitative synthesized findings. This guidance aims to support review authors to undertake a qualitative evidence synthesis that is intended to be integrated subsequently with the findings of one or more Cochrane reviews of the effects of similar interventions. The review of intervention effects may be undertaken concurrently with or separate to the qualitative evidence synthesis. We encourage further development through reflection and formal testing. Copyright © 2017 Elsevier Inc. All rights reserved.

  4. Thermodynamics parameters of nano-Ni/PS composites prepared by in situ polymerization method

    International Nuclear Information System (INIS)

    Liao Qilong; Xiong Jie; Ning Haixia

    2011-01-01

    Spherical nickel nanoparticles with about 75∼200 nm in size were obtained by a liquid reduction method. The nickel nanoparticles/PS composites were synthesized via in situ polymerization method. XRD, FTIR, SEM and TG-DSC were respectively used to measure the properties of nickel nanoparticles, the microstructure of as-prepared composites samples, the distribution of nickel nanoparticles in PS and the thermodynamic parameters of as-prepared composites. The results show that the nickel nanoparticles will enhance the glass transition temperature of nano-Ni/PS composites. The enthalpy of composites is heightened by increasing of doping dose, and it reaches the top when the doping dose is from 1% to 2%. The specific heat of the composites will reduce with the doping dose of nickel nanoparticles increasing. (authors)

  5. Rh(III)-catalyzed olefination of N-sulfonyl imines: synthesis of ortho-olefinated benzaldehydes.

    Science.gov (United States)

    Zhang, Tao; Wu, Lamei; Li, Xingwei

    2013-12-20

    Rh(III)-catalyzed olefination of N-sulfonyl imines using acrylates and styrenes has been achieved for the synthesis of ortho-olefinated benaldehydes. This reaction proceeds via a chelation assisted C-H olefination/in situ hydrolysis process.

  6. Enantioselective Synthesis of α-Mercapto-β-amino Esters via Rh(II)/Chiral Phosphoric Acid-Cocatalyzed Three-Component Reaction of Diazo Compounds, Thiols, and Imines.

    Science.gov (United States)

    Xiao, Guolan; Ma, Chaoqun; Xing, Dong; Hu, Wenhao

    2016-12-02

    An enantioselective method for the synthesis of α-mercapto-β-amino esters has been developed via a rhodium(II)/chiral phosphoric acid-cocatalyzed three-component reaction of diazo compounds, thiols, and imines. This transformation is proposed to proceed through enantioselective trapping of the sulfonium ylide intermediate generated in situ from the diazo compound and thiol by the phosphoric acid-activated imine. With this method, a series of α-mercapto-β-amino esters were obtained in good yields with moderate to good stereoselectivities.

  7. Methods of producing alkylated hydrocarbons from an in situ heat treatment process liquid

    Science.gov (United States)

    Roes, Augustinus Wilhelmus Maria [Houston, TX; Mo, Weijian [Sugar Land, TX; Muylle, Michel Serge Marie [Houston, TX; Mandema, Remco Hugo [Houston, TX; Nair, Vijay [Katy, TX

    2009-09-01

    A method for producing alkylated hydrocarbons is disclosed. Formation fluid is produced from a subsurface in situ heat treatment process. The formation fluid is separated to produce a liquid stream and a first gas stream. The first gas stream includes olefins. The liquid stream is fractionated to produce at least a second gas stream including hydrocarbons having a carbon number of at least 3. The first gas stream and the second gas stream are introduced into an alkylation unit to produce alkylated hydrocarbons. At least a portion of the olefins in the first gas stream enhance alkylation.

  8. Size Controlled Synthesis of Starch Nanoparticles by a Microemulsion Method

    Directory of Open Access Journals (Sweden)

    Suk Fun Chin

    2014-01-01

    Full Text Available Controllable particles sizes of starch nanoparticles were synthesized via a precipitation in water-in-oil microemulsion approach. Microemulsion method offers the advantages of ultralow interfacial tension, large interfacial area, and being thermodynamically stable and affords monodispersed nanoparticles. The synthesis parameters such as stirring rates, ratios of oil/cosurfactant, oil phases, cosurfactants, and ratios of water/oil were found to affect the mean particle size of starch nanoparticles. Starch nanoparticles with mean particles sizes of 109 nm were synthesized by direct nanoprecipitation method, whereas by using precipitation in microemulsion approach, starch nanoparticles with smaller mean particles sizes of 83 nm were obtained.

  9. Current status and future directions for in situ transmission electron microscopy

    Energy Technology Data Exchange (ETDEWEB)

    Taheri, Mitra L. [Department of Materials Science and Engineering, Drexel University (United States); Stach, Eric A. [Center for Functional Nanomaterials, National Laboratory, Brookhaven (United States); Arslan, Ilke [Pacific Northwest National Laboratory, Physical and Computational Sciences Directorate, 902 Battelle Blvd, Richland, WA (United States); Crozier, P.A. [School for Engineering of Matter, Transport and Energy, Arizona State University, Tempe, AZ 85281 (United States); Kabius, Bernd C. [The Pennsylvania State University, University Park, PA 16802 (United States); LaGrange, Thomas [Lawrence Livermore National Laboratory, Physical and Life Science Directorate, Condensed Matter and Materials Division, 7000 East Avenue, P.O. 808 L-356 (United States); Minor, Andrew M. [Department of Materials Science & Engineering, University of California, Berkeley and National Center for Electron Microscopy, Molecular Foundry, Lawrence Berkeley National Laboratory, One Cyclotron Road, MS 72, Berkeley, CA (United States); Takeda, Seiji [Institute of Scientific and Industrial Research (ISIR), Osaka University, 8-1 Mihogaoka, Ibaraki, Osaka 567-0047 (Japan); Tanase, Mihaela [Center for Nanoscale Science and Technology, National Institute of Standards and Technology, Gaithersburg, MD 20899-6203 (United States); Wagner, Jakob B. [Center for Electron Nanoscopy, Technical University of Denmark, Kgs, Lyngby (Denmark); Sharma, Renu, E-mail: renu.sharma@nist.gov [Center for Nanoscale Science and Technology, National Institute of Standards and Technology, Gaithersburg, MD 20899-6203 (United States)

    2016-11-15

    This review article discusses the current and future possibilities for the application of in situ transmission electron microscopy to reveal synthesis pathways and functional mechanisms in complex and nanoscale materials. The findings of a group of scientists, representing academia, government labs and private sector entities (predominantly commercial vendors) during a workshop, held at the Center for Nanoscale Science and Technology- National Institute of Science and Technology (CNST-NIST), are discussed. We provide a comprehensive review of the scientific needs and future instrument and technique developments required to meet them. - Highlights: • Evaluation of currently available technology for performing in situ experiments using transmission electron microscope. • Limitations of currently available instrumentation with respect to base TEM, specialty TEM holders, and data acquisition systems. • Guidelines and wish list for the areas of future development.

  10. Current status and future directions for in situ transmission electron microscopy

    International Nuclear Information System (INIS)

    Taheri, Mitra L.; Stach, Eric A.; Arslan, Ilke; Crozier, P.A.; Kabius, Bernd C.; LaGrange, Thomas; Minor, Andrew M.; Takeda, Seiji; Tanase, Mihaela; Wagner, Jakob B.; Sharma, Renu

    2016-01-01

    This review article discusses the current and future possibilities for the application of in situ transmission electron microscopy to reveal synthesis pathways and functional mechanisms in complex and nanoscale materials. The findings of a group of scientists, representing academia, government labs and private sector entities (predominantly commercial vendors) during a workshop, held at the Center for Nanoscale Science and Technology- National Institute of Science and Technology (CNST-NIST), are discussed. We provide a comprehensive review of the scientific needs and future instrument and technique developments required to meet them. - Highlights: • Evaluation of currently available technology for performing in situ experiments using transmission electron microscope. • Limitations of currently available instrumentation with respect to base TEM, specialty TEM holders, and data acquisition systems. • Guidelines and wish list for the areas of future development.

  11. Triplex in-situ hybridization

    Science.gov (United States)

    Fresco, Jacques R.; Johnson, Marion D.

