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Sample records for temperature hpht synthesis

  1. 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.

  2. Synthesis of diamonds in Fe–C systems using nitrogen and hydrogen co-doped impurities under HPHT

    International Nuclear Information System (INIS)

    Sun Shi-Shuai; Xu Zhi-Hui; Cui Wen; Jia Xiao-Peng; Ma Hong-An

    2017-01-01

    In this study, we investigate the effect of nitrogen and hydrogen impurities on colors, morphologies, impurity structures and synthesis conditions of diamond crystals in Fe–C systems with C 3 N 6 H 6 additives at pressures in the range 5.0–6.5 GPa and temperatures of 1400–1700 °C in detail. Our results reveal that the octahedron diamond nucleation in a Fe–C system is evidently inhibited by co-doped N–H elements, thereby resulting in the increase of minimum pressure and temperature of diamond synthesis by spontaneous nucleation. The octahedron diamond crystals synthesized from a pure Fe–C system are colorless, while they become green in the system with C 3 N 6 H 6 additive. The surface defects of diamond will deteriorate when the nitrogen and hydrogen atoms simultaneously incorporate in the diamond growth environment in the Fe–C system. We believe that this study will provide some important information and be beneficial for the deep understanding of the crystallization of diamonds from different component systems. (paper)

  3. Plasma synthesis and HPHT consolidation of BN nanoparticles, nanospheres, and nanotubes to produce nanocrystalline cubic boron nitride

    Science.gov (United States)

    Stout, Christopher

    Plasma methods offer a variety of advantages to nanomaterials synthesis. The process is robust, allowing varying particle sizes and phases to be generated simply by modifying key parameters. The work here demonstrates a novel approach to nanopowder synthesis using inductively-coupled plasma to decompose precursor, which are then quenched to produce a variety of boron nitride (BN)-phase nanoparticles, including cubic phase, along with short-range-order nanospheres (e.g., nano-onions) and BN nanotubes. Cubic BN (c-BN) powders can be generated through direct deposition onto a chilled substrate. The extremely-high pyrolysis temperatures afforded by the equilibrium plasma offer a unique particle growth environment, accommodating long deposition times while exposing resulting powders to temperatures in excess of 5000K without any additional particle nucleation and growth. Such conditions can yield short-range ordered amorphous BN structures in the form of 20nm diameter nanospheres. Finally, when introducing a rapid-quenching counter-flow gas against the plasma jet, high aspect ratio nanotubes are synthesized, which are collected on substrate situated radially. The benefits of these morphologies are also evident in high-pressure/high-temperature consolidation experiments, where nanoparticle phases can offer a favorable conversion route to super-hard c-BN while maintaining nanocrystallinity. Experiments using these morphologies are shown to begin to yield c-BN conversion at conditions as low as 2.0 GPa and 1500°C when using micron sized c-BN seeding to create localized regions of high pressures due to Hertzian forces acting on the nanoparticles.

  4. PhaseWatcher Vx subsea for HPHT - a new deepwater multiphase and wet gas flowmeter for HPHT

    Energy Technology Data Exchange (ETDEWEB)

    Rustad, Rolf

    2010-07-01

    A new deepwater multiphase and wet gas flowmeter for HPHT applications has been developed. The flowmeter covers all multiphase and wet gas applications from heavy oil to lean and dry gas. Key features include a pressure rating of 15,000psi, a maximum process temperature of 205 C (400F) and a maximum water depth of 3500m (11500feet). This paper will discuss the design, the qualification program and the application of industry standards and codes in the qualification program. The qualification philosophy and the selected standards and codes may be applied in qualification of most types of equipment for the deepwater HPHT oil and gas industry. (Author)

  5. Size-dependent concentration of N0 paramagnetic centres in HPHT nanodiamonds

    OpenAIRE

    Yavkin, Boris V; Mamin, Georgy V; Gafurov, Marat R.; Orlinskii, Sergei B.

    2015-01-01

    Size-calibrated commercial nanodiamonds synthesized by high-pressure high-temperature (HPHT) technique were studied by high-frequency W and conventional X band electron paramagnetic resonance (EPR) spectroscopy. The numbers of spins in the studied samples were estimated. The core-shell model of the HPHT nanodiamonds was proposed to explain the observed dependence of the concentration of the N0 paramagnetic centers. Two other observed paramagnetic centers are attributed to the two types of str...

  6. Size-dependent concentration of N0 paramagnetic centres in HPHT nanodiamonds

    Directory of Open Access Journals (Sweden)

    B.V. Yavkin, G.V. Mamin, M.R. Gafurov, S.B. Orlinskii

    2015-12-01

    Full Text Available Size-calibrated commercial nanodiamonds synthesized by high-pressure high-temperature (HPHT technique were studied by high-frequency W- and conventional X-band electron paramagnetic resonance (EPR spectroscopy. The numbers of spins in the studied samples were estimated. The core-shell model of the HPHT nanodiamonds was proposed to explain the observed dependence of the concentration of the N0 paramagnetic centers. Two other observed paramagnetic centers are attributed to the two types of structures in the nanodiamond shell.

  7. HPHT growth and x-ray characterization of high-quality type IIa diamond.

    Science.gov (United States)

    Burns, R C; Chumakov, A I; Connell, S H; Dube, D; Godfried, H P; Hansen, J O; Härtwig, J; Hoszowska, J; Masiello, F; Mkhonza, L; Rebak, M; Rommevaux, A; Setshedi, R; Van Vaerenbergh, P

    2009-09-09

    The trend in synchrotron radiation (x-rays) is towards higher brilliance. This may lead to a very high power density, of the order of hundreds of watts per square millimetre at the x-ray optical elements. These elements are, typically, windows, polarizers, filters and monochromators. The preferred material for Bragg diffracting optical elements at present is silicon, which can be grown to a very high crystal perfection and workable size as well as rather easily processed to the required surface quality. This allows x-ray optical elements to be built with a sufficient degree of lattice perfection and crystal processing that they may preserve transversal coherence in the x-ray beam. This is important for the new techniques which include phase-sensitive imaging experiments like holo-tomography, x-ray photon correlation spectroscopy, coherent diffraction imaging and nanofocusing. Diamond has a lower absorption coefficient than silicon, a better thermal conductivity and lower thermal expansion coefficient which would make it the preferred material if the crystal perfection (bulk and surface) could be improved. Synthetic HPHT-grown (high pressure, high temperature) type Ib material can readily be produced in the necessary sizes of 4-8 mm square and with a nitrogen content of typically a few hundred parts per million. This material has applications in the less demanding roles such as phase plates: however, in a coherence-preserving beamline, where all elements must be of the same high quality, its quality is far from sufficient. Advances in HPHT synthesis methods have allowed the growth of type IIa diamond crystals of the same size as type Ib, but with substantially lower nitrogen content. Characterization of this high purity type IIa material has been carried out with the result that the crystalline (bulk) perfection of some of the HPHT-grown materials is approaching the quality required for the more demanding applications such as imaging applications and imaging

  8. Structural and functional characterization of HPHT diamond crystals used in photoconductive devices

    Energy Technology Data Exchange (ETDEWEB)

    Pace, E.; Pini, A. [Florence Univ. (Italy). Ist. di Astronomia; Vinattieri, A.; Bogani, F.; Santoro, M.; Messina, G.; Santangelo, S.; Sato, Y.

    2000-09-01

    Diamond films are extensively studied for applications as functional material for UV photoconductors. CVD-grown polycrystalline diamond films show very interesting performances, but their complete exploitation is actually limited by a slow time response if compared to other materials, by a relatively high concentration of structural defects, impurities and grain boundaries, which may affect the collection length of photogenerated charges. High-quality single crystal diamonds could solve some of these problems. The absence of grain boundaries can produce longer collection lengths. The nitrogen and impurity contents can be reduced and then large type-IIa diamond single-crystals can be obtained. In this work, a detailed structural and functional characterization of type Ib HPHT diamond crystals has been carried out and the results have been compared to similar characterizations of CVD films to evaluate the different behavior, taking also into account that these high pressure high temperature (HPHT) diamond crystals contain several tens ppm of nitrogen. (orig.)

  9. AG, TL, and IRSL dosimetric properties in X-ray irradiated HPHT diamond crystals

    Energy Technology Data Exchange (ETDEWEB)

    Gil-Tolano, M.I. [Programa de Posgrado, Departamento de Investigacion en Fisica, Universidad de Sonora, A. P. 5-088, Hermosillo, Sonora, 83190, Mexico (Mexico); Melendrez, R.; Lancheros-Olmos, J.C.; Soto-Puebla, D.; Chernov, V.; Pedroza-Montero, M.; Barboza-Flores, M. [Departamento de Investigacion en Fisica, Universidad de Sonora, A. P. 5-088, Hermosillo, Sonora, 83190, Mexico (Mexico); Castaneda, B. [Departamento de Fisica, Universidad de Sonora, Blvd. Luis Encinas y Rosales S/N, Hermosillo, Sonora, 83000, Mexico (Mexico)

    2014-10-15

    HPHT diamonds have been studied for several years for their potential in different applications. In previous studies it has been found that the thermoluminescence (TL) glow curves of ''as-grown'' HPHT diamonds are non-reproducible. In this work, we study the afterglow (AG), thermoluminescent (TL), and optically stimulated luminescence (OSL) response of commercial samples of synthetic HPHT type-Ib diamond crystals exposed to X-ray irradiation (0.75 mA, 35 kV) at a dose rate of 0.624 Gy/s, after a high gamma ({sup 60}Co) dose irradiation of 500 kGy followed by a thermal treatment at 1073 K for 1 h in nitrogen atmosphere. Deconvolution of the TL glow curves shows four peaks, located around 379, 509, 561, and 609 K. The crystals exhibit evident AG recorded for 300 s immediately after X-ray irradiation, due to the thermal emptying of the traps responsible for the low-temperature TL peaks (below 400 K). The stimulation of irradiated crystals with 870-nm light, creates pronounced OSL and destroys all TL peaks with the exception of the high-temperature peak at 609 K. The dose responses of the integrated AG, TL, and OSL are linear in the range of 0.6-5 Gy and saturated at higher doses. The reproducibility of AG, TL, and OSL measurements is about 5%. The fading in the first hour of storage in dark conditions at RT of TL signal of HPHT diamond is mainly associated to the emptying of the traps responsible for the 379-K TL peaks. (copyright 2014 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  10. Ammonia synthesis at low temperatures

    DEFF Research Database (Denmark)

    Rod, Thomas Holm; Logadottir, Ashildur; Nørskov, Jens Kehlet

    2000-01-01

    have been carried out to evaluate its feasibility. The calculations suggest that it might be possible to catalytically produce ammonia from molecular nitrogen at low temperatures and pressures, in particular if energy is fed into the process electrochemically. (C) 2000 American Institute of Physics.......Density functional theory (DFT) calculations of reaction paths and energies for the industrial and the biological catalytic ammonia synthesis processes are compared. The industrial catalyst is modeled by a ruthenium surface, while the active part of the enzyme is modeled by a MoFe6S9 complex...

  11. Temperature uniformity mapping in a high pressure high temperature reactor using a temperature sensitive indicator

    NARCIS (Netherlands)

    Grauwet, T.; Plancken, van der I.; Vervoort, L.; Matser, A.M.; Hendrickx, M.; Loey, van A.

    2011-01-01

    Recently, the first prototype ovomucoid-based pressure–temperature–time indicator (pTTI) for high pressure high temperature (HPHT) processing was described. However, for temperature uniformity mapping of high pressure (HP) vessels under HPHT sterilization conditions, this prototype needs to be

  12. Production of hard metal by HPHT using NB as a new binder

    International Nuclear Information System (INIS)

    Oliveira, M.P.; Barros, R.A.; Pecanha Junior, L.A.F.; Guimaraes, R.S.; Filgueira, M.

    2016-01-01

    Full text: Due to the growing metalworking sector, development of new materials for use as cutting tools is necessary, seeking the reduction of energy consumption, as well as the machining time. In this sense, carbide inserts are widely used as tools. Usually, these inserts are manufactured with the use of cobalt as a binder. However, this material is scarce in the market and its cost is very high, and has high toxicity. This paper aims to produce carbide inserts by sintering at high pressure and high temperature (HP-HT), using innovative alloying elements, more easily accessible and at a low cost, such as Nb and Ni. The inserts were produced as follows: powders were sintered under 7,7GPa pressure and temperatures between 1550 deg C and 1850 deg C. Excellent results of densification, hardness and fracture toughness of the inserts was achieved. The phases formed in the sintering were analyzed by XRD. Microstructure was studied by scanning electron microscopy (SEM) and laser microscopy (CONFOCAL). Machining tests were carried out according to the ISO-3685 standard, indicating improved performance for the produced inserts. (author)

  13. Thermoelectric properties of In-substituted Ge-based clathrates prepared by HPHT

    Directory of Open Access Journals (Sweden)

    Binwu Liu

    2018-03-01

    Full Text Available Bulk materials Ba8Ga16InxGe30-x (x = 0.5, 1.0, 1.5 were prepared by High-Pressure and High-Temperature (HPHT method and the crystal structure has been confirmed by X-ray diffraction and cell refinement. The actual In composition was much lower than the starting composition, and lattice constants increased with the increase of substitution. As the temperature increased, the Seebeck coefficient and electrical resistivity increased first and then decreased, while the thermal conductivity was the opposite, which leads to significant enhancement on thermoelectric properties of the clathrates. The substitution of indium elements decreased the seebeck coefficient and electrical resistivity, and also changed the microstructure of the compounds. A minimum thermal conductivity of 0.84 Wm−1K−1 was obtained, and a good ZT value of 0.52 was achieved. The grain boundaries and lattice defects generated by high pressure can effectively scatter phonons of different frequencies, which reduce the lattice thermal conductivity.

  14. Production of hard metal by HPHT using NB as a new binder

    Energy Technology Data Exchange (ETDEWEB)

    Oliveira, M.P.; Barros, R.A.; Pecanha Junior, L.A.F.; Guimaraes, R.S.; Filgueira, M. [Universidade Estadual do Norte Fluminense (UENF), Niteroi, RJ (Brazil)

    2016-07-01

    Full text: Due to the growing metalworking sector, development of new materials for use as cutting tools is necessary, seeking the reduction of energy consumption, as well as the machining time. In this sense, carbide inserts are widely used as tools. Usually, these inserts are manufactured with the use of cobalt as a binder. However, this material is scarce in the market and its cost is very high, and has high toxicity. This paper aims to produce carbide inserts by sintering at high pressure and high temperature (HP-HT), using innovative alloying elements, more easily accessible and at a low cost, such as Nb and Ni. The inserts were produced as follows: powders were sintered under 7,7GPa pressure and temperatures between 1550 deg C and 1850 deg C. Excellent results of densification, hardness and fracture toughness of the inserts was achieved. The phases formed in the sintering were analyzed by XRD. Microstructure was studied by scanning electron microscopy (SEM) and laser microscopy (CONFOCAL). Machining tests were carried out according to the ISO-3685 standard, indicating improved performance for the produced inserts. (author)

  15. Low Temperature Synthesis of Magnesium Aluminate Spinel

    International Nuclear Information System (INIS)

    Lebedovskaya, E.G.; Gabelkov, S.V.; Litvinenko, L.M.; Logvinkov, D.S.; Mironova, A.G.; Odejchuk, M.A.; Poltavtsev, N.S.; Tarasov, R.V.

    2006-01-01

    The low-temperature synthesis of magnesium-aluminum spinel is carried out by a method of thermal decomposition in combined precipitated hydrates. The fine material of magnesium-aluminium spinel with average size of coherent dispersion's area 4...5 nanometers is obtained. Magnesium-aluminum spinel and initial hydrates were investigated by methods of the differential thermal analysis, the x-ray phase analysis and measurements of weight loss during the dehydration and thermal decomposition. It is established that synthesis of magnesium-aluminum spinel occurs at temperature 300 degree C by method of the x-ray phase analysis

  16. Room temperature synthesis of biodiesel using sulfonated ...

    Science.gov (United States)

    Sulfonation of graphitic carbon nitride (g-CN) affords a polar and strongly acidic catalyst, Sg-CN, which displays unprecedented reactivity and selectivity in biodiesel synthesis and esterification reactions at room temperature. Prepared for submission to Royal Society of Chemistry (RSC) journal, Green Chemistry as a communication.

  17. High-Pressure-High-Temperature Processing Reduces Maillard Reaction and Viscosity in Whey Protein-Sugar Solutions.

    Science.gov (United States)

    Avila Ruiz, Geraldine; Xi, Bingyan; Minor, Marcel; Sala, Guido; van Boekel, Martinus; Fogliano, Vincenzo; Stieger, Markus

    2016-09-28

    The aim of the study was to determine the influence of pressure in high-pressure-high-temperature (HPHT) processing on Maillard reactions and protein aggregation of whey protein-sugar solutions. Solutions of whey protein isolate containing either glucose or trehalose at pH 6, 7, and 9 were treated by HPHT processing or conventional high-temperature (HT) treatments. Browning was reduced, and early and advanced Maillard reactions were retarded under HPHT processing at all pH values compared to HT treatment. HPHT induced a larger pH drop than HT treatments, especially at pH 9, which was not associated with Maillard reactions. After HPHT processing at pH 7, protein aggregation and viscosity of whey protein isolate-glucose/trehalose solutions remained unchanged. It was concluded that HPHT processing can potentially improve the quality of protein-sugar-containing foods, for which browning and high viscosities are undesired, such as high-protein beverages.

  18. Size and purity control of HPHT nanodiamonds down to 1 nm

    Czech Academy of Sciences Publication Activity Database

    Stehlík, Štěpán; Varga, Marián; Ledinský, Martin; Jirásek, Vít; Artemenko, Anna; Kozak, Halyna; Ondič, Lukáš; Skákalová, V.; Argentero, G.; Pennycook, T.; Meyer, J.C.; Fejfar, Antonín; Kromka, Alexander; Rezek, Bohuslav

    2015-01-01

    Roč. 119, č. 49 (2015), s. 27708-27720 ISSN 1932-7447 R&D Projects: GA ČR GA15-01809S Institutional support: RVO:68378271 Keywords : HPHT nanodiamond * detonation nanodiamond * air-annealing * phonon confinement * Raman spectroscopy * STEM Subject RIV: BM - Solid Matter Physics ; Magnetism Impact factor: 4.509, year: 2015

  19. Manufacturing Demonstration Facility: Low Temperature Materials Synthesis

    International Nuclear Information System (INIS)

    Graham, David E.; Moon, Ji-Won; Armstrong, Beth L.; Datskos, Panos G.; Duty, Chad E.; Gresback, Ryan; Ivanov, Ilia N.; Jacobs, Christopher B.; Jellison, Gerald Earle; Jang, Gyoung Gug; Joshi, Pooran C.; Jung, Hyunsung; Meyer, Harry M.; Phelps, Tommy

    2015-01-01

    The Manufacturing Demonstration Facility (MDF) low temperature materials synthesis project was established to demonstrate a scalable and sustainable process to produce nanoparticles (NPs) for advanced manufacturing. Previous methods to chemically synthesize NPs typically required expensive, high-purity inorganic chemical reagents, organic solvents and high temperatures. These processes were typically applied at small laboratory scales at yields sufficient for NP characterization, but insufficient to support roll-to-roll processing efforts or device fabrication. The new NanoFermentation processes described here operated at a low temperature (~60 C) in low-cost, aqueous media using bacteria that produce extracellular NPs with controlled size and elemental stoichiometry. Up-scaling activities successfully demonstrated high NP yields and quality in a 900-L pilot-scale reactor, establishing this NanoFermentation process as a competitive biomanufacturing strategy to produce NPs for advanced manufacturing of power electronics, solid-state lighting and sensors.

  20. Manufacturing Demonstration Facility: Low Temperature Materials Synthesis

    Energy Technology Data Exchange (ETDEWEB)

    Graham, David E. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Moon, Ji-Won [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Armstrong, Beth L. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Datskos, Panos G. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Duty, Chad E. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Gresback, Ryan [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Ivanov, Ilia N. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Jacobs, Christopher B. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Jellison, Gerald Earle [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Jang, Gyoung Gug [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Joshi, Pooran C. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Jung, Hyunsung [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Meyer, III, Harry M. [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States); Phelps, Tommy [Oak Ridge National Lab. (ORNL), Oak Ridge, TN (United States)

    2015-06-30

    The Manufacturing Demonstration Facility (MDF) low temperature materials synthesis project was established to demonstrate a scalable and sustainable process to produce nanoparticles (NPs) for advanced manufacturing. Previous methods to chemically synthesize NPs typically required expensive, high-purity inorganic chemical reagents, organic solvents and high temperatures. These processes were typically applied at small laboratory scales at yields sufficient for NP characterization, but insufficient to support roll-to-roll processing efforts or device fabrication. The new NanoFermentation processes described here operated at a low temperature (~60 C) in low-cost, aqueous media using bacteria that produce extracellular NPs with controlled size and elemental stoichiometry. Up-scaling activities successfully demonstrated high NP yields and quality in a 900-L pilot-scale reactor, establishing this NanoFermentation process as a competitive biomanufacturing strategy to produce NPs for advanced manufacturing of power electronics, solid-state lighting and sensors.

  1. Lateral overgrowth of diamond film on stripes patterned Ir/HPHT-diamond substrate

    Science.gov (United States)

    Wang, Yan-Feng; Chang, Xiaohui; Liu, Zhangcheng; Liu, Zongchen; Fu, Jiao; Zhao, Dan; Shao, Guoqing; Wang, Juan; Zhang, Shaopeng; Liang, Yan; Zhu, Tianfei; Wang, Wei; Wang, Hong-Xing

    2018-05-01

    Epitaxial lateral overgrowth (ELO) of diamond films on patterned Ir/(0 0 1)HPHT-diamond substrates have been carried out by microwave plasma CVD system. Ir/(0 0 1)HPHT-diamond substrates are fabricated by photolithographic and magnetron sputtering technique. The morphology of the as grown ELO diamond film is characterized by optical microscopy and scanning electronic microscopy. The quality and stress of the ELO diamond film are investigated by surface etching pit density and micro-Raman spectroscopy. Two ultraviolet photodetectors are fabricated on ELO diamond area and non-ELO diamond area prepared on same substrate, and that one on ELO diamond area indicates better photoelectric properties. All results indicate quality of ELO diamond film is improved.

  2. Stability of Basalt plus Anhydrite plus Calcite at HP-HT: Implications for Venus, the Earth and Mars

    Science.gov (United States)

    Martin, A. M.; Righter, K.; Treiman, A. H.

    2010-01-01

    "Canali" observed at Venus surface by Magellan are evidence for very long melt flows, but their composition and origin remain uncertain. The hypothesis of water-rich flow is not reasonable regarding the temperature at Venus surface. The length of these channels could not be explained by a silicate melt composition but more likely, by a carbonate-sulfate melt which has a much lower viscosity (Kargel et al 1994). One hypothesis is that calcite CaCO3 and anhydrite CaSO4 which are alteration products of basalts melted during meteorite impacts. A famous example recorded on the Earth (Chicxulub) produced melt and gas rich in carbon and sulfur. Calcite and sulfate evaporites are also present on Mars surface, associated with basalts. An impact on these materials might release C- and S-rich melt or fluid. Another type of planetary phenomenon (affecting only the Earth) might provoke a high pressure destabilization of basalt+anhydrite+calcite. Very high contents of C and S are measured in some Earth s magmas, either dissolved or in the form of crystals (Luhr 2008). As shown by the high H content and high fO2 of primary igneous anhydrite-bearing lavas, the high S content in their source may be explained by subduction of an anhydrite-bearing oceanic crust, either directly (by melting followed by eruption) or indirectly (by release of S-rich melt or fluid that metasomatize the mantle) . Calcite is a major product of oceanic sedimentation and alteration of the crust. Therefore, sulfate- and calcite-rich material may be subducted to high pressures and high temperatures (HP-HT) and release S- and C-rich melts or fluids which could influence the composition of subduction zone lavas or gases. Both phenomena - meteorite impact and subduction - imply HP-HT conditions - although the P-T-time paths are different. Some HP experimental/theoretical studies have been performed on basalt/eclogite, calcite and anhydrite separately or on a combination of two. In this study we performed piston

  3. Evaluation des fluides de forage HP/HT pour forages profonds Evaluation of Hp/Ht Drilling Fluid Formulations for Deep Drilling

    Directory of Open Access Journals (Sweden)

    Argillier J. F.

    2006-11-01

    Full Text Available Le forage de puits profonds exige la mise au point de fluides de forage dont la formulation est adaptée aux températures élevées de formation : l'une des principales difficultés est la dégradation thermique des additifs chimiques utilisés dans les formulations à base d'eau qui se produit fréquemment lors du forage de puits à température élevée. Cette dégradation peut conduire à des variations importantes des caractéristiques rhéologiques et de filtration et à une perte de propriétés nécessaires à leur performance. De plus, même s'il n'y a pas de dégradation des composants la viscosité des solutions de polymères hydrosolubles couramment utilisés dans les formulations de fluides diminue fortement avec l'augmentation de la température au-dessus de 60°C. Une autre source de difficulté qui apparaît à forte température avec les boues à base d'eau est la gélification des argiles utilisées dans la formulation. Ce phénomène provoque une forte augmentation de la viscosité de la formulation et des pertes de charges, en particulier en cas de reprise de forage. Diverses méthodes ont été mises au point pour étudier le comportement des boues à base d'eau dans des conditions de pression et de température élevées, entre autres : - des expériences de laboratoire, pour étudier par exemple la stabilité en conditions anaérobies des solutions de polymères et le comportement rhéologique des suspensions d'argile dans des conditions de pression et de température élevées afin de simuler les caractéristiques de gélification des argiles à haute température; - des essais sur boucle d'étude HP/HT en utilisant une boucle expérimentale conçue pour étudier les fluides de forage dans des conditions de fond réalistes, c'est-à-dire des températures atteignant 180°C, des pressions atteignant 500 bar et des taux de cisaillement atteignant 10 000 s puissance( -1 Cette méthodologie a permis d'étudier un certain

  4. Synthesis and processing of nanostructured BN and BN/Ti composites

    Science.gov (United States)

    Horvath, Robert Steven

    Superhard materials, such as cubic-BN, are widely used in machine tools, grinding wheels, and abrasives. Low density combined with high hardness makes c-BN and its composites attractive candidate materials for personnel and vehicular armor. However, improvements in toughness, and ballistic-impact performance, are needed to meet anticipated performance requirements. To achieve such improvements, we have targeted for development nanostructured c-BN, and its composites with Ti. Current research utilizes an experimental high pressure/high temperature (HPHT) method to produce these materials on a laboratory scale. Results from this work should transfer well into the industrial arena, utilizing high-tonnage presses used in the production of synthetic diamond and c-BN. Progress has been made in: (1) HPHT synthesis of cBN powder using Mg as catalyst; (2) HPHT consolidation of cBN powder to produce nanostructured cBN; (3) reactive-HPHT consolidation of mixed cBN/Ti powder to produce nanostructured Ti- or TiB2/TiN-bonded cBN; and (4) reactive-HPHT consolidation of mixed hBN/Ti powder to produce nanostructured Ti-bonded TiB2/TiN or TiB2/TiN. Even so, much remains to be done to lay a firm scientific foundation to enable the reproducible fabrication of large-area panels for armor applications. To this end, Rutgers has formed a partnership with a major producer of hard and superhard materials. The ability to produce hard and superhard nanostructured composites by reacting cBN or hBN with Ti under high pressure also enables multi-layered structures to be developed. Such structures may be designed to satisfy impedance-mismatch requirements for high performance armor, and possibly provide a multi-hit capability. A demonstration has been made of reactive-HPHT processing of multi-layered composites, consisting of alternating layers of superhard Ti-bonded cBN and tough Ti. It is noteworthy that the pressure requirements for processing Ti-bonded cBN, Ti-bonded TiB2/TiN, and their

  5. Factors affecting shut-in pressure rise: kicks in offshore HPHT wells

    Energy Technology Data Exchange (ETDEWEB)

    Schilhab, L C [Sedco Forex, (Country unknown/Code not available); Rezmer-Cooper, I M [Anadril, (Country unknown/Code not available)

    1997-05-01

    Deep water and HPHT operations are two areas where the use of sophisticated simulators can enable difficult processes and procedures to be broken down into individual identifiable contributions. In the paper we discuss some of the factors that are likely to affect shut-in pressure rise in offshore drilling operations, and how a simulator can be used to answer other, less obvious questions concerning deep water well control operations. We examine the effect of gas solubility by considering a gas-kick in a deep HPHT well drilled with oil-base mud. In this case, most of the influx will be dissolved in the mud, thus removing one of the processes for increasing the wellbore pressure. In terms of s safe state to disconnect from a well in rough weather, provided that the mud yield stress negates migration of the gas-cut mud, leaving the influx in solution at the bottom of the well should not lead to increasing wellbore pressures. Significant wellbore pressure effects may also occur after closing the blowout preventers (BOP`s) on a well without an influx (or with an influx in solution), and allowing the mud to heat up. We show that in typical HPHT geometries the pressure can rise by up to 8 bar/deg C. Similar magnitudes of pressure can also increase whilst circulating trapped gas out of a BOP at the end of a well control operation. We note that these effects may also be attenuated by fluid loss and wellbore compliance for wells with significant open hole sections. Indeed, gas trapped in the BOP should be safety removed by established well control procedures. However, preliminary studies with the simulator (and confirmed by field tests in the literature) have shown that an accidental release of a small amount of gas into a deep water riser may disperse, and not cause the riser to unload. (authors) 5 refs.

  6. Synthesis of pure ozone by nanosecond discharge at cryogenic temperatures

    International Nuclear Information System (INIS)

    Amirov, R.H.; Asinovsky, E.I.; Samoilov, I.S.

    1996-01-01

    Synthesis of pure ozone by nanosecond discharge at cryogenic temperatures was experimentally examined. The average ozone concentration in the volume of the discharge tube was less at cryogenic temperatures than at room temperatures. The production of condensed ozone have been determined by measuring the ozone concentration when the walls was heated and ozone evaporated. The energy yield of ozone generation at cryogenic temperatures has been calculated. The maximum value was 200 g/kWh

  7. Low-temperature synthesis of silicon carbide powder using shungite

    International Nuclear Information System (INIS)

    Gubernat, A.; Pichor, W.; Lach, R.; Zientara, D.; Sitarz, M.; Springwald, M.

    2017-01-01

    The paper presents the results of investigation the novel and simple method of synthesis of silicon carbide. As raw material for synthesis was used shungite, natural mineral rich in carbon and silica. The synthesis of SiC is possible in relatively low temperature in range 1500–1600°C. It is worth emphasising that compared to the most popular method of SiC synthesis (Acheson method where the temperature of synthesis is about 2500°C) the proposed method is much more effective. The basic properties of products obtained from different form of shungite and in wide range of synthesis temperature were investigated. The process of silicon carbide formation was proposed and discussed. In the case of synthesis SiC from powder of raw materials the product is also in powder form and not requires any additional process (crushing, milling, etc.). Obtained products are pure and after grain classification may be used as abrasive and polishing powders. (Author)

  8. Low-temperature synthesis of silicon carbide powder using shungite

    Energy Technology Data Exchange (ETDEWEB)

    Gubernat, A.; Pichor, W.; Lach, R.; Zientara, D.; Sitarz, M.; Springwald, M.

    2017-07-01

    The paper presents the results of investigation the novel and simple method of synthesis of silicon carbide. As raw material for synthesis was used shungite, natural mineral rich in carbon and silica. The synthesis of SiC is possible in relatively low temperature in range 1500–1600°C. It is worth emphasising that compared to the most popular method of SiC synthesis (Acheson method where the temperature of synthesis is about 2500°C) the proposed method is much more effective. The basic properties of products obtained from different form of shungite and in wide range of synthesis temperature were investigated. The process of silicon carbide formation was proposed and discussed. In the case of synthesis SiC from powder of raw materials the product is also in powder form and not requires any additional process (crushing, milling, etc.). Obtained products are pure and after grain classification may be used as abrasive and polishing powders. (Author)

  9. Effect of temperature and time on solvothermal synthesis of ...

    Indian Academy of Sciences (India)

    Effect of temperature and time study on solvothermal synthesis of BaTiO3 revealed that a moderate reaction temperature i.e. 185◦C and longer reaction time favour tetragonal phase stabiliza- tion. Dissolution–precipitation appears to be the transformation mechanism for the crystallization of BaTiO3 from particulate TiO2 ...

  10. Robust Temperature Control of a Thermoelectric Cooler via μ -Synthesis

    Science.gov (United States)

    Kürkçü, Burak; Kasnakoğlu, Coşku

    2018-02-01

    In this work robust temperature control of a thermoelectric cooler (TEC) via μ -synthesis is studied. An uncertain dynamical model for the TEC that is suitable for robust control methods is derived. The model captures variations in operating point due to current, load and temperature changes. A temperature controller is designed utilizing μ -synthesis, a powerful method guaranteeing robust stability and performance. For comparison two well-known control methods, namely proportional-integral-derivative (PID) and internal model control (IMC), are also realized to benchmark the proposed approach. It is observed that the stability and performance on the nominal model are satisfactory for all cases. On the other hand, under perturbations the responses of PID and IMC deteriorate and even become unstable. In contrast, the μ -synthesis controller succeeds in keeping system stability and achieving good performance under all perturbations within the operating range, while at the same time providing good disturbance rejection.

  11. Multi-Temperature Zone, Droplet-based Microreactor for Increased Temperature Control in Nanoparticle Synthesis

    KAUST Repository

    Erdem, E. Yegâ n; Cheng, Jim C.; Doyle, Fiona M.; Pisano, Albert P.

    2013-01-01

    Microreactors are an emerging technology for the controlled synthesis of nanoparticles. The Multi-Temperature zone Microreactor (MTM) described in this work utilizes thermally isolated heated and cooled regions for the purpose of separating

  12. High pressure synthesis and investigations of properties of boron allotropes and boron carbide

    International Nuclear Information System (INIS)

    Chuvashova, Irina

    2017-01-01

    This work aimed at the development of the high-pressure high-temperature (HPHT) synthesis of single crystals of boron allotropes and boron-rich compounds, which could be used further for precise investigations of their structures, properties, and behavior at extreme conditions. To summarize, the present work resulted in the HPHT synthesis of the first previously unknown non-icosahedral boron allotrope ζ-B. This finding confirmed earlier theoretical predictions, which stayed unproven for decades because of experimental challenges which couldn't be overcome until recently. Structural stability of α-B and β-B in the Mbar pressure range and B 13 C 2 up to 68 GPa was experimentally proven. Accurate measurements of the unit cell and B 12 icosahedra volumes of the stoichiometric boron carbide B 13 C 2 as a function of pressure led to conclusion that they undergo a similar reduction upon compression that is typical for covalently bonded solids. Neither 'molecular-like' nor 'inversed molecular-like' solid behavior upon compression was detected that has closed a long-standing scientific dispute. A comparison of the compressional behavior of B 13 C 2 with that of α-B and γ-B allotropes and B 4 C showed that it is determined by the types of bonding involved in the course of compression.

  13. High pressure synthesis and investigations of properties of boron allotropes and boron carbide

    Energy Technology Data Exchange (ETDEWEB)

    Chuvashova, Irina

    2017-06-12

    This work aimed at the development of the high-pressure high-temperature (HPHT) synthesis of single crystals of boron allotropes and boron-rich compounds, which could be used further for precise investigations of their structures, properties, and behavior at extreme conditions. To summarize, the present work resulted in the HPHT synthesis of the first previously unknown non-icosahedral boron allotrope ζ-B. This finding confirmed earlier theoretical predictions, which stayed unproven for decades because of experimental challenges which couldn't be overcome until recently. Structural stability of α-B and β-B in the Mbar pressure range and B{sub 13}C{sub 2} up to 68 GPa was experimentally proven. Accurate measurements of the unit cell and B{sub 12} icosahedra volumes of the stoichiometric boron carbide B{sub 13}C{sub 2} as a function of pressure led to conclusion that they undergo a similar reduction upon compression that is typical for covalently bonded solids. Neither 'molecular-like' nor 'inversed molecular-like' solid behavior upon compression was detected that has closed a long-standing scientific dispute. A comparison of the compressional behavior of B{sub 13}C{sub 2} with that of α-B and γ-B allotropes and B{sub 4}C showed that it is determined by the types of bonding involved in the course of compression.

  14. Moderate Temperature Synthesis of Mesoporous Carbon

    KAUST Repository

    Dua, Rubal; Wang, Peng

    2013-01-01

    Methods and composition for preparation of mesoporous carbon material are provided. For example, in certain aspects methods for carbonization and activation at selected temperature ranges are described. Furthermore, the invention provides products prepared therefrom.

  15. Moderate Temperature Synthesis of Mesoporous Carbon

    KAUST Repository

    Dua, Rubal

    2013-01-03

    Methods and composition for preparation of mesoporous carbon material are provided. For example, in certain aspects methods for carbonization and activation at selected temperature ranges are described. Furthermore, the invention provides products prepared therefrom.

  16. IMPROVED SYNTHESIS OF ROOM TEMPERATURE IONIC LIQUIDS

    Science.gov (United States)

    Room temperature ionic liquids (RTILs), molten salts comprised of N-alkylimidazolium cations and various anions, have received significant attention due to their commercial potential in a variety of chemical applications especially as substitutes for conventional volatile organic...

  17. Self-propagating high temperature synthesis and magnetic

    Indian Academy of Sciences (India)

    Ni–Zn ferrite powders were synthesized by self-propagating high temperature synthesis (SHS) method. X-ray diffraction, TEM and vibrating sample magnetometry (VSM) were used to characterize the phase composition, microstructure and magnetic properties of the combustion products. The effect of the combustion ...

  18. Solution-phase synthesis of nanomaterials at low temperature

    Science.gov (United States)

    Zhu, Yongchun; Qian, Yitai

    2009-01-01

    This paper reviews the solution-phase synthesis of nanoparticles via some routes at low temperatures, such as room temperature route, wave-assisted synthesis (γ-irradiation route and sonochemical route), directly heating at low temperatures, and hydrothermal/solvothermal methods. A number of strategies were developed to control the shape, the size, as well as the dispersion of nanostructures. Using diethylamine or n-butylamine as solvent, semiconductor nanorods were yielded. By the hydrothermal treatment of amorphous colloids, Bi2S3 nanorods and Se nanowires were obtained. CdS nanowires were prepared in the presence of polyacrylamide. ZnS nanowires were obtained using liquid crystal. The polymer poly (vinyl acetate) tubule acted as both nanoreactor and template for the CdSe nanowire growth. Assisted by the surfactant of sodium dodecyl benzenesulfonate (SDBS), nickel nanobelts were synthesized. In addition, Ag nanowires, Te nanotubes and ZnO nanorod arrays could be prepared without adding any additives or templates.

  19. Towards room temperature, direct, solvent free synthesis of tetraborohydrides

    International Nuclear Information System (INIS)

    Remhof, A; Yan, Y; Friedrichs, O; Kim, J W; Mauron, Ph; Borgschulte, A; Züttel, A; Wallacher, D; Buchsteiner, A; Hoser, A; Oh, K H; Cho, Y W

    2012-01-01

    Due to their high hydrogen content, tetraborohydrides are discussed as potential synthetic energy carriers. On the example of lithium borohydride LiBH 4 , we discuss current approaches of direct, solvent free synthesis based on gas solid reactions of the elements or binary hydrides and/or borides with gaseous H 2 or B 2 H 6 . The direct synthesis from the elements requires high temperature and high pressure (700°C, 150bar D 2 ). Using LiB or AlB 2 as boron source reduces the required temperature by more than 300 K. Reactive milling of LiD with B 2 H 6 leads to the formation of LiBD 4 already at room temperature. The reactive milling technique can also be applied to synthesize other borohydrides from their respective metal hydrides.

  20. Catalytic chemical amide synthesis at room temperature: one more step toward peptide synthesis.

    Science.gov (United States)

    Mohy El Dine, Tharwat; Erb, William; Berhault, Yohann; Rouden, Jacques; Blanchet, Jérôme

    2015-05-01

    An efficient method has been developed for direct amide bond synthesis between carboxylic acids and amines via (2-(thiophen-2-ylmethyl)phenyl)boronic acid as a highly active bench-stable catalyst. This catalyst was found to be very effective at room temperature for a large range of substrates with slightly higher temperatures required for challenging ones. This methodology can be applied to aliphatic, α-hydroxyl, aromatic, and heteroaromatic acids as well as primary, secondary, heterocyclic, and even functionalized amines. Notably, N-Boc-protected amino acids were successfully coupled in good yields with very little racemization. An example of catalytic dipeptide synthesis is reported.

  1. Synthesis of observer furnace temperature control

    OpenAIRE

    Жученко, А. І.; Цапар, В. С.

    2015-01-01

    В даній роботі проведено синтез спостерігачів стану температурного режиму скловарної печі на базі різних модифікацій фільтра Калмана. Проведено імітаційне моделювання роботи скловарної печі із синтезованими спостерігачами. Досліджено результати моделювання та зроблено висновки щодо доцільності використання даних спостерігачів при різних видах збурень. Показано, що найкраще працює модифікований фільтр Калмана з фільтрами шумів, що діють на стан об’єкту. The synthesis of observer status furn...

  2. Multi-Temperature Zone, Droplet-based Microreactor for Increased Temperature Control in Nanoparticle Synthesis

    KAUST Repository

    Erdem, E. Yegân

    2013-12-12

    Microreactors are an emerging technology for the controlled synthesis of nanoparticles. The Multi-Temperature zone Microreactor (MTM) described in this work utilizes thermally isolated heated and cooled regions for the purpose of separating nucleation and growth processes as well as to provide a platform for a systematic study on the effect of reaction conditions on nanoparticle synthesis. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  3. High pressure sintering (HP-HT) of diamond powders with titanium and titanium carbide

    International Nuclear Information System (INIS)

    Jaworska, L.

    1999-01-01

    Polycrystalline diamond compacts for cutting tools are mostly manufactured using high pressure sintering (HP-HT). The standard diamond compacts are prepared by diamond powders sintering with metallic binding phase. The first group of metallic binder are metals able to solve carbon - Co, Ni. The second group of metal binders are carbide forming elements - Ti, Cr, W and others. The paper describes high pressure sintering of diamond powder with titanium and nonstoichiometry titanium carbide for cutting tool application. A type of binding phase has the significant influence on microstructure and mechanical properties of diamond compacts. Very homogeneous structure was achieved in case of compacts obtained from metalized diamond where diamond-TiC-diamond connection were predominant. In the case of compacts prepared by mechanical mixing of diamond with titanium powders the obtained structure was nonhomogeneous with titanium carbide clusters. They had more diamond to diamond connections. These compacts compared to the compact made of metallized diamond have greater wear resistance. In the case of the diamond and TiC 0.92 sintering the strong bonding of TiC diamond grains was obtained. The microstructure observations for diamond with 5% wt. Ti and diamond with 5% wt. TiC 0.92 (the initial composition) compacts were performed in transmission microscope. For two type of compacts the strong bonding phase TiC without defects is creating. (author)

  4. Alcohol synthesis in a high-temperature slurry reactor

    Energy Technology Data Exchange (ETDEWEB)

    Roberts, G.W.; Marquez, M.A.; McCutchen, M.S. [North Carolina State Univ., Raleigh, NC (United States)

    1995-12-31

    The overall objective of this contract is to develop improved process and catalyst technology for producing higher alcohols from synthesis gas or its derivatives. Recent research has been focused on developing a slurry reactor that can operate at temperatures up to about 400{degrees}C and on evaluating the so-called {open_quotes}high pressure{close_quotes} methanol synthesis catalyst using this reactor. A laboratory stirred autoclave reactor has been developed that is capable of operating at temperatures up to 400{degrees}C and pressures of at least 170 atm. The overhead system on the reactor is designed so that the temperature of the gas leaving the system can be closely controlled. An external liquid-level detector is installed on the gas/liquid separator and a pump is used to return condensed slurry liquid from the separator to the reactor. In order to ensure that gas/liquid mass transfer does not influence the observed reaction rate, it was necessary to feed the synthesis gas below the level of the agitator. The performance of a commercial {open_quotes}high pressure {close_quotes} methanol synthesis catalyst, the so-called {open_quotes}zinc chromite{close_quotes} catalyst, has been characterized over a range of temperature from 275 to 400{degrees}C, a range of pressure from 70 to 170 atm., a range of H{sub 2}/CO ratios from 0.5 to 2.0 and a range of space velocities from 2500 to 10,000 sL/kg.(catalyst),hr. Towards the lower end of the temperature range, methanol was the only significant product.

  5. The effect of High Pressure and High Temperature processing on carotenoids and chlorophylls content in some vegetables.

    Science.gov (United States)

    Sánchez, Celia; Baranda, Ana Beatriz; Martínez de Marañón, Iñigo

    2014-11-15

    The effect of High Pressure (HP) and High Pressure High Temperature (HPHT) processing on carotenoid and chlorophyll content of six vegetables was evaluated. In general, carotenoid content was not significantly influenced by HP or HPHT treatments (625 MPa; 5 min; 20, 70 and 117 °C). Regarding chlorophylls, HP treatment caused no degradation or slight increases, while HPHT processes degraded both chlorophylls. Chlorophyll b was more stable than chlorophyll a at 70 °C, but both of them were highly degraded at 117 °C. HPHT treatment at 117 °C provided products with a good retention of carotenoids and colour in the case of red vegetables. Even though the carotenoids also remained in the green vegetables, their chlorophylls and therefore their colour were so affected that milder temperatures need to be applied. As an industrial scale equipment was used, results will be useful for future industrial implementation of this technology. Copyright © 2014 Elsevier Ltd. All rights reserved.

  6. Ruthenium(V) oxides from low-temperature hydrothermal synthesis

    Energy Technology Data Exchange (ETDEWEB)

    Hiley, Craig I.; Walton, Richard I. [Department of Chemistry, University of Warwick, Coventry (United Kingdom); Lees, Martin R. [Department of Physics, University of Warwick, Coventry (United Kingdom); Fisher, Janet M.; Thompsett, David [Johnson Matthey Technology Centre, Reading (United Kingdom); Agrestini, Stefano [Max-Planck Institut, CPfS, Dresden (Germany); Smith, Ronald I. [ISIS Neutron and Muon Source, Rutherford Appleton Laboratory, Harwell Oxford, Didcot (United Kingdom)

    2014-04-22

    Low-temperature (200 C) hydrothermal synthesis of the ruthenium oxides Ca{sub 1.5}Ru{sub 2}O{sub 7}, SrRu{sub 2}O{sub 6}, and Ba{sub 2}Ru{sub 3}O{sub 9}(OH) is reported. Ca{sub 1.5}Ru{sub 2}O{sub 7} is a defective pyrochlore containing Ru{sup V/VI}; SrRu{sub 2}O{sub 6} is a layered Ru{sup V} oxide with a PbSb{sub 2}O{sub 6} structure, whilst Ba{sub 2}Ru{sub 3}O{sub 9}(OH) has a previously unreported structure type with orthorhombic symmetry solved from synchrotron X-ray and neutron powder diffraction. SrRu{sub 2}O{sub 6} exhibits unusually high-temperature magnetic order, with antiferromagnetism persisting to at least 500 K, and refinement using room temperature neutron powder diffraction data provides the magnetic structure. All three ruthenates are metastable and readily collapse to mixtures of other oxides upon heating in air at temperatures around 300-500 C, suggesting they would be difficult, if not impossible, to isolate under conventional high-temperature solid-state synthesis conditions. (copyright 2014 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  7. Temperature Dependence on The Synthesis of Jatropha Biolubricant

    International Nuclear Information System (INIS)

    Resul, Muhammad Faiz M Gunam; Ghazi, Tinia Idaty Mohd; Idris, Azni

    2011-01-01

    Jatropha oil has good potential as the renewable energy as well as lubricant feedstock. The synthesis of jatropha biolubricant was performed by transesterification of jatropha methyl ester (JME) with trimethyl-ol-propane (TMP) with sodium methoxide (NaOCH3) catalyst. The effects of temperature on the synthesis were studied at a range between 120 deg. C and 200 deg. C with pressure kept at 10mbar. The conversion of JME to jatropha biolubricant was found to be the highest (47%) at 200 deg. C. However, it was suggested that the optimum temperature of the reaction is at 150 deg. C due to insignificant improvement in biolubricant production. To maintain forward reaction, the excess amount of JME was maintained at 3.9:1 ratios to TMP. Kinetic study was done and compared. The synthesis was found to follow a second order reaction with overall rate constant of 1.49 x 10-1 (%wt/wt.min.deg. C)-1. The estimated activation energy was 3.94 kJ/mol. Pour point for jatropha biolubricant was at -3 deg. C and Viscosity Index (VI) ranged from 178 to 183. The basic properties of jatropha biolubricant, pour point and viscosities are found comparable to other plant based biolubricant, namely palm oil and soybean based biolubricant.

  8. Temperature dependence on the synthesis of Jatropha bio lubricant

    International Nuclear Information System (INIS)

    Gunam Resul, M.F.M.; Tinia Idaty Mohd Ghazi; Idris, A.

    2009-01-01

    Full text: Jatropha oil has good potential as the renewable energy as well as lubricant feedstock. The synthesis of jatropha bio lubricant was performed by transesterification of jatropha methyl ester (JME) with trimethyl-ol-propane (TMP) with sodium methoxide (NaOCH 3 ) catalyst. The effects of temperature on the synthesis were studied at a range between 120 degree Celsius and 200 degree Celsius with pressure kept at 10 mbar. The conversion of JME to jatropha bio lubricant was found to be the highest (47 %) at 200 degree Celsius. However, it was suggested that the optimum temperature of the reaction is at 150 degree Celsius due to insignificant improvement in bio lubricant production. To maintain forward reaction, the excess amount of JME was maintained at 3.9:1 ratios to TMP. Kinetic study was done and compared. The synthesis was found to follow a second order reaction with overall rate constant of 1.49 x 10 -1 (% wt/ wt.min.degree Celsius) -1 . The estimated activation energy was 3.94 kJ/mol. Pour point for jatropha bio lubricant was at -3 degree Celsius and Viscosity Index (VI) ranged from 178 to 183. The basic properties of jatropha bio lubricant, pour point and viscosities are found comparable to other plant based bio lubricant, namely palm oil and soybean based bio lubricant. (author)

  9. Low-Temperature Synthesis Routes to Intermetallic Superconductors

    Energy Technology Data Exchange (ETDEWEB)

    Schaak, Raymond E

    2008-01-08

    Over the past few years, our group has gained expertise at developing low-temperature solution-based synthetic pathways to complex nanoscale solids, with particular emphasis on nanocrystalline intermetallic compounds. Our synthetic capabilities are providing tools to reproducibly generate intermetallic nanostructures with simultaneous control over crystal structure, composition, and morphology. This DOE-funded project aims to expand these capabilities to intermetallic superconductors. This could represent an important addition to the tools that are available for the synthesis and processing of intermetallic superconductors, which traditionally utilize high-temperature, high-pressure, thin film, or gas-phase vacuum deposition methods. Our current knowledge of intermetallic superconductors suggests that significant enhancements could result from the inherent benefits of low-temperature solution synthesis, e.g. metastable phase formation, control over nanoscale morphology to facilitate size-dependent property studies, robust and inexpensive processability, low-temperature annealing and consolidation, and impurity incorporation (for doping, stoichiometry control, flux pinning, and improving the critical fields). Our focus is on understanding the superconducting properties as a function of synthetic route, crystal structure, crystallite size, and morphology, and developing the synthetic tools necessary to accomplish this. This research program can currently be divided into two classes of superconducting materials: intermetallics (transition metal/post transition metal) and metal carbides/borides. Both involve the development and exploitation of low-temperature synthesis routes followed by detailed characterization of structures and properties, with the goal of understanding how the synthetic pathways influence key superconducting properties of selected target materials. Because of the low-temperature methods used to synthesize them and the nanocrystalline morphologies

  10. High temperature bismuth cuprate superconductors synthesis and characterization

    International Nuclear Information System (INIS)

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

    1993-01-01

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

  11. Temperature lowering in cryogenic chemical-synthesis techniques and system

    International Nuclear Information System (INIS)

    Martinez, H.E.; Nelson, T.O.; Vikdal, L.N.

    1993-01-01

    When evaluating a chemical synthesis process for a reaction that occurs on the cryogenically cooled walls, it is sometimes necessary to reduce the wall temperatures to enhance the chemical process. To evaluate the chemical process at lower than atmospheric boiling of liquid nitrogen, we built a system and used it to reduce the temperature of the liquid nitrogen. The technique of lowering the liquid nitrogen temperature by reducing the pressure of the boil-off is established knowledge. This paper presents the engineering aspects of the system, design features, equipment requirements, methods of control, and results of the chemical synthesis. The heat input to the system was ∼400 watts, placing a relatively large demand on the pumping system. Our system is a scale-up of the small laboratory experiment, and it provides the information needed to design an effective system. The major problem encountered was the large quantity of liquid escaping the system during the processing, placing a large gas load on the vacuum system

  12. Excitation temperature of a solution plasma during nanoparticle synthesis

    Energy Technology Data Exchange (ETDEWEB)

    Saito, Genki, E-mail: genki@eng.hokudai.ac.jp; Nakasugi, Yuki; Akiyama, Tomohiro [Center for Advanced Research of Energy and Materials, Hokkaido University, Sapporo 060-8628 (Japan)

    2014-08-28

    Excitation temperature of a solution plasma was investigated by spectroscopic measurements to control the nanoparticle synthesis. In the experiments, the effects of edge shielding, applied voltage, and electrode material on the plasma were investigated. When the edge of the Ni electrode wire was shielded by a quartz glass tube, the plasma was uniformly generated together with metallic Ni nanoparticles. The emission spectrum of this electrode contained OH, H{sub α}, H{sub β}, Na, O, and Ni lines. Without an edge-shielded electrode, the continuous infrared radiation emitted at the edge created a high temperature on the electrode surface, producing oxidized coarse particles as a result. The excitation temperature was estimated from the Boltzmann plot. When the voltages were varied at the edge-shielded electrode with low average surface temperature by using different electrolyte concentrations, the excitation temperature of current-concentration spots increased with an increase in the voltage. The size of the Ni nanoparticles decreased at high excitation temperatures. Although the formation of nanoparticles via melting and solidification of the electrode surface has been considered in the past, vaporization of the electrode surface could occur at a high excitation temperature to produce small particles. Moreover, we studied the effects of electrodes of Ti, Fe, Ni, Cu, Zn, Zr, Nb, Mo, Pd, Ag, W, Pt, Au, and various alloys of stainless steel and Cu–Ni alloys. With the exception of Ti, the excitation temperatures ranged from 3500 to 5500 K and the particle size depended on both the excitation temperature and electrode-material properties.

  13. Single Crystal Synthesis and STM Studies of High Temperature Superconductors

    Science.gov (United States)

    Barrientos, Alfonso

    1997-01-01

    This is a final report for the work initiated in September of 1994 under the grant NAG8-1085 - NASA/OMU, on the fabrication of bulk and single crystal synthesis, specific heat measuring and STM studies of high temperature superconductors. Efforts were made to fabricate bulk and single crystals of mercury based superconducting material. A systematic thermal analysis on the precursors for the corresponding oxides and carbonates were carried out to synthesized bulk samples. Bulk material was used as seed in an attempt to grow single crystals by a two-step self flux process. On the other hand bulk samples were characterized by x-ray diffraction, electrical resistivity and magnetic susceptibility, We studied the specific heat behavior in the range from 80 to 300 K. Some preliminary attempts were made to study the atomic morphology of our samples. As part of our efforts we built an ac susceptibility apparatus for measuring the transition temperature of our sintered samples.

  14. Studies on synthesis of diamond at high pressure and temperature

    Science.gov (United States)

    Kailath, Ansu J.

    Diamond is an essential material of modern industry and probably the most versatile abrasive available today. It also has many other industrial applications attributable to its unique mechanical, optical, thermal and electrical properties. Its usage has grown to the extent that there is hardly a production process in modern industry in which industrial diamond does not play a part. Bulk diamond production today is a major industry. Diamonds can be produced in its thermodynamically stable regions either by direct static conversion, or shock-wave conversion. The pressures and temperatures required for direct static conversion are very high. In the catalyst-solvent method, the material used establishes a reaction path with lower activation energy than for direct transformation. This helps in a quicker transformation under more benign conditions. Hence, catalyst-solvent synthesis is readily accomplished and is now a viable and successful industrial process. Diamonds produced by shock wave are very small (approximately 60mu). Therefore this diamond is limited to applications such as polishing compounds only. The quality, quantity, size and morphology of the crystals synthesized by catalyst-solvent process depend on different conditions employed for synthesis. These details, because of commercial reasons are not disclosed in published literature. Hence, systematic studies have been planned to investigate the effect of various growth parameters on the synthesized crystals. During the growth of synthetic diamond crystals, some catalyst-solvent is retained into the crystals in some form and behaves like an impurity. Several physico-mechanical properties of the crystals are found to depend on the total quantity and distribution of these inclusions. Thus, detailed investigation of the crystallization medium and inclusions in synthesized diamonds was also undertaken in the present work. The work incorporated in this thesis has been divided into seven chapters. The first

  15. High-pressure-high-temperature treatment of natural diamonds

    CERN Document Server

    Royen, J V

    2002-01-01

    The results are reported of high-pressure-high-temperature (HPHT) treatment experiments on natural diamonds of different origins and with different impurity contents. The diamonds are annealed in a temperature range up to 2000 sup o C at stabilizing pressures up to 7 GPa. The evolution is studied of different defects in the diamond crystal lattice. The influence of substitutional nitrogen atoms, plastic deformation and the combination of these is discussed. Diamonds are characterized at room and liquid nitrogen temperature using UV-visible spectrophotometry, Fourier transform infrared spectrophotometry and photoluminescence spectrometry. The economic implications of diamond HPHT treatments are discussed.

  16. Shock-induced synthesis of high temperature superconducting materials

    Science.gov (United States)

    Ginley, D.S.; Graham, R.A.; Morosin, B.; Venturini, E.L.

    1987-06-18

    It has now been determined that the unique features of the high pressure shock method, especially the shock-induced chemical synthesis technique, are fully applicable to high temperature superconducting materials. Extraordinarily high yields are achievable in accordance with this invention, e.g., generally in the range from about 20% to about 99%, often in the range from about 50% to about 90%, lower and higher yields, of course, also being possible. The method of this invention involves the application of a controlled high pressure shock compression pulse which can be produced in any conventional manner, e.g., by detonation of a high explosive material, the impact of a high speed projectile or the effect of intense pulsed radiation sources such as lasers or electron beams. Examples and a discussion are presented.

  17. Low temperature synthesis of InP nanocrystals

    Energy Technology Data Exchange (ETDEWEB)

    Ung Thi Dieu Thuy [Institute of Materials Science (IMS), Vietnamese Academy of Science and Technology (VAST), 18 Hoang Quoc Viet, Cau Giay, Hanoi (Viet Nam); Tran Thi Thuong Huyen [Institute of Materials Science (IMS), Vietnamese Academy of Science and Technology (VAST), 18 Hoang Quoc Viet, Cau Giay, Hanoi (Viet Nam); National University of Thai Nguyen, 2 Luong Ngoc Quyen, Thai Nguyen (Viet Nam); Nguyen Quang Liem [Institute of Materials Science (IMS), Vietnamese Academy of Science and Technology (VAST), 18 Hoang Quoc Viet, Cau Giay, Hanoi (Viet Nam)], E-mail: liemnq@ims.vast.ac.vn; Reiss, Peter [DSM/INAC/SPrAM, UMR 5819 CEA-CNRS-Universite Joseph Fourier/LEMOH, CEA Grenoble, 17 rue des Martyrs, 38054 Grenoble Cedex 9 (France)

    2008-12-20

    We present a simple method for the chemical synthesis of InP nanocrystals, which comprises several advantages: (i) the use of simple reagents, namely InCl{sub 3}.4H{sub 2}O and yellow P as the In and P precursors, respectively, and NaBH{sub 4} as the reducing agent in a mixed solvent of ethanol and toluene; (ii) a short reaction time (1-5 h) and low temperature (<75 deg. C); (iii) a high reaction yield approaching 100%. InP NCs in the zinc-blende structure have been obtained as confirmed by powder X-ray diffraction and Raman scattering measurements. Their mean size of 4 nm has been determined by transmission electron microscopy, Raman scattering and absorption spectroscopy.

  18. Low temperature synthesis of InP nanocrystals

    International Nuclear Information System (INIS)

    Ung Thi Dieu Thuy; Tran Thi Thuong Huyen; Nguyen Quang Liem; Reiss, Peter

    2008-01-01

    We present a simple method for the chemical synthesis of InP nanocrystals, which comprises several advantages: (i) the use of simple reagents, namely InCl 3 .4H 2 O and yellow P as the In and P precursors, respectively, and NaBH 4 as the reducing agent in a mixed solvent of ethanol and toluene; (ii) a short reaction time (1-5 h) and low temperature (<75 deg. C); (iii) a high reaction yield approaching 100%. InP NCs in the zinc-blende structure have been obtained as confirmed by powder X-ray diffraction and Raman scattering measurements. Their mean size of 4 nm has been determined by transmission electron microscopy, Raman scattering and absorption spectroscopy

  19. Room and low temperature synthesis of carbon nanofibres

    International Nuclear Information System (INIS)

    Boskovic, Bojan O.

    2002-01-01

    Carbon nanotubes and nanofibres have attracted attention in recent years as new materials with a number of very promising potential applications. Carbon nanotubes are potential candidates for field emitters in flat panel displays. Carbon nanofibres could also be used as a hydrogen storage material and as a filling material in polymer composites. Carbon nanotubes are already used as tips in scanning probe microscopy due to their remarkable mechanical and electrical properties, and could be soon used as nanotweezers. Use of carbon nanotubes in nanoelectronics will open further miniaturisation prospects. Temperatures ranging from 450 to 1000 deg C have been a required for catalytic growth of carbon nanotubes and nanofibres. Researchers have been trying to reduce the growth temperatures for decades. Low temperature growth conditions will allow the growth of carbon nanotubes on different substrates, such glass (below 650 deg C) and as plastics (below 150 deg C) over relatively large areas, which is especially suitable for fiat panel display applications. Room temperature growth conditions could open up the possibility of using different organic substrates and bio-substrates for carbon nanotubes synthesis. Carbon nanofibres have been synthesised at room temperature and low temperatures below 250 deg C using radio frequency plasma enhanced chemical vapour deposition (r.f. PECVD). Previously, the growth of carbon nanofibres has been via catalytic decomposition of hydrocarbons or carbon monoxide at temperatures above 300 deg C. To the best of our knowledge, this is the first evidence of the growth of carbon nanofibres at temperatures lower than 300 deg C by any method. The use of a transition metal catalyst and r.f.-PECVD system is required for the growth of the carbon nanofibre when a hydrocarbon flows above the catalyst. Within the semiconductor industry r.f.-PECVD is a well established technique which lends itself for the growth of carbon nanofibres for various

  20. Room temperature synthesis and high temperature frictional study of silver vanadate nanorods.

    Science.gov (United States)

    Singh, D P; Polychronopoulou, K; Rebholz, C; Aouadi, S M

    2010-08-13

    We report the room temperature (RT) synthesis of silver vanadate nanorods (consisting of mainly beta-AgV O(3)) by a simple wet chemical route and their frictional study at high temperatures (HT). The sudden mixing of ammonium vanadate with silver nitrate solution under constant magnetic stirring resulted in a pale yellow coloured precipitate. Structural/microstructural characterization of the precipitate through x-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) revealed the high yield and homogeneous formation of silver vanadate nanorods. The length of the nanorods was 20-40 microm and the thickness 100-600 nm. The pH variation with respect to time was thoroughly studied to understand the formation mechanism of the silver vanadate nanorods. This synthesis process neither demands HT, surfactants nor long reaction time. The silver vanadate nanomaterial showed good lubrication behaviour at HT (700 degrees C) and the friction coefficient was between 0.2 and 0.3. HT-XRD revealed that AgV O(3) completely transformed into silver vanadium oxide (Ag(2)V(4)O(11)) and silver with an increase in temperature from RT to 700 degrees C.

  1. Room temperature synthesis and high temperature frictional study of silver vanadate nanorods

    Energy Technology Data Exchange (ETDEWEB)

    Singh, D P; Aouadi, S M [Department of Physics, Southern Illinois University, Carbondale-62901 (United States); Polychronopoulou, K [Department of Chemistry, University of Cyprus, Nicosia, 1678 (Cyprus); Rebholz, C, E-mail: dineshpsingh@gmail.com, E-mail: saouadi@physics.siu.edu [Department of Mechanical and Manufacturing Engineering, University of Cyprus, Nicosia, 1678 (Cyprus)

    2010-08-13

    We report the room temperature (RT) synthesis of silver vanadate nanorods (consisting of mainly {beta}-AgV O{sub 3}) by a simple wet chemical route and their frictional study at high temperatures (HT). The sudden mixing of ammonium vanadate with silver nitrate solution under constant magnetic stirring resulted in a pale yellow coloured precipitate. Structural/microstructural characterization of the precipitate through x-ray diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM) revealed the high yield and homogeneous formation of silver vanadate nanorods. The length of the nanorods was 20-40 {mu}m and the thickness 100-600 nm. The pH variation with respect to time was thoroughly studied to understand the formation mechanism of the silver vanadate nanorods. This synthesis process neither demands HT, surfactants nor long reaction time. The silver vanadate nanomaterial showed good lubrication behaviour at HT (700 deg. C) and the friction coefficient was between 0.2 and 0.3. HT-XRD revealed that AgV O{sub 3} completely transformed into silver vanadium oxide (Ag{sub 2}V{sub 4}O{sub 11}) and silver with an increase in temperature from RT to 700 deg. C.

  2. Protein synthesis during the initial phase of the temperature-induced bleaching response in Euglena gracilis

    International Nuclear Information System (INIS)

    Ortiz, W.

    1990-01-01

    Growing cultures of photoheterotrophic Euglena gracilis experience an increase in chlorophyll accumulation during the initial phase of the temperature-induced bleaching response suggesting an increase in the synthesis of plastid components at the bleaching temperature of 33 degree C. A primary goal of this work was to establish whether an increase in the synthesis of plastid proteins accompanies the observed increase in chlorophyll accumulation. In vivo pulse-labeling experiments with [ 35 S]sodium sulfate were carried out with cells grown at room temperature or at 33 degree C. The synthesis of a number of plastid polypeptides of nucleocytoplasmic origin, including some presumably novel polypeptides, increased in cultures treated for 15 hours at 33 degree C. In contrast, while synthesis of thylakoid proteins by the plastid protein synthesis machinery decreased modestly, synthesis of the large subunit of the enzyme ribulosebisphosphate carboxylase was strongly affected at the elevated temperature. Synthesis of novel plastid-encoded polypeptides was not induced at the bleaching temperature. It is concluded that protein synthesis in plastids declines during the initial phase of the temperature response in Euglena despite an overall increase in cellular protein synthesis and an increase in chlorophyll accumulation per cell

  3. Synthesis of manganese spinel nanoparticles at room temperature by coprecipitation

    Energy Technology Data Exchange (ETDEWEB)

    Giovannelli, F., E-mail: fabien.giovannelli@univ-tours.fr [GREMAN, UMR 7347 CNRS-CEA, Universite Francois Rabelais, 15 rue de la chocolaterie, 41000 BLOIS (France); Autret-Lambert, C.; Mathieu, C.; Chartier, T.; Delorme, F. [GREMAN, UMR 7347 CNRS-CEA, Universite Francois Rabelais, 15 rue de la chocolaterie, 41000 BLOIS (France); Seron, A [BRGM, 3 Avenue Claude Guillemin, BP 36009, 45060 ORLEANS Cedex 2 (France)

    2012-08-15

    This paper is focused on a new route to synthesize Mn{sub 3}O{sub 4} nanoparticles by alkalisation by sodium hydroxide on a manganeous solution at room temperature. The precipitates obtained at different pH values have been characterized by XRD and TEM. Since the first addition of sodium hydroxide, a white Mn(OH){sub 2} precipitate appears. At pH=7, {gamma}-MnOOH phase is predominant with needle like shaped particles. At pH=10, hausmanite nanoparticles, which exhibits well defined cubic shape in the range 50-120 nm are obtained. This new precipitation route is a fast and easy environmentally friendly process to obtain well crystallized hausmanite nanoparticles. - Graphical abstract: TEM image showing Mn{sub 3}O{sub 4} particles after a precipitation at pH=10. Highlights: Black-Right-Pointing-Pointer A new route to synthesize Mn{sub 3}O{sub 4} nanoparticles has been demonstrated. Black-Right-Pointing-Pointer Synthesis has been performed by precipitation at room temperature. Black-Right-Pointing-Pointer The size of the Mn{sub 3}O{sub 4} nanoparticles is between 50 and 120 nm.

  4. Synthesis and characterization of strontium carboxylates at room temperature and at high temperature in autoclave vessels

    DEFF Research Database (Denmark)

    Christgau, Stephan; Ståhl, Kenny; Andersen, Jens Enevold Thaulov

    2006-01-01

    A novel method was developed for synthesis of strontium coordination compounds in high yields. The synthesis proceeded along three pathways that provided strontium salts in high purity and high yields, close to 100%, as confirmed by flame atomic absorption spectroscopy (FAAS) and powder x......-ray crystallography. Optimum conditions were found at T = 120-1400C, a base-to-acid ratio of 1.2 and 15 min. of reaction-time in an autoclave vessel. Large crystals were readily obtained within a time period of hours. The crystal structures of strontium D-glutamate hexahydrate (I) and strontium di-(hydrogen L......-glutamate) pentahydrate (II) were confirmed by X-ray powder diffraction at 295 K and Rietveld refinements (I: Space group P212121, Z=4, a=7.3519(2), b=8.7616(2), c=20.2627(5) Å, and II: Space group P21, Z=2, a=8.7243(1), b=7.2635(1), c=14.6840(2) Å, β=100.5414(7) °). Synthesis at room temperature provided four additional...

  5. Hardness of high-pressure high-temperature treated single-walled carbon nanotubes

    International Nuclear Information System (INIS)

    Kawasaki, S.; Nojima, Y.; Yokomae, T.; Okino, F.; Touhara, H.

    2007-01-01

    We have performed high-pressure high-temperature (HPHT) treatments of high quality single-walled carbon nanotubes (SWCNTs) over a wide pressure-temperature range up to 13 GPa-873 K and have investigated the hardness of the HPHT-treated SWCNTs using a nanoindentation technique. It was found that the hardness of the SWCNTs treated at pressures greater than 11 GPa and at temperatures higher than 773 K is about 10 times greater than that of the SWCNTs treated at low temperature. It was also found that the hardness change of the SWCNTs is related to the structural change by the HPHT treatments which was based on synchrotron X-ray diffraction measurements

  6. 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.

  7. Carvacrol suppresses high pressure high temperature inactivation of Bacillus cereus spores.

    Science.gov (United States)

    Luu-Thi, Hue; Corthouts, Jorinde; Passaris, Ioannis; Grauwet, Tara; Aertsen, Abram; Hendrickx, Marc; Michiels, Chris W

    2015-03-16

    The inactivation of bacterial spores generally proceeds faster and at lower temperatures when heat treatments are conducted under high pressure, and high pressure high temperature (HPHT) processing is, therefore, receiving an increased interest from food processors. However, the mechanisms of spore inactivation by HPHT treatment are poorly understood, particularly at moderately elevated temperature. In the current work, we studied inactivation of the spores of Bacillus cereus F4430/73 by HPHT treatment for 5 min at 600MPa in the temperature range of 50-100°C, using temperature increments of 5°C. Additionally, we investigated the effect of the natural antimicrobial carvacrol on spore germination and inactivation under these conditions. Spore inactivation by HPHT was less than about 1 log unit at 50 to 70°C, but gradually increased at higher temperatures up to about 5 log units at 100°C. DPA release and loss of spore refractility in the spore population were higher at moderate (≤65°C) than at high (≥70°C) treatment temperatures, and we propose that moderate conditions induced the normal physiological pathway of spore germination resulting in fully hydrated spores, while at higher temperatures this pathway was suppressed and replaced by another mechanism of pressure-induced dipicolinic acid (DPA) release that results only in partial spore rehydration, probably because spore cortex hydrolysis is inhibited. Carvacrol strongly suppressed DPA release and spore rehydration during HPHT treatment at ≤65°C and also partly inhibited DPA release at ≥65°C. Concomitantly, HPHT spore inactivation was reduced by carvacrol at 65-90°C but unaffected at 95-100°C. Copyright © 2014 Elsevier B.V. All rights reserved.

  8. Differential chromosomal and mitochondrial DNA synthesis in temperature-sensitive mutants of Ustilago maydis

    Energy Technology Data Exchange (ETDEWEB)

    Unrau, P.

    1977-01-01

    The amount and type of residual DNA synthesis was determined in eight temperature-sensitive mutants of the smut fungus Ustilago maydis after incubation at the restrictive temperature (32/sup 0/C) for eight hours. Mutants ts-220, ts-207, ts-432 and ts-346 were found to have an overall reduction in the synthesis of both nuclear and mitochondrial DNA in comparison to the wild-type. In mutants ts-20, tsd 1-1, ts-84 and pol 1-1 nuclear DNA synthesis was depressed relative to mitochondrial synthesis. The DNA-polymerase mutant pol 1-1 had persistent nuclear synthesis at about 50% of the rate of synthesis of mitochondrial DNA and similar behavior was observed in a diploid homozygous strain. Mutant ts-84 had an initial burst of DNA synthesis which was reduced for nuclear but not mitochondrial synthesis after three hours preincubation at 32/sup 0/C. tsd 1-1 and ts-20 had nuclear residual synthesis amounting to about 25% of the relative rate of mitochondrial synthesis which correlates to increasing UV sensitivity of these strains on incubation at 32/sup 0/C. A pol 1-1 ts-84 double mutant had an additive loss of nuclear DNA synthesis which indicates that the steps of replication involved may be sequential.

  9. Self-sustained high-temperature reactions : Initiation, propagation and synthesis

    NARCIS (Netherlands)

    Martinez Pacheco, M.

    2007-01-01

    Self-Propagating High-Temperature Synthesis (SHS), also called combustion synthesis is an exothermic and self-sustained reaction between the constituents, which has assumed significance for the production of ceramics and ceramic-metallic materials (cermets), because it is a very rapid processing

  10. Room temperature synthesis of protonated layered titanate sheets using peroxo titanium carbonate complex solution.

    Science.gov (United States)

    Sutradhar, Narottam; Sinhamahapatra, Apurba; Pahari, Sandip Kumar; Bajaj, Hari C; Panda, Asit Baran

    2011-07-21

    We report the synthesis of peroxo titanium carbonate complex solution as a novel water-soluble precursor for the direct synthesis of layered protonated titanate at room temperature. The synthesized titanates showed excellent removal capacity for Pb(2+) and methylene blue. Based on experimental observations, a probable mechanism for the formation of protonated layered dititanate sheets is also discussed.

  11. 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.

  12. 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

  13. Required developments towards ultra high pressure and temperature subsea tree system solutions

    Energy Technology Data Exchange (ETDEWEB)

    Queseth, Per-Olaf

    2010-07-01

    For the subsea High Pressure High Temperature oil and gas production systems, the primary challenge is to provide good, reliable solutions for HPHT reservoir exploitation based on an overview of parameters for already discovered potential fields. The paper will present a resume of Aker Solutions' previous development in this area exemplified with experiences from testing and operator observations during production start of HPHT fields in the North Sea. Further improvements are required to comply with the extreme pressures and temperatures sought to overcome. 'The Devil is in the details' is a very relevant proverb. A program to qualify subsea production X-mas trees for Ultra HPHT use will be presented with highlight on sealing systems, feed-through solutions and materials as well as impact on interfacing systems. Preliminary and intermediate analytical and test results will be presented and remaining activities summarised. (Author)

  14. XPS analysis for cubic boron nitride crystal synthesized under high pressure and high temperature using Li3N as catalysis

    International Nuclear Information System (INIS)

    Guo, Xiaofei; Xu, Bin; Zhang, Wen; Cai, Zhichao; Wen, Zhenxing

    2014-01-01

    Highlights: • The cBN was synthesized by Li 3 N as catalyst under high pressure and high temperature (HPHT). • The film coated on the as-grown cBN crystals was studied by XPS. • The electronic structure variation in the film was investigated. • The growth mechanism of cubic boron nitride crystal was analyzed briefly. - Abstract: Cubic boron nitride (cBN) single crystals are synthesized with lithium nitride (Li3N) as catalyst under high pressure and high temperature. The variation of electronic structures from boron nitride of different layers in coating film on the cBN single crystal has been investigated by X-ray photoelectron spectroscopy. Combining the atomic concentration analysis, it was shown that from the film/cBN crystal interface to the inner, the sp 2 fractions are decreasing, and the sp 3 fractions are increasing in the film at the same time. Moreover, by transmission electron microscopy, a lot of cBN microparticles are found in the interface. For there is no Li 3 N in the film, it is possible that Li 3 N first reacts with hexagonal boron nitride to produce Li 3 BN 2 during cBN crystals synthesis under high pressure and high temperature (HPHT). Boron and nitrogen atoms, required for cBN crystals growth, could come from the direct conversion from hexagonal boron nitride with the catalysis of Li 3 BN 2 under high pressure and high temperature, but not directly from the decomposition of Li 3 BN 2

  15. Kinetics of the ammonia synthesis at low temperatures. II. Sources of discrepancies

    International Nuclear Information System (INIS)

    Kuchaev, V.L.; Shapatina, E.N.; Temkin, M.I.

    1988-01-01

    A method is developed for calculating the degree of conversion during the synthesis of ammonia in a continuous flow, tubular reactor, taking longitudinal diffusion into account. Such a calculation shows that the available data in the literature on the rate of ammonia synthesis at low temperatures in a tubular reactor agree with the rate equation based on the idea that the predominant intermediate substance is adsorbed ammonia (and not imide). The seeming conflict between this idea and the ratio of the rates of synthesis of ammonia and deuteroammonia at low temperatures is explained

  16. Development of coating technology for nuclear fuel by self-propagating high temperature synthesis

    International Nuclear Information System (INIS)

    Choi, Y.; Kim, Bong G.; Lee, Y. W.

    1997-01-01

    This paper presents experimental results of the preparation of silicon carbide and graphite layers on a nuclear fuel from silane and propane gases by a conventional chemical vapor deposition and combustion synthesis technologies. The direct reaction between silicon and pyrolytic carbon in a high temperature releases sufficient amount of energy to make a synthesis self-sustaining under the preheating of about 1200 deg C. During this high temperature process, lamellar structure with isotropic carbon synthesis. A full characterization of phase composition and final morphology of the coated layers by X-ray diffraction, SEM and AES is presented. (author). 6 refs., 1 tab., 11 figs

  17. Self-propagating high-temperature synthesis of nonstoichiometric wuestite

    Energy Technology Data Exchange (ETDEWEB)

    Hiramoto, Maki [Graduate School of Engineering, Hokkaido University, Sapporo 060-8628 (Japan); Okinaka, Noriyuki [Center for Advanced Research of Energy and Materials, Faculty of Engineering, Hokkaido University, Sapporo 060-8628 (Japan); Akiyama, Tomohiro, E-mail: takiyama@eng.hokudai.ac.jp [Center for Advanced Research of Energy and Materials, Faculty of Engineering, Hokkaido University, Sapporo 060-8628 (Japan)

    2012-04-15

    Highlights: Black-Right-Pointing-Pointer The manuscript describes an SHS method of producing Fe{sub x}O. Black-Right-Pointing-Pointer Focus on the effects of nonstoichiometric Fe content and diluent addition on the phase of the SHS product. Black-Right-Pointing-Pointer Without the NaCl diluent, the lattice parameter of SHS Fe{sub 0.947}O corresponded to the theoretical lattice parameter. Black-Right-Pointing-Pointer Nonstoichiometric compounds of Fe{sub x}O (0.942 {<=} x {<=} 0.952) were obtained through SHS without additional external heating. - Abstract: This paper describes the self-propagating high-temperature synthesis (SHS) of nonstoichiometric Fe{sub x}O (x = 0.833-1), with particular focus on the effects of nonstoichiometric Fe content and diluent addition on the phase of the SHS product. In the SHS process, the raw materials Fe, NaClO{sub 4} (oxidizer), and NaCl (diluent) were thoroughly mixed in the desired ratio by ball milling, and the lower surfaces of the disk-shaped green compacts were subsequently electrically ignited to produce Fe{sub x}O through the propagation of the sustainable exothermic reaction. X-ray diffraction analysis showed that the SHS products comprised double phases of Fe{sub x}O and Fe{sub 3}O{sub 4}. The peaks of products with 0.947 {<=} x {<=} 1.00 shifted to lower angles in comparison to those of the product with x = 0.833 attributed to the lattice parameter distortion of the crystal structure because of the Fe defects. In the presence of the NaCl diluent, the raw materials were converted to high-purity Fe{sub x}O powders during the SHS process. Without the NaCl diluent, the lattice parameter of SHS Fe{sub 0.947}O corresponded to the theoretical lattice parameter. Nonstoichiometric compounds of Fe{sub x}O (0.942 {<=} x {<=} 0.952) were obtained through SHS without additional external heating.

  18. ROOM TEMPERATURE BULK SYNTHESIS OF SILVER NANOCABLES WRAPPED WITH POLYPYRROLE

    Science.gov (United States)

    Wet chemical synthesis of silver cables wrapped with polypyrrole is reported in aqueous media without use of any surfactant/capping agent and/or template. The method employs direct polymerization of pyrrole of an aqueous solution with AgNO3 as an oxidizing agent. The four probe c...

  19. Modelling of flame temperature of solution combustion synthesis of ...

    Indian Academy of Sciences (India)

    Administrator

    The basis of combustion synthesis technique comes from the ... of oxidizer to fuel is calculated using the total oxidizing ..... +. −. ∑. (4) where S/Nm is the mean S/N ratio of all the experimental ..... Minitab Inc., User manual of MINITAB. TM.

  20. The effect of temperature in flux-assisted synthesis of SnNb2O6

    KAUST Repository

    Noureldine, Dalal; Takanabe, Kazuhiro

    2014-01-01

    A flux-assisted method was used to synthesize SnNb2O6 as a visible-light-responsive metal oxide photocatalyst. The role of synthesis temperature was investigated in detail using different reaction temperatures (300, 500, 600, 800, 1000 °C

  1. Application of low-temperature plasma for the synthesis of hydrogenated graphene (graphane)

    Science.gov (United States)

    Shavelkina, M. B.; Amirov, R. H.; Katarzhis, V. A.; Kiselev, V. I.

    2017-12-01

    The possibility of a direct synthesis of hydrogenated graphene in decomposition of methane by means of low-temperature plasma was investigated. A DC plasma torch with an expanding channel-anode, a vortex gas supply and a self-setting arc length was used as a generator of low-temperature plasma. Argon was used as the plasma-forming gas. The temperatures of argon plasma and with methane addition to it were determined on the basis of spectral measurements. The synthesis products were characterized by electron microscopy and thermogravimetry. The effect of hydrogenated graphene as a nanomodifier on the properties of the cubic boron nitride based functional ceramics was investigated.

  2. Influence of air annealing on the luminescence dynamics of HPHT nanodiamonds

    Czech Academy of Sciences Publication Activity Database

    Salava, J.; Trojánek, F.; Stehlík, Štěpán; Varga, Marián; Rezek, Bohuslav; Malý, P.

    2016-01-01

    Roč. 68, Sep (2016), s. 62-65 ISSN 0925-9635 R&D Projects: GA ČR GA15-01809S Institutional support: RVO:68378271 Keywords : nanodiamond * time-resolved spectroscopy * annealing * carrier dynamics * high-pressure high-temperature nanodiamonds Subject RIV: BH - Optics, Masers, Lasers Impact factor: 2.561, year: 2016

  3. 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

  4. Precise estimation of HPHT nanodiamond size distribution based on transmission electron microscopy image analysis

    Czech Academy of Sciences Publication Activity Database

    Řehoř, Ivan; Cígler, Petr

    2014-01-01

    Roč. 46, Jun (2014), s. 21-24 ISSN 0925-9635 R&D Projects: GA ČR GAP108/12/0640; GA MŠk(CZ) LH11027 Grant - others:OPPK(CZ) CZ.2.16/3.1.00/24016 Institutional support: RVO:61388963 Keywords : TEM * nanoparticles * nanodiamonds * size distribution * high-pressure high-temperature * image analysis Subject RIV: CC - Organic Chemistry Impact factor: 1.919, year: 2014

  5. Room temperature growth of ZnO nanorods by hydrothermal synthesis

    Science.gov (United States)

    Tateyama, Hiroki; Zhang, Qiyan; Ichikawa, Yo

    2018-05-01

    The effect of seed layer morphology on ZnO nanorod growth at room temperature was studied via hydrothermal synthesis on seed layers with different thicknesses and further annealed at different temperatures. The change in the thickness and annealing temperature enabled us to control over a diameter of ZnO nanorods which are attributed to the changing of crystallinity and roughness of the seed layers.

  6. The flavoprotein Tah18-dependent NO synthesis confers high-temperature stress tolerance on yeast cells

    Energy Technology Data Exchange (ETDEWEB)

    Nishimura, Akira; Kawahara, Nobuhiro [Graduate School of Biological Sciences, Nara Institute of Science and Technology, 8916-5 Takayama, Ikoma, Nara 630-0192 (Japan); Takagi, Hiroshi, E-mail: hiro@bs.naist.jp [Graduate School of Biological Sciences, Nara Institute of Science and Technology, 8916-5 Takayama, Ikoma, Nara 630-0192 (Japan)

    2013-01-04

    Highlights: Black-Right-Pointing-Pointer NO is produced from L-arginine in response to elevated temperature in yeast. Black-Right-Pointing-Pointer Tah18 was first identified as the yeast protein involved in NO synthesis. Black-Right-Pointing-Pointer Tah18-dependent NO synthesis confers tolerance to high-temperature on yeast cells. -- Abstract: Nitric oxide (NO) is a ubiquitous signaling molecule involved in the regulation of a large number of cellular functions. In the unicellular eukaryote yeast, NO may be involved in stress response pathways, but its role is poorly understood due to the lack of mammalian NO synthase (NOS) orthologues. Previously, we have proposed the oxidative stress-induced L-arginine synthesis and its physiological role under stress conditions in yeast Saccharomyces cerevisiae. Here, our experimental results indicated that increased conversion of L-proline into L-arginine led to NO production in response to elevated temperature. We also showed that the flavoprotein Tah18, which was previously reported to transfer electrons to the Fe-S cluster protein Dre2, was involved in NO synthesis in yeast. Gene knockdown analysis demonstrated that Tah18-dependent NO synthesis confers high-temperature stress tolerance on yeast cells. As it appears that such a unique cell protection mechanism is specific to yeasts and fungi, it represents a promising target for antifungal activity.

  7. The flavoprotein Tah18-dependent NO synthesis confers high-temperature stress tolerance on yeast cells

    International Nuclear Information System (INIS)

    Nishimura, Akira; Kawahara, Nobuhiro; Takagi, Hiroshi

    2013-01-01

    Highlights: ► NO is produced from L-arginine in response to elevated temperature in yeast. ► Tah18 was first identified as the yeast protein involved in NO synthesis. ► Tah18-dependent NO synthesis confers tolerance to high-temperature on yeast cells. -- Abstract: Nitric oxide (NO) is a ubiquitous signaling molecule involved in the regulation of a large number of cellular functions. In the unicellular eukaryote yeast, NO may be involved in stress response pathways, but its role is poorly understood due to the lack of mammalian NO synthase (NOS) orthologues. Previously, we have proposed the oxidative stress-induced L-arginine synthesis and its physiological role under stress conditions in yeast Saccharomyces cerevisiae. Here, our experimental results indicated that increased conversion of L-proline into L-arginine led to NO production in response to elevated temperature. We also showed that the flavoprotein Tah18, which was previously reported to transfer electrons to the Fe–S cluster protein Dre2, was involved in NO synthesis in yeast. Gene knockdown analysis demonstrated that Tah18-dependent NO synthesis confers high-temperature stress tolerance on yeast cells. As it appears that such a unique cell protection mechanism is specific to yeasts and fungi, it represents a promising target for antifungal activity.

  8. Product engineering by high-temperature flame synthesis

    DEFF Research Database (Denmark)

    Johannessen, Tue; Johansen, Johnny; Mosleh, Majid

    product gas can be applied directly in additional product engineering concepts. A brief overview of on-going product developments and product engineering projects is outlined below. These projects, which are all founded on flame synthesis of nano-structured materials, include: • Preparation of catalyzed...... hardware by direct deposition of catalysts on process equipment • Modifications of the substrate surfaces to obtain good adhesion during flame-coating • Formation of membrane layers by gas-phase deposition of nano-particles • Catalyst deposition in micro-reactors for rapid catalyst screening...

  9. Low Temperature Synthesis and Properties of Gadolinium-Doped Cerium Oxide Nanoparticles

    DEFF Research Database (Denmark)

    Machado, Marina F. S.; P. R. Moraes, Leticia; Monteiro, Natalia K.

    2017-01-01

    Gadolinium-doped cerium oxide (GDC) is an attractive ceramic material for solid oxide fuel cells (SOFCs) both as the electrolyte or in composite electrodes. The Ni/GDC cermet can be tuned as a catalytic layer, added to the conventional Ni/yttria-stabilized zirconia (YSZ), for the internal steam...... sintering temperature needed to obtain a fully dense ceramic body, which can result in undesired reactions with YSZ. In this study, a green chemistry route for the synthesis of 10 mol% GDC nanoparticles is proposed. Such a low temperature synthesis provides control over particle size and sinterability...

  10. Process assessment of small scale low temperature methanol synthesis

    Energy Technology Data Exchange (ETDEWEB)

    Hendriyana [Chemical Engineering Department, Faculty of Engineering, Jenderal Achmad Yani Univerity (Indonesia); Chemical Engineering Department, Faculty of Industrial Technology, InstitutTeknologi Bandung (Indonesia); Susanto, Herri, E-mail: herri@che.itb.ac.id; Subagjo [Chemical Engineering Department, Faculty of Industrial Technology, InstitutTeknologi Bandung (Indonesia)

    2015-12-29

    Biomass is a renewable energy resource and has the potential to make a significant impact on domestic fuel supplies. Biomass can be converted to fuel like methanol via several step process. The process can be split into following main steps: biomass preparation, gasification, gas cooling and cleaning, gas shift and methanol synthesis. Untill now these configuration still has a problem like high production cost, catalyst deactivation, economy of scale and a huge energy requirements. These problems become the leading inhibition for biomass conversion to methanol, which should be resolved to move towards the economical. To address these issues, we developed various process and new configurations for methanol synthesis via methyl formate. This configuration combining two reactors: the one reactor for the carbonylation of methanol and CO to form methyl formate, and the second for the hydrogenolysis of methyl formate and H{sub 2} to form two molecule of methanol. Four plant process configurations were compared with the biomass basis is 300 ton/day. The first configuration (A) is equipped with a steam reforming process for converting methane to CO and H{sub 2} for increasing H{sub 2}/CO ratio. CO{sub 2} removal is necessary to avoid poisoning the catalyst. COSORB process used for the purpose of increasing the partial pressure of CO in the feed gas. The steam reforming process in B configuration is not used with the aim of reducing the number of process equipment, so expect lower investment costs. For C configuration, the steam reforming process and COSORB are not used with the aim of reducing the number of process equipment, so expect lower investment costs. D configuration is almost similar to the configuration A. This configuration difference is in the synthesis of methanol which was held in a single reactor. Carbonylation and hydrogenolysis reactions carried out in the same reactor one. These processes were analyzed in term of technical process, material and energy

  11. Process assessment of small scale low temperature methanol synthesis

    International Nuclear Information System (INIS)

    Hendriyana; Susanto, Herri; Subagjo

    2015-01-01

    Biomass is a renewable energy resource and has the potential to make a significant impact on domestic fuel supplies. Biomass can be converted to fuel like methanol via several step process. The process can be split into following main steps: biomass preparation, gasification, gas cooling and cleaning, gas shift and methanol synthesis. Untill now these configuration still has a problem like high production cost, catalyst deactivation, economy of scale and a huge energy requirements. These problems become the leading inhibition for biomass conversion to methanol, which should be resolved to move towards the economical. To address these issues, we developed various process and new configurations for methanol synthesis via methyl formate. This configuration combining two reactors: the one reactor for the carbonylation of methanol and CO to form methyl formate, and the second for the hydrogenolysis of methyl formate and H 2 to form two molecule of methanol. Four plant process configurations were compared with the biomass basis is 300 ton/day. The first configuration (A) is equipped with a steam reforming process for converting methane to CO and H 2 for increasing H 2 /CO ratio. CO 2 removal is necessary to avoid poisoning the catalyst. COSORB process used for the purpose of increasing the partial pressure of CO in the feed gas. The steam reforming process in B configuration is not used with the aim of reducing the number of process equipment, so expect lower investment costs. For C configuration, the steam reforming process and COSORB are not used with the aim of reducing the number of process equipment, so expect lower investment costs. D configuration is almost similar to the configuration A. This configuration difference is in the synthesis of methanol which was held in a single reactor. Carbonylation and hydrogenolysis reactions carried out in the same reactor one. These processes were analyzed in term of technical process, material and energy balance and economic

  12. Synthesis of ammonia directly from air and water at ambient temperature and pressure

    Science.gov (United States)

    Lan, Rong; Irvine, John T. S.; Tao, Shanwen

    2013-01-01

    The N≡N bond (225 kcal mol−1) in dinitrogen is one of the strongest bonds in chemistry therefore artificial synthesis of ammonia under mild conditions is a significant challenge. Based on current knowledge, only bacteria and some plants can synthesise ammonia from air and water at ambient temperature and pressure. Here, for the first time, we report artificial ammonia synthesis bypassing N2 separation and H2 production stages. A maximum ammonia production rate of 1.14 × 10−5 mol m−2 s−1 has been achieved when a voltage of 1.6 V was applied. Potentially this can provide an alternative route for the mass production of the basic chemical ammonia under mild conditions. Considering climate change and the depletion of fossil fuels used for synthesis of ammonia by conventional methods, this is a renewable and sustainable chemical synthesis process for future. PMID:23362454

  13. Synthesis of ammonia directly from air and water at ambient temperature and pressure.

    Science.gov (United States)

    Lan, Rong; Irvine, John T S; Tao, Shanwen

    2013-01-01

    The N≡N bond (225 kcal mol⁻¹) in dinitrogen is one of the strongest bonds in chemistry therefore artificial synthesis of ammonia under mild conditions is a significant challenge. Based on current knowledge, only bacteria and some plants can synthesise ammonia from air and water at ambient temperature and pressure. Here, for the first time, we report artificial ammonia synthesis bypassing N₂ separation and H₂ production stages. A maximum ammonia production rate of 1.14 × 10⁻⁵ mol m⁻² s⁻¹ has been achieved when a voltage of 1.6 V was applied. Potentially this can provide an alternative route for the mass production of the basic chemical ammonia under mild conditions. Considering climate change and the depletion of fossil fuels used for synthesis of ammonia by conventional methods, this is a renewable and sustainable chemical synthesis process for future.

  14. Room-temperature Electrochemical Synthesis of Carbide-derived Carbons and Related Materials

    Energy Technology Data Exchange (ETDEWEB)

    Gogotsi, Yury [Drexel Univ., Philadelphia, PA (United States). Nanomaterials Group. Materials Science and Engineering Dept.

    2015-02-28

    This project addresses room-temperature electrochemical etching as an energy-efficient route to synthesis of 3D nanoporous carbon networks and layered 2D carbons and related structures, as well as provides fundamental understanding of structure and properties of materials produced by this method. Carbide-derived-carbons (CDCs) are a growing class of nanostructured carbon materials with properties that are desirable for many applications, such as electrical energy and gas storage. The structure of these functional materials is tunable by the choice of the starting carbide precursor, synthesis method, and process parameters. Moving from high-temperature synthesis of CDCs through vacuum decomposition above 1400°C and chlorination above 400°C, our studies under the previous DOE BES support led to identification of precursor materials and processing conditions for CDC synthesis at temperatures as low as 200°C, resulting in amorphous and highly reactive porous carbons. We also investigated synthesis of monolithic CDC films from carbide films at 250-1200°C. The results of our early studies provided new insights into CDC formation, led to development of materials for capacitive energy storage, and enabled fundamental understanding of the electrolyte ions confinement in nanoporous carbons.

  15. A self-propagation high-temperature synthesis and annealing route to synthesis of wave-like boron nitride nanotubes

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Jilin; Zhang, Laiping [School of Materials Science and Engineering, Wuhan Institute of Technology, Wuhan, Hubei, 430073 (China); Gu, Yunle, E-mail: ncm@mail.wit.edu.cn [School of Materials Science and Engineering, Wuhan Institute of Technology, Wuhan, Hubei, 430073 (China); Pan, Xinye; Zhao, Guowei; Zhang, Zhanhui [School of Materials Science and Engineering, Wuhan Institute of Technology, Wuhan, Hubei, 430073 (China)

    2013-03-15

    Highlights: ► Large quantities of wave-like BN nanotubes were synthesized by SHS-annealing method. ► The catalytic boron-containing porous precursor was produced by self-propagation high-temperature synthesis method. ► Three growth models were proposed to explain the growth mechanism of the wave-like BN nanotubes. - Abstract: Large quantities of boron nitride (BN) nanotubes were synthesized by annealing a catalytic boron-containing porous precursor in flowing NH{sub 3} gas at 1180 °C. The porous precursor was prepared by self-propagation high-temperature synthesis (SHS) method at 800 °C using Mg, B{sub 2}O{sub 3} and amorphous boron powder (α-B) as the starting materials. The porous precursor played an important role in large quantities synthesis of BN nanotubes. The as-synthesized product was characterized by X-ray diffractometer (XRD), Fourier transform infrared spectrometer (FTIR), Raman, Scanning electron microscopy (SEM), X-ray energy dispersive spectroscopy (EDS), Transmission electron microscopy (TEM) and High-resolution transmission electron microscopy (HRTEM). Characterization results indicated that the BN nanotubes displayed wave-like inner structures with diameters in the range of 50–300 nm and average lengths of more than 10 μm. The possible growth mechanism of the BN nanotubes was also discussed.

  16. Low-temperature synthesis of graphene on nickel foil by microwave plasma chemical vapor deposition

    International Nuclear Information System (INIS)

    Kim, Y.; Song, W.; Lee, S. Y.; Jeon, C.; Jung, W.; Kim, M.; Park, C.-Y.

    2011-01-01

    Microwave plasma chemical vapor deposition (MPCVD) was employed to synthesize high quality centimeter scale graphene film at low temperatures. Monolayer graphene was obtained by varying the gas mixing ratio of hydrogen and methane to 80:1. Using advantages of MPCVD, the synthesis temperature was decreased from 750 deg. C down to 450 deg. C. Optical microscopy and Raman mapping images exhibited that a large area monolayer graphene was synthesized regardless of the temperatures. Since the overall transparency of 89% and low sheet resistances ranging from 590 to 1855 Ω/sq of graphene films were achieved at considerably low synthesis temperatures, MPCVD can be adopted in manufacturing future large-area electronic devices based on graphene film.

  17. Low-temperature synthesis of graphene on nickel foil by microwave plasma chemical vapor deposition

    Science.gov (United States)

    Kim, Y.; Song, W.; Lee, S. Y.; Jeon, C.; Jung, W.; Kim, M.; Park, C.-Y.

    2011-06-01

    Microwave plasma chemical vapor deposition (MPCVD) was employed to synthesize high quality centimeter scale graphene film at low temperatures. Monolayer graphene was obtained by varying the gas mixing ratio of hydrogen and methane to 80:1. Using advantages of MPCVD, the synthesis temperature was decreased from 750 °C down to 450 °C. Optical microscopy and Raman mapping images exhibited that a large area monolayer graphene was synthesized regardless of the temperatures. Since the overall transparency of 89% and low sheet resistances ranging from 590 to 1855 Ω/sq of graphene films were achieved at considerably low synthesis temperatures, MPCVD can be adopted in manufacturing future large-area electronic devices based on graphene film.

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

    OpenAIRE

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

    2009-01-01

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

  19. The synthesis of [2-13C]2-nitropropane at room temperature and at atmospheric pressure

    NARCIS (Netherlands)

    Jacquemijns M; Zomer G

    1990-01-01

    In this report the synthesis of [2-13C]2-nitropropane at room temperature is described. [2-13C]Acetone was converted into the oxime with hydroxy hydrochloridelamine and sodium carbonate. Treatment with hypobromic acid resulted in 2-13C]2-bromo-2-nitropropane. Hydrogenation with sodium borohydride

  20. Synthesis, structure and low temperature study of electric transport ...

    Indian Academy of Sciences (India)

    1. Introduction. Layered perovskite oxides are a promising group of mixed- conducting materials with potential applications for oxygen- separation membranes, gas sensor devices and electrodes of intermediate-temperature solid oxide fuel cells (Moseley and. Williams 1989; Meixner and Lampe 1996; Skinner and Kil-.

  1. Self-propagating high temperature synthesis and magnetic ...

    Indian Academy of Sciences (India)

    Unknown

    phase composition, microstructure and magnetic properties of the combustion products. The effect ... The size and shapes of the ... Figure 3 shows the effect of combustion temperature on ... ducts at 1200°C are too hard to be ground easily and.

  2. Gold catalysed synthesis of 3-alkoxyfurans at room temperature.

    Science.gov (United States)

    Pennell, Matthew N; Foster, Robert W; Turner, Peter G; Hailes, Helen C; Tame, Christopher J; Sheppard, Tom D

    2014-02-09

    Synthetically important 3-alkoxyfurans can be prepared efficiently via treatment of acetal-containing propargylic alcohols (obtained from the addition of 3,3-diethoxypropyne to aldehydes) with 2 mol% gold catalyst in an alcohol solvent at room temperature. The resulting furans show useful reactivity in a variety of subsequent transformations.

  3. Synthesis of cadmium chalcogenide nanotubes at room temperature

    KAUST Repository

    Pan, Jun

    2012-10-01

    Cadmium chalcogenide (CdE, E=S, Se, Te) polycrystalline nanotubes have been synthesized from precursor of CdS/cadmium thiolate complex at room temperature. The precursor was hydrothermally synthesized at 180 °C using thioglycolic acid (TGA) and cadmium acetate as starting materials. The transformation from the rod-like precursor of CdS/cadmium thiolate complex to CdS, CdSe and CdTe nanotubes were performed under constant stirring at room temperature in aqueous solution containing S 2-, Se 2- and Te 2-, respectively. The nanotube diameter can be controlled from 150 to 400 nm related to the dimension of templates. The XRD patterns show the cadmium chalcogenide nanotubes all corresponding to face-centered cubic structure. © 2012 Elsevier B.V. All rights reserved.

  4. Synthesis of cadmium chalcogenide nanotubes at room temperature

    KAUST Repository

    Pan, Jun; Qian, Yitai

    2012-01-01

    Cadmium chalcogenide (CdE, E=S, Se, Te) polycrystalline nanotubes have been synthesized from precursor of CdS/cadmium thiolate complex at room temperature. The precursor was hydrothermally synthesized at 180 °C using thioglycolic acid (TGA) and cadmium acetate as starting materials. The transformation from the rod-like precursor of CdS/cadmium thiolate complex to CdS, CdSe and CdTe nanotubes were performed under constant stirring at room temperature in aqueous solution containing S 2-, Se 2- and Te 2-, respectively. The nanotube diameter can be controlled from 150 to 400 nm related to the dimension of templates. The XRD patterns show the cadmium chalcogenide nanotubes all corresponding to face-centered cubic structure. © 2012 Elsevier B.V. All rights reserved.

  5. Low temperature synthesis of Zn nanowires by physical vapor deposition

    Energy Technology Data Exchange (ETDEWEB)

    Schroeder, Philipp; Kast, Michael; Brueckl, Hubert [Austrian Research Centers GmbH ARC, Nano- Systemtechnologies, Donau-City-Strasse 1, A-1220 Wien (Austria)

    2007-07-01

    We demonstrate catalytic growth of zinc nanowires by physical vapor deposition at modest temperatures of 125-175 C on various substrates. In contrast to conventional approaches using tube furnaces our home-built growth system allows to control the vapor sources and the substrate temperature separately. The silicon substrates were sputter coated with a thin gold layer as metal catalyst. The samples were heated to the growth temperature and subsequently exposed to the zinc vapor at high vacuum conditions. The work pressure was adjusted by the partial pressure of oxygen or argon flow gas. Scanning electron microscopy and atomic force microscopy characterizations revealed that the nanowires exhibit straight, uniform morphology and have diameters in the range of 50-350 nm and lengths up to 70 {mu}m. The Zn nanowires grow independently of the substrates crystal orientation via a catalytic vapor-solid growth mechanism. Since no nanowire formation was observed without gold coating, we expect that the onedimensional growth is initiated by a surface reactive Au seed. ZnO nanowires can be produced in the same preparation chamber by oxidation at 500 C in 1atm (80% Ar, 20% O{sub 2}) for 1 hour. ZnO is highly attractive for sensor applications.

  6. Synthesis of MIL-100(Fe at Low Temperature and Atmospheric Pressure

    Directory of Open Access Journals (Sweden)

    Jing Shi

    2013-01-01

    Full Text Available MIL-100(Fe, a mesoporous metal-organic framework (MOF, has a large BET specific surface area and pore volume with the presence of a significant amount of accessible Lewis acid metal sites upon dehydration. The structural characteristics of MIL-100(Fe make it a good candidate for potential applications in gas storage, separation, and heterogeneous catalysis. Mainly, this MOF is obtained by the hydrothermal synthesis in a Teflon-lined autoclave at high temperature (>150°C under static conditions. However, this method has several disadvantages such as high temperature, high (autogenous pressure, long time, and comparable low MOF yield. Therefore, development of a facile method for synthesis of MIL-100(Fe is vitally important for fundamental understanding and practical application. Herein, MIL-100(Fe is synthesized by a facile low-temperature (90% still could be achieved, suggesting that this simple and energy saving method has the potential to be used practically.

  7. 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.

  8. Numerical investigation of high temperature synthesis gas premixed combustion via ANSYS Fluent

    Directory of Open Access Journals (Sweden)

    Pashchenko Dmitry

    2018-01-01

    Full Text Available A numerical model of the synthesis gas pre-mixed combustion is developed. The research was carried out via ANSYS Fluent software. Verification of the numerical results was carried out using experimental data. A visual comparison of the flame contours that obtained by the synthesis gas combustion for Re = 600; 800; 1000 was performed. A comparison of the wall temperature of the combustion chamber, obtained with the help of the developed model, with the results of a physical experiment was also presented. For all cases, good convergence of the results is observed. It is established that a change in the temperature of the syngas/air mixture at the inlet to the combustion chamber does not significantly affect the temperature of the combustion products due to the dissipation of the H2O and CO2 molecules. The obtained results are of practical importance for the design of heat engineering plants with thermochemical heat recovery.

  9. Synthesis of ZnO Nanostructures for Low Temperature CO and UV Sensing

    Directory of Open Access Journals (Sweden)

    Nazar Abbas Shah

    2012-10-01

    Full Text Available In this paper, synthesis and results of the low temperature sensing of carbon monoxide (CO gas and room temperature UV sensors using one dimensional (1-D ZnO nanostructures are presented. Comb-like structures, belts and rods, and needle-shaped nanobelts were synthesized by varying synthesis temperature using a vapor transport method. Needle-like ZnO nanobelts are unique as, according to our knowledge, there is no evidence of such morphology in previous literature. The structural, morphological and optical characterization was carried out using X-ray diffraction, scanning electron microscopy and diffused reflectance spectroscopy techniques. It was observed that the sensing response of comb-like structures for UV light was greater as compared to the other grown structures. Comb-like structure based gas sensors successfully detect CO at 75 °C while other structures did not show any response.

  10. Low-temperature graphene synthesis using microwave plasma CVD

    International Nuclear Information System (INIS)

    Yamada, Takatoshi; Kim, Jaeho; Ishihara, Masatou; Hasegawa, Masataka

    2013-01-01

    The graphene chemical vapour deposition (CVD) technique at substrate temperatures around 300 °C by a microwave plasma sustained by surface waves (surface wave plasma chemical vapour deposition, SWP-CVD) is discussed. A low-temperature, large-area and high-deposition-rate CVD process for graphene films was developed. It was found from Raman spectra that the deposited films on copper (Cu) substrates consisted of high-quality graphene flakes. The fabricated graphene transparent conductive electrode showed uniform optical transmittance and sheet resistance, which suggests the possibility of graphene for practical electrical and optoelectronic applications. It is intriguing that graphene was successfully deposited on aluminium (Al) substrates, for which we did not expect the catalytic effect to decompose hydrocarbon and hydrogen molecules. We developed a roll-to-roll SWP-CVD system for continuous graphene film deposition towards industrial mass production. A pair of winder and unwinder systems of Cu film was installed in the plasma CVD apparatus. Uniform Raman spectra were confirmed over the whole width of 297 mm of Cu films. We successfully transferred the deposited graphene onto PET films, and confirmed a transmittance of about 95% and a sheet resistance of less than 7 × 10 5 Ω/sq.

  11. Low-temperature graphene synthesis using microwave plasma CVD

    Science.gov (United States)

    Yamada, Takatoshi; Kim, Jaeho; Ishihara, Masatou; Hasegawa, Masataka

    2013-02-01

    The graphene chemical vapour deposition (CVD) technique at substrate temperatures around 300 °C by a microwave plasma sustained by surface waves (surface wave plasma chemical vapour deposition, SWP-CVD) is discussed. A low-temperature, large-area and high-deposition-rate CVD process for graphene films was developed. It was found from Raman spectra that the deposited films on copper (Cu) substrates consisted of high-quality graphene flakes. The fabricated graphene transparent conductive electrode showed uniform optical transmittance and sheet resistance, which suggests the possibility of graphene for practical electrical and optoelectronic applications. It is intriguing that graphene was successfully deposited on aluminium (Al) substrates, for which we did not expect the catalytic effect to decompose hydrocarbon and hydrogen molecules. We developed a roll-to-roll SWP-CVD system for continuous graphene film deposition towards industrial mass production. A pair of winder and unwinder systems of Cu film was installed in the plasma CVD apparatus. Uniform Raman spectra were confirmed over the whole width of 297 mm of Cu films. We successfully transferred the deposited graphene onto PET films, and confirmed a transmittance of about 95% and a sheet resistance of less than 7 × 105 Ω/sq.

  12. Chemical synthesis of Cu2Se nanoparticles at room temperature

    International Nuclear Information System (INIS)

    Rong, Fengxia; Bai, Yan; Chen, Tianfeng; Zheng, Wenjie

    2012-01-01

    Graphical abstract: The Cu 2 Se nanoparticles were synthesized by a simple and rapid method at room temperature. The TEM and SEM images show that the Cu 2 Se nanoparticles were spherical. Highlights: ► Cu 2 Se nanoparticles were synthesized by the reaction of nanoSe 0 sol with Cu + ions. ► The Cu 2 Se nanoparticles were spherical with cubic structure and well crystallized. ► Optical and electrochemical properties of Cu 2 Se nanoparticles were observed. ► The formation mechanism of Cu 2 Se nanoparticles was proposed. -- Abstract: A simple and rapid method has been developed to synthesize cuprous selenide (Cu 2 Se) nanoparticles by the reaction of selenium nanoparticles sol with copper sulfate solution containing ascorbic acid at room temperature. Cu 2 Se nanoparticles were characterized by scanning electron microscopy (SEM), transmission electron microscopy (TEM), X-ray diffraction (XRD), and energy dispersive X-ray analysis (EDX). The results indicated that Cu 2 Se nanoparticles were cubic crystal structure and spherical with the diameter about 75 nm. The ultraviolet–visible absorption spectrum (UV–vis) and cyclic voltammetry of Cu 2 Se nanoparticles were also investigated. The optical band gap energy of Cu 2 Se nanoparticles was 1.94 eV. On the basis of a series of experiments and characterizations, the formation mechanism of Cu 2 Se nanoparticles was discussed.

  13. Low-temperature synthesis of superconducting nanocrystalline MgB2

    International Nuclear Information System (INIS)

    Lu, J.; Xiao, Z.; Lin, Q.; Claus, H.; Fang, Z.Z.

    2010-01-01

    Magnesium diboride (MgB 2 ) is considered a promising material for practical application in superconducting devices, with a transition temperature near 40 K. In the present paper, nanocrystalline MgB 2 with an average particle size of approximately 70 nm is synthesized by reacting LiBH 4 with MgH 2 at temperatures as low as 450 C. This synthesis approach successfully bypasses the usage of either elemental boron or toxic diborane gas. The superconductivity of the nanostructures is confirmed by magnetization measurements, showing a superconducting critical temperature of 38.7 K.

  14. Low Temperature Synthesis and Properties of Gadolinium-Doped Cerium Oxide Nanoparticles

    DEFF Research Database (Denmark)

    Machado, M. F. S.; Moraes, L. P. R.; Monteiro, N. K.

    2017-01-01

    Gadolinium-doped cerium oxide (GDC) is an attractive ceramic material for solid oxide fuel cells (SOFCs) both as the electrolyte and in composite electrodes operating at low and intermediate temperatures. GDC exhibits high oxygen ion conductivity at a wide range of temperatures and displays a high...... resistance to carbon deposition when hydrocarbons are used as fuels. However, an inconvenience of ceria-based oxides is the high sintering temperature needed to obtain a fully dense ceramic body. In this study, a green chemistry route for the synthesis of 10 mol% GDC nanoparticles is proposed. The aqueous...

  15. Room temperature synthesis of water-repellent polystyrene nanocomposite coating

    International Nuclear Information System (INIS)

    Guo Yonggang; Jiang Dong; Zhang Xia; Zhang Zhijun; Wang Qihua

    2010-01-01

    A stable superhydrophobic polystyrene nanocomposite coating was fabricated by means of a very simple and easy method. The coating was characterized by scanning electron microscopy and X-ray photoelectron spectrum. The wettability of the products was also investigated. By adding the surface-modified SiO 2 nanoparticles, the wettability of the coating changed to water-repellent superhydrophobic, not only for pure water, but also for a wide pH range of corrosive liquids. The influence of the drying temperature and SiO 2 content on the wettability of the nanocomposite coating was also investigated. It was found that both factors had little or no significant effect on the wetting behavior of the coating surface.

  16. High-Pressure-High-Temperature Processing Reduces Maillard Reaction and Viscosity in Whey Protein-Sugar Solutions

    NARCIS (Netherlands)

    Avila Ruiz, Geraldine; Xi, Bingyan; Minor, Marcel; Sala, Guido; Boekel, van Tiny; Fogliano, Vincenzo; Stieger, Markus

    2016-01-01

    The aim of the study was to determine the influence of pressure in high-pressure-high-temperature (HPHT) processing on Maillard reactions and protein aggregation of whey protein-sugar solutions. Solutions of whey protein isolate containing either glucose or trehalose at pH 6, 7, and 9 were

  17. Facile synthesis of graphene on dielectric surfaces using a two-temperature reactor CVD system

    International Nuclear Information System (INIS)

    Zhang, C; Man, B Y; Yang, C; Jiang, S Z; Liu, M; Chen, C S; Xu, S C; Sun, Z C; Gao, X G; Chen, X J

    2013-01-01

    Direct deposition of graphene on a dielectric substrate is demonstrated using a chemical vapor deposition system with a two-temperature reactor. The two-temperature reactor is utilized to offer sufficient, well-proportioned floating Cu atoms and to provide a temperature gradient for facile synthesis of graphene on dielectric surfaces. The evaporated Cu atoms catalyze the reaction in the presented method. C atoms and Cu atoms respectively act as the nuclei for forming graphene film in the low-temperature zone and the zones close to the high-temperature zones. A uniform and high-quality graphene film is formed in an atmosphere of sufficient and well-proportioned floating Cu atoms. Raman spectroscopy, scanning electron microscopy and atomic force microscopy confirm the presence of uniform and high-quality graphene. (paper)

  18. Vacancy-impurity centers in diamond: prospects for synthesis and applications

    Science.gov (United States)

    Ekimov, E. A.; Kondrin, M. V.

    2017-06-01

    The bright luminescence of impurity-vacancy complexes, combined with high chemical and radiation resistance, makes diamond an attractive platform for the production of single-photon emitters and luminescent biomarkers for applications in nanoelectronics and medicine. Two representatives of this kind of defects in diamond, silicon-vacancy (SiV) and germanium-vacancy (GeV) centers, are discussed in this review; their similarities and differences are demonstrated in terms of the more thoroughly studied nitrogen-vacancy (NV) complexes. The recent discovery of GeV luminescent centers opens a unique opportunity for the controlled synthesis of single-photon emitters in nanodiamonds. We demonstrate prospects for the high-pressure high-temperature (HPHT) technique to create single-photon emitters, not only as an auxiliary to chemical vapor deposition (CVD) and ion-implantation methods but also as a primary synthesis tool for producing color centers in nanodiamonds. Besides practical applications, comparative studies of these two complexes, which belong to the same structural class of defects, have a fundamental importance for deeper understanding of shelving levels, the electronic structure, and optical properties of these centers. In conclusion, we discuss several open problems regarding the structure, charge state, and practical application of these centers, which still require a solution.

  19. Influence of Plasma Jet Temperature Profiles in Arc Discharge Methods of Carbon Nanotubes Synthesis.

    Science.gov (United States)

    Raniszewski, Grzegorz; Wiak, Slawomir; Pietrzak, Lukasz; Szymanski, Lukasz; Kolacinski, Zbigniew

    2017-02-23

    One of the most common methods of carbon nanotubes (CNTs) synthesis is application of an electric-arc plasma. However, the final product in the form of cathode deposit is composed of carbon nanotubes and a variety of carbon impurities. An assay of carbon nanotubes produced in arc discharge systems available on the market shows that commercial cathode deposits contain about 10% CNTs. Given that the quality of the final product depends on carbon-plasma jet parameters, it is possible to increase the yield of the synthesis by plasma jet control. Most of the carbon nanotubes are multiwall carbon nanotubes (MWCNTs). It was observed that the addition of catalysts significantly changes the plasma composition, effective ionization potential, the arc channel conductance, and in effect temperature of the arc and carbon elements flux. This paper focuses on the influence of metal components on plasma-jet forming containing carbon nanotubes cathode deposit. The plasma jet temperature control system is presented.

  20. Influence of Plasma Jet Temperature Profiles in Arc Discharge Methods of Carbon Nanotubes Synthesis

    Directory of Open Access Journals (Sweden)

    Grzegorz Raniszewski

    2017-02-01

    Full Text Available One of the most common methods of carbon nanotubes (CNTs synthesis is application of an electric-arc plasma. However, the final product in the form of cathode deposit is composed of carbon nanotubes and a variety of carbon impurities. An assay of carbon nanotubes produced in arc discharge systems available on the market shows that commercial cathode deposits contain about 10% CNTs. Given that the quality of the final product depends on carbon–plasma jet parameters, it is possible to increase the yield of the synthesis by plasma jet control. Most of the carbon nanotubes are multiwall carbon nanotubes (MWCNTs. It was observed that the addition of catalysts significantly changes the plasma composition, effective ionization potential, the arc channel conductance, and in effect temperature of the arc and carbon elements flux. This paper focuses on the influence of metal components on plasma-jet forming containing carbon nanotubes cathode deposit. The plasma jet temperature control system is presented.

  1. The effect of temperature in flux-assisted synthesis of SnNb2O6

    KAUST Repository

    Noureldine, Dalal

    2014-10-03

    A flux-assisted method was used to synthesize SnNb2O6 as a visible-light-responsive metal oxide photocatalyst. The role of synthesis temperature was investigated in detail using different reaction temperatures (300, 500, 600, 800, 1000 °C). The obtained products were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), Brunauer-Emmett-Teller method (BET). The synthesis with SnCl2 as a flux led to tin niobate particles in the platelet morphology with smooth surfaces. The synthesized crystal showed 2D anisotropic growth along the (600) plane as the flux ratio increased. The particles synthesized with a high reactant to flux ratio (1:10 or higher) exhibited improved photocatalytic activity for hydrogen evolution from an aqueous methanol solution under visible radiation (λ > 420 nm). © (2014) COPYRIGHT Society of Photo-Optical Instrumentation Engineers (SPIE). Downloading of the abstract is permitted for personal use only.

  2. Reduce synthesis temperature and improve dispersion of YAG nanopowders based on the co-crystallization method

    Energy Technology Data Exchange (ETDEWEB)

    Fan, G.F.; Tang, Y.Q.; Lu, W.Z., E-mail: lwz@mail.hust.edu.cn; Zhang, X.R.; Xu, X.

    2015-01-05

    Highlights: • YAG nanopowders were synthesized through a co-crystallization method. • A three-layer core–shell structure was made to lower the synthesis temperature. • PAA again reduced the synthesis temperature based on the core–shell structure. • YAG nanopowders were synthesized at 700 °C in normal apparatus. • Agglomeration was greatly improved by PAA. - Abstract: Pure yttrium aluminum garnet (YAG) nanopowders were synthesized at 950 °C from the co-crystallization precursor of Y(NO{sub 3}){sub 3}⋅6H{sub 2}O and Al(NO{sub 3}){sub 3}⋅9H{sub 2}O (nitrate process). When 17 wt.% of Y(NO{sub 3}){sub 3}⋅6H{sub 2}O was replaced by Y{sub 2}O{sub 3} nanopowders, so as to make up a three-layer core–shell structure of the precursor, the synthesis temperature was reduced to 850 °C (Y{sub 2}O{sub 3} process). Based on Y{sub 2}O{sub 3} process, further reducing the synthesis temperature to 700 °C was realized by adding polyacrylic acid (PAA, 50% M), which was used to shorten the distance of the metal ions and provide combustion heat (PAA process). TEM characterizations indicated that the powders produced through nitrate and Y{sub 2}O{sub 3} processes agglomerated, while the powders produced through PAA process were dispersed much better. The agglomerate size analysis results demonstrated that the powders produced through PAA process were with smaller agglomerate size and wider agglomerate size distribution than those through nitrate process or Y{sub 2}O{sub 3} process. And they were more likely to be sintered to YAG transparent ceramics.

  3. The synthesis of [2-13C]2-nitropropane at room temperature and at atmospheric pressure

    OpenAIRE

    Jacquemijns M; Zomer G

    1990-01-01

    In this report the synthesis of [2-13C]2-nitropropane at room temperature is described. [2-13C]Acetone was converted into the oxime with hydroxy hydrochloridelamine and sodium carbonate. Treatment with hypobromic acid resulted in 2-13C]2-bromo-2-nitropropane. Hydrogenation with sodium borohydride gave [2-13C]2-nitropropane in 14,3% overall yield.

  4. Room temperature chemical synthesis of Cu(OH){sub 2} thin films for supercapacitor application

    Energy Technology Data Exchange (ETDEWEB)

    Gurav, K.V. [Thin Film Photonic and Electronics Lab, Department of Materials Science and Engineering, Chonnam National University, 300 Yongbong-dong, Puk-Gu, Gwangju 500-757 (Korea, Republic of); Patil, U.M. [Thin Film Physics Laboratory, Department of Physics, Shivaji University, Kolhapur 416 007 (M.S.) (India); Shin, S.W.; Agawane, G.L.; Suryawanshi, M.P.; Pawar, S.M.; Patil, P.S. [Thin Film Photonic and Electronics Lab, Department of Materials Science and Engineering, Chonnam National University, 300 Yongbong-dong, Puk-Gu, Gwangju 500-757 (Korea, Republic of); Lokhande, C.D. [Thin Film Physics Laboratory, Department of Physics, Shivaji University, Kolhapur 416 007 (M.S.) (India); Kim, J.H., E-mail: jinhyeok@chonnam.ac.kr [Thin Film Photonic and Electronics Lab, Department of Materials Science and Engineering, Chonnam National University, 300 Yongbong-dong, Puk-Gu, Gwangju 500-757 (Korea, Republic of)

    2013-10-05

    Highlights: •Cu(OH){sub 2} is presented as the new supercapacitive material. •The novel room temperature method used for the synthesis of Cu(OH){sub 2}. •The hydrous, nanograined Cu(OH){sub 2} shows higher specific capacitance of 120 F/g. -- Abstract: Room temperature soft chemical synthesis route is used to grow nanograined copper hydroxide [Cu(OH){sub 2}] thin films on glass and stainless steel substrates. The structural, morphological, optical and wettability properties of Cu(OH){sub 2} thin films are studied by means of X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), field emission scanning electron microscopy (FESEM), UV–vis spectrophotometer and water contact angle measurement techniques. The results showed that, room temperature chemical synthesis route allows to form the nanograined and hydrophilic Cu(OH){sub 2} thin films with optical band gap energy of 3.0 eV. The electrochemical properties of Cu(OH){sub 2} thin films are studied in an aqueous 1 M NaOH electrolyte using cyclic voltammetry. The sample exhibited supercapacitive behavior with 120 F/g specific capacitance.

  5. Room temperature chemical synthesis of Cu(OH)2 thin films for supercapacitor application

    International Nuclear Information System (INIS)

    Gurav, K.V.; Patil, U.M.; Shin, S.W.; Agawane, G.L.; Suryawanshi, M.P.; Pawar, S.M.; Patil, P.S.; Lokhande, C.D.; Kim, J.H.

    2013-01-01

    Highlights: •Cu(OH) 2 is presented as the new supercapacitive material. •The novel room temperature method used for the synthesis of Cu(OH) 2 . •The hydrous, nanograined Cu(OH) 2 shows higher specific capacitance of 120 F/g. -- Abstract: Room temperature soft chemical synthesis route is used to grow nanograined copper hydroxide [Cu(OH) 2 ] thin films on glass and stainless steel substrates. The structural, morphological, optical and wettability properties of Cu(OH) 2 thin films are studied by means of X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), field emission scanning electron microscopy (FESEM), UV–vis spectrophotometer and water contact angle measurement techniques. The results showed that, room temperature chemical synthesis route allows to form the nanograined and hydrophilic Cu(OH) 2 thin films with optical band gap energy of 3.0 eV. The electrochemical properties of Cu(OH) 2 thin films are studied in an aqueous 1 M NaOH electrolyte using cyclic voltammetry. The sample exhibited supercapacitive behavior with 120 F/g specific capacitance

  6. Low temperature synthesis of graphene on arbitrary substrates and its transport properties

    Science.gov (United States)

    Zhao, Rong; Akhtar, Meysam; Alruqi, Adel; Jasinski, Jacek; Sumanasekera, Gamini; Department of Physics; Astronomy, University of Louisville Collaboration; Conn CenterRenewable Energy, University of Louisville Collaboration

    Here we report the direct synthesis of uniform and vertically oriented graphene films on multiple substrates including glass, Si/SiO2, and copper foil by radio-frequency plasma enhanced chemical vapor deposition (PECVD) using methane as the carbon precursor at relatively low temperatures. Raman spectra of all the samples show characteristic Raman peaks of graphene. The temperature dependence of electrical transport properties such as 4-probe resistance, thermo electrical power and hall mobility were measured for graphene grown on glass substrates at varying temperature from 500 ° C to 700 ° C. The morphological and surface characteristics were also studied by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). This work demonstrates the potential of low temperature and transfer-free graphene growth for future graphene-based electronic applications.

  7. Low temperature synthesis of Ba1–xSrxSnO3 (x = 0–1) from molten ...

    Indian Academy of Sciences (India)

    Administrator

    first time by molten salt synthesis (MSS) method using KOH as the flux at lower temperature (400°C) compared to other ... chemical methods have been adopted by many research- ers. .... financial support and Technology Business Incubator,.

  8. Timing matters: the underappreciated role of temperature ramp rate for shape control and reproducibility of quantum dot synthesis

    KAUST Repository

    Baumgardner, William J.; Quan, Zewei; Fang, Jiye; Hanrath, Tobias

    2012-01-01

    Understanding the coupled kinetic and thermodynamics factors governing colloidal nanocrystals nucleation and growth are critical factors in the predictable and reproducible synthesis of advanced nanomaterials. We show that the temporal temperature

  9. Synthesis of Carbon Nanotubes and Nanospheres from Coconut Fibre and the Role of Synthesis Temperature on Their Growth

    Science.gov (United States)

    Adewumi, Gloria A.; Inambao, Freddie; Eloka-Eboka, Andrew; Revaprasadu, Neerish

    2018-04-01

    Carbon nanotubes (CNT) and carbon nanospheres were successfully synthesized from coconut fibre-activated carbon. The biomass was first carbonized then physically activated, followed by treatment using ethanol vapor at 700°C to 1100°C at 100°C intervals. The effect of synthesis temperature on the formation of the nanomaterials was studied using scanning electron microscopy (SEM), transmission electron microscopy (TEM), energy dispersive x-ray spectrometry, x-ray diffraction (XRD), Fourier transform infrared microscopy (FTIR) and thermogravimetric analysis. SEM analysis revealed that nanospheres were formed at higher temperatures of 1000°C and 1100°C, while lower temperatures of 800°C and 900°C favored the growth of CNT. At 700°C, however, no tubes or spheres were formed. TEM and FTIR were used to observe spectral features, such as the peak positions, intensity and bandwidth, which are linked to some structural properties of the samples investigated. All these observations provided facts on the nanosphere and nanotube dimensions, vibrational modes and the degree of purity of the obtained samples. The TEM results show spheres of diameter in the range 50 nm to 250 nm while the tubes had diameters between 50 nm to 100 nm. XRD analysis reveals the materials synthesized are amorphous in nature with a hexagonal graphite structure.

  10. Room temperature synthesis of porous SiO2 thin films by plasma enhanced chemical vapor deposition

    OpenAIRE

    Barranco Quero, Ángel; Cotrino Bautista, José; Yubero Valencia, Francisco; Espinós, J. P.; Rodríguez González-Elipe, Agustín

    2004-01-01

    Synthesis of porous SiO2 thin films in room temperature was carried out using plasma enhanced chemical vapor deposition (CVD) in an electron cyclotron resonance microwave reactor with a downstream configuration.The gas adsorption properties and the type of porosity of the SiO2 thin films were assessed by adsorption isotherms of toluene at room temperature.The method could also permit the tailoring synthesis of thin films when both composition and porosity can be simultaneously and independent...

  11. Foundations of low-temperature plasma enhanced materials synthesis and etching

    Science.gov (United States)

    Oehrlein, Gottlieb S.; Hamaguchi, Satoshi

    2018-02-01

    Low temperature plasma (LTP)-based synthesis of advanced materials has played a transformational role in multiple industries, including the semiconductor industry, liquid crystal displays, coatings and renewable energy. Similarly, the plasma-based transfer of lithographically defined resist patterns into other materials, e.g. silicon, SiO2, Si3N4 and other electronic materials, has led to the production of nanometer scale devices that are the basis of the information technology, microsystems, and many other technologies based on patterned films or substrates. In this article we review the scientific foundations of both LTP-based materials synthesis at low substrate temperature and LTP-based isotropic and directional etching used to transfer lithographically produced resist patterns into underlying materials. We cover the fundamental principles that are the basis of successful application of the LTP techniques to technological uses and provide an understanding of technological factors that may control or limit material synthesis or surface processing with the use of LTP. We precede these sections with a general discussion of plasma surface interactions, the LTP-generated particle fluxes including electrons, ions, radicals, excited neutrals and photons that simultaneously contact and modify surfaces. The surfaces can be in the line of sight of the discharge or hidden from direct interaction for structured substrates. All parts of the article are extensively referenced, which is intended to help the reader study the topics discussed here in more detail.

  12. SYNTHESIS AND FABRICATION OF MO-W COMPONENTS FOR NEUTRON RESONANCE SPECTROSCOPY TEMPERATURE MEASUREMENT

    International Nuclear Information System (INIS)

    BINGERT, S.; DESCH, P.; TRUJILLO, E.

    1999-01-01

    A Molybdenum-- 182 Tungsten (Mo- 182 W) alloy was specified for an application that would ultimately result in the measurement of temperature and particle velocity during the steady state time following the shock loading of various materials. The 182 W isotope provides a tag for the analysis of neutron resonance line shape from which the temperature may be calculated. The material was specified to have 1.8 atom percent W, with W-rich regions no larger than 1 microm in size. Both the composition and W distribution were critical to the experiment. Another challenge to the processing was the very small quantity of 182 W material available for the synthesis of the alloy. Therefore, limited fabrication routes were available for evaluation. Several synthesis and processing routes were explored to fabricate the required alloy components. First, precipitation of W onto Mo powder using ammonium metatungstate was investigated for powder synthesis followed by uniaxial hot pressing. Second, mechanical alloying (MA) followed by hot isostatic pressing (HIP) and warm forging was attempted. Finally, arc-melting techniques followed by either hot rolling or crushing the alloyed button into powder and consolidation were pursued. The results of the processing routes and characterization of the materials produced will be discussed

  13. Room temperature synthesis of an optically and thermally responsive hybrid PNIPAM-gold nanoparticle

    International Nuclear Information System (INIS)

    Morones, J. Ruben; Frey, Wolfgang

    2010-01-01

    Composites of metal nanoparticles and environmentally sensitive polymers are useful as nanoactuators that can be triggered externally using light of a particular wavelength. We demonstrate a synthesis route that is easier than grafting techniques and allows for the in situ formation of individual gold nanoparticles encapsulated by an environmentally sensitive polymer, while also providing a strong interaction between the polymer and the metal particle. We present a one-pot, room-temperature synthesis route for gold metal nanoparticles that uses poly-N-isopropyl acrylamide as the capping and stabilizing agent and ascorbic acid as the reducing agent and achieves size control similar to the most common citric acid synthesis. We show that the composite can be precipitated reversibly by temperature or light using the non-radiative decay and conversion to heat of the surface plasmon resonance of the metal nanoparticle. The precipitation is induced by the collapse of the polymer cocoon surrounding each gold nanoparticle, as can be seen by surface plasmon spectroscopy. The experiments agree with theoretical models for the heat generation in a colloidal suspension that support fast switching with low laser power densities. The synthesized composite is a simple nanosized opto-thermal switch.

  14. Synthesis of indium nanoparticles at ambient temperature; simultaneous phase transfer and ripening

    Energy Technology Data Exchange (ETDEWEB)

    Aghazadeh Meshgi, Mohammad; Kriechbaum, Manfred [Graz University of Technology, Institute of Inorganic Chemistry (Austria); Biswas, Subhajit; Holmes, Justin D., E-mail: j.holmes@ucc.ie [University College Cork, Materials Chemistry and Analysis Group, Department of Chemistry and the Tyndall National Institute (Ireland); Marschner, Christoph, E-mail: christoph.marschner@tugraz.at [Graz University of Technology, Institute of Inorganic Chemistry (Austria)

    2016-12-15

    The synthesis of size-monodispersed indium nanoparticles via an innovative simultaneous phase transfer and ripening method is reported. The formation of nanoparticles occurs in a one-step process instead of well-known two-step phase transfer approaches. The synthesis involves the reduction of InCl{sub 3} with LiBH{sub 4} at ambient temperature and although the reduction occurs at room temperature, fine indium nanoparticles, with a mean diameter of 6.4 ± 0.4 nm, were obtained directly in non-polar n-dodecane. The direct synthesis of indium nanoparticles in n-dodecane facilitates their fast formation and enhances their size-monodispersity. In addition, the nanoparticles were highly stable for more than 2 months. The nanoparticles were characterised by dynamic light scattering (DLS), small angle X-ray scattering (SAXS), transmission electron microscopy (TEM), energy dispersive X-ray spectroscopy (EDS) and Fourier transform infrared (FT-IR) spectroscopy to determine their morphology, structure and phase purity.

  15. Synthesis and characterization of boron-oxygen-hydrogen thin films at low temperatures

    International Nuclear Information System (INIS)

    Music, D.; Koelpin, H.; Atiser, A.; Kreissig, U.; Bobek, T.; Hadam, B.; Schneider, J.M.

    2005-01-01

    We have studied the influence of synthesis temperature on chemical composition and mechanical properties of X-ray amorphous boron-oxygen-hydrogen (B-O-H) films. These B-O-H films have been synthesized by RF sputtering of a B-target in an Ar atmosphere. Upon increasing the synthesis temperature from room temperature to 550 deg. C, the O/B and H/B ratios decrease from 0.73 to 0.15 and 0.28 to 0.07, respectively, as determined by elastic recoil detection analysis. It is reasonable to assume that potential sources of O and H are residual gas and laboratory atmosphere. The elastic modulus, as measured by nanoindentation, increases from 93 to 214 GPa, as the O/B and H/B ratios decreases within the range probed. Hence, we have shown that the effect of impurity incorporation on the elastic properties is extensive and that the magnitude of the incorporation is a strong function of the substrate temperature

  16. High-pressure high-temperature phase diagram of organic crystal paracetamol

    Science.gov (United States)

    Smith, Spencer J.; Montgomery, Jeffrey M.; Vohra, Yogesh K.

    2016-01-01

    High-pressure high-temperature (HPHT) Raman spectroscopy studies have been performed on the organic crystal paracetamol in a diamond anvil cell utilizing boron-doped heating diamond anvil. Isobaric measurements were conducted at pressures up to 8.5 GPa and temperature up to 520 K in five different experiments. Solid state phase transitions from monoclinic Form I  →  orthorhombic Form II were observed at various pressures and temperatures as well as transitions from Form II  →  unknown Form IV. The melting temperature for paracetamol was observed to increase with increasing pressures to 8.5 GPa. This new data is combined with previous ambient temperature high-pressure Raman and x-ray diffraction data to create the first HPHT phase diagram of paracetamol.

  17. High-pressure high-temperature phase diagram of organic crystal paracetamol

    International Nuclear Information System (INIS)

    Smith, Spencer J; Montgomery, Jeffrey M; Vohra, Yogesh K

    2016-01-01

    High-pressure high-temperature (HPHT) Raman spectroscopy studies have been performed on the organic crystal paracetamol in a diamond anvil cell utilizing boron-doped heating diamond anvil. Isobaric measurements were conducted at pressures up to 8.5 GPa and temperature up to 520 K in five different experiments. Solid state phase transitions from monoclinic Form I  →  orthorhombic Form II were observed at various pressures and temperatures as well as transitions from Form II  →  unknown Form IV. The melting temperature for paracetamol was observed to increase with increasing pressures to 8.5 GPa. This new data is combined with previous ambient temperature high-pressure Raman and x-ray diffraction data to create the first HPHT phase diagram of paracetamol. (paper)

  18. Production of advanced materials by methods of self-propagating high-temperature synthesis

    CERN Document Server

    Tavadze, Giorgi F

    2013-01-01

    This translation from the original Russian book outlines the production of a variety of materials by methods of self-propagating high-temperature synthesis (SHS). The types of materials discussed include: hard, refractory, corrosion and wear-resistant materials, as well as other advanced and speciality materials. The authors address the issue of optimal parameters for SHS reactions occurring during processes involving a preliminary metallothermic reduction stage, and they calculate this using thermodynamic approaches. In order to confirm the effectiveness of this approach, the authors describe experiments focussing on the synthesis of elemental crysalline boron, boron carbides and nitrides. Other parts of this brief include theoretical and experimental results on single-stage production of hard alloys on the basis of titanium and zirconium borides, as well as macrokinetics of degassing and compaciton of SHS-products.This brief is suitable for academics, as well as those working in industrial manufacturing com...

  19. Synthesis of monoclinic potassium niobate nanowires that are stable at room temperature.

    Science.gov (United States)

    Kim, Seungwook; Lee, Ju-Hyuck; Lee, Jaeyeon; Kim, Sang-Woo; Kim, Myung Hwa; Park, Sungnam; Chung, Haegeun; Kim, Yong-Il; Kim, Woong

    2013-01-09

    We report the synthesis of KNbO(3) nanowires (NWs) with a monoclinic phase, a phase not observed in bulk KNbO(3) materials. The monoclinic NWs can be synthesized via a hydrothermal method using metallic Nb as a precursor. The NWs are metastable, and thermal treatment at ∼450 °C changed the monoclinic phase into the orthorhombic phase, which is the most stable phase of KNbO(3) at room temperature. Furthermore, we fabricated energy-harvesting nanogenerators by vertically aligning the NWs on SrTiO(3) substrates. The monoclinic NWs showed significantly better energy conversion characteristics than orthorhombic NWs. Moreover, the frequency-doubling efficiency of the monoclinic NWs was ∼3 times higher than that of orthorhombic NWs. This work may contribute to the synthesis of materials with new crystalline structures and hence improve the properties of the materials for various applications.

  20. Rod-Shaped Magnetite Nano/Microparticles Synthesis at Ambient Temperature

    Directory of Open Access Journals (Sweden)

    Balaprasad Ankamwar

    2013-01-01

    Full Text Available Here, we reported room temperature synthesis of Fe3O4 rod-shaped nano/microparticles by chemical reduction method from FeCl3 precursor and NaBH4 as the reducing agent in the presence of the pyrrole as a capping agent. The magnetic Fe3O4 particles were characterized by several methods, such as SEM, XRD, FTIR, and TGA. The average aspect ratio of Fe3O4 rod-shaped particles was ~2.8. These particles were redispersed in deionised water to form a colloidal solution and showed magnetic properties. This economical synthesis route is scalable, and Fe3O4 particles can be exploited for various applications such as MRI contrast enhancement, biodiseperations, Ni-Fe batteries, and as a catalyst.

  1. Room temperature synthesis of ReS2 through aqueous perrhenate sulfidation

    Science.gov (United States)

    Borowiec, Joanna; Gillin, William P.; Willis, Maureen A. C.; Boi, Filippo S.; He, Y.; Wen, J. Q.; Wang, S. L.; Schulz, Leander

    2018-02-01

    In this study, a direct sulfidation reaction of ammonium perrhenate (NH4ReO4) leading to a synthesis of rhenium disulfide (ReS2) is demonstrated. These findings reveal the first example of a simplistic bottom-up approach to the chemical synthesis of crystalline ReS2. The reaction presented here takes place at room temperature, in an ambient and solvent-free environment and without the necessity of a catalyst. The atomic composition and structure of the as-synthesized product were characterized using several analysis techniques including energy dispersive x-ray spectroscopy, x-ray photoelectron spectroscopy, x-ray diffraction, transmission electron microscopy, Raman spectroscopy, thermogravimetric analysis and differential scanning calorimetry. The results indicated the formation of a lower symmetry (1Tʹ) ReS2 with a low degree of layer stacking.

  2. Effect of temperature on synthesis and properties of aluminum-magnesium mechanical alloys

    International Nuclear Information System (INIS)

    Umbrajkar, Swati M.; Schoenitz, Mirko; Jones, Steven R.; Dreizin, Edward L.

    2005-01-01

    The synthesis of an Al 0.7 Mg 0.3 mechanical alloy was studied using a planetary mill. Several distinct temperature regimes of mechanical alloying were achieved using milling jars equipped with finned heat sinks and an external air conditioner installed to cool the entire milling chamber. Wireless temperature sensors were attached to the milling jars to monitor the process temperature. Intermediate and final products were collected and were analyzed by electron microscopy and X-ray diffraction. The temperature history of the milling jars exhibited two peaks during mechanical alloying. The first peak occurred when particles of the starting powders deformed to produce flakes. The second peak was observed when the flakes agglomerated and re-fragmented forming layered composites that served as precursors for the mechanical alloy. The temperature of milling affected the magnesium solubility of the produced Al-Mg mechanical alloys. Decreasing the milling temperature from ∼70-80 deg. C to 20-30 deg. C resulted in an increase of the dissolved Mg concentration in Al from 2-3 at.% to ∼25 at.% for the Al 0.7 Mg 0.3 composition. The formation of intermetallic phases was favored at higher milling temperatures, where high solubilities cannot be achieved

  3. Effect of temperature on synthesis and properties of aluminum-magnesium mechanical alloys

    Energy Technology Data Exchange (ETDEWEB)

    Umbrajkar, Swati M. [New Jersey Institute of Technology, Department of Mechanical Engineering, Newark, NJ 07102-1982 (United States); Schoenitz, Mirko [New Jersey Institute of Technology, Department of Mechanical Engineering, Newark, NJ 07102-1982 (United States); Jones, Steven R. [New Jersey Institute of Technology, Department of Mechanical Engineering, Newark, NJ 07102-1982 (United States); Dreizin, Edward L. [New Jersey Institute of Technology, Department of Mechanical Engineering, Newark, NJ 07102-1982 (United States)]. E-mail: dreizin@njit.edu

    2005-10-27

    The synthesis of an Al{sub 0.7}Mg{sub 0.3} mechanical alloy was studied using a planetary mill. Several distinct temperature regimes of mechanical alloying were achieved using milling jars equipped with finned heat sinks and an external air conditioner installed to cool the entire milling chamber. Wireless temperature sensors were attached to the milling jars to monitor the process temperature. Intermediate and final products were collected and were analyzed by electron microscopy and X-ray diffraction. The temperature history of the milling jars exhibited two peaks during mechanical alloying. The first peak occurred when particles of the starting powders deformed to produce flakes. The second peak was observed when the flakes agglomerated and re-fragmented forming layered composites that served as precursors for the mechanical alloy. The temperature of milling affected the magnesium solubility of the produced Al-Mg mechanical alloys. Decreasing the milling temperature from {approx}70-80 deg. C to 20-30 deg. C resulted in an increase of the dissolved Mg concentration in Al from 2-3 at.% to {approx}25 at.% for the Al{sub 0.7}Mg{sub 0.3} composition. The formation of intermetallic phases was favored at higher milling temperatures, where high solubilities cannot be achieved.

  4. Synthesis of free standing nanocrystalline Cu by ball milling at cryogenic temperature

    Energy Technology Data Exchange (ETDEWEB)

    Barai, K. [Department of Metallurgy and Materials Engineering, Bengal Engineering College, Shibpur, Howrah 711103 (India); Tiwary, C.S. [Department of Materials Engineering, Indian Institute of Science, Bangalore 560012 (India); Chattopadhyay, P.P. [Department of Metallurgy and Materials Engineering, Bengal Engineering College, Shibpur, Howrah 711103 (India); Chattopadhyay, K., E-mail: kamanio@materials.iisc.ernet.in [Department of Materials Engineering, Indian Institute of Science, Bangalore 560012 (India)

    2012-12-15

    This paper reports for the first time synthesis of free standing nano-crystalline copper crystals of a {approx}30-40 nm by ball milling of copper powder at 150 K under Argon atmosphere in a specially designed cryomill. The detailed characterization of these particles using multiple techniques that includes transmission electron microscopy confirms our conclusion. Careful analysis of the chemistry of these particles indicates that these particles are essentially contamination free. Through the analysis of existing models of grain size refinements during ball milling and low temperature deformation, we argue that the suppression of thermal processes and low temperature leads to formation of free nanoparticles as the process of fracture dominates over possible cold welding at low temperatures.

  5. Room temperature synthesis of high temperature stable lanthanum phosphate–yttria nano composite

    International Nuclear Information System (INIS)

    Sankar, Sasidharan; Raj, Athira N.; Jyothi, C.K.; Warrier, K.G.K.; Padmanabhan, P.V.A.

    2012-01-01

    Graphical abstract: A facile aqueous sol–gel route involving precipitation–peptization mechanism followed by electrostatic stabilization is used for synthesizing nanocrystalline composite containing lanthanum phosphate and yttria. Highlights: ► A novel lanthanum phosphate–Y 2 O 3 nano composite is synthesized for the first time using a modified facile sol gel process. ► The composite becomes crystalline at 600 °C and X-ray diffraction pattern is indexed for monoclinic LaPO 4 and cubic yttria. ► The composite synthesized was tested up to 1300 °C and no reaction between the phases of the constituents is observed with the morphologies of the phases being retained. -- Abstract: A facile aqueous sol–gel route involving precipitation–peptization mechanism followed by electrostatic stabilization is used for synthesizing nanocrystalline composite containing lanthanum phosphate and yttria. Lanthanum phosphate (80 wt%)–yttria (20 wt%) nano composite (LaPO 4 –20%Y 2 O 3 ), has an average particle size of ∼70 nm after heat treatment of precursor at 600 °C. TG–DTA analysis reveals that stable phase of the composite is formed on heating the precursor at 600 °C. The TEM images of the composite show rod shape morphology of LaPO 4 in which yttria is acquiring near spherical shape. Phase identification of the composite as well as the phase stability up to 1300 °C was carried out using X-ray diffraction technique. With the phases being stable at higher temperatures, the composite synthesized should be a potential material for high temperature applications like thermal barrier coatings and metal melting applications.

  6. Room-temperature solution synthesis of Ag nanoparticle functionalized molybdenum oxide nanowires and their catalytic applications

    International Nuclear Information System (INIS)

    Dong Wenjun; Huang Huandi; Zhu Yanjun; Li Xiaoyun; Wang Xuebin; Li Chaorong; Chen Benyong; Wang Ge; Shi Zhan

    2012-01-01

    A simple chemical solution route for the synthesis of large-scale high-quality Ag nanoparticle functionalized molybdenum oxide nanowire at room temperature has been developed. In the synthesis, the protonated amine was intercalated into the molybdenum bronze layers to reduce the electrostatic force of the lamellar structures, and then the Ag nanoparticle functionalized long nanowires could be easily induced by a redox reaction between a molybdenum oxide–amine intermediate and Ag + at room temperature. The intercalation lamellar structures improved the nucleation and growth of the Ag nanoparticles, with the result that uniform Ag nanoparticles occurred on the surface of the MoO 3 nanowire. In this way Ag nanoparticles with average sizes of around 6 nm, and high-purity nanowires with mean diameter of around 50 nm and with typical lengths of several tens to hundreds of micrometers were produced. The heteronanostructured nanowires were intricately and inseparably connected to each other with hydrogen bonds and/or bridge oxygen atoms and packed together, forming a paper-like porous network film. The Ag–MoO 3 nanowire film performs a promoted catalytic property for the epoxidation of cis-cyclooctene, and the heteronanostructured nanowire film sensor shows excellent sensing performance to hydrogen and oxygen at room temperature. (paper)

  7. Room-temperature solution synthesis of Ag nanoparticle functionalized molybdenum oxide nanowires and their catalytic applications.