    2002-01-01

    Disclosed are methods for detecting in situ the presence of a target sequence in a substantially double-stranded nucleic acid segment, which comprises: a) contacting in situ under conditions suitable for hybridization a substantially double-stranded nucleic acid segment with a detectable third strand, said third strand being capable of hybridizing to at least a portion of the target sequence to form a triple-stranded structure, if said target sequence is present; and b) detecting whether hybridization between the third strand and the target sequence has occured.

  12. Transmission electron microscopic method for gene mapping on polytene chromosomes by in situ hybridization

    OpenAIRE

    Wu, Madeline; Davidson, Norman

    1981-01-01

    A transmission electron microscope method for gene mapping by in situ hybridization to Drosophila polytene chromosomes has been developed. As electron-opaque labels, we use colloidal gold spheres having a diameter of 25 nm. The spheres are coated with a layer of protein to which Escherichia coli single-stranded DNA is photochemically crosslinked. Poly(dT) tails are added to the 3' OH ends of these DNA strands, and poly(dA) tails are added to the 3' OH ends of a fragmented cloned Drosophila DN...

  13. Neutron reflectivity as method to study in-situ adsorption of phospholipid layers to solid-liquid interfaces

    DEFF Research Database (Denmark)

    Gutberlet, Thomas; Klösgen, Beate Maria; Krastev, Rumen

    2004-01-01

    variation. It was observed that the method was capable of visualizing the adsorption of phospholipid layers to different solid-liquid interfaces and to resolve structural details at Angstroem resolution. The results depended strongly on a sufficiently good signal-to-noise ratio of the specific measurements......The use of neutron reflectivity as a method to study in-situ adsorption of phospholipid layers to solid-liquid interfaces was analyzed. The most important advantage of neutron reflectometry is the possibility to very the refractive index of the specific sample by isotope exchange, called contrast...

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

    NARCIS (Netherlands)

    Koutsopoulos, S.

    2002-01-01

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

  15. Detection of short repeated genomic sequences on metaphase chromosomes using padlock probes and target primed rolling circle DNA synthesis

    Directory of Open Access Journals (Sweden)

    Stougaard Magnus

    2007-11-01

    Full Text Available Abstract Background In situ detection of short sequence elements in genomic DNA requires short probes with high molecular resolution and powerful specific signal amplification. Padlock probes can differentiate single base variations. Ligated padlock probes can be amplified in situ by rolling circle DNA synthesis and detected by fluorescence microscopy, thus enhancing PRINS type reactions, where localized DNA synthesis reports on the position of hybridization targets, to potentially reveal the binding of single oligonucleotide-size probe molecules. Such a system has been presented for the detection of mitochondrial DNA in fixed cells, whereas attempts to apply rolling circle detection to metaphase chromosomes have previously failed, according to the literature. Methods Synchronized cultured cells were fixed with methanol/acetic acid to prepare chromosome spreads in teflon-coated diagnostic well-slides. Apart from the slide format and the chromosome spreading everything was done essentially according to standard protocols. Hybridization targets were detected in situ with padlock probes, which were ligated and amplified using target primed rolling circle DNA synthesis, and detected by fluorescence labeling. Results An optimized protocol for the spreading of condensed metaphase chromosomes in teflon-coated diagnostic well-slides was developed. Applying this protocol we generated specimens for target primed rolling circle DNA synthesis of padlock probes recognizing a 40 nucleotide sequence in the male specific repetitive satellite I sequence (DYZ1 on the Y-chromosome and a 32 nucleotide sequence in the repetitive kringle IV domain in the apolipoprotein(a gene positioned on the long arm of chromosome 6. These targets were detected with good efficiency, but the efficiency on other target sites was unsatisfactory. Conclusion Our aim was to test the applicability of the method used on mitochondrial DNA to the analysis of nuclear genomes, in particular as

  16. In situ surface roughness measurement using a laser scattering method

    Science.gov (United States)

    Tay, C. J.; Wang, S. H.; Quan, C.; Shang, H. M.

    2003-03-01

    In this paper, the design and development of an optical probe for in situ measurement of surface roughness are discussed. Based on this light scattering principle, the probe which consists of a laser diode, measuring lens and a linear photodiode array, is designed to capture the scattered light from a test surface with a relatively large scattering angle ϕ (=28°). This capability increases the measuring range and enhances repeatability of the results. The coaxial arrangement that incorporates a dual-laser beam and a constant compressed air stream renders the proposed system insensitive to movement or vibration of the test surface as well as surface conditions. Tests were conducted on workpieces which were mounted on a turning machine that operates with different cutting speeds. Test specimens which underwent different machining processes and of different surface finish were also studied. The results obtained demonstrate the feasibility of surface roughness measurement using the proposed method.

  17. Parametric synthesis of a robust controller on a base of mathematical programming method

    Science.gov (United States)

    Khozhaev, I. V.; Gayvoronskiy, S. A.; Ezangina, T. A.

    2018-05-01

    Considered paper is dedicated to deriving sufficient conditions, linking root indices of robust control quality with coefficients of interval characteristic polynomial, on the base of mathematical programming method. On the base of these conditions, a method of PI- and PID-controllers, providing aperiodic transient process with acceptable stability degree and, subsequently, acceptable setting time, synthesis was developed. The method was applied to a problem of synthesizing a controller for a depth control system of an unmanned underwater vehicle.

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

    International Nuclear Information System (INIS)

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

    2012-01-01

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

  19. Hydrothermal synthesis and sol-gel methods for CdS particle production in different morphologies and their use in wastewater applications

    OpenAIRE

    Tuncer, Cansel

    2018-01-01

    In this study, CdSnanoparticles were synthesized in different sizes and morphologies using twodifferent methods. First, the synthesis of both cauliflower-type CdS microspheresand CdS nanoflower-type microstructures by hydrothermal synthesis was carriedout in a steel reactors with teflon chamber. While polyethylene glycol andthioacetamide were used in the synthesis of cauliflower-type CdS microspheres,thiourea was used as a sulfur source in the synthesis of nanoflower CdS microstructures.Spher...

  20. Synthesis of anhydrous K2TiOF4 via a mild hydrothermal method

    Science.gov (United States)

    Felder, Justin B.; Yeon, Jeongho; zur Loye, Hans-Conrad

    2015-10-01

    The synthesis of anhydrous K2TiOF4 has been previously attempted by transforming precursor compounds, such as the peroxide (K2Ti(O2)F4), hydrate (K2TiOF4·H2O) and fluoride (K2TiF6). Due to the large structural differences between these precursors and the anhydrous oxyfluorides, however, these preparations have been unsuccessful. Therefore, a direct method of synthesis has been employed to grow single crystals of K2TiOF4 that were characterized by single crystal x-ray diffraction. K2TiOF4 was found to be isostructural with the previously known K2VOF4.

  1. In-situ Fabrication of a Freestanding Acrylate-based Hierarchical Electrolyte for Lithium-sulfur Batteries

    International Nuclear Information System (INIS)

    Liu, M.; Jiang, H.R.; Ren, Y.X.; Zhou, D.; Kang, F.Y.; Zhao, T.S.