    Science.gov (United States)

    Dong, Wenjun; Huang, Huandi; Zhu, Yanjun; Li, Xiaoyun; Wang, Xuebin; Li, Chaorong; Chen, Benyong; Wang, Ge; Shi, Zhan

    2012-10-26

    A simple chemical solution route for the synthesis of large-scale high-quality Ag nanoparticle functionalized molybdenum oxide nanowire at room temperature has been developed. In the synthesis, the protonated amine was intercalated into the molybdenum bronze layers to reduce the electrostatic force of the lamellar structures, and then the Ag nanoparticle functionalized long nanowires could be easily induced by a redox reaction between a molybdenum oxide-amine intermediate and Ag(+) at room temperature. The intercalation lamellar structures improved the nucleation and growth of the Ag nanoparticles, with the result that uniform Ag nanoparticles occurred on the surface of the MoO(3) nanowire. In this way Ag nanoparticles with average sizes of around 6 nm, and high-purity nanowires with mean diameter of around 50 nm and with typical lengths of several tens to hundreds of micrometers were produced. The heteronanostructured nanowires were intricately and inseparably connected to each other with hydrogen bonds and/or bridge oxygen atoms and packed together, forming a paper-like porous network film. The Ag-MoO(3) nanowire film performs a promoted catalytic property for the epoxidation of cis-cyclooctene, and the heteronanostructured nanowire film sensor shows excellent sensing performance to hydrogen and oxygen at room temperature.

  8. Control of nanoparticle agglomeration through variation of the time-temperature profile in chemical vapor synthesis

    Energy Technology Data Exchange (ETDEWEB)

    Djenadic, Ruzica; Winterer, Markus, E-mail: markus.winterer@uni-due.de [Universität Duisburg-Essen, Nanoparticle Process Technology, Faculty of Engineering and CENIDE (Germany)

    2017-02-15

    The influence of the time-temperature history on the characteristics of nanoparticles such as size, degree of agglomeration, or crystallinity is investigated for chemical vapor synthesis (CVS). A simple reaction-coagulation-sintering model is used to describe the CVS process, and the results of the model are compared to experimental data. Nanocrystalline titania is used as model material. Titania nanoparticles are generated from titanium-tetraisopropoxide (TTIP) in a hot-wall reactor. Pure anatase particles and mixtures of anatase, rutile (up to 11 vol.%), and brookite (up to 29 vol.%) with primary particle sizes from 1.7 nm to 10.5 nm and agglomerate particle sizes from 24.3 nm to 55.6 nm are formed depending on the particle time-temperature history. An inductively heated furnace with variable inductor geometry is used as a novel system to control the time-temperature profile in the reactor externally covering a large wall temperature range from 873 K to 2023 K. An appropriate choice of inductor geometry, i.e. time-temperature profile, can significantly reduce the degree of agglomeration. Other particle characteristics such as crystallinity are also substantially influenced by the time-temperature profile.

  9. Changes in the pattern of protein synthesis of prosopis chilensis induced by high temperatures

    Energy Technology Data Exchange (ETDEWEB)

    Medina, C.; Cardemil, L. (Univ. de Chile, Santiago (USA))

    1989-04-01

    Seeds of Prosopis chilensis, a leguminous tree from semi-arid regions of Central Chile, were germinated at temperatures of 25-30-35-40-45 and 50{degree}C. Germination was 100% between 25 and 40{degree}C, being faster at 35{degree}C. The best temperature for root growth was also 35{degree}C. There was not germination at 50{degree}C. However, seedlings coming from seeds germinated at 35{degree}C were capable of growing at higher temperatures of 45 and 50{degree}C. Pattern of protein synthesis was followed in roots incubated with {sup 35}S-methionine at increasing temperatures between 35 and 50{degree}C. SDS-PAGE of the proteins followed by fluorography shows that at temperatures above 35{degree}C, new protein bands appear while others become thicker. Most of the protein bands have decreased at 50{degree}C, with the exception of the new bands. A band of 70 KD, that is present at 35{degree}C, is more prominent at 50{degree}C. These proteins may have an important role in the thermotolerance of Prosopis chilensis to stressing temperatures.

  10. Changes in the pattern of protein synthesis of prosopis chilensis induced by high temperatures

    International Nuclear Information System (INIS)

    Medina, C.; Cardemil, L.

    1989-01-01

    Seeds of Prosopis chilensis, a leguminous tree from semi-arid regions of Central Chile, were germinated at temperatures of 25-30-35-40-45 and 50 degree C. Germination was 100% between 25 and 40 degree C, being faster at 35 degree C. The best temperature for root growth was also 35 degree C. There was not germination at 50 degree C. However, seedlings coming from seeds germinated at 35 degree C were capable of growing at higher temperatures of 45 and 50 degree C. Pattern of protein synthesis was followed in roots incubated with 35 S-methionine at increasing temperatures between 35 and 50 degree C. SDS-PAGE of the proteins followed by fluorography shows that at temperatures above 35 degree C, new protein bands appear while others become thicker. Most of the protein bands have decreased at 50 degree C, with the exception of the new bands. A band of 70 KD, that is present at 35 degree C, is more prominent at 50 degree C. These proteins may have an important role in the thermotolerance of Prosopis chilensis to stressing temperatures

  11. Obtaining low temperature catalysts for methanol synthesis by no-waste process

    Energy Technology Data Exchange (ETDEWEB)

    Il' ko, E G; Sushchaya, L E; Bondar' , P G

    1982-11-01

    Low temperature production of catalysts for methanol synthesis involves considerable pollution of the environment as well as formation of side products. The authors propose producing such catalysts from joint precipitates of copper and zinc carbonates includiing stabilizers produced by decomposing solvents, then drying, aging and shaping. This method avoids waste water usually formed in scrubbing to remove ions of alkaline metals. Aluminum hydroxide is suggested as a stabilizer. The catalyst tablets prepared in this way were found to have activity like those produced by other methods, and were suitable for industrial use.

  12. Low temperature solution synthesis of zinc antimonide, manganese antimonide, and strontium ruthenate compounds

    Science.gov (United States)

    Noblitt, Jennifer Lenkner

    2011-12-01

    Increasing energy demands are fueling research in the area of renewable energy and energy storage. In particular, Li-ion batteries and superconducting wires are attractive choices for energy storage. Improving safety, simplifying manufacturing processes, and advancing technology to increase energy storage capacity is necessary to compete with current marketed energy storage devices. These advancements are accomplished through the study of new materials and new morphologies. Increasing dependence on and rising demand for portable electronic devices has continued to drive research in the area of Li-ion batteries. In order to compete with existing batteries and be applicable to future energy needs such as powering hybrid vehicles, the drawbacks of Li-ion batteries must be addressed including (i) low power density, (ii) safety, and (iii) high manufacturing costs. These drawbacks can be addressed through new materials and morphologies for the anode, cathode, and electrolyte. New intermetallic anode materials such as ZnSb, MnSb, and Mn2Sb are attractive candidates to replace graphite, the current industry standard anode material, because they are safer while maintaining comparable theoretical capacity. Electrodeposition is an inexpensive method that could be used for the synthesis of these electrode materials. Direct electrodeposition allows for excellent electrical contact to the current collector without the use of a binder. To successfully electrodeposit zinc and manganese antimonides, metal precursors with excellent solubility in water were needed. To promote solubility, particularly for the antimony precursor, coordinating ligands were added to the deposition bath solutions. This work shows that the choice of coordinating ligand and metal-ligand speciation can alter both the electrochemistry and the film composition. This work focuses on the search for appropriate coordinating ligands, solution pH, and bath temperatures so that high quality films of ZnSb, MnSb, and

  13. Mechanically activated combustion synthesis of molybdenum borosilicides for ultrahigh-temperature structural applications

    Energy Technology Data Exchange (ETDEWEB)

    Esparza, Alan A.; Shafirovich, Evgeny, E-mail: eshafirovich2@utep.edu

    2016-06-15

    The thermal efficiency of gas-turbine power plants could be dramatically increased by the development of new structural materials based on molybdenum silicides and borosilicides, which can operate at temperatures higher than 1300 °C with no need for cooling. A major challenge, however, is to simultaneously achieve high oxidation resistance and acceptable mechanical properties at high temperatures. Materials based on Mo{sub 5}SiB{sub 2} (called T{sub 2}) phase are promising materials that offer favorable combinations of high temperature mechanical properties and oxidation resistance. In the present paper, T{sub 2} phase based materials have been obtained using mechanically activated self-propagating high-temperature synthesis (MASHS). Upon ignition, Mo/Si/B/Ti mixtures exhibited a self-sustained propagation of a spinning combustion wave, but the products were porous, contained undesired secondary phases, and had low oxidation resistance. The “chemical oven” technique has been successfully employed to fabricate denser and stronger Mo{sub 5}SiB{sub 2}–TiC, Mo{sub 5}SiB{sub 2}–TiB{sub 2}, and Mo–Mo{sub 5}SiB{sub 2}–Mo{sub 3}Si materials. Among them, Mo{sub 5}SiB{sub 2}–TiB{sub 2} material exhibits the best oxidation resistance at temperatures up to 1500 °C. - Highlights: • Mechanical activation has enabled combustion synthesis of Mo{sub 5}SiB{sub 2} based materials. • For the first time, the fabrication of Mo{sub 5}SiB{sub 2}–TiB{sub 2} material has been reported. • Among the obtained materials, Mo{sub 5}SiB{sub 2}–TiB{sub 2} exhibits the best oxidation resistance.

  14. Synthesis and characterization of Cu-MFI catalyst for the direct medium temperature range NO decomposition

    Directory of Open Access Journals (Sweden)

    Valkaj Karolina Maduna

    2016-03-01

    Full Text Available In this study the physico-chemical and catalytic properties of copper bearing MFI zeolites (Cu-MFI with different Si/Al and Si/Cu ratios were investigated. Two different methods for incorporation of metal ions into the zeolite framework were used: the ion exchange from the solution of copper acetate and the direct hydrothermal synthesis. Direct synthesis of a zeolite in the presence of copper-phosphate complexes was expected to generate more active copper species necessary for the desired reaction than the conventional ion exchange method. Direct decomposition of NO was used as a model reaction, because this reaction still offers a very attractive approach to NOX removal. The catalytic properties of zeolite samples were studied using techniques, such as XRD, SEM, EPR and nitrogen adsorption/desorption measurements at 77 K. Results of the kinetic investigation revealed that both methods are applicable for the preparation of the catalysts with active sites capable of catalyzing the NO decomposition. It was found out that Cu-MFI zeolites obtained through direct synthesis are promising catalysts for NO decomposition, especially at lower reaction temperatures. The efficiency of the catalysts prepared by both methods is compared and discussed.

  15. Instant synthesis of gold nanoparticles at room temperature and SERS applications

    International Nuclear Information System (INIS)

    Britto Hurtado, R.; Cortez-Valadez, M.; Ramírez-Rodríguez, L.P.; Larios-Rodriguez, Eduardo; Alvarez, Ramón A.B.; Rocha-Rocha, O.; Delgado-Beleño, Y.; Martinez-Nuñez, C.E.; Arizpe-Chávez, H.; Hernández-Martínez, A.R.; Flores-Acosta, M.

    2016-01-01

    Nowadays, gold nanoparticles (AuNps) can be used in a variety of applications, thus efficient methods to produce them are necessary. Several methods have been proposed in this area, but NPs production time is one limitation of these approaches. In this study, we propose a high competitive method to synthesize gold colloidal nanoparticles, instantaneously, using no-toxic reducing agents. These substances allow the instantaneous synthesis at room temperature, even without magnetic stirrers, ovens or ultrasonic baths. Optic analysis showed two absorption bands, associated with surface Plasmon as function of HAuCl_4 concentration. The nanoparticles synthesized have a 10–20 nm size, seen by the transmission electron microscopy (TEM). Therefore, it was possible to obtain several geometric patterns of AuNps, and the synthesis was performed reducing significantly processing time. Additionally, Mie and Fuchs theories were used to predict the location of the absorption bands linked to the plasmon surface in gold nanoparticles. The Surface Enhanced Raman Spectroscopy (SERS) effect was analyzed considering natural zeolite (Chabazite) as analyte, in order to determinate its possible application in soil analysis. - Highlights: • Cubic and spherical morphologies in AuNp. • Surface plasmon prediction in cubic and spherical AuNp. • Instant synthesis of AuNp. • SERS applications in soil analysis.

  16. Effect of reducing agents on low-temperature synthesis of nanostructured LiFePO4

    Science.gov (United States)

    Kulka, Andrzej; Walczak, Katarzyna; Zając, Wojciech; Molenda, Janina

    2017-09-01

    Simple co-precipitation synthesis procedure yielding nanometric LiFePO4 with enhanced electrochemical properties without any post-synthesis heat treatment is presented. XRD, SEM and TEM analysis of the obtained powders revealed platelet crystallites and well crystalized bulk structure. Effective way of decreasing amount of Fe3+ containing phases by addition of reducing agents (KI, (NH4)2S2O3, glucose and the atmosphere of 5%H2-95%Ar) during low-temperature (107 °C) synthesis is described. The traditional analytical chemistry methods or the Mӧssbauer spectroscopy methods revealed that utilization of selected reducing agents diminished Fe3+ concentration from 25 to 12 at%. The constructed cells with optimized LiFePO4 as a cathode material showed superior electrochemical performances, including high reversible capacity up to 162 mAh/g at C/10 current discharge rate, flat voltage plateau with a value close to 3.45 V vs. Li0/+.

  17. Instant synthesis of gold nanoparticles at room temperature and SERS applications

    Energy Technology Data Exchange (ETDEWEB)

    Britto Hurtado, R. [Departamento de Investigación en Física, Universidad de Sonora, Apdo. Postal 5-88, 83190, Hermosillo, Sonora (Mexico); Cortez-Valadez, M., E-mail: jose.cortez@unison.mx [CONACYT-Departamento de Investigación en Física, Universidad de Sonora, Apdo. Postal 5-88, 83190, Hermosillo, Sonora (Mexico); Ramírez-Rodríguez, L.P. [Departamento de Física, Universidad de Sonora, Apdo. Postal 5-88, 83190, Hermosillo, Sonora (Mexico); Larios-Rodriguez, Eduardo [Departamento de Ingeniería Química y Metalurgia, Universidad de Sonora, Rosales y Luis Encinas S/N, Hermosillo, Sonora (Mexico); Alvarez, Ramón A.B.; Rocha-Rocha, O.; Delgado-Beleño, Y.; Martinez-Nuñez, C.E.; Arizpe-Chávez, H. [Departamento de Investigación en Física, Universidad de Sonora, Apdo. Postal 5-88, 83190, Hermosillo, Sonora (Mexico); Hernández-Martínez, A.R. [Centro de Física Aplicada y Tecnología Avanzada (CFATA), Universidad Nacional Autónoma de México, Campus Juriquilla, Querétaro C.P. 76130 (Mexico); Flores-Acosta, M. [Departamento de Investigación en Física, Universidad de Sonora, Apdo. Postal 5-88, 83190, Hermosillo, Sonora (Mexico)

    2016-08-06

    Nowadays, gold nanoparticles (AuNps) can be used in a variety of applications, thus efficient methods to produce them are necessary. Several methods have been proposed in this area, but NPs production time is one limitation of these approaches. In this study, we propose a high competitive method to synthesize gold colloidal nanoparticles, instantaneously, using no-toxic reducing agents. These substances allow the instantaneous synthesis at room temperature, even without magnetic stirrers, ovens or ultrasonic baths. Optic analysis showed two absorption bands, associated with surface Plasmon as function of HAuCl{sub 4} concentration. The nanoparticles synthesized have a 10–20 nm size, seen by the transmission electron microscopy (TEM). Therefore, it was possible to obtain several geometric patterns of AuNps, and the synthesis was performed reducing significantly processing time. Additionally, Mie and Fuchs theories were used to predict the location of the absorption bands linked to the plasmon surface in gold nanoparticles. The Surface Enhanced Raman Spectroscopy (SERS) effect was analyzed considering natural zeolite (Chabazite) as analyte, in order to determinate its possible application in soil analysis. - Highlights: • Cubic and spherical morphologies in AuNp. • Surface plasmon prediction in cubic and spherical AuNp. • Instant synthesis of AuNp. • SERS applications in soil analysis.

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

    Science.gov (United States)

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

    2010-06-01

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

  19. Advantage of low-temperature hydrothermal synthesis to grow stoichiometric crednerite crystals

    Science.gov (United States)

    Poienar, Maria; Martin, Christine; Lebedev, Oleg I.; Maignan, Antoine

    2018-06-01

    This work reports a new approach for the growth of stoichiometric crednerite CuMnO2 crystals. The hydrothermal reaction, starting from soluble metal sulphates as precursors, is assisted by ethylene glycol and the formation of crednerite is found to depend strongly on pH and temperature. This method allows obtaining small hexagonal platelets with the larger dimension about 1.0-1.5 μm and with a composition characterized by a Cu/Mn ratio of 1. Thus, these crystals differ from the needle-like millimetric ones obtained by the flux technique for which the composition departs from the expected one and is close to Cu1.04Mn0.96. This monitoring of the cationic composition in crednerite, using hydrothermal synthesis, is important as the Cu/Mn ratio controls the low temperature antiferromagnetic ground-state.

  20. Droplet-fused microreactors for room temperature synthesis of nanoscale needle-like hydroxyapatite

    International Nuclear Information System (INIS)

    Liu Kaiying; Qin Jianhua

    2013-01-01

    A microfluidic device using droplet-fused microreactors is introduced for room temperature synthesis of nanoscale needle-shaped hydroxyapatite (HAp, Ca 10 (PO 4 ) 6 (OH) 2 ). The device is integrated with multifunctional units, e.g., T-junctions for droplet generation and fusion, winding channels for rapid mixing, and a delay line for simple visualization of the HAp formation process. The necessary conditions such as surfactant and fluid flow rate for an aqueous stream to merge with water-in-oil droplets are investigated. The nanoscale morphologies of the HAp produced by this method are also compared with HAp prepared by conventional bulk mixing. This paper shows that further reaction could be initiated by flowing additional reagent streams directly into the droplets of the initial reaction mixture, which is a novel approach for synthesizing a needle-like morphology of the HAp with a high aspect ratio under room temperature. (paper)

  1. Influence of temperature on the synthesis of calcining cement α--tricalcium phosphate

    International Nuclear Information System (INIS)

    Vieira, R.S.; Thurmer, M.B.; Coelho, W.T.; Fernandes, J.M.; Santos, L.A.

    2011-01-01

    The calcium phosphate cement (CFCs) bone substitutes are of great potential use in medical and dental. However, one of the great difficulties of using this type of cement is its low mechanical strength due to the presence of undesirable phases, such as beta-tricalcium phosphate. The step of obtaining this compound is done at high temperature by solid state reaction. With the aim of obtaining calcium phosphate cements more resistant, we studied the conditions for obtaining an alpha-TCP at temperatures of 1300, 1400 and 1500 ° C with time 2h calcination. The samples were analyzed for crystalline phases, density, porosity and mechanical strength. The results show that the synthesis parameters studied strongly influence the obtained phases and the mechanical properties of cement. (author)

  2. High-Pressure High-Temperature Phase Diagram of the Organic Crystal Paracetamol

    Science.gov (United States)

    Smith, Spencer; Montgomery, Jeffrey; Vohra, Yogesh

    High-pressure high-temperature (HPHT) Raman spectroscopy studies have been performed on the organic crystal paracetamol in a diamond anvil cell utilizing boron-doped diamond as heating anvil. The HPHT data obtained from boron-doped diamond heater is cross-checked with data obtained using a standard block heater diamond anvil cell. Isobaric measurements were conducted at pressures up to 8.5 GPa and temperature up to 520 K in a number of different experiments. Solid state phase transitions from monoclinic Form I --> orthorhombic Form II were observed at various pressures and temperatures as well as transitions from Form II --> unknown Form IV. The melting temperature for paracetamol was observed to increase with increasing pressures to 8.5 GPa. Our previous angle dispersive x-ray diffraction studies at the Advanced Photon Source has confirmed the existence of two unknown crystal structures Form IV and Form V of paracetamol at high pressure and ambient temperature. The phase transformation from Form II to Form IV occurs at ~8.5 GPa and from Form IV to Form V occurs at ~11 GPa at ambient temperature. Our new data is combined with the previous ambient temperature high-pressure Raman and X- ray diffraction data to create the first HPHT phase diagram of paracetamol. Doe-NNSA Carnegie DOE Alliance Center (CDAC) under Grant Number DE-NA0002006.

  3. Low-temperature synthesis of nanocrystalline ZrC coatings on flake graphite by molten salts

    Energy Technology Data Exchange (ETDEWEB)

    Ding, Jun, E-mail: dingjun@wust.edu.cn; Guo, Ding; Deng, Chengji; Zhu, Hongxi; Yu, Chao

    2017-06-15

    Highlights: • Uniform ZrC coatings are prepared on flake graphite at 900 °C. • ZrC coatings are composed of nanosized (30–50 nm) particles. • The template growth mechanism is believed to be dominant in the molten salt synthesis process. - Abstract: A novel molten salt synthetic route has been developed to prepare nanocrystalline zirconium carbide (ZrC) coatings on flake graphite at 900 °C, using Zr powder and flake graphite as the source materials in a static argon atmosphere, along with molten salts as the media. The effects of different molten salt media, the sintered temperature, and the heat preservation time on the phase and microstructure of the synthetic materials were investigated. The ZrC coatings formed on the flake graphite were uniform and composed of nanosized particles (30–50 nm). With an increase in the reaction temperature, the ZrC nanosized particles were more denser, and the heat preservation time and thickness of the ZrC coating also increased accordingly. Electron microscopy was used to observe the ZrC coatings on the flake graphite, indicating that a “template mechanism” played an important role during the molten salt synthesis.

  4. Synthesis of Li2SiO3 at low temperature

    International Nuclear Information System (INIS)

    Mondragon G, G.

    2007-01-01

    The main objective of this work is to develop a new synthesis method to obtain one of the more studied ceramics in this field Li 2 SiO 3 ) in a simple and economic way using different solutions (urea and ammonium hydroxide). The particular objectives are first to prepare the Li 2 SiO 3 ceramic, by means of the use of the reaction conventional technique in solid state at temperatures between 800 and 900 C to compare it with the one proposed in this work and this way to observe the advantages that it would gives us the new method. Later on, the same one was synthesized lithium ceramic (Li 2 SiO 3 ) by means of the new method at low temperature (between 80 and 90 C), using silicic acid and lithium hydroxide like precursory reagents and different solutions (urea and ammonium hydroxide) for the optimization in their synthesis. Finally, it was carried out the characterization of these materials by means of X-ray diffraction (XRD), electronic microscopes (SEM and TEM), nitrogen physisorption (method BET) and thermal gravimetric analysis (TGA) to observe the differences that exist among the conventional method and the proposed method and by this way to determine the advantages of the last method. (Author)

  5. The Role of Solvent Polarity on Low-Temperature Methanol Synthesis Catalyzed by Cu Nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Ahoba-Sam, Christian [Department of Process, Energy and Environmental Technology, University College of Southeast Norway, Porsgrunn (Norway); Olsbye, Unni [Department of Chemistry, University of Oslo, Oslo (Norway); Jens, Klaus-Joachim, E-mail: Klaus.J.Jens@usn.no [Department of Process, Energy and Environmental Technology, University College of Southeast Norway, Porsgrunn (Norway)

    2017-07-14

    Methanol syntheses at low temperature in a liquid medium present an opportunity for full syngas conversion per pass. The aim of this work was to study the role of solvents polarity on low-temperature methanol synthesis reaction using eight different aprotic polar solvents. A “once through” catalytic system, which is composed of Cu nanoparticles and sodium methoxide, was used for methanol synthesis at 100°C and 20 bar syngas pressure. Solvent polarity rather than the 7–10 nm Cu (and 30 nm Cu on SiO{sub 2}) catalyst used dictated trend of syngas conversion. Diglyme with a dielectric constant (ε) = 7.2 gave the highest syngas conversion among the eight different solvents used. Methanol formation decreased with either increasing or decreasing solvent ε value of diglyme (ε = 7.2). To probe the observed trend, possible side reactions of methyl formate (MF), the main intermediate in the process, were studied. MF was observed to undergo two main reactions; (i) decarbonylation to form CO and MeOH and (ii) a nucleophilic substitution to form dimethyl ether and sodium formate. Decreasing polarity favored the decarbonylation side reaction while increasing polarity favored the nucleophilic substitution reaction. In conclusion, our results show that moderate polarity solvents, e.g., diglyme, favor MF hydrogenolysis and, hence, methanol formation, by retarding the other two possible side reactions.

  6. Heat-equilibrium low-temperature plasma decay in synthesis of ammonia via transient components N2H6

    International Nuclear Information System (INIS)

    Cao Guobin; Song Youqun; Chen Qing; Zhou Qiulan; Cao Yun; Wang Chunhe

    2001-01-01

    The author introduced a new method of heat-equilibrium low-temperature plasma in ammonia synthesis and a technique of continuous real-time inlet sampling mass-spectrometry to detect the reaction channel and step of the decay of transient component N 2 H 6 into ammonia. The experimental results indicated that in the process of ammonia synthesis by discharge of N 2 and H 2 mixture, the transient component N 2 H 6 is a necessary step

  7. Rheological assessment of nanofluids at high pressure high temperature

    Science.gov (United States)

    Kanjirakat, Anoop; Sadr, Reza

    2013-11-01

    High pressure high temperature (HPHT) fluids are commonly encountered in industry, for example in cooling and/or lubrications applications. Nanofluids, engineered suspensions of nano-sized particles dispersed in a base fluid, have shown prospective as industrial cooling fluids due to their enhanced rheological and heat transfer properties. Nanofluids can be potentially utilized in oil industry for drilling fluids and for high pressure water jet cooling/lubrication in machining. In present work rheological characteristics of oil based nanofluids are investigated at HPHT condition. Nanofluids used in this study are prepared by dispersing commercially available SiO2 nanoparticles (~20 nm) in a mineral oil. The basefluid and nanofluids with two concentrations, namely 1%, and 2%, by volume, are considered in this investigation. The rheological characteristics of base fluid and the nanofluids are measured using an industrial HPHT viscometer. Viscosity values of the nanofluids are measured at pressures of 100 kPa to 42 MPa and temperatures ranging from 25°C to 140°C. The viscosity values of both nanofluids as well as basefluid are observed to have increased with the increase in pressure. Funded by Qatar National Research Fund (NPRP 08-574-2-239).

  8. The facile and low temperature synthesis of nanophase hydroxyapatite crystals using wet chemistry

    International Nuclear Information System (INIS)

    Dhand, Vivek; Rhee, K.Y.; Park, Soo-Jin

    2014-01-01

    A simple and facile wet chemistry route was used to synthesize nanophase hydroxyapatite (HaP) crystals at low temperature. The synthesis was carried out at a pH of 11.0 and at a temperature of 37 °C. The resulting samples were washed several times and subjected to further analysis. XRD studies revealed that the HaP crystals were polycrystalline in nature with a crystallite size of ∼ 15–60 ± 5 nm. SEM-EDXA images confirmed the presence of calcium (Ca), phosphorous (P), and oxygen (O) peaks. Likewise, FTIR confirmed the presence of characteristic phosphate and hydroxyl peaks in samples. Lastly, HRTEM images clearly showed distinctive lattice fringes positioned in the 100 and 002 planes. TGA analysis shows that HaP crystals can withstand higher calcination temperatures and are thermally stable. - Highlights: • Facile and low temperature nanophase HaP crystals synthesized at pH 11 and 37 °C • Electron microscopy image of HaP shows characteristic rice grain like morphology. • FTIR results show the characteristic and fingerprint functional groups of HaP. • Thermal stability of HaP crystals up to 500 °C • Growth of Hap crystals occur parallel to c-axis and a possible mechanism proposed

  9. Novel low temperature synthesis of spinel nano-magnesium chromites from secondary resources

    Energy Technology Data Exchange (ETDEWEB)

    El-Sheikh, S.M., E-mail: selsheikh2001@gmail.com [Nanostructured Materials Laboratory, Advanced Material Department, Central Metallurgical R and D Institute (CMRDI), P.O. Box 78, Helwan, 11421 Cairo (Egypt); Rabbah, M., E-mail: mahmoud.rabah@ymail.com [Electrochemical and Chemical Treatment Laboratory, Minerals Department, Central Metallurgical R and D Institute (CMRDI), P.O. Box 78, Helwan, 11421 Cairo (Egypt)

    2013-09-20

    Graphical abstract: FE-SEM micrograph and TEM image of magnesium chromite sample heated at 500 °C. - Highlights: • No study has been reported to prepare spinel magnesium chromite form waste resources. • Novel low synthesis temperature of magnesium chromite. • Selective removal of Ca ions from industrial waste tannery solution is rarely reported. • The method applied is simple and safe. - Abstract: A novel low temperature method for synthesis of nano-crystalline magnesium chromites from the tannery waste solution was investigated. Magnesium and chromium hydroxides gel was co-precipitated at pH 8.5 using ammonia solution. MgCr{sub 2}O{sub 4} was obtained by heating the gel formed at different temperatures 300–500 °C for to 8 h. FT-IR, TG-DTG-DTA, FE-SEM and TEM were used to investigate the produced materials. XRD patterns of the primary oxides revealed the formation of amorphous oxide phase by heating at 300 °C. Heating at 400 °C produces nano-crystallite magnesium chromites partly having the structure MgCrO{sub 4} and mainly MgCr{sub 2}O{sub 4} and traces of Cr{sub 2}O{sub 3}{sup +} 500 °C MgCrO{sub 4} mostly decomposed into MgCr{sub 2}O{sub 4} structure{sub .} After 8 h of heating at 500 °C, Cr{sub 2}O{sub 3} completely disappeared. A high surface area about 42.6 m{sup 2}/g and mesoporous structure was obtained for the produced sample at 500 °C for 8 h. A thermodynamic model has been suggested to explain the findings.

  10. Surface-Bound Intermediates in Low-Temperature Methanol Synthesis on Copper. Participants and Spectators

    Energy Technology Data Exchange (ETDEWEB)

    Yang, Yong; Mei, Donghai; Peden, Charles HF; Campbell, Charles T.; Mims, Charles A.

    2015-11-03

    The reactivity of surface adsorbed species present on copper catalysts during methanol synthesis at low temperatures was studied by simultaneous infrared spectroscopy (IR) and mass spectroscopy (MS) measurements during “titration” (transient surface reaction) experiments with isotopic tracing. The results show that adsorbed formate is a major bystander species present on the surface under steady-state methanol synthesis reaction conditions, but it cannot be converted to methanol by reaction with pure H2, nor with H2 plus added water. Formate-containing surface adlayers for these experiments were produced during steady state catalysis in (a) H2:CO2 (with substantial formate coverage) and (b) moist H2:CO (with no IR visible formate species). Both these reaction conditions produce methanol at steady state with relatively high rates. Adlayers containing formate were also produced by (c) formic acid adsorption. Various "titration" gases were used to probe these adlayers at modest temperatures (T = 410-450K) and 6 bar total pressure. Methanol gas (up to ~1% monolayer equivalent) was produced in "titration" from the H2:CO2 catalytic adlayers by H2 plus water, but not by dry hydrogen. The decay in the formate IR features accelerated in the presence of added water vapor. The H2:CO:H2O catalytic adlayer produced similar methanol titration yields in H2 plus water but showed no surface formate features in IR (less than 0.2% monolayer coverage). Finally, formate from formic acid chemisorption produced no methanol under any titration conditions. Even under (H2:CO2) catalytic reaction conditions, isotope tracing showed that pre-adsorbed formate from formic acid did not contribute to the methanol produced. Although non-formate intermediates exist during low temperature methanol synthesis on copper which can be converted to methanol gas

  11. Timing matters: the underappreciated role of temperature ramp rate for shape control and reproducibility of quantum dot synthesis

    KAUST Repository

    Baumgardner, William J.

    2012-01-01

    Understanding the coupled kinetic and thermodynamics factors governing colloidal nanocrystals nucleation and growth are critical factors in the predictable and reproducible synthesis of advanced nanomaterials. We show that the temporal temperature profile is decisive in tuning the particle shape from pseudo-spherical to monodisperse cubes. The shape of the nanocrystals was characterized by transmission electron microscopy and X-ray diffraction. We introduce a mechanism for the shape controlled synthesis in the context of temperature-dependent nucleation and growth and provide experimental evidence to support it. © 2013 The Royal Society of Chemistry.

  12. Carbon Isotope Systematics in Mineral-Catalyzed Hydrothermal Organic Synthesis Processes at High Temperature and Pressures

    Science.gov (United States)

    Fu, Qi; Socki, R. A.; Niles, Paul B.

    2011-01-01

    Observation of methane in the Martian atmosphere has been reported by different detection techniques. Reduction of CO2 and/or CO during serpentization by mineral surface catalyzed Fischer-Tropsch Type (FTT) synthesis may be one possible process responsible for methane generation on Mars. With the evidence a recent study has discovered for serpentinization in deeply buried carbon rich sediments, and more showing extensive water-rock interaction in Martian history, it seems likely that abiotic methane generation via serpentinization reactions may have been common on Mars. Experiments involving mineral-catalyzed hydrothermal organic synthesis processes were conducted at 750 C and 5.5 Kbars. Alkanes, alcohols and carboxylic acids were identified as organic compounds. No "isotopic reversal" of delta C-13 values was observed for alkanes or carboxylic acids, suggesting a different reaction pathway than polymerization. Alcohols were proposed as intermediaries formed on mineral surfaces at experimental conditions. Carbon isotope data were used in this study to unravel the reaction pathways of abiotic formation of organic compounds in hydrothermal systems at high temperatures and pressures. They are instrumental in constraining the origin and evolution history of organic compounds on Mars and other planets.

  13. Low temperature synthesis of hydroxyapatite nano-rods by a modified sol-gel technique

    International Nuclear Information System (INIS)

    Jadalannagari, Sushma; More, Sandeep; Kowshik, Meenal; Ramanan, Sutapa Roy

    2011-01-01

    Hydroxyapatite (HAp) nano-rods were successfully synthesized by a modified sol-gel method using a solution of CaCl 2 .2H 2 O in water, along with a solution of H 3 PO 4 in triethylamine and NH 4 OH as starting materials. The Ca/P molar ratio was maintained at 1.67. The sol obtained was dried in an oven for 2 days at 100 deg. C after being dialyzed for 12 h. Pellets were made from the crystalline powders and immersed in simulated body fluid (SBF) to check its biocompatibility after 15, 45 and 180 days of immersion. The HAp powders and pellets were characterized by X-Ray Diffraction crystallography (XRD), Fourier transform Infrared spectroscopy (FTIR), scanning electron microscopy (SEM), and Transmission electron microscopy (TEM). The HAp nano-rods had an average diameter of 25 nm and length 110-120 nm. Immersion of the HAp pellets in SBF led to the formation of a highly porous interconnecting HAp layer on the surface. The porosity increased with increase in immersion time. Highlights: → Low temperature synthesis of hydroxyapatite nanorods using Ca and P sources and triethylamine. → The synthesis time was only 0.5 hours. → Crystalline material was obtained after drying at 100oC only in air. → SBF studies showed the HAP bodies to be biocompatible.

  14. Low Temperature Solid-State Synthesis and Characterization of LaBO3

    Directory of Open Access Journals (Sweden)

    Azmi Seyhun KIPÇAK

    2016-11-01

    Full Text Available Rare earth (lanthanide series borates, possess high vacuum ultraviolet (VUV transparency, large electronic band gaps, chemical and environmental stability and exceptionally large optical damage thresholds and used in the development of plasma display panels (PDPs. In this study the synthesis of lanthanum borates via solid-state method is studied. For this purpose, lanthanum oxide (La2O3 and boric acid (H3BO3 are used for as lanthanum and boron sources, respectively. Different elemental molar ratios of La to B (between 3:1 to 1:6 as La2O3:H3BO3 were reacted by solid-state method at the reaction temperatures between 500°C - 700°C with the constant reaction time of 4 h. Following the synthesis, characterizations of the synthesized products are conducted by X-ray diffraction (XRD, Fourier transform infrared spectroscopy (FT-IR, Raman spectroscopy and scanning electron microscope (SEM. From the results of the experiments, three types of lanthanum borates of; La3BO6, LaBO3 and La(BO23 were observed at different reaction parameters. Among these three types of lanthanum borates LaBO3 phase were obtained as a major phase.

  15. Mechanical alloying and self-propagating high-temperature synthesis of stable icosahedral quasicrystals

    International Nuclear Information System (INIS)

    Bokhonov, B.B.

    2008-01-01

    The phase evolution of the mechanically alloyed ternary 63%Al + 25%Cu + 12%Fe and 65%Al + 20%Cu + 15%Fe powder mixtures with milling time has been studied by X-ray diffraction method. It was found that an icosahedral quasicrystalline phase was formed directly during high-energy ball milling of the Al-Cu-Fe mixtures. The X-ray and scanning electron microscopic investigations demonstrated the possibility to use self-propagating high-temperature synthesis (SHS) in combination with preliminary mechanical activation for the synthesis of stable icosahedral quasicrystals. The typical morphology of the Al 63 Cu 25 Fe 12 icosahedral quasicrystals formed in the SHS process is a pentagonal dodecahedron with a size of 3-5 mm. The phase composition of the SHS products depends on the time of preliminary mechanical activation. The content of cubic intermetallic phase in SHS products increases with the time of preliminary mechanical activation of the 63%Al + 25%Cu + 12%Fe powder mixtures

  16. Cuprous Oxide Scale up: Gram Production via Bulk Synthesis using Classic Solvents at Low Temperatures

    Energy Technology Data Exchange (ETDEWEB)

    Hall, A. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States); Han, T. Y. [Lawrence Livermore National Lab. (LLNL), Livermore, CA (United States)

    2015-05-07

    Cuprous oxide is a p-type semiconducting material that has been highly researched for its interesting properties. Many small-scale syntheses have exhibited excellent control over size and morphology. As the demand for cuprous oxide grows, the synthesis method need to evolve to facilitate large-scale production. This paper supplies a facile bulk synthesis method for Cu₂O on average, 1-liter reaction volume can produce 1 gram of particles. In order to study the shape and size control mechanisms on such a scale, the reaction volume was diminished to 250 mL producing on average 0.3 grams of nanoparticles per batch. Well-shaped nanoparticles have been synthesized using an aqueous solution of CuCl₂, NaOH, SDS surfactant, and NH₂OH-HCl at mild temperatures. The time allotted between the addition of NaOH and NH₂OH-HCl was determined to be critical for Cu(OH)2 production, an important precursor to the final produce The effects of stirring rates on a large scale was also analyzed during reagent addition and post reagent addition. A morphological change from rhombic dodecahedra to spheres occurred as the stirring speed was increased. The effects of NH₂OH-HCl concentration were also studied to control the etching effects of the final product.

  17. Room-Temperature Synthesis of Thiostannates from {[Ni(tren)]2[Sn2S6]}n.

    Science.gov (United States)

    Hilbert, Jessica; Näther, Christian; Weihrich, Richard; Bensch, Wolfgang

    2016-08-15

    The compound {[Ni(tren)]2[Sn2S6]}n (1) (tren = tris(2-aminoethyl)amine, C6H18N4) was successfully applied as source for the room-temperature synthesis of the new thiostannates [Ni(tren)(ma)(H2O)]2[Sn2S6]·4H2O (2) (ma = methylamine, CH5N) and [Ni(tren)(1,2-dap)]2[Sn2S6]·2H2O (3) (1,2-dap = 1,2-diaminopropane, C3H10N2). The Ni-S bonds in the Ni2S2N8 bioctahedron in the structure of 1 are analyzed with density functional theory calculations demonstrating significantly differing Ni-S bond strengths. Because of this asymmetry they are easily broken in the presence of an excess of ma or 1,2-dap immediately followed by Ni-N bond formation to N donor atoms of the amine ligands thus generating [Ni(tren)(amine)](2+) complexes. The chemical reactions are fast, and compounds 2 and 3 are formed within 1 h. The synthesis concept presented here opens hitherto unknown possibilities for preparation of new thiostannates.

  18. Room temperature synthesis of ReS2 through aqueous perrhenate sulfidation.

    Science.gov (United States)

    Borowiec, Joanna; Gillin, William P; Willis, Maureen; Boi, Filippo; He, Yi; Wen, Jiqiu; Wang, Shanling; Schulz, Leander

    2017-12-29

    In this study, a direct sulfidation reaction of ammonium perrhenate (NH4ReO4) leading to a synthesis of rhenium disulfide (ReS2) is demonstrated. These finding reveal the first example of a simplistic bottom-up approach to the chemical synthesis of crystalline ReS2. The reaction presented here takes place at room temperature, in an ambient and solvent-free environment and without the necessity of a catalyst. The atomic composition and structure of the as-synthesized product were characterized using several analysis techniques including energy dispersive X-ray (EDX) spectroscopy, X-ray photoelectron spectroscopy (XPS), X-ray diffraction (XRD), transmission electron microscopy (TEM), Raman spectroscopy, thermogravimetric analysis (TGA) and differential scannig calorimetry (DSC). The results indicated the formation of a lower symmetry (1Td) ReS2 with a low degree of layer stacking. © 2017 IOP Publishing Ltd.

  19. An Investigation of Porous Structure of TiNi-Based SHS-Materials Produced at Different Initial Synthesis Temperatures

    Science.gov (United States)

    Khodorenko, V. N.; Anikeev, S. G.; Kokorev, O. V.; Yasenchuk, Yu. F.; Gunther, V. É.

    2018-02-01

    An investigation of structural characteristics and behavior of TiNi-based pore-permeable materials manufactured by the methods of selfpropagating high-temperature synthesis (SHS) at the initial synthesis temperatures T = 400 and 600°C is performed. It is shown that depending on the temperature regime, the resulting structure and properties of the material can differ. It is found out that the SHS-material produced at the initial synthesis temperature T = 400°C possesses the largest number of micropores in the pore wall surface structure due to a high phase inhomogeneity of the alloy. The regime of structure optimization of the resulting materials is described and the main stages of formation of the pore wall microporous surfaces are revealed. It is demonstrated that after optimization of the surface structure of a TiNi-based fine-pore alloy by its chemical etching, the fraction of micropores measuring in size less than 50 nm increased from 59 to 68%, while the number of pores larger than 1 μm increased twofold from 11 to 22%. In addition, peculiar features of interaction between certain cell cultures with the surface of the SHS-material manufactured at different initial synthesis temperatures are revealed. It is found out that the dynamics of the cell material integration depends on the pore wall surface morphology and dimensions of macropores.

  20. Low temperature synthesis and field emission characteristics of single to few layered graphene grown using PECVD

    Energy Technology Data Exchange (ETDEWEB)

    Kumar, Avshish; Khan, Sunny; Zulfequar, M.; Harsh; Husain, Mushahid, E-mail: mush_reslab@rediffmail.com

    2017-04-30

    Highlights: • Graphene was synthesized by PECVD system at a low temperature of 600 °C. • From different characterization techniques, the presence of single and few layered graphene was confirmed. • X-ray diffraction pattern of the graphene showed single crystalline nature of the film. • The as-grown graphene films were observed extremely good field emitters with long term emission current stability. - Abstract: In this work, high-quality graphene has successfully been synthesized on copper (Cu) coated Silicon (Si) substrate at very large-area by plasma enhanced chemical vapor deposition system. This method is low cost and highly effective for synthesizing graphene relatively at low temperature of 600 °C. Electron microscopy images have shown that surface morphology of the grown samples is quite uniform consisting of single layered graphene (SLG) to few layered graphene (FLG). Raman spectra reveal that graphene has been grown with high-quality having negligible defects and the observation of G and G' peaks is also an indicative of stokes phonon energy shift caused due to laser excitation. Scanning probe microscopy image also depicts the synthesis of single to few layered graphene. The field emission characteristics of as-grown graphene samples were studied in a planar diode configuration at room temperature. The graphene samples were observed to be a good field emitter having low turn-on field, higher field amplification factor and long term emission current stability.

  1. Silver nanoparticles: Influence of the temperature synthesis on the particles’ morphology

    International Nuclear Information System (INIS)

    Piñero, S; Camero, S; Blanco, S

    2017-01-01

    Silver nanoparticles have a wide range of applications in the medical field, textile and food industries. These and other applications can be found due to the relation between its size and morphology. In this study the influence of bath temperature on the morphology and size of silver nanoparticles are evaluated, which are obtained by chemical reduction of AgNO 3 using three reducing agents: sodium borohydride, ascorbic acid and sodium citrate. The evaluation carried out by the traditional UV-vis Spectrophotometric analysis and with High Resolution Transmission Electron Microscopy. The UV-vis spectrum of the silver colloids obtained by chemical reduction using three different reducing agents shows the effect of the temperature change on the growing and aggregative process. The final effect on the morphology, size and aggregation of the particles was confirmed by TEM. The result suggests a change in the growing mechanism, conducted by aggregation of atoms at 5 and 20°C degrees and aggregation of clusters at higher temperatures. Moreover in this work the main synthesis methods of nanomaterials are described. (paper)

  2. Synthesis and characterization of nickel oxide particulate annealed at different temperatures

    Science.gov (United States)

    Sharma, Khem Raj; Thakur, Shilpa; Negi, N. S.

    2018-04-01

    Nickel oxide has been synthesized by solution combustion technique. The nickel oxide ceramic was annealed at 600°C and 1000°C for 2 hours. Structural, electrical, dielectric and magnetic properties were analyzed which are strongly dependent upon the synthesis method. Structural properties were examined by X-ray diffractometer (XRD), which confirmed the purity and cubic phase of nickel oxide. XRD data reveals the increase in crystallite size and decrease in full width half maximum (FWHM) as the annealing temperature increases. Electrical conductivity is found to increase from 10-6 to 10-5 (Ω-1cm-1) after annealing. Dielectric constant is observed to increase from 26 to 175 when the annealing temperature is increased from 600°C to 1000°C. Low value of coercive field is found which shows weak ferromagnetic behavior of NiO. It is observed that all the properties of NiO particulate improve with increasing annealing temperature.

  3. Low temperature synthesis & characterization of lead-free BCZT ceramics using molten salt method

    Science.gov (United States)

    Jai Shree, K.; Chandrakala, E.; Das, Dibakar

    2018-04-01

    Piezoelectric properties are greatly influenced by the synthesis route, microstructure, stoichiometry of the chemical composition, purity of the starting materials. In this study, molten salt method was used to prepare lead-free BCZT ceramics. Molten salt method is one of the simplestmethods to prepare chemically-purified, single phase powders in high yield often at lower temperatures and shorten reaction time. Calcination of the molten salt synthesized powders resulted in asingle-phase perovskite structure at 1000 °C which is ˜ 350 °C less than the conventional solid-sate reaction method. With increasing calcination temperature the average template size was increased (˜ 0.5-2 µm). Formation of well dispersive templates improves the sinterability at lower temperatures. Lead-free BCZT ceramics sintered at 1500 °C for 2 h resulted in homogenous and highly dense microstructure with ˜92% of the theoretical density and a grain size of ˜ 35 µm. This highly dense microstructure could enhance the piezoelectric properties of the system.

  4. Room temperature synthesis of 2D CuO nanoleaves in aqueous solution

    International Nuclear Information System (INIS)

    Zhao Yan; Li Yunling; Wang Zichen; Zhao Jingzhe; Ma Dechong; Hou Shengnan; Li Linzhi; Hao Xinli

    2011-01-01

    A simple room temperature method was reported for the synthesis of CuO nanocrystals in aqueous solution through the sequence of Cu 2+ → Cu(OA) 2 → Cu(OH) 2 → Cu(OH) 4 2- → CuO. Sodium oleate (SOA) was used as the surfactant and shape controller. The as-prepared samples were characterized by x-ray diffraction (XRD), scanning electron microscopy (SEM), UV-visible absorption spectroscopy (UV-vis) and differential thermal analysis (DTA). It can be seen that 1D Cu(OH) 2 nanowires were first obtained from Cu(OA) 2 and, at room temperature, converted into 2D CuO nanoleaves (CuO NLs) in a short time under a weakly basic environment. On prolonging the reaction time, the top part of these 2D nanoleaves branched and separated along the long axis to form 1D rod-like nano-CuO because of the assistance of SOA. A possible transformation mechanism of Cu(OH) 2 to CuO nanostructures at room temperature in aqueous solution is discussed. The transformation velocity can be controlled by changing the pH value of the system. The prepared CuO NLs were used to construct an enzyme-free glucose sensor. The detecting results showed that the designed sensor exhibited good amperometric responses towards glucose with good anti-interferent ability.

  5. Low-temperature direct synthesis of mesoporous vanadium nitrides for electrochemical capacitors

    Energy Technology Data Exchange (ETDEWEB)

    Lee, Hae-Min [Institute of NT-IT Fusion Technology, Ajou University, 206 Worldcup-ro, Yeongtong-gu, Suwon 16499 (Korea, Republic of); Jeong, Gyoung Hwa [Department of Chemistry, Ulsan National Institute of Science and Technology (UNIST), Banyeon 100, Ulsan 44919 (Korea, Republic of); Kim, Sang-Wook [Department of Molecular Science and Technology, Ajou University, 206 Worldcup-ro, Yeongtong-gu, Suwon 16499 (Korea, Republic of); Kim, Chang-Koo, E-mail: changkoo@ajou.ac.kr [Department of Chemical Engineering and Department of Energy Systems Research, Ajou University, 206 Worldcup-ro, Yeongtong-gu, Suwon 16499 (Korea, Republic of)

    2017-04-01

    Highlights: • Vanadium nitrides were directly synthesized by a one-step chemical precipitation method. • This method was carried out at a low temperature of 70 °C. • Vanadium nitrides had a specific capacitance of 598 F/g. • The equivalent series resistance of the vanadium nitride electrode was 1.42 Ω after 5000 cycles. - Abstract: Mesoporous vanadium nitrides are directly synthesized by a one-step chemical precipitation method at a low temperature (70 °C). Structural and morphological analyses reveal that vanadium nitride consist of long and slender nanowhiskers, and mesopores with diameters of 2–5 nm. Compositional analysis confirms the presence of vanadium in the VN structure, along with oxidized vanadium. The cyclic voltammetry and charge-discharge tests indicate that the obtained material stores charges via a combination of electric double-layer capacitance and pseudocapacitance mechanisms. The vanadium nitride electrode exhibits a specific capacitance of 598 F/g at a current density of 4 A/g. After 5000 charge-discharge cycles, the electrode has an equivalent series resistance of 1.42 Ω and retains 83% of its initial specific capacitance. This direct low-temperature synthesis of mesoporous vanadium nitrides is a simple and promising method to achieve high specific capacitance and low equivalent series resistance for electrochemical capacitor applications.

  6. Synthesis of high saturation magnetic iron oxide nanomaterials via low temperature hydrothermal method

    Energy Technology Data Exchange (ETDEWEB)

    Bhavani, P.; Rajababu, C.H. [Department of Materials Science & Nanotechnology, Yogivemana University, Vemanapuram 516003, Kadapa (India); Arif, M.D. [Environmental Magnetism Laboratory, Indian Institute of Geomagnetism (IIG), Navi Mumbai 410218, Mumbai (India); Reddy, I. Venkata Subba [Department of Physics, Gitam University, Hyderabad Campus, Rudraram, Medak 502329 (India); Reddy, N. Ramamanohar, E-mail: manoharphd@gmail.com [Department of Materials Science & Nanotechnology, Yogivemana University, Vemanapuram 516003, Kadapa (India)

    2017-03-15

    Iron oxide nanoparticles (IONPs) were synthesized through a simple low temperature hydrothermal approach to obtain with high saturation magnetization properties. Two series of iron precursors (sulfates and chlorides) were used in synthesis process by varying the reaction temperature at a constant pH. The X-ray diffraction pattern indicates the inverse spinel structure of the synthesized IONPs. The Field emission scanning electron microscopy and high resolution transmission electron microscopy studies revealed that the particles prepared using iron sulfate were consisting a mixer of spherical (16–40 nm) and rod (diameter ~20–25 nm, length <100 nm) morphologies that synthesized at 130 °C, while the IONPs synthesized by iron chlorides are found to be well distributed spherical shapes with size range 5–20 nm. On other hand, the IONPs synthesized at reaction temperature of 190 °C has spherical (16–46 nm) morphology in both series. The band gap values of IONPs were calculated from the obtained optical absorption spectra of the samples. The IONPs synthesized using iron sulfate at temperature of 130 °C exhibited high saturation magnetization (M{sub S}) of 103.017 emu/g and low remanant magnetization (M{sub r}) of 0.22 emu/g with coercivity (H{sub c}) of 70.9 Oe{sub ,} which may be attributed to the smaller magnetic domains (d{sub m}) and dead magnetic layer thickness (t). - Highlights: • Comparison of iron oxide materials prepared with Fe{sup +2}/Fe{sup +3} sulfates and chlorides at different temperatures. • We prepared super-paramagnetic and soft ferromagnetic magnetite nanoparticles. • We report higher saturation magnetization with lower coercivity.

  7. Low-temperature synthesis of actinide tetraborides by solid-state metathesis reactions

    Science.gov (United States)

    Lupinetti, Anthony J [Los Alamos, NM; Garcia, Eduardo [Los Alamos, NM; Abney, Kent D [Los Alamos, NM

    2004-12-14

    The synthesis of actinide tetraborides including uranium tetraboride (UB.sub.4), plutonium tetraboride (PuB.sub.4) and thorium tetraboride (ThB.sub.4) by a solid-state metathesis reaction are demonstrated. The present method significantly lowers the temperature required to .ltoreq.850.degree. C. As an example, when UCl.sub.4 is reacted with an excess of MgB.sub.2, at 850.degree. C., crystalline UB.sub.4 is formed. Powder X-ray diffraction and ICP-AES data support the reduction of UCl.sub.3 as the initial step in the reaction. The UB.sub.4 product is purified by washing water and drying.

  8. Immobilization of simulated radioactive soil waste containing cerium by self-propagating high-temperature synthesis

    Science.gov (United States)

    Mao, Xianhe; Qin, Zhigui; Yuan, Xiaoning; Wang, Chunming; Cai, Xinan; Zhao, Weixia; Zhao, Kang; Yang, Ping; Fan, Xiaoling

    2013-11-01

    A simulated radioactive soil waste containing cerium as an imitator element has been immobilized by a thermite self-propagating high-temperature synthesis (SHS) process. The compositions, structures, and element leaching rates of products with different cerium contents have been characterized. To investigate the influence of iron on the chemical stability of the immobilized products, leaching tests of samples with different iron contents with different leaching solutions were carried out. The results showed that the imitator element cerium mainly forms the crystalline phases CeAl11O18 and Ce2SiO5. The leaching rate of cerium over a period of 28 days was 10-5-10-6 g/(m2 day). Iron in the reactants, the reaction products, and the environment has no significant effect on the chemical stability of the immobilized SHS products.

  9. Immobilization of simulated radioactive soil waste containing cerium by self-propagating high-temperature synthesis

    International Nuclear Information System (INIS)

    Mao, Xianhe; Qin, Zhigui; Yuan, Xiaoning; Wang, Chunming; Cai, Xinan; Zhao, Weixia; Zhao, Kang; Yang, Ping; Fan, Xiaoling

    2013-01-01

    A simulated radioactive soil waste containing cerium as an imitator element has been immobilized by a thermite self-propagating high-temperature synthesis (SHS) process. The compositions, structures, and element leaching rates of products with different cerium contents have been characterized. To investigate the influence of iron on the chemical stability of the immobilized products, leaching tests of samples with different iron contents with different leaching solutions were carried out. The results showed that the imitator element cerium mainly forms the crystalline phases CeAl 11 O 18 and Ce 2 SiO 5 . The leaching rate of cerium over a period of 28 days was 10 −5 –10 −6 g/(m 2 day). Iron in the reactants, the reaction products, and the environment has no significant effect on the chemical stability of the immobilized SHS products

  10. Synthesis and high temperature stability of amorphous Si(B)CN-MWCNT composite nanowires

    Science.gov (United States)

    Bhandavat, Romil; Singh, Gurpreet

    2012-02-01

    We demonstrate synthesis of a hybrid nanowire structure consisting of an amorphous polymer-derived silicon boron-carbonitride (Si-B-C-N) shell with a multiwalled carbon nanotube core. This was achieved through a novel process involving preparation of a boron-modified liquid polymeric precursor through a reaction of trimethyl borate and polyureasilazane under atmospheric conditions; followed by conversion of polymer to glass-ceramic on carbon nanotube surfaces through controlled heating. Chemical structure of the polymer was studied by liquid-NMR while evolution of various ceramic phases was studied by Raman spectroscopy, solid-NMR, Fourier transform infrared and X-ray photoelectron spectroscopy. Electron microscopy and X-ray diffraction confirms presence of amorphous Si(B)CN coating on individual nanotubes for all specimen processed below 1400 degree C. Thermogravimetric analysis, followed by TEM revealed high temperature stability of the carbon nanotube core in flowing air up to 1300 degree C.

  11. Mesoporous Structure Control of Silica in Room-Temperature Synthesis under Basic Conditions

    Directory of Open Access Journals (Sweden)

    Jeong Wook Seo

    2015-01-01

    Full Text Available Various types of mesoporous silica, such as continuous cubic-phase MCM-48, hexagonal-phase MCM-41, and layer-phase spherical silica particles, have been synthesized at room temperature using cetyltrimethylammonium bromide as a surfactant, ethanol as a cosurfactant, tetraethyl orthosilicate as a silica precursor, and ammonia as a condensation agent. Special care must be taken both in the filtering of the resultant solid products and in the drying process. In the drying process, further condensation of the silica after filtering was induced. As the surfactant and cosurfactant concentrations in the reaction mixture increased and the NH3 concentration decreased, under given conditions, continuous cubic MCM-48 and layered silica became the dominant phases. A cooperative synthesis mechanism, in which both the surfactant and silica were involved in the formation of mesoporous structures, provided a good explanation of the experimental results.

  12. Room temperature chemical synthesis of lead selenide thin films with preferred orientation

    Science.gov (United States)

    Kale, R. B.; Sartale, S. D.; Ganesan, V.; Lokhande, C. D.; Lin, Yi-Feng; Lu, Shih-Yuan

    2006-11-01

    Room temperature chemical synthesis of PbSe thin films was carried out from aqueous ammoniacal solution using Pb(CH3COO)2 as Pb2+ and Na2SeSO3 as Se2- ion sources. The films were characterized by a various techniques including, X-ray diffraction (XRD), energy dispersive X-ray analysis (EDAX), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high resolution transmission electron microscopy (HR-TEM), selected area electron diffraction (SAED), Fast Fourier transform (FFT) and UV-vis-NIR techniques. The study revealed that the PbSe thin film consists of preferentially oriented nanocubes with energy band gap of 0.5 eV.

  13. Room temperature chemical synthesis of lead selenide thin films with preferred orientation

    Energy Technology Data Exchange (ETDEWEB)

    Kale, R.B. [Department of Chemical Engineering, National Tsing-Hua University, Hsin-Chu, Taiwan 30043 (China)]. E-mail: rb_kale@yahoo.co.in; Sartale, S.D. [Hahn Meitner Institute, Glienicker Strasse-100, D-14109 Berlin (Germany); Ganesan, V. [UGC-DAE Consortium for Scientific Research, University Campus, Khandwa Road, Indore 452017 (India); Lokhande, C.D. [Thin Film Physics Laboratory, Department of Physics, Shivaji University, Kolhapur 416004 (India); Lin, Y.-F. [Department of Chemical Engineering, National Tsing-Hua University, Hsin-Chu, Taiwan 30043 (China); Lu, S.-Y. [Department of Chemical Engineering, National Tsing-Hua University, Hsin-Chu, Taiwan 30043 (China)]. E-mail: sylu@mx.nthu.edu.tw

    2006-11-15

    Room temperature chemical synthesis of PbSe thin films was carried out from aqueous ammoniacal solution using Pb(CH{sub 3}COO){sub 2} as Pb{sup 2+} and Na{sub 2}SeSO{sub 3} as Se{sup 2-} ion sources. The films were characterized by a various techniques including, X-ray diffraction (XRD), energy dispersive X-ray analysis (EDAX), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high resolution transmission electron microscopy (HR-TEM), selected area electron diffraction (SAED), Fast Fourier transform (FFT) and UV-vis-NIR techniques. The study revealed that the PbSe thin film consists of preferentially oriented nanocubes with energy band gap of 0.5 eV.

  14. Rapid, room-temperature synthesis of amorphous selenium/protein composites using Capsicum annuum L extract

    Science.gov (United States)

    Li, Shikuo; Shen, Yuhua; Xie, Anjian; Yu, Xuerong; Zhang, Xiuzhen; Yang, Liangbao; Li, Chuanhao

    2007-10-01

    We describe the formation of amorphous selenium (α-Se)/protein composites using Capsicum annuum L extract to reduce selenium ions (SeO32-) at room temperature. The reaction occurs rapidly and the process is simple and easy to handle. A protein with a molecular weight of 30 kDa extracted from Capsicum annuum L not only reduces the SeO32- ions to Se0, but also controls the nucleation and growth of Se0, and even participates in the formation of α-Se/protein composites. The size and shell thickness of the α-Se/protein composites increases with high Capsicum annuum L extract concentration, and decreases with low reaction solution pH. The results suggest that this eco-friendly, biogenic synthesis strategy could be widely used for preparing inorganic/organic biocomposites. In addition, we also discuss the possible mechanism of the reduction of SeO32- ions by Capsicum annuum L extract.

  15. Room temperature synthesis and optical properties of small diameter (5 nm) ZnO nanorod arrays.

    Science.gov (United States)

    Cho, Seungho; Jang, Ji-Wook; Lee, Jae Sung; Lee, Kun-Hong

    2010-10-01

    We report a simple wet-chemical synthesis of ∼5 nm diameter ZnO nanorod arrays at room temperature (20 °C) and normal atmospheric pressure (1 atm) and their optical properties. They were single crystalline in nature, and grew in the [001] direction. These small diameter ZnO nanorod arrays can also be synthesized at 0 °C. Control experiments were also conducted. On the basis of the results, we propose a mechanism for the spontaneous growth of the small diameter ZnO structures. The optical properties of the 5 nm diameter ZnO nanorod arrays synthesized using this method were probed by UV-Visible diffuse reflectance spectroscopy. A clear blue-shift, relative to the absorption band from 50 nm diameter ZnO nanorod arrays, was attributed to the quantum confinement effects caused by the small nanocrystal size in the 5 nm diameter ZnO nanorods.

  16. Room temperature synthesis and characterization of CdO nanowires by chemical bath deposition (CBD) method

    International Nuclear Information System (INIS)

    Dhawale, D.S.; More, A.M.; Latthe, S.S.; Rajpure, K.Y.; Lokhande, C.D.

    2008-01-01

    A chemical synthesis process for the fabrication of CdO nanowires is described. In the present work, transparent and conductive CdO films were synthesized on the glass substrate using chemical bath deposition (CBD) at room temperature. These films were annealed in air at 623 K and characterized for the structural, morphological, optical and electrical properties were studied by means of X-ray diffraction (XRD), scanning electron microscopy (SEM), optical and electrical resistivity. The XRD analysis showed that the as-deposited amorphous can be converted in to polycrystalline after annealing. Annealed CdO nanowires are 60-65 nm in diameter and length ranges typically from 2.5 to 3 μm. The optical properties revealed the presence of direct and indirect band gaps with energies 2.42 and 2.04 eV, respectively. Electrical resistivity measurement showed semiconducting behavior and thermoemf measurement showed n-type electrical conductivity

  17. Room temperature chemical synthesis of lead selenide thin films with preferred orientation

    International Nuclear Information System (INIS)

    Kale, R.B.; Sartale, S.D.; Ganesan, V.; Lokhande, C.D.; Lin, Y.-F.; Lu, S.-Y.

    2006-01-01

    Room temperature chemical synthesis of PbSe thin films was carried out from aqueous ammoniacal solution using Pb(CH 3 COO) 2 as Pb 2+ and Na 2 SeSO 3 as Se 2- ion sources. The films were characterized by a various techniques including, X-ray diffraction (XRD), energy dispersive X-ray analysis (EDAX), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high resolution transmission electron microscopy (HR-TEM), selected area electron diffraction (SAED), Fast Fourier transform (FFT) and UV-vis-NIR techniques. The study revealed that the PbSe thin film consists of preferentially oriented nanocubes with energy band gap of 0.5 eV

  18. 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

  19. Organic titanates: a model for activating rapid room-temperature synthesis of shape-controlled CsPbBr3 nanocrystals and their derivatives.

    Science.gov (United States)

    Fang, Shaofan; Li, Guangshe; Li, Huixia; Lu, Yantong; Li, Liping

    2018-04-12

    The application of lead halide perovskite nanocrystals is challenged by the lack of strategies in rapid room-temperature synthesis with controlled morphologies. Here, we report on an initial study of adopting organic titanates as a model activator that promotes rapid room-temperature synthesis of shape-controlled, highly luminescent CsPbBr3 nanocrystals and their derivatives.

  20. BF3.SiO2: an efficient catalyst for the synthesis of azo dyes at room temperature

    Directory of Open Access Journals (Sweden)

    Bi Bi Fatemeh Mirjalili

    2012-07-01

    Full Text Available A rapid one-pot method has been developed for the synthesis of azo dyes via ‎sequential diazotization–diazo coupling of aromatic amines with coupling agents at room ‎temperature in the presence of BF3.SiO2 as acidic catalyst. The obtained aryl diazonium salts bearing silica supported boron tri-flouride counter ion‎ was sufficiently stable to be kept at room ‎temperature in the dry state.‎

  1. Low-temperature synthesis of allyl dimethylamine by selective heating under microwave irradiation used for water treatment

    International Nuclear Information System (INIS)

    Tian Binghui; Luan Zhaokun; Li Mingming

    2005-01-01

    Low-temperature synthesis of allyl dimethylamine (ADA) by selective heating under microwave irradiation (MI) used for water treatment is investigated. The effect of MI, ultrasound irradiation (UI) and conventional heating on yield of ADA, reaction time and the flocculation efficiency of polydiallyl dimethylammunion chloride (PDADMAC) prepared form ADA were studied. The results show that by selective heating at low temperature, MI not only increases yield of ADA and reduces reaction time, but also greatly enhances the flocculation efficiency of PDADMAC

  2. Facile synthesis of improved room temperature gas sensing properties of TiO2 nanostructures: Effect of acid treatment

    CSIR Research Space (South Africa)

    Tshabalala, Zamaswazi P

    2016-03-01

    Full Text Available and Actuators B: Chemical Facile synthesis of improved room temperature gas sensing properties of TiO2 nanostructures: Effect of acid treatment Z.P. Tshabalalaa,b, D.E. Motaunga,∗, G.H. Mhlongoa,∗, O.M. Ntwaeaborwab,∗ a DST/CSIR, National Centre...

  3. Ambient temperature aqueous synthesis of ultrasmall copper doped ceria nanocrystals for the water gas shift and carbon monoxide oxidation reactions

    Energy Technology Data Exchange (ETDEWEB)

    Curran, Christopher D. [Department of Chemical and Biomolecular Engineering; Lehigh University; Bethlehem; USA; Lu, Li [Department of Materials Science and Engineering; Lehigh University; Bethlehem; USA; Kiely, Christopher J. [Department of Chemical and Biomolecular Engineering; Lehigh University; Bethlehem; USA; Department of Materials Science and Engineering; McIntosh, Steven [Department of Chemical and Biomolecular Engineering; Lehigh University; Bethlehem; USA

    2018-01-01

    Ultra-small CuxCe1-xO2-δnanocrystals were prepared through a room temperature, aqueous synthesis method, achieving high copper doping and low water gas shift activation energy.

  4. Facile room-temperature solution-phase synthesis of a spherical covalent organic framework for high-resolution chromatographic separation.

    Science.gov (United States)

    Yang, Cheng-Xiong; Liu, Chang; Cao, Yi-Meng; Yan, Xiu-Ping

    2015-08-07

    A simple and facile room-temperature solution-phase synthesis was developed to fabricate a spherical covalent organic framework with large surface area, good solvent stability and high thermostability for high-resolution chromatographic separation of diverse important industrial analytes including alkanes, cyclohexane and benzene, α-pinene and β-pinene, and alcohols with high column efficiency and good precision.

  5. A rapid room temperature chemical route for the synthesis of graphene: metal-mediated reduction of graphene oxide.

    Science.gov (United States)

    Dey, Ramendra Sundar; Hajra, Saumen; Sahu, Ranjan K; Raj, C Retna; Panigrahi, M K

    2012-02-07

    A rapid and facile route for the synthesis of reduced graphene oxide sheets (rGOs) at room temperature by the chemical reduction of graphene oxide using Zn/acid in aqueous solution is demonstrated. This journal is © The Royal Society of Chemistry 2012

  6. A new practical approach towards the synthesis of unsymmetric and symmetric 1,10-phenanthroline derivatives at room temperature.

    Science.gov (United States)

    Cheng, Yongfeng; Han, Xuesong; Ouyang, Huangche; Rao, Yu

    2012-03-18

    An efficient method towards synthesis of 1,10-phenanthrolines is described. Through Lewis acid-catalyzed annulation reaction between 3-ethoxycyclobutanones and 8-aminoquinolines, a variety of unsymmetric and symmetric 1,10-phenanthroline derivatives were readily prepared with high regioselectivity at room temperature.

  7. Low temperature synthesis of Ba1–xSrxSnO3 (x= 0–1) from molten ...

    Indian Academy of Sciences (India)

    ... Lecture Workshops · Refresher Courses · Symposia · Live Streaming. Home; Journals; Bulletin of Materials Science; Volume 33; Issue 1. Low temperature synthesis of Ba1–SrSnO3 ( = 0–1) from molten alkali hydroxide flux. B Ramdas R Vijayaraghavan. Electrical Properties Volume 33 Issue 1 February 2010 pp 75- ...

  8. Analysis of the structural stability of the smectite submitted to high pressures and temperatures

    International Nuclear Information System (INIS)

    Alabarse, Frederico Gil

    2009-10-01

    The thermal stability of bentonite is of particular interest for containment barrier in nuclear waste disposal facilities. However, very little is known about the stability of smectite (principal component of bentonite) under high-pressure and high-temperature conditions (HPHT). The objective of this work was to investigate the stability of the smectite structure under HP-HT conditions. The HP-HT experiments were performed on toroidal chambers (TC) with pressure up 7.7 GPa and temperatures of 1000 deg C. The samples were characterized by X-ray diffraction after the HP-HT processing. Furthermore, one sample from the original material was analyzed using Fourier transformed infra-red (FTIR) in situ measurements on a diamond anvil cell (DAC) in experiments up to 12 GPa. The original sample of bentonite, calcium dioctahedral montmorillonite with small fraction of quartz, was characterized by FTIR, XRD, X-ray fluorescence (XRF), scanning electron microscopy (SEM), surface area, thermogravimetric analysis (TGA) and differential thermal analysis (DTA). In the experiment performed using the DAC up to 12 GPa, the FTIR in situ measurements analysis showed that the smectite structure is stable with a reversible deformation in the Si-O bond and that the smectite did not loose water. Experiments performed in TC at 7.7 GPa of pressure and 250 deg C of temperature, during 3.5 h showed, after analysis by XRD and FTIR, that the smectite structure is stable and did not loose water. Experiments performed in TC at 7.7 GPa of pressure and 1000 deg C of temperature, during 3.5 h showed, after analysis by XRD and SEM, the transformation of bentonite to the mineral assemblage: Coesite, Quartz, Kyanite and Pyrope. (author)

  9. Low-temperature direct synthesis of mesoporous vanadium nitrides for electrochemical capacitors

    Science.gov (United States)

    Lee, Hae-Min; Jeong, Gyoung Hwa; Kim, Sang-Wook; Kim, Chang-Koo

    2017-04-01

    Mesoporous vanadium nitrides are directly synthesized by a one-step chemical precipitation method at a low temperature (70 °C). Structural and morphological analyses reveal that vanadium nitride consist of long and slender nanowhiskers, and mesopores with diameters of 2-5 nm. Compositional analysis confirms the presence of vanadium in the VN structure, along with oxidized vanadium. The cyclic voltammetry and charge-discharge tests indicate that the obtained material stores charges via a combination of electric double-layer capacitance and pseudocapacitance mechanisms. The vanadium nitride electrode exhibits a specific capacitance of 598 F/g at a current density of 4 A/g. After 5000 charge-discharge cycles, the electrode has an equivalent series resistance of 1.42 Ω and retains 83% of its initial specific capacitance. This direct low-temperature synthesis of mesoporous vanadium nitrides is a simple and promising method to achieve high specific capacitance and low equivalent series resistance for electrochemical capacitor applications.

  10. Solid-State Synthesis and Effect of Temperature on Optical Properties of CuO Nanoparticles

    Institute of Scientific and Technical Information of China (English)

    C.C.Vidyasagar; Y.Arthoba Naik; T.G.Venkatesha; R.Viswanatha

    2012-01-01

    Modulation of band energies through size control offers new ways to control photoresponse and photoconversion efficiency of the solar cell. The P-type semiconductor of copper oxide is an important functional material used for photovoltaic cells. Cu O is attractive as a selective solar absorber since it has high solar absorbance and a low thermal emittance. The present work describes the synthesis and characterization of semiconducting Cu O nanoparticles via one-step, solid-state reaction in the presence of Polyethylene glycol400 as size controlling agent for the preparation of Cu O nanoparticles at different temperatures. Solid-state mechanochemical processing, which is not only a physical size reduction process in conventional milling but also a chemical reaction, is mechanically activated at the nanoscale during grinding. The present method is a simple and efficient method of preparing nanoparticles with high yield at low cost. The structural and chemical composition of the nanoparticles were analyzed by X-ray diffraction, field emission scanning electron microscopy and energy-dispersive spectrometer, respectively. Optical properties and band gap of Cu O nanoparticles were studied by UV-Vis spectroscopy. These results showed that the band gap energy decreased with increase of annealing temperature, which can be attributed to the improvement in grain size of the samples.

  11. Thermochemistry of some binary lead and transition metal compounds by high temperature direct synthesis calorimetry

    Energy Technology Data Exchange (ETDEWEB)

    Meschel, S.V., E-mail: meschel@jfi.uchicago.edu [Illinois Institute of Technology,Thermal Processing Technology Center, 10 W. 32nd Street, Chicago, Illinois 60615 (United States); Gordon Center for Integrated Science, 929 E. 57th Street, Chicago, Illinois 60637 (United States); Nash, P. [Illinois Institute of Technology,Thermal Processing Technology Center, 10 W. 32nd Street, Chicago, Illinois 60615 (United States); Chen, X.Q.; Wei, P. [Materials processing Modeling Division, Shenyang National Laboratory for Materials Science, Institute of Metals Research, 72 Wenhua Road, Shenyang City (China)

    2015-06-05

    Highlights: • Studied binary lead-transition metal alloys by high temperature calorimetry. • Determined the enthalpies of formation of 8 alloys. • Compared the measurements with predictions by the model of Miedema and by the ab initio method. - Abstract: The standard enthalpies of formation of some binary lead and transition metal compounds have been measured by high temperature direct synthesis calorimetry. The reported results are: Pb{sub 3}Sc{sub 5}(−61.3 ± 2.9); PbTi{sub 4}(−16.6 ± 2.4); Pb{sub 3}Y{sub 5}(−64.8 ± 3.6); Pb{sub 3}Zr{sub 5}(−50.6 ± 3.1); PbNb{sub 3}(−10.4 ± 3.4); PbRh(−16.5 ± 3.3); PbPd{sub 3}(−29.6 ± 3.1); PbPt(−34.7 ± 3.3) kJ/mole of atoms. We will compare our results with previously published measurements. We will also compare the experimental measurements with enthalpies of formation of transition metal compounds with elements in the same vertical column in the periodic table. We will compare our measurements with predicted values on the basis of the semi empirical model of Miedema and coworkers and with ab initio values when available.

  12. Radiation synthesis of the water-soluble, temperature sensitive polymer, copolymer and study on their properties

    International Nuclear Information System (INIS)

    Zhai Maolin; Yin Min; Ha Hongfei

    1994-01-01

    In order to obtain the water-soluble, temperature sensitive polymer and activated copolymer, the radiation polymerization of N-isopropylacrylamide (NIPAAm), radiation copolymerization of NIPAAm and N-acryloxysuccide (NASI) in aqueous solution or in buffer solution (PBS pH = 7.4) have been carried out by γ-rays from 60 Co source at room temperature. The optimum dose range (1-7 kGy), dose rate (>40 Gy/min) and monomer concentration (1%) were chosen through determining the monomer conversion yield and molecular weight (M w = 6.8 x 10 5 ) of product. Synthesis of the reversible linear polymer was performed in tetrahydrofuran (THF) as well. In this way a white powder product could be obtained which possesses of thermally reversible property too, when it was dissolved in water or PBS. The only disadvantages of this method is that the molecular weight of the polymer produced in THF was much lower than that in aqueous solution

  13. The Effects of Light and Temperature on Biotin Synthesis in Pea Sprouts.

    Science.gov (United States)

    Kamiyama, Shin; Ohnuki, Risa; Moriki, Aoi; Abe, Megumi; Ishiguro, Mariko; Sone, Hideyuki

    2016-01-01

    Biotin is an essential micronutrient, and is a cofactor for several carboxylases that are involved in the metabolism of glucose, fatty acids, and amino acids. Because plant cells can synthesize their own biotin, a wide variety of plant-based foods contains significant amounts of biotin; however, the influence of environmental conditions on the biotin content in plants remains largely unclear. In the present study, we investigated the effects of different cultivation conditions on the biotin content and biotin synthesis in pea sprouts (Pisum sativum). In the experiment, the pea sprouts were removed from their cotyledons and cultivated by hydroponics under five different lighting and temperature conditions (control [25ºC, 12-h light/12-h dark cycle], low light [25ºC, 4-h light/20-h dark cycle], dark [25ºC, 24 h dark], low temperature [12ºC, 12-h light/12-h dark cycle], and cold [6ºC, 12-h light/12-h dark cycle]) for 10 d. Compared to the biotin content of pea sprouts under the control conditions, the biotin contents of pea sprouts under the low-light, dark, and cold conditions had significantly decreased. The dark group showed the lowest biotin content among the groups. Expression of the biotin synthase gene (bio2) was also significantly decreased under the dark and cold conditions compared to the control condition, in a manner similar to that observed for the biotin content. No significant differences in the adenosine triphosphate content were observed among the groups. These results indicate that environmental conditions such as light and temperature modulate the biotin content of pea plant tissues by regulating the expression of biotin synthase.

  14. ACBC to Balcite: Bioinspired Synthesis of a Highly Substituted High-Temperature Phase from an Amorphous Precursor

    Energy Technology Data Exchange (ETDEWEB)

    Whittaker, Michael L.; Joester, Derk (NWU)

    2017-04-28

    Energy-efficient synthesis of materials locked in compositional and structural states far from equilibrium remains a challenging goal, yet biomineralizing organisms routinely assemble such materials with sophisticated designs and advanced functional properties, often using amorphous precursors. However, incorporation of organics limits the useful temperature range of these materials. Herein, the bioinspired synthesis of a highly supersaturated calcite (Ca0.5Ba0.5CO3) called balcite is reported, at mild conditions and using an amorphous calcium–barium carbonate (ACBC) (Ca1- x Ba x CO3·1.2H2O) precursor. Balcite not only contains 50 times more barium than the solubility limit in calcite but also displays the rotational disorder on carbonate sites that is typical for high-temperature calcite. It is significantly harder (30%) and less stiff than calcite, and retains these properties after heating to elevated temperatures. Analysis of balcite local order suggests that it may require the formation of the ACBC precursor and could therefore be an example of nonclassical nucleation. These findings demonstrate that amorphous precursor pathways are powerfully enabling and provide unprecedented access to materials far from equilibrium, including high-temperature modifications by room-temperature synthesis.

  15. 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.

  16. Application of Self-Propagating High Temperature Synthesis to the Fabrication of Actinide Bearing Nitride and Other Ceramic Nuclear Fuels

    International Nuclear Information System (INIS)

    Moore, John J.; Reigel, Marissa M.; Donohoue, Collin D.

    2009-01-01

    The project uses an exothermic combustion synthesis reaction, termed self-propagating high-temperature synthesis (SHS), to produce high quality, reproducible nitride fuels and other ceramic type nuclear fuels (cercers and cermets, etc.) in conjunction with the fabrication of transmutation fuels. The major research objective of the project is determining the fundamental SHS processing parameters by first using manganese as a surrogate for americium to produce dense Zr-Mn-N ceramic compounds. These fundamental principles will then be transferred to the production of dense Zr-Am-N ceramic materials. A further research objective in the research program is generating fundamental SHS processing data to the synthesis of (i) Pu-Am-Zr-N and (ii) U-Pu-Am-N ceramic fuels. In this case, Ce will be used as the surrogate for Pu, Mn as the surrogate for Am, and depleted uranium as the surrogate for U. Once sufficient fundamental data has been determined for these surrogate systems, the information will be transferred to Idaho National Laboratory (INL) for synthesis of Zr-Am-N, Pu-Am-Zr-N and U-Pu-Am-N ceramic fuels. The high vapor pressures of americium (Am) and americium nitride (AmN) are cause for concern in producing nitride ceramic nuclear fuel that contains Am. Along with the problem of Am retention during the sintering phases of current processing methods, are additional concerns of producing a consistent product of desirable homogeneity, density and porosity. Similar difficulties have been experienced during the laboratory scale process development stage of producing metal alloys containing Am wherein compact powder sintering methods had to be abandoned. Therefore, there is an urgent need to develop a low-temperature or low-heat fuel fabrication process for the synthesis of Am-containing ceramic fuels. Self-propagating high temperature synthesis (SHS), also called combustion synthesis, offers such an alternative process for the synthesis of Am nitride fuels. Although SHS

  17. Kinetically controlled synthesis of large-scale morphology-tailored silver nanostructures at low temperature

    Science.gov (United States)

    Zhang, Ling; Zhao, Yuda; Lin, Ziyuan; Gu, Fangyuan; Lau, Shu Ping; Li, Li; Chai, Yang

    2015-08-01

    Ag nanostructures are widely used in catalysis, energy conversion and chemical sensing. Morphology-tailored synthesis of Ag nanostructures is critical to tune physical and chemical properties. In this study, we develop a method for synthesizing the morphology-tailored Ag nanostructures in aqueous solution at a low temperature (45 °C). With the use of AgCl nanoparticles as the precursor, the growth kinetics of Ag nanostructures can be tuned with the pH value of solution and the concentration of Pd cubes which catalyze the reaction. Ascorbic acid and cetylpyridinium chloride are used as the mild reducing agent and capping agent in aqueous solution, respectively. High-yield Ag nanocubes, nanowires, right triangular bipyramids/cubes with twinned boundaries, and decahedra are successfully produced. Our method opens up a new environmentally-friendly and economical route to synthesize large-scale and morphology-tailored Ag nanostructures, which is significant to the controllable fabrication of Ag nanostructures and fundamental understanding of the growth kinetics.Ag nanostructures are widely used in catalysis, energy conversion and chemical sensing. Morphology-tailored synthesis of Ag nanostructures is critical to tune physical and chemical properties. In this study, we develop a method for synthesizing the morphology-tailored Ag nanostructures in aqueous solution at a low temperature (45 °C). With the use of AgCl nanoparticles as the precursor, the growth kinetics of Ag nanostructures can be tuned with the pH value of solution and the concentration of Pd cubes which catalyze the reaction. Ascorbic acid and cetylpyridinium chloride are used as the mild reducing agent and capping agent in aqueous solution, respectively. High-yield Ag nanocubes, nanowires, right triangular bipyramids/cubes with twinned boundaries, and decahedra are successfully produced. Our method opens up a new environmentally-friendly and economical route to synthesize large-scale and morphology

  18. Auger electron spectroscopy analysis for growth interface of cubic boron nitride single crystals synthesized under high pressure and high temperature

    Science.gov (United States)

    Lv, Meizhe; Xu, Bin; Cai, Lichao; Guo, Xiaofei; Yuan, Xingdong

    2018-05-01

    After rapid cooling, cubic boron nitride (c-BN) single crystals synthesized under high pressure and high temperature (HPHT) are wrapped in the white film powders which are defined as growth interface. In order to make clear that the transition mechanism of c-BN single crystals, the variation of B and N atomic hybrid states in the growth interface is analyzed with the help of auger electron spectroscopy in the Li-based system. It is found that the sp2 fractions of B and N atoms decreases, and their sp3 fractions increases from the outer to the inner in the growth interface. In addition, Lithium nitride (Li3N) are not found in the growth interface by X-ray diffraction (XRD) experiment. It is suggested that lithium boron nitride (Li3BN2) is produced by the reaction of hexagonal boron nitride (h-BN) and Li3N at the first step, and then B and N atoms transform from sp2 into sp3 state with the catalysis of Li3BN2 in c-BN single crystals synthesis process.

  19. Temperature and Pressure Effects on Drilling Fluid Rheology and ECD in Very Deep Wells

    Energy Technology Data Exchange (ETDEWEB)

    Rommetveit, R.; Bjoerkvoll, K.S.

    1997-12-31

    The rheological properties of drilling fluids are usually approximated to be independent of pressure and temperature. In many cases this is a good approximation. However, for wells with small margins between pore and fracture pressure, careful evaluations and analysis of the effects of temperature and pressure on well bore hydraulics and kick probability are needed. In this publication the effects of pressure and temperature are discussed and described for typical HPHT (High Pressure High Temperature) wells. Laboratory measurements show that rheology is very pressure and temperature dependent. The practical implications of these observations are illustrated through a series of calculations with an advanced pressure and temperature simulator. 10 refs., 15 figs.

  20. Low Temperature Synthesis of Li2SiO3: Effect on Its Morphological and Textural Properties

    Directory of Open Access Journals (Sweden)

    Georgina Mondragón-Gutiérrez

    2008-01-01

    Full Text Available Synthesis, at low temperature, of Li2SiO3 was investigated using different Li : Si molar ratios and urea, which was used as template. This new synthesis was performed in order to look for different textural and morphological properties than those obtained usually by conventional methods in this kind of ceramics. XRD and SEM analyses showed that Li2SiO3 was obtained pure and with ceramic particle morphology of hollow spheres of 2–6 μm. TEM analysis showed that those spheres were composed by needle-like particles crosslinked among them. This morphology provided a high surface area, probed by N2 adsorption. Therefore, this method of synthesis may be used to obtain other similar ceramics and test them in different applications.

  1. Low temperature synthesis of nano alpha-alumina powder by two-step hydrolysis

    International Nuclear Information System (INIS)

    Yan, Ting; Guo, Xiaode; Zhang, Xiang; Wang, Zhixiang; Shi, Jinqiu

    2016-01-01

    Highlights: • The nano α-Al 2 O 3 with good dispersion was prepared by two-step hydrolysis. • α-Al 2 O 3 powders were added as seed particles in the hydrolysis. • This article indicated that the glucose could impel the γ-Al 2 O 3 transformed to α-Al 2 O 3 directly. • This article indicated that the addictive of α-Al 2 O 3 seed could improve the phase transformation rate of γ-Al 2 O 3 to α-Al 2 O 3 . • In this article, the pure α-Al 2 O 3 could be obtained by calcining at 1000 °C for 1.5 h. - Abstract: The ultral fine alpha-alumina powder has been successfully synthesized via two-step hydrolysis of aluminum isopropoxide. Glucose and polyvinyl pyrrolidone were used as surfactants during the appropriate processing step. The alpha-alumina powder was used as seed particles. Several synthesis parameters, such as the amount of seeds, surfactants, and calcination temperature, were studied by X-ray diffraction (XRD), Fourier transform infrared spectra (FTIR), Thermogravimetry-differential scanning calorimetry (TG-DSC), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The experimental results showed that glucose greatly lower the phase transformation temperature of alpha-alumina by impelling the gamma-alumina transformed to alpha-alumina directly, and the seed could improve the phase transformation rate of alpha-alumina, the polyvinylpyrrolidone have an effect on preventing excessive grain growth and agglomeration of alpha-alumina powder. Comparatively well dispersed alpha-alumina powder with particle size less than 50 nm can be synthesized through this method after calcinations at 1000 °C for 2 h.

  2. Effect of Temperature and Mole Ratio on the Synthesis Yield of Rhenium-Tetrofosmin

    Directory of Open Access Journals (Sweden)

    Widyastuti

    2015-08-01

    Full Text Available Technetium-99m (99mTc tetrofosmin is widely used in nuclear medicine as a diagnostic agent for myocardial perfusion and as a tumor imaging agent. As a parenteral preparation it requires an evaluation of its pharmacokinetics and stability in-vivo. Since 99mTc has a short half-life and is only available in very low concentrations, it is impossible to characterize its chemical properties and presence in the body. Due to this reason, only technetium-99 (T1/2 = 5 × 105 years, which is available in macro quantities, or natural rhenium can be used for this purpose. In this study rhenium-188 (188Re tetrofosmin will be synthesized and applied, because non-radioactive Re can be easily obtained. Synthesis and radiochemical purity analysis of carrier-added 188Re-tetrofosmin were carried out as a model to study the in-vivo stability of technetium-99m tetrofosmin. Rhenium-188 was used as a tracer to identify the formation of rhenium tetrofosmin. Rhenium gluconate was synthesized first prior to the formation of rhenium tetrofosmin. The quality of labeling for both rhenium gluconate and rhenium tetrofosmin was analyzed using paper- and thin-layer chromatography, respectively. Rhenium gluconate can be synthesized with high labeling yield within 1 hour, whereas rhenium tetrofosmin was synthesized both in room temperature and in an elevated temperature with various tetrofosmin-to-rhenium mole ratios.The results showed that heating at 95oC led to a higher yield of more than 90% within 30 minutes. Rhenium tetrofosmin could be produced in high radiochemical purity using an excess of tetrofosmin with mole ratio of 2000. It is concluded that rhenium tetrofosmin could be synthesized through the formation of rhenium gluconate, and a higher yield could be obtained in a shorter time by heating process.

  3. Microstructure evolution of Mo–Si–Al system during self-propagation high-temperature synthesis

    International Nuclear Information System (INIS)

    Jia, Lei; Xie, Hui; Lu, Zhen-lin; Zhang, Chao

    2013-01-01

    Highlights: ► Phase transformation subsequence of the reaction system was given by a sketch. ► Transformation of MoSi 2 to Mo(Si, Al) 2 phase was observed by XRD analysis. ► Variation of diffraction peaks was discussed by lattice parameters calculation. -- Abstract: The microstructure and phase constitution of Mo(Si 1−x , Al x ) 2 alloys (x = 0.03, 0.1 and 0.4) prepared by self-propagation high-temperature synthesis is first investigated using SEM, EDS and XRD analysis. Then the lattice parameters and adiabatic temperature are calculated. Based on the above experimental and calculated results, the variation mechanism of diffraction peaks and phase transformation subsequence of the Mo–MoO 3 –Si–Al powders is discussed. Results show that, when the self-propagation reaction is over, there are a homogeneous Mo–Si–Al alloy melt and a fused Al 2 O 3 with lower density at top. Subsequently, MoSi 2 or Mo(Si, Al) 2 phase nucleates and grows as a primary phase in the Mo–Si–Al alloy melts, and then Al, Si substances are generated from the intergranular residual Al–Si liquid according to Al–Si binary phase diagram. The Al increase in the starting powder mixtures leads to the Al concentration increase in the Mo–Si–Al alloy melt. Consequently, MoSi 2 is transformed to Mo(Si, Al) 2 to phase in which Si is replaced by Al atoms and Al substance in the intergranular zones increased accordingly

  4. Urea-assisted low temperature green synthesis of graphene nanosheets for transparent conducting film

    Science.gov (United States)

    Chamoli, Pankaj; Das, Malay K.; Kar, Kamal K.

    2018-02-01

    Present work demonstrates the fabrication of graphene nanosheet (GN) based transparent conducting film (TCF) using spray coating. Green synthesis of GN is carried out by reduction of graphene oxide (GO) using urea as green reducing agent. The reductive ability of urea with varied concentration is studied for GO at low temperature (i.e., 90 °C). As synthesized graphene nanosheets (GNs) are characterized by Raman spectroscopy, Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), UV-visible spectroscopy, field emission scanning electron microscopy (FESEM), atomic force microscope (AFM), and X-ray Photon spectroscopy (XPS). Raman analysis confirms that the maximum reduction of oxygen species is noticed using 30 mg/ml urea concentration at 90 °C from GO, and found Raman D to G band ratio (ID/IG) of ∼1.30. XPS analysis validates the Raman signature of removal of oxygen functional groups from GO, and obtained C/O ratio of ∼5.28. Further, transparent conducting films (TCFs) are fabricated using synthesized GNs. Thermal graphitization is carried out to enhance the optical and electrical properties of TCFs. TCF shows best performance when it is annealed at 900 °C for 1 h in vacuum, and obtained sheet resistance is ∼1.89 kΩ/□ with transmittance of ∼62.53%.

  5. Room-temperature synthesis and enhanced catalytic performance of silver-reduced graphene oxide nanohybrids

    International Nuclear Information System (INIS)

    Thu, Tran Viet; Ko, Pil Ju; Phuc, Nguyen Huu Huy; Sandhu, Adarsh

    2013-01-01

    The synthesis of supported, ultrasmall metallic nanoparticles (NPs) is of great importance for catalytic applications. In this study, silver-reduced graphene oxide nanohybrids (Ag–rGO NHs) were prepared by reducing Ag ions and graphene oxide (GO) at room temperature using sodium borohydride (NaBH 4 ) and trisodium citrate. The resulting products were characterized using UV–Vis spectroscopy, X-ray diffraction, Raman spectroscopy, scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM), and X-ray photoelectron spectroscopy. The rich chemistry of GO surface provided many sites for the nucleation of Ag ions and efficiently limited their growth. Ag NPs were uniformly grown on basal planes of rGO with a high density (∼1,700 NPs μm −2 ) and well-defined size (3.6 ± 0.6 nm) as evidenced in SEM and HRTEM studies. The resulting Ag–rGO NHs were readily dispersed in water and exhibited enhanced catalytic activity toward the reduction of 4-nitrophenol by NaBH 4 in comparison to unsupported Ag NPs. The role of rGO as an excellent support for Ag catalyst is discussed

  6. Room-temperature synthesis and enhanced catalytic performance of silver-reduced graphene oxide nanohybrids

    Energy Technology Data Exchange (ETDEWEB)

    Thu, Tran Viet, E-mail: thu@eiiris.tut.ac.jp; Ko, Pil Ju, E-mail: ko@eiiris.tut.ac.jp [Toyohashi University of Technology, Electronics-Inspired Interdisciplinary Research Institute (Japan); Phuc, Nguyen Huu Huy [Toyohashi University of Technology, Department of Electrical and Electronic Information Engineering (Japan); Sandhu, Adarsh [Toyohashi University of Technology, Electronics-Inspired Interdisciplinary Research Institute (Japan)

    2013-10-15

    The synthesis of supported, ultrasmall metallic nanoparticles (NPs) is of great importance for catalytic applications. In this study, silver-reduced graphene oxide nanohybrids (Ag-rGO NHs) were prepared by reducing Ag ions and graphene oxide (GO) at room temperature using sodium borohydride (NaBH{sub 4}) and trisodium citrate. The resulting products were characterized using UV-Vis spectroscopy, X-ray diffraction, Raman spectroscopy, scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HRTEM), and X-ray photoelectron spectroscopy. The rich chemistry of GO surface provided many sites for the nucleation of Ag ions and efficiently limited their growth. Ag NPs were uniformly grown on basal planes of rGO with a high density ({approx}1,700 NPs {mu}m{sup -2}) and well-defined size (3.6 {+-} 0.6 nm) as evidenced in SEM and HRTEM studies. The resulting Ag-rGO NHs were readily dispersed in water and exhibited enhanced catalytic activity toward the reduction of 4-nitrophenol by NaBH{sub 4} in comparison to unsupported Ag NPs. The role of rGO as an excellent support for Ag catalyst is discussed.

  7. Vapor Phase Synthesis of Organometal Halide Perovskite Nanowires for Tunable Room-Temperature Nanolasers.

    Science.gov (United States)

    Xing, Jun; Liu, Xin Feng; Zhang, Qing; Ha, Son Tung; Yuan, Yan Wen; Shen, Chao; Sum, Tze Chien; Xiong, Qihua

    2015-07-08

    Semiconductor nanowires have received considerable attention in the past decade driven by both unprecedented physics derived from the quantum size effect and strong isotropy and advanced applications as potential building blocks for nanoscale electronics and optoelectronic devices. Recently, organic-inorganic hybrid perovskites have been shown to exhibit high optical absorption coefficient, optimal direct band gap, and long electron/hole diffusion lengths, leading to high-performance photovoltaic devices. Herein, we present the vapor phase synthesis free-standing CH3NH3PbI3, CH3NH3PbBr3, and CH3NH3PbIxCl3(-x) perovskite nanowires with high crystallinity. These rectangular cross-sectional perovskite nanowires have good optical properties and long electron hole diffusion length, which ensure adequate gain and efficient optical feedback. Indeed, we have demonstrated optical-pumped room-temperature CH3NH3PbI3 nanowire lasers with near-infrared wavelength of 777 nm, low threshold of 11 μJ/cm(2), and a quality factor as high as 405. Our research advocates the promise of optoelectronic devices based on organic-inorganic perovskite nanowires.

  8. High-temperature superconducting oxide synthesis and the chemical doping of the Cu-O planes

    International Nuclear Information System (INIS)

    Tarascon, J.M.; Barboux, P.; Bagley, B.G.; Greene, L.H.; McKinnon, W.R.; Hull, G.W.

    1987-01-01

    Different synthesis techniques for the preparation of dense superconducting ceramics are discussed, and a sol-gel process is shown to be very promising. The effect of oxygen content, and the effect of substitution of Ni and Zn for copper, on the structural, transport and superconducting properties of the La-Sr-Cu-O and Y-Ba-Cu-O systems are presented. The authors find that substitution on the copper sites destroys T/sub c/ in the La-Sr-Cu-O system and decreases it in the Y-Ba-Cu-O system, and this effect is insensitive as to whether the 3d metal is magnetic (Ni) or diamagnetic (Zn). A detailed study of the YBa/sub 2/Cu/sub 3/O/sub 7-y/ system as a function of oxygen content (y) shows that superconductivity can be destroyed in these materials by the removal of oxygen and restored by reinjecting oxygen; either thermally at 500 0 C or at temperatures (80 0 C) compatible with device processing by means of a novel plasma oxidation process. Of scientific interest, the plasma process induces bulk superconductivity in the undoped La/sub 2/CuO/sub 4/

  9. Rapid, room-temperature synthesis of amorphous selenium/protein composites using Capsicum annuum L extract

    Energy Technology Data Exchange (ETDEWEB)

    Li Shikuo; Shen Yuhua; Xie Anjian; Yu Xuerong; Zhang Xiuzhen; Yang Liangbao; Li Chuanhao [School of Chemistry and Chemical Engineering, Anhui University, Hefei 230039 (China)

    2007-10-10

    We describe the formation of amorphous selenium ({alpha}-Se)/protein composites using Capsicum annuum L extract to reduce selenium ions (SeO{sub 3}{sup 2-}) at room temperature. The reaction occurs rapidly and the process is simple and easy to handle. A protein with a molecular weight of 30 kDa extracted from Capsicum annuum L not only reduces the SeO{sub 3}{sup 2-} ions to Se{sup 0}, but also controls the nucleation and growth of Se{sup 0}, and even participates in the formation of {alpha}-Se/protein composites. The size and shell thickness of the {alpha}-Se/protein composites increases with high Capsicum annuum L extract concentration, and decreases with low reaction solution pH. The results suggest that this eco-friendly, biogenic synthesis strategy could be widely used for preparing inorganic/organic biocomposites. In addition, we also discuss the possible mechanism of the reduction of SeO{sub 3}{sup 2-} ions by Capsicum annuum L extract.

  10. Rapid, room-temperature synthesis of amorphous selenium/protein composites using Capsicum annuum L extract

    International Nuclear Information System (INIS)

    Li Shikuo; Shen Yuhua; Xie Anjian; Yu Xuerong; Zhang Xiuzhen; Yang Liangbao; Li Chuanhao

    2007-01-01

    We describe the formation of amorphous selenium (α-Se)/protein composites using Capsicum annuum L extract to reduce selenium ions (SeO 3 2- ) at room temperature. The reaction occurs rapidly and the process is simple and easy to handle. A protein with a molecular weight of 30 kDa extracted from Capsicum annuum L not only reduces the SeO 3 2- ions to Se 0 , but also controls the nucleation and growth of Se 0 , and even participates in the formation of α-Se/protein composites. The size and shell thickness of the α-Se/protein composites increases with high Capsicum annuum L extract concentration, and decreases with low reaction solution pH. The results suggest that this eco-friendly, biogenic synthesis strategy could be widely used for preparing inorganic/organic biocomposites. In addition, we also discuss the possible mechanism of the reduction of SeO 3 2- ions by Capsicum annuum L extract

  11. High-temperature Ionization-induced Synthesis of Biologically Relevant Molecules in the Protosolar Nebula

    Science.gov (United States)

    Bekaert, David V.; Derenne, Sylvie; Tissandier, Laurent; Marrocchi, Yves; Charnoz, Sebastien; Anquetil, Christelle; Marty, Bernard

    2018-06-01

    Biologically relevant molecules (hereafter biomolecules) have been commonly observed in extraterrestrial samples, but the mechanisms accounting for their synthesis in space are not well understood. While electron-driven production of organic solids from gas mixtures reminiscent of the photosphere of the protosolar nebula (PSN; i.e., dominated by CO–N2–H2) successfully reproduced key specific features of the chondritic insoluble organic matter (e.g., elementary and isotopic signatures of chondritic noble gases), the molecular diversity of organic materials has never been investigated. Here, we report that a large range of biomolecules detected in meteorites and comets can be synthesized under conditions typical of the irradiated gas phase of the PSN at temperatures = 800 K. Our results suggest that organic materials—including biomolecules—produced within the photosphere would have been widely dispersed in the protoplanetary disk through turbulent diffusion, providing a mechanism for the distribution of organic meteoritic precursors prior to any thermal/photoprocessing and subsequent modification by secondary parent body processes. Using a numerical model of dust transport in a turbulent disk, we propose that organic materials produced in the photosphere of the disk would likely be associated with small dust particles, which are coupled to the motion of gas within the disk and therefore preferentially lofted into the upper layers of the disk where organosynthesis occurs.

  12. Characterization of ceramics and intermetallics fabricated by self-propagating high-temperature synthesis

    International Nuclear Information System (INIS)

    Hurst, J.B.

    1989-05-01

    Three efforts aimed at investigating the process of self-propagating high temperature synthesis (SHS) for the fabrication of structural ceramics and intermetallics are summarized. Of special interest was the influence of processing variables such as exothermic dopants, gravity, and green state morphology in materials produced by SHS. In the first effort directed toward the fabrication of SiC, exothermic dopants of yttrium and zirconium were added to SiO2 or SiO2 + NiO plus carbon powder mix and processed by SHS. This approach was unsuccessful since it did not produce the desired product of crystalline SiC. In the second effort, the influence of gravity was investigated by examining Ni-Al microstructures which were produced by SHS combustion waves traveling with and opposite the gravity direction. Although final composition and total porosities of the combusted Ni-Al compounds were found to be gravity independent, larger pores were created in those specimens which were combusted opposite to the gravity force direction. Finally, it was found that green microstructure has a significant effect on the appearance of the combusted piece. Severe pressing laminations were observed to arrest the combustion front for TiC samples

  13. 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.

  14. Mechanically activated self-propagated high-temperature synthesis of nanometer-structured MgB2

    International Nuclear Information System (INIS)

    Radev, D.D.; Marinov, M.; Tumbalev, V.; Radev, I.; Konstantinov, L.

    2005-01-01

    Nanometer-sized MgB 2 was prepared via a two-step modification of the mechanically activated self-propagated high-temperature synthesis. The experimental conditions and some structural and phase characteristics of the synthesized product are reported. It is shown that a single-phase material can be prepared after 2 h of intense mechanical treatment of the starting magnesium and boron powders and a synthesis induced at a current-pulse density of 30 A cm -2 . The average size of MgB 2 particles synthesized in this way is 70-80 nm. It is also shown that using the same reagents and the 'classic' high-temperature interaction at 850 deg C with a protective atmosphere of pure Ar, mean particle size of the MgB 2 obtained is 50 μm

  15. P25-graphene hydrogels: room-temperature synthesis and application for removal of methylene blue from aqueous solution.

    Science.gov (United States)

    Hou, Chengyi; Zhang, Qinghong; Li, Yaogang; Wang, Hongzhi

    2012-02-29

    Herein we report a room-temperature synthesis of chemically bonded TiO2 (P25)-graphene composite hydrogels and their use as high performance visible light photocatalysts. The three-dimensional (3D) TiO2-carbon composite exhibits a significant enhancement in the reaction rate in the decontamination of methylene blue, compared to the bare P25. The 3D P25-graphene hydrogel is much easier to prepare and apply as a macroscopic device, compared to the 2D P25-graphene sheets. This work could provide new insights into the room-temperature synthesis of graphene-based materials. As a kind of the novel 3D graphene-based composite, the obtained high performance P25-graphene gel could be widely used in the environmental protection issues. Copyright © 2012. Published by Elsevier B.V.

  16. Room temperature synthesis of Ni-based alloy nanoparticles by radiolysis.

    Energy Technology Data Exchange (ETDEWEB)

    Nenoff, Tina Maria; Berry, Donald T.; Lu, Ping; Leung, Kevin; Provencio, Paula Polyak; Stumpf, Roland Rudolph; Huang, Jian Yu; Zhang, Zhenyuan

    2009-09-01

    Room temperature radiolysis, density functional theory, and various nanoscale characterization methods were used to synthesize and fully describe Ni-based alloy nanoparticles (NPs) that were synthesized at room temperature. These complementary methods provide a strong basis in understanding and describing metastable phase regimes of alloy NPs whose reaction formation is determined by kinetic rather than thermodynamic reaction processes. Four series of NPs, (Ag-Ni, Pd-Ni, Co-Ni, and W-Ni) were analyzed and characterized by a variety of methods, including UV-vis, TEM/HRTEM, HAADF-STEM and EFTEM mapping. In the first focus of research, AgNi and PdNi were studied. Different ratios of Ag{sub x}- Ni{sub 1-x} alloy NPs and Pd{sub 0.5}- Ni{sub 0.5} alloy NP were prepared using a high dose rate from gamma irradiation. Images from high-angle annular dark-field (HAADF) show that the Ag-Ni NPs are not core-shell structure but are homogeneous alloys in composition. Energy filtered transmission electron microscopy (EFTEM) maps show the homogeneity of the metals in each alloy NP. Of particular interest are the normally immiscible Ag-Ni NPs. All evidence confirmed that homogeneous Ag-Ni and Pd-Ni alloy NPs presented here were successfully synthesized by high dose rate radiolytic methodology. A mechanism is provided to explain the homogeneous formation of the alloy NPs. Furthermore, studies of Pd-Ni NPs by in situ TEM (with heated stage) shows the ability to sinter these NPs at temperatures below 800 C. In the second set of work, CoNi and WNi superalloy NPs were attempted at 50/50 concentration ratios using high dose rates from gamma irradiation. Preliminary results on synthesis and characterization have been completed and are presented. As with the earlier alloy NPs, no evidence of core-shell NP formation occurs. Microscopy results seem to indicate alloying occurred with the CoNi alloys. However, there appears to be incomplete reduction of the Na{sub 2}WO{sub 4} to form the W

  17. A Novel Practical Synthesis of Phenanthrenes Using Iron(Ⅲ) Chloride Involved Intramolecular Oxidative Coupling at Room Temperature

    Institute of Scientific and Technical Information of China (English)

    L(U),Mao-Yun; WANG,Kai-Liang; CAI,Fei; WANG,Hai-Ying; WANG,Qing-Min

    2008-01-01

    Iron(Ⅲ) chloride has been used to prepare the polymethoxy substituted phenanthrene derivatives via in-tramolecular oxidative coupling of (E or Z)-2,3-di(substituted phenyl)acrylate at room temperature in excellent yields. Mild reaction conditions and the use of inexpensive and nontoxic FeCI3 provide a novel practical and large-scaled viable route for the synthesis of the important phenanthrene rings.

  18. Environmentally friendly room temperature strecker reaction:one-pot synthesis of α-aminonitriles in ionic liquid

    International Nuclear Information System (INIS)

    Mojtahedi, M. M.; Abaee, M.S.; Abbasi, H.

    2006-01-01

    A three component efficient and facile procedure is developed for the synthesis of a-aminonitriles from aromatic-and aliphatic aldehydes, amines, and trimethylsilyl cyanide in 1-butyl-3-methyl-1H-imidazolium perchlorate ([bmim][C1O 4 ]) ionic liquid as the reaction medium at room temperature. Excellent yields are obtained in this one-pot procedure with short reaction times and the ionic liquid medium reused several times in a row

  19. Low-temperature synthesis and characterization of helical carbon fibers by one-step chemical vapour deposition

    Energy Technology Data Exchange (ETDEWEB)

    Jin, Yongzhong [Department of Materials and Chemistry Engineering, Sichuan University of Science and Engineering, 643000 Zigong, Sichuan (China); Chen, Jian, E-mail: wuhangzs@163.com [Department of Materials and Chemistry Engineering, Sichuan University of Science and Engineering, 643000 Zigong, Sichuan (China); Fu, Qingshan [Department of Materials and Chemistry Engineering, Sichuan University of Science and Engineering, 643000 Zigong, Sichuan (China); Li, Binghong [China Rubber Group Carbon Black Industry Research and Design Institute, 643000 Zigong, Sichuan (China); Zhang, Huazhi; Gong, Yong [Department of Materials and Chemistry Engineering, Sichuan University of Science and Engineering, 643000 Zigong, Sichuan (China)

    2015-01-01

    Graphical abstract: - Highlights: • HCNFs were synthesized by one-step CVD using cupric tartrate as a catalyst at temperature below 500 °C. • The synthesis of HCNFs is highly temperature-dependent at the synthesis temperature of 280–480 °C. • The addition of HCNFs makes a noticeable contribution to the reinforcement of NR/CB system. - Abstract: Helical carbon fibers (HCNFs) were synthesized by one-step chemical vapour deposition using cupric tartrate as a catalyst at temperature below 500 °C. The bound rubber of natural rubber (NR)/HCNFs were also prepared in this study. The results of thermogravimetry–differential scanning calorimetry (TG/DSC) for cupric tartrate nanoparticles show that the transformation of C{sub 4}H{sub 4}CuO{sub 6} → Cu reaction occurs at ∼250–310 °C. The characterization of scanning electron microscopy (SEM), transmission electron microscope (TEM), X-ray diffraction (XRD) and Raman spectrum for the synthesized products confirms that the synthesis of HCNFs is highly temperature-dependent. The straight fibers with the fiber diameter of 100–400 nm are obtained at 280 °C and HCNFs can be synthesized at higher temperature, with the coil diameter of 0.5–1 μm and fiber diameter of 100–200 nm at 380 °C, and the coil diameter of ∼100 nm and fiber diameter of ∼80 nm at 480 °C. The maximum of the bound-rubber content (37%) can be obtained with the addition of 100 wt.% HCNFs in NR, which indicates that the coiled configuration of HCNFs makes a noticeable contribution to the reinforcement of NR/CB system.

  20. Low-temperature synthesis and characterization of helical carbon fibers by one-step chemical vapour deposition

    International Nuclear Information System (INIS)

    Jin, Yongzhong; Chen, Jian; Fu, Qingshan; Li, Binghong; Zhang, Huazhi; Gong, Yong

    2015-01-01

    Graphical abstract: - Highlights: • HCNFs were synthesized by one-step CVD using cupric tartrate as a catalyst at temperature below 500 °C. • The synthesis of HCNFs is highly temperature-dependent at the synthesis temperature of 280–480 °C. • The addition of HCNFs makes a noticeable contribution to the reinforcement of NR/CB system. - Abstract: Helical carbon fibers (HCNFs) were synthesized by one-step chemical vapour deposition using cupric tartrate as a catalyst at temperature below 500 °C. The bound rubber of natural rubber (NR)/HCNFs were also prepared in this study. The results of thermogravimetry–differential scanning calorimetry (TG/DSC) for cupric tartrate nanoparticles show that the transformation of C 4 H 4 CuO 6 → Cu reaction occurs at ∼250–310 °C. The characterization of scanning electron microscopy (SEM), transmission electron microscope (TEM), X-ray diffraction (XRD) and Raman spectrum for the synthesized products confirms that the synthesis of HCNFs is highly temperature-dependent. The straight fibers with the fiber diameter of 100–400 nm are obtained at 280 °C and HCNFs can be synthesized at higher temperature, with the coil diameter of 0.5–1 μm and fiber diameter of 100–200 nm at 380 °C, and the coil diameter of ∼100 nm and fiber diameter of ∼80 nm at 480 °C. The maximum of the bound-rubber content (37%) can be obtained with the addition of 100 wt.% HCNFs in NR, which indicates that the coiled configuration of HCNFs makes a noticeable contribution to the reinforcement of NR/CB system

  1. Room temperature synthesis of Si-MCM-41 using polymeric version of ethyl silicate as a source of silica

    International Nuclear Information System (INIS)

    Gaydhankar, T.R.; Samuel, V.; Jha, R.K.; Kumar, R.; Joshi, P.N.

    2007-01-01

    Synthesis of mesoporous MCM-41 materials at room temperature using less expensive polymeric version of ethyl silicate (40 wt% SiO 2 ) as a source of silica was established. The influence of crucial synthesis parameters such as molar ratios of H 2 O/NH 4 OH, NH 4 OH/SiO 2 and CTMABr/SiO 2 in gel on the quality of the phase formed was investigated. Powder X-ray diffraction (XRD), scanning electron microscopy (SEM) and low temperature N 2 adsorption-desorption isotherms have been employed to characterize the products. The magnitude of orderness, textural properties and thermal stability of the Si-MCM-41 samples prepared under identical judiciously pre-controlled synthesis conditions using ethyl silicate and conventional tetraethyl orthosilicate (TEOS) were assessed. Even though, ethyl silicate has proved to be suitable source for the preparation of MCM-41 at room temperature, there exists an optimum value of H 2 O/NH 4 OH for different NH 4 OH/SiO 2 molar ratios in the gel. Changes in the morphology were observed when NH 4 OH/SiO 2 , H 2 O/NH 4 OH molar ratios in the gels were changed

  2. Low-temperature hydrothermal synthesis of ZnO nanorods: Effects of zinc salt concentration, various solvents and alkaline mineralizers

    Energy Technology Data Exchange (ETDEWEB)

    Edalati, Khatereh, E-mail: kh_ed834@stu.um.ac.ir [Department of Metallurgical Engineering, Faculty of Engineering, Ferdowsi University of Mashhad (FUM) Campus, Azadi Sq., Mashhad, Khorasan Razavi (Iran, Islamic Republic of); Shakiba, Atefeh [Department of Material Science and Metallurgy, Amirkabir University of Technology, Tehran (Iran, Islamic Republic of); Vahdati-Khaki, Jalil; Zebarjad, Seyed Mojtaba [Department of Metallurgical Engineering, Faculty of Engineering, Ferdowsi University of Mashhad (FUM) Campus, Azadi Sq., Mashhad, Khorasan Razavi (Iran, Islamic Republic of)

    2016-02-15

    Highlights: • We synthesized ZnO nanorods by a simple hydrothermal process at 60 °C. • Effects of zinc salt concentration, solvent and alkaline mineralizer was studied. • Increasing concentration of zinc salt changed ZnO nucleation system. • NaOH yielded better results in the production of nanorods in both solvents. • Methanol performed better in the formation of nanorods using the two mineralizers. - Abstract: ZnO has been produced using various methods in the solid, gaseous, and liquid states, and the hydrothermal synthesis at low temperatures has been shown to be an environmentally-friendly one. The current work utilizes a low reaction temperature (60 °C) for the simple hydrothermal synthesis of ZnO nanorod morphologies. Furthermore, the effects of zinc salt concentration, solvent type and alkaline mineralizer type on ZnO nanorods synthesis at a low reaction temperature by hydrothermal processing was studied. Obtained samples were analyzed using X-ray powder diffraction (XRD) and scanning electron microscopy (SEM). Increasing the concentration of the starting zinc salt from 0.02 to 0.2 M changed ZnO nucleation system from the homogeneous to the heterogeneous state. The XRD results confirmed the production hexagonal ZnO nanostructures of with a crystallite size of 40.4 nm. Varying the experimental parameters (mineralizer and solvent) yielded ZnO nanorods with diameters ranging from 90–250 nm and lengths of 1–2 μm.

  3. Synthesis and characterization of CoPt nanoparticles prepared by room temperature chemical reduction with PAMAM dendrimer as template.

    Science.gov (United States)

    Wan, Haiying; Shi, Shifan; Bai, Litao; Shamsuzzoha, Mohammad; Harrell, J W; Street, Shane C

    2010-08-01

    We describe an approach to synthesize monodisperse CoPt nanoparticles with dendrimer as template by a simple chemical reduction method in aqueous solution using NaBH4 as reducing agent at room temperature. The as-made CoPt nanoparticles buried in the dendrimer matrix have the chemically disordered fcc structure and can be transformed to the fct phase after annealing at 700 degrees C. This is the first report of dendrimer-mediated room temperature synthesis of monodisperse magnetic nanoparticles in aqueous solution.

  4. The thermochemical behavior of some binary shape memory alloys by high temperature direct synthesis calorimetry

    International Nuclear Information System (INIS)

    Meschel, S.V.; Pavlu, J.; Nash, P.

    2011-01-01

    Research highlights: → We studied 14 shape memory alloys. → The enthalpies of formation and structure characteristics are summarized. → Theoretical predictions by ab initio calculations compare better with experimental measurements than Miedema's semi empirical model. - Abstract: The standard enthalpies of formation of some shape memory alloys have been measured by high temperature direct synthesis calorimetry at 1373 K. The following results (in kJ/mol of atoms) are reported: CoCr (-0.3 ± 2.9); CuMn (-3.7 ± 3.2); Cu 3 Sn (-10.4 ± 3.1); Fe 2 Tb (-5.5 ± 2.4); Fe 2 Dy (-1.6 ± 2.9); Fe 17 Tb 2 (-2.1 ± 3.1); Fe 17 Dy 2 (-5.3 ± 1.7); FePd 3 (-16.0 ± 2.7); FePt (-23.0 ± 1.9); FePt 3 (-20.7 ± 2.3); NiMn (-24.9 ± 2.6); TiNi (-32.7 ± 1.0); TiPd (-60.3 ± 2.5). The results are compared with some earlier experimental values obtained by calorimetry and by EMF technique. They are also compared with predicted values on the basis of the semi empirical model of Miedema and co-workers and with ab initio calculations when available. We will also assess the available information regarding the structures of these alloys.

  5. Synthesis of zinc oxide microrods and nano-fibers with dominant exciton emission at room temperature

    Energy Technology Data Exchange (ETDEWEB)

    Ramos-Brito, F., E-mail: fro_brito@yahoo.com.m [Laboratorio de Materiales Optoelectronicos del Centro de Ciencias de Sinaloa, Ave. de las Americas 2771 Col. Villa Universidad 80010, Culiacan, Sinaloa (Mexico); Alejo-Armenta, C. [Laboratorio de Materiales Optoelectronicos del Centro de Ciencias de Sinaloa, Ave. de las Americas 2771 Col. Villa Universidad 80010, Culiacan, Sinaloa (Mexico); Garcia-Hipolito, M. [Departamento de Materiales Metalicos y Ceramicos, Instituto de Investigaciones en Materiales, Universidad Nacional Autonoma de Mexico, AP 70-360, Coyoacan 04510, DF (Mexico); Camarillo, E.; Hernandez A, J. [Instituto de Fisica, Universidad Nacional Autonoma de Mexico, AP 20-364, Alvaro Obregon 01000, DF (Mexico); Falcony, C. [Departamento de Fisica, CINVESTAV-IPN, AP 14-740, 07000, DF (Mexico); Murrieta S, H. [Instituto de Fisica, Universidad Nacional Autonoma de Mexico, AP 20-364, Alvaro Obregon 01000, DF (Mexico)

    2011-05-15

    Employing a simple chemical synthesis method, hexagonal-shaped zinc oxide microrods and zinc oxide nano-fibers were deposited on pyrex-glass and aluminum substrates, respectively. Both kinds of deposits showed zincite crystalline phase with lattice parameters: a=3.2498 A and c=5.2066 A. Microrods showed very uniform wide and large sizes of around 1 and 10 {mu}m, respectively. Both deposits were homogeneous over all substrate surfaces. Microrods and nano-fibers resulted with good optical quality and with preferential crystalline growth in [1 0 1 0]and [0 0 0 1]directions. The principal optical characteristics for both microrods and nano-fibers were: a) room-temperature photo and cathodo-luminescent spectra with strong exciton emission centered around 390 nm and with FWHMs around 125 and 160 meV, respectively, b) poor photo and cathode-luminescent emissions in the visible region of the electromagnetic spectrum, c) energy band gap of 3.32 eV, d) good emission efficiency supported by the not-required high energy densities to obtain strong exciton emission and e) good ZnO stoichiometry endorsed by photoluminescent results. These characteristics make of these microrods and nano-fibers good for potential photonic applications. - Research highlights: {yields} Microrods and nano-fibers resulted with good optical quality and with preferential crystalline growth in [1 0 1 0]and [0 0 0 1]directions. {yields} Microrods and nano-fibers resulted with good emission efficiency supported by the not-required high energy densities to obtain strong exciton emission. {yields} The wet chemical method is appropriated for deposition of microrods and nano-fibers with the desired optical properties for its possible application in photonics.

  6. Synthesis of zinc oxide microrods and nano-fibers with dominant exciton emission at room temperature

    International Nuclear Information System (INIS)

    Ramos-Brito, F.; Alejo-Armenta, C.; Garcia-Hipolito, M.; Camarillo, E.; Hernandez A, J.; Falcony, C.; Murrieta S, H.

    2011-01-01

    Employing a simple chemical synthesis method, hexagonal-shaped zinc oxide microrods and zinc oxide nano-fibers were deposited on pyrex-glass and aluminum substrates, respectively. Both kinds of deposits showed zincite crystalline phase with lattice parameters: a=3.2498 A and c=5.2066 A. Microrods showed very uniform wide and large sizes of around 1 and 10 μm, respectively. Both deposits were homogeneous over all substrate surfaces. Microrods and nano-fibers resulted with good optical quality and with preferential crystalline growth in [1 0 1 0] and [0 0 0 1] directions. The principal optical characteristics for both microrods and nano-fibers were: a) room-temperature photo and cathodo-luminescent spectra with strong exciton emission centered around 390 nm and with FWHMs around 125 and 160 meV, respectively, b) poor photo and cathode-luminescent emissions in the visible region of the electromagnetic spectrum, c) energy band gap of 3.32 eV, d) good emission efficiency supported by the not-required high energy densities to obtain strong exciton emission and e) good ZnO stoichiometry endorsed by photoluminescent results. These characteristics make of these microrods and nano-fibers good for potential photonic applications. - Research highlights: → Microrods and nano-fibers resulted with good optical quality and with preferential crystalline growth in [1 0 1 0] and [0 0 0 1] directions. → Microrods and nano-fibers resulted with good emission efficiency supported by the not-required high energy densities to obtain strong exciton emission. → The wet chemical method is appropriated for deposition of microrods and nano-fibers with the desired optical properties for its possible application in photonics.

  7. Influence of Synthesis Temperature on the Growth and Surface Morphology of Co3O4 Nanocubes for Supercapacitor Applications

    Science.gov (United States)

    Samal, Rashmirekha; Dash, Barsha; Sarangi, Chinmaya Kumar; Subbaiah, Tondepu; Senanayake, Gamini; Minakshi, Manickam

    2017-01-01

    A facile hydrothermal route to control the crystal growth on the synthesis of Co3O4 nanostructures with cube-like morphologies has been reported and tested its suitability for supercapacitor applications. The chemical composition and morphologies of the as-prepared Co3O4 nanoparticles were extensively characterized using X-ray diffraction (XRD) and transmission electron microscopy (TEM). Varying the temperature caused considerable changes in the morphology, the electrochemical performance increased with rising temperature, and the redox reactions become more reversible. The results showed that the Co3O4 synthesized at a higher temperature (180 °C) demonstrated a high specific capacitance of 833 F/g. This is attributed to the optimal temperature and the controlled growth of nanocubes. PMID:29088061

  8. Graphene synthesis on SiC: Reduced graphitization temperature by C-cluster and Ar-ion implantation

    International Nuclear Information System (INIS)

    Zhang, R.; Li, H.; Zhang, Z.D.; Wang, Z.S.; Zhou, S.Y.; Wang, Z.; Li, T.C.; Liu, J.R.; Fu, D.J.

    2015-01-01

    Thermal decomposition of SiC is a promising method for high quality production of wafer-scale graphene layers, when the high decomposition temperature of SiC is substantially reduced. The high decomposition temperature of SiC around 1400 °C is a technical obstacle. In this work, we report on graphene synthesis on 6H–SiC with reduced graphitization temperature via ion implantation. When energetic Ar, C 1 and C 6 -cluster ions implanted into 6H–SiC substrates, some of the Si–C bonds have been broken due to the electronic and nuclear collisions. Owing to the radiation damage induced bond breaking and the implanted C atoms as an additional C source the graphitization temperature was reduced by up to 200 °C

  9. Mg(OH){sub 2} nanoparticles produced at room temperature by an innovative, facile, and scalable synthesis route

    Energy Technology Data Exchange (ETDEWEB)

    Taglieri, Giuliana, E-mail: giuliana.taglieri@univaq.it; Felice, Benito; Daniele, Valeria; Ferrante, Fabiola [University of L’Aquila, Department of Industrial and Information Engineering and Economics (Italy)

    2015-10-15

    Nanoparticles form the fundamental building blocks for many exciting applications in various scientific disciplines. However, the problem of the large-scale synthesis of nanoparticles remains challenging. An original, eco-friendly, single step, and scalable method to produce magnesium hydroxide nanoparticles in aqueous suspensions is here presented. The method, based on an exchange ion process, is extremely simple and rapid (few minutes). It employs cheap or renewable reactants, operates at room temperature and does not require intermediate steps (washings/purifications) to eliminate undesired compounds. Moreover, it is possible to regenerate the exchange material and to reuse it for new operation of synthesis, according to a cyclic procedure, providing potential aptitudes of scalability of nanoparticles production. Some of the synthesis parameters are varied, and structural and morphological features of the produced nanoparticles, after few seconds from the beginning of the synthesis up to the ending time, are investigated by means of several techniques, such as X-ray diffraction (profile fitting and Rietveld refinement), transmission electron microscopy, infrared spectroscopy, thermal analyses, and surface area measurements. In any case, pure and stable suspensions are produced, characterized by crystalline and mesoporous Mg(OH){sub 2} nanoparticles, with lamellar morphology. In particular, the nanolamellas appeared constituted by a superimposition of hexagonally plated and crystalline nanosized precursors (2–3 nm in dimensions), crystallographically oriented.

  10. Ab Initio Guided Low Temperature Synthesis Strategy for Smooth Face–Centred Cubic FeMn Thin Films

    Directory of Open Access Journals (Sweden)

    Friederike Herrig

    2018-05-01

    Full Text Available The sputter deposition of FeMn thin films with thicknesses in the range of hundred nanometres and beyond requires relatively high growth temperatures for the formation of the face-centred cubic (fcc phase, which results in high thin film roughness. A low temperature synthesis strategy, based on local epitaxial growth of a 100 nm thick fcc FeMn film as well as a Cu nucleation layer on an α-Al2O3 substrate at 160 °C, enables roughness values (Ra as low as ~0.6 nm, which is in the same order of magnitude as the pristine substrate (~0.1 nm. The synthesis strategy is guided by ab initio calculations, indicating very strong interfacial bonding of the Cu nucleation layer to an α-Al2O3 substrate (work of separation 5.48 J/m²—which can be understood based on the high Cu coordination at the interface—and between fcc FeMn and Cu (3.45 J/m². Accompanied by small lattice misfits between these structures, the strong interfacial bonding is proposed to enable the local epitaxial growth of a smooth fcc FeMn thin film. Based on the here introduced synthesis strategy, the implementation of fcc FeMn based thin film model systems for materials with interface dominated properties such as FeMn steels containing κ-carbide precipitates or secondary phases appears meaningful.

  11. Facile synthesis of concentrated gold nanoparticles with low size-distribution in water: temperature and pH controls

    Directory of Open Access Journals (Sweden)

    Li Chunfang

    2011-01-01

    Full Text Available Abstract The citrate reduction method for the synthesis of gold nanoparticles (GNPs has known advantages but usually provides the products with low nanoparticle concentration and limits its application. Herein, we report a facile method to synthesize GNPs from concentrated chloroauric acid (2.5 mM via adding sodium hydroxide and controlling the temperature. It was found that adding a proper amount of sodium hydroxide can produce uniform concentrated GNPs with low size distribution; otherwise, the largely distributed nanoparticles or instable colloids were obtained. The low reaction temperature is helpful to control the nanoparticle formation rate, and uniform GNPs can be obtained in presence of optimized NaOH concentrations. The pH values of the obtained uniform GNPs were found to be very near to neutral, and the pH influence on the particle size distribution may reveal the different formation mechanism of GNPs at high or low pH condition. Moreover, this modified synthesis method can save more than 90% energy in the heating step. Such environmental-friendly synthesis method for gold nanoparticles may have a great potential in large-scale manufacturing for commercial and industrial demand.

  12. Facile synthesis of concentrated gold nanoparticles with low size-distribution in water: temperature and pH controls

    Science.gov (United States)

    Li, Chunfang; Li, Dongxiang; Wan, Gangqiang; Xu, Jie; Hou, Wanguo

    2011-07-01

    The citrate reduction method for the synthesis of gold nanoparticles (GNPs) has known advantages but usually provides the products with low nanoparticle concentration and limits its application. Herein, we report a facile method to synthesize GNPs from concentrated chloroauric acid (2.5 mM) via adding sodium hydroxide and controlling the temperature. It was found that adding a proper amount of sodium hydroxide can produce uniform concentrated GNPs with low size distribution; otherwise, the largely distributed nanoparticles or instable colloids were obtained. The low reaction temperature is helpful to control the nanoparticle formation rate, and uniform GNPs can be obtained in presence of optimized NaOH concentrations. The pH values of the obtained uniform GNPs were found to be very near to neutral, and the pH influence on the particle size distribution may reveal the different formation mechanism of GNPs at high or low pH condition. Moreover, this modified synthesis method can save more than 90% energy in the heating step. Such environmental-friendly synthesis method for gold nanoparticles may have a great potential in large-scale manufacturing for commercial and industrial demand.

  13. Experimental and Numerical Studies on Self-Propagating High-Temperature Synthesis of Ta5Si3 Intermetallics

    Directory of Open Access Journals (Sweden)

    Chun-Liang Yeh

    2015-09-01

    Full Text Available Formation of Ta5Si3 by self-propagating high-temperature synthesis (SHS from elemental powder compacts of Ta:Si = 5:3 was experimentally and numerically studied. Experimental evidence showed that the increase of either sample density or preheating temperature led to the increase of combustion wave velocity and reaction temperature. The apparent activation energy, Ea ≈ 108 kJ/mol, was determined for the synthesis reaction. Based upon numerical simulation, the Arrhenius factor of the rate function, K0 = 2.5 × 107 s−1, was obtained for the 5Ta + 3Si combustion system. In addition, the influence of sample density on combustion wave kinetics was correlated with the effective thermal conductivity (keff of the powder compact. By adopting 0.005 ≤ keff/kbulk ≤ 0.016 in the computation model, the calculated combustion velocity and temperature were in good agreement with experimental data of the samples with compaction densities between 35% and 45% theoretical maximum density (TMD.

  14. Effect of temperature on the synthesis of silver nanoparticles with polyethylene glycol: new insights into the reduction mechanism

    Energy Technology Data Exchange (ETDEWEB)

    Fleitas-Salazar, Noralvis; Silva-Campa, Erika; Pedroso-Santana, Seidy; Tanori, Judith; Pedroza-Montero, Martín R.; Riera, Raúl, E-mail: rriera@cifus.uson.mx [Universidad de Sonora (Mexico)

    2017-03-15

    Polyethylene glycol (PEG) molecules act as a reducing and stabilizing agent in the formation of silver nanoparticles. PEG undergoes thermal oxidative degradation at temperatures over 70 °C in the presence of oxygen. Here, we studied how the temperature and an oxidizing atmosphere could affect the synthesis of silver nanoparticles with PEG. We tested different AgNO{sub 3} concentrations for nanoparticles syntheses using PEG of low molecular weight, at 60 and 100 °C. At the higher temperature, the reducing action of PEG increased and the effect of PEG/Ag{sup +} ratio on nanoparticles aggregation changed. These results suggest that different synthesis mechanisms operate at 60 and 100 °C. Thus, at 60 °C the reduction of silver ions can occur through the oxidation of the hydroxyl groups of PEG, as has been previously reported. We propose that the thermal oxidative degradation of PEG at 100 °C increases the number of both, functional groups and molecules that can reduce silver ions and stabilize silver nanoparticles. This degradation process could explain the enhancement of PEG reducing action observed by other authors when they increase the reaction temperature or use a PEG of higher molecular weight.

  15. A novel high pressure, high temperature vessel used to conduct long-term stability measurements of silicon MEMS pressure transducers

    Science.gov (United States)

    Wisniewiski, David

    2014-03-01

    The need to quantify and to improve long-term stability of pressure transducers is a persistent requirement from the aerospace sector. Specifically, the incorporation of real-time pressure monitoring in aircraft landing gear, as exemplified in Tire Pressure Monitoring Systems (TPMS), has placed greater demand on the pressure transducer for improved performance and increased reliability which is manifested in low lifecycle cost and minimal maintenance downtime through fuel savings and increased life of the tire. Piezoresistive (PR) silicon MEMS pressure transducers are the primary choice as a transduction method for this measurement owing to their ability to be designed for the harsh environment seen in aircraft landing gear. However, these pressure transducers are only as valuable as the long-term stability they possess to ensure reliable, real-time monitoring over tens of years. The "heart" of the pressure transducer is the silicon MEMS element, and it is at this basic level where the long-term stability is established and needs to be quantified. A novel High Pressure, High Temperature (HPHT) vessel has been designed and constructed to facilitate this critical measurement of the silicon MEMS element directly through a process of mechanically "floating" the silicon MEMS element while being subjected to the extreme environments of pressure and temperature, simultaneously. Furthermore, the HPHT vessel is scalable to permit up to fifty specimens to be tested at one time to provide a statistically significant data population on which to draw reasonable conclusions on long-term stability. With the knowledge gained on the silicon MEMS element, higher level assembly to the pressure transducer envelope package can also be quantified as to the build-effects contribution to long-term stability in the same HPHT vessel due to its accommodating size. Accordingly, a HPHT vessel offering multiple levels of configurability and robustness in data measurement is presented, along

  16. Computer modeling of the process of self-propagating high-temperature synthesis in thin system Ni-Al

    International Nuclear Information System (INIS)

    Poletayev, G.M.; Starostenkov, M.D.; Denisova, N.F.; Skakov, M.K.

    2004-01-01

    Full text: The process of synthesis of thermal phases of the system Ni-Al is studied through the method of molecular dynamics. As the object of investigation was chosen two-dimensional crystal, that corresponds to atomic packing laying at the plane of volumetric fcc crystal. Clean Ni was taken as a matrix crystal. A particle of clean Al is packed in the center of matrix block. Beyond the bounds of calculated block crystal packing is repeated with the help of periodical border conditions. The interaction between different pairs of atoms is set by pair potential function of Morse, considering interatomic bonding of the point of the sixth coordinate sphere. The allocation of speeds of atomic function in the system is set through the Boltzmann factor, depending the temperature. When the bicrystal is represented by the ideal atom packing and there are no vacancies , the process of structural adjustment is only observed at the temperature, that is higher than melting point. At that, structural adjustment is observed in circular mechanism of atom allocation, also through the border between phases of clean Ni and Al. As a result, Al particle is transformed, at the border between metals, fields of positional disorder and embryos of intermetallide phases NiAl 2 , Ni 2 Al, Ni 3 Al. The introduction of of free volume through the creation of vacancies significantly lowers the temperature of the beginning of the synthesis process of intermetallide phases. The greatest decrease in temperature to the point of 300 K happens, when the vacancies are located in Ni field of bicrystal, the beginning of the thermo-activation is directly connected with the distance from interphase borders. As the process of thermo-activation continues, vacancies located in Ni matrix right up to seventh neighborhood relatively the border bicrystal. During thermo-activation Al particles enter the field and activate the synthesis process

  17. Analysis of the structural stability of the smectite submitted to high pressures and temperatures; Analise da estabilidade estrutural da esmectita sob altas pressoes e altas temperaturas

    Energy Technology Data Exchange (ETDEWEB)

    Alabarse, Frederico Gil

    2009-10-15

    The thermal stability of bentonite is of particular interest for containment barrier in nuclear waste disposal facilities. However, very little is known about the stability of smectite (principal component of bentonite) under high-pressure and high-temperature conditions (HPHT). The objective of this work was to investigate the stability of the smectite structure under HP-HT conditions. The HP-HT experiments were performed on toroidal chambers (TC) with pressure up 7.7 GPa and temperatures of 1000 deg C. The samples were characterized by X-ray diffraction after the HP-HT processing. Furthermore, one sample from the original material was analyzed using Fourier transformed infra-red (FTIR) in situ measurements on a diamond anvil cell (DAC) in experiments up to 12 GPa. The original sample of bentonite, calcium dioctahedral montmorillonite with small fraction of quartz, was characterized by FTIR, XRD, X-ray fluorescence (XRF), scanning electron microscopy (SEM), surface area, thermogravimetric analysis (TGA) and differential thermal analysis (DTA). In the experiment performed using the DAC up to 12 GPa, the FTIR in situ measurements analysis showed that the smectite structure is stable with a reversible deformation in the Si-O bond and that the smectite did not loose water. Experiments performed in TC at 7.7 GPa of pressure and 250 deg C of temperature, during 3.5 h showed, after analysis by XRD and FTIR, that the smectite structure is stable and did not loose water. Experiments performed in TC at 7.7 GPa of pressure and 1000 deg C of temperature, during 3.5 h showed, after analysis by XRD and SEM, the transformation of bentonite to the mineral assemblage: Coesite, Quartz, Kyanite and Pyrope. (author)

  18. Low temperature synthesis of Mo2C/W2C superlattices via ultra-thin modulated reactants

    International Nuclear Information System (INIS)

    Johnson, C.D.; Johnson, D.C.

    1996-01-01

    The authors report here a synthesis method of preparing carbide superlattices using ultra-thin modulated reactants. Initial investigations into the synthesis of the binary systems, Mo 2 C and W 2 C using ultra-thin modulated reactants revealed that both can be formed at relatively low temperatures (500 and 600 C respectively). DSC and XRD data suggested a two step reaction pathway involving interdiffusion of the initial modulated reactant followed by crystallization of the final product, if the modulation length is on the order of 10 angstrom. This information was used to form Mo 2 C/W 2 C superlattices using the structure of the ultra-thin modulated reactant to control the final superlattice period. Relatively large superlattice modulations were kinetically trapped by having several repeat units of each binary within the total repeat of the initial reactant. DSC and XRD data again are consistent with a two step reaction pathway leading to the formation of carbide superlattices

  19. Simple and Efficient Generation of Aryl Radicals from Aryl Triflates: Synthesis of Aryl Boronates and Aryl Iodides at Room Temperature.

    Science.gov (United States)

    Liu, Wenbo; Yang, Xiaobo; Gao, Yang; Li, Chao-Jun

    2017-06-28

    Despite the wide use of aryl radicals in organic synthesis, current methods to prepare them from aryl halides, carboxylic acids, boronic acids, and diazonium salts suffer from limitations. Aryl triflates, easily obtained from phenols, are promising aryl radical progenitors but remain elusive in this regard. Inspired by the single electron transfer process for aryl halides to access aryl radicals, we developed a simple and efficient protocol to convert aryl triflates to aryl radicals. Our success lies in exploiting sodium iodide as the soft electron donor assisted by light. This strategy enables the scalable synthesis of two types of important organic molecules, i.e., aryl boronates and aryl iodides, in good to high yields, with broad functional group compatibility in a transition-metal-free manner at room temperature. This protocol is anticipated to find potential applications in other aryl-radical-involved reactions by using aryl triflates as aryl radical precursors.

  20. Influence of temperature and precursor concentration on the synthesis of HDA-capped Ag{sub 2}Se nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Mlambo, M. [Department of Chemistry, Vaal University of Technology, Private Bag X021, Vanderbijlpark 1900 (South Africa); Molecular Science Institute, School of Chemistry, University of the Witwatersrand, Private Bag 3, Wits 2050 (South Africa); Moloto, M.J., E-mail: makwenam@vut.ac.za [Department of Chemistry, Vaal University of Technology, Private Bag X021, Vanderbijlpark 1900 (South Africa); Moloto, N. [Molecular Science Institute, School of Chemistry, University of the Witwatersrand, Private Bag 3, Wits 2050 (South Africa); Mdluli, P.S. [Nanotechnology Innovation Centre, Advanced Materials Division, Mintek, Private Bag X3015, Randburg 2125 (South Africa)

    2013-06-01

    Graphical abstract: The temperature effect on the growth and size of silver selenide nanoparticles with the size distribution and XRD patterns. Highlights: ► The HDA-capped Ag{sub 2}Se nanoparticles were synthesized via the colloidal route. ► Temperature and monomer concentration of the reaction were varied. ► The concentration as a factor influenced particles with a decrease observed as the amount of Ag{sup +} ion source is increased. ► Temperature has expected influence on the growth of particles resulting in increase as the temperature is increased. ► TEM images shows spherical particles and their orthorhombic phase from structural analysis by XRD. - Abstract: The size dependent of temperature and precursor concentration on the synthesis of hexadecylamine capped Ag{sub 2}Se nanoparticles via the colloidal route were studied using the combination of optical and structural analysis. The as-prepared Ag{sub 2}Se nanoparticles showed the quantum confinement with all the obtained absorption band edges blue-shifted from the bulk and their corresponding emission maxima displaying a red-shift from band edges characterised by UV–vis absorption and photoluminescence spectroscopy. The particle sizes were obtained from transmission electron microscopy analysis. The increase in precursor concentration resulted in a decrease in nanoparticle sizes. The increase in reaction temperature showed an increase in the nanoparticle sizes, when the critical temperature at 160 °C was reached, the nanoparticle sizes decreased.

  1. ZrC Ceramics Prepared by Self-propagating High-temperature Synthesis/Single Action Pressing

    Directory of Open Access Journals (Sweden)

    CHENG Yong

    2017-01-01

    Full Text Available ZrC ceramics were prepared by mechanical axial compression of self-propagating high-temperature synthesis/single action pressing (SHS/SAP.The effects of pressure on microstructure and densification of the products,as well as the relationship between displacement/variation of the load curve and SHS reaction,were studied.The structure and properties of the products were investigated by XRD and SEM.In addition,the density was measured by the drain away liquid method.Meanwhile,universal testing machine was used to record the displacement and load curve alternations.The results indicate that products are mainly composed of ZrC phase,the process of exhaust are accelerated as the increasing of pressure as well,leading to the smaller size of porosity and crystal particles.Density manifested as an increasing pattern by the elevated pressure with no longer change at 80MPa.Due to the strong attenuation of pressure at the peak of temperature,the density of the production is only 65.7% in 120MPa.The end point of the SHS reaction and the plastic time of the products can be monitored by displacement and load curve.The results provide evidence for the application of self-propagating high-temperature synthesis/pseudo-hot isostatic pressing to further improve the density of ceramics.

  2. Synthesis of AuPd alloyed nanoparticles via room-temperature electron reduction with argon glow discharge as electron source.

    Science.gov (United States)

    Yang, Manman; Wang, Zongyuan; Wang, Wei; Liu, Chang-Jun

    2014-01-01

    Argon glow discharge has been employed as a cheap, environmentally friendly, and convenient electron source for simultaneous reduction of HAuCl4 and PdCl2 on the anodic aluminum oxide (AAO) substrate. The thermal imaging confirms that the synthesis is operated at room temperature. The reduction is conducted with a short time (30 min) under the pressure of approximately 100 Pa. This room-temperature electron reduction operates in a dry way and requires neither hydrogen nor extra heating nor chemical reducing agent. The analyses using X-ray photoelectron spectroscopy (XPS) confirm all the metallic ions have been reduced. The characterization with X-ray diffraction (XRD) and high-resolution transmission electron microscopy (HRTEM) shows that AuPd alloyed nanoparticles are formed. There also exist some highly dispersed Au and Pd monometallic particles that cannot be detected by XRD and transmission electron microscopy (TEM) because of their small particle sizes. The observed AuPd alloyed nanoparticles are spherical with an average size of 14 nm. No core-shell structure can be observed. The room-temperature electron reduction can be operated in a larger scale. It is an easy way for the synthesis of AuPd alloyed nanoparticles.

  3. Synthesis and high (pressure, temperature) stability of ZnTiO3 polymorphs studied by Raman spectroscopy

    Science.gov (United States)

    Bernert, T.; Ruiz-Fuertes, J.; Bayarjargal, L.; Winkler, B.

    2015-05-01

    The phase-purity of ilmenite-type ZnTiO3 prepared by the ceramic method was investigated in dependence of the conditions during ball milling. The previously proposed addition of 2 ml ethanol to the starting materials led to a significant contamination of the product phase after a subsequent sintering process at 1073 K. However, by omitting ethanol this synthesis route led to a phase-pure sample of ZnTiO3 as confirmed by X-ray powder diffraction and Raman spectroscopy. High-temperature high-pressure experiments gave an ilmenite-type to perovskite-type phase boundary with a slope of dT/dP∼-135 K GPa-1 crossing ambient temperature conditions at ∼ 24 GPa in good agreement with previous calculations. Room-temperature high-pressure Raman spectroscopy experiments have shown the stability of the ilmenite-type phase up to a pressure of at least 38.5 GPa, the highest pressure applied in this study, indicating the presence of a kinetic barrier in this phase transition. The synthesis of ferroelectric LiNbO3-type ZnTiO3 was confirmed by second harmonic generation.

  4. STUDY OF GRINDING PROCESS OF TITANIUM CARBIDE PRODUCED WITH SELF-PROPAGATING HIGH TEMPERATURE SYNTHESIS (SPHTS)

    International Nuclear Information System (INIS)

    Kovziridze, Z.; Tabatadze, G.; Donadze, G.; Lezhava, A.; Gventsadze, D.

    2006-01-01

    It is stated that the specific character of SPHTS-preparations of TiC_x consists in crystal lattice strength reflecting the condition of synthesis in ''burning wave''. The use of roentgenographic and other methods of analysis allows to estimate the effect of the conditions of synthesis, causing carbon sublattice defect on grinding intensity of TiC_x phases. Study of the kinetics of vibro-grinding of TiC_x-phases in ethanol and benzene medium allows to establish high grinding intensity of the phases close to stoichiometry and the possibility of high depresion powderds (S_s_p H'' 4.5-6 m"2/g). (author)

  5. Low-temperature synthesis of 2D MoS2 on a plastic substrate for a flexible gas sensor.

    Science.gov (United States)

    Zhao, Yuxi; Song, Jeong-Gyu; Ryu, Gyeong Hee; Ko, Kyung Yong; Woo, Whang Je; Kim, Youngjun; Kim, Donghyun; Lim, Jun Hyung; Lee, Sunhee; Lee, Zonghoon; Park, Jusang; Kim, Hyungjun

    2018-05-08

    The efficient synthesis of two-dimensional molybdenum disulfide (2D MoS2) at low temperatures is essential for use in flexible devices. In this study, 2D MoS2 was grown directly at a low temperature of 200 °C on both hard (SiO2) and soft substrates (polyimide (PI)) using chemical vapor deposition (CVD) with Mo(CO)6 and H2S. We investigated the effect of the growth temperature and Mo concentration on the layered growth by Raman spectroscopy and microscopy. 2D MoS2 was grown by using low Mo concentration at a low temperature. Through optical microscopy, Raman spectroscopy, X-ray photoemission spectroscopy, photoluminescence, and transmission electron microscopy measurements, MoS2 produced by low-temperature CVD was determined to possess a layered structure with good uniformity, stoichiometry, and a controllable number of layers. Furthermore, we demonstrated the realization of a 2D MoS2-based flexible gas sensor on a PI substrate without any transfer processes, with competitive sensor performance and mechanical durability at room temperature. This fabrication process has potential for burgeoning flexible and wearable nanotechnology applications.