    2016-01-01

    Graphical abstract: We present a freestanding acrylate-based hierarchical electrolyte. This quasi-solid electrolyte is assembled by in-situ gelation of a pentaerythritol tetraacrylate (PETEA)-based gel polymer electrolyte (GPE) into a polymethyl methacrylate (PMMA)-based electrospun network. The prepared polymer battery renders a suppressed shuttle effect and much enhanced cycle life. - Highlights: • A freestanding Acrylate-based Hierarchical Electrolyte was in-situ crafted. • The high conductivity is due to strong uptake ability and elimination of separator. • The polymer battery renders a superior high rate capability and excellent retention. • First-principle calculations prove anchoring ability of ester functional groups. • Cell modeling shows geometric design effectively suppresses polysulfide flux. - Abstract: A number of methods have been attempted to suppress the shuttle effect in lithium-sulfur (Li-S) batteries to improve battery performance. Conventional methods, however, reduce the ionic conductivity, sacrifice the overall energy density and increase the cost of production. Here, we report a facile synthesis of an acrylate-based hierarchical electrolyte (AHE). This quasi-solid electrolyte is assembled by in-situ gelation of a pentaerythritol tetraacrylate (PETEA)-based gel polymer electrolyte (GPE) into a polymethyl methacrylate (PMMA)-based electrospun network. The structural similarity and synergetic compatibility between the electrospun network and GPE provide the AHE an ester-rich robust structure with a high ionic conductivity of 1.02 × 10 −3 S cm −1 due to the strong uptake ability and the elimination of commercial separator. The S/AHE/Li polymer battery also renders a high rate capability of 645 mAh g −1 at 3C, while maintaining excellent retention at both high and low current densities (80.3% after 500 cycles at 0.3C and 91.9% after 500 cycles at 3C). First-principle calculations reveal that the reduced shuttle effect can be

  2. Direct Synthesis of H{sub 2}O{sub 2} over Ti-Containing Molecular Sieves Supported Gold Catalysts: A Comparative Study for In-situ-H{sub 2}O{sub 2}-ODS of Fuel

    Energy Technology Data Exchange (ETDEWEB)

    Zhang, Han; Song, Haiyan; Chen, Chunxia; Han, Fuqin; Hu, Shaozheng [Northeast Forestry Univ., Harbin (China); Liu, Guangliang [Univ. of Connecticut, Storrs (United States); Chen, Ping; Zhao, Zhixi [Xinjiang Normal Univ., Urumqi (China)

    2013-10-15

    Direct synthesis of H{sub 2}O{sub 2} and in situ oxidative desulfurization of model fuel over Au/Ti-HMS and Au/TS-1 catalysts has been comparatively investigated in water or methanol. Maximum amount (82%) of active Au{sup 0} species for H{sub 2}O{sub 2} synthesis was obtained. Au/Ti-HMS and Au/TS-1 exhibited the contrary performances in H{sub 2}O{sub 2} synthesis as CH{sub 3}OH/H{sub 2}O ratio of solvent changed. H{sub 2}O{sub 2} decomposition and hydrogenation in water was inhibited by the introduction of methanol. Effect of O{sub 2}/H{sub 2} ratio on H{sub 2}O{sub 2} concentration, H{sub 2} conversion and H{sub 2}O{sub 2} selectivity revealed a relationship between H{sub 2}O{sub 2} generation and H2 consumption. The highest dibenzothiophene removal rate (83.2%) was obtained over Au/Ti-HMS in methanol at 1.5 of O{sub 2}/H{sub 2} ratio and 60 .deg. C. But removal of thiophene over Au/TS-1 should be performed in water without heating to obtain a high removal rate (61.3%). Meanwhile, H{sub 2} conversion and oxidative desulfurization selectivity of H{sub 2} were presented.

  3. Guided in Situ Polymerization of MEH-PPV in Mesoporous Titania Photoanodes.

    Science.gov (United States)

    Minar, Norma K; Docampo, Pablo; Fattakhova-Rohlfing, Dina; Bein, Thomas

    2015-05-20

    Incorporation of conjugated polymers into porous metal oxide networks is a challenging task, which is being pursued via many different approaches. We have developed the guided in situ polymerization of poly(2-methoxy-5-(2'-ethylhexyloxy)-p-phenylenevinylene) (MEH-PPV) in porous titania films by means of surface functionalization. The controlled polymerization via the Gilch route was induced by an alkoxide base and by increasing the temperature. The selected and specially designed surface-functionalizing linker molecules mimic the monomer or its activated form, respectively. In this way, we drastically enhanced the amount of MEH-PPV incorporated into the porous titania phase compared to nonfunctionalized samples by a factor of 6. Additionally, photovoltaic measurements were performed. The devices show shunting or series resistance limitations, depending on the surface functionalization prior to in situ polymerization of MEH-PPV. We suggest that the reason for this behavior can be found in the orientation of the grown polymer chains with respect to the titania surface. Therefore, the geometry of the anchoring via the linker molecules is relevant for exploiting the full electronic potential of the conjugated polymer in the resulting hybrid composite. This observation will help to design future synthesis methods for new hybrid materials from conjugated polymers and n-type semiconductors to take full advantage of favorable electronic interactions between the two phases.

  4. Microwave combustion synthesis of in situ Al{sub 2}O{sub 3} and Al{sub 3}Zr reinforced aluminum matrix composites

    Energy Technology Data Exchange (ETDEWEB)

    Zhu, Heguo, E-mail: zhg1200@sina.com [College of Materials Science and Engineering, Nanjing University of Science and Technology, Nanjing 210094 (China); Key Laboratory of Advanced Micro-Nano Materials and Technology, Jiangsu Province Higher Education Institutions, 210094 (China); Synergetic Center for Advanced Materials Research, Jiangsu Province Higher Education Institutions, 210094 (China); Hua, Bo; Cui, Tao; Huang, Jiewen; Li, Jianliang [College of Materials Science and Engineering, Nanjing University of Science and Technology, Nanjing 210094 (China); Xie, Zonghan, E-mail: zonghan.xie@adelaide.edu.au [School of Mechanical & Electrical Engineering, Wuhan Institute of Technology, Wuhan 430073 (China); School of Mechanical Engineering, University of Adelaide, SA 5005 (Australia)

    2015-08-15

    Al{sub 2}O{sub 3} and Al{sub 3}Zr reinforced aluminum matrix composites were fabricated from Al and ZrO{sub 2} powders by SiC assisted microwave combustion synthesis. The microstructure and reaction pathways were analyzed by using differential scanning calorimetry (DSC), X-ray diffraction (XRD), scanning electron microscopy (SEM), transmission electron microscopy (TEM) and energy dispersive spectroscopy (EDS). The results showed that the heating rate during microwave synthesis was very high and the entire process took several minutes and that the ignition temperature of the reaction was much lower than that of conventional methods. In addition, the resulting microstructure was found to be finer than that prepared by the conventional methods and no cracks can be seen in the Al{sub 3}Zr reinforcements. As such, the newly developed composites have potential for safety-critical applications where catastrophic failure is not tolerated.

  5. Guidance for deciding upon use of primary mixed methods studies in research synthesis : Lessons learned in childhood trauma

    NARCIS (Netherlands)

    Boeije, H.; van Wesel, F.; Slagt, M.

    2014-01-01

    When reviewing literature, mixed methods studies (MMS) are increasingly retrieved, yet it is unclear how they should be dealt with in a research synthesis. In this article we examine the inclusion of primary MMS in research synthesis, based on experiences with a meta-analysis (MA) and a qualitative

  6. Guidance for deciding upon use of primary mixed methods studies in research synthesis: lessons learned in childhood trauma

    NARCIS (Netherlands)

    Boeije, H.R.; van Wesel, F.; Slagt, M.I.

    2014-01-01

    When reviewing literature, mixed methods studies (MMS) are increasingly retrieved, yet it is unclear how they should be dealt with in a research synthesis. In this article we examine the inclusion of primary MMS in research synthesis, based on experiences with a meta-analysis (MA) and a qualitative

  7. Guidance for deciding upon use of primary mixed methods studies in research synthesis: lessons learned in childhood trauma.

    NARCIS (Netherlands)

    Boeije, H.; Wesel, F. van; Slagt, M.