  6. Tuning the shell thickness-dependent plasmonic absorption of Ag coated Au nanocubes: The effect of synthesis temperature

    Energy Technology Data Exchange (ETDEWEB)

    Zhu, Jian, E-mail: jianzhusummer@163.com; Zhang, Fan; Chen, Bei-Bei; Li, Jian-Jun; Zhao, Jun-Wu, E-mail: nanoptzhao@163.com

    2015-09-15

    Graphical abstract: Ag coating leads to great enhancement of SPR absorbance of Au nanocubes, and the Ag coating-dependent non-monotonous SPR shift is greater at lower temperature. - Highlights: • Au nanocubes with more uniform shape can be obtained at lower growth temperature. • Ag coating leads to great enhancement of SPR absorption intensity. • The Ag coating dependent non-monotonous SPR shift is greater at lower temperature. - Abstract: The temperature dependent synthesis and plasmonic optical properties of Ag coated Au nanocubes have been investigated experimentally. It has been found that the Au nanocubes with more uniform morphology and higher yield could be obtained by decreasing the growth temperature. Because of the non-spherical symmetry of the particles shape and the plasmon coupling between Au–Ag interface and outer Ag surface, four absorption peaks at most have been observed. As the Ag coating thickness is increased, the absorbance intensity of these plasmon peaks gets intense greatly, and the absorption peak at longest wavelength blue shifts firstly and then red shifts. The non-monotonous plasmonic shift has been attributed to the competition between the increase of Ag composition and the enlargement of the particle size. What's more, the wavelength region of both blue shift and red shift could also be enhanced by decreasing the temperature.

  7. Tuning the shell thickness-dependent plasmonic absorption of Ag coated Au nanocubes: The effect of synthesis temperature

    International Nuclear Information System (INIS)

    Zhu, Jian; Zhang, Fan; Chen, Bei-Bei; Li, Jian-Jun; Zhao, Jun-Wu

    2015-01-01

    Graphical abstract: Ag coating leads to great enhancement of SPR absorbance of Au nanocubes, and the Ag coating-dependent non-monotonous SPR shift is greater at lower temperature. - Highlights: • Au nanocubes with more uniform shape can be obtained at lower growth temperature. • Ag coating leads to great enhancement of SPR absorption intensity. • The Ag coating dependent non-monotonous SPR shift is greater at lower temperature. - Abstract: The temperature dependent synthesis and plasmonic optical properties of Ag coated Au nanocubes have been investigated experimentally. It has been found that the Au nanocubes with more uniform morphology and higher yield could be obtained by decreasing the growth temperature. Because of the non-spherical symmetry of the particles shape and the plasmon coupling between Au–Ag interface and outer Ag surface, four absorption peaks at most have been observed. As the Ag coating thickness is increased, the absorbance intensity of these plasmon peaks gets intense greatly, and the absorption peak at longest wavelength blue shifts firstly and then red shifts. The non-monotonous plasmonic shift has been attributed to the competition between the increase of Ag composition and the enlargement of the particle size. What's more, the wavelength region of both blue shift and red shift could also be enhanced by decreasing the temperature

  8. An Efficient Protocol for the Synthesis of Quinoxaline Derivatives at Room Temperature Using Recyclable Alumina-Supported Heteropolyoxometalates

    Directory of Open Access Journals (Sweden)

    Diego M. Ruiz

    2012-01-01

    Full Text Available We report a suitable quinoxaline synthesis using molybdophosphovanadates supported on commercial alumina cylinders as catalysts. These catalysts were prepared by incipient wetness impregnation. The catalytic test was performed under different reaction conditions in order to know the performance of the synthesized catalysts. The method shows high yields of quinoxaline derivatives under heterogeneous conditions. Quinoxaline formation was obtained using benzyl, o-phenylenediamine, and toluene as reaction solvent at room temperature. The CuH2PMo11VO40 supported on alumina showed higher activity in the tested reaction. Finally, various quinoxalines were prepared under mild conditions and with excellent yields.

  9. Influence of the temperature on the synthesis of CdS quantum dots stabilized with poly (vinil alcohol)

    International Nuclear Information System (INIS)

    Carvalho, Andre L.B. de; Mansur, Alexandra A.P.; Mansur, Herman S.; Gonzalez, Juan C.

    2011-01-01

    Semiconductor nanoparticles (Quantum Dots, QDs) have been the subject of recent research by presenting quantum properties. This property has stimulated the study of these particles in biological applications such as bookmarks, which creates the necessity of using different synthesis routes resulting in biocompatible systems. Thus, this study aimed to evaluate the effect of temperature on the properties of QDs cadmium sulfide, aqueous route using poly (vinyl alcohol), a biocompatible polymer, such as stabilizing agent. The characterization of particles produced was performed by UV-Vis spectroscopy and photoluminescence (PL) spectra for obtaining the absorption and emission, respectively and Transmission microscopy (TEM) for analysis of the diameter of the nanocrystals. (author)

  10. Direct synthesis of multi-layer graphene film on various substrates by microwave plasma at low temperature

    Energy Technology Data Exchange (ETDEWEB)

    Park, Hyun Jae [Plasma Technology Research Center, 814-2 Osickdo-dong (SGFEZ), Gunsan, Jeollabuk-do 573-540 (Korea, Republic of); Ahn, Byung Wook; Kim, Tae Yoo; Lee, Jung Woo [School of Advanced Materials Science and Engineering, Advanced Materials and Process Research Center (AMPRC), Sungkyunkwan University, Suwon 440-746 (Korea, Republic of); Jung, Yong Ho; Choi, Yong Sup [Plasma Technology Research Center, 814-2 Osickdo-dong (SGFEZ), Gunsan, Jeollabuk-do 573-540 (Korea, Republic of); Song, Young Il, E-mail: physein01@skku.edu [School of Advanced Materials Science and Engineering, Advanced Materials and Process Research Center (AMPRC), Sungkyunkwan University, Suwon 440-746 (Korea, Republic of); Suh, Su Jeong, E-mail: suhsj@skku.edu [School of Advanced Materials Science and Engineering, Advanced Materials and Process Research Center (AMPRC), Sungkyunkwan University, Suwon 440-746 (Korea, Republic of)

    2015-07-31

    We introduce a possible route for vertically standing multi-layer graphene films (VMGs) on various substrates at low temperature by electron cyclone resonance microwave plasma. VMG films on various substrates, including copper sheet, glass and silicon oxide wafer, were analyzed by studying their structural, electrical, and optical properties. The density and temperature of plasma were measured using Cylindrical Langmuir probe analysis. The morphologies and microstructures of multi-layer graphene were characterized using field emission scattering electron microscope, high resolution transmission electron microscope, and Raman spectra measurement. The VMGs on different substrates at the same experimental conditions synthesized the wrinkled VMGs with different heights. In addition, the transmittance and electrical resistance were measured using ultra-violet visible near-infrared spectroscopy and 4 probe point surface resistance measurement. The VMGs on glass substrate obtained a transmittance of 68.8% and sheet resistance of 796 Ω/square, whereas the VMGs on SiO{sub 2} wafer substrate showed good sheet resistance of 395 Ω/square and 278 Ω/square. The results presented herein demonstrate a simple method of synthesizing of VMGs on various substrates at low temperature for mass production, in which the VMGs can be used in a wide range of application fields for energy storage, catalysis, and field emission due to their unique orientation. - Highlights: • We present for synthesis method of graphene at low temperature on various substrates. • We grow the graphene films at low temperature under of 432 °C. • Structural information of graphene films were studied upon Raman spectroscopy. • Inter-layer spacing of vertically standing graphene relies on synthesis time. • We measured a transmittance and a resistance for graphene films on difference substrate.

  11. OMS-2-Supported Cu Hydroxide-Catalyzed Benzoxazoles Synthesis from Catechols and Amines via Domino Oxidation Process at Room Temperature.

    Science.gov (United States)

    Meng, Xu; Wang, Yanmin; Wang, Yuanguang; Chen, Baohua; Jing, Zhenqiang; Chen, Gexin; Zhao, Peiqing

    2017-07-07

    In the presence of manganese oxide octahedral molecular sieve (OMS-2) supported copper hydroxide Cu(OH) x /OMS-2, aerobic synthesis of benzoxazoles from catechols and amines via domino oxidation/cyclization at room temperature is achieved. This heterogeneous benzoxazoles synthesis initiated by the efficient oxidation of catechols over Cu(OH) x /OMS-2 tolerates a variety of substrates, especially amines containing sensitive groups (hydroxyl, cyano, amino, vinyl, ethynyl, ester, and even acetyl groups) and heterocycles, which affords functionalized benzoxazoles in good to excellent yields by employing low catalyst loading (2 mol % Cu). The characterization and plausible catalytic mechanism of Cu(OH) x /OMS-2 are described. The notable features of our catalytic protocol such as the use of air as the benign oxidant and EtOH as the solvent, mild conditions, ease of product separation, being scalable up to the gram level, and superior reusability of catalyst (up to 10 cycles) make it more practical and environmentally friendly for organic synthesis.

  12. Trispyrazolylborate Complexes: An Advanced Synthesis Experiment Using Paramagnetic NMR, Variable-Temperature NMR, and EPR Spectroscopies

    Science.gov (United States)

    Abell, Timothy N.; McCarrick, Robert M.; Bretz, Stacey Lowery; Tierney, David L.

    2017-01-01

    A structured inquiry experiment for inorganic synthesis has been developed to introduce undergraduate students to advanced spectroscopic techniques including paramagnetic nuclear magnetic resonance and electron paramagnetic resonance. Students synthesize multiple complexes with unknown first row transition metals and identify the unknown metals by…

  13. Low temperature synthesis of nanosized Mn1–xZnxFe2O4 ferrites ...

    Indian Academy of Sciences (India)

    Administrator

    spectrum analysis were carried out to confirm the spinel phase formation as well as to ascertain the cation distri- bution in the ferrite ... structured materials technology opening up in the last few ... recent years, the design and synthesis of nano-magnetic particles ..... complex system like the ferrites where many cations are.

  14. ROOM TEMPERATURE BULK AND TEMPLATE-FREE SYNTHESIS OF LEUCOEMARLDINE POLYANILINE NANOFIBERS

    Science.gov (United States)

    An extremely simple single-step method is described for the bulk synthesis of nanofibers of the electronic polymer polyaniline in fully reduced state (leucoemarldine form) without using any reducing agents, surfactants, and/or large amounts of insoluble templates. Chemical oxida...

  15. Room-temperature Pd-catalyzed C-H chlorination by weak coordination: one-pot synthesis of 2-chlorophenols with excellent regioselectivity.

    Science.gov (United States)

    Sun, Xiuyun; Sun, Yonghui; Zhang, Chao; Rao, Yu

    2014-02-07

    A room-temperature Pd(II)-catalyzed regioselective chlorination reaction has been developed for a facile one-pot synthesis of a broad range of 2-chlorophenols. The reaction demonstrates an excellent regioselectivity and reactivity for C-H chlorination. This reaction represents one of the rare examples of mild C-H functionalization at ambient temperature.

  16. A green synthesis of a layered titanate, potassium lithium titanate; lower temperature solid-state reaction and improved materials performance

    International Nuclear Information System (INIS)

    Ogawa, Makoto; Morita, Masashi; Igarashi, Shota; Sato, Soh

    2013-01-01

    A layered titanate, potassium lithium titanate, with the size range from 0.1 to 30 µm was prepared to show the effects of the particle size on the materials performance. The potassium lithium titanate was prepared by solid-state reaction as reported previously, where the reaction temperature was varied. The reported temperature for the titanate preparation was higher than 800 °C, though 600 °C is good enough to obtain single-phase potassium lithium titanate. The lower temperature synthesis is cost effective and the product exhibit better performance as photocatalysts due to surface reactivity. - Graphical abstract: Finite particle of a layered titanate, potassium lithium titanate, was prepared by solid-state reaction at lower temperature to show modified materials performance. Display Omitted - Highlights: • Potassium lithium titanate was prepared by solid-state reaction. • Lower temperature reaction resulted in smaller sized particles of titanate. • 600 °C was good enough to obtain single phased potassium lithium titanate. • The product exhibited better performance as photocatalyst

  17. High temperature synthesis of ceramic composition by directed reaction of molten titanium or zirconium with boron carbide

    International Nuclear Information System (INIS)

    Johnson, W.B.

    1990-01-01

    Alternative methods of producing ceramics and ceramic composites include sintering, hot pressing and more recently hot isostatic pressing (HIP) and self-propagating high temperature synthesis (SHS). Though each of these techniques has its advantages, each suffers from several restrictions as well. Sintering may require long times at high temperatures and for most materials requires sintering aids to get full density. These additives can, and generally do, change (often degrade) the properties of the ceramic. Hot pressing and hot isostatic pressing are convenient methods to quickly prepare samples of some materials to full density, but generally are expensive and may damage some types of reinforcements during densification. This paper focuses on the preparation and processing of composites prepared by the directed reaction of molten titanium or zirconium with boron carbide. Advantages and disadvantages of this approach when compared to traditional methods are discussed, with reference to specific examples. Examples of microstructure are properties of these materials are reported

  18. Room Temperature Co-Precipitation Synthesis of Magnetite Nanoparticles in a Large pH Window with Different Bases.

    Science.gov (United States)

    Mascolo, Maria Cristina; Pei, Yongbing; Ring, Terry A

    2013-11-28

    Magnetite nanoparticles (Fe₃O₄) represent the most promising materials in medical applications. To favor high-drug or enzyme loading on the nanoparticles, they are incorporated into mesoporous materials to form a hybrid support with the consequent reduction of magnetization saturation. The direct synthesis of mesoporous structures appears to be of interest. To this end, magnetite nanoparticles have been synthesized using a one pot co-precipitation reaction at room temperature in the presence of different bases, such as NaOH, KOH or (C₂H₅)₄NOH. Magnetite shows characteristics of superparamagnetism at room temperature and a saturation magnetization (Ms) value depending on both the crystal size and the degree of agglomeration of individual nanoparticles. Such agglomeration appears to be responsible for the formation of mesoporous structures, which are affected by the pH, the nature of alkali, the slow or fast addition of alkaline solution and the drying modality of synthesized powders.

  19. Antagonistic effects of high and low temperature pretreatments on the germination and pregermination ethylene synthesis of lettuce seeds.

    Science.gov (United States)

    Burdett, A N

    1972-08-01

    Red light-induced germination of Grand Rapids lettuce seeds (Lactuca sativa L.) incubated at 20 C was inhibited if the seeds were first imbibed at 30 C for 36 hours. This effect was counteracted by exogenous ethylene and associated with a reduction in the rate at which the seeds produced ethylene throughout the pregermination period. A chilling treatment reversed the effect of a prior imbibition at 30 C on both germination and ethylene production. The possibility that the pretreatments influence germination through their effects on ethylene production is discussed.Other evidence presented indicates that the inability of seeds to germinate at supraoptimal temperature is not due either to a rapid loss of far red-absorbing phytochrome or to an inadequate capacity for ethylene synthesis. It was also shown that a chilling treatment potentiated germination at high temperature without affecting the ethylene synthetic capacity of the seeds.

  20. Room Temperature Co-Precipitation Synthesis of Magnetite Nanoparticles in a Large pH Window with Different Bases

    Directory of Open Access Journals (Sweden)

    Maria Cristina Mascolo

    2013-11-01

    Full Text Available Magnetite nanoparticles (Fe3O4 represent the most promising materials in medical applications. To favor high-drug or enzyme loading on the nanoparticles, they are incorporated into mesoporous materials to form a hybrid support with the consequent reduction of magnetization saturation. The direct synthesis of mesoporous structures appears to be of interest. To this end, magnetite nanoparticles have been synthesized using a one pot co-precipitation reaction at room temperature in the presence of different bases, such as NaOH, KOH or (C2H54NOH. Magnetite shows characteristics of superparamagnetism at room temperature and a saturation magnetization (Ms value depending on both the crystal size and the degree of agglomeration of individual nanoparticles. Such agglomeration appears to be responsible for the formation of mesoporous structures, which are affected by the pH, the nature of alkali, the slow or fast addition of alkaline solution and the drying modality of synthesized powders.

  1. Identification of paramagnetic nitrogen centers (P1) in diamond crystallites synthesized via the sintering of detonation nanodiamonds at high pressure and temperature

    Science.gov (United States)

    Osipov, V. Yu.; Shakhov, F. M.; Efimov, N. N.; Minin, V. V.; Kidalov, S. V.; Vul', A. Ya.

    2017-06-01

    Diamond single crystals synthesized from powder detonation nanodiamonds (DNDs) by means of treatment at high pressures ( P 7 GPa) and temperatures ( T > 1300°C) have been studied by electron paramagnetic resonance (EPR). A key feature of treatment (high-pressure high-temperature (HPHT) sintering) is the use of low molecular weight alcohols in the process. The appearance of a hyperfine EPR signal structure due to "paramagnetic nitrogen" (P1 centers) is explained by the growth of submicron and micron diamond single crystals from DND nanocrystals by the oriented attachment and coalescence mechanism. Such growth and coarsening of crystals appreciably decreases the concentration of paramagnetic centers, the presence of which hinders the detection of a hyperfine structure in the EPR signal from P1 centers, in the near-surface areas of coalesced and grown together DND particles. It has been shown that the concentration of paramagnetic defects of all types decreases to 3.1 × 1018 g-1 ( 60 ppm) during HPHT treatment at T = 1650°C. This causes the successful identification of P1 centers, whose fraction is no less than 40% of the total amount of paramagnetic centers in microcrystals synthesized by HPHT sintering.

  2. Low temperature synthesis of silicon quantum dots with plasma chemistry control in dual frequency non-thermal plasmas.

    Science.gov (United States)

    Sahu, Bibhuti Bhusan; Yin, Yongyi; Han, Jeon Geon; Shiratani, Masaharu

    2016-06-21

    The advanced materials process by non-thermal plasmas with a high plasma density allows the synthesis of small-to-big sized Si quantum dots by combining low-temperature deposition with superior crystalline quality in the background of an amorphous hydrogenated silicon nitride matrix. Here, we make quantum dot thin films in a reactive mixture of ammonia/silane/hydrogen utilizing dual-frequency capacitively coupled plasmas with high atomic hydrogen and nitrogen radical densities. Systematic data analysis using different film and plasma characterization tools reveals that the quantum dots with different sizes exhibit size dependent film properties, which are sensitively dependent on plasma characteristics. These films exhibit intense photoluminescence in the visible range with violet to orange colors and with narrow to broad widths (∼0.3-0.9 eV). The observed luminescence behavior can come from the quantum confinement effect, quasi-direct band-to-band recombination, and variation of atomic hydrogen and nitrogen radicals in the film growth network. The high luminescence yields in the visible range of the spectrum and size-tunable low-temperature synthesis with plasma and radical control make these quantum dot films good candidates for light emitting applications.

  3. Cooperation between catalytic and DNA binding domains enhances thermostability and supports DNA synthesis at higher temperatures by thermostable DNA polymerases.

    Science.gov (United States)

    Pavlov, Andrey R; Pavlova, Nadejda V; Kozyavkin, Sergei A; Slesarev, Alexei I

    2012-03-13

    We have previously introduced a general kinetic approach for comparative study of processivity, thermostability, and resistance to inhibitors of DNA polymerases [Pavlov, A. R., et al. (2002) Proc. Natl. Acad. Sci. U.S.A.99, 13510-13515]. The proposed method was successfully applied to characterize hybrid DNA polymerases created by fusing catalytic DNA polymerase domains with various sequence-nonspecific DNA binding domains. Here we use the developed kinetic analysis to assess basic parameters of DNA elongation by DNA polymerases and to further study the interdomain interactions in both previously constructed and new chimeric DNA polymerases. We show that connecting helix-hairpin-helix (HhH) domains to catalytic polymerase domains can increase thermostability, not only of DNA polymerases from extremely thermophilic species but also of the enzyme from a faculatative thermophilic bacterium Bacillus stearothermophilus. We also demonstrate that addition of Topo V HhH domains extends efficient DNA synthesis by chimerical polymerases up to 105 °C by maintaining processivity of DNA synthesis at high temperatures. We found that reversible high-temperature structural transitions in DNA polymerases decrease the rates of binding of these enzymes to the templates. Furthermore, activation energies and pre-exponential factors of the Arrhenius equation suggest that the mechanism of electrostatic enhancement of diffusion-controlled association plays a minor role in binding of templates to DNA polymerases.

  4. Room temperature chemical synthesis of highly oriented PbSe nanotubes based on negative free energy of formation

    Energy Technology Data Exchange (ETDEWEB)

    Sankapal, B.R., E-mail: brsankapal@rediffmail.com [Thin Film and Nano Science Laboratory, Department of Physics, School of Physical Sciences, North Maharashtra University, Jalgaon 425 001 (MS) (India); Ladhe, R.D.; Salunkhe, D.B.; Baviskar, P.K. [Thin Film and Nano Science Laboratory, Department of Physics, School of Physical Sciences, North Maharashtra University, Jalgaon 425 001 (MS) (India); Gupta, V.; Chand, S. [Organic and Hybrid Solar Cell, Physics of Energy Harvesting Division, Dr. K.S. Krishnan Marg, National Physical Laboratory, New Delhi 110012 (India)

    2011-10-13

    Highlights: > Simple, inexpensive and room temperature chemical synthesis route. > Highly oriented PbSe nanotubes from Cd(OH){sub 2} nanowires through lead hydroxination. > The process was template free without the use of any capping agent. > Reaction kinetics was accomplished due to more negative free energy of formation. > The ion exchange mechanism due to difference in the solubility products. - Abstract: The sacrificial template free chemical synthesis of PbSe nanotubes at room temperature has been performed by lead hydroxination from cadmium hydroxide nanowires. This process was based on the ion exchange reaction to replace Cd{sup 2+} with Pb{sup 2+} ions from hydroxyl group followed by replacement of hydroxyl group with selenium ions. The reaction kinetics was accomplished due to more negative free energy of formation and thus the difference in the solubility products. The formed nanotubes were inclusive of Pb and Se with proper inter-chemical bonds with preferred orientations having diameter in tens of nanometer. These nanotubes can have future applications in electronic, optoelectronics and photovoltaic's as well.

  5. Room temperature chemical synthesis of highly oriented PbSe nanotubes based on negative free energy of formation

    International Nuclear Information System (INIS)

    Sankapal, B.R.; Ladhe, R.D.; Salunkhe, D.B.; Baviskar, P.K.; Gupta, V.; Chand, S.

    2011-01-01

    Highlights: → Simple, inexpensive and room temperature chemical synthesis route. → Highly oriented PbSe nanotubes from Cd(OH) 2 nanowires through lead hydroxination. → The process was template free without the use of any capping agent. → Reaction kinetics was accomplished due to more negative free energy of formation. → The ion exchange mechanism due to difference in the solubility products. - Abstract: The sacrificial template free chemical synthesis of PbSe nanotubes at room temperature has been performed by lead hydroxination from cadmium hydroxide nanowires. This process was based on the ion exchange reaction to replace Cd 2+ with Pb 2+ ions from hydroxyl group followed by replacement of hydroxyl group with selenium ions. The reaction kinetics was accomplished due to more negative free energy of formation and thus the difference in the solubility products. The formed nanotubes were inclusive of Pb and Se with proper inter-chemical bonds with preferred orientations having diameter in tens of nanometer. These nanotubes can have future applications in electronic, optoelectronics and photovoltaic's as well.

  6. Low temperature synthesis of carbon encapsulated Fe7S8 nanocrystals as high performance anode for lithium-ion batteries

    International Nuclear Information System (INIS)

    Liu, Boyang; Zhang, Fuhua; Wu, Qianlin; Wang, Junhua; Li, Wenge; Dong, Lihua; Yin, Yansheng

    2015-01-01

    A novel method is developed for low temperature synthesis of carbon encapsulated spherical Fe 7 S 8 nanocrystals with core–shell structure (Fe 7 S 8 @C) by the reaction of ferrocene with ammonium persulphate. The phase structure, morphology, specific surface area and composition of the nanocomposite are systematically characterized. It is found that the Fe 7 S 8 nanocrystals with a weight percent of 33.5% have a median size of 25.2 nm. The Fe 7 S 8 @C electrodes retain a reversible capacity of 815 and 539 mAh g −1 after 50 cycles at a current density of 200 and 2284 mA g −1 , respectively. The high capacity, good cycling behavior and rate capability of Fe 7 S 8 @C electrodes are attributed to the good protection and electrical conductivity of carbon shell. - Highlights: • Large scale and low temperature synthesis of Fe 7 S 8 @C with core–shell structure. • The Fe 7 S 8 @C electrodes retain a capacity of 815 mAh g −1 after 50 cycles at 200 mA g −1 . • The Fe 7 S 8 @C electrodes show good cycling behavior and rate capability

  7. Room-Temperature Synthesis of Transition Metal Clusters and Main Group Polycations from Ionic Liquids

    OpenAIRE

    Ahmed, Ejaz

    2011-01-01

    Main group polycations and transition metal clusters had traditionally been synthesized via high-temperature routes by performing reactions in melts or by CTR, at room-temperature or lower temperature by using so-called superacid solvents, and at room-temperature in benzene–GaX3 media. Considering the major problems associated with higher temperature routes (e.g. long annealing time, risk of product decomposition, and low yield) and taking into account the toxicity of benzene and liquid SO2 i...

  8. Role of Plasma Temperature and Residence Time in Stagnation Plasma Synthesis of c-BN Nanopowders

    Science.gov (United States)

    2013-01-01

    7 A plasma ion source creates the ions, which are then separated by magnetic mass separation to guide the separate beams into a deposition...generator is the soul contributor to sustaining the plasma. Figure 3.3 Plasma synthesis setup. Solid powder-form precursors are sublimated and...operation frequency gives the proper magnetic field skin depth to match the overall plasma torch diameter. The magnetic field skin depth is inversely

  9. Room temperature synthesis of glycerol carbonate catalyzed by spray dried sodium aluminate microspheres

    OpenAIRE

    Sreerangappa, Ramesh; Debecker, Damien P.; 13th European Congress on Catalysis – EuropaCat 2017

    2017-01-01

    Nanostructured NaAlO2 microspheres are produced by one-pot spray dried route, and are characterized by various physico-chemical methods. The obtained solids are composed of spherical aggregates of sodium aluminate with small crystallite size and strong surface basicity. This makes them highly active catalysts in the base-catalyzed synthesis of glycerol carbonate from glycerol and dimethyl carbonate. The catalyst does not leach and showed good reusability up to three cycles.

  10. Synthesis of Hafnium-Based Ceramic Materials for Ultra-High Temperature Aerospace Applications

    Science.gov (United States)

    Johnson, Sylvia; Feldman, Jay

    2004-01-01

    This project involved the synthesis of hafnium (Hf)-based ceramic powders and Hf-based precursor solutions that were suitable for preparation of Hf-based ceramics. The Hf-based ceramic materials of interest in this project were hafnium carbide (with nominal composition HE) and hafnium dioxide (HfO2). The materials were prepared at Georgia Institute of Technology and then supplied to research collaborators Dr. Sylvia Johnson and Dr. Jay Feldman) at NASA Ames Research Center.

  11. Branched carbon nanofiber network synthesis at room temperature using radio frequency supported microwave plasmas

    OpenAIRE

    Boskovic, BO; Stolojan, V; Zeze, DA; Forrest, RD; Silva, SRP; Haq, S

    2004-01-01

    Carbon nanofibers have been grown at room temperature using a combination of radio frequency and microwave assisted plasma-enhanced chemical vapor deposition. The nanofibers were grown, using Ni powder catalyst, onto substrates kept at room temperature by using a purposely designed water-cooled sample holder. Branched carbon nanofiber growth was obtained without using a template resulting in interconnected carbon nanofiber network formation on substrates held at room temperatur...

  12. Radiation synthesis of a water-soluble temperature sensitive polymer, activated copolymer and applications in immobilization of proteins

    International Nuclear Information System (INIS)

    Zhai Maolin; Ha Hongfei; Wu Jilan

    1993-01-01

    In this work the radiation polymerization of N-isopropylacrylamide (NIPAAM) in aqueous solutions has been carried out and a water-soluble, temperature sensitive polymer and copolymer were obtained by using γ-rays from Co-60 source at room temperature. We have gained the optimum dose and dose-rate of radiation synthesis of linear polyNIPAAM through determining conversion yield and viscosity. In order to immobilize protein (BSA) and enzyme (HRP) into this water-soluble polymer, we prepared an activated copolymer, poly(N-isopropylacrylamide-co-N-acryloxysuccinimide). The BSA and HRP has been immobilized onto the activated copolymer. The BSA (HRP)/copolymer conjugates still kept the original thermally sensitive properties of the linear polyNIPAAM. The conjugation yield of BSA to the activated copolymer decreased with increasing dose. Immobilized HRP was stable at 0 o C for a long time and has, at least, 4 days stability at room temperature. Immobilized HRP activity was lowered when the temperature was raised. This phenomenon was reversible and the immobilized HRP regained activity. The optimum pH of the immobilized HRP shifted from ca.5 upward to ca. 7. (author)

  13. Synthesis of Monodisperse CdSe QDs using Controlled Growth Temperatures

    International Nuclear Information System (INIS)

    Noor Razinah Rahmat; Akrajas Ali Umar; Muhammad Yahya; Muhamad Mat Salleh; Mohammad Hafizuddin Jumali

    2011-01-01

    The effect of growth temperatures on size of CdSe quantum dots (QDs) has been investigated. CdSe QDs were synthesized using thermolysis of organometallics precursor route using wet chemical method. The growth temperature was varied from 260-310 degree Celsius with growth period fixed at 60 s. As the growth temperature increased, the monodispersed CdSe QDs with diameter in the range 3-7 nm were obtained. Both absorption and PL spectra of the QDs revealed a strong red-shift supporting the increment size of QDs with the rise of growth temperature. (author)

  14. Room-temperature sol–gel synthesis of organic ligand-capped ZnO nanoparticles

    Energy Technology Data Exchange (ETDEWEB)

    Zobel, Mirijam, E-mail: mirijam.zobel@fau.de; Chatterjee, Haimantee [Friedrich-Alexander University Erlangen-Nürnberg (FAU), Department of Physics, Lehrstuhl für Kristallographie und Strukturphysik (Germany); Matveeva, Galina; Kolb, Ute [Johannes Gutenberg-Universität, Institut für Physikalische Chemie (Germany); Neder, Reinhard B., E-mail: reinhard.neder@fau.de [Friedrich-Alexander University Erlangen-Nürnberg (FAU), Department of Physics, Lehrstuhl für Kristallographie und Strukturphysik (Germany)

    2015-05-15

    Powders of zinc oxide nanoparticles with individual particle sizes below 10 nm in diameter are readily produced in base-induced sol–gel processes from ethanolic solutions of zinc acetate dihydrate. These particles are covered with acetate molecules and without further stabilization, they grow when stored as a powder. Here, we present three organic ligands, which reproducibly stabilize individual particle sizes <5 nm within the agglomerated powders for extended periods of time, up to months. Citric acid and 1,5-diphenyl-1,3,5-pentanetrione result in average diameters of 3 nm, whereas dimethyl-L-tartrate stabilizes 2.1 nm. X-ray diffraction and pair distribution function analysis were used to investigate the structural properties of the particles. TEM data confirm the individual particle size and crystallinity and show that the particles are agglomerated without structural coherence. Besides the introduction of these novel ligands for ZnO nanoparticles, we investigated, in particular, the influence of each synthesis step onto the final nanoparticle size in the powder. Previous studies often reported the employed synthesis parameters, but did not motivate the reasoning for their choice based on detailed experimental observations. Herein, we regard separately the steps of (i) the synthesis of the colloids, (ii) their precipitation, and (iii) the drying of the resulting gel to understand the role of the ligands therein. ZnO particles only covered with acetate grow to 5 nm during the drying process, whereas particles with any of the additional ligands retain their colloidal size of 2–3 nm. This clearly shows the efficient binding and effect of the presented ligands.

  15. Thermodynamic approach to the synthesis of silicon carbide using tetramethylsilane as the precursor at high temperature

    Science.gov (United States)

    Jeong, Seong-Min; Kim, Kyung-Hun; Yoon, Young Joon; Lee, Myung-Hyun; Seo, Won-Seon

    2012-10-01

    Tetramethylsilane (TMS) is commonly used as a precursor in the production of SiC(β) films at relatively low temperatures. However, because TMS contains much more C than Si, it is difficult to produce solid phase SiC at high temperatures. In an attempt to develop a more efficient TMS-based SiC(α) process, computational thermodynamic simulations were performed under various temperatures, working pressures and TMS/H2 ratios. The findings indicate that each solid phase has a different dependency on the H2 concentration. Consequently, a high H2 concentration results in the formation of a single, solid phase SiC region at high temperatures. Finally, TMS appears to be useful as a precursor for the high temperature production of SiC(α).

  16. Branched carbon nanofiber network synthesis at room temperature using radio frequency supported microwave plasmas

    International Nuclear Information System (INIS)

    Boskovic, Bojan O.; Stolojan, Vlad; Zeze, Dagou A.; Forrest, Roy D.; Silva, S. Ravi P.; Haq, Sajad

    2004-01-01

    Carbon nanofibers have been grown at room temperature using a combination of radio frequency and microwave assisted plasma-enhanced chemical vapor deposition. The nanofibers were grown, using Ni powder catalyst, onto substrates kept at room temperature by using a purposely designed water-cooled sample holder. Branched carbon nanofiber growth was obtained without using a template resulting in interconnected carbon nanofiber network formation on substrates held at room temperature. This method would allow room-temperature direct synthesized nanofiber networks over relatively large areas, for a range of temperature sensitive substrates, such as organic materials, plastics, and other polymers of interest for nanoelectronic two-dimensional networks, nanoelectromechanical devices, nanoactuators, and composite materials

  17. A Versatile Route for the Synthesis of Nickel Oxide Nanostructures Without Organics at Low Temperature

    Directory of Open Access Journals (Sweden)

    Shah MA

    2008-01-01

    Full Text Available AbstractNickel oxide nanoparticles and nanoflowers have been synthesized by a soft reaction of nickel powder and water without organics at 100 °C. The mechanism for the formation of nanostructures is briefly described in accordance with decomposition of metal with water giving out hydrogen. The structure, morphology, and the crystalline phase of resulting nanostructures have been characterized by various techniques. Compared with other methods, the present method is simple, fast, economical, template-free, and without organics. In addition, the approach is nontoxic without producing hazardous waste and could be expanded to provide a general and convenient strategy for the synthesis of nanostructures to other functional nanomaterials.

  18. Room temperature synthesis of glycerol carbonate catalyzed by spray dried sodium aluminate microspheres

    OpenAIRE

    Sreerangappa, Ramesh; Debecker, Damien P.

    2017-01-01

    Nanostructured NaAlO2 microspheres are produced from an aqueous solution, by a one-pot spray drying route. The obtained solids are composed of spherical aggregates of sodium aluminate with small crystallite size and strong surface basicity. This makes them highly active catalysts in the base-catalyzed synthesis of glycerol carbonate from glycerol and dimethyl carbonate. The new catalyst does not leach and is recyclable. NaAlO2 microspheres outcompete commercially available NaAlO2 as well as o...

  19. Effects of electromagnetic radiation (bright light, extremely low-frequency magnetic fields, infrared radiation) on the circadian rhythm of melatonin synthesis, rectal temperature, and heart rate.

    Science.gov (United States)

    Griefahn, Barbara; Künemund, Christa; Blaszkewicz, Meinolf; Lerchl, Alexander; Degen, Gisela H

    2002-10-01

    Electromagnetic spectra reduce melatonin production and delay the nadirs of rectal temperature and heart rate. Seven healthy men (16-22 yrs) completed 4 permuted sessions. The control session consisted of a 24-hours bedrest at infrared radiation (65 degrees C) was applied from 5 pm to 1 am. Salivary melatonin level was determined hourly, rectal temperature and heart rate were continuously recorded. Melatonin synthesis was completely suppressed by light but resumed thereafter. The nadirs of rectal temperature and heart rate were delayed. The magnetic field had no effect. Infrared radiation elevated rectal temperature and heart rate. Only bright light affected the circadian rhythms of melatonin synthesis, rectal temperature, and heart rate, however, differently thus causing a dissociation, which might enhance the adverse effects of shiftwork in the long run.

  20. Synthesis of quinoxaline 1,4-di-n-oxide derivatives on solid support using room temperature and microwave-assisted solvent-free procedures

    International Nuclear Information System (INIS)

    Gomez-Caro, Lilia C.; Sanchez-Sanchez, Mario; Bocanegra-Garcia, Virgilio; Rivera, Gildardo; Monge, Antonio

    2011-01-01

    We describe the synthesis of 12 new ethyl and methyl quinoxaline-7-carboxylate 1,4-di-N-oxide derivatives on solid supports with room temperature and microwave-assisted solvent-free procedures. Results show that solid supports have good catalytic activity in the formation of quinoxaline 1,4-di-N-oxide derivatives. We found that florisil and montmorillonite KSF and K10 could be used as new, easily available, inexpensive alternatives of catalysts. Additionally, room temperature and microwave-irradiation solvent-free synthesis was more efficient than a conventional procedure (Beirut reaction), reducing reaction time and increasing yield. (author)

  1. Synthesis of quinoxaline 1,4-di-n-oxide derivatives on solid support using room temperature and microwave-assisted solvent-free procedures

    Energy Technology Data Exchange (ETDEWEB)

    Gomez-Caro, Lilia C.; Sanchez-Sanchez, Mario; Bocanegra-Garcia, Virgilio; Rivera, Gildardo [Universidad Autonoma de Tamaulipas, Reynosa (Mexico). Dept. de Farmacia y Quimica Medicinal; Monge, Antonio [Universidad de Navarra, Pamplona (Spain). Centro de Investigacion en Farmacobiologia Aplicada. Unidad de Investigacion y Desarrollo de Medicamentos

    2011-07-01

    We describe the synthesis of 12 new ethyl and methyl quinoxaline-7-carboxylate 1,4-di-N-oxide derivatives on solid supports with room temperature and microwave-assisted solvent-free procedures. Results show that solid supports have good catalytic activity in the formation of quinoxaline 1,4-di-N-oxide derivatives. We found that florisil and montmorillonite KSF and K10 could be used as new, easily available, inexpensive alternatives of catalysts. Additionally, room temperature and microwave-irradiation solvent-free synthesis was more efficient than a conventional procedure (Beirut reaction), reducing reaction time and increasing yield. (author)

  2. One-step synthesis of multi-emission carbon nanodots for ratiometric temperature sensing

    Science.gov (United States)

    Nguyen, Vanthan; Yan, Lihe; Xu, Huanhuan; Yue, Mengmeng

    2018-01-01

    Measuring temperature with greater precision at localized small length scales or in a nonperturbative manner is a necessity in widespread applications, such as integrated photonic devices, micro/nano electronics, biology, and medical diagnostics. To this context, use of nanoscale fluorescent temperature probes is regarded as the most promising method for temperature sensing because they are noninvasive, accurate, and enable remote micro/nanoscale imaging. Here, we propose a novel ratiometric fluorescent sensor for nanothermometry using carbon nanodots (C-dots). The C-dots were synthesized by one-step method using femtosecond laser ablation and exhibit unique multi-emission property due to emissions from abundant functional groups on its surface. The as-prepared C-dots demonstrate excellent ratiometric temperature sensing under single wavelength excitation that achieves high temperature sensitivity with a 1.48% change per °C ratiometric response over wide-ranging temperature (5-85 °C) in aqueous buffer. The ratiometric sensor shows excellent reversibility and stability, holding great promise for the accurate measurement of temperature in many practical applications.

  3. Synthesis copolymer use to reduce pour point temperature of diamond crude oil

    Science.gov (United States)

    Than, Dao Viet; Chuong, Thai Hong; Tuy, Dao Quoc

    2017-09-01

    Diamond oil field is located in Block 01&02 Offshore Vietnam. Crude oil from Diamond Well Head Platform (WHP) is evacuated to FPSO via 20km 10" subsea flexible pipeline. The lowest seabed temperature in the field is 22°C, while the pour point temperature (PPT) of Diamond crude oil is very high (36°C) due to high paraffin content (25%). So studying to research a suitable Pour Point Depressant (PPD) for the crude oil is very important. The PPD must have ability to reduce pour point temperature of crude oil from 36°C to 21°C.

  4. Growth Mechanism for Low Temperature PVD Graphene Synthesis on Copper Using Amorphous Carbon

    Science.gov (United States)

    Narula, Udit; Tan, Cher Ming; Lai, Chao Sung

    2017-03-01

    Growth mechanism for synthesizing PVD based Graphene using Amorphous Carbon, catalyzed by Copper is investigated in this work. Different experiments with respect to Amorphous Carbon film thickness, annealing time and temperature are performed for the investigation. Copper film stress and its effect on hydrogen diffusion through the film grain boundaries are found to be the key factors for the growth mechanism, and supported by our Finite Element Modeling. Low temperature growth of Graphene is achieved and the proposed growth mechanism is found to remain valid at low temperatures.

  5. Bio-synthesis of triangular and hexagonal gold nanoparticles using palm oil fronds’ extracts at room temperature

    Science.gov (United States)

    Usman, Adamu Ibrahim; Aziz, Azlan Abdul; Abu Noqta, Osama

    2018-01-01

    Development of bio-reduction techniques for nanoparticles (NPs) synthesis in medical application remains a challenge to numerous researchers. This work reports a novel technique for the synthesis of triangular and hexagonal gold nanoparticles (AuNP) using palm oil fronds’ (POFs) extracts. The functional groups in the POFs’ extracts operate as a persuasive capping and reducing agent to growth AuNPs. The prepared AuNPs were characterized using UV-vis spectrophotometry, Fourier-transform infrared (FTIR) spectroscopy, dynamic light scattering, energy filtered transmission electron microscopy (EFTEM), and x-ray diffraction (XRD). The analysis of FTIR validates the coating of alkynes and phenolic composites on the AuNPs. This shows a feasible function of biomolecules for efficient stabilization of the AuNPs. EFTEM clearly show the triangular and hexagonal shapes of the prepared AuNPs. The XRD patterns display the peaks of fcc crystal structures at (111), (200), (220), (311) and (222), with average particle sizes of 66.7 and 79.02 nm for 1% and 5% POFs extracts concentrations respectively at room temperature. While at 120 °C the average particles size recorded for 1% and 5% of POFs extract concentrations were 32.17 nm and 45.66 nm respectively, and the reaction completed in less than 2 min. The prepared NPs could be potentially applied in biomedical application, due to their excellent stability and refine morphology without agglomeration.

  6. Selective recovery of silver from waste low-temperature co-fired ceramic and valorization through silver nanoparticle synthesis.

    Science.gov (United States)

    Swain, Basudev; Shin, Dongyoon; Joo, So Yeong; Ahn, Nak Kyoon; Lee, Chan Gi; Yoon, Jin-Ho

    2017-11-01

    Considering the value of silver metal and silver nanoparticles, the waste generated during manufacturing of low temperature co-fired ceramic (LTCC) were recycled through the simple yet cost effective process by chemical-metallurgy. Followed by leaching optimization, silver was selectively recovered through precipitation. The precipitated silver chloride was valorized though silver nanoparticle synthesis by a simple one-pot greener synthesis route. Through leaching-precipitation optimization, quantitative selective recovery of silver chloride was achieved, followed by homogeneous pure silver nanoparticle about 100nm size were synthesized. The reported recycling process is a simple process, versatile, easy to implement, requires minimum facilities and no specialty chemicals, through which semiconductor manufacturing industry can treat the waste generated during manufacturing of LTCC and reutilize the valorized silver nanoparticles in manufacturing in a close loop process. Our reported process can address issues like; (i) waste disposal, as well as value-added silver recovery, (ii) brings back the material to production stream and address the circular economy, and (iii) can be part of lower the futuristic carbon economy and cradle-to-cradle technology management, simultaneously. Copyright © 2017 Elsevier Ltd. All rights reserved.

  7. Flash pyrolysis at high temperature of ligno-cellulosic biomass and its components - production of synthesis gas

    International Nuclear Information System (INIS)

    Couhert, C.

    2007-11-01

    Pyrolysis is the first stage of any thermal treatment of biomass and governs the formation of synthesis gas for the production of electricity, hydrogen or liquid fuels. The objective of this work is to establish a link between the composition of a biomass and its pyrolysis gas. We study experimental flash pyrolysis and fix the conditions in which quantities of gas are maximal, while aiming at a regime without heat and mass transfer limitations (particles about 100 μm): temperature of 950 C and residence time of about 2 s. Then we try to predict gas yields of any biomass according to its composition, applicable in this situation where thermodynamic equilibrium is not reached. We show that an additivity law does not allow correlating gas yields of a biomass with fractions of cellulose, hemi-cellulose and lignin contained in this biomass. Several explanations are suggested and examined: difference of pyrolytic behaviour of the same compound according to the biomass from which it is extracted, interactions between compounds and influence of mineral matter. With the aim of industrial application, we study pyrolysis of millimetric and centimetric size particles, and make a numerical simulation of the reactions of pyrolysis gases reforming. This simulation shows that the choice of biomass affects the quantities of synthesis gas obtained. (author)

  8. Low temperature synthesis of ternary metal phosphides using plasma for asymmetric supercapacitors

    KAUST Repository

    Liang, Hanfeng; Xia, Chuan; Jiang, Qiu; Gandi, Appala; Schwingenschlö gl, Udo; Alshareef, Husam N.

    2017-01-01

    We report a versatile route for the preparation of metal phosphides using PH plasma for supercapacitor applications. The high reactivity of plasma allows rapid and low temperature conversion of hydroxides into monometallic, bimetallic, or even more

  9. Synthesis of full-density nanocrystalline tungsten carbide by reduction of tungstic oxide at room temperature

    International Nuclear Information System (INIS)

    El-Eskandarany, M.S.; Omori, M.; Ishikuro, M.; Konno, T.J.; Takada, K.; Sumiyama, K.; Hirai, T.; Suzuki, K.

    1996-01-01

    Among the hard alloys, WC alloys find wide industrial applications as tips for cutting tools and wear-resistant parts. Their intrinsic resistance to oxidation and corrosion at high temperatures also makes them desirable as a protective coating for devices at elevated temperatures. In the industrial scale of production, WC is prepared by a direct union of the elements at a temperature of 3,273 to 3,473 K. Accordingly, the high cost of preparation is a disadvantage of this process. Here, the authors report a novel technique for preparing a large amount of WC powder using a simple method. This process is based on mechanical solid-state reduction (MSSR) followed y solid-state reaction (SSR) during room-temperature ball milling (a high energy ball mill, Fritsch P6, was used at a rotation speed of 4.2 s -1 ) of a mixture of WO 3 , Mg, and C powders

  10. Nickel-catalyzed synthesis of aryl trifluoromethyl sulfides at room temperature.

    Science.gov (United States)

    Zhang, Cheng-Pan; Vicic, David A

    2012-01-11

    Inexpensive nickel-bipyridine complexes were found to be active for the trifluoromethylthiolation of aryl iodides and aryl bromides at room temperature using the convenient [NMe(4)][SCF(3)] reagent. © 2011 American Chemical Society

  11. Synthesis and characterization of L-tyrosine hydrochloride crystals submitted to high and low temperatures

    Energy Technology Data Exchange (ETDEWEB)

    Santos, C.A.A.S.; Facanha Filho, P.F.; Ribeiro, L.H.L.; Victor, F.M.S.; Abreu, D.C.; Santos, A.O. dos; Carvalho, J.O.; Soares, R.A.; Sousa, J.C.F.; Lima, R.C.; Cavaignac, A.O. [Universidade Federal do Maranhao (UFMA), MA (Brazil)

    2016-07-01

    Full text: New materials are emerging and generate advances in nonlinear optics that studies the phenomena related to changes in optical properties when occurs interaction of light with the matter. Semi organic crystals present such properties. The goal is this work is to produce semi organic single crystal of L-tyrosine hydrochloride (LTHCl) and verify their thermal stability when subjected to high and low temperatures. The single crystals of LTHCl were produced for solubilization of amino acid L-tyrosine in hydrochloric acid using slow solvent evaporation technique at a constant temperature of 25 deg C. The X-ray diffraction (XRD) and refining by the Rietveld method were used to confirm the structure of the material. The thermal stability was investigated using DSC, TGA-DTA. The LTHCl crystal belongs to the monoclinic system, with two molecules per unit cell. The refinement by the Rietveld method showed good results with Rwp= 8.49% and Rp= 6.29% with S=1.13. Thermal analysis shown an endothermic event at about 160°C, which can be associated with phase transition occurred in LTHCl crystal. It was also observed that the crystal melting point occurs at a temperature of 230°C. No water of crystallization was found in the crystal structure, which was confirmed by Raman spectroscopy and thermal analysis. From the Raman spectroscopy experiments in function of temperature, no significant changes was observe in the behavior of vibrational normal modes between temperatures of -253 and 170 deg C. Finally, a monoclinic crystal system LTHCl is stable up to 160°C at high temperatures and -253°C at low temperatures. Therefore, our investigation has proved that LTHCl crystals can be used in this range of temperature without the lost of their nonlinear optical properties. (author)

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

    Science.gov (United States)

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

    2018-01-01

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

  13. Self-assembled 3D zinc borate florets via surfactant assisted synthesis under moderate pressures: Process temperature dependent morphology study

    Science.gov (United States)

    Mahajan, Dhiraj S.; Deshpande, Tushar; Bari, Mahendra L.; Patil, Ujwal D.; Narkhede, Jitendra S.

    2018-04-01

    In the present study, we prepared zinc borates using aqueous phase synthesis under moderate pressures (MP) (ethanol as a co-solvent in the presence of a quaternary ammonium surfactant-Cetyltrimethylammonium bromide (CTAB). 3D morphologies of self-assembled zinc borate (Zn(H2O)B2O4 · 0.12 H2O, Zn3B6O12 · 3.5H2O, ZnB2O4) resembling flower-like structures were obtained by varying temperature under moderate pressure conditions. Synthesized zinc borates’ florets were morphologically characterized by Field Emission Scanning Electron Microscopy. The x-ray diffractions of borate species reveal rhombohydra, monoclinic and cubic phases of zinc borate crystals as a function of process temperature. Additionally, thermal analysis confirms excellent dehydration/degradation behavior for the zinc borate crystals synthesized at moderate pressures and elevated temperatures and could be utilized as potential flame retardant fillers in the polymer matrices.

  14. Low-temperature synthesis and characterization of helical carbon fibers by one-step chemical vapour deposition

    Science.gov (United States)

    Jin, Yongzhong; Chen, Jian; Fu, Qingshan; Li, Binghong; Zhang, Huazhi; Gong, Yong

    2015-01-01

    Helical carbon fibers (HCNFs) were synthesized by one-step chemical vapour deposition using cupric tartrate as a catalyst at temperature below 500 °C. The bound rubber of natural rubber (NR)/HCNFs were also prepared in this study. The results of thermogravimetry-differential scanning calorimetry (TG/DSC) for cupric tartrate nanoparticles show that the transformation of C4H4CuO6 → Cu reaction occurs at ∼250-310 °C. The characterization of scanning electron microscopy (SEM), transmission electron microscope (TEM), X-ray diffraction (XRD) and Raman spectrum for the synthesized products confirms that the synthesis of HCNFs is highly temperature-dependent. The straight fibers with the fiber diameter of 100-400 nm are obtained at 280 °C and HCNFs can be synthesized at higher temperature, with the coil diameter of 0.5-1 μm and fiber diameter of 100-200 nm at 380 °C, and the coil diameter of ∼100 nm and fiber diameter of ∼80 nm at 480 °C. The maximum of the bound-rubber content (37%) can be obtained with the addition of 100 wt.% HCNFs in NR, which indicates that the coiled configuration of HCNFs makes a noticeable contribution to the reinforcement of NR/CB system.

  15. Seed-free synthesis of 1D silver nanowires ink using clove oil (Syzygium Aromaticum) at room temperature.

    Science.gov (United States)

    Jeevika, Alagan; Ravi Shankaran, Dhesingh

    2015-11-15

    Silver nanowires (AgNWs) have been demonstrated to be a promising next generation conducting material and an alternative to the traditional electrode (ITO) because of its high conductivity, transparency and stability. Generally, AgNWs are synthesized by chemical method (mainly polyol reduction method) at high temperature in the presence of exotic seeds. The present work aims at the green approach for preparation and characterization of 1D AgNWs ink using clove oil (Syzygium Aromaticum) at room temperature. AgNWs was prepared by green synthesis using clove oil as reducing as well as capping agent at room temperature. The obtained ink was purified, filtered and redissolved in methanol. The prepared AgNWs showed an absorption peaks at 350 and 387nm in the UV-vis spectrum due to transverse SPR mode of silver. From the HR-TEM analysis, it was observed that the AgNWs possess an average diameter and length of ∼39±0.01nm and ∼3μm, respectively. The obtained AgNWs are crystalline in nature and are arranged in a perfect crystal lattice orientation, which was confirmed from the selected area electron diffraction studies. Moreover, the X-ray diffraction analysis confirms the face centered cubic structure. The AgNWs coated glass substrate shows an electrical conductivity of ∼0.48×10(6)S/m. Copyright © 2015 Elsevier Inc. All rights reserved.

  16. Low-temperature solid-state synthesis and optical properties of ZnO/CdS nanocomposites

    International Nuclear Information System (INIS)

    Liu, Jinsong; Zhu, Kongjun; Sheng, Beibei; Li, Ziquan; Tai, Guoan; Qiu, Jinhao; Wang, Jing; Chen, Jiankang; You, Yuncheng; Gu, Qilin; Liu, Pengcheng

    2015-01-01

    Highlights: • Using a low-temperature solid-state method, ZnO/CdS nanocomposites were obtained • Grain growth kinetics of cubic CdS and hexagonal ZnO phase was described. • Sufficient grinding and heating treatment was a key for formation of composites. • Optical properties could be easily manipulated by reaction temperature and time. - Abstract: A simple low-temperature solid-state reaction in the presence of the surfactant PEG400 was developed to obtain ZnO/CdS nanocomposites. The effects of synthesis temperature and reaction time on crystal structure and optical properties of the nanocomposites were investigated by several technologies. X-ray diffraction (XRD) and high resolution transmission electron microscope (HRTEM) characterizations showed that the products consisted of the nanoparticles, and the grain growth kinetics of the cubic CdS and the hexagonal ZnO phase in the nanocomposites was described. The mechanism analysis suggested that sufficient grinding and heating treatment was a key to form the ZnO/CdS nanocomposites, and the surfactant PEG400 was proved not to involve the reaction and prevent the nanoparticles from aggregating to larger in whole grinding and heat-treatment process. Ultraviolet–visible (UV–vis) spectra revealed that the band gaps of the nanocomposites could be tuned by the reaction temperature and reaction time. Photoluminescence (PL) spectra showed that the changing position and the intensity of the emission peaks resulted from the rate of electron transfer and recombination probability under the different conditions

  17. Application of self-propagation high-temperature synthesis for immobilization of hard radioactive wastes in ceramet materials

    International Nuclear Information System (INIS)

    Ilyin, E.; Pashkeev, I.; Senin, A.; Gerasimova, N.

    2001-01-01

    The possibility of self-propagating high-temperature synthesis (SPHTS) application for an immobilization of solid high level wastes (HLW) in cermet materials is considered. The schemes of multilayer cermet blocks formation are offered. Such blocks consist of a ceramet core with immobilized HLW and a protective cover - ceramet without HLW. The influence of the base components form (pure Ti and Si, ferrotitanium and ferrosilicon), metallic components (Ni, Cu, Cr, Fe, ferrochromium) and nonmetallic components (SiO 2 , Al 2 O 3 , TiO 2 ) on burning rate and cover ceramet structure is investigated in compositions on a basis of Ti+B, Ti+Si, Ti+C systems. Model samples of multilayer cermet blocks are manufactured using of HLW simulators. (authors)

  18. Lanthanide ions doped Y2Sn2O7 nano-particles: low temperature synthesis and photoluminescence study

    International Nuclear Information System (INIS)

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

    2008-01-01

    During the past decade, pyrochlore-type oxides (A 2 B 2 O 7 ) have emerged as important host matrices for lanthanide doped luminescent materials due to their higher thermal stability. Up to now, conventional solid-state reaction is the most commonly used synthetic method for preparation, of rare-earth pyrochlore oxides. This synthesis route employs a solid-state reaction of metal-oxide with appropriate rare-earth oxides at high temperature (>1200 deg C) for a long time (several days). However, in present work, Y 2 Sn 2 O 7 nanoparticles co-doped with lanthanide ions Tb 3+ and Ce 3+ were prepared based on the urea hydrolysis of Y 3+ , Sn 4+ , and Ln 3+ in ethylene glycol medium at 150 deg C followed by heating at 500, 700 and 900 deg C

  19. One-pot low-temperature green synthesis of magnetic graphene nanocomposite for the selective reduction of nitrobenzene

    Science.gov (United States)

    Haridas, Vijayasree; Sugunan, Sankaran; Narayanan, Binitha N.

    2018-06-01

    In the present study, a green one-pot low-temperature method is adopted for the synthesis of a novel magnetic graphene nanocomposite catalyst. Graphene preparation is performed without employing any oxidizing agents or corrosive chemicals, under mild sonication in isopropyl alcohol - water mixture. Monolayered nanoplatelets of graphene are obtained in the green solvent mixture and the composite material is found to be ferromagnetic in nature, obvious from the vibrating sample magnetometric measurements. Fe in the nanocomposite exists in two different forms i.e., α-Fe2O3 and α-FeOOH, as evident from the material characterization results. The graphene nanocomposite is found to be highly efficient in the selective reduction of nitrobenzene to aniline under solvent free reaction conditions and magnetic separation of this fine nanomaterial from the reaction mixture is successfully carried out. The catalyst is efficiently reusable till five repeated cycles.

  20. Optimization of self-propagating high-temperature synthesis using a halogen fluoride as an igniter for reagents

    Science.gov (United States)

    Gaidar, S. M.; Karelina, M. Yu.; Zhigarev, V. D.

    2016-12-01

    The minimum quantity of the high-activity chemical reagent (HACR) that is required for the initiation of self-propagating high-temperature synthesis (SHS) is determined. The experimental results show that 1-1.3 mg ClF3 (gravity flow from a dosing device), BrF3 on the end of a filling knife, or a few ClF2 + SbF6 - crystals are sufficient for the initiation of titanium-boron or titanium-carbon high-energy powder charge compositions. Since the quantity of HACR required for SHS initiation is very small, the chemical method of initiation can be used for the development of a mobile ignition device for estimating the ignition of various SHS charge compositions under laboratory conditions and for application in standard reactors.

  1. Controllable synthesis of spindle-like ZnO nanostructures by a simple low-temperature aqueous solution route

    International Nuclear Information System (INIS)

    Lu Hongxia; Zhao Yunlong; Yu Xiujun; Chen Deliang; Zhang Liwei; Xu Hongliang; Yang Daoyuan; Wang Hailong; Zhang Rui

    2011-01-01

    Spindle-like ZnO nanostructures were successfully synthesized through direct precipitation of zinc acetate aqueous solution at 60 deg. C. Phase structure, morphology and microstructure of the products were investigated by X-ray diffraction, TG-DTA, FTIR and field emission scanning electron microscopy (FESEM). Result showed that hexagonal wurtzite structure ZnO nanostructures with about 100 nm in diameter and 100-200 nm in length were obtained. HMTA acted as a soft template in the process and played an important role in the formation of spindle-like ZnO nanostructures. Meanwhile, different morphologies were also obtained by altering synthetic temperature, additional agents and the ratios of Zn 2+ /OH - . Possible mechanism for the variations of morphology with synthesis parameters was also discussed in this paper.

  2. Effect of pretreatment temperature on catalytic performance of the catalysts derived from cobalt carbonyl cluster in Fischer-Tropsch Synthesis

    Directory of Open Access Journals (Sweden)

    Byambasuren O

    2017-02-01

    Full Text Available The monometallic cobalt-based catalysts were prepared by pretreating the catalysts derived from carbonyl cluster precursor (CO6Co2CC(COOH2 supported on γ-Al2O3 with hydrogen at 180, 220, and 260°C respectively. The temperature effect of the pretreatments on the structure evolution of cluster precursors and the catalytic performance of the Fischer-Tropsch (F-T synthesis was investigated. The pretreated catalyst at 220°C with unique phase structure exhibited best catalytic activity and selectivity among three pretreated catalysts. Moreover, the catalysts exhibited high dispersion due to the formation of hydrogen bonds between the cluster precursor and γ-Al2O3 support.

  3. Room temperature metathetic synthesis and characterization of α-hopeite, Zn3(PO4)2.4H2O

    International Nuclear Information System (INIS)

    Parhi, Purnendu; Manivannan, V.; Kohli, Sandeep; McCurdy, Patrick

    2008-01-01

    The synthesis of crystalline zinc phosphates (α-hopeite phase) through the metathetic pathway has been investigated. The reaction has been carried out by room-temperature grinding. High lattice energy of the by-product NaCl has driven the reaction in the forward direction, and as a result, stable phosphate phases have been synthesized. Reaction of a different phosphorus source (like Na 3 PO 4 , Na 2 HPO 4 , NaH 2 PO 4 , and K 2 HPO 4 ) with ZnCl 2 has been attempted. The structural, vibrational, thermal, optical, and chemical properties of synthesized powders are determined by powder X-ray diffraction (XRD), scanning electron microscope (SEM), thermogravimetric analysis (TGA), X-ray photoelectron spectroscopy (XPS), Fourier transform infrared spectroscopy (FTIR) and diffused reflectance spectra (DR) in the UV-vis range. The direct band gap of the title compound was determined to be 3.6 ± 0.2 eV

  4. Nanoparticles of Sr(OH)2: synthesis in homogeneous phase at low temperature and application for cultural heritage artefacts

    International Nuclear Information System (INIS)

    Ciliberto, E.; Condorelli, G.G.; La Delfa, S.; Viscuso, E.

    2008-01-01

    This paper concerns the synthesis and the characterization of nanometer particles of Sr(OH) 2 , a moderately high water soluble hydroxide (Ksp=3.2 x 10 -4 at 25 C). The reported process yields strontium hydroxide nanoparticles starting from low cost raw materials in aqueous medium (homogeneous phase) at low temperature (below 100 C) by chemical precipitation from salt solutions, involving very simple operational steps and avoiding the use of organic solvents. Observations by X-ray diffraction (XRD), scanning electron microscopy (SEM), electron dispersive X-Ray (EDX) and Fourier transform infrared spectroscopy (FTIR) indicate that the particles are well-crystallized and have nanometer dimensions (∝30 nm in diameter). Moreover, experimental evidence shows the potential use of this material for the protection and the consolidation of wall paintings (frescoes), paper, stone, wood and other artistic artefacts. (orig.)

  5. Synthesis and studies of Y-Ba-Cu-O high temperature superconductor prepared by sol-gel method

    International Nuclear Information System (INIS)

    Grigoryan, S.G.; Manukyan, A.L.; Hayrapetyan, A.G.; Arzumanyan, A.M.; Rashidyan, L.H.; Mkrtichyan, N.Y.; Mkrtchyan, A.A.; Kurginyan, K.A.; Trozyan, A.H.; Vardanyan, R.S.

    2004-01-01

    The method of preparation of Y-Ba-Cu-O high temperature superconducting materials by sol-gel processing technique both for powders and thin films are described. All these methods are based on using yttrium alkoxides as precursors, which are not ready available reagents, besides the majority of these methods use copper alkoxides, which show low solubility in organic solvents, moreover they are very sensitive to hydrolysis in air. The new method of preparation of Y-Ba-Cu-O ceramic materials by sol-gel processing technique based on new and convenient precursors stable in air, having high compatibility with each other is offered. Basic scientific and technological issues related to the synthesis of bulk materials, their structure and electrical conductivity are discussed

  6. Nanoparticles of Sr(OH){sub 2}: synthesis in homogeneous phase at low temperature and application for cultural heritage artefacts

    Energy Technology Data Exchange (ETDEWEB)

    Ciliberto, E.; Condorelli, G.G.; La Delfa, S.; Viscuso, E. [Universita di Catania, Dipartimento di Scienze Chimiche, Catania (Italy)

    2008-07-15

    This paper concerns the synthesis and the characterization of nanometer particles of Sr(OH){sub 2}, a moderately high water soluble hydroxide (Ksp=3.2 x 10{sup -4} at 25 C). The reported process yields strontium hydroxide nanoparticles starting from low cost raw materials in aqueous medium (homogeneous phase) at low temperature (below 100 C) by chemical precipitation from salt solutions, involving very simple operational steps and avoiding the use of organic solvents. Observations by X-ray diffraction (XRD), scanning electron microscopy (SEM), electron dispersive X-Ray (EDX) and Fourier transform infrared spectroscopy (FTIR) indicate that the particles are well-crystallized and have nanometer dimensions ({proportional_to}30 nm in diameter). Moreover, experimental evidence shows the potential use of this material for the protection and the consolidation of wall paintings (frescoes), paper, stone, wood and other artistic artefacts. (orig.)

  7. Origin of low temperature deactivation of Ni5Ga3 nanoparticles as catalyst for methanol synthesis

    DEFF Research Database (Denmark)

    Gardini, Diego; Sharafutdinov, Irek; Damsgaard, Christian Danvad

    that the highest methanol yield is obtained with a Ni5Ga3 alloy exposed to a 25% CO2 – 75% H2 reaction mixture at 210 °C [2]. Under these experimental conditions, the catalyst is found to lose 35% of its activity after 20 hours of continuous testing at both 1 and 5 Bars. Although in situ XRD and EXAFS studies [3......In an effort to find alternative energy sources capable to compete with fossil fuels, methanol synthesis could represent a realistic solution to store “green” hydrogen produced from electrolysis or photo-induced water splitting. Recently, density functional theory (DFT) calculations [1] proposed Ni......-Ga alloys as active catalysts for methanol production from syngas mixtures and Ni-Ga nanoparticles supported on highly porous silica have been prepared using an incipient wetness impregnation technique from a solution of nickel and gallium nitrates [2]. Tests conducted in a fixed-bed reactor showed...

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

    Energy Technology Data Exchange (ETDEWEB)

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

    2015-05-01

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

  9. Synthesis and characterization of novel electrolyte materials for intermediate temperature solid oxide fuel cells

    International Nuclear Information System (INIS)

    Chaubey, Nityanand; Chattopadhyaya, M.C.; Wani, B.N.; Bharadwaj, S.R.

    2008-01-01

    The high operating temperature of SOFCs using zirconia based electrolyte have several restrictions on materials used as interconnect and sealing and also requires use of expensive ceramics. Lowering the operating temperature of SOFCs to 600-800 deg C will enable to use cheaper materials and reduce the cost of fabrication while keeping the high power density. Lanthanide gallates are considered to be very promising solid electrolytes for intermediate temperature (600-800 deg C) solid oxide fuel cells (IT-SOFCs) due to their high ionic conductivity at lower temperatures. Phase purity of this material is a concern for the researchers for a long time. These materials are prepared at very high temperature (∼1400 deg C), since it is known that at around 1100 deg C, solubilities of Sr and Mg in LaGaO 3 were close to zero. Hence in the present work perovskite oxides of Ln 1-x Sr x Ga 1-y Mg y O 3-δ (Ln= Sm, Gd and x = 0.10, y=0.20) have been prepared by different methods i.e. solid state reaction, gel combustion and co-precipitation methods

  10. Synthesis and Self-Assembly of Block Copolymers Containing Temperature Sensitive and Degradable Chain Segments.

    Science.gov (United States)

    Gong, Hong-Liang; Lei, Lei; Shi, Shu-Xian; Xia, Yu-Zheng; Chen, Xiao-Nong

    2018-05-01

    In this work, polylactide-b-poly(N-isopropylacrylamide) were synthesized by the combination of controlled ring-opening polymerization and reversible addition fragmentation chain transfer polymerization. These block copolymers with molecular weight range from 7,900 to 12,000 g/mol and narrow polydispersity (≤1.19) can self-assemble into micelles (polylactide core, poly(N-isopropylacrylamide) shell) in water at certain temperature range, which have been evidenced by laser particle size analyzer proton nuclear magnetic resonance and transmission electron microscopy. Such micelles exhibit obvious thermo-responsive properties: (1) Poly(N-isopropylacrylamide) blocks collapse on the polylactide core as system temperature increase, leading to reduce of micelle size. (2) Micelles with short poly(N-isopropylacrylamide) blocks tend to aggregate together when temperature increased, which is resulted from the reduction of the system hydrophilicity and the decreased repulsive force between micelles.

  11. Supercritical temperature synthesis of fluorine-doped VO2(M) nanoparticle with improved thermochromic property

    Science.gov (United States)

    Riapanitra, Anung; Asakura, Yusuke; Cao, Wenbin; Noda, Yasuto; Yin, Shu

    2018-06-01

    Fluorine-doped VO2(M) nanoparticles have been successfully synthesized using the hydrothermal method at a supercritical temperature of 490 °C. The pristine VO2(M) has the critical phase transformation temperature of 64 °C. The morphology and homogeneity of the monoclinic structure VO2(M) were adopted by the fluorine-doped system. The obtained particle size of the samples is smaller at the higher concentration of anion doping. The best reduction of critical temperature was achieved by fluorine doping of 0.13% up to 48 °C. The thin films of the fluorine-doped VO2(M) showed pronounced thermochromic property and therefore are suitable for smart window applications.

  12. Low Temperature Synthesis, Chemical and Electrochemical Characterization of LiNi(x)Co(1-x)O2 (0 less than x less than 1)

    Science.gov (United States)

    Nanjundaswamy, K. S.; Standlee, D.; Kelly, C. O.; Whiteley, R. V., Jr.

    1997-01-01

    A new method of synthesis for the solid solution cathode materials LiNi(x)Co(1-x)O2 (0 less than x less than 1) involving enhanced reactions at temperatures less than or equal to 700 deg. C, between metal oxy-hydroxide precursors MOOH (M = Ni, Co) and Li-salts (Li2CO3, LiOH, and LiNO3) has been investigated. The effects of synthesis conditions and sources of Li, on phase purity, microstructure, and theoretical electrochemical capacity (total M(3+) content) are characterized by powder X-ray diffraction analysis, scanning electron microscopy, chemical analysis and room temperature magnetic susceptibility. An attempt has been made to correlate the electrochemical properties with the synthesis conditions and microstructure.

  13. Synthesis of high-temperature viscosity stabilizer used in drilling fluid

    Science.gov (United States)

    Zhang, Yanna; Luo, Huaidong; Shi, Libao; Huang, Hongjun

    2018-02-01

    Abstract For a well performance drilling fluid, when it operates in deep wells under high temperature, the most important property required is the thermal stability. The drilling fluid properties under high temperature can be controlled by proper selection of viscosity stabilizer, which can capture oxygen to protect polymer agent in the drilling fluid. In this paper a viscosity stabilizer PB-854 is described, which was synthesized by 4-phenoxybutyl bromide, paraformaldehyde, and phloroglucinol using etherification method and condensation reaction. We studied the effect of catalyst dosage, temperature, time, and stirring rate on the synthetic yield. Under this condition: molar ratio of 2-tert-Butylphenol, paraformaldehyde and phloroglucinol of 2:1:2.5, reacting temperature of 100 °C, stirring rate of 100 r min-1, and mass content of catalyst of 15 %, char yield of 5-bromine-3-tert-butyl salicylaldehyde reached 86 %. Under this condition: molar ratio of 5-bromine-3-tert-butyl salicylaldehyde and phloroglucinol of 4, reacting temperature of 60 °C, reacting time of 30 min, volume content of sulphuric acid of 80 %, char yield of the target product viscosity stabilizer PB-854 is 86%. Finally, in this paper, infrared spectroscopy is adopted to analyse the structure of the synthetic product PB-854.The improvement in the stability of drilling fluid was further shown after adding the viscosity stabilizer in the common polymer drilling fluid under high temperature conditions of 120 °C ˜ 180 °C. The results show significant change in terms of fluid stability in the presence of this new stabilizer as it provides better stability.

  14. Low-temperature sol-gel synthesis of NaZr2P3O12

    International Nuclear Information System (INIS)

    Agrawal, D.K.; Adair, J.H.

    1990-01-01

    The NZP family of new low-expansion materials has attracted wide interest for its potential in advanced technological applications. NaZr 2 P 3 O 12 , which is the parent composition of this family, has been synthesized by the solution sol-gel method using special precursor solutions, which led to its formation (although poorly crystalline) at temperatures as low as 120 degrees C. The lowest temperature of formation of a single phase of NaZr 2 P 3 O 12 with a high degree of crystallinity was found to be 600 degrees C

  15. Synthesis of polystyrene with high melting temperature through BDE/CuCl catalyzed polymerization

    Institute of Scientific and Technical Information of China (English)

    WAN; Xiaolong

    2001-01-01

    Lecomte, P., Drapier, I., Dubios, P. et al., Controlled radical polymerization of methyl methacrylate in the presence of palladium acetate, triphenyl phosphine, and carbon tetrachloride, Macromolecules, 1997, 30: 7631.[12]Kotani, Y., Kamigaito, Y., Sawamoto, M., Re(V)-mediated living radical polymerization of styrene: ReO2I(PPh3)2/RI initiating system, Macromolecules, 1999, 32: 2420.[13]Makino, T., Tokunaga, E., Hogen-Esch, T. E., Controlled atom transfer radical polymerizations of methyl methacrylate under micellar conditions, Polym. Prep., 1998, 39(1): 288.[14]Gaynor, S. G., Qiu, J., Matyjaszewski, K., Controlled/"living" radical polymerization applied to water-borne system, Macromolecule, 1998, 31: 5951.[15]Qiu, J., Gaynor, S. G., Matyjaszewski, K., Controlled/"living" radical polymerization of n-butyl methacrylate by reverse atom transfer radical polymerization, Macromolecules, 1999, 32: 2872.[16]Shipp, D. A., McMurtry, G. P., Gaynor, S. G. et al., Water-borne block copolymer synthesis and a simple and effective one-pot synthesis of acrylate-methacrylate block copolymers by atom transfer radical polymerization, Polym. Prep., 1999, 40(2): 448.[17]Nishikawa, T., Kamigaito, M., Sawamoto, M., Living radical polymerization in water and alcohols: suspension polymerization of methyl methacrylate with RuCl2(PPh3)3 complex, Macromolecules, 1999, 32: 2204.[18]Wan, X. L., Ying, S. K., "Living" radical emulsion polymerization of styrene under Cu0/Bpy/CCl4 and CuCl2/Bpy/AIBN system, Chinese J. Polym. Sci., 2000, (1): 27.[19]Wan, X. L., Ying, S. K., Controlled radical polymerization catalyzed by Cu/BDE complex in water medium, 1. Polymerization of styrene and synthesis of poly(St-b-MMA), J. Appl. Polym. Sci., 2000, 75(1): 802.[20]Wan, X. L., Ying, S. K., Synthesis of block copolymers by emulsion "living"/controlled radical polymerization of vinyl monomers in sequence, Polym. Prep., 1999, 40: 1055.[21]Keller, R. N., Wycoff, H. D., The synthesis

  16. Low temperature molten salt synthesis of Y(sub2)Sn(sub2)O(sub7) anode material for lithium ion batteries

    CSIR Research Space (South Africa)

    Nithyadharseni, P

    2015-10-01

    Full Text Available Acta 182 (2015) 1060–1069 Low temperature molten salt synthesis of Y2Sn2O7 anode material for lithium ion batteries P. Nithyadharsenia,b, M.V. Reddya,c,*, Kenneth I. Ozoemenab,d, R. Geetha Balakrishnae, B.V.R. Chowdaria a Advanced Batteries...

  17. A facile synthesis of substituted 2-alkylquinolines through [3+3] annulation between 3-ethoxycyclobutanones and aromatic amines at room temperature.