    2014-01-01

    When reviewing literature, mixed methods studies (MMS) are increasingly retrieved, yet it is unclear how they should be dealt with in a research synthesis. In this article we examine the inclusion of primary MMS in research synthesis, based on experiences with a meta-analysis (MA) and a qualitative

  8. Space synthesis: an application of synthesis method to two and three dimensional multigroup neutron diffusion equations; Synthese spatiale: une application de la methode de synthese aux equations de diffusion neutronique multigroupe a deux et trois dimensions

    Energy Technology Data Exchange (ETDEWEB)

    Nguyen-Ngoc, H [Commissariat a l' Energie Atomique, Saclay (France). Centre d' Etudes Nucleaires

    1969-07-01

    In order to reduce computing time, two and three-dimensional multigroup neutron diffusion equations in cylindrical, rectangular (X, Y), (X, Y, Z) and hexagonal geometries are solved by the method of synthesis using an appropriate variational principle (stationary principle). The basic idea is to reduce the number of independent variables by constructing two or three-dimensional solutions from solutions of fewer variables, hence the name 'synthesis method'. Whatever the geometry, we are led to solve a system of ordinary differential equations with matrix coefficients to which one can apply well-known numerical methods: CHEBYSHEV's polynomial method, Gaussian elimination. Numerical results furnished by synthesis programs written for the IBM 7094, the IBM 360-75 and the CDC 6600 computers, are confronted with those which are given by programs employing the classical finite difference method. [French] En vue de reduire le-temps de calcul, les equations de diffusion neutronique, multigroupe, a deux et trois dimensions d'espace dans les geometries cylindrique, rectangulaire (X, Y), (X, Y, Z) et hexagonale sont resolues par la methode de synthese utilisant un principe variationnel approprie (principe stationnaire). L'idee consiste a reduire le nombre de variables independantes par construction d'une solution bi ou tridimensionnelle au moyen de solutions dependant d'un nombre inferieur de variables, d'ou le nom de la methode. Dans tous les cas de geometrie, nous sommes conduits a resoudre un systeme d'equations differentielles a coefficients matriciels auquel peuvent s'appliquer les methodes numeriques courantes; methode polynomiale de TCHEBYCHEFF et methode d'elimination de GAUSS. Les resultats numeriques obtenus par nos codes de synthese programmes sur IBM 7094, IBM 360-75 et CDC 6600, sont confrontes avec ceux que fournissent les programmes adoptant la methode classique des differences finies. (auteur)

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

    International Nuclear Information System (INIS)

    Dowlati, Bahram; Othman, Mohamed Rozali

    2013-01-01

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

  10. Evaluation and analysis of geological condition of in-situ fragmentation leaching uranium

    International Nuclear Information System (INIS)

    Yang Jianming; Tan Kaixuan; Huang Xiaonai

    2003-01-01

    The ore geological condition, hydrogeological condition, engineering geological condition and technological mineralogical character of in-situ fragmentation leaching uranium are analyzed, and it is considered that the implementation of in-situ fragmentation leaching uranium technology is decided by different geological factor. Previously prospecting and geological condition evaluation of uranium ore is based on traditional mining method. If in-situ fragmentation leaching uranium method is adopted, one must re-evaluate previously prospected deposits before they are mined, or one must evaluate new prospecting deposits according to geological conditions of in-situ fragmentation leaching uranium method. The feasibility evaluation method of uranium deposit by in-situ fragmentation leaching uranium put forward by B. N. Mociniets is introducd, and it is considered that B. N. Mociniets method has guidable significance for geological condition evaluation before uranium deposits are mined. A feasibility study is done by applying B. N. Mociniets method to a uranium deposit. (authors)

  11. Three methods for in situ cross-linking of polyvinyl alcohol films for application as ion-conducting membranes in potassium hydroxide electrolyte. [battery separators

    Science.gov (United States)

    Philipp, W. H.; Hsu, L. C.

    1979-01-01

    Three methods of in situ cross-linking polyvinyl alcohol films are presented. They are: (1) acetalization with a dialdehyde such as glutaraldehyde, (2) acetalization with aldehyde groups formed by selective oxidative cleaving of the few percent of 1,2 diol units present in polyvinyl alcohol, and (3) cross-linking by hydrogen abstraction by reaction with hydrogen atoms and hydroxyl radicals from irradiated water. For the third method, improvement in film conductivity in KOH solution at the expense of mechanical strength is obtained by the presence of polyacrylic acid in the polyvinyl alcohol films. Resistivities in 45 percent KOH are given for in situ cross-linked films prepared by each of the three methods.

  12. In-situ anatase phase stabilization of titania photocatalyst by sintering in presence of Zr4+ organic salts

    Science.gov (United States)

    Strini, Alberto; Sanson, Alessandra; Mercadelli, Elisa; Bendoni, Riccardo; Marelli, Marcello; Dal Santo, Vladimiro; Schiavi, Luca

    2015-08-01

    The direct in-situ stabilization of an anatase-based nanocrystalline photocatalyst (Degussa P25) was obtained by sintering the catalyst powder in presence of Zr4+ organic salts. This approach allows the doping of an already-formed nanocrystalline photocatalyst instead of introducing the dopant in the crystal lattice during the catalyst synthesis. The procedure was demonstrated by the production of thick ceramic layers using the screen printing technique. This new method allows to easily stabilize the anatase phase 200 °C higher than the undoped P25 maintaining the same photocatalytic activity. The process was studied using specifically formulated screen-printing inks added with Zr4+ organic salt at 1% and 2% Zr/Ti molar ratio. The anatase phase stability was investigated in the 500-900 °C temperature range analysing the resulting catalysts with XRD, TEM and (S)TEM-EDS. The catalytic activity of the screen-printed layers was assessed by measuring the degradation of toluene in air at ambient concentration (500 nmol m-3) and low UV-A irradiance (180 μW cm-2). The described in-situ stabilization method could be potentially applied to any deposition process involving already formed anatase photocatalyst, allowing higher sintering temperature and then an improved mechanical stability of the active layers without photocatalytic activity degradation.

  13. Synthesis of Mechanisms

    DEFF Research Database (Denmark)

    Hansen, John Michael

    1999-01-01

    These notes describe an automated procedure for analysis and synthesis of mechanisms. The analysis method is based on the body coordinate formulation, and the synthesis is based on applying optimization methods, used to minimize the difference between an actual and a desired behaviour...

  14. Green synthesis of silver nanoparticles using Stevia leaves extracts

    Science.gov (United States)

    Laguta, Iryna; Stavinskaya, Oksana; Kazakova, Olga; Fesenko, Tetiana; Brychka, Sergey

    2018-02-01

    Three extracts of Stevia rebaudiana (Bertoni) were prepared using different types of raw materials: leaves of plants grown ex situ, leaves of plants grown in vitro, callus culture formed on damaged leaves. Composition of the extracts was studied by means of high-performance liquid chromatography and laser desorption/ionization mass spectrometry; total phenol content was estimated using Folin-Ciocalteau method. Flavonoids and hydroxycinnamic acids were found to be the main groups of phenol antioxidants available in the Stevia leaves, with the amount of these compounds in the extract being dependent on the type of raw material. The reducing properties of phenol compounds identified in the extracts were characterized using quantum chemical method; flavonoids and hydroxycinnamic acids were found to have similar redox parameters. Silver nanoparticles (AgNPs) colloids were synthesized using three Stevia extracts; AgNPs size distribution were characterized by means of scanning electron microscopy. All the extracts revealed significant activity in AgNPs synthesis; the nanoparticles of predominantly spherical shape with the average sizes of 16-25 nm were formed. The reducing properties of the extracts were found to correlate with total phenol content; the activity of extracts from the leaves of plants grown ex situ and from callus culture in Ag+ ions reduction was similar to each other and exceeded the activity of extract from the leaves of plants grown in vitro.

  15. The influence of the roll diameter in flat rolling of of superconducting in situ and ex situ MgB2 tape

    DEFF Research Database (Denmark)

    Hancock, Michael Halloway; Bay, Niels

    2007-01-01

    , 150 and 210 mm in each step. The investigation has shown that the in situ powder is more readily compacted than the ex situ powder, with an average increase of relative density after mechanical processing of 37% for in situ powder and 19% for ex situ powder. Statistical analysis showed that the choice......Applying the powder in tube (PIT) method, single-filament MgB2/Fe wire and tape has been manufactured applying both the ex situ and the in situ approach. The influence of the roll diameter in three-step flat rolling on the powder density and critical temperature has been examined using rolls of 70...... roll in the first and second reductions followed by the 150 mm or 210 mm roll in the last reduction was the optimum strategy for both powder types. AC susceptibility testing showed that for the in situ tapes there was no correlation between the powder density and the critical temperature. For ex situ...

  16. Fe3O4 nanocubes assembled on RGO nanosheets: Ultrasound induced in-situ and eco-friendly synthesis, characterization and their excellent catalytic performance for the production of liquid fuel in Fischer-tropsch synthesis.