    Science.gov (United States)

    Shan, Gang; Sun, Xiuyun; Xia, Qian; Rao, Yu

    2011-11-04

    An efficient single-step approach toward the synthesis of 2-alkylquinolines is described. Through a Lewis acid mediated [3+3] annulation reaction between 3-ethoxycyclobutanones and aromatic amines, a variety of multisubstituted 2-alkylquinoline derivatives were prepared regioselectively at room temperature. © 2011 American Chemical Society

  18. FeCl3/Egg shell: An Effective Catalytic System for the Synthesis of 2,3-Dihydroquinazolin-4(1H)-ones at Room Temperature

    OpenAIRE

    Zakaria Benzekri; Houda Serrar; Said Boukhris; Abdelaziz Souizi

    2017-01-01

    The FeCl3/eggshell has been a new and efficient catalyst for the rapid and simple synthesis of 2,3-dihydroquinazolin-4-ones in ethanol at room temperature. The present method has advantages of low cost, mild reaction conditions, simple workup process, better recovery and reusability of catalyst, excellent yields and environmentally friendly procedure.

  19. Low temperature synthesis of nanosized Mn1–xZnxFe2O4 ferrites ...

    Indian Academy of Sciences (India)

    There is a systematic decrease in the particle size, Curie temperature and magnetization with the increase in the Zn2+ ion doping, measured using magneto thermal gravimetric analysis (MTGA) and vibrating sample magnetometer (VSM), respectively. The lattice constant is found to be constantly decreasing till = 0.6 and ...

  20. Green synthesis of Ni-Nb oxide catalysts for low-temperature oxidative dehydrogenation of ethane.

    Science.gov (United States)

    Zhu, Haibo; Rosenfeld, Devon C; Anjum, Dalaver H; Caps, Valérie; Basset, Jean-Marie

    2015-04-13

    The straightforward solid-state grinding of a mixture of Ni nitrate and Nb oxalate crystals led to, after mild calcination (Tethane to ethylene at a relatively low temperature (Tethane. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  1. Seeding technique for lowering temperature during synthesis of α-alumina

    Directory of Open Access Journals (Sweden)

    Yoshio Kobayashi

    2015-03-01

    Full Text Available This paper reports a method for producing α-Al2O3 at low temperature using a seeding technique. A white product obtained by hydrolyzing aluminum isopropoxide in water at 80 °C was peptized using acetic acid at 80 °C, which transformed the white product to a transparent alumina sol. α-Al2O3 particles were added to the alumina sol as seed material; the sol containing α-Al2O3 particles was then transformed to an α-Al2O3-seeded alumina gel by drying the sol at room temperature. The non-seeded alumina gel remained boehmite after annealing at 300 °C and crystallized into γ-Al2O3 and α-Al2O3 at temperatures between 300 and 500 °C and between 900 and 1100 °C, respectively. The α-Al2O3 seeding promoted crystallization of the alumina gel into α-Al2O3. The promotion of crystallization was significant with an increase in α-Al2O3 particle content by weight in the final seeded alumina gel. With an α-Al2O3 particle content of 5%, the seeded alumina gel was partially crystallized into α-Al2O3 by annealing at a temperature as low as 900 °C.

  2. Room temperature vortex fluidic synthesis of monodispersed amorphous proto-vaterite.

    Science.gov (United States)

    Peng, Wenhong; Chen, Xianjue; Zhu, Shenmin; Guo, Cuiping; Raston, Colin L

    2014-10-11

    Monodispersed particles of amorphous calcium carbonate (ACC) 90 to 200 nm in diameter are accessible at room temperature in ethylene glycol and water using a vortex fluidic device (VFD). The ACC material is stable for at least two weeks under ambient conditions.

  3. Aqueous synthesis of porous platinum nanotubes at room temperature and their intrinsic peroxidase-like activity.

    Science.gov (United States)

    Cai, Kai; Lv, Zhicheng; Chen, Kun; Huang, Liang; Wang, Jing; Shao, Feng; Wang, Yanjun; Han, Heyou

    2013-07-11

    Platinum nanotubes (PtNTs) exhibiting high porosity were constructed by sacrificing the exterior of tellurium nanowires (TeNWs) and disintegrating the inner part spontaneously in aqueous solution at room temperature, in which the Kirkendall effect may play an important role. The present PtNTs exhibited intrinsic peroxidase-like activity in the presence of H2O2.

  4. GREEN SYNTHESIS OF SILVER AND PALLADIUM NANOPARTICLES AT ROOM TEMPERATURE USING COFFEE AND TEA EXTRACT

    Science.gov (United States)

    An extremely simple green approach that generates bulk quantities of nanocrystals of noble metals such as silver (Ag) and palladium (Pd) using coffee and tea extract at room temperature is described. The single-pot method uses no surfactant, capping agent, and/or template. The ob...

  5. Novel method of room temperature ionic liquid assisted Fe3O4 nanocubes and nanoflakes synthesis

    International Nuclear Information System (INIS)

    Ramalakshmi, M.; Shakkthivel, P.; Sundrarajan, M.; Chen, S.M.

    2013-01-01

    Graphical abstract: - Highlights: • First time [Bmim][TfO] IL is used for the Fe 3 O 4 nanoparticle synthesis. • Novel method tunes Fe 3 O 4 nanocubes and nanoflakes forms influenced by the base and IL. • Fe 3 O 4 oxidized topotactically into γ-Fe 2 O 3 nanoparticles by annealing and base. • Uniform morphology with average size of 33 nm negligible superstructure are formed. • Ms values are characterized by thin layer of γ-Fe 2 O 3 on the nanoparticle surface. - Abstract: For the first time, the nanomagnetite superparamagnetic particles are successfully synthesized by precipitation method using 1-n-butyl-3-methylimidazolium trifluoromethane sulfonate [Bmim][TfO] ionic liquid medium/surfactant. The obtained Fe 3 O 4 particles are nanocubes and nanoflakes and this formation is influenced by the base concentration and anisotropic circumstances produced by the ionic liquid and their size varies from 20 nm to 150 × 300 nm (width × length). The synthesized magnetite nanoparticles are characterized by X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FT-IR), Raman spectroscopy, Field emission scanning electron microscopy (FE-SEM), Transmission electron microscopy (TEM) and Vibrating sample magnetometer (VSM) studies. The results show that the core of the Fe 3 O 4 nanoparticles is surrounded by a thin layer of γ-Fe 2 O 3 by topotactical partial oxidation, which is remarkably proceed with the subsequent calcination. The magnetite nanocubes have high saturation magnetization value and exhibit superparamagnetic hysteresis loop

  6. One pot synthesis of copper nanoparticles at room temperature and its catalytic activity

    Directory of Open Access Journals (Sweden)

    Nikhil V. Suramwar

    2016-11-01

    Full Text Available A facile reduction approach with sodium borohydride as a reducing agent and starch as a stabilizing agent leads to monodispersed Cu nanoparticles in aqueous medium at an ambient condition. The synthesized nanoparticles are highly pure with no traces of CuO found on surface. They are uniform in size in the range of 40–80 nm. The Cu nanoparticles have a FCC structure as characterized by powder X-ray diffraction (XRD. Transmission electron microscopy (TEM images show that they are arranged in a regular array which is separated by starch thin layer which controls the growth as well as stabilizes the Cu nanoparticles from air oxidation. The catalytic activity of prepared Cu nanomaterial was tested in Ullman reaction for the synthesis of biphenyl from iodobenzene. We have shown in this paper that the size as well as exposed surface area of the copper nanoparticles is responsible for the increase in yield of biphenyl up to 92%. This is higher compare to the 40% yield with the normal size copper powder under the same reaction condition.

  7. Synthesis of high-temperature superconducting oxides and chemical alloying in Cu-O planes

    International Nuclear Information System (INIS)

    Tarascon, J.M.; Barboux, P.; Bagley, B.G.; Green, L.H.; Mckinnon, W.R.; Hull, G.W.

    1988-01-01

    Some methods for synthesis permitting to fabricate dense superconducting ceramics are considered. The Zole-Hell method is the most perspective one among them. Effect of oxygen content in a sample and copper substitution for nickel and zinc on structural, transition and superconducting properties of samples of the La-Sr-Cu-O(1) and Y-Ba-Cu-O(2) systems is studied. Copper substitution is established to suppress superconductivity in system 1 and to decrease T c in system 2, and this effect doesn't depend on the fact whether the substituting 3d-metal is magnetic (nickel) or diamagnetic (zinc). Detailed study of YBa 2 Cu 3 O 7-y properties as a function of oxygen content has shown that superconductivty in this composition can be suppressed as a result of oxygen removal and it can be reduced with its interoduction. The possibility to prepare nonalloyed La 2 CuO 4 in superconducting state as a result of plasma treatment comprises a scientific interest. 27 refs.; 5 figs.; 1 tab

  8. Hydrophilic Graphene Preparation from Gallic Acid Modified Graphene Oxide in Magnesium Self-Propagating High Temperature Synthesis Process

    Science.gov (United States)

    Cao, Lei; Li, Zhenhuan; Su, Kunmei; Cheng, Bowen

    2016-10-01

    Hydrophilic graphene sheets were synthesized from a mixture of magnesium and gallic acid (GA) modified graphene oxide (GO) in a self-propagating high-temperature synthesis (SHS) process, and hydrophilic graphene sheets displayed the higher C/O ratio (16.36), outstanding conductivity (~88900 S/m) and excellent water-solubility. GO sheets were connected together by GA, and GA was captured to darn GO structure defects through the formation of hydrogen bonds and ester bonds. In SHS process, the most oxygen ions of GO reacted with magnesium to prevent the escape of carbon dioxide and carbon monoxide to from the structure defects associated with vacancies, and GA could take place the high-temperature carbonization, during which a large-area graphene sheets formed with a part of the structure defects being repaired. When only GO was reduced by magnesium in SHS process, and the reduced GO (rGO) exhibited the smaller sheets, the lower C/O ratio (15.26), the weaker conductivity (4200 S/m) and the poor water-solubility because rGO inevitably left behind carbon vacancies and topological defects. Therefore, the larger sheet, less edge defects and free structure defects associated with vacancies play a key role for graphene sheets good dispersion in water.

  9. Synthesis and Characterization of Si Oxide Coated Nano Ceria by Hydrolysis, and Hydrothermal Treatment at Low Temperature

    Directory of Open Access Journals (Sweden)

    Kong M.

    2017-06-01

    Full Text Available The purpose of this work was to the application of Si oxide coatings. This study deals with the preparation of ceria (CeO2 nanoparticles coating with SiO2 by water glass and hydrolysis reaction. First, the low temperature hydro-reactions were carried out at 30~100°C. Second, Silicon oxide-coated Nano compounds were obtained by the catalyzing synthesis. CeO2 Nano-powders have been successfully synthesized by means of the hydrothermal method, in a low temperature range of 100~200°C. In order to investigate the structure and morphology of the Nano-powders, scanning electron microscopy (SEM and X-ray diffraction (XRD were employed. The XRD results revealed the amorphous nature of silica nanoparticles. To analyze the quantity and properties of the compounds coated with Si oxide, transmission electron microscopy (TEM in conjunction with electron dispersive spectroscopy was used. Finally, it is suggested that the simple growth process is more favorable mechanism than the solution/aggregation process.

  10. Low temperature synthesis, characterization and tunable optical properties of Eu3+, Tb3+ doped CaMoO4 nanoparticles

    International Nuclear Information System (INIS)

    Sharma, K. Gayatri; Singh, Th. Prasanta; Singh, N. Rajmuhon

    2014-01-01

    Highlights: • Red and green nanophosphors of CaMoO 4 :Eu 3+ and Tb 3+ were synthesized via an ethylene glycol route at very low temperature. • The prepared nanoparticles have tetragonal structure. • The luminescence properties of the nanoparticles are also studied extensively. • CIE chromaticity coordinates of the phosphors are also studied. • The blue-green emission of host could be easily tuned to red or green by varying the dopant ion used in the host. - Abstract: CaMoO 4 doped with Eu 3+ and Tb 3+ nanoparticles are obtained using ethylene glycol as the solvent. The synthesis has been carried out at 130 °C temperature. The XRD patterns reveal that all the doped samples are well assigned to the scheelite structure of the CaMoO 4 phase. Upon excitation by ultraviolet radiation, the CaMoO 4 :Eu 3+ , Tb 3+ phosphors show the characteristic emission lines of Eu 3+ and Tb 3+ . For Eu 3+ doped samples, red emission dominates over other transitions and for Tb 3+ doped, green emission is the predominant one. The blue-green emission of the host could be easily tuned to red and green by doping with activator ions. The emission intensity is also dependent on the concentration of the dopant ions. The prepared nanoparticles could find applications in LEDs and other optical devices

  11. Single-source-precursor Synthesis and High-temperature Behavior of SiC Ceramics Containing Boron

    Science.gov (United States)

    Gui, Miaomiao; Fang, Yunhui; Yu, Zhaoju

    2014-12-01

    In this paper, a hyperbranched polyborocarbosilane (HPBCS) was prepared by a one-pot synthesis with Cl2Si(CH3)CH2Cl, Cl3SiCH2Cl and BCl3 as the starting materials. The obtained HPBCS was characterized by GPC, FT-IR and NMR, and was confirmed to have hyperbranched structures. The thermal property of the resulting HPBCS was investigated by TGA. The ceramic yield of the HPBCS is about 84% and that of the counterpart hyperbranched hydridopolycarbosilane is only 45%, indicating that the introduction of boron into the preceramic polymer significantly improved the ceramic yield. With the polymer-derived ceramic route, the final ceramics were annealed at 1800 °C in argon atmosphere for 2 h in order to characterize the microstructure and to evaluate the high-temperature behavior. The final ceramic microstructure was studied by XRD and SEM, indicating that the introduction of boron dramatically inhibits SiC crystallization. The boron-containing SiC ceramic shows excellent high-temperature behavior against decomposition and crystallization at 1800 °C.

  12. Synthesis of indium oxide cubic crystals by modified hydrothermal route for application in room temperature flexible ethanol sensors

    Energy Technology Data Exchange (ETDEWEB)

    Seetha, M., E-mail: seetha.phy@gmail.com [Department of Physics, SRM University, Kattankulathur, Kancheepuram Dt 603 203 (India); Meena, P. [Department of Physics, PSGR Krishnammal College for Women, Coimbatore 641 046 (India); Mangalaraj, D., E-mail: dmraj800@yahoo.com [DRDO-BU Centre for Life Sciences, Bharathiar University Campus, Coimbatore (India); Department of Nanoscience and Technology, Bharathiar University, Coimbatore 641 014 (India); Masuda, Yoshitake [National Institute of Advanced Industrial Science and Technology (AIST), Nagoya 463-8560 (Japan); Senthil, K. [School of Advanced Materials Science and Engineering, Sungkyunkwan University (Suwon Campus), Cheoncheon-dong 300, Jangan-gu, Suwon 440-746 (Korea, Republic of)

    2012-03-15

    Highlights: Black-Right-Pointing-Pointer For the first time HMT is used in the preparation of indium oxide. Black-Right-Pointing-Pointer HMT itself acts as base for the precursor and results in cubic indium hydroxide. Black-Right-Pointing-Pointer Modified hydrothermal route used for the preparation of cubic indium oxide crystals. Black-Right-Pointing-Pointer As a new approach a composite film synthesized with prepared indium oxide. Black-Right-Pointing-Pointer Film showed good response to ethanol vapours with quick response and recovery times. - Abstract: Indium oxide cubic crystals were prepared by using hexamethylenetetramine and indium chloride without the addition of any structure directing agents. The chemical route followed in the present work was a modified hydrothermal synthesis. The average crystallite size of the prepared cubes was found to be 40 nm. A blue emission at 418 nm was observed at room temperature when the sample was excited with a 380 nm Xenon lamp. This emission due to oxygen vacancies made the material suitable for gas sensing applications. The synthesized material was made as a composite film with polyvinyl alcohol which was more flexible than the films prepared on glass substrates. This flexible film was used as a sensing element and tested with ethanol vapours at room temperature. The film showed fast response as well as recovery to ethanol vapours with a sensor response of about 1.4 for 100 ppm of the gas.

  13. Synthesis of indium oxide cubic crystals by modified hydrothermal route for application in room temperature flexible ethanol sensors

    International Nuclear Information System (INIS)

    Seetha, M.; Meena, P.; Mangalaraj, D.; Masuda, Yoshitake; Senthil, K.

    2012-01-01

    Highlights: ► For the first time HMT is used in the preparation of indium oxide. ► HMT itself acts as base for the precursor and results in cubic indium hydroxide. ► Modified hydrothermal route used for the preparation of cubic indium oxide crystals. ► As a new approach a composite film synthesized with prepared indium oxide. ► Film showed good response to ethanol vapours with quick response and recovery times. - Abstract: Indium oxide cubic crystals were prepared by using hexamethylenetetramine and indium chloride without the addition of any structure directing agents. The chemical route followed in the present work was a modified hydrothermal synthesis. The average crystallite size of the prepared cubes was found to be 40 nm. A blue emission at 418 nm was observed at room temperature when the sample was excited with a 380 nm Xenon lamp. This emission due to oxygen vacancies made the material suitable for gas sensing applications. The synthesized material was made as a composite film with polyvinyl alcohol which was more flexible than the films prepared on glass substrates. This flexible film was used as a sensing element and tested with ethanol vapours at room temperature. The film showed fast response as well as recovery to ethanol vapours with a sensor response of about 1.4 for 100 ppm of the gas.

  14. A chemical route to room-temperature synthesis of nanocrystalline TiO2 thin films

    International Nuclear Information System (INIS)

    Pathan, Habib M.; Kim, Woo Young; Jung, Kwang-Deog; Joo, Oh-Shim

    2005-01-01

    A lot of methods are developed for the deposition of TiO 2 thin films; however, in each of these methods as-deposited films are amorphous and need further heat treatment at high temperature. In the present article, a chemical bath deposition (CBD) method was used for the preparation of TiO 2 thin films. We investigated nanocrystalline TiO 2 thin films using CBD at room temperature onto glass and ITO coated glass substrate. The films were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM), and high-resolution transmission electron microscopy (HRTEM) techniques. The chemically synthesized films were nanocrystalline and composed of crystal grains of 2-3 nm

  15. Synthesis of nanocrystalline ceria thin films by low-temperature thermal decomposition of Ce-propionate

    International Nuclear Information System (INIS)

    Roura, P.; Farjas, J.; Ricart, S.; Aklalouch, M.; Guzman, R.; Arbiol, J.; Puig, T.; Calleja, A.; Peña-Rodríguez, O.; Garriga, M.; Obradors, X.

    2012-01-01

    Thin films of Ce-propionate (thickness below 20 nm) have been deposited by spin coating and pyrolysed into ceria at temperatures below 200 °C. After 1 h of thermal treatment, no signature of the vibrational modes of Ce-propionate is detected by infrared spectroscopy, indicating that decomposition has been completed. The resulting ceria films are nanocrystalline as revealed by X-ray diffraction (average grain size of 2–2.5 nm) and confirmed by microscopy. They are transparent in the visible region and show the characteristic band gap absorption below 400 nm. A direct band gap energy of 3.50 ± 0.05 eV has been deduced irrespective of the pyrolysis temperature (160, 180 and 200 °C).

  16. CTAB assisted synthesis of tungsten oxide nanoplates as an efficient low temperature NOX sensor

    Science.gov (United States)

    Mehta, Swati S.; Tamboli, Mohaseen S.; Mulla, Imtiaz S.; Suryavanshi, Sharad S.

    2018-02-01

    Tungsten oxide nanoplates with porous morphology were effectively prepared by acidification using CTAB (HexadeCetyltrimethyl ammonium bromide) as a surfactant. For characterization, the synthesized materials were subjected to X-Ray powder diffraction (XRD), scanning electron microscopy (SEM), high resolution transmission electron microscopy (HRTEM), UV-Visible spectroscopy (UV-Vis) and surface area (BET) measurements. The morphology and size of the particles were controlled by solution acidity. The BET results confirmed that the materials are well crystallized and mesoporous in nature. The nanocrystalline powder was used to prepare thick films by screen printing on alumina substrate for the investigation of gas sensing properties. The gas response measurements revealed that the samples acidified using 10 M H2SO4 exhibits highest response of 91% towards NOX at optimum temperature of 200 °C for 100 ppm, and it also exhibits 35% response at room temperature.

  17. Green synthesis of Ni-Nb oxide catalysts for low-temperature oxidative dehydrogenation of ethane

    KAUST Repository

    Zhu, Haibo

    2015-03-05

    The straightforward solid-state grinding of a mixture of Ni nitrate and Nb oxalate crystals led to, after mild calcination (T<400°C), nanostructured Ni-Nb oxide composites. These new materials efficiently catalyzed the oxidative dehydrogenation (ODH) of ethane to ethylene at a relatively low temperature (T<300°C). These catalysts appear to be much more stable than the corresponding composites prepared by other chemical methods; more than 90% of their original intrinsic activity was retained after 50h with time on-stream. Furthermore, the stability was much less affected by the Nb content than in composites prepared by classical "wet" syntheses. These materials, obtained in a solvent-free way, are thus promising green and sustainable alternatives to the current Ni-Nb candidates for the low-temperature ODH of ethane.

  18. Synthesis of zirconium dioxide by ultrasound assisted precipitation: effect of calcination temperature.

    Science.gov (United States)

    Prasad, Krishnamurthy; Pinjari, D V; Pandit, A B; Mhaske, S T

    2011-09-01

    Nanostructured zirconium dioxide was synthesized from zirconyl nitrate using both conventional and ultrasound assisted precipitation in alkaline medium. The synthesized samples were calcinated at temperatures ranging from 400°C to 900°C in steps of 100°C. The ZrO(2) specimens were characterized using X-ray Diffraction (XRD) and Scanning Electron Microscopy (SEM). The thermal characteristics of the samples were studied via Differential Scanning Calorimetry-Thermo-Gravimetry Analysis (DSC-TGA). The influence of the calcination temperature on the phase transformation process from monoclinic to tetragonal to cubic zirconia and its consequent effect on the crystallite size and % crystallinity of the synthesized ZrO(2) was studied and interpreted. It was observed that the ultrasound assisted technique helped to hasten to the phase transformation and also at some point resulted in phase stabilization of the synthesized zirconia. Copyright © 2011 Elsevier B.V. All rights reserved.

  19. Effect of growth temperature and precursor concentration on synthesis of CVD-graphene from camphor

    Science.gov (United States)

    Rajaram, Narasimman; Patel, Biren; Ray, Abhijit; Mukhopadhyay, Indrajit

    2018-05-01

    Here, we have synthesized CVD-graphene from camphor by using atmospheric pressure (AP)-CVD system on Cu foil. We have studied the effect of growth temperature and camphor concentration by using scanning electron microscopy (SEM) and Raman spectroscopy. The domain size of the graphene is increasing with an increase in the temperature and camphor quantity. The complete coverage of graphene on the Cu foil achieved at 1020 °C. Higher camphor quantity leads to growth of multilayer graphene. The graphene is transferred by PMMA-assisted method onto the glass substrate. The sheet resistance and transmittance of the graphene are 1.5 kohm/sq and 92.7%, respectively.

  20. Synthesis of Eu3+-doped calcium and strontium carbonate phosphors at room temperature

    International Nuclear Information System (INIS)

    Pan Yuexiao; Wu Mingmei; Su Qiang

    2003-01-01

    Red phosphors CaCO 3 :Eu 3+ and SrCO 3 :Eu 3+ have been prepared by co-precipitation with ammonium bicarbonate (NH 4 HCO 3 ) at room temperature. Pure calcite CaCO 3 can be obtained by prolonging the reaction time at 220 deg. C and it decomposes to cubic CaO at 1000 deg. C. Trivalent Eu 3+ acts as a luminescent probe to determine both the calcite and the mixed phase of calcite and vaterite phase of CaCO 3 host and to analyze its decomposition process. High temperature sintering improved both the crystallization and luminescence of SrCO 3 :Eu 3+ in aragonite phase

  1. Low temperature synthesis of coiled carbon nanotubes and their magnetic properties

    Science.gov (United States)

    Krishna, Vemula Mohana; Somanathan, T.; Manikandan, E.

    2018-04-01

    In this paper, coiled like structure of carbon nanotubes (c-CNTs) have been effectively grown on bi-metal substituted α-alumina nanoparticles catalyst by chemical vapor deposition (CVD) system. Highly graphitized and dense bundles of carbon product were attained at a low temperature of 550 °C. The coiled carbon nanostructures in very longer lengths were noticed by field emission scanning electron microscope (FESEM) observation. Furthermore, high purity material was achieved, which correlates the energy dispersive x-ray spectroscopy (EDX) analysis. High resolution transmission electron microscope (HRTEM) revealed the diameter and graphitization of coiled structures. The superparamagnetic like behavior was observed at room temperature for the as-synthesized product, which was found by VSM investigation.

  2. Low-temperature synthesis of homogeneous nanocrystalline cubic silicon carbide films

    International Nuclear Information System (INIS)

    Cheng Qijin; Xu, S.

    2007-01-01

    Silicon carbide films are fabricated by inductively coupled plasma chemical vapor deposition from feedstock gases silane and methane heavily diluted with hydrogen at a low substrate temperature of 300 deg. C. Fourier transform infrared absorption spectroscopy, Raman spectroscopy, x-ray photoelectron spectroscopy, and high-resolution transmission electron microscopy analyses show that homogeneous nanocrystalline cubic silicon carbide (3C-SiC) films can be synthesized at an appropriate silane fraction X[100%xsilane flow(SCCM)/silane+methane flow(SCCM)] in the gas mixture. The achievement of homogeneous nanocrystalline 3C-SiC films at a low substrate temperature of 300 deg. C is a synergy of a low deposition pressure (22 mTorr), high inductive rf power (2000 W), heavy dilution of feedstock gases silane and methane with hydrogen, and appropriate silane fractions X (X≤33%) in the gas mixture employed in our experiments

  3. Tannic acid assisted synthesis of flake-like hydroxyapatite nanostructures at room temperature

    Science.gov (United States)

    Vázquez, Maricela Santana; Estevez, O.; Ascencio-Aguirre, F.; Mendoza-Cruz, R.; Bazán-Díaz, L.; Zorrila, C.; Herrera-Becerra, R.

    2016-09-01

    A simple and non-expensive procedure was performed to synthesize hydroxyapatite (HAp) flake-like nanostructures, by using a co-precipitation method with tannic acid as stabilizing agent at room temperature and freeze drying. Samples were synthesized with two different salts, Ca(NO3)2 and CaCl2. X-ray diffraction analysis, Raman spectroscopy, scanning and transmission electron microscopy characterizations reveal Ca10(PO4)6(OH)2 HAp particles with hexagonal structure and P63/m space group in both cases. In addition, the particle size was smaller than 20 nm. The advantage of this method over the works reported to date lies in the ease for obtaining HAp particles with a single morphology (flakes), in high yield. This opens the possibility of expanding the view to the designing of new composite materials based on the HAp synthesized at room temperature.

  4. Low temperature synthesis and photoluminescence study of Y2Ti2O7:Eu nanoparticles

    International Nuclear Information System (INIS)

    Selvi, E.; Prasad, A.I.; Nigam, Sandeep; Sudarsan, V.; Vatsa, R.K.

    2014-01-01

    Very small nanoparticles both undoped and doped Y 2 Ti 2 O 7 were prepared at a low temperature (700℃). The obtained undoped and doped Y 2 Ti 2 O 7 samples exhibit good crystallinity, smaller average crystallite size. Based on the detailed luminescence studies, it is confirmed that the lanthanide doped nano-materials have improved luminescence properties compared to the corresponding bulk samples. (author)

  5. Investigation of Room Temperature Synthesis of Titanium Dioxide Nanoclusters Dispersed on Cubic MCM-48 Mesoporous Materials

    OpenAIRE

    Sridhar Budhi; Chia-Ming Wu; Dan Zhao; Ranjit T. Koodali

    2015-01-01

    Titania containing cubic MCM-48 mesoporous materials were synthesized successfully at room temperature by a modified Stöber method. The integrity of the cubic mesoporous phase was retained even at relatively high loadings of titania. The TiO2-MCM-48 materials were extensively characterized by a variety of physico-chemical techniques. The physico-chemical characterization indicate that Ti4+ ions can be substituted in framework tetrahedral positions. The relative amount of Ti4+ ions in tetrahe...

  6. Effect of calcination temperature on the synthesis of potassium titanate with platy morphology

    International Nuclear Information System (INIS)

    Farina, R.; Fredericci, C.; Yoshimura, H.N.

    2011-01-01

    The dramatic increases in the number of pneumoconiosis cases have stimulated the search of new materials for replacement of asbestos fibers. Titanate plates with formula A y Ti 2-x M x O 4 , where A = K, Rb, Cs and M = Li, Mg, Co, Ni, Cu, Zn, Mn (III), Fe (III) have been studied as an alternative for the use of fibers. The effect of the variation of calcination temperature on the reaction of K 2 CO 3 -TiO 2 -Mg(OH) 2 system was studied with the aim of understanding the relationship of this parameter with the morphology and symmetry of the obtained plates. For this study the samples were calcined for 5 hours at temperatures of 950°C, 1000°C, 1050°C and 1100°C. The powders were analyzed by X-ray diffraction and scanning electron microscopy. It was concluded that 1000°C is the better calcination temperature for obtaining more symmetric plates with smaller particle size dispersion. (author)

  7. SnO2 thin film synthesis for organic vapors sensing at ambient temperature

    Directory of Open Access Journals (Sweden)

    N.H. Touidjen

    2016-12-01

    Full Text Available The present work is a study of tin dioxide (SnO2 based thin sensitive layer dedicated to organic vapors detection at ambient temperature. SnO2 thin film was deposited by chemical spray pyrolysis technique. The glass substrate temperature was kept to 400 °C, using a starting solution of 0.1 M tin (II dichloride dihydrate (SnCl2, 2H2O. Films structural and morphological properties were characterized using X-ray diffraction (XRD, scanning electron microscopy (SEM and atomic force microscope (AFM respectively. Films optical characteristics were studied using UV-VIS spectrophotometer. XRD revealed the presence of pure SnO2 polycrystalline thin film with a tetragonal rutile structure. The SEM and AFM observations confirmed the granular morphology with presence of pores in the film surface. The prepared film was tested in various organic vapors (ethanol, methanol and acetone at ambient operating temperature (25 °C ± 2 °C. The obtained results suggested that SnO2 is more sensitive to ethanol vapor with a maximum sensitivity of 35% higher than to methanol and acetone vapors (1% and 3%. The realized SnO2 based sensor demonstrated fast response and recovery times as revealed by the values of 2 s to 3 s towards 47 ppm of ethanol vapor. Keywords: SnO2 thin film, Sensitivity, XRD, SEM, AFM, UV–visible

  8. Room temperature ferromagnetism of tin oxide nanocrystal based on synthesis methods

    Energy Technology Data Exchange (ETDEWEB)

    Sakthiraj, K.; Hema, M. [Department of Physics, Kamaraj College of Engineering and Technology, Virudhunagar 626001, Tamil Nadu (India); Balachandrakumar, K. [Department of Physics, Raja Doraisingam Government Arts College, Sivagangai 630561, Tamil Nadu (India)

    2016-04-15

    The experimental conditions used in the preparation of nanocrystalline oxide materials play an important role in the room temperature ferromagnetism of the product. In the present work, a comparison was made between sol–gel, microwave assisted sol–gel and hydrothermal methods for preparing tin oxide nanocrystal. X-ray diffraction analysis indicates the formation of tetragonal rutile phase structure for all the samples. The crystallite size was estimated from the HRTEM images and it is around 6–12 nm. Using optical absorbance measurement, the band gap energy value of the samples has been calculated. It reveals the existence of quantum confinement effect in all the prepared samples. Photoluminescence (PL) spectra confirms that the luminescence process originates from the structural defects such as oxygen vacancies present in the samples. Room temperature hysteresis loop was clearly observed in M–H curve of all the samples. But the sol–gel derived sample shows the higher values of saturation magnetization (M{sub s}) and remanence (M{sub r}) than other two samples. This study reveals that the sol–gel method is superior to the other two methods for producing room temperature ferromagnetism in tin oxide nanocrystal.

  9. Synthesis of Highly Uniform and Compact Lithium Zinc Ferrite Ceramics via an Efficient Low Temperature Approach.

    Science.gov (United States)

    Xu, Fang; Liao, Yulong; Zhang, Dainan; Zhou, Tingchuan; Li, Jie; Gan, Gongwen; Zhang, Huaiwu

    2017-04-17

    LiZn ferrite ceramics with high saturation magnetization (4πM s ) and low ferromagnetic resonance line widths (ΔH) represent a very critical class of material for microwave ferrite devices. Many existing approaches emphasize promotion of the grain growth (average size is 10-50 μm) of ferrite ceramics to improve the gyromagnetic properties at relatively low sintering temperatures. This paper describes a new strategy for obtaining uniform and compact LiZn ferrite ceramics (average grains size is ∼2 μm) with enhanced magnetic performance by suppressing grain growth in great detail. The LiZn ferrites with a formula of Li 0.415 Zn 0.27 Mn 0.06 Ti 0.1 Fe 2.155 O 4 were prepared by solid reaction routes with two new sintering strategies. Interestingly, results show that uniform, compact, and pure spinel ferrite ceramics were synthesized at a low temperature (∼850 °C) without obvious grain growth. We also find that a fast second sintering treatment (FSST) can further improve their gyromagnetic properties, such as higher 4πM s and lower ΔH. The two new strategies are facile and efficient for densification of LiZn ferrite ceramics via suppressing grain growth at low temperatures. The sintering strategy reported in this study also provides a referential experience for other ceramics, such as soft magnetism ferrite ceramics or dielectric ceramics.

  10. Perylene diimide: Synthesis, fabrication and temperature dependent electrical characterization of heterojunction with p-silicon

    Energy Technology Data Exchange (ETDEWEB)

    Tahir, Muhammad [Faculty of Engineering Sciences, GIK Institute of Engineering Sciences and Technology Topi, KPK 23640 (Pakistan); Department of Physics, Abdul Wali Khan University Mardan, 23200 KPK (Pakistan); Sayyad, Muhammad Hassan; Wahab, Fazal [Faculty of Engineering Sciences, GIK Institute of Engineering Sciences and Technology Topi, KPK 23640 (Pakistan); Aziz, Fakhra, E-mail: fakhra69@yahoo.com [Department of Electronics, Jinnah College for Women, University of Peshawar, Peshawar 25120 (Pakistan); Shahid, Muhammad; Munawar, Munawar Ali [Institute of Chemistry, University of the Punjab, Lahore 54000 (Pakistan)

    2013-10-01

    A novel, n-type, organic semiconductor N-Butyl-N′-(6-hydroxyhexyl)perylene-3,4,9,10-tetracarboxylic acid diimide (N-BuHHPDI) has been successfully synthesized in high yield. The compound has been characterized by atomic force microscopy (AFM) to understand the morphological properties of a new n-type organic semiconducting material. A 120 nm thin film of N-BuHHPDI has been sandwiched between Al and p-Si to form Al/N-BuHHPDI/p-Si device using the vacuum thermal evaporation technique. The electrical properties of sandwich type Al/N-BuHHPDI/p-Si device have been investigated. The current voltage (I–V) characteristics of the device, in dark, have been measured in the temperature range of 300–330 K. At room temperature, the device exhibits rectifying behavior with a rectification ratio of 51.5 at ±6.8 V. The device parameters such as ideality factor, barrier height, series and shunt resistances have been extracted using the conventional I–V characterization method. The effect of temperature on these parameters is also studied. Alternative electrical characterization methods such as Cheung's functions and Norde's techniques have been employed to measure the device parameters for comparison. The conduction mechanisms are investigated through the interface of N-BuHHPDI and p-Si.

  11. Tunable Synthesis of SiC/SiO2 Heterojunctions via Temperature Modulation

    Directory of Open Access Journals (Sweden)

    Wei Li

    2018-05-01

    Full Text Available A large-scale production of necklace-like SiC/SiO2 heterojunctions was obtained by a molten salt-mediated chemical vapor reaction technique without a metallic catalyst or flowing gas. The effect of the firing temperature on the evolution of the phase composition, microstructure, and morphology of the SiC/SiO2 heterojunctions was studied. The necklace-like SiC/SiO2 nanochains, several centimeters in length, were composed of SiC/SiO2 core-shell chains and amorphous SiO2 beans. The morphologies of the as-prepared products could be tuned by adjusting the firing temperature. In fact, the diameter of the SiO2 beans decreased, whereas the diameter of the SiC fibers and the thickness of the SiO2 shell increased as the temperature increased. The growth mechanism of the necklace-like structure was controlled by the vapor-solid growth procedure and the modulation procedure via a molten salt-mediated chemical vapor reaction process.

  12. Low temperature synthesis, photoluminescence, magnetic properties of the transition metal doped wurtzite ZnS nanowires

    International Nuclear Information System (INIS)

    Cao, Jian; Han, Donglai; Wang, Bingji; Fan, Lin; Fu, Hao; Wei, Maobin; Feng, Bo; Liu, Xiaoyan; Yang, Jinghai

    2013-01-01

    In this paper, we synthesized the transition metal ions (Mn, Cu, Fe) doped and co-doped ZnS nanowires (NWs) by a one-step hydrothermal method. The results showed that the solid solubility of the Fe 2+ ions in the ZnS NWs was about two times larger than that of the Mn 2+ or Cu 2+ ions in the ZnS NWs. There was no phase transformation from hexagonal to cubic even in a large quantity transition metal ions introduced for all the samples. The Mn 2+ /Cu 2+ /Fe 2+ related emission peaks can be observed in the Mn 2+ ,Cu 2+ and Fe 2+ doped ZnS NWs. The ferromagnetic properties of the co-doped samples were investigated at room temperature. - graphical abstract: The stable wurtzite ZnS:TM 2+ (TM=Mn, Cu, Fe) nanowires with room temperature ferromagnetism properties were obtained. The different elongation of unit cell caused by the different doped ions was observed. Highlights: ► The transition metal ions doped wurtzite ZnS nanowires were synthesized at 180 °C. ► There was no phase transformation from hexagonal to cubic even in a large quantity introduced for all the samples. ► The room temperature ferromagnetism properties of the co-doped nanowires were investigated

  13. Synthesis and thermal properties of a novel high temperature alkyl-center-trisphenolic-based phthalonitrile polymer

    International Nuclear Information System (INIS)

    Sheng, Haitong; Peng, Xuegang; Guo, Hui; Yu, Xiaoyan; Tang, Chengchun; Qu, Xiongwei; Zhang, Qingxin

    2013-01-01

    A novel alkyl-center-trisphenolic-based high-temperature phthalonitrile monomer, namely, 1,1,1-tris-[4-(3,4-dicyanophenoxy)phenyl]ethane (TDPE), was synthesized from 1,1,1-tris-(4-hydroxyphenyl)ethane (THPE) via a facile nucleophilic displacement of a nitro-substituent from 4-nitrophthalonitrile (NPN). The structure of TDPE monomer was characterized by Fourier transform infrared spectroscopy (FT-IR), nuclear magnetic resonance spectroscopy ( 1 H and 13 C NMR), elemental analysis (EA). Curing behaviors of TDPE with 4-(aminophenoxy)phthalonitrile (APPH) were recorded by differential scanning calorimetric (DSC) and it showed a large processing window (122 °C) which is favorable to processing TDPE polymers. The structure of TDPE polymer was discussed and the thermal stabilities of TDPE polymer were evaluated by thermogravimetric analysis (TGA). The TDPE polymer exhibits excellent thermal stability, and mechanism of thermal decompositions was explored. Dynamic mechanical analysis (DMA) revealed that the TDPE polymer has high storage modulus and high glass transition temperature (T g > 380 °C). - Highlights: • A novel high-temperature phthalonitrile polymer was synthesized. • Polymerization mechanism was explored. • The polymer shows excellent thermal stability. • Outstanding mechanical properties was achieved: storage modulus = 3.7 GPa, T g > 380 °C. • Thermal decomposition mechanism was discussed

  14. Synthesis of InGaZnO{sub 4} nanoparticles using low temperature multistep co-precipitation method

    Energy Technology Data Exchange (ETDEWEB)

    Wu, Ming-Chung, E-mail: mingchungwu@mail.cgu.edu.tw; Hsiao, Kai-Chi; Lu, Hsin-Chun

    2015-07-15

    Indium gallium zinc oxide (InGaZnO{sub 4}, IGZO) has attracted explosive growth in investigations over the last decades as an important material in the thin-film transistor. In this study, the various nitrate precursors, including indium nitrate, gallium nitrate, and zinc nitrate, were prepared from the various metals dissolved in nitric acid. Then, we used these nitrate precursors to synthesize the IGZO precursor powder by the multistep co-precipitation method. The synthesis parameters of the co-precipitation method, such as reaction temperature, pH value and reaction time, were controlled precisely to prepare the high quality IGZO precursor powder. Finally, IGZO precursor powder was calcined at 900 °C. Then, the microstructure, the crystalline structure, the particle size distribution and specific surface area of calcined IGZO precursor powder were characterized by electron transmission microscopy, X-ray diffraction technique, dynamic light scattering method and the surface area and porosimetry analyzer, respectively. The relative density of IGZO tablet sintered at 1200 °C for 12 h is as high as 97.30%, and it showed highly InGaZnO{sub 4} crystalline structure and the large grain size. The IGZO nanoparticles developed in our study has the potential for the high quality target materials used in the application of electronic devices. - Graphical abstract: Display Omitted - Highlights: • InGaZnO{sub 4} (IGZO) nanoparticle was synthesized by multistep co-precipitation method. • The synthesis parameters were controlled precisely to prepare high quality powder. • The relative density of highly crystalline IGZO tablet is as high as 97.30%. • IGZO tablet exhibited highly crystalline structure and the large grain size.

  15. Synthesis of InGaZnO4 nanoparticles using low temperature multistep co-precipitation method

    International Nuclear Information System (INIS)

    Wu, Ming-Chung; Hsiao, Kai-Chi; Lu, Hsin-Chun

    2015-01-01

    Indium gallium zinc oxide (InGaZnO 4 , IGZO) has attracted explosive growth in investigations over the last decades as an important material in the thin-film transistor. In this study, the various nitrate precursors, including indium nitrate, gallium nitrate, and zinc nitrate, were prepared from the various metals dissolved in nitric acid. Then, we used these nitrate precursors to synthesize the IGZO precursor powder by the multistep co-precipitation method. The synthesis parameters of the co-precipitation method, such as reaction temperature, pH value and reaction time, were controlled precisely to prepare the high quality IGZO precursor powder. Finally, IGZO precursor powder was calcined at 900 °C. Then, the microstructure, the crystalline structure, the particle size distribution and specific surface area of calcined IGZO precursor powder were characterized by electron transmission microscopy, X-ray diffraction technique, dynamic light scattering method and the surface area and porosimetry analyzer, respectively. The relative density of IGZO tablet sintered at 1200 °C for 12 h is as high as 97.30%, and it showed highly InGaZnO 4 crystalline structure and the large grain size. The IGZO nanoparticles developed in our study has the potential for the high quality target materials used in the application of electronic devices. - Graphical abstract: Display Omitted - Highlights: • InGaZnO 4 (IGZO) nanoparticle was synthesized by multistep co-precipitation method. • The synthesis parameters were controlled precisely to prepare high quality powder. • The relative density of highly crystalline IGZO tablet is as high as 97.30%. • IGZO tablet exhibited highly crystalline structure and the large grain size

  16. Effects of process parameters on tungsten boride production from WO{sub 3} by self propagating high temperature synthesis

    Energy Technology Data Exchange (ETDEWEB)

    Yazici, Sertac [Metallurgical and Materials Engineering Department, Istanbul Technical University, Maslak, Istanbul 34469 (Turkey); Derin, Bora, E-mail: bderin@itu.edu.tr [Metallurgical and Materials Engineering Department, Istanbul Technical University, Maslak, Istanbul 34469 (Turkey)

    2013-01-01

    Highlights: Black-Right-Pointing-Pointer We produced tungsten boride compounds by SHS method. Black-Right-Pointing-Pointer Mg containing byproducts were leached out by using a hot aqueous HCl media. Black-Right-Pointing-Pointer The ratio of W{sub 2}B{sub 5}/WB was found to be {approx}2.0 containing minor phases of W{sub 2}B and W. - Abstract: In the present study, the production parameters of tungsten boride compounds by self-propagating high-temperature synthesis (SHS) method and following leaching process were investigated. In the SHS stage, the products consisting of tungsten borides, magnesium oxide, magnesium borate, and also minor compounds were obtained by using different initial molar ratios of WO{sub 3}, Mg and B{sub 2}O{sub 3} as starting materials. In the leaching step, Mg containing byproducts, i.e. MgO and Mg{sub 3}B{sub 2}O{sub 6}, existed in the selected SHS product synthesized at 1:8:2.5 initial molar ratio of WO{sub 3}:Mg:B{sub 2}O{sub 3} were leached out by using aqueous HCl solution to obtain clean tungsten boride compounds at different experimental parameters which are time, acid concentration and temperature. The acid leaching experiments of the SHS product showed that optimum leaching conditions could be achieved by using 5.8 M HCl at 1/10 S/L ratio and the temperature of 80 Degree-Sign C for 60 min.

  17. Synthesis and characterisation of novel low temperature ceramic and its implementation as substrate in dual segment CDRA

    Science.gov (United States)

    Kumari, Preeti; Tripathi, Pankaj; Sahu, Bhagirath; Singh, S. P.; Parkash, Om; Kumar, Devendra

    2018-02-01

    Li2O-(2-3x)MgO-(x)Al2O3-P2O5 (LMAP) (x = 0.00-0.08) ceramic system was prepared through solid state synthesis route at different sintering temperatures (800-925 °C). A small addition of Al2O3 (x = 0.02) in LMAP ceramics lowers the sintering temperature by more than 100 °C with good relative density of 94.13%. The sintered samples were characterized in terms of density, apparent porosity, water absorption, crystal structure, micro-structure and microwave dielectric properties. Silver compatibility test is also performed for its use as electrode material in low temperature co-fired ceramic (LTCC) application. To check the performance of the prepared LTCC as substrate, a microstrip-fed aperture-coupled dual segment cylindrical dielectric resonator antenna (DS-CDRA) is designed using LMAP (x = 0.02) ceramic as substrate material and Barium Strontium Titanate with 10 wt% of PbO-BaO-B2O3-SiO2 glass (BSTG) and Teflon as the components of resonating material. The simulation study of the DS-CDRA is performed using the Ansys High Frequency Structure Simulator (HFSS) software. A conductive coating of silver is used on the substrate. The simulated and measured -10 dB reflection coefficient bandwidths of 910 MHz (9.07-9.98 GHz at resonant frequency of 9.49 GHz) and 1080 MHz (8.68-9.76 GHz at resonant frequency of 9.36 GHz), respectively are achieved. The measured results of the fabricated antenna are found in good agreement with the simulation results. The prepared material can find potential applications in radar and radio navigation as well as radio astronomy and military satellite communication.

  18. Self-propagating high-temperature synthesis of Sr-doped LaMnO3 perovskite as oxidation catalyst

    International Nuclear Information System (INIS)

    Hirano, T.; Purwanto, H.; Watanabe, T.; Akiyama, T.

    2007-01-01

    Sr-doped LaMnO 3 perovskite oxide has been focused on as one of the alternative catalysts to precious metals such as platinum that are used for cleaning automotive emission gas. The conventional Solid-state reaction method is a popular productive process for perovskite oxide, however, it is time and energy consuming process because it requires repeated prolonged heat treatment at high temperatures. Therefore, the purposes of this work are to produce Sr-doped LaMnO 3 perovskite by using Self-propagating high-temperature synthesis (SHS) and experimentally examine the oxidation catalytic activity of the product for cleaning automotive emission gas. In the SHS, powders of La 2 O 3 , SrCO 3 , Mn and NaClO 4 were well mixed at the desired ratio and poured in a graphite crucible, where at one end it was ignited by using an electrically heated carbon foil. The wave of exothermic reaction due to oxidation of manganese propagated to the other end in a short time. The obtained products were characterized by means of XRD, FE-SEM, BET and particle size distribution analysis and then evaluated via catalytic oxidation tests by using propane in a fixed bed reactor at several temperatures. From the XRD analysis, the products had the desired composition of La 1-x Sr x MnO 3 (x = 0, 0.1, 0.2 and 0.4) perovskite, in which the replacing ratio x of La and Sr in the products was easily controlled by changing the mixing ratio of raw materials. The catalytic activity test showed that the samples exhibited good catalytic activity for propane oxidation over 200 deg. C , although the products had a relatively small surface area. SHS showed the potential for the production of a relatively inexpensive catalytic converter

  19. Synthesis, characterization and performance of zinc ferrite nanorods for room temperature sensing applications

    International Nuclear Information System (INIS)

    Singh, Archana; Singh, Ajendra; Singh, Satyendra; Tandon, Poonam; Yadav, B.C.; Yadav, R.R.

    2015-01-01

    Highlights: • Fabrication of zinc ferrite thin film LPG and CO 2 gas sensors. • Morphological growth of nanorods. • Significant advancement towards the fabrication of a reliable LPG sensor. • A new pathway to produce nanorods as sensorial material. - Abstract: In the present communication, nanorods of zinc ferrite was synthesized and fabricated by employing sol–gel spin coating process. The synthesized material was characterized using X-ray diffraction, scanning electron microscopy, acoustic particle sizer, atomic force microscopy, UV–visible absorption and infrared spectroscopic techniques. Thermal properties were investigated using differential scanning calorimetry. The XRD reveals cubic spinel structure with minimum crystallite size 10 nm. SEM image of the film shows porous surface morphology with uniform distribution of nanorods. The band gap of the zinc ferrite nanorods was found 3.80 eV using the Tauc plot. ZnFe 2 O 4 shows weak super paramagnetic behavior at room temperature investigated using the vibrating sample magnetometer. Further, the liquefied petroleum gas (LPG) and carbon dioxide gas (CO 2 ) sensing properties of the fabricated film were investigated at room temperature (25 °C). More variations in electrical resistance were observed for LPG in comparison to CO 2 gas. The parameters such as lattice constant, X-ray density, porosity and specific surface area were also calculated for the better understanding of the observed gas sensing properties. High sensitivity and percentage sensor response, small response and recovery times, good reproducibility and stability characterized the fabricated sensor for the detection of LPG at room temperature

  20. Synthesis, characterization and performance of zinc ferrite nanorods for room temperature sensing applications

    Energy Technology Data Exchange (ETDEWEB)

    Singh, Archana; Singh, Ajendra [Macromolecular Research Laboratory, Department of Physics, University of Lucknow, Lucknow 226007, U.P. (India); Singh, Satyendra, E-mail: satyendra_nano84@rediffmail.com [Department of Physics, University of Allahabad, Allahabad 211002, U.P. (India); Tandon, Poonam [Macromolecular Research Laboratory, Department of Physics, University of Lucknow, Lucknow 226007, U.P. (India); Yadav, B.C. [Department of Applied Physics, School for Physical Sciences, Babasaheb Bhimrao Ambedkar University, Lucknow 226025, U.P. (India); Yadav, R.R. [Department of Physics, University of Allahabad, Allahabad 211002, U.P. (India)

    2015-01-05

    Highlights: • Fabrication of zinc ferrite thin film LPG and CO{sub 2} gas sensors. • Morphological growth of nanorods. • Significant advancement towards the fabrication of a reliable LPG sensor. • A new pathway to produce nanorods as sensorial material. - Abstract: In the present communication, nanorods of zinc ferrite was synthesized and fabricated by employing sol–gel spin coating process. The synthesized material was characterized using X-ray diffraction, scanning electron microscopy, acoustic particle sizer, atomic force microscopy, UV–visible absorption and infrared spectroscopic techniques. Thermal properties were investigated using differential scanning calorimetry. The XRD reveals cubic spinel structure with minimum crystallite size 10 nm. SEM image of the film shows porous surface morphology with uniform distribution of nanorods. The band gap of the zinc ferrite nanorods was found 3.80 eV using the Tauc plot. ZnFe{sub 2}O{sub 4} shows weak super paramagnetic behavior at room temperature investigated using the vibrating sample magnetometer. Further, the liquefied petroleum gas (LPG) and carbon dioxide gas (CO{sub 2}) sensing properties of the fabricated film were investigated at room temperature (25 °C). More variations in electrical resistance were observed for LPG in comparison to CO{sub 2} gas. The parameters such as lattice constant, X-ray density, porosity and specific surface area were also calculated for the better understanding of the observed gas sensing properties. High sensitivity and percentage sensor response, small response and recovery times, good reproducibility and stability characterized the fabricated sensor for the detection of LPG at room temperature.

  1. Synthesis colloidal Kyllinga brevifolia-mediated silver nanoparticles at different temperature for methylene blue removal

    Science.gov (United States)

    Isa, Norain; Sarijo, Siti Halimah; Aziz, Azizan; Lockman, Zainovia

    2017-09-01

    Metallic nanoparticles are well known of having wide applications in various fields such as, catalysis, electronics, energy, chemistry and medicine due to its unique physico-chemical properties. In this study, nanocatalyst Kyllinga brevifolia-mediated silver nanoparticles (AgNPs) were prepared by reduction of silver nitrate using aqueous extract of Kyllinga brevifolia at different temperature. The formations of AgNPs were monitored using UV-visible spectroscopy. Transmission electron microscope (TEM) results reveal that the AgNPs well dispersed with average particle size are 22.34 and 6.73 nm for synthesized at room temperature and cold temperature respectively. The biomolecules present in the Kyllinga brevifolia aqueous extract responsible for the formation of AgNPs were identified using Fourier transform infrared (FTIR). Our AgNPs performed excellent catalytic activity in degradation of methylene blue (MB) dyes via electron relay effect. MB is toxic to ecological system and also has carcinogenic properties. The AgNPs nanocatalysts synthesized in this study are highly dispersed, quasi-spherical and due to their size in nanoscale, they have shown effectiveness for degradation of MB dyes. More importantly, our AgNPs were prepared using biomolecules as capping and reducing agent, which make our product "greener" than available AgNPs that are commonly prepared using hydrazine and borohydride; which are harmful substances to human and environment. Not only the AgNPs can act as nanocatalyst for degradation of MB, they can also be expected to degrade other types of toxic dyes used in textiles industry.

  2. Highly temperature responsive core-shell magnetic particles: synthesis, characterization and colloidal properties.

    Science.gov (United States)

    Rahman, Md Mahbubor; Chehimi, Mohamed M; Fessi, Hatem; Elaissari, Abdelhamid

    2011-08-15

    Temperature responsive magnetic polymer submicron particles were prepared by two step seed emulsion polymerization process. First, magnetic seed polymer particles were obtained by emulsion polymerization of styrene using potassium persulfate (KPS) as an initiator and divinylbenzne (DVB) as a cross-linker in the presence of oil-in-water magnetic emulsion (organic ferrofluid droplets). Thereafter, DVB cross-linked magnetic polymer particles were used as seed in the precipitation polymerization of N-isopropylacrylamide (NIPAM) to induce thermosensitive PNIPAM shell onto the hydrophobic polymer surface of the cross-linked magnetic polymer particles. To impart cationic functional groups in the thermosensitive PNIPAM backbone, the functional monomer aminoethylmethacrylate hydrochloride (AEMH) was used to polymerize with NIPAM while N,N'-methylenebisacrylamide (MBA) and 2, 2'-azobis (2-methylpropionamidine) dihydrochloride (V-50) were used as a cross-linker and as an initiator respectively. The effect of seed to monomer (w/w) ratio along with seed nature on the final particle morphology was investigated. Dynamic light scattering (DLS) results demonstrated particles swelling at below volume phase transition temperature (VPTT) and deswelling above the VPTT. The perfect core (magnetic) shell (polymer) structure of the particles prepared was confirmed by Transmission Electron Microscopy (TEM). The chemical composition of the particles were determined by thermogravimetric analysis (TGA). The effect of temperature, pH, ionic strength on the colloidal properties such as size and zeta potential of the micron sized thermo-sensitive magnetic particles were also studied. In addition, a short mechanistic discussion on the formation of core-shell morphology of magnetic polymer particles has also been discussed. Copyright © 2011 Elsevier Inc. All rights reserved.

  3. Low temperature route synthesis of SiC–Al2O3 hetero-structural nanofibers

    International Nuclear Information System (INIS)

    Dai, Xiao; Wang, Hao; Cao, Fengfeng; Yi, Qinghua; Cong, Shan; Wang, Yun; Song, Pingyuan; Zhai, Pengfei; Zou, Guifu; Dong, Chao

    2014-01-01

    SiC–Al 2 O 3 hetero-structural nanofibers have been synthesized by the chemical solution approach at 200 ° C. The diameters of nanofibers are in the range of 60–100 nm while the lengths are from tens of micrometers to hundreds of micrometers. The microstructural analysis shows that the fibers possess a like-epitaxial relationship between (104) of hexagonal Al 2 O 3 and (111) of cubic SiC. Additionally, the optical investigation of the nanofibers suggests there are some defects in the low annealing temperature synthesized SiC–Al 2 O 3 nanofibers. (paper)

  4. Low Temperature Graphene Synthesis from Poly(methyl methacrylate) Using Microwave Plasma Treatment

    Science.gov (United States)

    Yamada, Takatoshi; Ishihara, Masatou; Hasegawa, Masataka

    2013-11-01

    A graphene film having low sheet resistance (600 Ω/sq.) was synthesized at low temperatures of 280 °C. Utilizing microwave plasma treatment, graphene films were synthesized from a solid phase on a copper surface. The full width at half maximum of the 2D-band in the Raman spectrum indicated that a high quality graphene film was formed. Cross-sectional transmission electron microscopy observation revealed that the deposited graphene films consisted of single- or double-layer graphene flakes of nanometer order on the Cu surface, which agrees with the estimated number of layers from an average optical transmittance of 96%.

  5. Low-temperature rapid synthesis and superconductivity of Fe-based oxypnictide superconductors.

    Science.gov (United States)

    Fang, Ai-Hua; Huang, Fu-Qiang; Xie, Xiao-Ming; Jiang, Mian-Heng

    2010-03-17

    Fe-based oxypnictide superconductors were successfully synthesized at lower reaction temperatures and with shorter reaction times made possible by starting with less stable compounds, which provide a larger driving force for reactions. Using ball-milled powders of intermediate compounds, phase-pure superconductors with T(c) above 50 K were synthesized at 1173 K in 20 min. This method is particularly advantageous for retaining F, a volatile dopant that enhances superconductivity. Bulk superconductivity and high upper critical fields up to 392 T in Sm(0.85)Nd(0.15)FeAsO(0.85)F(0.15) were demonstrated.

  6. Low temperature synthesis, magnetic and electrical properties of iron-magnesium superparamagnetic nanoalloy

    Energy Technology Data Exchange (ETDEWEB)

    Nazir, Rabia [Department of Chemistry, Quaid-i-Azam University, Islamabad 45320 (Pakistan); Mazhar, Muhammad [Department of Chemistry, Quaid-i-Azam University, Islamabad 45320 (Pakistan)], E-mail: mazhar42pk@yahoo.com; Akhtar, Muhammad Javed; Nadeem, Muhammad; Siddique, Muhammad [Physics Division, Pinstech, P.O. Nilore, Islamabad (Pakistan); Shah, Raza [HEJ Research Institute of Chemistry, University of Karachi, Karachi 75270 (Pakistan); Hasanain, S. Khurshid [Department of Physics, Quaid-i-Azam University, Islamabad 45320 (Pakistan)

    2009-06-24

    A low temperature chemical approach which beats the miscibility barrier of Fe and Mg has been designed to synthesize Fe-Mg{sub 2} nanoalloy and tested to result nanoparticles of average 30 nm size. The nanoalloy is amorphous in nature and characterized by XPRD, AFM, magnetometery, Moessbauer and impedance spectroscopies. The result of magnetic measurement suggests the sample to be superparamagnetic as evidenced by the {sup 57}Fe Moessbauer spectroscopy. The two Mg atoms occupy different positions around iron resulting in two phase system as shown by Moessbauer and impedance spectroscopies.

  7. Low temperature synthesis, magnetic and electrical properties of iron-magnesium superparamagnetic nanoalloy

    International Nuclear Information System (INIS)

    Nazir, Rabia; Mazhar, Muhammad; Akhtar, Muhammad Javed; Nadeem, Muhammad; Siddique, Muhammad; Shah, Raza; Hasanain, S. Khurshid

    2009-01-01

    A low temperature chemical approach which beats the miscibility barrier of Fe and Mg has been designed to synthesize Fe-Mg 2 nanoalloy and tested to result nanoparticles of average 30 nm size. The nanoalloy is amorphous in nature and characterized by XPRD, AFM, magnetometery, Moessbauer and impedance spectroscopies. The result of magnetic measurement suggests the sample to be superparamagnetic as evidenced by the 57 Fe Moessbauer spectroscopy. The two Mg atoms occupy different positions around iron resulting in two phase system as shown by Moessbauer and impedance spectroscopies.

  8. Room-temperature synthesis and photoluminescence of hexagonal CePO4 nanorods

    Science.gov (United States)

    Zhu, J.; Zhang, K.; Zhao, H. Y.

    2018-01-01

    Hexagonal CePO4 nanorods were synthesized via a simple chemical precipitation route at room-temperature without the presence of surfactants and then characterized by powder X-ray diffraction (XRD), energy-dispersive X-ray (EDX) spectrometry, scanning electron microscopy (SEM), transmission electron microscopy (TEM), ultraviolet-visible (UV-vis) absorption and photoluminescence (PL) spectroscopy. Hexagonal CePO4 nanorods exhibit strong ultraviolet absorption and ultraviolet luminescence, which correspond to the electronic transitions between 4f and 5d state of Ce3+ ions.

  9. Effect of the synthesis temperature of sodium nona-titanate on batch kinetics of strontium-ion adsorption from aqueous solution

    International Nuclear Information System (INIS)

    Merceille, A.; Weinzaepfel, E.; Grandjean, A.; Merceille, A.; Weinzaepfel, E.; Barre, Y.

    2011-01-01

    Sodium titanate materials are promising inorganic ion exchangers for the adsorption of strontium from aqueous solutions. Sodium nona-titanate exhibits a layered structure consisting of titanate layers and exchangeable sodium ions between the layers. The materials used in this study include samples synthesized by a hydrothermal method at temperatures between 60 degrees C and 200 degrees C. Their structure, composition, and morphology were investigated with X-Ray diffraction measurements; thermogravimetric, compositional and surface area analyses, and scanning electron microscopy. The structure, composition, and morphology depended on the synthesis temperature. Batch kinetics experiments for the removal of strontium from aqueous solutions were performed, and the data were fitted by a pseudo-second-order reaction model and a diffusive model. The strontium extraction capacity also depended on the synthesis temperature and exhibited a maximum for samples synthesized at 100 degrees C. The sorption process occurs in one or two diffusion-controlled steps that also depend on the synthesis temperature. These diffusion-limited steps are the boundary-layer diffusion and intra-particle diffusion in the case of pure nona-titanate synthesized at temperatures lower than 170 degrees C, and only intra-particle diffusion in the case of nona-titanate synthesized at 200 degrees C. (authors)

  10. Synthesis and regulation of α-LiZnPO4.H2O via a solid-state reaction at low-heating temperatures

    International Nuclear Information System (INIS)

    Liao Sen; Chen Zhipeng; Tian Xiaozhen; Wu Wenwei

    2009-01-01

    A simple and novel route for the synthesis of a lithium zinc phosphate hydrate, α-LiZnPO 4 .H 2 O, was studied, and the target product was obtained with LiH 2 PO 4 .H 2 O and ZnCO 3 as raw materials and polyethylene glycol-400 (PEG-400) as a surfactant via a one step solid-state reaction at room temperature (25 deg. C). The product was characterized with X-ray powder diffraction (XRD), thermogravimetric analysis and the 1st derivativative of thermogravimetric analysis (TG/DTG) and Fourier transform infrared spectroscopy (FTIR). The comparison experimental results suggested that aging temperature controlled the products of the synthesis, that is, the α-LiZnPO 4 .H 2 O was formed when the reaction mixture was aged at room temperature, and the α-LiZnPO 4 was obtained when the reaction mixture was aged at 80 deg. C.

  11. Room temperature synthesis of a Zn(II) metal-organic coordination polymer for dye removal

    Energy Technology Data Exchange (ETDEWEB)

    Abbasi, Alireza, E-mail: aabbasi@khayam.ut.ac.ir [School of Chemistry, College of Science, University of Tehran, Tehran (Iran, Islamic Republic of); Gharib, Maniya; Najafi, Mahnaz [School of Chemistry, College of Science, University of Tehran, Tehran (Iran, Islamic Republic of); Janczak, Jan [Institute of Low Temperature and Structure Research, Polish Academy of Sciences, PO Box 1410, 50-950 Wrocław (Poland)

    2016-03-15

    A new one-dimensional (1D) coordination polymer, [Zn(4,4′-bpy)(H{sub 2}O){sub 4}](ADC)·4H{sub 2}O (1) (4,4′-bpy=4,4′-bipyridine and H{sub 2}ADC=acetylenedicarboxylic acid), was synthesized at room temperature. The crystal structure of the coordination polymer was determined by single-crystal X-ray diffraction analysis. Compound 1 was also characterized by FT-IR, powder X-ray diffraction (PXRD) and thermogravimetric analysis (TGA). The catalytic activity of 1 was evaluated in the color removal of Bismarck brown as a representative of dye pollutant in water under mild conditions. Coordination polymer 1 exhibited good catalytic activity and stability in the decolorization of Bismarck brown and could be easily recovered and reused for at least three cycles. - Graphical abstract: A new 1D coordination polymer as catalyst for the degradation of Bismarck brown aqueous solution. - Highlights: • A 1D coordination polymer has been synthesized at room temperature. • The prepared compound was utilized for color removal of Bismarck brown dye. • Good catalytic activity and stability in the dye decolorization has been found.

  12. Synthesis, characterization and spectral temperature-dependence of thioglycerol-CdSe nanocrystals

    Energy Technology Data Exchange (ETDEWEB)

    Ben Brahim, Nassim, E-mail: nassim.benbrahim.fsm@gmail.com [Laboratoire des Interfaces et Matériaux Avancés, Faculté des Sciences de Monastir, Boulevard de l’Environnement, 5019 Monastir (Tunisia); Poggi, Mélanie [Laboratoire de Physique de la Matière Condensée, CNRS, Ecole Polytechnique, Université Paris-Saclay, 91128 Palaiseau (France); Haj Mohamed, Naim Bel; Ben Chaâbane, Rafik; Haouari, Mohamed [Laboratoire des Interfaces et Matériaux Avancés, Faculté des Sciences de Monastir, Boulevard de l’Environnement, 5019 Monastir (Tunisia); Negrerie, Michel, E-mail: michel.negrerie@polytechnique.fr [Laboratoire d' Optique et Biosciences, INSERM, CNRS, Ecole Polytechnique, Université Paris-Saclay, 91128 Palaiseau (France); Ben Ouada, Hafedh [Laboratoire des Interfaces et Matériaux Avancés, Faculté des Sciences de Monastir, Boulevard de l’Environnement, 5019 Monastir (Tunisia)

    2016-09-15

    Water-soluble CdSe quantum dots (QDs) have been synthesized with thioglycerol as a stabilizer through a novel hydrothermal route. The obtained thioglycerol capped CdSe (TG-CdSe) nanocrystals were characterized regarding their morphology and structural, thermal and optical properties. The resulting nanocrystals were synthesized in the cubic structure with a near spherical shape, as confirmed by X-ray diffraction and transmission electron microscopy. Combining transmission electron microscopy imaging and calculations using UV–visible absorption spectrum and X-ray diffraction pattern, the diameter of the synthesized nanocrystals was estimated to 2.26 nm. As confirmed by its Fourier transform IR spectrum, thioglycerol was successfully liganded on the surface of the resulting nanocrystals. Band structure parameters of the TG-CdSe nanoparticles were determined and quantum confinement effect was evidenced by optical absorption, fluorescence and Raman measurements. The thermal properties of the TG-CdSe were explored by thermal gravimetric analysis and differential scanning calorimetry. The temperature dependence of both the absorption and fluorescence spectra in the physiological range makes the TG-CdSe nanocrystals sensitive temperature markers, a property that must be taken into account when developing any probing applications, especially for cellular imaging.

  13. Electro-hydrodynamic spray synthesis and low temperature spectroscopic characterization of Perovskite thin films

    Science.gov (United States)

    Sarang, Som; Ishihara, Hidetaka; Tung, Vincent; Ghosh, Sayantani

    Utilizing a Marangoni flow inspired electrospraying technique, we synthesize hybrid perovskite (PVSK) thin films with broad absorption spectrum and high crystallinity. The precursor solvents are electrosprayed onto an indium tin oxide (ITO) substrate, resulting in a gradient force developing between the droplet surface and the bulk due to the varying vapor pressure in the bi-solvent system. This gradient force helps the droplets propagate and merge with surrounding ones, forming a uniform thin film with excellent morphological and topological characteristics, as evident from the average power conversion efficiency (PCE) of 16%. In parallel, we use low temperature static and dynamic photoluminescence spectroscopy to probe the grain boundaries and defects in the synthesized PVSK thin films. At 120 K, the emergence of the low temperature orthorhombic phase is accompanied by reduction in lifetimes by an order of magnitude, a result attributed to charge transfer between the orthorhombic and tetragonal domains, as well as due to a crossover from free charge carrier to excitonic recombination. Our fabrication technique and optical studies help in advancement of PVSK based technology by providing unique insights into the fundamental physics of these novel materials. This research was supported by National Aeronautics and Space administration (NASA) Grant No: NNX15AQ01A.

  14. Low temperature synthesis and electrical characterization of germanium doped Ti-based nanocrystals for nonvolatile memory

    International Nuclear Information System (INIS)

    Feng, Li-Wei; Chang, Chun-Yen; Chang, Ting-Chang; Tu, Chun-Hao; Wang, Pai-Syuan; Lin, Chao-Cheng; Chen, Min-Chen; Huang, Hui-Chun; Gan, Der-Shin; Ho, New-Jin; Chen, Shih-Ching; Chen, Shih-Cheng

    2011-01-01

    Chemical and electrical characteristics of Ti-based nanocrystals containing germanium, fabricated by annealing the co-sputtered thin film with titanium silicide and germanium targets, were demonstrated for low temperature applications of nonvolatile memory. Formation and composition characteristics of nanocrystals (NCs) at various annealing temperatures were examined by transmission electron microscopy and X-ray photon-emission spectroscopy, respectively. It was observed that the addition of germanium (Ge) significantly reduces the proposed thermal budget necessary for Ti-based NC formation due to the rise of morphological instability and agglomeration properties during annealing. NC structures formed after annealing at 500 °C, and separated well at 600 °C annealing. However, it was also observed that significant thermal desorption of Ge atoms occurs at 600 °C due to the sublimation of formatted GeO phase and results in a serious decrease of memory window. Therefore, an approach to effectively restrain Ge thermal desorption is proposed by encapsulating the Ti-based trapping layer with a thick silicon oxide layer before 600 °C annealing. The electrical characteristics of data retention in the sample with the 600 °C annealing exhibited better performance than the 500 °C-annealed sample, a result associated with the better separation and better crystallization of the NC structures.

  15. Low-Temperature Reverse Microemulsion Synthesis, Characterization, and Photocatalytic Performance of Nanocrystalline Titanium Dioxide

    Directory of Open Access Journals (Sweden)

    Zhang Liu

    2012-01-01

    Full Text Available Nanocrystalline titanium dioxide (TiO2 was synthesized in microemulsions by using cetyltrimethylammonium bromide (CTAB as surfactant. In order to investigate the crystal transformation and photoactivity at low temperature, the as-prepared precipitates were aged at 65°C or calcined at various temperatures. Analyses using powder X-ray diffraction (XRD and Fourier transform infrared microscopy (FT-IR showed that precursors without aging or calcination were noncrystal and adsorbed by surfactant. After aging for 6 h, the amorphous TiO2 began to change into anatase. The obtained catalysts, which were synthesized in microemulsions with weight ratios of n-hexanol/CTAB/water as 6 : 3 : 1 and calcined at 500°C, presented the highest photocatalytic degradation rate on methyl orange (MO, while the catalysts, which were aged at 65°C for 90 h, also exhibited an outstanding photocatalytic performance and a little higher than that of the commercial titania photocatalyst Degussa P25.

  16. Room temperature synthesis of PbSe quantum dots in aqueous solution: Stabilization by interactions with ligands

    Science.gov (United States)

    Primera-Pedrozo, Oliva M.; Arslan, Zikri; Rasulev, Bakhtiyor; Leszczynski, Jerzy

    2011-01-01

    An aqueous route of synthesis is described for rapid synthesis of lead selenide quantum dots (PbSe QDs) at room temperature in an attempt to produce water-soluble and stable nanocrystals. Several thiol-ligands, including thioglycolic acid (TGA), thioglycerol (TGC), 3-mercaptopropionic acid (MPA), 2-mercaptoethyleamine hydrochloride (MEA), 6-mercaptohexanoic acid (MHA), and L-cysteine (L-cys), were used for capping/stabilization of PbSe QDs. The effects of the ligands on the stability of PbSe QDs were evaluated for a period of two months at room temperature under normal light conditions and at 4 °C in dark. The TGA- and MEA-capped QDs exhibited the highest stability prior to purification, almost two months when kept in dark at 4 °C. However, the stability of TGA-capped QDs was reduced substantially after purification to about 5 days under same conditions, while MEA-capped QDs did not show any significant instability. The stabilization energies of Pb-thiolate complexes determined by theoretical DFT simulations supported the experimental results. The PbSe QDs capped with TGA, MPA and MEA were successfully purified and re-dispersed in water, while those stabilized with TGC, MHA and L-cys aggregated during purification attempts. The purified PbSe QDs possess very susceptible surface resulting in poor stability for about 30 – 45 min after re-dispersion in water. In the presence of an excess of free ligand, the stability increased up to 5 days for TGA-capped QDs at pH 7.19, 9 –12 days for MPA-capped QDs at pH 7.3–7.5 and 45–47 days for MEA-capped QDs at pH 7.35. X-Ray Diffraction (XRD) results showed that the QDs possess a cubic rock salt structure with the most intense peaks located at 2θ = 25.3° (200) and 2θ = 29.2° (100). TEM images showed that the size of the QDs ranges between 5 and 10 nm. ICP-MS results revealed that Pb:Se ratio was 1.26, 1.28, 3.85, 1.18, and 1.31 for the QDs capped with TGA, MPA, MEA, L-Cys, and TGC, respectively. The proposed method

  17. Development of CaO-swelling cements for cementing of natural gas underground storage wells in field trial (temperature range {<=} 60 C) and composition of CaO and MgO-swelling cements for a temperature range between 60 C-105 C. Final report; Entwicklung von CaO-Quellzementen fuer die Zementation von Erdgasspeicherbohrungen im Feldversuch (Temperaturbereich {<=} 60 C) sowie Formulierung von CaO- und MgO-Quellzementen fuer den Einsatz im Temperaturbereich 60 C-105 C. Abschlussbericht

    Energy Technology Data Exchange (ETDEWEB)

    Ghofrani, R.; Gheorghiu, A.S.; Radu, G.; Rogojinoiu, E.; Stan, M.; Miehe, H.