    Science.gov (United States)

    Abbas, Mohamed; Zhang, Juan; Lin, Ke; Chen, Jiangang

    2018-04-01

    In this study, Fe 3 O 4 nanocubes (NCs) decorated on RGO nanosheets (NSs) structures were successfully synthesized through an innovative and environmentally-friendly rapid sonochemical method. More importantly, iron(II) sulfate heptahydrate and GO were employed as precursors and water as reaction medium, meanwhile, NaOH within the generated free radicals from the high intensity ultrasound were sufficient as reducing and base agent in our clean synthesis. Moreover, the hydrothermal method as a conventional approach was employed to synthesize the same catalysts for the comparison with the ultrasonocation technique. The as-synthesized Fe 3 O 4 and RGO/Fe 3 O 4 NSs catalysts were exposed to industrially relevant Fischer-tropsch synthesis (FTS) conditions at various reaction temperatures (250-290 °C), and they subjected to fully characterization before and after FTS reaction using XRD, TEM, HRTEM, EDS mapping, XPS, FTIR, BET, H 2 -TPR, H 2 -TPD and CO-TPD to understand the structure-performance relationships. Notably, the catalysts produced using the sonochemical method had a better CO conversion rate [Fe 3 O 4 (80%), RGO/Fe 3 O 4 (82%)] than the hydrothermally synthesized catalysts. However, compared to the naked-Fe 3 O 4 catalysts, the sonochemically and hydrothermally synthesized RGO-supported Fe 3 O 4 catalysts had higher long chain hydrocarbon (C5+) selectivity values (72% and 67%) and C 2 -C 4 olefin/paraffin selectivity ratio (3.2 and 2) and low CH4 selectivity values (6% and 8.5%), respectively. This can be attributed to their high surface area, the degree of reducibility, and content of Hägg iron carbide (χ-Fe 5 C 2 ) as the most active phase of the FTS reaction. Proposed reaction mechanisms for the sonochemical and hydrothermal reaction synthesis of Fe 3 O 4 and RGO/Fe 3 O 4 nanoparticles are discussed. In conclusion, our developed surfactantless-sonochemical method holds promise for the eco-friendly synthesis of highly efficient catalysts materials for

  17. One-step synthesis of graphene/polyaniline hybrids by in situ intercalation polymerization and their electromagnetic properties

    Science.gov (United States)

    Chen, Xiangnan; Meng, Fanchen; Zhou, Zuowan; Tian, Xin; Shan, Liming; Zhu, Shibu; Xu, Xiaoling; Jiang, Man; Wang, Li; Hui, David; Wang, Yong; Lu, Jun; Gou, Jihua

    2014-06-01

    A new method is introduced for the preparation of graphene/polyaniline hybrids using a one-step intercalation polymerization of aniline inside the expanded graphite. The structural and morphological characterizations were performed by X-ray diffraction analysis, transmission electron microscopy and field emission scanning electron microscopy. Both the experimental and first-principles simulated results show that the aniline cation formed by aniline and H+ tends to be drawn towards the electron-enriched zone and to intercalate into the interlayer of graphite. Subsequently, an in situ polymerization leads to the separation of graphite into graphene sheet, resulting from the exothermic effect and more vigorous movements of the chain molecules of polyaniline. The interactions between polyaniline and graphene were confirmed by Fourier transform infrared spectroscopy and Raman spectra. In addition, the graphene/polyaniline hybrid exhibited a breakthrough in the improvement of microwave absorption.A new method is introduced for the preparation of graphene/polyaniline hybrids using a one-step intercalation polymerization of aniline inside the expanded graphite. The structural and morphological characterizations were performed by X-ray diffraction analysis, transmission electron microscopy and field emission scanning electron microscopy. Both the experimental and first-principles simulated results show that the aniline cation formed by aniline and H+ tends to be drawn towards the electron-enriched zone and to intercalate into the interlayer of graphite. Subsequently, an in situ polymerization leads to the separation of graphite into graphene sheet, resulting from the exothermic effect and more vigorous movements of the chain molecules of polyaniline. The interactions between polyaniline and graphene were confirmed by Fourier transform infrared spectroscopy and Raman spectra. In addition, the graphene/polyaniline hybrid exhibited a breakthrough in the improvement of

  18. In-situ calibration of nuclear-plant platinum resistance thermometers using Johnson noise methods. Final report

    International Nuclear Information System (INIS)

    Blalock, T.V.; Shepard, R.L.

    1983-06-01

    Methods for in situ calibration of reactor plant platinum resistance thermometers using Johnson noise measurements were tested in the laboratory and in two operating reactors: Diablo Canyon and Sequoyah. The Johnson noise methods provide an absolute measurement of the thermometer temperature and can be compared with the dc calibration of the thermometers to confirm their calibration without removing the thermometers from the plant coolant loops. Inaccuracies of less than 0.1% were obtained with these methods for ideal situations where the noise measuring equipment could be connected directly to the installed thermometer terminals. For measurements made at the ends of long extension cables, inaccuracies were 0.5 to 1.0%, at best. Extension cables must be optimized and well characterized electrically to achieve such accuracies. Other factors that affect the accuracy of these methods were evaluated

  19. Possibilities of surface-sensitive X-ray methods for studying the molecular mechanisms of interaction of nanoparticles with model membranes

    Energy Technology Data Exchange (ETDEWEB)

    Novikova, N. N., E-mail: nn-novikova07@yandex.ru; Kovalchuk, M. V.; Yakunin, S. N. [National Research Centre “Kurchatov Institute,” (Russian Federation); Konovalov, O. V. [European Synchrotron Radiation Facility (France); Stepina, N. D. [Russian Academy of Sciences, Shubnikov Institute of Crystallography, Federal Scientific Research Centre “Crystallography and Photonics,” (Russian Federation); Rogachev, A. V. [National Research Centre “Kurchatov Institute,” (Russian Federation); Yurieva, E. A. [Moscow Research Institute of Pediatrics and Pediatric Surgery (Russian Federation); Marchenko, I. V.; Bukreeva, T. V. [National Research Centre “Kurchatov Institute,” (Russian Federation); Ivanova, O. S.; Baranchikov, A. E.; Ivanov, V. K. [Russian Academy of Sciences, Kurnakov Institute of General and Inorganic Chemistry (Russian Federation)

    2016-09-15

    The processes of structural rearrangement in a model membrane, i.e., an arachic acid monolayer formed on a colloidal solution of cerium dioxide or magnetite, are studied in situ in real time by the methods of X-ray standing waves and 2D diffraction. It is shown that the character of the interaction of nanoparticles with the monolayer is determined by their nature and sizes and depends on the conditions of nanoparticle synthesis. In particular, the structure formation in the monolayer–particle system is greatly affected by the stabilizer (citric acid), which is introduced into the colloidal solution during synthesis.

  20. In situ Sn2+-incorporation synthesis of titanate nanotubes for photocatalytic dye degradation under visible light illumination

    International Nuclear Information System (INIS)

    Tsai, Chien-Cheng; Chen, Liang-Che; Yeh, Te-Fu; Teng, Hsisheng

    2013-01-01

    Highlights: ► Sn 2+ ions sensitize titanate nanotubes for photocatalysis under visible-light illumination. ► The Sn 5s orbital replaces the O 2p orbital as the top level of the valence band of titanates. ► The presence of Sn 2+ lifts the valence band of titanate nanotubes by approximately 0.9 eV. ► The doped Sn 2+ sites are active in donating photo-induced charges to dye degradation. - Abstract: Sn 2+ -incorporated titanate nanotubes, prepared by washing a layered sodium titanate with a SnCl 2 solution for tube formation, exhibit noticeable photocatalytic activity under visible light irradiation. This in situ synthesis results in a Sn/Ti ratio of approximately 0.6. Because of the introduction of Sn 2+ ions, the Sn 5s orbital replaces the O 2p orbital as the top level of the valence band of titanate nanotubes. Optical absorption analysis shows that Sn doping reduces the bandgap of titanate nanotubes from 3.5 to 2.6 eV. Oxidation of the Sn 2+ -incorporated titanate nanotubes leads to oxidation of Sn 2+ to Sn 4+ , hence, widening the bandgap. Under visible light irradiation, Sn 2+ -incorporated titanate nanotubes effectively degrade methylene blue in an aqueous solution, whereas the bare titanate nanotubes exhibit substantially lower photocatalytic activity. Photoluminescence analysis demonstrates that the induced charges from excitation of the Sn 2+ ions tend to be relaxed through chemical interactions, rather than irradiative recombination.

  1. Identification of MYCN gene amplification in neuroblastoma using chromogenic in situ hybridization (CISH): an alternative and practical method.

    Science.gov (United States)

    Bhargava, Rohit; Oppenheimer, Orit; Gerald, William; Jhanwar, Suresh C; Chen, Beiyun

    2005-06-01

    Chromogenic in situ hybridization (CISH) is a recently developed technique, which utilizes the general principles of in situ hybridization and a detection system similar to immunohistochemistry. To assess the utility of CISH for analysis of MYCN gene amplification, we compared this assay with established diagnostic assays such as Southern blot analysis (SB) and fluorescent in situ hybridization (FISH). CISH was performed on 67 cases of neuroblastoma using tissue microarray (65 cases) and whole tissue sections (2 cases). Unequivocal, high-level amplification (> or =10 gene copies per tumor nucleus) was identified in 19 of 67 (28.4%) tumors. Two (3%) tumors showed low-level amplification (6-9 gene copies per tumor nucleus). No amplification was seen in 46 of 67 (68.6%) tumors. SB data were available in 44 tumors. Forty-one of the 44 tumors (93%) showed concordant results between CISH and SB. Three tumors showed MYCN amplification by CISH but no amplification by SB, most likely due to dilution effect of nonneoplastic tissue in the test samples. Two of these three tumors also showed MYCN amplification by FISH, and the third tumor was not analyzed by FISH. FISH data were available in total of 30 tumors. All 30 tumors showed concordant results between CISH and FISH for classifying a tumor as MYCN amplified or not amplified. We conclude that CISH is an accurate method for determining MYCN gene amplification, with added advantages that make it a more practically useful method.

  2. Study on the fabrication of Al matrix composites strengthened by combined in-situ alumina particle and in-situ alloying elements

    International Nuclear Information System (INIS)

    Huang Zanjun; Yang Bin; Cui Hua; Zhang Jishan

    2003-01-01

    A new idea to fabricate aluminum matrix composites strengthened by combined in-situ particle strengthening and in-situ alloying has been proposed. Following the concept of in-situ alloying and in-situ particle strengthening, aluminum matrix composites reinforced by Cu and α-Al 2 O 3 particulate (material I) and the same matrix reinforced by Cu, Si alloying elements and α-Al 2 O 3 particulate (material II) have been obtained. SEM observation, EDS and XRD analysis show that the alloy elements Cu and Si exist in the two materials, respectively. In-situ Al 2 O 3 particulates are generally spherical and their mean size is less than 0.5 μm. TEM observation shows that the in-situ α-Al 2 O 3 particulates have a good cohesion with the matrix. The reaction mechanism of the Al 2 O 3 particulate obtained by this method was studied. Thermodynamic considerations are given to the in-situ reactions and the distribution characteristic of in-situ the α-Al 2 O 3 particulate in the process of solidification is also discussed

  3. Direct in situ activation of Ag0 nanoparticles in synthesis of Ag/TiO2 and its photoactivity

    International Nuclear Information System (INIS)

    Jaafar, N.F.; Jalil, A.A.; Triwahyono, S.; Efendi, J.; Mukti, R.R.; Jusoh, R.; Jusoh, N.W.C.; Karim, A.H.; Salleh, N.F.M.; Suendo, V.

    2015-01-01

    Graphical abstract: - Highlights: • Ag 0 loaded on TiO 2 was prepared by a direct in situ electrochemical method. • 5 wt% Ag–TiO 2 demonstrated the best photocatalytic degradation of 2-CP. • Isomorphous substitution of Ag with Ti occurred to form Ti−O−Ag bonds. • Ag 0 and oxygen vacancies trapped electrons to enhance e–H + separation. • Substitution of Ag in the TiO 2 structure decreased the number of oxygen vacancies. - Abstract: Metallic Ag nanoparticles (Ag 0 ) were successfully activated using a direct in situ electrochemical method before being supported on TiO 2 . Catalytic testing showed that 5 wt% Ag–TiO 2 gave the highest photodegradation (94%) of 50 mg L −1 2-chlorophenol (2-CP) at pH 5 using 0.375 g L −1 catalyst within 6 h, while under similar conditions, 1 wt% and 10 wt% Ag–TiO 2 only gave 75% and 78% degradation, respectively. Characterization results illustrated that the photoactivity was affected by the amount of Ag 0 and oxygen vacancies which act as an electrons trap to enhance the electron–hole separation. While, the Ag−O−Ti bonds formation reduced the photoactivity. The degradation followed a pseudo-first order Langmuir–Hinshelwood model where adsorption was the controlling step. Study on the effect of scavengers showed that the hole (H + ) and hydroxyl radical (OH·) play important roles in the photodegradation. The regenerated photocatalyst was still stable after five cycling runs

  4. Synthesis and assessment methods for an edge-alignment-free hybrid image

    Science.gov (United States)

    Sripian, Peeraya; Yamaguchi, Yasushi

    2017-07-01

    A hybrid image allows multiple image interpretations to be modulated by the viewing distance. It can be constructed on the basis of the multiscale perceptual mechanisms of the human visual system by combining the low and high spatial frequencies of two different images. The hybrid image was introduced as an experimental tool for visual recognition study in terms of spatial frequency perception. To produce a compelling hybrid image, the original hybrid image synthesis method could only use similar shapes of source images that were aligned in the edges. If any two different images can be hybrid, it would be beneficial as a new experimental tool. In addition, there is no measure for the actual perception of spatial frequency, whether a single spatial frequency or both spatial frequencies are perceived from the hybrid stimulus. This paper describes two methods for synthesizing a hybrid image from dissimilar shape images or unaligned images; this hybrid image is known as an "edge-alignment-free hybrid image." A noise-inserted method can be done by intentionally inserting and enhancing noises into the high-frequency image. With this method, the low-frequency blobs are covered with high-frequency noises when viewed up close. A color-inserted method uses complementary color gratings in the background of the high-frequency image to emphasize the high-frequency image when viewed up close, whereas the gratings disappear when viewed from far away. To ascertain that our approach successfully separates the spatial frequency at each viewing distance, we measured this property using our proposed assessment method. Our proposed method allows the experimenter to quantify the probability of perceiving both spatial frequencies and a single spatial frequency in a hybrid image. The experimental results confirmed that our proposed synthesis methods successfully hid the low-frequency image and emphasized the high-frequency image at a close viewing distance. At the same time, the

  5. An in situ method for real-time monitoring of soil gas diffusivity

    Science.gov (United States)

    Laemmel, Thomas; Maier, Martin; Schack-Kirchner, Helmer; Lang, Friederike

    2016-04-01

    Soil aeration is an important factor for the biogeochemistry of soils. Generally, gas exchange between soil and atmosphere is assumed to be governed by molecular diffusion and by this way fluxes can be calculated using by Fick's Law. The soil gas diffusion coefficient DS represents the proportional factor between the gas flux and the gas concentration gradient in the soil and reflects the ability of the soil to "transport passively" gas through the soil. One common way to determine DS is taking core samples in the field and measuring DS in the lab. Unfortunately this method is destructive and laborious and it can only reflect a small fraction of the whole soil. As a consequence, uncertainty about the resulting effective diffusivity on the profile scale, i.e. the real aeration status remains. We developed a method to measure and monitor DS in situ. The set-up consists of a custom made gas sampling device, the continuous injection of an inert tracer gas and inverse gas transport modelling in the soil. The gas sampling device has seven sampling depths (from 0 to -43 cm of depth) and can be easily installed into vertical holes drilled by an auger, which allows for fast installation of the system. Helium (He) as inert tracer gas was injected continuously at the lower end of the device. The resulting steady state distribution of He was used to deduce the DS depth distribution of the soil. For Finite Element Modeling of the gas-sampling-device/soil system the program COMSOL was used. We tested our new method both in the lab and in a field study and compared the results with a reference lab method using soil cores. DS profiles obtained by our in-situ method were consistent with DS profiles determined based on soil core analyses. Soil gas profiles could be measured with a temporal resolution of 30 minutes. During the field study, there was an important rain event and we could monitor the decrease in soil gas diffusivity in the top soil due to water infiltration. The effect