    2000-11-01

    The investigations conducted within the scope of this project are a consistent continuation of the work already performed at ITE, especially DGMK research projects 444-1, 444-2 and 444-3. These investigations should lead to a field trial of selected CaO-swelling cement recipes. Essential parameters examined within the course of this project include the HPHT-consistency behavior, HPHT-expansion behavior and the long-term stability behavior of CaO-swelling cements under similar conditions to those prevailing in the borehole. The swelling cement will be made up in correlation with the appropriate industrial make up method using the ITE-equipment; in accordance to the borehole conditions, the swelling cement slurry will be then treated in the ITE-Circulating Facility with respect to shear, temperature and pressure. The cement slurry treated in the ITE-Circulating Facility in accordance to the borehole conditions will be then experimentally investigated regarding the HPHT-consistency behavior and HPHT-expansion behavior. With respect to the long-term stability the swelling cement slurry treated in the Circulating Facility will be cured in autoclaves under appropriate pT-conditions. After evacuation from the autoclaves the compressive strength, the shear strength and the system permeability of the samples will be measured. With respect to the properties of a CaO-reference swelling cement recipe measured under the same experimental conditions, the ITE-make up method has been correlated to the common industrial make up methods LPHM, LPRM and HPRM; the alignment of the ITE-make up method with the planned industrial make up method for an appropriate cement job should make sure that the properties of a swelling cement measured in lab will be of practice relevance. For filling in and annular cementing of selected boreholes CaO-swelling cement recipes have been composed, optimized after experimental investigation results, and ultimately released to field usage after the results

  18. A handheld low temperature atmospheric pressure air plasma gun for nanomaterial synthesis in liquid phase

    Energy Technology Data Exchange (ETDEWEB)

    Yu, Shuang; Wang, Kaile; Zuo, Shasha; Liu, Jiahui [Academy for Advanced Interdisciplinary Studies, Peking University, Beijing 100871 (China); Zhang, Jue, E-mail: zhangjue@pku.edu.cn; Fang, Jing [Academy for Advanced Interdisciplinary Studies, Peking University, Beijing 100871 (China); College of Engineering, Peking University, Beijing 100871 (China)

    2015-10-15

    A handheld low temperature atmospheric pressure air plasma gun based on a dielectric barrier structure with hollow electrodes was proposed. The portable plasma gun with an embedded mini air pump was driven by a 12 V direct voltage battery. The air plasma jet generated from the gun could be touched without a common shock hazard. Besides working in air, the plasma gun can also work in water. The diagnostic result of optical emission spectroscopy showed the difference in reactive species of air plasma jet between in air and in water. The plasma gun was excited in 20 ml chloroauric acid aqueous solution with a concentration of 1.214 mM. A significant amount of gold nanoparticles were synthesized after 2 min continuous discharge. The plasma gun with these unique features is applicable in plasma medicine, etching, and s-nthesis of nanomaterials.

  19. Room-temperature synthesis and characterization of porous CeO{sub 2} thin films

    Energy Technology Data Exchange (ETDEWEB)

    Chu, Dewei; Masuda, Yoshitake; Ohji, Tatsuki; Kato, Kazumi [National Institute of Advanced Industrial Science and Technology (AIST), Anagahora, Shimoshidami, Moriyama-ku, Nagoya (Japan)

    2012-01-15

    CeO{sub 2} thin films with hexagonal-shaped pores were successfully prepared by a facile electrodeposition at room temperature combined with an etching process. By using electrodeposited ZnO nanorods as a soft template, the morphology, and microstructure of the CeO{sub 2} could be controlled. TEM observation indicated that as-prepared CeO{sub 2} film is composed of nanocrystals with average size of several nanometers, while XPS analysis showed the coexistence of Ce{sup 3+} and Ce{sup 4+} in the film. The photoluminescence properties of CeO{sub 2} films were measured, which showed much higher sensitivity compared to bare substrate. (Copyright copyright 2012 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  20. Room-temperature synthesis and characterization of porous CeO2 thin films

    International Nuclear Information System (INIS)

    Chu, Dewei; Masuda, Yoshitake; Ohji, Tatsuki; Kato, Kazumi

    2012-01-01

    CeO 2 thin films with hexagonal-shaped pores were successfully prepared by a facile electrodeposition at room temperature combined with an etching process. By using electrodeposited ZnO nanorods as a soft template, the morphology, and microstructure of the CeO 2 could be controlled. TEM observation indicated that as-prepared CeO 2 film is composed of nanocrystals with average size of several nanometers, while XPS analysis showed the coexistence of Ce 3+ and Ce 4+ in the film. The photoluminescence properties of CeO 2 films were measured, which showed much higher sensitivity compared to bare substrate. (Copyright copyright 2012 WILEY-VCH Verlag GmbH and Co. KGaA, Weinheim)

  1. Synthesis, ionic conductivity, and thermal properties of proton conducting polymer electrolyte for high temperature fuel cell

    Energy Technology Data Exchange (ETDEWEB)

    Itoh, Takahito; Hamaguchi, Yohei; Uno, Takahiro; Kubo, Masataka [Department of Chemistry for Materials, Faculty of Engineering, Mie University, 1577 Kurima Machiya-cho, Tsu, Mie 514-8507 (Japan); Aihara, Yuichi; Sonai, Atsuo [Samsung Yokohama Research Institute, 2-7 Sugasawa-cho, Tsurumi-ku, Yokohama 230-0027 (Japan)

    2006-01-16

    Hyperbranched polymer (poly-1a) with sulfonic acid groups at the end of chains was successfully synthesized. Interpenetration reaction of poly-1a with a hyperbranched polymer with acryloyl groups at the end of chains (poly-1b) as a cross-linker afforded a tough electrolyte membrane. The poly-1a and the resulting electrolyte membrane showed the ionic conductivities of 7x10{sup -4} and 8x10{sup -5} S/cm, respectively, at 150C under dry condition. The ionic conductivities of the poly-1a and the electrolyte membrane exhibited the VTF type temperature dependence. And also, both poly-1a and the resulting electrolyte membrane were thermally stable up to 200C. (author)

  2. Synthesis of hydrogen-carbon clathrate material and hydrogen evolution therefrom at moderate temperatures and pressures

    Science.gov (United States)

    Lueking, Angela [State College, PA; Narayanan, Deepa [Redmond, WA

    2011-03-08

    A process for making a hydrogenated carbon material is provided which includes forming a mixture of a carbon source, particularly a carbonaceous material, and a hydrogen source. The mixture is reacted under reaction conditions such that hydrogen is generated and/or released from the hydrogen source, an amorphous diamond-like carbon is formed, and at least a portion of the generated and/or released hydrogen associates with the amorphous diamond-like carbon, thereby forming a hydrogenated carbon material. A hydrogenated carbon material including a hydrogen carbon clathrate is characterized by evolution of molecular hydrogen at room temperature at atmospheric pressure in particular embodiments of methods and compositions according to the present invention.

  3. Ultrafine ferromagnetic iron oxide nanoparticles: Facile synthesis by low temperature decomposition of iron glycerolate

    Energy Technology Data Exchange (ETDEWEB)

    Bartůněk, Vilém, E-mail: vilem.bartunek@vscht.cz [Department of Inorganic Chemistry, Faculty of Chemical Technology, University of Chemistry and Technology, Technická 5, 166 28 Prague 6 (Czech Republic); Průcha, David [Department of Inorganic Chemistry, Faculty of Chemical Technology, University of Chemistry and Technology, Technická 5, 166 28 Prague 6 (Czech Republic); Švecová, Marie [Department of Analytical Chemistry, Faculty of Chemical Engineering, University of Chemistry and Technology, Technická 5, 166 28 Prague 6 (Czech Republic); Ulbrich, Pavel [Department of Biochemistry and Microbiology, Faculty of Food and Biochemical Technology, University of Chemistry and Technology, Technická 3, 166 28 Prague 6 (Czech Republic); Huber, Štěpán; Sedmidubský, David; Jankovský, Ondřej [Department of Inorganic Chemistry, Faculty of Chemical Technology, University of Chemistry and Technology, Technická 5, 166 28 Prague 6 (Czech Republic)

    2016-09-01

    We synthesized dark colored ultrafine – sub 10 nm iron oxide nanoparticles by a facile and low temperature process based on thermal decomposition of an affordable precursor – iron glycerolate. Simultaneous thermal analysis (STA) was used to study the thermal behaviour during the decomposition. The iron glycerolate was thoroughly analysed by various methods. The size of the iron nanoparticles was determined from XRD patterns and by transmission electron microscopy (TEM) and their composition has been confirmed by XPS. Magnetic properties of the nanoparticles were studied by vibrating sample magnetometry. The prepared single phase material exhibiting ferromagnetic properties is usable in a wide range of applications and may be suitable even for large scale industrial applications. - Highlights: • Iron glycerolate prepared and characterised. • Iron oxide nanoparticles prepared by thermal decomposition of iron glycerolate. • STA used to study the decomposition. • Products characterised by XRD, XPS, FT-IR, SEM and TEM. • Magnetic behaviour of monophasic samples determined.

  4. Room-Temperature Synthesis of Ni Nanoparticles as the Absorbent Used for Sewage Treatment

    Directory of Open Access Journals (Sweden)

    Genhua Zhang

    2015-01-01

    Full Text Available The magnetic Ni nanoparticles of 10–30 nm in size were synthesized by the reduction of Ni2+ by NaBH4 at room temperature. The amount of added water in the formation of Ni nanoparticles is a significant factor, which ensures that Ni nanoparticles are not oxidized by oxygen. XRD patterns and FESEM micrographs showed the constituent and structure and micromorphology. Congo red was used as adsorbate to quantitatively examine the adsorption capability of Ni nanoparticles for the organic dyes in industry wastewater. The magnetic hysteresis measurement indicated that the Ni nanoparticles presented ferromagnetic properties. The experimental results showed the as-obtained Ni nanoparticles might be a potential adsorbent in sewage treatment process.

  5. 'Green' synthesis of starch capped CdSe nanoparticles at room temperature

    International Nuclear Information System (INIS)

    Li Jinhua; Ren Cuiling; Liu Xiaoyan; Hu Zhide; Xue Desheng

    2007-01-01

    The nearly monodisperse starch capped CdSe nanoparticles were successfully synthesized by a simple and 'green' route at room temperature. The as-prepared nanoparticles were characterized by X-ray diffraction (XRD), transmission electron microscope (TEM), UV-vis absorption and photoluminescence (PL) spectra. The XRD analysis showed that the starch capped CdSe nanoparticles were of the cubic structure, the average particle size was calculated to be about 3 nm according to the Debye-Scherrer equation. TEM micrographs exhibited that the starch capped CdSe nanoparticles were well dispersed than the uncapped CdSe nanoparticles, the mean particles size of the capped CdSe was about 3 nm in the TEM image, which was in good agreement with the XRD

  6. Self propagating high temperature synthesis of mixed carbide and boride powder systems for cutting tools manufacturing

    International Nuclear Information System (INIS)

    Vallauri, D.; Cola, P.L. de; Piscone, F.; Amato, I.

    2001-01-01

    TiC-TiB 2 composites have been produced via SHS technique starting from low cost raw materials like TiO 2 , B 4 C, Mg. The influence of the diluent phase (Mg, TiC) content on combustion temperature has been investigated. The use of magnesium as the reductant phase allowed acid leaching of the undesired oxide product (MgO), leaving pure hard materials with fine particle size suitable to be employed in cutting tools manufacturing through cold pressing and sintering route. The densification has shown to be strongly dependent on the wetting additions. The influence of the metal binder and wetting additions on the sintering process has been investigated. A characterization of the obtained materials was performed by the point of view of cutting tools life (hardness, toughness, strength). (author)

  7. Room temperature synthesis of a Zn(II) metal-organic coordination polymer for dye removal

    Science.gov (United States)

    Abbasi, Alireza; Gharib, Maniya; Najafi, Mahnaz; Janczak, Jan

    2016-03-01

    A new one-dimensional (1D) coordination polymer, [Zn(4,4‧-bpy)(H2O)4](ADC)·4H2O (1) (4,4‧-bpy=4,4‧-bipyridine and H2ADC=acetylenedicarboxylic acid), was synthesized at room temperature. The crystal structure of the coordination polymer was determined by single-crystal X-ray diffraction analysis. Compound 1 was also characterized by FT-IR, powder X-ray diffraction (PXRD) and thermogravimetric analysis (TGA). The catalytic activity of 1 was evaluated in the color removal of Bismarck brown as a representative of dye pollutant in water under mild conditions. Coordination polymer 1 exhibited good catalytic activity and stability in the decolorization of Bismarck brown and could be easily recovered and reused for at least three cycles.

  8. Kinetics and mechanism of the low-temperature yttrium-aluminium garnet synthesis

    International Nuclear Information System (INIS)

    Ivakin, Yu.D.; Danchevskaya, M.N.; Yanchenko, P.A.; Murav'eva, G.P.

    2000-01-01

    Kinetics and formation mechanism of finely crystalline yttrium-aluminium garnet (YAG) during hydrothermal and hot steam treatment of stoichiometric mixture of oxides in the range of temperature 200-400 Deg C and pressures of 1.5-26 MPa were studied. It is ascertained that formation of YAG occurs via intermediate stage of Y(OH) 3 structure formation, whereas the aluminia component is X-ray amorphous. Kinetics of YAG formation is described by the equation of solid phase transformation with the limiting stage of nucleation. The YAG formed contains 7-5 % of water, which corresponds to hydrogarnet structure. Unit cell parameters of the YAG samples synthesized are somewhat high and after heating up to 1200 Deg C they decrease [ru

  9. Room-temperature Synthesis of Amorphous Molybdenum Oxide Nanodots with Tunable Localized Surface Plasmon Resonances.

    Science.gov (United States)

    Zhu, Chuanhui; Xu, Qun; Ji, Liang; Ren, Yumei; Fang, Mingming

    2017-12-05

    Two-dimensional (2D) semiconductors have recently emerged as a remarkable class of plasmonic alternative to conventional noble metals. However, tuning of their plasmonic resonances towards different wavelengths in the visible-light region with physical or chemical methods still remains challenging. In this work, we design a simple room-temperature chemical reaction route to synthesize amorphous molybdenum oxide (MoO 3-x ) nanodots that exhibit strong localized surface plasmon resonances (LSPR) in the visible and near-infrared region. Moreover, tunable plasmon resonances can be achieved in a wide range with the changing surrounding solvent, and accordingly the photoelectrocatalytic activity can be optimized with the varying LSPR peaks. This work boosts the light-matter interaction at the nanoscale and could enable photodetectors, sensors, and photovoltaic devices in the future. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

  10. Room temperature synthesis of heptazine-based microporous polymer networks as photocatalysts for hydrogen evolution.

    Science.gov (United States)

    Kailasam, Kamalakannan; Schmidt, Johannes; Bildirir, Hakan; Zhang, Guigang; Blechert, Siegfried; Wang, Xinchen; Thomas, Arne

    2013-06-25

    Two emerging material classes are combined in this work, namely polymeric carbon nitrides and microporous polymer networks. The former, polymeric carbon nitrides, are composed of amine-bridged heptazine moieties and showed interesting performance as a metal-free photocatalyst. These materials have, however, to be prepared at high temperatures, making control of their chemical structure difficult. The latter, microporous polymer networks have received increasing interest due to their high surface area, giving rise to interesting applications in gas storage or catalysis. Here, the central building block of carbon nitrides, a functionalized heptazine as monomer, and tecton are used to create microporous polymer networks. The resulting heptazine-based microporous polymers show high porosity, while their chemical structure resembles the ones of carbon nitrides. The polymers show activity for the photocatalytic production of hydrogen from water, even under visible light illumination. Copyright © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  11. Low Temperature Synthesis of Metal Oxides by a Supercritical Seed Enhanced Crystallization (SSEC) Process

    DEFF Research Database (Denmark)

    Jensen, Henrik; Brummerstedt Iversen, Steen; Joensen, Karsten Dan

    2006-01-01

    A novel method for producing crystalline nanosized metal oxides by a Supercritical Seed Enhanced Crystallization (SSEC) Process has been developed. The process is a modified sol-gel process taking place at temperatures as low as 95 ºC with supercritical CO2 as solvent and polypropylene as seeding...... material. The nanocrystalline product is obtained without having to resort to costly post-reaction processing and the product is obtained directly after the SSEC process. TiO2 powders produced by the SSEC process were shown to have a crystallinity of 60 % and a crystal size of 7.3 ± 2.6 nm....... The crystallinity can be controlled by changing the heating rate of the initial formation of the nanoparticles and the morphology can be altered by changing the process time....

  12. In situ synthesis of manganese oxides on polyester fiber for formaldehyde decomposition at room temperature

    International Nuclear Information System (INIS)

    Wang, Jinlong; Yunus, Rizwangul; Li, Jinge; Li, Peilin; Zhang, Pengyi; Kim, Jeonghyun

    2015-01-01

    Graphical abstract: - Highlights: • The MnO x particles assembled with nanosheets were uniformly coated on PET fibers. • The growth process of MnO x layer on PET is clearly clarified. • MnO x /PET showed good activity for HCHO decomposition at room temperature. • MnO x /PET material is promising for indoor air purification due to its light, flexible and low air-resistant properties. - Abstract: Removal of low-level formaldehyde (HCHO) is of great interest for indoor air quality improvement. Supported materials especially those with low air pressure drop are of necessity for air purification. Manganese oxides (MnO x ) was in situ deposited on the surface of fibers of a non-woven fabric made of polyethylene terephthalate (PET). As-synthesized MnO x /PET were characterized by SEM, XRD, TEM, ATR-FTIR and XPS analysis. The growth of MnO x layer on PET is thought to start with partial hydrolysis of PET, followed by surface oxidation by KMnO 4 and then surface-deposition of MnO x particles from the bulk phase. The MnO x particles assembled with nanosheets were uniformly coated on the PET fibers. MnO x /PET showed good activity for HCHO decomposition at room temperature which followed the Mars–van Krevelen mechanism. The removal of HCHO was kept over 94% after 10 h continuous reaction under the conditions of inlet HCHO concentration ∼0.6 mg/m 3 , space velocity ∼17,000 h −1 and relative humidity∼50%. This research provides a facile method to deposit active MnO x onto polymers with low air resistance, and composite MnO x /PET material is promising for indoor air purification.

  13. In situ synthesis of manganese oxides on polyester fiber for formaldehyde decomposition at room temperature

    Energy Technology Data Exchange (ETDEWEB)

    Wang, Jinlong [State Key Joint Laboratory of Environment Simulation and Pollution Control, School of Environment, Tsinghua University, Beijing 100084 (China); Collaborative Innovation Center for Regional Environmental Quality (China); Yunus, Rizwangul [State Key Joint Laboratory of Environment Simulation and Pollution Control, School of Environment, Tsinghua University, Beijing 100084 (China); Xinjiang Zhongtai Chemical Company, Xinjiang 831511 (China); Li, Jinge; Li, Peilin [State Key Joint Laboratory of Environment Simulation and Pollution Control, School of Environment, Tsinghua University, Beijing 100084 (China); Zhang, Pengyi, E-mail: zpy@tsinghua.edu.cn [State Key Joint Laboratory of Environment Simulation and Pollution Control, School of Environment, Tsinghua University, Beijing 100084 (China); Collaborative Innovation Center for Regional Environmental Quality (China); Kim, Jeonghyun [State Key Joint Laboratory of Environment Simulation and Pollution Control, School of Environment, Tsinghua University, Beijing 100084 (China); Collaborative Innovation Center for Regional Environmental Quality (China)

    2015-12-01

    Graphical abstract: - Highlights: • The MnO{sub x} particles assembled with nanosheets were uniformly coated on PET fibers. • The growth process of MnO{sub x} layer on PET is clearly clarified. • MnO{sub x}/PET showed good activity for HCHO decomposition at room temperature. • MnO{sub x}/PET material is promising for indoor air purification due to its light, flexible and low air-resistant properties. - Abstract: Removal of low-level formaldehyde (HCHO) is of great interest for indoor air quality improvement. Supported materials especially those with low air pressure drop are of necessity for air purification. Manganese oxides (MnO{sub x}) was in situ deposited on the surface of fibers of a non-woven fabric made of polyethylene terephthalate (PET). As-synthesized MnO{sub x}/PET were characterized by SEM, XRD, TEM, ATR-FTIR and XPS analysis. The growth of MnO{sub x} layer on PET is thought to start with partial hydrolysis of PET, followed by surface oxidation by KMnO{sub 4} and then surface-deposition of MnO{sub x} particles from the bulk phase. The MnO{sub x} particles assembled with nanosheets were uniformly coated on the PET fibers. MnO{sub x}/PET showed good activity for HCHO decomposition at room temperature which followed the Mars–van Krevelen mechanism. The removal of HCHO was kept over 94% after 10 h continuous reaction under the conditions of inlet HCHO concentration ∼0.6 mg/m{sup 3}, space velocity ∼17,000 h{sup −1} and relative humidity∼50%. This research provides a facile method to deposit active MnO{sub x} onto polymers with low air resistance, and composite MnO{sub x}/PET material is promising for indoor air purification.

  14. Simonkolleite nano-platelets: Synthesis and temperature effect on hydrogen gas sensing properties

    Energy Technology Data Exchange (ETDEWEB)

    Sithole, J. [NANOAFNET, MRD-iThemba LABS, National Research Foundation,1 Old Faure road, Somerset West 7129 (South Africa); Dept. of Physics, University of Western Cape, Private Bag X 17, Belleville (South Africa); Ngom, B.D., E-mail: bdngom@tlabs.ac.za [NANOAFNET, MRD-iThemba LABS, National Research Foundation,1 Old Faure road, Somerset West 7129 (South Africa) and African Laser Centre, CSIR campus, P.O. Box 395, Pretoria (South Africa); Laboratoire de Photonique et de Nano-Fabrication, Groupe de Physique du Solide et Sciences des Materiaux, Departement de Physique Facultes des Sciences et Technique Universite Cheikh Anta Diop de Dakar, Dakar (Senegal); Khamlich, S. [NANOAFNET, MRD-iThemba LABS, National Research Foundation,1 Old Faure road, Somerset West 7129 (South Africa); African Laser Centre, CSIR campus, P.O. Box 395, Pretoria (South Africa); Manikanadan, E. [National Centre for Nano-Structured Materials (NCNSM), Council for Scientific and Industrial Research, Pretoria (South Africa); Manyala, N. [Department of Physics, SARCHI Chair in Carbon Technology and Materials, Institute of Applied Materials, University of Pretoria, Pretoria 0028 (South Africa); Saboungi, M.L. [Centre de Recherche sur la Matiere Divisee, CNRS-Orleans, Orleans (France); Knoessen, D. [Dept. of Physics, University of Western Cape, Private Bag X 17, Belleville (South Africa); Nemutudi, R.; Maaza, M. [NANOAFNET, MRD-iThemba LABS, National Research Foundation,1 Old Faure road, Somerset West 7129 (South Africa)

    2012-08-01

    In this work, the new refined mineral platelets-like morphology of simonkolleite based particles described by Shemetzer et al. (1985) were synthesized in zinc nitrate aqueous solution by a moderate solution process. The morphological and structural properties of the platelets-like Zn{sub 5}(OH){sub 8}Cl{sub 2}{center_dot}H{sub 2}O were characterized by scanning electron microscope energy dispersed X-ray spectroscopy, transmission electron microscope, powder X-ray diffraction and selected area electron diffraction as well as attenuated total reflection infrared spectroscopy. The morphology as well as the size in both basal and transversal directions of the simonkolleite Zn{sub 5}(OH){sub 8}Cl{sub 2}{center_dot}H{sub 2}O nano/micro crystals was found to be significantly depending on the specific concentration of 0.1 M of Zn{sup 2+}/Cl{sup -} ions in the precursor solution. The simonkolleite Zn{sub 5}(OH){sub 8}Cl{sub 2}{center_dot}H{sub 2}O nano-platelets revealed a significant and singular H{sub 2} gas sensing characteristics. The operating temperature was found to play a key role on the sensing properties of simonkolleite. The effect of temperature on the simonkolleite sample as a hydrogen gas sensor was studied by recording the change in resistivity of the film in presence of the test gas. The results on the sensitivity and response time as per comparison to earlier reported ZnO based sensors are indicated and discussed.

  15. Candida antartica lipase B catalyzed polycaprolactone synthesis: effects of organic media and temperature.

    Science.gov (United States)

    Kumar, A; Gross, R A

    2000-01-01

    Engineering of the reaction medium and study of an expanded range of reaction temperatures were carried out in an effort to positively influence the outcome of Novozyme-435 (immobilized Lipase B from Candida antarctica) catalyzed epsilon-CL polymerizations. A series of solvents including acetonitrile, dioxane, tetrahydrofuran, chloroform, butyl ether, isopropyl ether, isooctane, and toluene (log P from -1.1 to 4.5) were evaluated at 70 degrees C. Statistically (ANOVA), two significant regions were observed. Solvents having log P values from -1.1 to 0.49 showed low propagation rates (< or = 30% epsilon-CL conversion in 4 h) and gave products of short chain length (Mn < or = 5200 g/mol). In contrast, solvents with log P values from 1.9 to 4.5 showed enhanced propagation rates and afforded polymers of higher molecular weight (Mn = 11,500-17,000 g/mol). Toluene, a preferred solvent for this work, was studied at epsilon-CL to toluene (wt/vol) ratios from 1:1 to 10:1. The ratio 1:2 was selected since, for polymerizations at 70 degrees C, 0.3 mL of epsilon-CL and 4 h, gave high monomer conversions and Mn values (approximately 85% and approximately 17,000 g/mol, respectively). Increasing the scale of the reaction from 0.3 to 10 mL of CL resulted in a similar isolated product yield, but the Mn increased from 17,200 to 44,800 g/mol. Toluene appeared to help stabilize Novozyme-435 so that lipase-catalyzed polymerizations could be conducted effectively at 90 degrees C. For example, within only 2 h at 90 degrees C (toluene-d8 to epsilon-CL, 5:1, approximately 1% protein), the % monomer conversion reached approximately 90%. Also, the controlled character of these polymerizations as a function of reaction temperature was evaluated.

  16. CuSn(OH)6 submicrospheres: Room-temperature synthesis, growth mechanism, and weak antiferromagnetic behavior

    International Nuclear Information System (INIS)

    Zhong, Sheng-Liang; Xu, Rong; Wang, Lei; Li, Yuan; Zhang, Lin-Fei

    2011-01-01

    Highlights: ► CuSn(OH) 6 spheres have been synthesized via an aqueous solution method at room temperature. ► The diameters of the CuSn(OH) 6 spheres can be tuned by adjusting the molar ratio of SnO 3 2− to Cu 2+ . ► The as-obtained CuSn(OH) 6 spheres are antiferromagnetic and have a weak spin-Peierls transition at about 78 K -- Abstract: CuSn(OH) 6 submicrospheres with diameters of 400–900 nm have been successfully fabricated using a simple aqueous solution method at room temperature. Influencing factors such as the dosage of reactants and reaction time on the preparation were systematically investigated. The products were characterized with X-ray diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), transmission electron microscopy (TEM), thermogravimetric analysis (TG) and differential thermal analysis (DTA). Results reveal that the CuSn(OH) 6 spheres are built from numerous nanoparticles. It is found that the diameter of CuSn(OH) 6 spheres can be readily tuned by adjusting the molar ratio of SnO 3 2− to Cu 2+ . A possible growth mechanism for the CuSn(OH) 6 submicrospheres has been proposed. Amorphous CuSnO 3 submicrospheres were obtained after thermal treatment of the CuSn(OH) 6 submicrospheres at 300 °C for 4 h. Standard magnetization measurements demonstrate that the CuSn(OH) 6 submicrospheres are antiferromagnetic and have a weak spin-Peierls transition at about 78 K.

  17. Depression of leukocyte protein synthesis, immune function and growth performance induced by high environmental temperature in broiler chickens

    Science.gov (United States)

    Kamel, Nancy N.; Ahmed, Ayman M. H.; Mehaisen, Gamal M. K.; Mashaly, Magdi M.; Abass, Ahmed O.

    2017-09-01

    In tropical and semitropical regions, raising broiler chickens out of their thermal comfort zone can cause an added economic loss in the poultry industry. The cause for the deleterious effects on immunity and growth performance of broilers under high environmental temperatures is still poorly understood. Therefore, the aim of the current investigation was to evaluate the effect of heat stress on leukocytes protein synthesis and immune function as a possible direct cause of low performance in broiler chickens under such condition. In this study, 300 one-day-old male broiler chicks (Cobb500™) were randomly assigned into 2 groups with 5 replicates of 30 chicks each. From 21 to 42 days of age, one group was exposed to non-stressed condition at 24 °C and 50% relative humidity (control group), while the other group was exposed to heat stress at 35 °C and 50% relative humidity (HS group). At 42 days of age, blood samples were collected from each group to evaluate stress indicators, immune function, and leukocytes protein synthesis. Production performance was also recorded. Noteworthy, protein synthesis in leukocytes was significantly ( P < 0.05) inhibited in HS group by 38% compared to control group. In contrast, the phosphorylation level on threonine 56 site (Thr56) of eukaryotic elongation factor (eEF2), which indicates the suppression of protein translation process through altering the protein elongation phase, was significantly threefold higher in HS group than in control ( P < 0.05). In addition, an increase in stress indicators was markedly ( P < 0.05) presented in the HS birds by twofold increase in heterophil/lymphocyte (H/L) ratio and threefold increase in plasma corticosterone level compared to control. Furthermore, the immune function was significantly ( P < 0.05) suppressed in HS birds than control (0.99 vs. 1.88 mg/mL plasma IgG, 89.2 vs. 148.0 μg/mL plasma IgM, 4.80 vs. 7.20 antibody titer against SRBC, and 1.38 vs. 3.39 stimulation index of lymphocyte

  18. 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

  19. The Effect of CaO and MgO as Expanding Additives to Improve Cement Isolation Strength under HPHT Exposure

    Directory of Open Access Journals (Sweden)

    Rudi Rubiandini

    2005-05-01

    Full Text Available Cementing is one of the most important parts in oil-well drilling. Recent development in oil-well drilling technology has led to a more problematic case in cementing. High temperature cementing is one of the problems. High temperature cementing may cover steam recovery wells, geothermal wells and ultra deep wells.The use of expanding cements as an effort to improve the sealing efficacy of annulus cementing has been considered for a long time as a promising solution to the existing problems. CaO and MgO have been proposed as two of the most effective additives to create excellent expanding cement. The purpose of this study is to find the effect of adding up burnt pure CaO and MgO to the value of compressive strength and shear bond strength of API class G cement in high pressure and high temperature condition. The method that we used within this research is an evaluation of the data taken from a simulator that simulated within temperature range of 100 – 250oC and pressure of 2000 psi.The conclusion is taken according to the results which saying that the addition of burnt pure CaO and MgO would increase the shear bond strength and the compressive strength on specific condition up to 200oC temperature. The addition won’t be effective for the condition of 250oC temperature. The behavior of cement strength was also influenced by the length of curing time.Further more, research on expanding cement needs to be developed and extended whether to vary its compositions, temperatures, or curing time conditions. The compatibility when mixed with other additives together with silica flour has not yet been figured out.

  20. Hydrothermal Synthesis of Zeolite from Coal Class F Fly Ash. Influence of Temperature

    Directory of Open Access Journals (Sweden)

    Goñi, S.

    2010-06-01

    Full Text Available The influence of temperature of alkaline hydrothermal treatment on the conversion in zeolite of Spanish coal low calcium-fly ash (ASTM class F is presented in this work. Zeolite Na-P1 gismondine type (Na6Al6Si10O32.12H2O was formed at the temperature of 100ºC, which transformed in zeolite; analcime-C type (Na(Si2AlO6H2O and sodalite (1.08 Na2O.Al2O3.1.68SiO2.1.8H2O at 200ºC together with traces of tobermorite-11Å (Ca5(OH2Si6O16.4H2O. At this temperature the 100% of the fly ash reaction was allowed. An equivalent study was carried out in water as reference. The zeolite conversion of the fly ash was characterized by X ray diffraction (XRD, FT infrared (FTIR spectroscopy, surface area (BET-N2 and thermal analyses.

    En este trabajo se presenta el papel que juega la temperatura durante el tratamiento hidrotermal en medio alcalino para convertir una ceniza volante de bajo contenido en cal (clase F, según la norma ASTM en zeolita. Durante este tratamiento a la temperatura de 100ºC se forma Zeolita Na-P1 tipo gismondina (Na6Al6Si10O32.12H2O; al elevar la temperatura a 200ºC, dicha zeolita se transforma en zeolita Analcima C (Na(Si2AlO6H2O y en fase sodalita (1.08 Na2O.Al2O3.1.68SiO2.1.8H2O junto con trazas de tobermorita-11Å (Ca5(OH2Si6O16.4H2O. A esta temperatura y en estas condiciones se ha conseguido un 100% de reacción. Un estudio equivalente se ha llevado a cabo empleando agua como medio de referencia. La conversión de ceniza volante en zeolita se ha caracterizado mediante técnicas, como difracción de Rayos X (DRX, espectroscopia

  1. Low temperature synthesis of nanocrystalline lanthanum monoaluminate powders by chemical coprecipitation

    Energy Technology Data Exchange (ETDEWEB)

    Kuo, C.-L. [Department of Materials Science and Engineering, National Cheng Kung University, 1 Ta-Hsueh Road, Tainan 70101, Taiwan (China); Wang, C.-L. [Department of Materials Science and Engineering, I-Shou University, 1 Section 1, Hsueh-Cheng Road, Ta-Hsu Hsiang, Kaohsiung 840, Taiwan (China); Chen, T.-Y. [Department of Materials Science and Engineering, National Cheng Kung University, 1 Ta-Hsueh Road, Tainan 70101, Taiwan (China); Chen, G.-J. [Department of Materials Science and Engineering, I-Shou University, 1 Section 1, Hsueh-Cheng Road, Ta-Hsu Hsiang, Kaohsiung 840, Taiwan (China); Hung, I-M. [Department of Chemical Engineering and Materials Science, Yuan Ze University, 135 Yuan-Tung Road, Chungli, Taoyuan 320, Taiwan (China); Shih, C.-J. [Faculty of Fragrance and Cosmetics, Kaohsiung Medical University, 100 Shi-Chuan 1st Road, Kaohsiung 807, Taiwan (China)]. E-mail: CJShih@kmu.edu.tw; Fung, K.-Z. [Department of Materials Science and Engineering, National Cheng Kung University, 1 Ta-Hsueh Road, Tainan 70101, Taiwan (China)

    2007-08-16

    Nanocrystalline lanthanum monoaluminate (LaAlO{sub 3}) powders were prepared by chemical coprecipitation using 25 vol.% of NH{sub 4}OH, 0.05 M La(NO{sub 3}){sub 3}.6H{sub 2}O and 0.05 M Al(NO{sub 3}){sub 3}.9H{sub 2}O aqueous solutions as the starting materials. Fourier transform infrared spectroscopy (FT-IR), thermogravimetric and differential thermal analyses (TGA/DTA), X-ray diffraction (XRD), Raman spectrometry, specific surface area (BET) analysis, scanning electron microscopy (SEM), transmission electron microscopy (TEM) and electron diffraction (ED) were utilized to characterize the LaAlO{sub 3} powders prepared by chemical coprecipitation. The crystallization temperature of the LaAlO{sub 3} precursor gels precipitated at pH 9 is estimated as 810 deg. C by TG/DTA. The XRD pattern of the LaAlO{sub 3} precursor gels precipitated at pH 8-12 and calcined at 700 deg. C for 6 h shows a broad arciform continuum exist between 24{sup o} and 32{sup o} and sharp peaks of LaAlO{sub 3} except the precursor gels precipitated at pH 9. For the LaAlO{sub 3} precursor gels precipitated at pH 9 and calcined at 700 deg. C for 6 h, the formation of the perovskite LaAlO{sub 3} phase occurs and the presence of crystalline impurities is not found. The crystallite size of LaAlO{sub 3} slightly increases from 37.8 to 41.5 nm with calcination temperature increasing from 700 to 900 deg. C for 6 h. The LaAlO{sub 3} powders prepared by chemical coprecipitation have a considerably large specific surface of 30 m{sup 2}/g. The relative density greater than 97% is obtained when these nanocrystalline LaAlO{sub 3} powders are sintered at 1550 deg. C for 2 h.

  2. Mechano-chemical synthesis K2MF6 (M = Mn, Ni) by cation-exchange reaction at room temperature

    Science.gov (United States)

    Rawat, Pooja; Nagarajan, Rajamani

    2018-02-01

    In order to establish the power of mechanochemistry to produce industrially important phosphors, synthesis of K2MnF6 has been attempted by the successive grinding reactions of manganese (II) acetate with ammonium fluoride and potassium fluoride. The progress of reaction was followed by ex-situ characterization after periodic intervals of time. Cubic symmetry of K2MnF6 was evident from its powder X-ray diffraction pattern which was refined successfully in cubic space group (Fm-3m) with a = 8.4658 (20) Å. Stretching and bending vibration modes of MnF62- octahedral units appeared at 740 and 482 cm-1 in the fourier transformed infrared spectrum. Bands at 405 and 652 cm-1 appeared in the Raman spectrum and they were finger-print positions of cubic K2MnF6. Other than the ligand to metal charge transfer transition at 242 nm, transitions from 4A2g to 4T1g, 4T2g and 2T2g of Mn4+-ion appeared at 352, 429, 474 and 569 nm in the UV-visible diffuse reflectance spectrum of the sample. Red emission due to Mn4+ was observed in the photoluminescence spectrum with a decay time of 0.22 ms. Following the success in forming cubic K2MnF6, this approach has been extended to synthesize cubic K2NiF6 at room temperature. All these results confirmed the susceptibility of acetate salts of transition metals belonging to first-row of the periodic table to facile fluorination at room temperature aided by mechanical forces.

  3. I. The synthesis and characterization of annulated uranocenes. II. The variable temperature 1H NMR of uranocenes

    International Nuclear Information System (INIS)

    Luke, W.D.

    1980-01-01

    A general synthetic route to alkyl annulated cyclooctatetraene dianions and the corresponding annulated uranocenes has been developed. Dideprotonation of bicyclooctatrienes, resulting from reaction of cyclooctatetraene dianion with l,n-dialkylbromides or methanesulfonates, affords alkyl annulated cyclooctatetraene dianions in moderate yields. Dicyclopenteno-, bisdimethylcyclopenteno- and dicyclohexenouranocene were prepared from the corresponding cyclooctatetraene dianions and UCl 4 . The structures of dicyclobuteno- and dicyclopentenouranocene were elucidated by single crystal X-ray diffraction, and the effects of annulation on the uranocene skeleton are discussed. Attempted synthesis of benzocyclooctatetraene and a benzannulated uranocene is reported. The variable temperature 1 H NMR spectrum of uranocene has been reinvestigated from -100 to 100 0 C. The isotropic shift was found to be linear in T -1 with an extrapolated intercept of 0 at T -1 = 0. Variable temperature 1 H NMR spectra, from -80 to 70 0 C, of 17 substituted uranocenes are reported. The energy barrier to ring rotation in 1,1', 4,4'-tetra-t-butyl-uranocene was determined to be 8.24 +- 0.5 kcal/mole while the barrier in the corresponding 1,1', 3,3'-tetra-t-butylferrocene was determined to be 13.1 kcal/mole. Alkyl substitution is shown to have little effect on the electronic and magnetic properties of the uranocene skeleton, and thus alkyl substituted uranocenes are treated as having effective axial symmetry in analysis of the observed isotropic shifts. Using diannulated uranocenes as model systems an analysis of the contact and pseudocontact components of the observed isotropic shifts in uranocene and alkyl substituted uranocenes is presented

  4. Formulation and catalytic performance of MOF-derived Fe@C/Al composites for high temperature Fischer–Tropsch synthesis

    KAUST Repository

    Oar-Arteta, Lide; Valero-Romero, Marí a José ; Wezendonk, Tim; Kapteijn, Freek; Gascon, Jorge

    2017-01-01

    High productivity towards C-2-C-4 olefins together with high catalyst stability are key for optimum operation in high temperature Fischer-Tropsch synthesis (HT-FTS). Here, we report the fabrication of Fe@C/Al composites that combine both the outstanding catalytic properties of the Fe-BTC MOF-derived Fe catalyst and the excellent mechanical resistance and textural properties provided by the inorganic AlOOH binder. The addition of AlOOH to Fe-BTC followed by pyrolysis in N-2 atmosphere at 500 degrees C results in composites with a large mesoporosity, a high Fe/Fe3O4 ratio, 10-35 nm average Fe crystallite size and coordinatively unsaturated Al3+ sites. In catalytic terms, the addition of AlOOH binder gives rise to enhanced C-2-C-4 selectivity and catalyst mechanical stability in HT-FTS, but at high Al contents the activity decreases. Altogether, the productivity of these Fe@C/Al composites is well above most known Fe catalysts for this process.

  5. Synthesis and evaluation of nitroxide-based oligoradicals for low-temperature dynamic nuclear polarization in solid state NMR

    Science.gov (United States)

    Yau, Wai-Ming; Thurber, Kent R.; Tycko, Robert

    2014-07-01

    We describe the synthesis of new nitroxide-based biradical, triradical, and tetraradical compounds and the evaluation of their performance as paramagnetic dopants in dynamic nuclear polarization (DNP) experiments in solid state nuclear magnetic resonance (NMR) spectroscopy with magic-angle spinning (MAS). Under our experimental conditions, which include temperatures in the 25-30 K range, a 9.4 T magnetic field, MAS frequencies of 6.2-6.8 kHz, and microwave irradiation at 264.0 GHz from a 800 mW extended interaction oscillator source, the most effective compounds are triradicals that are related to the previously-described compound DOTOPA-TEMPO (see Thurber et al., 2010), but have improved solubility in glycerol/water solvent near neutral pH. Using these compounds at 30 mM total nitroxide concentration, we observe DNP enhancement factors of 92-128 for cross-polarized 13C NMR signals from 15N,13C-labeled melittin in partially protonated glycerol/water, and build-up times of 2.6-3.8 s for 1H spin polarizations. Net sensitivity enhancements with biradical and tetraradical dopants, taking into account absolute 13C NMR signal amplitudes and build-up times, are approximately 2-4 times lower than with the best triradicals.

  6. Synthesis of metastable A-15 ''Nb3Si'' by ion implantation and on its superconducting transition temperature

    International Nuclear Information System (INIS)

    Clapp, M.T.; Rose, R.M.

    1980-01-01

    The authors have found a new technique for the synthesis of metastable compounds of well-defined composition: namely, ion implantation of a selected element into the desired crystal structure. [M.T. Clapp and R.M. Rose, Appl. Phys. Lett. 33, 205 (1978)]. Starting with a substrate material of A-15 Nb 3 Al/sub 0.9/Si/sub 0.1/, two basic approaches were tried towards the formation of A-15 Nb 3 Si by Si implantation: (1) direct replacement of the Al by Si and (2) implantation into a surface layer depleted of Al. This latter approach proved to be the most successful. It consisted of removing the Al by a diffusion anneal and replacing the Al deficiency by sequential Si implantations. Upon subsequent heat treatment a surface layer of A-15 Nb 3 Al/sub 0.2/Si/sub 0.8/ was produced. Details of the experimental procedure and a discussion of the superconducting transition temperature measurements of the implanted surfaces are presented

  7. Mg-doped VO2 nanoparticles: hydrothermal synthesis, enhanced visible transmittance and decreased metal-insulator transition temperature.

    Science.gov (United States)

    Zhou, Jiadong; Gao, Yanfeng; Liu, Xinling; Chen, Zhang; Dai, Lei; Cao, Chuanxiang; Luo, Hongjie; Kanahira, Minoru; Sun, Chao; Yan, Liuming

    2013-05-28

    This paper reports the successful preparation of Mg-doped VO2 nanoparticles via hydrothermal synthesis. The metal-insulator transition temperature (T(c)) decreased by approximately 2 K per at% Mg. The Tc decreased to 54 °C with 7.0 at% dopant. The composite foils made from Mg-doped VO2 particles displayed excellent visible transmittance (up to 54.2%) and solar modulation ability (up to 10.6%). In addition, the absorption edge blue-shifted from 490 nm to 440 nm at a Mg content of 3.8 at%, representing a widened optical band gap from 2.0 eV for pure VO2 to 2.4 eV at 3.8 at% doping. As a result, the colour of the Mg-doped films was modified to increase their brightness and lighten the yellow colour over that of the undoped-VO2 film. A first principle calculation was conducted to understand how dopants affect the optical, Mott phase transition and structural properties of VO2.

  8. Fabrication of FeAl Intermetallic Foams by Tartaric Acid-Assisted Self-Propagating High-Temperature Synthesis

    Directory of Open Access Journals (Sweden)

    Krzysztof Karczewski

    2018-04-01

    Full Text Available Iron aluminides are intermetallics with interesting applications in porous form thanks to their mechanical and corrosion resistance properties. However, making porous forms of these materials is not easy due to their high melting points. We formed FeAl foams by elemental iron and aluminum powders sintering with tartaric acid additive. Tartaric acid worked as an in situ gas-releasing agent during the self-propagating high-temperature synthesis of FeAl intermetallic alloy, which was confirmed by X-ray diffraction measurements. The porosity of the formed foams was up to 36 ± 4%. In the core of the sample, the average equivalent circle diameter was found to be 47 ± 20 µm, while on the surface, it was 35 ± 16 µm; thus, the spread of the pore size was smaller than reported previously. To investigate functional applications of the formed FeAl foam, the pressure drop of air during penetration of the foam was examined. It was found that increased porosity of the material increased the flow of the air through the metallic foam.

  9. An assessment of the process of Self-propagating High-Temperature Synthesis for the fabrication of porous copper composite

    International Nuclear Information System (INIS)

    Moloodi, A.; Raiszadeh, R.; Vahdati-Khaki, J.; Babakhani, A.

    2009-01-01

    The present article describes the process of Self-propagating High-temperature Synthesis (SHS) that is employed for fabricating open cell copper-alumina composite foam. This foam was fabricated by the reactions between the powders of CuO, Al and C. The gas released during these reactions as well as the initial porosity of the green powder compact were suggested to be the sources of the produced pores. Further, the effect of C content and the precursor compressing pressure on the porosity content and morphology of the SHS product was determined. Optical microscopy (OM), scanning electron microscopy (SEM), and X-ray diffraction (XRD) were utilized to characterize the porous samples. The optimum weight fractions for blending the initial powders were determined to be 84 wt.% CuO, 9.5 wt.% Al, and 6.5 wt.% C, and the SHS reaction was sustainable only if the initial compacting pressure of the powders was between 100 and 300 MPa.

  10. The effect of synthesis temperature on the formation of hydrotalcites in Bayer liquor: a vibrational spectroscopic analysis.

    Science.gov (United States)

    Palmer, Sara J; Frost, Ray L

    2009-07-01

    The seawater neutralization process is currently used in the alumina industry to reduce the pH and dissolved metal concentrations in bauxite refinery residues through the precipitation of Mg, Al, and Ca hydroxide and carbonate minerals. This neutralization method is very similar to the co-precipitation method used to synthesize hydrotalcite (Mg6Al2(OH)16CO3.4H2O). This study looks at the effect of temperature on the type of precipitates that form from the seawater neutralization process of Bayer liquor. The Bayer precipitates have been characterized by a variety of techniques, including X-ray diffraction (XRD), Raman spectroscopy, and infrared spectroscopy. The mineralogical composition of Bayer precipitates largely includes hydrotalcite, hydromagnesite, and calcium carbonate species. Analysis with XRD determined that Bayer hydrotalcites that are synthesized at 55 degrees C have a larger interlayer distance, indicating that more anions are removed from Bayer liquor. Vibrational spectroscopic techniques have identified an increase in hydrogen bond strength for precipitates formed at 55 degrees C, suggesting the formation of a more stable Bayer hydrotalcite. Raman spectroscopy identified the intercalation of sulfate and carbonate anions into Bayer hydrotalcites using these synthesis conditions.

  11. One-step synthesis and characterizations of cerium oxide nanoparticles in an ambient temperature via Co-precipitation method

    Science.gov (United States)

    Pujar, Malatesh S.; Hunagund, Shirajahammad M.; Desai, Vani R.; Patil, Shivaprasadgouda; Sidarai, Ashok H.

    2018-04-01

    We report the simple Co-precipitation method for the synthesis of Cerium oxide (CeO2) nanoparticles (NPs) in an ambient temperature. We have taken the Cerium (III) nitrate hexahydrate (Ce(NO3)3.6H2O) and Sodium hydroxide (NaOH) as the precursors. The obtained NPs were analyzed using the UV-Vis spectrophotometer, Fourier transform infrared spectroscopy (FT-IR) and X-ray diffraction (XRD). The obtained results signify that UV-Vis spectrum exhibited a well-defined absorption peak at 274 nm and the estimated energy gap (Eg) is 4.05 eV. The FT-IR analysis provides the supporting evidence for the presence of bonding of O-H, nitrates, alcohols and O-Ce-O vibrations. The XRD result reveals that the synthesized CeO2 NPs was crystallite with cubic phase structure and the estimated average crystallite size of CeO2 NPs using Scherer's and W-H method was significantly different due to their assumptions. Further, it is purposed to study their photocatalytic biological activities.

  12. Production of porous sintered materials using wastes of manufacturing engineering in self-propagating high-temperature synthesis

    Directory of Open Access Journals (Sweden)

    Y. S. Povstyana

    2016-06-01

    Full Text Available The increasing amount of wastes produced by the manufacturing engineering, as well as their physical and mechanical properties and restorability provide a search for sphere of their application. The actual problem of modern science is the utilization of wastes and using them in further production that will minimize their harmful impact on the environment and reduce the cost of expensive raw materials. Wastes are ideally suitable for the manufacture of porous permeable materials (filters. Powder metallurgy allows obtaining products with controlled filtration, physical and mechanical properties. Such materials are good filters for regeneration of technical liquids, oils, cooling fluids, sewage etc. The article analyzes the methods and technologies for the manufacture of porous ceramic materials and a new technology for their manufacture, which is based on use of mill scale and natural mineral – saponite as the main components. Compression technology provides products at low pressures and sintering by passing high-temperature synthesis. The proposed technology is characterized by low cost and good physical and mechanical properties of the product that gives a reason to use them for filtering and regeneration of technical liquids.

  13. Room-Temperature and Aqueous-Phase Synthesis of Plasmonic Molybdenum Oxide Nanoparticles for Visible-Light-Enhanced Hydrogen Generation.

    Science.gov (United States)

    Shi, Jiayuan; Kuwahara, Yasutaka; Wen, Meicheng; Navlani-García, Miriam; Mori, Kohsuke; An, Taicheng; Yamashita, Hiromi

    2016-09-06

    A straightforward aqueous synthesis of MoO3-x nanoparticles at room temperature was developed by using (NH4 )6 Mo7 O24 ⋅4 H2 O and MoCl5 as precursors in the absence of reductants, inert gas, and organic solvents. SEM and TEM images indicate the as-prepared products are nanoparticles with diameters of 90-180 nm. The diffuse reflectance UV-visible-near-IR spectra of the samples indicate localized surface plasmon resonance (LSPR) properties generated by the introduction of oxygen vacancies. Owing to its strong plasmonic absorption in the visible-light and near-infrared region, such nanostructures exhibit an enhancement of activity toward visible-light catalytic hydrogen generation. MoO3-x nanoparticles synthesized with a molar ratio of Mo(VI) /Mo(V) 1:1 show the highest yield of H2 evolution. The cycling catalytic performance has been investigated to indicate the structural and chemical stability of the as-prepared plasmonic MoO3-x nanoparticles, which reveals its potential application in visible-light catalytic hydrogen production. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

  14. Formulation and catalytic performance of MOF-derived Fe@C/Al composites for high temperature Fischer–Tropsch synthesis

    KAUST Repository

    Oar-Arteta, Lide

    2017-11-15

    High productivity towards C-2-C-4 olefins together with high catalyst stability are key for optimum operation in high temperature Fischer-Tropsch synthesis (HT-FTS). Here, we report the fabrication of Fe@C/Al composites that combine both the outstanding catalytic properties of the Fe-BTC MOF-derived Fe catalyst and the excellent mechanical resistance and textural properties provided by the inorganic AlOOH binder. The addition of AlOOH to Fe-BTC followed by pyrolysis in N-2 atmosphere at 500 degrees C results in composites with a large mesoporosity, a high Fe/Fe3O4 ratio, 10-35 nm average Fe crystallite size and coordinatively unsaturated Al3+ sites. In catalytic terms, the addition of AlOOH binder gives rise to enhanced C-2-C-4 selectivity and catalyst mechanical stability in HT-FTS, but at high Al contents the activity decreases. Altogether, the productivity of these Fe@C/Al composites is well above most known Fe catalysts for this process.

  15. Low-temperature synthesis of hexagonal transition metal ion doped ZnS nanoparticles by a simple colloidal method

    International Nuclear Information System (INIS)

    Wang, Liping; Huang, Shungang; Sun, Yujie

    2013-01-01

    A general route to synthesize transition metal ions doped ZnS nanoparticles with hexagonal phase by means of a conventional reverse micelle at a low temperature is developed. The synthesis involves N,N-dimethylformamide, Zn(AC) 2 solution, thiourea, ammonia, mercaptoacetic acid, as oil phase, water phase, sulfide source, pH regulator, and surfactant, respectively. Thiourea, ammonia and mercaptoacetic acid are demonstrated crucial factors, whose effects have been studied in detail. In addition, the FT-IR spectra suggest that mercaptoacetic acid may form complex chelates with Zn 2+ in the preparation. In the case of Cu 2+ as a doped ion, hexagonal ZnS:Cu 2+ nanoparticles were synthesized at 95 °C for the first time. The X-ray diffraction (XRD) and transmission electron microscope (TEM) measurements show that the ZnS:Cu 2+ nanoparticles are polycrystalline and possess uniform particle size. The possible formation mechanism of the hexagonal doped ZnS is discussed.

  16. In situ synthesis of manganese oxides on polyester fiber for formaldehyde decomposition at room temperature

    Science.gov (United States)

    Wang, Jinlong; Yunus, Rizwangul; Li, Jinge; Li, Peilin; Zhang, Pengyi; Kim, Jeonghyun

    2015-12-01

    Removal of low-level formaldehyde (HCHO) is of great interest for indoor air quality improvement. Supported materials especially those with low air pressure drop are of necessity for air purification. Manganese oxides (MnOx) was in situ deposited on the surface of fibers of a non-woven fabric made of polyethylene terephthalate (PET). As-synthesized MnOx/PET were characterized by SEM, XRD, TEM, ATR-FTIR and XPS analysis. The growth of MnOx layer on PET is thought to start with partial hydrolysis of PET, followed by surface oxidation by KMnO4 and then surface-deposition of MnOx particles from the bulk phase. The MnOx particles assembled with nanosheets were uniformly coated on the PET fibers. MnOx/PET showed good activity for HCHO decomposition at room temperature which followed the Mars-van Krevelen mechanism. The removal of HCHO was kept over 94% after 10 h continuous reaction under the conditions of inlet HCHO concentration ∼0.6 mg/m3, space velocity ∼17,000 h-1 and relative humidity∼50%. This research provides a facile method to deposit active MnOx onto polymers with low air resistance, and composite MnOx/PET material is promising for indoor air purification.

  17. Low-temperature synthesis of ZrB2 powder from oxides using Na

    Directory of Open Access Journals (Sweden)

    Haruhiko Morito

    2017-12-01

    Full Text Available ZrB2 was synthesized by heating a mixture of ZrO2, B2O3, and Na in a molar ratio of 1:1:5 at 873–1273 K. While unreacted ZrO2 remained in the sample synthesized at 873 K, single phase ZrB2 powders were obtained at temperatures ≥1073 K. The diameters of the ZrB2 particles obtained at 1073 and 1273 K were 0.1–20 and 10–100 μm, respectively. Single phase ZrB2 was also obtained at 873 K when the starting material was rich in B2O3 and Na (ZrO2:B2O3:Na = 1:5:15. This route yielded fine particle aggregates of ZrB2, which were found to be <0.1 μm in size.

  18. Room-temperature synthesis of gold nanoparticles and nanoplates using Shewanella algae cell extract

    Energy Technology Data Exchange (ETDEWEB)

    Ogi, Takashi; Saitoh, Norizoh; Nomura, Toshiyuki; Konishi, Yasuhiro, E-mail: yasuhiro@chemeng.osakafu-u.ac.j [Osaka Prefecture University, Department of Chemical Engineering (Japan)

    2010-09-15

    Biosynthesis of spherical gold nanoparticles and gold nanoplates was achieved at room temperature and pH 2.8 when cell extract from the metal-reducing bacterium Shewanella algae was used as both a reducing and shape-controlling agent. Cell extract, prepared by sonicating a suspension of S. algae cells, was capable of reducing 1 mol/m{sup 3} aqueous AuCl{sub 4}{sup -} ions into elemental gold within 10 min when H{sub 2} gas was provided as an electron donor. The time interval lapsed since the beginning of the bioreductive reaction was found to be an important factor in controlling the morphology of biogenic gold nanoparticles. After 1 h, there was a large population of well-dispersed, spherical gold nanoparticles with a mean size of 9.6 nm. Gold nanoplates with an edge length of 100 nm appeared after 6 h, and 60% of the total nanoparticle population was due to gold nanoplates with an edge length of 100-200 nm after 24 h. The yield of gold nanoplates prepared with S. algae extract was four times higher than that prepared with resting cells of S. algae. The resulting biogenic gold nanoparticle suspensions showed a large variation in color, ranging from pale pink to purple due to changes in nanoparticle morphology.

  19. Low temperature synthesis of ternary metal phosphides using plasma for asymmetric supercapacitors

    KAUST Repository

    Liang, Hanfeng

    2017-04-06

    We report a versatile route for the preparation of metal phosphides using PH plasma for supercapacitor applications. The high reactivity of plasma allows rapid and low temperature conversion of hydroxides into monometallic, bimetallic, or even more complex nanostructured phosphides. These same phosphides are much more difficult to synthesize by conventional methods. Further, we present a general strategy for significantly enhancing the electrochemical performance of monometallic phosphides by substituting extrinsic metal atoms. Using NiCoP as a demonstration, we show that the Co substitution into NiP not only effectively alters the electronic structure and improves the intrinsic reactivity and electrical conductivity, but also stabilizes Ni species when used as supercapacitor electrode materials. As a result, the NiCoP nanosheet electrodes achieve high electrochemical activity and good stability in 1 M KOH electrolyte. More importantly, our assembled NiCoP nanoplates//graphene films asymmetric supercapacitor devices can deliver a high energy density of 32.9 Wh kg at a power density of 1301 W kg, along with outstanding cycling performance (83% capacity retention after 5000 cycles at 20 A g). This activity outperforms most of the NiCo-based materials and renders the NiCoP nanoplates a promising candidate for capacitive storage devices.

  20. Low-temperature molten salt synthesis and characterization of CoWO4 nano-particles

    International Nuclear Information System (INIS)

    Song Zuwei; Ma Junfeng; Sun Huyuan; Sun Yong; Fang Jingrui; Liu Zhengsen; Gao Chang; Liu Ye; Zhao Jingang

    2009-01-01

    CoWO 4 nano-particles were successfully synthesized at a low temperature of 270 deg. C by a molten salt method, and effects of such processing parameters as holding time and salt quantity on the crystallization and development of CoWO 4 crystallites were initially studied. The products were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), and photoluminescent spectra techniques (PL), respectively. Experimental results showed that the well-crystallized CoWO 4 nano-particles with ca. 45 nm in diameter could be obtained at 270 deg. C for a holding time of 8 h with 6:1 mass ratio of the salt to CoWO 4 precursor, and XRD analysis evidenced that the as-prepared sample was a pure monoclinic phase of CoWO 4 with wolframite structure. Their PL spectra revealed that the CoWO 4 nano-particles displayed a very strong PL peak at 453 nm with the excitation wavelength of 230 nm, and PL properties of CoWO 4 crystallites relied on their crystalline state, especially on their particle size.

  1. Room-temperature synthesis of gold nanoparticles and nanoplates using Shewanella algae cell extract

    International Nuclear Information System (INIS)

    Ogi, Takashi; Saitoh, Norizoh; Nomura, Toshiyuki; Konishi, Yasuhiro

    2010-01-01

    Biosynthesis of spherical gold nanoparticles and gold nanoplates was achieved at room temperature and pH 2.8 when cell extract from the metal-reducing bacterium Shewanella algae was used as both a reducing and shape-controlling agent. Cell extract, prepared by sonicating a suspension of S. algae cells, was capable of reducing 1 mol/m 3 aqueous AuCl 4 - ions into elemental gold within 10 min when H 2 gas was provided as an electron donor. The time interval lapsed since the beginning of the bioreductive reaction was found to be an important factor in controlling the morphology of biogenic gold nanoparticles. After 1 h, there was a large population of well-dispersed, spherical gold nanoparticles with a mean size of 9.6 nm. Gold nanoplates with an edge length of 100 nm appeared after 6 h, and 60% of the total nanoparticle population was due to gold nanoplates with an edge length of 100-200 nm after 24 h. The yield of gold nanoplates prepared with S. algae extract was four times higher than that prepared with resting cells of S. algae. The resulting biogenic gold nanoparticle suspensions showed a large variation in color, ranging from pale pink to purple due to changes in nanoparticle morphology.

  2. MgO:Eu3+ red nanophosphor: Low temperature synthesis and photoluminescence properties

    Science.gov (United States)

    Devaraja, P. B.; Avadhani, D. N.; Prashantha, S. C.; Nagabhushana, H.; Sharma, S. C.; Nagabhushana, B. M.; Nagaswarupa, H. P.; Premkumar, H. B.

    2014-03-01

    Nanoparticles of Eu3+ doped (0-9 mol%) MgO were prepared using low temperature (400 °C) solution combustion technique with metal nitrate as precursor and glycine as fuel. The powder X-ray diffraction (PXRD) patterns of the as-formed products show single cubic phase and no further calcination was required. The crystallite size was obtained using Scherer's formula and was found to be 5-6 nm. The effect of Eu3+ ions on luminescence characteristics of MgO was studied and the results were discussed in detail. These phosphors exhibit bright red emission upon 395 nm excitation. The characteristic photoluminescence (PL) emission peaks at ∼580, 596, 616, 653, 696 and 706 nm (5D0 → 7Fj= 0, 1, 2, 3, 4) were recorded due to Eu3+ ions. The electronic transition corresponding to 5D0 → 7F2 of Eu3+ ions (616 nm) was stronger than the magnetic dipole transition corresponding to 5D0 → 7F1 of Eu3+ ions (596 nm). The international commission on illumination (CIE) chromaticity co-ordinates were calculated from emission spectra, the values (x, y) were very close to national television system committee (NTSC) standard value of red emission. Therefore the present phosphor was highly useful for display applications.

  3. In situ synthesis of zero-valent silver nanoparticles in polymethylmethacrylate under high temperature

    International Nuclear Information System (INIS)

    Xiong Yuanlu; Luo Guoqiang; Chen Cheng; Yuan Huan; Shen Qiang; Li Meijuan

    2012-01-01

    In this work, the silver nanoparticles were synthesized in polymethylmethacrylate (PMMA) matrix under high temperature with polyvinylpyrrolidone (PVP) as additional stabilizer and N,N-dimethylformamide (DMF) as reaction medium. The UV-vis spectroscopy and transmission electron microscopy (TEM) were adopted to investigate the growth and shape conversion of Ag nanoparticles with the lacking of additional Ag source. The results showed that the stable zero-valent Ag in PMMA was obtained successfully. Two types of Ag nanoparticles, single-crystal and twinned ones, could form in the initial period. While the twinned ones will gradually disappear along with the reaction processed, the single-crystal ones could survive and slowly grow by consuming the Ag atoms which were etched form twinned ones. The single-crystal ones will take shape conversion from sphere to nanocube with nearly the same particle size after the total disappearance of twinned ones. The size and shape of Ag nanoparticles can be well controlled by reaction time. The high viscosity PMMA matrix plays the important role of controlling the growth of the Ag nanoparticles, and the PVP takes the responsibility of the shape conversion.

  4. Green synthesis of CuxO nanoscale MOS capacitors processed at low temperatures

    KAUST Repository

    Al-Shehri, Safeyah

    2017-01-10

    In this work, we employed two nontoxic green chemistry methods to develop solution-processed copper oxide CuxO thin films at low annealing temperature of 200 °C. The first aqueous precursor of CuxO was prepared by mixing the copper powder with spinach leaves extract, whereas the other solution was formulated using the water-based polyol reduction method of Cu(II) nitrate. The as-prepared precursors were then spun on SiO2/P+ Si substrates to form nanoscale Metal-Oxide-Semiconductor (MOS) capacitors by which some valuable information about the CuxO semiconductor films and their interfaces with dielectric were acquired. Both fabricated MOS capacitors exhibited p-type polarity with negative flat-band voltages. However, the MOS based on spinach extract-CuxO films showed small hysteresis of 100 mV, which could be attributed to its large grain size that sequentially leads to smooth interface and less trap density.

  5. Low Temperature Synthesis of MnO2/Graphene Nanocomposites for Supercapacitors

    Directory of Open Access Journals (Sweden)

    Hao Huang

    2015-01-01

    Full Text Available MnO2/graphene nanocomposites were synthesized through a simple route in a water-reflux condenser system. The as-prepared composites were characterized by scanning electron microscopy, transmission electron microscopy, X-ray diffraction, Raman microscope, and Brunauer-Emmett-Teller surface area analysis. Capacitive properties of the synthesized composite electrodes were investigated via cyclic voltammetry, galvanostatic charge/discharge, and electrochemical impedance spectrometry in a 0.5 M Na2SO4 electrolyte. Results show that this method can control the morphology and structure of MnO2 loaded onto the graphene sheets. Because excessive MnO2 enwrapping graphene would affect the overall conductivity, the composite prepared by lower temperature has better characteristics of supercapacitor. 60-MnO2/graphene composite (48 wt% MnO2 displays the specific capacitance as high as 350 F/g at 1000 mA/g, which is higher than that of 100-MnO2/graphene (302 F/g, and it is almost two times higher than that of MnO2 (163 F/g. Furthermore, the composite exhibits excellent long cycle life along with ~93% specific capacitance retained after 5000 cycle tests.

  6. Rational design and synthesis of an orally bioavailable peptide guided by NMR amide temperature coefficients

    Science.gov (United States)

    Wang, Conan K.; Northfield, Susan E.; Colless, Barbara; Chaousis, Stephanie; Hamernig, Ingrid; Lohman, Rink-Jan; Nielsen, Daniel S.; Schroeder, Christina I.; Liras, Spiros; Price, David A.; Fairlie, David P.; Craik, David J.

    2014-01-01

    Enhancing the oral bioavailability of peptide drug leads is a major challenge in drug design. As such, methods to address this challenge are highly sought after by the pharmaceutical industry. Here, we propose a strategy to identify appropriate amides for N-methylation using temperature coefficients measured by NMR to identify exposed amides in cyclic peptides. N-methylation effectively caps these amides, modifying the overall solvation properties of the peptides and making them more membrane permeable. The approach for identifying sites for N-methylation is a rapid alternative to the elucidation of 3D structures of peptide drug leads, which has been a commonly used structure-guided approach in the past. Five leucine-rich peptide scaffolds are reported with selectively designed N-methylated derivatives. In vitro membrane permeability was assessed by parallel artificial membrane permeability assay and Caco-2 assay. The most promising N-methylated peptide was then tested in vivo. Here we report a novel peptide (15), which displayed an oral bioavailability of 33% in a rat model, thus validating the design approach. We show that this approach can also be used to explain the notable increase in oral bioavailability of a somatostatin analog. PMID:25416591

  7. Room temperature synthesis of silver nanowires from tabular silver bromide crystals in the presence of gelatin

    Science.gov (United States)

    Liu, Suwen; Wehmschulte, Rudolf J.; Lian, Guoda; Burba, Christopher M.

    2006-03-01

    Long silver nanowires were synthesized at room temperature by a simple and fast process derived from the development of photographic films. A film consisting of an emulsion of tabular silver bromide grains in gelatin was treated with a photographic developer (4-(methylamino)phenol sulfate (metol), citric acid) in the presence of additional aqueous silver nitrate. The silver nanowires have lengths of more than 50 μm, some even more than 100 μm, and average diameters of about 80 nm. Approximately, 70% of the metallic silver formed in the reduction consists of silver nanowires. Selected area electron diffraction (SAED) results indicate that the silver nanowires grow along the [111] direction. It was found that the presence of gelatin, tabular silver bromide crystals and silver ions in solution are essential for the formation of the silver nanowires. The nanowires appear to originate from the edges of the silver bromide crystals. They were characterized by transmission electron microscopy (TEM), SAED, scanning electron microscopy (SEM), and powder X-ray diffraction (XRD).

  8. Room temperature synthesis of silver nanowires from tabular silver bromide crystals in the presence of gelatin

    International Nuclear Information System (INIS)

    Liu Suwen; Wehmschulte, Rudolf J.; Lian Guoda; Burba, Christopher M.

    2006-01-01

    Long silver nanowires were synthesized at room temperature by a simple and fast process derived from the development of photographic films. A film consisting of an emulsion of tabular silver bromide grains in gelatin was treated with a photographic developer (4-(methylamino)phenol sulfate (metol), citric acid) in the presence of additional aqueous silver nitrate. The silver nanowires have lengths of more than 50 μm, some even more than 100 μm, and average diameters of about 80 nm. Approximately, 70% of the metallic silver formed in the reduction consists of silver nanowires. Selected area electron diffraction (SAED) results indicate that the silver nanowires grow along the [111] direction. It was found that the presence of gelatin, tabular silver bromide crystals and silver ions in solution are essential for the formation of the silver nanowires. The nanowires appear to originate from the edges of the silver bromide crystals. They were characterized by transmission electron microscopy (TEM), SAED, scanning electron microscopy (SEM), and powder X-ray diffraction (XRD)

  9. Green synthesis of CuxO nanoscale MOS capacitors processed at low temperatures

    KAUST Repository

    Al-Shehri, Safeyah; Al-Senany, Norah; Altuwirqi, Reem; Bayahya, Amani; Alshammari, Fwzah Hamud; Wang, Zhenwei; Al-Jawhari, Hala

    2017-01-01

    In this work, we employed two nontoxic green chemistry methods to develop solution-processed copper oxide CuxO thin films at low annealing temperature of 200 °C. The first aqueous precursor of CuxO was prepared by mixing the copper powder with spinach leaves extract, whereas the other solution was formulated using the water-based polyol reduction method of Cu(II) nitrate. The as-prepared precursors were then spun on SiO2/P+ Si substrates to form nanoscale Metal-Oxide-Semiconductor (MOS) capacitors by which some valuable information about the CuxO semiconductor films and their interfaces with dielectric were acquired. Both fabricated MOS capacitors exhibited p-type polarity with negative flat-band voltages. However, the MOS based on spinach extract-CuxO films showed small hysteresis of 100 mV, which could be attributed to its large grain size that sequentially leads to smooth interface and less trap density.

  10. Colloidal Fe-doped ZnO nanocrystals: Facile low temperature synthesis, characterization and properties

    Energy Technology Data Exchange (ETDEWEB)

    Singhal, A. [Chemistry Division, Bhabha Atomic Research Centre, Mumbai 400085 (India)], E-mail: ansing@barc.gov.in; Achary, S.N.; Tyagi, A.K. [Chemistry Division, Bhabha Atomic Research Centre, Mumbai 400085 (India); Manna, P.K.; Yusuf, S.M. [Solid State Physics Division, Bhabha Atomic Research Centre, Mumbai 400085 (India)

    2008-09-25

    Colloidal Fe-doped ZnO nanocrystals, Zn{sub 1-x}Fe{sub x}O (x = 0.00, 0.05, 0.07 and 0.1) have been prepared by thermal decomposition of metal precursors at 200 deg. C with hexadecylamine (HDA) as solvent and surfactant. The nanocrystals so prepared can be easily dispersed in non-polar solvents like chloroform and toluene. The nanocrystals have been structurally characterized using X-ray diffraction (XRD), high resolution transmission electron microscopy (HRTEM), energy dispersive X-ray analysis (EDX) and X-ray photoelectron spectroscopy (XPS). Magnetization measurements on a representative sample, Zn{sub 0.95}Fe{sub 0.05}O using a vibrating sample magnetometer (VSM) reveal that the nanocrystals exhibit a weak ferromagnetic behavior at 300 K. This observation is further confirmed by the electron paramagnetic resonance spectrum of Zn{sub 0.95}Fe{sub 0.05}O nanocrystals, which shows a distinct ferromagnetic resonance signal at room temperature.

  11. Low-temperature synthesis of single-phase Co7Sb2O12

    International Nuclear Information System (INIS)

    Brito, M.S.L.; Escote, M.T.; Santos, C.O.P.; Lisboa-Filho, P.N.; Leite, E.R.; Oliveira, J.B.L.; Gama, L.; Longo, E.

    2004-01-01

    Polycrystalline Co 7 Sb 2 O 12 compounds have been synthesized by a chemical route, which is based on a modified polymeric precursor method. In order to study the physical properties of the samples, X-ray diffraction (XRD), thermal analyses (TG and DSC), infrared spectroscopy (IR), specific surface area (BET), and magnetization measurements were performed on these materials. Characterization through XRD revealed that the samples are single-phase after a heat-treatment at 1100 deg. C for 2 h, while the X-ray patterns of the samples heat-treated at lower temperatures revealed the presence of additional Bragg reflections belonging to the Co 6 Sb 2 O 6 phase. These data were analyzed by means of Rietveld refinement and further analyze showed that Co 7 Sb 2 O 12 displays an inverse spinel crystalline structure. In this structure, the Co 2+ ions occupy the eight tetrahedral positions, and the sixteen octahedral positions are randomly occupied by the Sb 5+ and Co 2+ ions. IR studies disclosed two strong absorption bands, ν 1 and ν 2 , in the expected spectral range for a spinel-type binary oxide with space group Fd3m. Exploratory studies concerning the magnetic properties indicated that this sample presents a spin-glass transition at T f ∼ 64 K

  12. Low-temperature synthesis of MgB{sub 2} via powder metallurgy processing

    Energy Technology Data Exchange (ETDEWEB)

    Birol, Yucel [Dokuz Eylul University, Department of Metallurgical and Materials Engineering, Faculty of Engineering, Buca, Izmir (Turkey)

    2016-12-15

    Ball-milled Mg/B{sub 2}O{sub 3} powder blends reveal interpenetrating layers of deformed magnesium and boron oxide grains that are increasingly refined with increasing milling time. Boron oxide is reduced by Mg and MgO thus formed reacts with the remaining B{sub 2}O{sub 3} to produce Mg{sub 3}(BO{sub 3}){sub 2} during ball milling for 30 min. Both B{sub 2}O{sub 3} and Mg{sub 3}(BO{sub 3}){sub 2} react with Mg to produce MgB{sub 2} upon further ball milling. An annealing treatment can be employed when ball milling is performed for less than 1 h as thermal exposure of the ball-milled Mg/B{sub 2}O{sub 3} powder blends also leads to the formation of MgB{sub 2}. The above reactions take place between 500 and 700 C when the Mg/B{sub 2}O{sub 3} powder blend is ball milled for 30 min, and between 450 and 550 C, after ball milling for 1 h. This is a very attractive route owing to processing temperatures where the volatility of Mg is no longer a problem. (orig.)