  6. A novel In-situ Enzymatic Cleaning Method for Reducing Membrane Fouling in Membrane Bioreactors (MBRs

    Directory of Open Access Journals (Sweden)

    M. R. Bilad

    2016-05-01

    Full Text Available A novel in-situ enzymatic cleaning method was developed for fouling control in membrane bioreactors (MBRs. It is achieved by bringing the required enzymes near the membrane surface by pulling the enzymes to a magnetic membrane (MM surface by means of magnetic forces, exactly where the cleaning is required. To achieve this, the enzyme was coupled to a magnetic nanoparticle (MNP and the membrane it self was loaded with MNP. The magnetic activity was turned by means of an external permanent magnet. The effectiveness of concept was tested in a submerged membrane filtration using the model enzyme-substrate of Bacillus subitilis xylanase-arabinoxylan. The MM had almost similar properties compared to the unloaded ones, except for its well distributed MNPs. The enzyme was stable during coupling conditions and the presence of coupling could be detected using a high-performance anion-exchange chromatography (HPAEC analysis and Fourier transform infrared spectroscopy (FTIR. The system facilitated an in-situ enzymatic cleaning and could be effectively applied for control fouling in membrane bioreactors (MBRs.

  7. Usage of modal synthesis method with condensation in rotor

    Directory of Open Access Journals (Sweden)

    Zeman V.

    2008-11-01

    Full Text Available The paper deals with mathematical modelling of vibration and modal analysis of rotors composed of a flexible shaft and several flexible disks. The shaft is modelled as a one dimensional continuum whereon flexible disks modelled as a three dimensional continuum are rigid mounted to shaft. The presented approach allows to introduce continuously distributed centrifugal and gyroscopic effects. The finite element method was used for shaft and disks discretization. The modelling of such flexible multi-body rotors with large DOF number is based on the system decomposition into subsystems and on the modal synthesis method with condensation. Lower vibration mode shapes of the mutually uncoupled and non-rotating subsystems are used for creation of the rotor condensed mathematical model. An influence of the different level of a rotor condensation model on the accuracy of calculated eigenfrequencies and eigenvectors is discussed.

  8. Influence of starting precursors and synthesis methods on the physiochemical properties of zirconia

    Energy Technology Data Exchange (ETDEWEB)

    Gaydhankar, T.R., E-mail: tr.gaydhankar@ncl.res.in [Catalysis Division, National Chemical Laboratory, Pune 411008 (India); Jha, R.K. [Catalysis Division, National Chemical Laboratory, Pune 411008 (India); Nikalje, M.D. [Department of Chemistry, University of Pune, Pune 411 007 (India); Waghmare, K.J. [Catalysis Division, National Chemical Laboratory, Pune 411008 (India)

    2014-07-01

    Graphical abstract: Crystallite size of tetragonal phase of the zirconia samples prepared using different synthesis parameters and precursors as a function of calcination temperature. Surface area values of the zirconia samples calcined at 500 and 700 °C are in given brackets. - Highlights: • Zirconia prepared with modified sol–gel method is less stable compared with zirconia prepared by precipitation method. • Optimized synthesis conditions shifted the glow exotherm to higher temperature range indicating better thermal stability. • Tetragonal-zirconia could be synthesized in cost-effective manner using zirconium oxy-nitrate. • In our studies no co-relation between the surface area and crystallite size was observed. - Abstract: Under identical and judiciously pre-optimized synthesis conditions, the influence of different combinations of zirconium sources and/or post treatment conditions on structural properties, thermal stability, phase composition and morphology of zirconia has been investigated. High surface area tetragonal zirconia could be synthesized in a cost-effective manner from 1 M solution of zirconium oxy-nitrate at pH 11 using aqueous ammonia solution as a precipitant when calcined at 400 °C for 3 h. Irrespective of the preparation method, pH and starting precursor, zirconia samples prepared without digestion contained dominant monoclinic phase with some traces of tetragonal phase when calcined at 700 °C. Even though there is linear decrease in surface area with increase in the crystallite size for each sample as a function of calcination temperature, no co-relation between the surface area and crystallite size could be achieved. SEM images show agglomerated and irregular shape particles between 10 to 20 μm.

  9. Comparison among structural characteristics of Ce1-xCuxO2 nanocatalysts obtained by two methods of distinct synthesis

    International Nuclear Information System (INIS)

    Neiva, L.S.; Bispo, A.; Santos, P.T.A.; Costa, A.C.F.M.; Gama, L.; Mascarenhas, A.J.S.

    2009-01-01

    The objective this work is to synthesize nano catalysts Ce 1-x Cu x O 2 type by the synthesis methods of the combustion reaction and Pechini. The value of the concentration (x) of the element dope (Cu) varies between 0,1 and 0,5 mols. It intends evaluate that form the synthesis method influences in the physical structural characteristics of this material. nano catalysts were characterized by ray- X diffraction. The results showed nano catalysts formation with a formed structure for the most part by the phase CeO 2 , as it was expected, since this is the hostess matrix of the element dope (Cu). Nano catalysts obtained by the method Pechini presents crystallinity larger deg, according with patterns of ray-X. Thus, it was concluded that synthesis employee method the kind in the methodology, as well as the value of the concentration of the element dope has influence on the final structural characteristics of the developed material. (author)

  10. Solid-phase synthesis of polynucleotides. III. Synthesis of polynucleotides with defined sequences by the block coupling phosphotriester method.

    OpenAIRE

    Miyoshi, K; Huang, T; Itakura, K

    1980-01-01

    Preparation of the three hexadecanucleotides, dGpTpApTpCpApCpGpApGpGpCpCpCpTpT, dCpGpApCpGpApGpCpGpTpGpApCpApCpC and cTpGpCpCpGpGpCpCpApCpGpApTpGpCpG, is described by a rapid and simple solid-phase method on polyacrylamide supports. The synthesis were performed by the extension of the method described in the previous paper using di and trinucleotides of defined sequences as an incoming 3'-phosphodiester unit. Although the coupling yields to form phosphotriester bonds are slightly lower than t...

  11. Equivalence Checking between Pre-synthesis and Post-synthesis Programs by Using VIS

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Jonghoon; Yoo, Junbeom [Konkuk Univ., Seoul (Korea, Republic of); Choi, Jonggyun; Lee, Jangsoo [Korea Atomic Energy Research Institute, Daejeon (Korea, Republic of)

    2013-05-15

    PLC (Programmable Logic Controller)-based Software development, the design programs are translated into implementation programs, and behavioral equivalence between the design and implementation is demonstrated by formal method based technique. In FPGA-based software development, the design programs are also synthesized into implementation programs. However, in this process, testing and simulation based comparison techniques are mainly used. This paper proposes a formal method based technique to demonstrate behavioral equivalence between pre-synthesis and post-synthesis programs with VIS (Verification Interacting with Synthesis) verification system. We translated into BLIF-MV which is front-end of VIS, from Verlag and EDIF net list which synthesized from the same Verlag by an automatic synthesis tool. This paper proposes a formal method based technique to confirm correctness of synthesis by using equivalence checking of VIS verification system. In order to confirm the effectiveness of the proposed technique, we performed a case study with a part of prototype version of the RPS BP, and demonstrated a behavioral equivalence between Verlag HDL and EDIF post-synthesis net list.