  13. Nanocellulose-assisted low-temperature synthesis and supercapacitor performance of reduced graphene oxide aerogels

    Science.gov (United States)

    Wang, Jie; Ran, Ran; Sunarso, Jaka; Yin, Chao; Zou, Honggang; Feng, Yi; Li, Xiaobao; Zheng, Xu; Yao, Jianfeng

    2017-04-01

    Here, we have synthesized reduced graphene oxide (rGO) aerogels using a nanocellulose-assisted low temperature (less than 500 °C) thermal treatment route where nanocelluloses promote the gelation of graphene oxide (GO) solution that benefits the fabrication of GO aerogels from low concentration dispersion (2.85 mg mL-1), and after their thermal decomposition the residual nanofibers act as spacer both prevent the re-stacking of graphene sheets and integrate with rGO sheets to give a particular kind of carbon-based aerogel along with numerous defects (holes). Thermal decomposition of nanocellulose appears to be complete beyond 350 °C thus its presence in form of amorphous carbon nanofibers in rGO sheets. The rGO aerogels synthesized at 350 °C provide the best balance in terms of wide interlayer spacing, high content of CO-type functional groups, and high defects content. This translates into a high discharge capacitance of 270 F g-1 at a current rate of 1 A g-1 for compressed rGO aerogels without any binder or conductive additive. Detailed electrochemical tests using 6 M KOH electrolyte establish the fact that pseudocapacitance component has substantial contribution towards the overall capacitance; closely approaching the contribution of the double layer capacitance that is the most dominant capacitance component.

  14. Solution equilibrium behind the room-temperature synthesis of nanocrystalline titanium dioxide

    Science.gov (United States)

    Seisenbaeva, Gulaim A.; Daniel, Geoffrey; Nedelec, Jean-Marie; Kessler, Vadim G.

    2013-03-01

    Formation of nanocrystalline and monodisperse TiO2 from a water soluble and stable precursor, ammonium oxo-lactato-titanate, (NH4)8Ti4O4(Lactate)8.4H2O, often referred to as TiBALDH or TALH, is demonstrated to be due to a coordination equilibrium. This compound, individual in the solid state, exists in solution in equilibrium with ammonium tris-lactato-titanate, (NH4)2Ti(Lactate)3 and uniform crystalline TiO2 nanoparticles (anatase) stabilized by surface-capping with lactate ligands. This equilibrium can be shifted towards nano-TiO2via application of a less polar solvent like methanol or ethanol, dilution of the solution, introduction of salts or raising the temperature, and reverted on addition of polar and strongly solvating media such as dimethyl sulfoxide, according to NMR. Aggregation and precipitation of the particles were followed by DLS and could be achieved by a decrease in their surface charge by adsorption of strongly hydrogen-bonding cations, e.g. in solutions of ammonia, ethanolamine or amino acid arginine or by addition of ethanol. The observed equilibrium may be involved in formation of nano-titania on the surface of plant roots exerting chelating organic carboxylate ligands and thus potentially influencing plant interactions.Formation of nanocrystalline and monodisperse TiO2 from a water soluble and stable precursor, ammonium oxo-lactato-titanate, (NH4)8Ti4O4(Lactate)8.4H2O, often referred to as TiBALDH or TALH, is demonstrated to be due to a coordination equilibrium. This compound, individual in the solid state, exists in solution in equilibrium with ammonium tris-lactato-titanate, (NH4)2Ti(Lactate)3 and uniform crystalline TiO2 nanoparticles (anatase) stabilized by surface-capping with lactate ligands. This equilibrium can be shifted towards nano-TiO2via application of a less polar solvent like methanol or ethanol, dilution of the solution, introduction of salts or raising the temperature, and reverted on addition of polar and strongly solvating

  15. Immobilization of actinides in stable mineral type and ceramic materials (high temperature synthesis)

    Energy Technology Data Exchange (ETDEWEB)

    Starkov, O.; Konovalov, E.

    1996-05-01

    Alternative vitrification technologies are being developed in the world for the immobilization of high radioactive waste in materials with improved thermodynamic stability, as well as improved chemical and thermal stability and stability to radiation. Oxides, synthesized in the form of analogs to rock-forming minerals and ceramics, are among those materials that have highly stable properties and are compatible with the environment. In choosing the appropriate material, we need to be guided by its geometric stability, the minimal number of cations in the structure of the material and the presence of structural elements in the mineral that are isomorphs of uranium and thorium, actinoids found in nature. Rare earth elements, yttrium, zirconium and calcium are therefore suitable. The minerals listed in the table (with the exception of the zircon) are pegatites by origin, i.e. they are formed towards the end of the magma crystallization of silicates form the residual melt, enriched with Ta, Nb, Ti, Zr, Ce, Y, U and Th. Uranium and thorium in the form of isomorphic admixtures form part of the lattice of the mineral. These minerals, which are rather simple in composition and structure and are formed under high temperatures, may be viewed as natural physio-chemical systems that are stable and long-lived in natural environments. The similarity of the properties of actinoids and lanthanoids plays an important role in the geochemistry of uranium and thorium; however, uranium (IV) is closer to the {open_quotes}heavy{close_quotes} group of lanthanoids (the yttrium group) while thorium (IV) is closer to the {open_quotes}light{close_quotes} group (the cerium group). That is why rare earth minerals contain uranium and thorium in the form of isomorphic admixtures.

  16. 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.

  17. 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.

  18. One-step synthesis of lightly doped porous silicon nanowires in HF/AgNO3/H2O2 solution at room temperature

    International Nuclear Information System (INIS)

    Bai, Fan; Li, Meicheng; Song, Dandan; Yu, Hang; Jiang, Bing; Li, Yingfeng

    2012-01-01

    One-step synthesis of lightly doped porous silicon nanowire arrays was achieved by etching the silicon wafer in HF/AgNO 3 /H 2 O 2 solution at room temperature. The lightly doped porous silicon nanowires (pNWs) have circular nanopores on the sidewall, which can emit strong green fluorescence. The surface morphologies of these nanowires could be controlled by simply adjusting the concentration of H 2 O 2 , which influences the distribution of silver nanoparticles (Ag NPs) along the nanowire axis. A mechanism based on Ag NPs-induced lateral etching of nanowires was proposed to explain the formation of pNWs. The controllable and widely applicable synthesis of pNWs will open their potential application to nanoscale photoluminescence devices. - Graphical abstract: The one-step synthesis of porous silicon nanowire arrays is achieved by chemical etching of the lightly doped p-type Si (100) wafer at room temperature. These nanowires exhibit strong green photoluminescence. SEM, TEM, HRTEM and photoluminescence images of pNWs. The scale bars of SEM, TEM HRTEM and photoluminescence are 10 μm, 20 nm, 10 nm, and 1 μm, respectively. Highlights: ► Simple one-step synthesis of lightly doped porous silicon nanowire arrays is achieved at RT. ► Etching process and mechanism are illustrated with etching model from a novel standpoint. ► As-prepared porous silicon nanowire emits strong green fluorescence, proving unique property.

  19. Surface decoration through electrostatic interaction leading to enhanced reactivity: Low temperature synthesis of nanostructured chromium borides (CrB and CrB2)

    International Nuclear Information System (INIS)

    Menaka,; Kumar, Bharat; Kumar, Sandeep; Ganguli, A.K.

    2013-01-01

    The present study describes a novel low temperature route at ambient pressure for the synthesis of nanocrystalline chromium borides (CrB and CrB 2 ) without using any flux or additives. The favorable and intimate mixing of nanoparticles of chromium acetate (Cr source) and boron forms an active chromium–boron precursor which decomposes at much lower temperature (400 °C) to form CrB (which is ∼1000 °C less than the known ambient pressure synthesis). The chromium acetate nanoparticles (∼5 nm) decorate the larger boron particles (150–200 nm) due to electrostatic interactions resulting from opposing surface charges of boron (zeta potential:+48.101 mV) and chromium acetate (zeta potential:−4.021 mV) in ethanolic medium and is evident in the TEM micrographs. The above method leads to the formation of pure CrB film like structure at 400 °C and nanospheres (40–60 nm) at 600 °C. Also, chromium diboride (CrB 2 ) nanoparticles (25 nm) could be obtained at 1000 °C. - Graphical abstract: Variation of surface charge of reactants, precursor and the products, chromium borides (CrB and CrB 2 ). Highlights: ► Novel borothermal reduction process for synthesis of chromium boride. ► Significant lowering of reaction temperature to obtain nanocrystalline chromium boride. ► Enhanced reactivity due to appropriate surface interactions

  20. Melanin-gamma rays assistants for bismuth oxide nanoparticles synthesis at room temperature for enhancing antimicrobial, and photocatalytic activity.

    Science.gov (United States)

    El-Batal, Ahmed I; El-Sayyad, Gharieb S; El-Ghamry, Abbas; Agaypi, Kerolos M; Elsayed, Mohamed A; Gobara, Mohamed

    2017-08-01

    Melanin pigment has been deemed as a natural photoprotector with strong hydrophobicity. It allured considerable compatibility with many applications in medicine, food, and nanotechnology. Penicillium chrysogenium has been devoted to the green synthesis of melanin whereby optimizing its culture and environmental conditions. The impacts of alternative economic L-tyrosine natural sources (unprecedented alternate origins) and gamma radiation were pledged for the potential growing of the pigment. Herein, notable increases in melanin yield (6.4mg/ml; much higher than nonoptimized one by 40 folds) was obtained by optimizing the culture, and environmental requirements [potato starch (3.0%), yeast extract (5.0%), copper sulfate (0.2mM), 0.25% L-tyrosine, 0.1% L-glycine, and 0.1% Tween 20 at pH5.0, and 30°C for 7.0days using 180.0rpm shaking speed]. The addition of banana's peel (2.0%) has been led to increase the melanin production up to (8.3mg/ml; much higher than optimized one by 1.29 folds). It stimulated the induced enzymes, (i.e., tyrosinase) because it contained significant amounts of L-tyrosine, dopamine, and L-DOPA as resources for melanin biosynthesis. Then irradiated P. chrysogenium (2.5kGy) induced the pigment yield to 10.3mg/ml; much higher than optimized one by (1.61 folds). On the other hand, we tailored a methodology involved the product of melanin and gamma rays (25.0kGy) to an eco-friendly synthesis of Bismuth oxide nanoparticles (BiONPs) at the room temperature. Melanin under such alkaline condition functioning as simultaneously hydrolyzes, photoprotection of the Bi seeds, and stabilizer against the uncontrolled growth and the free radicals attack. Whereas the gamma irradiation induced the room temperature condensation reaction to occur, a novel mechanism proposal was discussed. BiONPs were characterized by UV-Vis., DLS, XRD, SEM, EDX, and FTIR. DLS and XRD calculations with TEM analysis exhibited the mean diameter of BiONPs was 29.82nm. Moreover, the as

  1. Low-temperature synthesis of Zn{sub 2}SiO{sub 4}:Mn green photoluminescence phosphor

    Energy Technology Data Exchange (ETDEWEB)

    Sivakumar, V. [Saveetha Engineering College, Thandalam, Chennai 602105 (India); Lakshmanan, Arunachalam, E-mail: arunachalamlakshmanan@yahoo.com [Saveetha Engineering College, Thandalam, Chennai 602105 (India); Kalpana, S.; Sangeetha Rani, R.; Satheesh Kumar, R. [Saveetha Engineering College, Thandalam, Chennai 602105 (India); Jose, M.T. [Radiological Safety Division, Indira Gandhi Centre for Atomic Research, Kalpakkam 603102 (India)

    2012-08-15

    Zn{sub 2}SiO{sub 4}:Mn green phosphor having comparable photoluminescence (PL) efficiency with commercial phosphor has been synthesized at 1000 Degree-Sign C using solid state reactions involving ZnO, silicic acid and manganese acetate. The water of crystallization attached to SiO{sub 2} in silicic acid whose dissociation at 1000 Degree-Sign C seem to promote the sintering efficiency of Zn{sub 2}SiO{sub 4}:Mn. Incremental ZnO addition and re-firing at 1000 Degree-Sign C promote the diffusion rate of ZnO and SiO{sub 2}. The formation of a single crystalline phase of willemite structure in the samples was confirmed by powder XRD measurements. The phosphor exhibit an intense excitation band centered around 275 nm and a relatively weak excitation centered around 380 nm while the broad band green emission peaks at 524 nm. Other parameters studied include PL spectra, grain morphology, ZnO/SiO{sub 2} molar ratio, Mn concentration, co-dopant/flux and the effect of chemical forms of Mn dopant as well as silica on the PL efficiency. - Highlights: Black-Right-Pointing-Pointer Synthesis of Zn{sub 2}SiO{sub 4}:Mn by solid state sintering at a low temperature of 1000 Degree-Sign C in air. Black-Right-Pointing-Pointer Dissociation of water of crystallization in silicic acid promote sintering efficiency. Black-Right-Pointing-Pointer Photoluminescence efficiency comparable with that of the commercial phosphor. Black-Right-Pointing-Pointer Enhancement in luminescence with MgCO{sub 3} co-doping and refiring as well as ZnO addition. Black-Right-Pointing-Pointer XRD confirm single phase willemite structure (rhombohedral) of Zn{sub 2}SiO{sub 4}:Mn.

  2. Preparation of Al-Ti-B grain refiner by SHS technology[Self-propagating High-temperature Synthesis

    Energy Technology Data Exchange (ETDEWEB)

    Nikitin, V.I.; Wanqi, J.I.E.; Kandalova, E.G.; Makarenko, A.G.; Yong, L.

    2000-02-01

    Since the discovery of the grain refinement effect of aluminum by titanium, especially with the existence of B or C in 1950, grain refiners are widely accepted in industry for microstructure control of aluminum alloys. Research on this topic is to obtain the highest grain refinement efficiency with the lowest possible addition of master alloy. It is widely accepted that the morphology and size of TiAl{sub 3} particles, which are known as heterogeneous nucleation centers, are important factors deterring the grain refinement efficiency. Fine TiAl{sub 3} particles are favorable. The grain refinement process shows a heredity phenomenon, which means that structural information from initial materials transfers through a melt to the final product. It is important to find the connection between microstructural parameters of the master alloy and the final product. To improve the quality of Al-Ti-B master alloys for the use as a grain refiner, a new method based on SHS (self-propagating high-temperature synthesis) technology has been developed in Samara State Technical University to produce the master alloys. SHS, as a new method for preparation of materials, was first utilized by Merzhanov in 1967. This method uses the energy from highly exothermic reactions to sustain the chemical reaction in a combustion wave. The advantages of SHS include simplicity, low energy requirement, and higher product purity. Because SHS reactions can take place between elemental reactants, it is easy to control product composition. The purposes of this investigation were to fabricate an SHS Al-5%Ti-1%B master alloy, to analyze its structure and to test its grain refining performance.

  3. Standard enthalpies of formation of some Lanthanide–Cobalt binary alloys by high temperature direct synthesis calorimetry

    Energy Technology Data Exchange (ETDEWEB)

    Meschel, S.V., E-mail: meschel@jfi.uchicago.edu [Illinois Institute of Technology, Thermal Processing Technology Center, 10 W. 32nd Street, Chicago, IL (United States); University of Chicago, Gordon Center of Interactive Science, 929 E 57th Street, Chicago, IL 60637 (United States); Nash, P. [Illinois Institute of Technology, Thermal Processing Technology Center, 10 W. 32nd Street, Chicago, IL (United States); Gao, Q.N.; Wang, J.C.; Du, Y. [Central South University, State Key Laboratory of Powder Metallurgy, Changsha, Hunan 410083 (China)

    2013-11-25

    Highlights: •Studied binary Lanthanide–Cobalt intermetallic alloys by high temperature calorimetry. •Determined the enthalpies of formation of 16 magnetostrictive alloys. •Compared the experimental measurements with theoretical predictions by two different models. -- Abstract: The standard enthalpies of formation of intermetallic compounds of some Lanthanide–Cobalt systems have been measured by high temperature direct synthesis calorimetry at 1373 ± 2 K. The following results in kJ/mol of atoms are reported: CeCo{sub 5}(−9.4 ± 3.3); Ce{sub 2}Co{sub 17}(−6.8 ± 3.2); PrCo{sub 5}(−10.5 ± 2.4); Pr{sub 2}Co{sub 17}(−6.8 ± 3.6); NdCo{sub 5}(−12.7 ± 2.6); Nd{sub 2}Co{sub 17}(−6.6 ± 2.7); SmCo{sub 5}(−12.2 ± 1.8); Sm{sub 2}Co{sub 17}(−7.2 ± 2.5); GdCo{sub 5}(−10.0 ± 2.4); Tb{sub 2}Co{sub 17}(−7.7 ± 2.9); Dy{sub 2}Co{sub 17}(−8.1 ± 2.9); HoCo{sub 3}(−17.5 ± 2.2); ErCo{sub 3}(−19.7 ± 3.3); TmCo{sub 3}(−22.9 ± 3.0); LuCo{sub 3}(−23.0 ± 2.6). The measurements are compared with values from the literature and with predicted values of the semi empirical model of Miedema and Coworkers. We also compare the measurements with predicted values by ab initio calculations. We will present a systematic picture of how the enthalpies of formation may be related to the atomic number of the Lanthanide element (LA). We will also compare the thermochemical behavior of the Fe, Co and Ni binary alloys with Lanthanide elements.

  4. Measured winter and spring-time indoor temperatures in UK homes over the period 1969–2010: A review and synthesis

    International Nuclear Information System (INIS)

    Vadodaria, K.; Loveday, D.L.; Haines, V.

    2014-01-01

    This paper presents a review and synthesis of average winter and spring-time indoor temperatures in UK homes measured over the period 1969–2010. Analysis of measured temperatures in a sample of solid wall dwellings in the UK, conducted as part of the CALEBRE research project, is included. The review suggests that, for periods when occupation was likely, there has been little or no increase in winter and spring-time average living room temperatures over the last 40 years, with average recorded living room temperatures having been historically lower than the WHO-recommended value of 21 °C. Correspondingly, for periods of likely occupation, average bedroom temperatures appear to have increased. Compared with non-domestic buildings, there have been fewer investigations of domestic thermal comfort, either in the UK or elsewhere, and hence the paper also calls for further detailed investigations of domestic indoor temperatures during occupied hours together with thermal comfort evaluations in order to better understand domestic thermal environments. Based on suggestions from the limited range of studies available to date, living room temperatures may need to be maintained within the range 20–22 °C for thermal satisfaction, though this requires confirmation through further research. The study also emphasises that improving the energy efficiency of homes should be the primary means to effect any increases in indoor temperatures that are deemed essential. Considerations for future policy are discussed. - Highlights: • We review indoor temperatures measured in UK homes during 1960-2010. • We present analysis of temperature recorded by our study in 20 UK homes. • Little or no increase observed in living room temperatures for the last 40 years. • Occupied bedroom temperatures appear to have increased. • Living room temperatures have been historically lower than the WHO guidelines

  5. High-throughput optimization of nitroxide mediated radical polymerizations as basis for the synthesis of temperature-responsive copolymers

    NARCIS (Netherlands)

    Hoogenboom, R.; Becer, C.R.; Eggenhuisen, T.M.; Schubert, U.S.

    2008-01-01

    The development of controlled radical polymn. techniques, namely atom transfer radical polymn. (ATRP), reversible addn. fragmentation transfer (RAFT) and nitroxide mediated radical polymn. (NMP), have opened up unprecedented possibilities for the synthesis of well-defined macromol. architectures

  6. Prediction and experimental determination of the solubility of exotic scales at high temperatures - Zinc sulfide

    DEFF Research Database (Denmark)

    Carolina Figueroa Murcia, Diana; Fosbøl, Philip Loldrup; Thomsen, Kaj

    2016-01-01

    The presence of "exotic" scale such as Zinc Sulfide (ZnS), Lead Sulfide (PbS) and Iron Sulfide (FeS) in HP/HT reservoirs has been identified. "Exotic" scale materials come as a new challenge in HP/HT reservoirs. This has led to the development of more advanced tools to predict their behavior...... at extreme conditions. The aim of this work is to include ZnS into the group of scale materials that can be modeled with the Extended UNIQUAC model. Solubility data for ZnS are scarce in the open literature. In order to improve the available data, we study the experimental behavior of ZnS solubility at high...... temperatures. The determination of the solubility of ZnS is carried out at temperatures up to 250°C. Zinc sulfide (99.99%) and ultra-pure water are placed in a vial in a reduced oxygen atmosphere. The sample is placed in a controlled bath and stirred until equilibrium is attained. The suspension is filtered...

  7. Low-temperature solid-state synthesis and optical properties of CdS-ZnS and ZnS-CdS alloy nanoparticles

    International Nuclear Information System (INIS)

    Liu Jinsong; Zhao Chuanbao; Li Ziquan; Chen Jiankang; Zhou Hengzhi; Gu Shanqun; Zeng Youhong; Li Yongchan; Huang Yongbing

    2011-01-01

    Highlights: → Using a simple low-temperature solid-state synthetic method, ZnS-CdS and CdS-ZnS alloy nanoparticles were obtained, respectively. → The size of the nanoparticles increased with increasing reaction temperature, and reaction sequence had no effect on the size of the nanoparticles under the same temperature. → The particle diameters of the CdS-ZnS products decreased gradually with increasing Cd 2+ /Zn 2+ molar ratio, whereas those of the ZnS-CdS products increased gradually with increasing Zn 2+ /Cd 2+ molar ratio. → The study shows that sufficient grinding and crystalline water may be a key in forming the alloy nanoparticles. → Optical properties of the products depend on reaction temperature, reactant addition sequence, and reactant molar ratio. - Abstract: A simple low-temperature solid-state synthetic method was employed to obtain ZnS-CdS and CdS-ZnS alloy nanoparticles. The effects of reaction sequence, reactant molar ratios, and synthesis temperature on the products were investigated. The crystal structure and morphology of the products were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), and fourier transform infrared (FT-IR) spectroscopy. The results show that the products are alloy nanoparticles with a cubic phase structure. The formation mechanism of the alloy nanoparticles is briefly discussed. Sufficient grinding and crystalline water may be essential to form alloy nanoparticles. Ultraviolet-visible (UV-vis) spectra show that the edge absorptions of the CdS-ZnS and ZnS-CdS nanoparticles were located between those of ZnS and CdS bulks, and the absorbance at the peak maximum was practically dependent on reaction temperature, reaction sequence, and molar ratio. Extrinsic deep-level emission resulted in strong peaks in the photoluminescence (PL) spectra. The position and intensity of the emission peaks varied with the conditions during synthesis.

  8. Lithium-deficient Li YMn2O4 spinels (0.9 ≤ Y < 1): Lithium content, synthesis temperature, thermal behaviour and electrochemical properties

    International Nuclear Information System (INIS)

    Pascual, Laura; Perez-Revenga, M. Luz; Rojas, Rosa M.; Rojo, Jose M.; Amarilla, J. Manuel

    2006-01-01

    Lithium-deficient Li Y Mn 2 O 4 spinels (LD-Li Y Mn 2 O 4 ) with nominal composition (0.9 ≤ Y 2 O 3 and LiNO 3 at temperatures ranging from 700 deg. C to 850 deg. C. X-ray diffraction data show that LD-Li Y Mn 2 O 4 spinels are obtained as single phases in the range Y = 0.975-1 at 700 deg. C and 750 deg. C. Morphological characterization by transmission electron microscopy shows that the particle size of LD-Li Y Mn 2 O 4 spinels increases on decreasing the Li-content. The influence of the Li-content and the synthesis temperature on the thermal and electrochemical behaviours has been systematically studied. Thermal analysis studies indicate that the temperature of the first thermal effect in the differential thermal analysis (DTA)/thermogravimetric (TG) curves, T C1 , linearly increases on decreasing the Li-content. The electrochemical properties of LD-Li Y Mn 2 O 4 spinels, determined by galvanostatic cycling, notably change with the synthesis conditions. So, the first discharge capacity, Q disch. , at C rate increases on rising the Li-content and the synthesis temperature. The sample Li 0.975 Mn 2 O 4 synthesized at 700 deg. C has a Q disch. = 123 mAh g -1 and a capacity retention of 99.77% per cycle. This LD-Li Y Mn 2 O 4 sample had the best electrochemical characteristics of the series

  9. Facile synthesis of both needle-like and spherical hydroxyapatite nanoparticles: effect of synthetic temperature and calcination on morphology, crystallite size and crystallinity.

    Science.gov (United States)

    Wijesinghe, W P S L; Mantilaka, M M M G P G; Premalal, E V A; Herath, H M T U; Mahalingam, S; Edirisinghe, M; Rajapakse, R P V J; Rajapakse, R M G

    2014-09-01

    Synthetic hydroxyapatite (HA) nanoparticles, that mimic natural HA, are widely used as biocompatible coatings on prostheses to repair and substitute human bones. In this study, HA nanoparticles are prepared by precipitating them from a precursor solution containing calcium sucrate and ammonium dihydrogen orthophosphate, at a Ca/P mole ratio of 1.67:1, at temperatures, ranging from 10°C to 95°C. A set of products, prepared at different temperatures, is analyzed for their crystallinity, crystallite size, morphology, thermal stability and composition, by X-ray diffraction (XRD), scanning electron microscopy (SEM), thermogravimetric analysis (TGA) and Fourier transform infrared (FT-IR) spectroscopic techniques, while the other set is analyzed after calcining the respective products, soon after their synthesis, for 3h, at 700°C. The as-prepared products, after 2h of drying, without any calcination, are not crystalline, but they grow very slowly into needle-like morphologies, as they are ripened with time. The percentage crystallinity of the final products increases from 15% to 52%, with increasing the preparative temperature. The calcined samples always produce spherical nanoparticles of essentially the same diameter, between 90 nm and 100 nm, which does not change due to aging and preparative temperatures. Therefore, the same method can be utilized to synthesize both spherical and needle-like nanoparticles of hydroxyapatite, with well-defined sizes and shapes. The ability to use readily available cheap raw materials, for the synthesis of such well-defined crystallites of hydroxyapatite, is an added advantage of this method, which may be explored further for the scaling up of the procedures to suit to industrial scale synthesis of such hydroxyapatite nanoparticles. Copyright © 2014 Elsevier B.V. All rights reserved.

  10. Facile synthesis of both needle-like and spherical hydroxyapatite nanoparticles: Effect of synthetic temperature and calcination on morphology, crystallite size and crystallinity

    International Nuclear Information System (INIS)

    Wijesinghe, W.P.S.L.; Mantilaka, M.M.M.G.P.G.; Premalal, E.V.A.; Herath, H.M.T.U.; Mahalingam, S.; Edirisinghe, M.; Rajapakse, R.P.V.J.; Rajapakse, R.M.G.

    2014-01-01

    Synthetic hydroxyapatite (HA) nanoparticles, that mimic natural HA, are widely used as biocompatible coatings on prostheses to repair and substitute human bones. In this study, HA nanoparticles are prepared by precipitating them from a precursor solution containing calcium sucrate and ammonium dihydrogen orthophosphate, at a Ca/P mole ratio of 1.67:1, at temperatures, ranging from 10 °C to 95 °C. A set of products, prepared at different temperatures, is analyzed for their crystallinity, crystallite size, morphology, thermal stability and composition, by X-ray diffraction (XRD), scanning electron microscopy (SEM), thermogravimetric analysis (TGA) and Fourier transform infrared (FT-IR) spectroscopic techniques, while the other set is analyzed after calcining the respective products, soon after their synthesis, for 3 h, at 700 °C. The as-prepared products, after 2 h of drying, without any calcination, are not crystalline, but they grow very slowly into needle-like morphologies, as they are ripened with time. The percentage crystallinity of the final products increases from 15% to 52%, with increasing the preparative temperature. The calcined samples always produce spherical nanoparticles of essentially the same diameter, between 90 nm and 100 nm, which does not change due to aging and preparative temperatures. Therefore, the same method can be utilized to synthesize both spherical and needle-like nanoparticles of hydroxyapatite, with well-defined sizes and shapes. The ability to use readily available cheap raw materials, for the synthesis of such well-defined crystallites of hydroxyapatite, is an added advantage of this method, which may be explored further for the scaling up of the procedures to suit to industrial scale synthesis of such hydroxyapatite nanoparticles. - Highlights: • Hydroxyapatite nanoparticles are synthesized using a simple precipitation method. • Both needle-like and spherical hydroxyapatite nanoparticles are synthesized. • The prepared

  11. Facile synthesis of both needle-like and spherical hydroxyapatite nanoparticles: Effect of synthetic temperature and calcination on morphology, crystallite size and crystallinity

    Energy Technology Data Exchange (ETDEWEB)

    Wijesinghe, W.P.S.L.; Mantilaka, M.M.M.G.P.G. [Department of Chemistry, Faculty of Science, University of Peradeniya, Peradeniya 20400 (Sri Lanka); Post-graduate Institute of Science, P.O. Box: 25, University of Peradeniya, Peradeniya 20400 (Sri Lanka); Premalal, E.V.A. [Department of Materials Science, Shizuoka University, Johoku, Naka-ku Hamamatsu, 432-8011 (Japan); Herath, H.M.T.U. [Department of Medical Laboratory Science, Faculty of Allied Health Sciences, University of Peradeniya, Peradeniya 20400 (Sri Lanka); Mahalingam, S.; Edirisinghe, M. [Department of Mechanical Engineering, University College London, London WC1E 7JE (United Kingdom); Rajapakse, R.P.V.J. [Department of Veterinary Pathobiology, Faculty of Veterinary, University of Peradeniya, Peradeniya 20400 (Sri Lanka); Rajapakse, R.M.G., E-mail: rmgr@pdn.ac.lk [Department of Chemistry, Faculty of Science, University of Peradeniya, Peradeniya 20400 (Sri Lanka); Post-graduate Institute of Science, P.O. Box: 25, University of Peradeniya, Peradeniya 20400 (Sri Lanka)

    2014-09-01

    Synthetic hydroxyapatite (HA) nanoparticles, that mimic natural HA, are widely used as biocompatible coatings on prostheses to repair and substitute human bones. In this study, HA nanoparticles are prepared by precipitating them from a precursor solution containing calcium sucrate and ammonium dihydrogen orthophosphate, at a Ca/P mole ratio of 1.67:1, at temperatures, ranging from 10 °C to 95 °C. A set of products, prepared at different temperatures, is analyzed for their crystallinity, crystallite size, morphology, thermal stability and composition, by X-ray diffraction (XRD), scanning electron microscopy (SEM), thermogravimetric analysis (TGA) and Fourier transform infrared (FT-IR) spectroscopic techniques, while the other set is analyzed after calcining the respective products, soon after their synthesis, for 3 h, at 700 °C. The as-prepared products, after 2 h of drying, without any calcination, are not crystalline, but they grow very slowly into needle-like morphologies, as they are ripened with time. The percentage crystallinity of the final products increases from 15% to 52%, with increasing the preparative temperature. The calcined samples always produce spherical nanoparticles of essentially the same diameter, between 90 nm and 100 nm, which does not change due to aging and preparative temperatures. Therefore, the same method can be utilized to synthesize both spherical and needle-like nanoparticles of hydroxyapatite, with well-defined sizes and shapes. The ability to use readily available cheap raw materials, for the synthesis of such well-defined crystallites of hydroxyapatite, is an added advantage of this method, which may be explored further for the scaling up of the procedures to suit to industrial scale synthesis of such hydroxyapatite nanoparticles. - Highlights: • Hydroxyapatite nanoparticles are synthesized using a simple precipitation method. • Both needle-like and spherical hydroxyapatite nanoparticles are synthesized. • The prepared

  12. Low-temperature synthesis of CuFeO{sub 2} (delafossite) at 70 °C: A new process solely by precipitation and ageing

    Energy Technology Data Exchange (ETDEWEB)

    John, Melanie, E-mail: melanie.john@min.uni-muenchen.de [Section Mineralogy, Petrology & Geochemistry, Department of Earth and Environmental Sciences, Ludwig-Maximilians-Universität München, Theresienstr. 41, 80333 Munich (Germany); Heuss-Aßbichler, Soraya [Section Mineralogy, Petrology & Geochemistry, Department of Earth and Environmental Sciences, Ludwig-Maximilians-Universität München, Theresienstr. 41, 80333 Munich (Germany); Park, So-Hyun [Section Crystallography, Department of Earth and Environmental Sciences, Ludwig-Maximilians-Universität München, Theresienstr. 41, 80333 Munich (Germany); Ullrich, Aladin [Experimental Physics II, University of Augsburg, Universitätsstr. 1, 86159 Augsburg (Germany); Benka, Georg [Physics Department, Technical University Munich, James-Franck-Straße 1, 85748 Garching (Germany); Petersen, Nikolai [Section Geophysics, Department of Earth and Environmental Sciences, Ludwig-Maximilians-Universität München, Theresienstr. 41, 80333 Munich (Germany); Rettenwander, Daniel [Department of Materials Research & Physics, University of Salzburg, Hellbrunnerstrasse 34, 5020 Salzburg (Austria); Horn, Siegfried R. [Experimental Physics II, University of Augsburg, Universitätsstr. 1, 86159 Augsburg (Germany)

    2016-01-15

    This study presents a new low temperature synthesis method to obtain pure delafossite (Cu{sup 1+}Fe{sup 3+}O{sub 2}) at a temperature of 70 °C within 24 h. For the first time delafossite is synthesized solely by precipitation and subsequent ageing process and without usage of any additives controlling the oxidation state of copper. The synthesized material, called LT-delafossite, consists of pure Cu{sup 1+}Fe{sup 3+}O{sub 2} exclusive of any side products. Rietveld analysis confirms the presence of both 3R (space group (SG): R-3m) and 2H (SG: P6{sub 3}/mmc) polytypes in LT-delafossite. Electron microscopy images show nanometer-sized hexagonal plates with a diameter <500 nm and a thickness of <30 nm. Measurements of the magnetic susceptibility from 2 K to 350 K in zero-field show one peak ∼18.5 K, which is attributed to an AFM phase transition. Zero-field-cooled magnetization data between −14 T and +14 T at 2 K revealed an s-shape form around the origin having no remanent magnetization. - Highlights: • New process: low temperature synthesis of pure CuFeO{sub 2} nanoparticles. • Synthesis at 70 °C within 24 h solely by precipitation and ageing. • Nanoparticle characterization by XRD, FTIR, SEM, ICP–OES, TEM and Mößbauer. • Special magnetic properties of nano-sized CuFeO{sub 2} synthesized at low temperatures.

  13. Low temperature synthesis of seed mediated CuO bundle of nanowires, their structural characterisation and cholesterol detection

    Energy Technology Data Exchange (ETDEWEB)

    Ibupoto, Z.H., E-mail: zafar.hussin.ibupoto@liu.se [Department of Science and Technology, Linköping University, Campus Norrköping, SE-60174 Norrköping (Sweden); Khun, K. [Department of Science and Technology, Linköping University, Campus Norrköping, SE-60174 Norrköping (Sweden); Liu, X. [Department of Physics, Chemistry, and Biology (IFM), Linköping University, 58183 Linköping Sweden (Sweden); Willander, M. [Department of Science and Technology, Linköping University, Campus Norrköping, SE-60174 Norrköping (Sweden)

    2013-10-15

    In this study, we have successfully synthesised CuO bundle of nanowires using simple, cheap and low temperature hydrothermal growth method. The growth parameters such as precursor concentration and time for duration of growth were optimised. The field emission scanning electron microscopy (FESEM) has demonstrated that the CuO bundles of nanowires are highly dense, uniform and perpendicularly oriented to the substrate. The high resolution transmission electron microscopy (HRTEM) has demonstrated that the CuO nanostructures consist of bundle of nanowires and their growth pattern is along the [010] direction. The X-ray diffraction (XRD) technique described that CuO bundle of nanowires possess the monoclinic crystal phase. The surface and chemical composition analyses were carried out with X-ray photoelectron spectroscopy (XPS) technique and the obtained results suggested the pure crystal state of CuO nanostructures. In addition, the CuO nanowires were used for the cholesterol sensing application by immobilising the cholesterol oxidase through electrostatic attraction. The infrared reflection absorption spectroscopy study has also revealed that CuO nanostructures are consisting of only Cu-O bonding and has also shown the possible interaction of cholesterol oxidase with the sharp edge surface of CuO bundle of nanowires. The proposed cholesterol sensor has demonstrated the wide range of detection of cholesterol with good sensitivity of 33.88 ± 0.96 mV/decade. Moreover, the CuO bundle of nanowires based sensor electrode has revealed good repeatability, reproducibility, stability, selectivity and a fast response time of less than 10 s. The cholesterol sensor based on the immobilised cholesterol oxidase has good potential applicability for the determination of cholesterol from the human serum and other biological samples. - Highlights: • This study describes the synthesis of bundle of CuO nanowires by hydrothermal method. • CuO nanostructures exhibit good alignment and

  14. Low temperature synthesis of seed mediated CuO bundle of nanowires, their structural characterisation and cholesterol detection

    International Nuclear Information System (INIS)

    Ibupoto, Z.H.; Khun, K.; Liu, X.; Willander, M.

    2013-01-01

    In this study, we have successfully synthesised CuO bundle of nanowires using simple, cheap and low temperature hydrothermal growth method. The growth parameters such as precursor concentration and time for duration of growth were optimised. The field emission scanning electron microscopy (FESEM) has demonstrated that the CuO bundles of nanowires are highly dense, uniform and perpendicularly oriented to the substrate. The high resolution transmission electron microscopy (HRTEM) has demonstrated that the CuO nanostructures consist of bundle of nanowires and their growth pattern is along the [010] direction. The X-ray diffraction (XRD) technique described that CuO bundle of nanowires possess the monoclinic crystal phase. The surface and chemical composition analyses were carried out with X-ray photoelectron spectroscopy (XPS) technique and the obtained results suggested the pure crystal state of CuO nanostructures. In addition, the CuO nanowires were used for the cholesterol sensing application by immobilising the cholesterol oxidase through electrostatic attraction. The infrared reflection absorption spectroscopy study has also revealed that CuO nanostructures are consisting of only Cu-O bonding and has also shown the possible interaction of cholesterol oxidase with the sharp edge surface of CuO bundle of nanowires. The proposed cholesterol sensor has demonstrated the wide range of detection of cholesterol with good sensitivity of 33.88 ± 0.96 mV/decade. Moreover, the CuO bundle of nanowires based sensor electrode has revealed good repeatability, reproducibility, stability, selectivity and a fast response time of less than 10 s. The cholesterol sensor based on the immobilised cholesterol oxidase has good potential applicability for the determination of cholesterol from the human serum and other biological samples. - Highlights: • This study describes the synthesis of bundle of CuO nanowires by hydrothermal method. • CuO nanostructures exhibit good alignment and

  15. Low temperature synthesis of polyaniline-crystalline TiO2-halloysite composite nanotubes with enhanced visible light photocatalytic activity.

    Science.gov (United States)

    Li, Cuiping; Wang, Jie; Guo, Hong; Ding, Shujiang

    2015-11-15

    A series of one-dimensional polyaniline-crystalline TiO2-halloysite composite nanotubes with different mass ratio of polyaniline to TiO2 are facilely prepared by employing the low-temperature synthesis of crystalline TiO2 on halloysite nanotubes. The halloysite nanotubes can adsorb TiO2/polyaniline precursors and induce TiO2 nanocrystals/polyaniline to grow on the support in situ simultaneously. By simply adjusting the acidity of reaction system, PANI-crystalline TiO2-HA composite nanotubes composed of anatase, a mixed phase TiO2 and different PANI redox state are obtained. The XRD and UV-vis results show that the surface polyaniline sensitization has no effect on the crystalline structure of halloysite and TiO2 and the light response of TiO2 is extended to visible-light regions. Photocatalysis test results reveal the photocatalytic activity will be affected by the pH value and the volume ratio of ANI to TTIP. The highest photocatalytic activity is achieved with the composite photocatalysts prepared at pH 0.5 and 1% volume ratio of ANI and TTIP owing to the sensitizing effect of polyaniline and the charge transfer from the photoexcited PANI sensitizer to TiO2. Moreover, the PANI-TiO2-HA composite nanotubes synthesized by one-step at pH 0.5 with 1% volume ratio of ANI to TTIP exhibit higher visible light photocatalytic activity than those synthesized by the two-step. Heterogeneous PANI-TiO2-HA composite nanotubes prepared at pH 0.5 exhibit a higher degradation activity than that prepared at pH 1.5. The redoped experiment proves that the PANI redox state plays the main contribution to the enhanced visible light catalytic degradation efficiency of PANI-TiO2-HA prepared at pH 0.5. Furthermore, the heterogeneous PANI-crystalline TiO2-HA nanotubes have good photocatalytic stability and can be reused four times with only gradual loss of activity under visible light irradiation. Copyright © 2015 Elsevier Inc. All rights reserved.

  16. A novel method for direct fabrication of ferromolybdenum using molybdenite via self-propagation high temperature synthesis

    International Nuclear Information System (INIS)

    Golmakani, M.H.; Vahdati khaki, J.; Babakhani, A.

    2017-01-01

    Direct production of ferromolybdenum from molybdenite (MoS 2 ), in the presence of lime as a desulfurizing reagent using combustion synthesis process is investigated. Thermodynamic calculations and measurement of the adiabatic temperature of the reaction denoted that the process is in agreement with the Merzhanov criterion for self-sustaining processes. The experimental results indicated a relatively complete separation between the molten metal droplets and the co-existing slag. The slag and metal phases were characterized by X-ray diffraction, electron microscopy and wet chemical analysis techniques. It was found that sulfur is mainly distributed into the slag in the form of solid calcium sulfide (CaS). The Lack of calcium oxide in the slag indicated a complete desulfurization reaction between lime and the sulfur in molybdenum sulfide. Characterization of the molted metal revealed that only two phases namely Fe 3 Mo 3 C and Fe 3 Mo exist in the melt. Mass balance calculations showed an Iron-molybdenum recovery greater than 85%. Analyses of the phases indicated that a significant amount of Fe 3 Mo 3 C phase (60–70 wt%) is present in ferromolybdenum molten droplets even though the raw materials were low in carbon. Chemical analysis and microstructural studies of the raw materials and the products showed that carbon is not present in sufficient quantities to produce this amount of Fe 3 Mo 3 C; therefore the structure of this phase should contain a high concentration of carbon vacancies. The deviation of Fe 3 Mo 3 C 1-x peaks in X-ray diffraction pattern compared to its standard reference peaks and a calculated 0.02% decrease in the lattice parameter of this phase are evidence of the presence of these carbon vacancies. - Highlights: • A new SHS method for direct fabrication of ferromolybdenum from MoS 2 is introduced. • Addition of CaO as an effective desulfurizing agent has been investigated. • Removing the oxidative roasting process, and sulfur gas emission

  17. A novel method for direct fabrication of ferromolybdenum using molybdenite via self-propagation high temperature synthesis

    Energy Technology Data Exchange (ETDEWEB)

    Golmakani, M.H.; Vahdati khaki, J., E-mail: vahdati@um.ac.ir; Babakhani, A.

    2017-06-15

    Direct production of ferromolybdenum from molybdenite (MoS{sub 2}), in the presence of lime as a desulfurizing reagent using combustion synthesis process is investigated. Thermodynamic calculations and measurement of the adiabatic temperature of the reaction denoted that the process is in agreement with the Merzhanov criterion for self-sustaining processes. The experimental results indicated a relatively complete separation between the molten metal droplets and the co-existing slag. The slag and metal phases were characterized by X-ray diffraction, electron microscopy and wet chemical analysis techniques. It was found that sulfur is mainly distributed into the slag in the form of solid calcium sulfide (CaS). The Lack of calcium oxide in the slag indicated a complete desulfurization reaction between lime and the sulfur in molybdenum sulfide. Characterization of the molted metal revealed that only two phases namely Fe{sub 3}Mo{sub 3}C and Fe{sub 3}Mo exist in the melt. Mass balance calculations showed an Iron-molybdenum recovery greater than 85%. Analyses of the phases indicated that a significant amount of Fe{sub 3}Mo{sub 3}C phase (60–70 wt%) is present in ferromolybdenum molten droplets even though the raw materials were low in carbon. Chemical analysis and microstructural studies of the raw materials and the products showed that carbon is not present in sufficient quantities to produce this amount of Fe{sub 3}Mo{sub 3}C; therefore the structure of this phase should contain a high concentration of carbon vacancies. The deviation of Fe{sub 3}Mo{sub 3}C{sub 1-x} peaks in X-ray diffraction pattern compared to its standard reference peaks and a calculated 0.02% decrease in the lattice parameter of this phase are evidence of the presence of these carbon vacancies. - Highlights: • A new SHS method for direct fabrication of ferromolybdenum from MoS{sub 2} is introduced. • Addition of CaO as an effective desulfurizing agent has been investigated. • Removing the

  18. Biomimetic and Aggregation-Driven Crystallization Route for Room-Temperature Material Synthesis: Growth of β-Ga2O3 Nanoparticles Using Peptide Assemblies as Nanoreactors

    Science.gov (United States)

    Lee, Sang-Yup; Gao, Xueyun; Matsui, Hiroshi

    2008-01-01

    The room temperature synthesis of β-Ga2O3 nanocrystal was examined by coupling two biomimetic crystallization techniques, the enzymatic peptide nano-assembly templating and the aggregation-driven crystallization. The catalytic template of peptide assembly nucleated and mineralized primary β-Ga2O3 crystals, and then fused them to grow single-crystalline and monodisperse nanoparticles in the cavity of the peptide assembly at room temperature. In this work, the peptide assembly was exploited as a nano-reactor with an enzymatic functionality catalyzing the hydrolysis of gallium precursors. In addition, the characteristic ring-structure of peptide assembly is expected to provide an efficient dehydration pathway and the crystallization control over the surface tension, which are advantageous for the β-Ga2O3 crystal growth. This multifunctional peptide assembly could be applied for syntheses of a variety of nanomaterials that are kinetically difficult to grow at room temperature. PMID:17302413

  19. Fabrication of intermetallic NiAl by self-propagating high-temperature synthesis reaction using aluminium nanopowder under high pressure

    CERN Document Server

    Dong Shu Shan; Cheng Hai Yong; Yang Hai Bin; Zou Guang Tian

    2002-01-01

    By using aluminium nanopowder prepared by wire electrical explosion, pure monophase NiAl compound with fine crystallites (<=10 mu m) and good densification (98% of the theoretical green density) was successfully fabricated by means of self-propagating high-temperature synthesis (SHS) under a high pressure of 50 MPa. Investigation shows that, due to the physical and chemical characteristics of the nanoparticles, the SHS reaction mode and mechanism are distinct from those when using conventional coarse-grained reactants. The SHS reaction process depends on the thermal conditions related to pressure and can occur at a dramatically low temperature of 308 sup o C, which cannot be expected in conventional SHS reaction. With increasing pressure, the SHS explosive ignition temperature (T sub i sub g) of forming NiAl decreases due to thermal and kinetic effects.

  20. Synthesis of ultrasmall CsPbBr3 nanoclusters and their transformation to highly deep-blue-emitting nanoribbons at room temperature.

    Science.gov (United States)

    Xu, Yibing; Zhang, Qiang; Lv, Longfei; Han, Wenqian; Wu, Guanhong; Yang, Dong; Dong, Angang

    2017-11-16

    Discretely sized semiconductor clusters have attracted considerable attention due to their intriguing optical properties and self-assembly behaviors. While lead halide perovskite nanostructures have been recently intensively explored, few studies have addressed perovskite clusters and their self-assembled superstructures. Here, we report the room-temperature synthesis of sub-2 nm CsPbBr 3 clusters and present strong evidence that these ultrasmall perovskite species, obtained under a wide range of reaction conditions, possess a specific size, with optical properties and self-assembly characteristics resembling those of well-known II-VI semiconductor magic-sized clusters. Unlike conventional CsPbBr 3 nanocrystals, the as-synthesized CsPbBr 3 nanoclusters spontaneously self-assemble into a hexagonally packed columnar mesophase in solution, which can be further converted to single-crystalline CsPbBr 3 quantum nanoribbons with bright deep-blue emission at room temperature. Such a conversion of CsPbBr 3 nanoclusters to nanoribbons is found to be driven by a ligand-destabilization-induced crystallization and mesophase transition process. Our study will facilitate the investigation of perovskite nanoclusters and offer new possibilities in the low-temperature synthesis of anisotropic perovskite nanostructures.

  1. 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.

  2. Low-temperature synthesis of Li{sub 7}La{sub 3}Zr{sub 2}O{sub 12} with cubic garnet-type structure

    Energy Technology Data Exchange (ETDEWEB)

    Xie, Hui [Texas Materials Institute, ETC 9.184, University of Texas at Austin, Austin, TX 78712 (United States); Li, Yutao [Texas Materials Institute, ETC 9.184, University of Texas at Austin, Austin, TX 78712 (United States); State Key Laboratory of New Ceramics and Fine Processing, Department of Materials Science and Engineering, Tsinghua University, Beijing 100084 (China); Goodenough, John B., E-mail: jgoodenough@mail.utexas.edu [Texas Materials Institute, ETC 9.184, University of Texas at Austin, Austin, TX 78712 (United States)

    2012-05-15

    Highlights: Black-Right-Pointing-Pointer One-step synthesis and its optimization of cubic garnet Li{sub 7}La{sub 3}Zr{sub 2}O{sub 12} at 750 Degree-Sign C. Black-Right-Pointing-Pointer Instability above 800 Degree-Sign C of the Al-free cubic Li{sub 7}La{sub 3}Zr{sub 2}O{sub 12}. Black-Right-Pointing-Pointer Li{sup +}-ion conductivity without adventitious Al{sup 3+}. -- Abstract: In this paper, we report the direct synthesis of Li{sub 7}La{sub 3}Zr{sub 2}O{sub 12} with the cubic garnet-type structure at low temperature with a lattice constant of 13.0035 Angstrom-Sign . The synthesis condition is optimized to be at 750 Degree-Sign C for 8 h with 30 wt% excess lithium salt. No intermediate grinding was involved in this straightforward route. Without the adventitious of Al{sup 3+}, the cubic Li{sub 7}La{sub 3}Zr{sub 2}O{sub 12} is unstable above 800 Degree-Sign C and has an ionic conductivity of the order of 10{sup -6} S cm{sup -1}.

  3. High-temperature synthesis of highly hydrothermal stable mesoporous silica and Fe-SiO2 using ionic liquid as a template

    International Nuclear Information System (INIS)

    Liu, Hong; Wang, Mengyang; Hu, Hongjiu; Liang, Yuguang; Wang, Yong; Cao, Weiran; Wang, Xiaohong

    2011-01-01

    Mesoporous silicas and Fe-SiO 2 with worm-like structures have been synthesized using a room temperature ionic liquid, 1-hexadecane-3-methylimidazolium bromide, as a template at a high aging temperature (150-190 o C) with the assistance of NaF. The hydrothermal stability of mesoporous silica was effectively improved by increasing the aging temperature and adding NaF to the synthesis gel. High hydrothermally stable mesoporous silica was obtained after being aged at 190 o C in the presence of NaF, which endured the hydrothermal treatment in boiling water at least for 10 d or steam treatment at 600 o C for 6 h. The ultra hydrothermal stability could be attributed to its high degree of polymerization of silicate. Furthermore, highly hydrothermal stable mesoporous Fe-SiO 2 has been synthesized, which still remained its mesostructure after being hydrothermally treated at 100 o C for 12 d or steam-treated at 600 o C for 6 h. -- Graphical abstract: Worm-like mesoporous silica and Fe-SiO 2 with high hydrothermal stability have been synthesized using ionic liquid 1-hexadecane-3-methylimidazolium bromide as a template under the assistance of NaF at high temperature. Display Omitted Research highlights: → Increasing aging temperature improved the hydrothermal stability of materials. →Addition of NaF enhanced the polymerization degree of silicates. → Mesoporous SiO 2 and Fe-SiO 2 obtained have remarkable hydrothermal stability.

  4. Self-propagating high-temperature synthesis of La(Sr)Ga(Mg)O3-δ for electrolyte of solid oxide fuel cells

    International Nuclear Information System (INIS)

    Ishikawa, Hiroyuki; Enoki, Makiko; Ishihara, Tatsumi; Akiyama, Tomohiro

    2007-01-01

    This paper describes self-propagating high-temperature synthesis (SHS) of an electrolyte for solid oxide fuel (SOFC), in comparison to a conventional solid-state reaction method (SRM). Doped-lanthanum gallate: La 0.9 Sr 0.1 Ga 0.8 Mg 0.2 O 3-δ (LSGM9182) and LSGM9173 as the SOFC electrolyte, was prepared by the SHS and sintered at different temperatures, for measuring the electrical conductivity of the sintered LSGM and the power generating performance at 1073 K, in comparison to the SRM. In the SHS, the LSGM powders with smaller size were obtained and easily sintered at the 100 K-lower temperature, 1673 K, than in the SRM. Most significantly, the electrical conductivity of the sintered LSGM9182 was as high as 0.11 S cm -1 and its maximum power density was a value of 245 mW cm -2 in the cell configuration of Ni/LSGM9182 (0.501 mm in thickness)/Sm 0.5 Sr 0.5 CoO 3 . The conclusion was that the proposed SHS-sintering method with many benefits of minimizing the energy requirement and the processing time in the production, easing temperature restriction for the sintering, and improving the electrolyte performance up to a conventional level is practicable for producing the LSGM-electrolyte of SOFC at an intermediate-temperature application

  5. Synthesis of POSS-based ionic conductors with low glass transition temperatures for efficient solid-state dye-sensitized solar cells.

    Science.gov (United States)

    Zhang, Wei; Wang, Zhong-Sheng

    2014-07-09

    Replacing liquid-state electrolytes with solid-state electrolytes has been proven to be an effective way to improve the durability of dye-sensitized solar cells (DSSCs). We report herein the synthesis of amorphous ionic conductors based on polyhedral oligomeric silsesquioxane (POSS) with low glass transition temperatures for solid-state DSSCs. As the ionic conductor is amorphous and in the elastomeric state at the operating temperature of DSSCs, good pore filling in the TiO2 film and good interfacial contact between the solid-state electrolyte and the TiO2 film can be guaranteed. When the POSS-based ionic conductor containing an allyl group is doped with only iodine as the solid-state electrolyte without any other additives, power conversion efficiency of 6.29% has been achieved with good long-term stability under one-sun soaking for 1000 h.

  6. Synthesis of aluminum oxide by the polymer precursor method (Pechini) in 4: 1 ratio of citric acid: metal cation: calcination temperature effect

    International Nuclear Information System (INIS)

    Silva, M.C.; Lira, H.L.; Ribeiro, P.C.; Freitas, N.L.

    2014-01-01

    The technology field is nanopowders prominent in science since these materials fall in various sectors regarding their applications. This work aims at the synthesis of aluminum oxide by polymeric precursors in 4:1 ratio of citric acid:metal cation and evaluate the influence of calcination temperature on their structural and morphological characteristics. The samples after reaction were characterized by XRD and thermal analysis. After calcination 500-1200°C the samples were characterized by XRD, SEM and particle size distribution. The results showed that the variation of the calcination temperature is sufficient to achieve a same material with different structural and morphological characteristics. The most stable phase aluminum oxide arose only after calcination at 1100°C, below 900°C, the amorphous material appeared. As regards the morphology, the change was not as significant as compared to the structure. (author)

  7. Synthesis of Li{sub 2}SiO{sub 3} at low temperature; Sintesis de Li{sub 2}SiO{sub 3} a baja temperatura

    Energy Technology Data Exchange (ETDEWEB)

    Mondragon G, G. [ININ, 52750 La Marquesa, Estado de Mexico (Mexico)

    2007-07-01

    The main objective of this work is to develop a new synthesis method to obtain one of the more studied ceramics in this field Li{sub 2}SiO{sub 3}) in a simple and economic way using different solutions (urea and ammonium hydroxide). The particular objectives are first to prepare the Li{sub 2}SiO{sub 3} ceramic, by means of the use of the reaction conventional technique in solid state at temperatures between 800 and 900 C to compare it with the one proposed in this work and this way to observe the advantages that it would gives us the new method. Later on, the same one was synthesized lithium ceramic (Li{sub 2}SiO{sub 3}) by means of the new method at low temperature (between 80 and 90 C), using silicic acid and lithium hydroxide like precursory reagents and different solutions (urea and ammonium hydroxide) for the optimization in their synthesis. Finally, it was carried out the characterization of these materials by means of X-ray diffraction (XRD), electronic microscopes (SEM and TEM), nitrogen physisorption (method BET) and thermal gravimetric analysis (TGA) to observe the differences that exist among the conventional method and the proposed method and by this way to determine the advantages of the last method. (Author)

  8. Cooperation between Catalytic and DNA-binding Domains Enhances Thermostability and Supports DNA Synthesis at Higher Temperatures by Thermostable DNA Polymerases

    Science.gov (United States)

    Pavlov, Andrey R.; Pavlova, Nadejda V.; Kozyavkin, Sergei A.; Slesarev, Alexei I.

    2012-01-01

    We have previously introduced a general kinetic approach for comparative study of processivity, thermostability, and resistance to inhibitors of DNA polymerases (Pavlov et. al., (2002) Proc. Natl. Acad. Sci. USA 99, 13510–13515). The proposed method was successfully applied to characterize hybrid DNA polymerases created by fusing catalytic DNA polymerase domains with various non-specific DNA binding domains. Here we use the developed kinetic analysis to assess basic parameters of DNA elongation by DNA polymerases and to further study the interdomain interactions in both previously constructed and new chimeric DNA polymerases. We show that connecting Helix-hairpin-Helix (HhH) domains to catalytic polymerase domains can increase thermostability, not only of DNA polymerases from extremely thermophilic species, but also of the enzyme from a faculatative thermophilic bacterium Bacillus stearothermophilus. We also demonstrate that addition of TopoV HhH domains extends efficient DNA synthesis by chimerical polymerases up to 105°C by maintaining processivity of DNA synthesis at high temperatures. We also found that reversible high-temperature structural transitions in DNA polymerases decrease the rates of binding of these enzymes to the templates. Furthermore, activation energies and pre-exponential factors of the Arrhenius equation suggest that the mechanism of electrostatic enhancement of diffusion-controlled association plays a minor role in binding templates to DNA polymerases. PMID:22320201

  9. Green synthesis of silver nanoparticles using Alternanthera dentata leaf extract at room temperature and their antimicrobial activity.

    Science.gov (United States)

    Kumar, Deenadayalan Ashok; Palanichamy, V; Roopan, Selvaraj Mohana

    2014-06-05

    A green rapid biogenic synthesis of silver nanoparticles AgNPs using Alternanthera dentata (A. dentata) aqueous extract was demonstrated in this present study. The formation of silver nanoparticles was confirmed by Surface Plasmon Resonance (SPR) at 430nm using UV-visible spectrophotometer. The reduction of silver ions to silver nanoparticles by A. dentata extract was completed within 10min. Synthesized nanoparticles were characterized using UV-visible spectroscopy; Fourier transformed infrared spectroscopy (FT-IR), X-ray diffraction (XRD), scanning electron microscopy and transmission electron microscopy (TEM). The extracellular silver nanoparticles synthesis by aqueous leaf extract demonstrates rapid, simple and inexpensive method comparable to chemical and microbial methods. The colloidal solution of silver nanoparticles were found to exhibit antibacterial activity against Escherichia coli, Pseudomonas aeruginosa, Klebsiella pneumonia and, Enterococcus faecalis. Copyright © 2014 Elsevier B.V. All rights reserved.

  10. Combined Effect of Pressure and Temperature on the Viscous Behaviour of All-Oil Drilling Fluids

    Directory of Open Access Journals (Sweden)

    Hermoso J.

    2014-12-01

    Full Text Available The overall objective of this research was to study the combined influence of pressure and temperature on the complex viscous behaviour of two oil-based drilling fluids. The oil-based fluids were formulated by dispersing selected organobentonites in mineral oil, using a high-shear mixer, at room temperature. Drilling fluid viscous flow characterization was performed with a controlled-stress rheometer, using both conventional coaxial cylinder and non-conventional geometries for High Pressure/High Temperature (HPHT measurements. The rheological data obtained confirm that a helical ribbon geometry is a very useful tool to characterise the complex viscous flow behaviour of these fluids under extreme conditions. The different viscous flow behaviours encountered for both all-oil drilling fluids, as a function of temperature, are related to changes in polymer-oil pair solvency and oil viscosity. Hence, the resulting structures have been principally attributed to changes in the effective volume fraction of disperse phase due to thermally induced processes. Bingham’s and Herschel-Bulkley’s models describe the rheological properties of these drilling fluids, at different pressures and temperatures, fairly well. It was found that Herschel-Bulkley’s model fits much better B34-based oil drilling fluid viscous flow behaviour under HPHT conditions. Yield stress values increase linearly with pressure in the range of temperature studied. The pressure influence on yielding behaviour has been associated with the compression effect of different resulting organoclay microstructures. A factorial WLF-Barus model fitted the combined effect of temperature and pressure on the plastic viscosity of both drilling fluids fairly well, being this effect mainly influenced by the piezo-viscous properties of the continuous phase.

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

    Science.gov (United States)

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

    2017-12-01

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

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

    Science.gov (United States)

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

    2018-01-01

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

  13. Novel Synthesis of Ultra-Small Dextran Coated Maghemite Nanoparticles for MRI and CT Contrast Agents via a Low Temperature Co-Precipitation Reaction.

    Science.gov (United States)

    Rabias, Ioannis; Fardis, Michael; Kehagias, Thomas; Kletsas, Dimitris; Pratsinis, Harris; Tsitrouli, Danai; Maris, Thomas G; Papavassiliou, George

    2015-01-01

    Ultra-small dextran coated maghemite nanoparticles are synthesized via a low temperature modified co-precipitation method. A monoethylene glycol/water solution of 1:1 molar ratios and a fixed apparatus is used at a constant temperature of 5-10 degrees C. The growth of nanoparticles is prohibited due to low temperature synthesis and differs from usual thermal decomposition methods via Ostwald ripening. Strict temperature control and reaction timing of less than 20 minutes are essential to maintain narrow distribution in particle size. These nanoparticles are water-dispersible and biocompatible by capping with polyethylene glycol ligands. The aqueous suspensions are tested for cytotoxic activity on normal human skin fibroblasts. There is no reduction of the cells' viability at any concentration tested, the highest being 1% v/v of the suspension in culture medium, corresponding to the highest concentrations to be administered in vivo. Initial comparison with a T1 MRI contrast agent in sale shows that maghemite nanoparticles exhibit high r1 and r2 relaxivities in MRI tomography and strong contrast in computed tomography, demonstrating that these nanoparticles can be efficient T1, T2 and CT contrast agents.

  14. Low temperature synthesis and characterization of Na–M–(O)–F phases with M=Ti, V

    Energy Technology Data Exchange (ETDEWEB)

    Nava-Avendaño, Jessica [Institut de Ciència de Materials de Barcelona (ICMAB-CSIC), Campus UAB, E-08193 Bellaterra, Catalonia (Spain); Ayllón, José A. [Departament de Química, Universitat Autònoma de Barcelona, Campus UAB, E-08193 Bellaterra, Catalonia (Spain); Frontera, Carlos; Oró-Solé, Judith [Institut de Ciència de Materials de Barcelona (ICMAB-CSIC), Campus UAB, E-08193 Bellaterra, Catalonia (Spain); Estruga, Marc [Departament de Química, Universitat Autònoma de Barcelona, Campus UAB, E-08193 Bellaterra, Catalonia (Spain); Molins, Elies [Institut de Ciència de Materials de Barcelona (ICMAB-CSIC), Campus UAB, E-08193 Bellaterra, Catalonia (Spain); Palacín, M. Rosa, E-mail: rosa.palacin@icmab.es [Institut de Ciència de Materials de Barcelona (ICMAB-CSIC), Campus UAB, E-08193 Bellaterra, Catalonia (Spain)

    2015-03-15

    Na{sub 5}Ti{sub 3}O{sub 3}F{sub 11} was prepared by the microwave assisted method, and presents a chiolite related structure with cell parameters a=10.5016(5), b=10.4025(5), and c=10.2911(5) Å and Cmca (no. 64) space group. From solvothermal synthesis at 100 °C the cryolite Na{sub 3−δ}VO{sub 1−δ}F{sub 5+δ} was prepared, which crystallizes in the monoclinic system with a=5.5403(2), b=5.6804(2), c=7.9523(2) Å, β=90.032(7)° cell parameters and P2{sub 1}/n (no. 14) space group. Under similar synthesis conditions but with higher HF concentration the chiolite-type phase Na{sub 5−δ}V{sub 3}F{sub 14} was achieved, which exhibits a=10.5482(2), b=10.4887(1) and c=10.3243(1) Å cell parameters and Cmc2{sub 1} (no. 36) space group. A single crystal also having the chiolite structure was synthesized at 200 °C which exhibits tetragonal symmetry (a=7.380(3) and c=10.381(11) Å and space group P4{sub 2}2{sub 1}2 (no. 94)). Bond valence sum indicates that it contains V{sup 4+} and therefore can be formulated as Na{sub 5}V{sub 3}O{sub 3}F{sub 11}. - Graphical abstract: Na{sub 5}M{sub 3}(O,F){sub 14} with M=Ti and V having chiolite structure and Na{sub 3−δ}VO{sub 1−δ}F{sub 5+δ} cryolite were prepared by means of microwave-assisted and solvothermal synthesis. - Highlights: • Na{sub 5}Ti{sub 3}O{sub 3}F{sub 11} chiolite was prepared by a microwave assisted method and characterized. • Na{sub 3−δ}VO{sub 1−δ}F{sub 5+δ} and Na{sub 5−δ}V{sub 3}F{sub 14} were prepared by solvothermal synthesis. • The compounds were structurally characterized by diffraction techniques. • O/F distribution was estimated by applying Pauling’s second rule.

  15. Mineralizer-assisted high-pressure high-temperature synthesis and characterization of novel phosphorus nitride imides and luminescent alkaline earth metal (oxo)nitridophosphates

    International Nuclear Information System (INIS)

    Marchuk, Alexey

    2016-01-01

    The main objectives of this thesis were the synthesis, identification and structural characterization of new alkaline earth metal (oxo)nitridophopshates and phosphorus nitrides. Furthermore, luminescence properties of the resulting materials should be investigated and a connection between these properties and the respective structures should be established. For this purpose, a range of synthesis strategies was employed, including conventional solid-state syntheses in silica ampoules and high-pressure high-temperature syntheses using the multianvil technique. The emphasis of the synthetic part of this thesis lies on the development of new synthetic strategies in order to increase crystallinity of alkaline earth metal (oxo)nitridophosphates and thus accelerate their structure determination. This involves the selection of a suitable mineralizer and the investigation of its interaction with the respective starting materials. In addition, the analytical methods applied in this thesis in order to identify and characterize the compounds are just as essential as the synthesis strategies. X-ray diffraction on single crystals and on powders was carried out as the main analytical method while being supported by quantitative and qualitative 1 H and 31 P solid-state NMR measurements, FTIR and energy-dispersive X-ray (EDX) spectroscopy, as well as electron microscopy methods including both imaging and diffraction techniques. Implied by the large number of novel structures investigated, theoretical studies including topological analysis, calculations of lattice energies and bond-valence sums also played a major role in this thesis. Optical analysis methods such as reflectance spectroscopy, luminescence microscopy and photoluminescence measurements helped to determine the luminescence properties of some of the presented compounds.

  16. Spectroscopic investigation on the chemical forms of Cu during the synthesis of zeolite X at low temperature

    International Nuclear Information System (INIS)

    Terzano, Roberto; Spagnuolo, Matteo; Medici, Luca; Tateo, Fabio; Vekemans, Bart; Janssens, Koen; Ruggiero, Pacifico

    2006-01-01

    The direct synthesis of zeolites in polluted soils has proved to be a promising process for the stabilization of metals inside these minerals. Nevertheless, more detailed information about this process is still needed in order to better foresee the fate of metals in treated soils. In this work, zeolite X has been synthesized under alkaline conditions in an aqueous solution containing 2500 mg kg -1 of Cu, starting from Na silicate and Al hydroxide at 60 deg. C. Aluminium, Si and Cu concentrations in the aqueous phase, during zeolite synthesis, were measured over a period of 160 h. The solid products have been characterized over time by XRD, SEM-EDX, ESR, FT-IR, and synchrotron radiation X-ray microbeam absorption near edge structure (μ-XANES) and extended X-ray absorption fine structure (μ-EXAFS) spectroscopy. It appears that the marked reduction of Cu concentration in solution is not only due to a simple precipitation effect, but also to processes connected with the formation of zeolite X which could entrap, inside its porous structure, nano- or micro-occlusions of precipitated Cu hydroxides and/or oxides. In addition, EXAFS observations strengthen the hypothesis of the presence of different Cu phases even at a short-range molecular level and suggest that some of these occlusions could be even bound to the zeolite framework. The results suggest that zeolite formation could be used to reduce the availability of metals in polluted soils

  17. Flash pyrolysis at high temperature of ligno-cellulosic biomass and its components - production of synthesis gas; Pyrolyse flash a haute temperature de la biomasse ligno-cellulosique et de ses composes - production de gaz de synthese

    Energy Technology Data Exchange (ETDEWEB)

    Couhert, C

    2007-11-15

    Pyrolysis is the first stage of any thermal treatment of biomass and governs the formation of synthesis gas for the production of electricity, hydrogen or liquid fuels. The objective of this work is to establish a link between the composition of a biomass and its pyrolysis gas. We study experimental flash pyrolysis and fix the conditions in which quantities of gas are maximal, while aiming at a regime without heat and mass transfer limitations (particles about 100 {mu}m): temperature of 950 C and residence time of about 2 s. Then we try to predict gas yields of any biomass according to its composition, applicable in this situation where thermodynamic equilibrium is not reached. We show that an additivity law does not allow correlating gas yields of a biomass with fractions of cellulose, hemi-cellulose and lignin contained in this biomass. Several explanations are suggested and examined: difference of pyrolytic behaviour of the same compound according to the biomass from which it is extracted, interactions between compounds and influence of mineral matter. With the aim of industrial application, we study pyrolysis of millimetric and centimetric size particles, and make a numerical simulation of the reactions of pyrolysis gases reforming. This simulation shows that the choice of biomass affects the quantities of synthesis gas obtained. (author)

  18. Room-temperature synthesis of ultraviolet-emitting nanocrystalline GaN films using photochemical vapor deposition

    International Nuclear Information System (INIS)

    Yamazaki, Shunsuke; Yatsui, Takashi; Ohtsu, Motoichi; Kim, Taw-Won; Fujioka, Hiroshi

    2004-01-01

    We fabricated UV-emitting nanocrystalline gallium nitride (GaN) films at room temperature using photochemical vapor deposition (PCVD). For the samples synthesized at room temperature with V/III ratios exceeding 5.0x10 4 , strong photoluminescence peaks at 3.365 and 3.310 eV, which can be ascribed to transitions in a mixed phase of cubic and hexagonal GaN, were observed at 5 K. A UV emission spectrum with a full width at half-maximum of 100 meV was observed, even at room temperature. In addition, x-ray photoelectron spectroscopy measurement revealed that the film deposited by PCVD at room temperature was well nitridized

  19. Room temperature large-scale synthesis of layered frameworks as low-cost 4 V cathode materials for lithium ion batteries

    Science.gov (United States)

    Hameed, A. Shahul; Reddy, M. V.; Nagarathinam, M.; Runčevski, Tomče; Dinnebier, Robert E; Adams, Stefan; Chowdari, B. V. R.; Vittal, Jagadese J.

    2015-01-01

    Li-ion batteries (LIBs) are considered as the best available technology to push forward the production of eco-friendly electric vehicles (EVs) and for the efficient utilization of renewable energy sources. Transformation from conventional vehicles to EVs are hindered by the high upfront price of the EVs and are mainly due to the high cost of LIBs. Hence, cost reduction of LIBs is one of the major strategies to bring forth the EVs to compete in the market with their gasoline counterparts. In our attempt to produce cheaper high-performance cathode materials for LIBs, an rGO/MOPOF (reduced graphene oxide/Metal-Organic Phosphate Open Framework) nanocomposite with ~4 V of operation has been developed by a cost effective room temperature synthesis that eliminates any expensive post-synthetic treatments at high temperature under Ar/Ar-H2. Firstly, an hydrated nanocomposite, rGO/K2[(VO)2(HPO4)2(C2O4)]·4.5H2O has been prepared by simple magnetic stirring at room temperature which releases water to form the anhydrous cathode material while drying at 90 °C during routine electrode fabrication procedure. The pristine MOPOF material undergoes highly reversible lithium storage, however with capacity fading. Enhanced lithium cycling has been witnessed with rGO/MOPOF nanocomposite which exhibits minimal capacity fading thanks to increased electronic conductivity and enhanced Li diffusivity. PMID:26593096

  20. Room temperature large-scale synthesis of layered frameworks as low-cost 4 V cathode materials for lithium ion batteries

    Science.gov (United States)

    Hameed, A. Shahul; Reddy, M. V.; Nagarathinam, M.; Runčevski, Tomče; Dinnebier, Robert E.; Adams, Stefan; Chowdari, B. V. R.; Vittal, Jagadese J.

    2015-11-01

    Li-ion batteries (LIBs) are considered as the best available technology to push forward the production of eco-friendly electric vehicles (EVs) and for the efficient utilization of renewable energy sources. Transformation from conventional vehicles to EVs are hindered by the high upfront price of the EVs and are mainly due to the high cost of LIBs. Hence, cost reduction of LIBs is one of the major strategies to bring forth the EVs to compete in the market with their gasoline counterparts. In our attempt to produce cheaper high-performance cathode materials for LIBs, an rGO/MOPOF (reduced graphene oxide/Metal-Organic Phosphate Open Framework) nanocomposite with ~4 V of operation has been developed by a cost effective room temperature synthesis that eliminates any expensive post-synthetic treatments at high temperature under Ar/Ar-H2. Firstly, an hydrated nanocomposite, rGO/K2[(VO)2(HPO4)2(C2O4)]·4.5H2O has been prepared by simple magnetic stirring at room temperature which releases water to form the anhydrous cathode material while drying at 90 °C during routine electrode fabrication procedure. The pristine MOPOF material undergoes highly reversible lithium storage, however with capacity fading. Enhanced lithium cycling has been witnessed with rGO/MOPOF nanocomposite which exhibits minimal capacity fading thanks to increased electronic conductivity and enhanced Li diffusivity.