  12. Equivalence Checking between Pre-synthesis and Post-synthesis Programs by Using VIS

    International Nuclear Information System (INIS)

    Lee, Jonghoon; Yoo, Junbeom; Choi, Jonggyun; Lee, Jangsoo

    2013-01-01

    PLC (Programmable Logic Controller)-based Software development, the design programs are translated into implementation programs, and behavioral equivalence between the design and implementation is demonstrated by formal method based technique. In FPGA-based software development, the design programs are also synthesized into implementation programs. However, in this process, testing and simulation based comparison techniques are mainly used. This paper proposes a formal method based technique to demonstrate behavioral equivalence between pre-synthesis and post-synthesis programs with VIS (Verification Interacting with Synthesis) verification system. We translated into BLIF-MV which is front-end of VIS, from Verlag and EDIF net list which synthesized from the same Verlag by an automatic synthesis tool. This paper proposes a formal method based technique to confirm correctness of synthesis by using equivalence checking of VIS verification system. In order to confirm the effectiveness of the proposed technique, we performed a case study with a part of prototype version of the RPS BP, and demonstrated a behavioral equivalence between Verlag HDL and EDIF post-synthesis net list

  13. Layer-by-Layer Method for the Synthesis and Growth of Surface Mounted Metal-Organic Frameworks (SURMOFs

    Directory of Open Access Journals (Sweden)

    Osama Shekhah

    2010-02-01

    Full Text Available A layer-by-layer method has been developed for the synthesis of metal-organic frameworks (MOFs and their deposition on functionalized organic surfaces. The approach is based on the sequential immersion of functionalized organic surfaces into solutions of the building blocks of the MOF, i.e., the organic ligand and the inorganic unit. The synthesis and growth of different types of MOFs on substrates with different functionalization, like COOH, OH and pyridine terminated surfaces, were studied and characterized with different surface characterization techniques. A controlled and highly oriented growth of very homogenous films was obtained using this method. The layer-by-layer method offered also the possibility to study the kinetics of film formation in more detail using surface plasmon resonance and quartz crystal microbalance. In addition, this method demonstrates the potential to synthesize new classes of MOFs not accessible by conventional methods. Finally, the controlled growth of MOF thin films is important for many applications like chemical sensors, membranes and related electrodes.

  14. Synthesis of CuO-NiO core-shell nanoparticles by homogeneous precipitation method

    International Nuclear Information System (INIS)

    Bayal, Nisha; Jeevanandam, P.

    2012-01-01

    Highlights: ► CuO-NiO core-shell nanoparticles have been synthesized using a simple homogeneous precipitation method for the first time. ► Mechanism of the formation of core-shell nanoparticles has been investigated. ► The synthesis route may be extended for the synthesis of other mixed metal oxide core-shell nanoparticles. - Abstract: Core-shell CuO–NiO mixed metal oxide nanoparticles in which CuO is the core and NiO is the shell have been successfully synthesized using homogeneous precipitation method. This is a simple synthetic method which produces first a layered double hydroxide precursor with core-shell morphology which on calcination at 350 °C yields the mixed metal oxide nanoparticles with the retention of core-shell morphology. The CuO–NiO mixed metal oxide precursor and the core-shell nanoparticles were characterized by powder X-ray diffraction, FT-IR spectroscopy, thermal gravimetric analysis, elemental analysis, scanning electron microscopy, transmission electron microscopy, and diffuse reflectance spectroscopy. The chemical reactivity of the core-shell nanoparticles was tested using catalytic reduction of 4-nitrophenol with NaBH 4 . The possible growth mechanism of the particles with core-shell morphology has also been investigated.

  15. DNA and RNA Synthesis in Animal Cells in Culture--Methods for Use in Schools

    Science.gov (United States)

    Godsell, P. M.; Balls, M.

    1973-01-01

    Describes the experimental procedures used for detecting DNA and RNA synthesis in xenopus cells by autoradiography. The method described is suitable for senior high school laboratory classes or biology projects, if supervised by a teacher qualified to handle radioisotopes. (JR)

  16. Autoradiographic study of transcription during early germination of Zea mays embryos maintained in situ

    International Nuclear Information System (INIS)

    Deltour, Roger

    1979-01-01

    Recovery of RNA synthesis was studied by autoradiography in primary root of Zea mays embryos germinating at 16 0 C. [H 3 ] uridine was provided to embryos maintained in situ. During the first 4hrs of germination the cell radioactivity is located almost exclusively in the extranucleolar chromatin. These observations agree well with previous results obtained when [H 3 ] uridine was provided to isolated embryos [fr

  17. In-Situ Burning of Crude Oil on Water

    DEFF Research Database (Denmark)

    van Gelderen, Laurens

    in the small scale water basin. Boilovers were also observed during the burning of a heavy crude oil with a substantial light fraction without a water layer, however, which suggests that water is not essential for boilover occurrence. Further studies are required to determine the conditions under which......The fire dynamics and fire chemistry of in-situ burning of crude oil on water was studied in order to improve predictions on the suitability of this oil spill response method. For this purpose, several operational parameters were studied to determine the factors that control the burning efficiency...... of in-situ burning, i.e. the amount of oil (in wt%) removed from the water surface by the burning process. The burning efficiency is the main parameter for expressing the oil removal effectiveness of in-situ burning as response method and is thus relevant for suitability predictions of in-situ burning...

  18. Application of the nuclear x-ray fluorescence method to prospecting for gold in-situ

    International Nuclear Information System (INIS)

    Zhang, Y.; Xie, T.; Zhou, S.; Ge, L.

    1989-01-01

    Arsenic and chalcophile elements are often associated with gold, and can be considered indicator elements when prospecting for gold deposits. The nuclear geophysics X-ray fluorescence method can be used to search for hidden gold deposits by measuring fluorescence intensities of the indicator elements in situ. The method can speed geologic investigation and reduce exploration cost. Three types of portable radioisotope X-ray fluorescence analyzers, designed and manufactured by Chengdu College of Geology and Chongqing Geological Instrument Factory, are briefly introduced. These analyzers are widely used in different stages of geologic investigation for gold in China. In the two case histories presented five anomalous zones of X-ray fluorescence intensity related to gold mineralization are located and one hidden gold deposit is discovered with gold content of 23 g/t

  19. Synthesis and Characterization of Encapsulated Nanosilica Particles with an Acrylic Copolymer by in Situ Emulsion Polymerization Using Thermoresponsive Nonionic Surfactant

    Directory of Open Access Journals (Sweden)

    Daryoosh Vashaee

    2013-08-01

    Full Text Available Nanocomposites of encapsulated silica nanoparticles were prepared by in situ emulsion polymerization of acrylate monomers. The synthesized material showed good uniformity and dispersion of the inorganic components in the base polymer, which enhances the properties of the nanocomposite material. A nonionic surfactant with lower critical solution temperature (LCST was used to encapsulate the silica nanoparticles in the acrylic copolymer matrix. This in situ method combined the surface modification and the encapsulation in a single pot, which greatly simplified the process compared with other conventional methods requiring separate processing steps. The morphology of the encapsulated nanosilica particles was investigated by dynamic light scattering (DLS and transmission electron microscopy (TEM, which confirmed the uniform distribution of the nanoparticles without any agglomerations. A neat copolymer was also prepared as a control sample. Both the neat copolymer and the prepared nanocomposite were characterized by Fourier transform infrared spectroscopy (FTIR, thermal gravimetric analyses (TGA, dynamic mechanical thermal analysis (DMTA and the flame resistance test. Due to the uniform dispersion of the non-agglomerated nanoparticles in the matrix of the polymer, TGA and flame resistance test results showed remarkably improved thermal stability. Furthermore, DMTA results demonstrated an enhanced storage modulus of the nanocomposite samples compared with that of the neat copolymer, indicating its superior mechanical properties.

  20. A Comparative Characterization of the HPA-MCM-48 Type Catalysts Produced by the Direct Hydrothermal and Room Temperature Synthesis Methods

    International Nuclear Information System (INIS)

    Gucbilmez, Y.; Calis, I.; Yargic, A. S.

    2012-01-01

    MCM-48 type support materials synthesized by the direct hydrothermal synthesis (HTS) and room temperature synthesis (RTS) methods were incorporated with tungstophosphoric acid (TPA) in the range of 10-40 wt% by using a wet impregnation technique in methanol solutions. Resulting HPA-MCM-48 catalysts were characterized by the XRD, Nitrogen Physisorption, SEM, TEM, EDS, and FT-IR methods in order to determine the effects of different initial synthesis conditions on the catalyst properties. RTS samples were found to have better crystalline structures, higher BET surface areas, and higher BJH pore volumes than HTS samples. They also had slightly higher TPA incorporation, except for the 40 wt% samples, as evidenced by the EDS results. Keggin ion structure was preserved, for both methods, even at the highest acid loading of 40 wt%. It was concluded that the simpler and more economical RTS method was more successful than the HTS method for hetero poly acid incorporation into MCM-48 type materials